data_chinmin4_c2byc
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C55 H37 B Cl F27 Ir N5 O'
_chemical_formula_weight 1535.36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ir' 'Ir' -1.4442 7.9887
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'C 2/c '
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 29.5110(16)
_cell_length_b 13.3179(7)
_cell_length_c 32.1453(17)
_cell_angle_alpha 90.00
_cell_angle_beta 109.255(3)
_cell_angle_gamma 90.00
_cell_volume 11927.2(11)
_cell_formula_units_Z 8
_cell_measurement_temperature 170(2)
_cell_measurement_reflns_used 8284
_cell_measurement_theta_min 2.288
_cell_measurement_theta_max 23.849
_exptl_crystal_description 'Plates'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.710
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 6016
_exptl_absorpt_coefficient_mu 2.412
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.5133
_exptl_absorpt_correction_T_max 0.9013
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 170(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 40150
_diffrn_reflns_av_R_equivalents 0.0527
_diffrn_reflns_av_sigmaI/netI 0.0588
_diffrn_reflns_limit_h_min -35
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -38
_diffrn_reflns_limit_l_max 38
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.00
_reflns_number_total 10497
_reflns_number_gt 7764
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10497
_refine_ls_number_parameters 870
_refine_ls_number_restraints 34
_refine_ls_R_factor_all 0.0804
_refine_ls_R_factor_gt 0.0509
_refine_ls_wR_factor_ref 0.1536
_refine_ls_wR_factor_gt 0.1341
_refine_ls_goodness_of_fit_ref 1.011
_refine_ls_restrained_S_all 1.010
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.707075(10) 0.66025(2) 0.811750(8) 0.03116(12) Uani 1 1 d . . .
Cl1 Cl 0.75138(7) 0.76719(15) 0.77970(6) 0.0478(5) Uani 1 1 d . . .
N1 N 0.7608(2) 0.4648(4) 0.80625(17) 0.0318(13) Uani 1 1 d . . .
N2 N 0.7654(2) 0.5610(4) 0.82123(18) 0.0359(14) Uani 1 1 d . . .
C3 C 0.8126(3) 0.5781(6) 0.8358(3) 0.044(2) Uani 1 1 d . . .
H3 H 0.8268 0.6399 0.8483 0.053 Uiso 1 1 calc R . .
C4 C 0.8384(3) 0.4956(7) 0.8304(3) 0.047(2) Uani 1 1 d . . .
H4 H 0.8723 0.4895 0.8383 0.056 Uiso 1 1 calc R . .
C5 C 0.8046(3) 0.4248(6) 0.8112(2) 0.0424(19) Uani 1 1 d . . .
H5 H 0.8106 0.3591 0.8027 0.051 Uiso 1 1 calc R . .
C1A C 0.7132(2) 0.4221(5) 0.7857(2) 0.0313(15) Uani 1 1 d . . .
H1A1 H 0.6958 0.4205 0.8073 0.038 Uiso 1 1 calc R . .
H1A2 H 0.7161 0.3523 0.7762 0.038 Uiso 1 1 calc R . .
N1' N 0.64701(19) 0.5486(4) 0.68440(17) 0.0325(13) Uani 1 1 d . . .
N2' N 0.6576(2) 0.6264(5) 0.71322(18) 0.0341(14) Uani 1 1 d . . .
N3' N 0.6805(2) 0.5834(4) 0.75142(18) 0.0322(13) Uani 1 1 d . . .
C4' C 0.6863(2) 0.4833(5) 0.7473(2) 0.0279(15) Uani 1 1 d . . .
C5' C 0.6649(2) 0.4599(5) 0.7044(2) 0.0313(16) Uani 1 1 d . . .
H5' H 0.6628 0.3956 0.6911 0.038 Uiso 1 1 calc R . .
C6' C 0.6230(2) 0.5664(6) 0.6383(2) 0.0374(18) Uani 1 1 d . A .
C7' C 0.6323(3) 0.5073(7) 0.6081(2) 0.049(2) Uani 1 1 d . . .
H7' H 0.6555 0.4554 0.6174 0.058 Uiso 1 1 calc R . .
C8' C 0.6082(3) 0.5214(9) 0.5633(3) 0.066(3) Uani 1 1 d . A .
H8' H 0.6142 0.4788 0.5420 0.080 Uiso 1 1 calc R . .
C9' C 0.5756(4) 0.5980(9) 0.5507(3) 0.068(3) Uani 1 1 d D . .
C10' C 0.5664(4) 0.6565(9) 0.5808(4) 0.077(3) Uani 1 1 d . A .
H10' H 0.5430 0.7082 0.5713 0.092 Uiso 1 1 calc R . .
C11' C 0.5903(3) 0.6434(7) 0.6259(3) 0.054(2) Uani 1 1 d . . .
H11' H 0.5842 0.6860 0.6472 0.065 Uiso 1 1 calc R A .
C12P C 0.5489(7) 0.6278(15) 0.5041(5) 0.066(5) Uani 0.50 1 d PDU A 1
F1P F 0.5664(13) 0.576(2) 0.4775(13) 0.133(12) Uani 0.50 1 d PDU A 1
F2P F 0.5515(9) 0.7240(17) 0.4941(11) 0.113(7) Uani 0.50 1 d PDU A 1
F3P F 0.5024(7) 0.6058(13) 0.4917(5) 0.079(5) Uani 0.50 1 d PDU A 1
C12Q C 0.5511(10) 0.595(2) 0.5018(5) 0.118(14) Uani 0.50 1 d PDU A 2
F1Q F 0.5621(14) 0.675(2) 0.4865(13) 0.27(3) Uani 0.50 1 d PDU A 2
F2Q F 0.5562(19) 0.528(3) 0.4762(18) 0.204(19) Uani 0.50 1 d PDU A 2
F3Q F 0.5063(12) 0.601(3) 0.4928(13) 0.220(16) Uani 0.50 1 d PDU A 2
C1B C 0.6378(3) 0.6814(6) 0.8199(2) 0.0412(19) Uani 1 1 d . . .
C2B C 0.6673(2) 0.6135(6) 0.8533(2) 0.0329(16) Uani 1 1 d . . .
C3B C 0.7087(3) 0.6688(5) 0.8797(2) 0.0387(18) Uani 1 1 d . . .
C4B C 0.7056(3) 0.7657(6) 0.8614(3) 0.0449(19) Uani 1 1 d . . .
C5B C 0.6620(3) 0.7740(5) 0.8257(3) 0.0433(19) Uani 1 1 d . . .
C6B C 0.5914(3) 0.6547(7) 0.7869(3) 0.055(2) Uani 1 1 d . . .
H6B1 H 0.5653 0.6716 0.7983 0.082 Uiso 1 1 calc R . .
H6B2 H 0.5907 0.5825 0.7808 0.082 Uiso 1 1 calc R . .
H6B3 H 0.5872 0.6922 0.7597 0.082 Uiso 1 1 calc R . .
C7BC C 0.6531(3) 0.5084(6) 0.8630(3) 0.0434(19) Uani 1 1 d . . .
H7B1 H 0.6366 0.5124 0.8849 0.065 Uiso 1 1 calc R . .
H7B2 H 0.6820 0.4669 0.8747 0.065 Uiso 1 1 calc R . .
H7B3 H 0.6317 0.4782 0.8359 0.065 Uiso 1 1 calc R . .
C8B C 0.7481(3) 0.6283(7) 0.9187(3) 0.052(2) Uani 1 1 d . . .
H8B1 H 0.7769 0.6700 0.9242 0.078 Uiso 1 1 calc R . .
H8B2 H 0.7555 0.5592 0.9127 0.078 Uiso 1 1 calc R . .
H8B3 H 0.7378 0.6294 0.9447 0.078 Uiso 1 1 calc R . .
C9B C 0.7406(4) 0.8513(6) 0.8799(3) 0.070(3) Uani 1 1 d . . .
H9B1 H 0.7454 0.8893 0.8556 0.104 Uiso 1 1 calc R . .
H9B2 H 0.7714 0.8240 0.8987 0.104 Uiso 1 1 calc R . .
H9B3 H 0.7275 0.8959 0.8974 0.104 Uiso 1 1 calc R . .
C10B C 0.6438(4) 0.8681(7) 0.7988(3) 0.070(3) Uani 1 1 d . . .
H10A H 0.6401 0.9219 0.8182 0.105 Uiso 1 1 calc R . .
H10B H 0.6128 0.8542 0.7763 0.105 Uiso 1 1 calc R . .
H10C H 0.6669 0.8891 0.7844 0.105 Uiso 1 1 calc R . .
B1C B 0.5964(3) 0.1468(6) 0.8942(2) 0.0306(18) Uani 1 1 d . . .
C11C C 0.5839(2) 0.0263(5) 0.8921(2) 0.0317(16) Uani 1 1 d . . .
C12C C 0.5421(3) -0.0112(6) 0.8609(2) 0.0382(17) Uani 1 1 d . . .
H12C H 0.5203 0.0345 0.8418 0.046 Uiso 1 1 calc R . .
C13C C 0.5315(3) -0.1132(7) 0.8570(3) 0.049(2) Uani 1 1 d . . .
C14C C 0.5627(3) -0.1817(7) 0.8851(3) 0.056(2) Uani 1 1 d . . .
H14C H 0.5553 -0.2513 0.8832 0.067 Uiso 1 1 calc R . .
C15C C 0.6045(3) -0.1466(6) 0.9156(3) 0.048(2) Uani 1 1 d . . .
C16C C 0.6150(3) -0.0458(6) 0.9182(2) 0.0378(18) Uani 1 1 d . . .
H16C H 0.6447 -0.0241 0.9385 0.045 Uiso 1 1 calc R . .
C17C C 0.4866(4) -0.1480(8) 0.8243(4) 0.073(3) Uani 1 1 d . . .
C18C C 0.6366(4) -0.2168(7) 0.9469(3) 0.062(3) Uani 1 1 d . . .
F171 F 0.4754(4) -0.1015(9) 0.7866(3) 0.184(6) Uani 1 1 d . . .
F172 F 0.4843(2) -0.2433(6) 0.8157(3) 0.129(3) Uani 1 1 d . . .
F173 F 0.4484(2) -0.1316(6) 0.8361(3) 0.128(3) Uani 1 1 d . . .
F181 F 0.6330(3) -0.3117(5) 0.9338(2) 0.100(2) Uani 1 1 d . . .
F182 F 0.6318(3) -0.2156(6) 0.9864(2) 0.115(3) Uani 1 1 d . . .
F183 F 0.6836(2) -0.1962(5) 0.9556(2) 0.092(2) Uani 1 1 d . . .
C21B C 0.6310(2) 0.1805(5) 0.9421(2) 0.0234(14) Uani 1 1 d . . .
C22B C 0.6313(3) 0.1372(5) 0.9815(2) 0.0350(17) Uani 1 1 d . . .
H22C H 0.6124 0.0788 0.9801 0.042 Uiso 1 1 calc R . .
C23C C 0.6579(3) 0.1746(5) 1.0230(2) 0.0382(18) Uani 1 1 d . . .
C24C C 0.6839(3) 0.2596(6) 1.0270(2) 0.0390(18) Uani 1 1 d . . .
H24C H 0.7017 0.2848 1.0554 0.047 Uiso 1 1 calc R . .
C25C C 0.6844(3) 0.3098(6) 0.9892(2) 0.0376(18) Uani 1 1 d . . .
C26C C 0.6590(2) 0.2696(6) 0.9479(2) 0.0376(18) Uani 1 1 d . . .
H26C H 0.6606 0.3036 0.9224 0.045 Uiso 1 1 calc R . .
C27C C 0.6582(4) 0.1210(7) 1.0638(3) 0.053(2) Uani 1 1 d . . .
C28C C 0.7101(3) 0.4055(7) 0.9918(3) 0.053(2) Uani 1 1 d . . .
F271 F 0.6479(3) 0.0258(5) 1.05799(19) 0.111(3) Uani 1 1 d . . .
F272 F 0.6332(4) 0.1623(7) 1.0836(3) 0.181(6) Uani 1 1 d . . .
F273 F 0.7022(2) 0.1153(5) 1.09355(18) 0.0902(19) Uani 1 1 d . . .
F281 F 0.7463(2) 0.4186(5) 1.02925(18) 0.100(2) Uani 1 1 d . . .
F282 F 0.6832(2) 0.4849(4) 0.9841(3) 0.103(2) Uani 1 1 d . . .
F283 F 0.7329(2) 0.4120(4) 0.96210(19) 0.0776(16) Uani 1 1 d . . .
C31C C 0.6210(2) 0.1602(5) 0.8554(2) 0.0280(15) Uani 1 1 d . . .
C32C C 0.6698(2) 0.1445(5) 0.8635(2) 0.0268(15) Uani 1 1 d . . .
H32C H 0.6900 0.1322 0.8929 0.032 Uiso 1 1 calc R . .
C33C C 0.6898(2) 0.1462(5) 0.8299(2) 0.0279(15) Uani 1 1 d . . .
C34C C 0.6621(3) 0.1635(5) 0.7869(2) 0.0332(16) Uani 1 1 d . . .
H34C H 0.6758 0.1632 0.7640 0.040 Uiso 1 1 calc R . .
C35C C 0.6134(2) 0.1815(6) 0.7779(2) 0.0379(18) Uani 1 1 d . B .
C36C C 0.5933(2) 0.1793(5) 0.8116(2) 0.0333(17) Uani 1 1 d . . .
H36C H 0.5599 0.1912 0.8045 0.040 Uiso 1 1 calc R . .
C37C C 0.7420(2) 0.1294(5) 0.8399(2) 0.0323(16) Uani 1 1 d . . .
C38C C 0.5835(3) 0.2022(6) 0.7321(3) 0.056(2) Uani 1 1 d DU . .
F371 F 0.76381(14) 0.0911(3) 0.87968(14) 0.0462(11) Uani 1 1 d . . .
F372 F 0.75085(16) 0.0644(4) 0.81131(16) 0.0608(14) Uani 1 1 d . . .
F373 F 0.76603(15) 0.2137(4) 0.83791(18) 0.0608(14) Uani 1 1 d . . .
F381 F 0.5381(4) 0.1805(15) 0.7217(4) 0.047(3) Uiso 0.40 1 d PDU B 1
F382 F 0.5851(9) 0.3006(11) 0.7261(6) 0.095(5) Uiso 0.40 1 d PDU B 1
F383 F 0.5976(6) 0.1647(16) 0.7007(4) 0.069(4) Uiso 0.40 1 d PDU B 1
F384 F 0.5377(4) 0.2312(18) 0.7266(4) 0.031(3) Uiso 0.30 1 d PDU B 2
F385 F 0.6041(6) 0.2701(17) 0.7115(6) 0.055(5) Uiso 0.30 1 d PDU B 2
F386 F 0.5790(8) 0.1159(12) 0.7065(5) 0.054(4) Uiso 0.30 1 d PDU B 2
F387 F 0.5551(9) 0.2815(16) 0.7305(6) 0.067(5) Uiso 0.30 1 d PDU B 3
F388 F 0.6077(4) 0.2209(17) 0.7047(4) 0.025(3) Uiso 0.30 1 d PDU B 3
F389 F 0.5533(10) 0.1266(18) 0.7148(8) 0.090(7) Uiso 0.30 1 d PDU B 3
C41C C 0.5480(2) 0.2175(5) 0.8853(2) 0.0296(15) Uani 1 1 d . . .
C42C C 0.5457(2) 0.3120(5) 0.8672(2) 0.0312(16) Uani 1 1 d . . .
H42C H 0.5708 0.3337 0.8570 0.037 Uiso 1 1 calc R . .
C43C C 0.5070(3) 0.3770(6) 0.8634(2) 0.0412(18) Uani 1 1 d . . .
C44C C 0.4703(3) 0.3477(6) 0.8773(3) 0.044(2) Uani 1 1 d . . .
H44C H 0.4443 0.3919 0.8748 0.052 Uiso 1 1 calc R . .
C45C C 0.4713(2) 0.2537(6) 0.8951(2) 0.0387(19) Uani 1 1 d . . .
C46C C 0.5102(3) 0.1884(6) 0.8988(2) 0.0357(17) Uani 1 1 d . . .
H46C H 0.5103 0.1233 0.9109 0.043 Uiso 1 1 calc R . .
C47C C 0.5058(3) 0.4764(7) 0.8417(4) 0.063(3) Uani 1 1 d . . .
C48C C 0.4314(3) 0.2194(8) 0.9101(3) 0.056(2) Uani 1 1 d . . .
F471 F 0.5290(3) 0.5461(5) 0.8691(3) 0.129(3) Uani 1 1 d . . .
F472 F 0.5256(3) 0.4757(5) 0.8099(3) 0.104(2) Uani 1 1 d . . .
F473 F 0.4621(2) 0.5109(4) 0.8217(2) 0.0871(19) Uani 1 1 d . . .
F481 F 0.38967(19) 0.2656(5) 0.8879(3) 0.103(2) Uani 1 1 d . . .
F482 F 0.4209(2) 0.1233(5) 0.9023(2) 0.0848(19) Uani 1 1 d . . .
F483 F 0.4382(3) 0.2346(8) 0.9507(2) 0.153(4) Uani 1 1 d . . .
O1X O 0.4931(4) 0.0569(6) 0.0364(3) 0.128(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.03566(18) 0.02725(18) 0.03097(16) 0.00216(12) 0.01154(11) -0.00332(12)
Cl1 0.0548(12) 0.0408(12) 0.0499(11) 0.0092(9) 0.0202(9) -0.0123(9)
N1 0.033(3) 0.033(4) 0.027(3) -0.001(2) 0.008(2) 0.002(3)
N2 0.046(4) 0.029(4) 0.035(3) -0.001(3) 0.016(3) -0.004(3)
C3 0.030(4) 0.047(5) 0.050(5) -0.003(4) 0.005(3) -0.010(4)
C4 0.025(4) 0.062(6) 0.048(4) 0.008(4) 0.004(3) 0.000(4)
C5 0.037(4) 0.048(5) 0.039(4) 0.003(4) 0.008(3) 0.014(4)
C1A 0.033(4) 0.031(4) 0.034(4) -0.001(3) 0.016(3) -0.001(3)
N1' 0.025(3) 0.041(4) 0.030(3) 0.005(3) 0.006(2) -0.001(3)
N2' 0.029(3) 0.041(4) 0.031(3) 0.003(3) 0.008(2) -0.001(3)
N3' 0.032(3) 0.033(4) 0.033(3) 0.007(3) 0.013(3) 0.001(3)
C4' 0.028(4) 0.028(4) 0.030(3) 0.002(3) 0.013(3) -0.002(3)
C5' 0.026(4) 0.029(4) 0.038(4) 0.002(3) 0.009(3) -0.004(3)
C6' 0.029(4) 0.046(5) 0.032(4) 0.002(3) 0.003(3) -0.010(3)
C7' 0.035(4) 0.068(6) 0.039(4) 0.003(4) 0.007(3) -0.017(4)
C8' 0.054(6) 0.104(9) 0.035(4) 0.003(5) 0.006(4) -0.029(6)
C9' 0.057(6) 0.087(8) 0.043(5) 0.025(5) -0.007(5) -0.029(6)
C10' 0.053(6) 0.086(9) 0.072(7) 0.040(6) -0.004(5) 0.002(5)
C11' 0.047(5) 0.056(6) 0.052(5) 0.019(4) 0.007(4) 0.003(4)
C12P 0.061(11) 0.081(12) 0.046(14) 0.042(9) 0.006(11) -0.023(12)
F1P 0.14(2) 0.21(3) 0.028(9) 0.003(19) 0.004(15) 0.02(3)
F2P 0.127(12) 0.097(12) 0.066(11) 0.054(10) -0.036(9) -0.077(9)
F3P 0.067(9) 0.085(12) 0.045(8) 0.036(7) -0.036(7) -0.047(8)
C12Q 0.092(17) 0.15(3) 0.08(3) 0.044(14) -0.03(2) -0.08(2)
F1Q 0.33(4) 0.28(4) 0.09(3) 0.11(3) -0.11(3) -0.25(4)
F2Q 0.21(3) 0.29(4) 0.052(12) 0.00(3) -0.029(15) -0.01(3)
F3Q 0.096(18) 0.27(4) 0.23(4) 0.09(3) -0.03(2) -0.005(19)
C1B 0.036(4) 0.054(6) 0.034(4) 0.009(3) 0.012(3) 0.010(4)
C2B 0.034(4) 0.038(4) 0.032(4) 0.003(3) 0.018(3) 0.000(3)
C3B 0.052(5) 0.035(5) 0.032(4) 0.000(3) 0.017(3) 0.008(3)
C4B 0.062(5) 0.032(5) 0.048(5) -0.003(4) 0.028(4) -0.003(4)
C5B 0.059(5) 0.016(4) 0.056(5) 0.006(3) 0.019(4) 0.010(3)
C6B 0.039(5) 0.070(7) 0.055(5) 0.012(4) 0.016(4) 0.005(4)
C7BC 0.054(5) 0.036(5) 0.049(4) 0.004(4) 0.029(4) -0.008(4)
C8B 0.061(6) 0.054(6) 0.036(4) 0.002(4) 0.008(4) -0.005(4)
C9B 0.107(9) 0.038(6) 0.067(6) -0.010(4) 0.034(6) -0.020(5)
C10B 0.097(8) 0.038(6) 0.078(7) 0.020(5) 0.033(6) 0.026(5)
B1C 0.033(4) 0.036(5) 0.023(4) 0.003(3) 0.009(3) 0.005(3)
C11C 0.031(4) 0.034(4) 0.035(4) -0.002(3) 0.017(3) 0.002(3)
C12C 0.038(4) 0.038(5) 0.040(4) -0.006(3) 0.015(3) -0.005(3)
C13C 0.046(5) 0.052(6) 0.054(5) -0.018(4) 0.023(4) -0.014(4)
C14C 0.072(6) 0.041(6) 0.066(6) -0.006(4) 0.038(5) -0.008(4)
C15C 0.054(5) 0.051(6) 0.045(4) -0.006(4) 0.023(4) 0.005(4)
C16C 0.039(4) 0.040(5) 0.036(4) -0.007(3) 0.015(3) 0.003(3)
C17C 0.069(7) 0.055(7) 0.090(8) -0.018(6) 0.020(6) -0.024(5)
C18C 0.086(8) 0.051(7) 0.063(6) -0.003(5) 0.040(5) 0.009(5)
F171 0.168(9) 0.213(11) 0.099(6) 0.032(7) -0.052(6) -0.136(8)
F172 0.086(5) 0.078(5) 0.183(8) -0.055(5) -0.008(5) -0.019(4)
F173 0.060(4) 0.114(6) 0.193(9) -0.060(6) 0.019(5) -0.009(4)
F181 0.150(7) 0.045(4) 0.107(5) 0.012(3) 0.046(5) 0.036(4)
F182 0.169(7) 0.117(6) 0.076(4) 0.046(4) 0.066(5) 0.083(5)
F183 0.082(5) 0.076(4) 0.112(5) 0.026(4) 0.025(4) 0.034(4)
C21B 0.018(3) 0.025(4) 0.028(3) 0.012(3) 0.009(3) 0.012(3)
C22B 0.033(4) 0.035(5) 0.036(4) -0.002(3) 0.010(3) -0.003(3)
C23C 0.050(5) 0.034(5) 0.030(4) 0.004(3) 0.013(3) 0.003(3)
C24C 0.045(4) 0.036(5) 0.027(4) 0.001(3) -0.001(3) 0.003(3)
C25C 0.039(4) 0.035(4) 0.031(4) 0.001(3) 0.001(3) -0.003(3)
C26C 0.035(4) 0.047(5) 0.025(3) 0.001(3) 0.003(3) 0.007(3)
C27C 0.077(7) 0.050(6) 0.033(4) 0.000(4) 0.018(4) -0.008(5)
C28C 0.061(6) 0.047(6) 0.041(5) 0.003(4) 0.004(4) -0.014(4)
F271 0.181(7) 0.086(5) 0.052(3) 0.027(3) 0.018(4) -0.039(5)
F272 0.254(11) 0.227(11) 0.134(7) 0.139(7) 0.160(8) 0.179(9)
F273 0.097(5) 0.115(5) 0.046(3) 0.028(3) 0.007(3) 0.005(4)
F281 0.111(5) 0.097(5) 0.056(3) 0.011(3) -0.023(3) -0.061(4)
F282 0.087(4) 0.031(3) 0.182(7) -0.008(4) 0.031(5) -0.003(3)
F283 0.086(4) 0.066(4) 0.078(4) 0.006(3) 0.025(3) -0.026(3)
C31C 0.028(4) 0.029(4) 0.024(3) -0.005(3) 0.006(3) -0.003(3)
C32C 0.023(3) 0.032(4) 0.022(3) 0.001(3) 0.003(3) 0.004(3)
C33C 0.028(4) 0.024(4) 0.031(3) 0.002(3) 0.008(3) 0.003(3)
C34C 0.036(4) 0.039(4) 0.027(3) -0.005(3) 0.014(3) -0.008(3)
C35C 0.028(4) 0.053(5) 0.030(4) 0.002(3) 0.007(3) 0.005(3)
C36C 0.023(4) 0.048(5) 0.025(3) -0.005(3) 0.003(3) 0.002(3)
C37C 0.028(4) 0.034(4) 0.036(4) -0.002(3) 0.011(3) 0.003(3)
C38C 0.054(6) 0.073(7) 0.041(5) 0.011(4) 0.018(4) 0.008(5)
F371 0.028(2) 0.059(3) 0.049(3) 0.010(2) 0.0092(19) 0.015(2)
F372 0.040(3) 0.082(4) 0.066(3) -0.025(3) 0.025(2) 0.009(2)
F373 0.036(3) 0.047(3) 0.094(4) 0.018(3) 0.014(2) -0.013(2)
C41C 0.029(4) 0.035(4) 0.023(3) -0.003(3) 0.007(3) 0.005(3)
C42C 0.022(3) 0.033(4) 0.036(4) -0.005(3) 0.008(3) 0.002(3)
C43C 0.036(4) 0.044(5) 0.040(4) -0.007(4) 0.007(3) 0.004(4)
C44C 0.026(4) 0.051(6) 0.055(5) -0.021(4) 0.015(3) -0.005(3)
C45C 0.020(4) 0.054(6) 0.040(4) -0.017(4) 0.008(3) -0.009(3)
C46C 0.032(4) 0.039(5) 0.032(4) -0.011(3) 0.006(3) -0.006(3)
C47C 0.039(5) 0.050(6) 0.103(8) 0.010(6) 0.028(5) 0.012(4)
C48C 0.044(5) 0.061(7) 0.071(6) -0.016(5) 0.028(5) -0.015(5)
F471 0.147(7) 0.034(4) 0.151(7) 0.003(4) -0.022(5) -0.013(4)
F472 0.108(5) 0.080(5) 0.153(6) 0.056(4) 0.082(5) 0.041(4)
F473 0.058(3) 0.074(4) 0.127(5) 0.038(4) 0.027(3) 0.032(3)
F481 0.040(3) 0.075(5) 0.201(8) 0.011(4) 0.050(4) 0.004(3)
F482 0.059(4) 0.066(4) 0.146(6) 0.003(4) 0.056(4) -0.012(3)
F483 0.132(7) 0.268(12) 0.101(5) -0.085(6) 0.094(5) -0.123(7)
O1X 0.216(11) 0.056(5) 0.142(8) 0.031(5) 0.102(8) 0.013(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N3' 2.102(6) . ?
Ir1 N2 2.111(6) . ?
Ir1 C4B 2.138(8) . ?
Ir1 C2B 2.140(6) . ?
Ir1 C5B 2.158(7) . ?
Ir1 C1B 2.165(8) . ?
Ir1 C3B 2.172(7) . ?
Ir1 Cl1 2.3848(19) . ?
N1 C5 1.357(9) . ?
N1 N2 1.360(8) . ?
N1 C1A 1.456(8) . ?
N2 C3 1.335(9) . ?
C3 C4 1.379(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.364(11) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.475(9) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.356(8) . ?
N1' C5' 1.366(9) . ?
N1' C6' 1.435(8) . ?
N2' N3' 1.321(7) . ?
N3' C4' 1.356(9) . ?
C4' C5' 1.349(9) . ?
C5' H5' 0.9500 . ?
C6' C7' 1.347(11) . ?
C6' C11' 1.374(11) . ?
C7' C8' 1.392(11) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.368(15) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.339(16) . ?
C9' C12P 1.500(16) . ?
C9' C12Q 1.501(16) . ?
C10' C11' 1.399(13) . ?
C10' H10' 0.9500 . ?
C11' H11' 0.9500 . ?
C12P F2P 1.329(13) . ?
C12P F3P 1.330(13) . ?
C12P F1P 1.329(13) . ?
C12Q F2Q 1.26(2) . ?
C12Q F1Q 1.26(2) . ?
C12Q F3Q 1.26(2) . ?
C1B C5B 1.406(11) . ?
C1B C2B 1.453(10) . ?
C1B C6B 1.473(11) . ?
C2B C3B 1.439(10) . ?
C2B C7BC 1.524(10) . ?
C3B C4B 1.409(10) . ?
C3B C8B 1.500(11) . ?
C4B C5B 1.420(11) . ?
C4B C9B 1.521(12) . ?
C5B C10B 1.517(11) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7BC H7B1 0.9800 . ?
C7BC H7B2 0.9800 . ?
C7BC H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C21B 1.605(10) . ?
B1C C11C 1.644(11) . ?
B1C C31C 1.648(10) . ?
B1C C41C 1.654(10) . ?
C11C C12C 1.399(10) . ?
C11C C16C 1.400(10) . ?
C12C C13C 1.390(11) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.395(13) . ?
C13C C17C 1.470(13) . ?
C14C C15C 1.380(13) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.374(11) . ?
C15C C18C 1.466(13) . ?
C16C H16C 0.9500 . ?
C17C F172 1.296(11) . ?
C17C F171 1.302(14) . ?
C17C F173 1.321(13) . ?
C18C F182 1.325(10) . ?
C18C F181 1.326(11) . ?
C18C F183 1.350(12) . ?
C21B C22B 1.389(9) . ?
C21B C26C 1.423(10) . ?
C22B C23C 1.398(10) . ?
C22B H22C 0.9500 . ?
C23C C24C 1.349(10) . ?
C23C C27C 1.490(11) . ?
C24C C25C 1.393(10) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.398(9) . ?
C25C C28C 1.472(11) . ?
C26C H26C 0.9500 . ?
C27C F272 1.251(11) . ?
C27C F271 1.302(10) . ?
C27C F273 1.338(10) . ?
C28C F282 1.296(10) . ?
C28C F281 1.332(9) . ?
C28C F283 1.339(10) . ?
C31C C32C 1.393(9) . ?
C31C C36C 1.398(9) . ?
C32C C33C 1.392(9) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.373(9) . ?
C33C C37C 1.483(9) . ?
C34C C35C 1.389(10) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.394(10) . ?
C35C C38C 1.473(10) . ?
C36C H36C 0.9500 . ?
C37C F371 1.329(8) . ?
C37C F373 1.342(8) . ?
C37C F372 1.350(8) . ?
C38C F381 1.301(10) . ?
C38C F383 1.310(11) . ?
C38C F382 1.327(11) . ?
C38C F388 1.329(11) . ?
C38C F387 1.338(12) . ?
C38C F389 1.338(12) . ?
C38C F384 1.358(11) . ?
C38C F385 1.375(11) . ?
C38C F386 1.393(11) . ?
C41C C42C 1.378(10) . ?
C41C C46C 1.382(10) . ?
C42C C43C 1.405(10) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.357(11) . ?
C43C C47C 1.492(12) . ?
C44C C45C 1.373(11) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.413(10) . ?
C45C C48C 1.483(11) . ?
C46C H46C 0.9500 . ?
C47C F471 1.308(12) . ?
C47C F473 1.319(10) . ?
C47C F472 1.333(11) . ?
C48C F483 1.270(10) . ?
C48C F482 1.321(11) . ?
C48C F481 1.351(11) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3' Ir1 N2 82.3(2) . . ?
N3' Ir1 C4B 156.3(3) . . ?
N2 Ir1 C4B 121.3(3) . . ?
N3' Ir1 C2B 108.7(2) . . ?
N2 Ir1 C2B 108.4(2) . . ?
C4B Ir1 C2B 64.8(3) . . ?
N3' Ir1 C5B 117.7(3) . . ?
N2 Ir1 C5B 159.8(3) . . ?
C4B Ir1 C5B 38.6(3) . . ?
C2B Ir1 C5B 64.7(3) . . ?
N3' Ir1 C1B 95.5(3) . . ?
N2 Ir1 C1B 145.3(3) . . ?
C4B Ir1 C1B 64.6(3) . . ?
C2B Ir1 C1B 39.5(3) . . ?
C5B Ir1 C1B 38.0(3) . . ?
N3' Ir1 C3B 146.2(3) . . ?
N2 Ir1 C3B 98.1(2) . . ?
C4B Ir1 C3B 38.1(3) . . ?
C2B Ir1 C3B 39.0(3) . . ?
C5B Ir1 C3B 64.3(3) . . ?
C1B Ir1 C3B 65.2(3) . . ?
N3' Ir1 Cl1 89.01(16) . . ?
N2 Ir1 Cl1 84.23(17) . . ?
C4B Ir1 Cl1 94.5(2) . . ?
C2B Ir1 Cl1 159.2(2) . . ?
C5B Ir1 Cl1 97.7(2) . . ?
C1B Ir1 Cl1 130.5(2) . . ?
C3B Ir1 Cl1 124.7(2) . . ?
C5 N1 N2 110.5(6) . . ?
C5 N1 C1A 129.7(6) . . ?
N2 N1 C1A 119.7(5) . . ?
C3 N2 N1 104.8(6) . . ?
C3 N2 Ir1 130.6(5) . . ?
N1 N2 Ir1 123.9(4) . . ?
N2 C3 C4 112.0(7) . . ?
N2 C3 H3 124.0 . . ?
C4 C3 H3 124.0 . . ?
C5 C4 C3 104.9(7) . . ?
C5 C4 H4 127.6 . . ?
C3 C4 H4 127.6 . . ?
N1 C5 C4 107.9(7) . . ?
N1 C5 H5 126.1 . . ?
C4 C5 H5 126.1 . . ?
N1 C1A C4' 109.7(6) . . ?
N1 C1A H1A1 109.7 . . ?
C4' C1A H1A1 109.7 . . ?
N1 C1A H1A2 109.7 . . ?
C4' C1A H1A2 109.7 . . ?
H1A1 C1A H1A2 108.2 . . ?
N2' N1' C5' 111.9(5) . . ?
N2' N1' C6' 120.2(6) . . ?
C5' N1' C6' 127.7(6) . . ?
N3' N2' N1' 103.7(6) . . ?
N2' N3' C4' 112.2(6) . . ?
N2' N3' Ir1 124.6(5) . . ?
C4' N3' Ir1 123.2(4) . . ?
C5' C4' N3' 107.2(6) . . ?
C5' C4' C1A 132.0(7) . . ?
N3' C4' C1A 120.8(6) . . ?
C4' C5' N1' 105.0(6) . . ?
C4' C5' H5' 127.5 . . ?
N1' C5' H5' 127.5 . . ?
C7' C6' C11' 121.1(7) . . ?
C7' C6' N1' 120.0(7) . . ?
C11' C6' N1' 118.9(7) . . ?
C6' C7' C8' 120.8(9) . . ?
C6' C7' H7' 119.6 . . ?
C8' C7' H7' 119.6 . . ?
C9' C8' C7' 118.3(10) . . ?
C9' C8' H8' 120.8 . . ?
C7' C8' H8' 120.8 . . ?
C10' C9' C8' 120.8(9) . . ?
C10' C9' C12P 113.7(13) . . ?
C8' C9' C12P 125.4(13) . . ?
C10' C9' C12Q 129.1(16) . . ?
C8' C9' C12Q 109.7(16) . . ?
C12P C9' C12Q 17.4(17) . . ?
C9' C10' C11' 121.5(10) . . ?
C9' C10' H10' 119.3 . . ?
C11' C10' H10' 119.3 . . ?
C6' C11' C10' 117.4(9) . . ?
C6' C11' H11' 121.3 . . ?
C10' C11' H11' 121.3 . . ?
F2P C12P F3P 106.1(12) . . ?
F2P C12P F1P 106.2(13) . . ?
F3P C12P F1P 106.0(13) . . ?
F2P C12P C9' 116(2) . . ?
F3P C12P C9' 113.0(13) . . ?
F1P C12P C9' 109(2) . . ?
F2Q C12Q F1Q 104.1(16) . . ?
F2Q C12Q F3Q 103.9(16) . . ?
F1Q C12Q F3Q 103.9(16) . . ?
F2Q C12Q C9' 126(4) . . ?
F1Q C12Q C9' 107(3) . . ?
F3Q C12Q C9' 110(3) . . ?
C5B C1B C2B 107.1(7) . . ?
C5B C1B C6B 128.2(7) . . ?
C2B C1B C6B 124.8(7) . . ?
C5B C1B Ir1 70.8(4) . . ?
C2B C1B Ir1 69.3(4) . . ?
C6B C1B Ir1 124.9(6) . . ?
C3B C2B C1B 107.7(6) . . ?
C3B C2B C7BC 125.9(6) . . ?
C1B C2B C7BC 125.8(7) . . ?
C3B C2B Ir1 71.7(4) . . ?
C1B C2B Ir1 71.2(4) . . ?
C7BC C2B Ir1 129.8(5) . . ?
C4B C3B C2B 107.3(7) . . ?
C4B C3B C8B 127.1(7) . . ?
C2B C3B C8B 125.6(7) . . ?
C4B C3B Ir1 69.6(4) . . ?
C2B C3B Ir1 69.3(4) . . ?
C8B C3B Ir1 125.1(6) . . ?
C3B C4B C5B 109.0(7) . . ?
C3B C4B C9B 125.6(8) . . ?
C5B C4B C9B 125.1(8) . . ?
C3B C4B Ir1 72.2(4) . . ?
C5B C4B Ir1 71.5(4) . . ?
C9B C4B Ir1 127.4(6) . . ?
C1B C5B C4B 108.9(6) . . ?
C1B C5B C10B 125.5(8) . . ?
C4B C5B C10B 125.5(8) . . ?
C1B C5B Ir1 71.3(4) . . ?
C4B C5B Ir1 69.9(4) . . ?
C10B C5B Ir1 126.0(6) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7BC H7B1 109.5 . . ?
C2B C7BC H7B2 109.5 . . ?
H7B1 C7BC H7B2 109.5 . . ?
C2B C7BC H7B3 109.5 . . ?
H7B1 C7BC H7B3 109.5 . . ?
H7B2 C7BC H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C21B B1C C11C 112.1(5) . . ?
C21B B1C C31C 113.4(6) . . ?
C11C B1C C31C 102.9(5) . . ?
C21B B1C C41C 104.4(5) . . ?
C11C B1C C41C 112.3(6) . . ?
C31C B1C C41C 112.1(5) . . ?
C12C C11C C16C 115.7(7) . . ?
C12C C11C B1C 120.7(6) . . ?
C16C C11C B1C 123.4(6) . . ?
C13C C12C C11C 122.2(7) . . ?
C13C C12C H12C 118.9 . . ?
C11C C12C H12C 118.9 . . ?
C12C C13C C14C 119.9(8) . . ?
C12C C13C C17C 119.8(9) . . ?
C14C C13C C17C 120.3(9) . . ?
C15C C14C C13C 118.9(8) . . ?
C15C C14C H14C 120.5 . . ?
C13C C14C H14C 120.5 . . ?
C16C C15C C14C 120.2(8) . . ?
C16C C15C C18C 120.0(8) . . ?
C14C C15C C18C 119.7(9) . . ?
C15C C16C C11C 122.9(7) . . ?
C15C C16C H16C 118.5 . . ?
C11C C16C H16C 118.5 . . ?
F172 C17C F171 106.8(11) . . ?
F172 C17C F173 103.5(9) . . ?
F171 C17C F173 102.2(12) . . ?
F172 C17C C13C 115.6(10) . . ?
F171 C17C C13C 114.1(9) . . ?
F173 C17C C13C 113.2(10) . . ?
F182 C18C F181 107.1(8) . . ?
F182 C18C F183 103.0(9) . . ?
F181 C18C F183 103.2(8) . . ?
F182 C18C C15C 113.6(8) . . ?
F181 C18C C15C 115.2(9) . . ?
F183 C18C C15C 113.6(8) . . ?
C22B C21B C26C 113.5(6) . . ?
C22B C21B B1C 124.7(6) . . ?
C26C C21B B1C 121.1(6) . . ?
C21B C22B C23C 123.8(7) . . ?
C21B C22B H22C 118.1 . . ?
C23C C22B H22C 118.1 . . ?
C24C C23C C22B 120.8(7) . . ?
C24C C23C C27C 118.6(7) . . ?
C22B C23C C27C 120.6(7) . . ?
C23C C24C C25C 119.3(7) . . ?
C23C C24C H24C 120.4 . . ?
C25C C24C H24C 120.4 . . ?
C24C C25C C26C 119.3(7) . . ?
C24C C25C C28C 121.3(7) . . ?
C26C C25C C28C 119.4(7) . . ?
C25C C26C C21B 123.3(7) . . ?
C25C C26C H26C 118.3 . . ?
C21B C26C H26C 118.3 . . ?
F272 C27C F271 110.6(10) . . ?
F272 C27C F273 104.9(8) . . ?
F271 C27C F273 100.0(8) . . ?
F272 C27C C23C 113.9(8) . . ?
F271 C27C C23C 114.0(7) . . ?
F273 C27C C23C 112.3(8) . . ?
F282 C28C F281 108.9(8) . . ?
F282 C28C F283 103.4(7) . . ?
F281 C28C F283 101.2(7) . . ?
F282 C28C C25C 115.0(8) . . ?
F281 C28C C25C 114.2(7) . . ?
F283 C28C C25C 112.7(7) . . ?
C32C C31C C36C 116.2(6) . . ?
C32C C31C B1C 121.8(6) . . ?
C36C C31C B1C 121.8(6) . . ?
C33C C32C C31C 121.9(6) . . ?
C33C C32C H32C 119.1 . . ?
C31C C32C H32C 119.1 . . ?
C34C C33C C32C 121.3(6) . . ?
C34C C33C C37C 118.4(6) . . ?
C32C C33C C37C 120.3(6) . . ?
C33C C34C C35C 118.0(6) . . ?
C33C C34C H34C 121.0 . . ?
C35C C34C H34C 121.0 . . ?
C34C C35C C36C 120.7(6) . . ?
C34C C35C C38C 118.6(6) . . ?
C36C C35C C38C 120.7(6) . . ?
C35C C36C C31C 121.9(6) . . ?
C35C C36C H36C 119.1 . . ?
C31C C36C H36C 119.1 . . ?
F371 C37C F373 105.8(5) . . ?
F371 C37C F372 105.5(6) . . ?
F373 C37C F372 106.2(6) . . ?
F371 C37C C33C 114.0(6) . . ?
F373 C37C C33C 113.1(6) . . ?
F372 C37C C33C 111.7(6) . . ?
F381 C38C F383 106.1(11) . . ?
F381 C38C F382 105.4(12) . . ?
F383 C38C F382 103.2(13) . . ?
F381 C38C F388 127.2(10) . . ?
F383 C38C F388 35.3(8) . . ?
F382 C38C F388 70.5(11) . . ?
F381 C38C F387 65.7(12) . . ?
F383 C38C F387 128.6(12) . . ?
F382 C38C F387 42.9(11) . . ?
F388 C38C F387 107.0(13) . . ?
F381 C38C F389 40.4(12) . . ?
F383 C38C F389 74.3(14) . . ?
F382 C38C F389 137.1(15) . . ?
F388 C38C F389 107.1(15) . . ?
F387 C38C F389 104.8(16) . . ?
F381 C38C F384 30.2(7) . . ?
F383 C38C F384 124.2(11) . . ?
F382 C38C F384 77.4(12) . . ?
F388 C38C F384 126.2(10) . . ?
F387 C38C F384 35.8(9) . . ?
F389 C38C F384 70.3(15) . . ?
F381 C38C F385 127.1(11) . . ?
F383 C38C F385 65.0(11) . . ?
F382 C38C F385 40.4(10) . . ?
F388 C38C F385 30.4(9) . . ?
F387 C38C F385 80.3(14) . . ?
F389 C38C F385 129.3(15) . . ?
F384 C38C F385 109.2(13) . . ?
F381 C38C F386 77.0(11) . . ?
F383 C38C F386 39.1(9) . . ?
F382 C38C F386 136.8(13) . . ?
F388 C38C F386 74.3(11) . . ?
F387 C38C F386 133.8(13) . . ?
F389 C38C F386 38.1(12) . . ?
F384 C38C F386 105.1(13) . . ?
F385 C38C F386 103.2(13) . . ?
F381 C38C C35C 116.3(8) . . ?
F383 C38C C35C 117.4(9) . . ?
F382 C38C C35C 107.0(10) . . ?
F388 C38C C35C 114.9(8) . . ?
F387 C38C C35C 110.4(10) . . ?
F389 C38C C35C 111.9(12) . . ?
F384 C38C C35C 115.2(8) . . ?
F385 C38C C35C 113.0(9) . . ?
F386 C38C C35C 110.1(9) . . ?
C42C C41C C46C 117.0(6) . . ?
C42C C41C B1C 120.9(6) . . ?
C46C C41C B1C 121.8(6) . . ?
C41C C42C C43C 121.7(7) . . ?
C41C C42C H42C 119.1 . . ?
C43C C42C H42C 119.1 . . ?
C44C C43C C42C 120.5(8) . . ?
C44C C43C C47C 120.7(7) . . ?
C42C C43C C47C 118.7(7) . . ?
C43C C44C C45C 119.3(7) . . ?
C43C C44C H44C 120.3 . . ?
C45C C44C H44C 120.3 . . ?
C44C C45C C46C 120.1(7) . . ?
C44C C45C C48C 120.4(7) . . ?
C46C C45C C48C 119.5(8) . . ?
C41C C46C C45C 121.3(7) . . ?
C41C C46C H46C 119.4 . . ?
C45C C46C H46C 119.4 . . ?
F471 C47C F473 107.0(8) . . ?
F471 C47C F472 105.0(9) . . ?
F473 C47C F472 103.5(9) . . ?
F471 C47C C43C 112.9(9) . . ?
F473 C47C C43C 113.8(8) . . ?
F472 C47C C43C 113.8(8) . . ?
F483 C48C F482 107.2(9) . . ?
F483 C48C F481 106.1(9) . . ?
F482 C48C F481 103.0(7) . . ?
F483 C48C C45C 114.4(7) . . ?
F482 C48C C45C 113.5(7) . . ?
F481 C48C C45C 111.8(8) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 C3 -0.7(7) . . . . ?
C1A N1 N2 C3 -176.9(6) . . . . ?
C5 N1 N2 Ir1 170.5(5) . . . . ?
C1A N1 N2 Ir1 -5.8(8) . . . . ?
N3' Ir1 N2 C3 133.8(7) . . . . ?
C4B Ir1 N2 C3 -47.8(7) . . . . ?
C2B Ir1 N2 C3 -119.0(7) . . . . ?
C5B Ir1 N2 C3 -52.5(11) . . . . ?
C1B Ir1 N2 C3 -137.6(7) . . . . ?
C3B Ir1 N2 C3 -80.3(7) . . . . ?
Cl1 Ir1 N2 C3 44.0(6) . . . . ?
N3' Ir1 N2 N1 -34.9(5) . . . . ?
C4B Ir1 N2 N1 143.5(5) . . . . ?
C2B Ir1 N2 N1 72.2(5) . . . . ?
C5B Ir1 N2 N1 138.7(7) . . . . ?
C1B Ir1 N2 N1 53.6(7) . . . . ?
C3B Ir1 N2 N1 111.0(5) . . . . ?
Cl1 Ir1 N2 N1 -124.7(5) . . . . ?
N1 N2 C3 C4 0.1(8) . . . . ?
Ir1 N2 C3 C4 -170.2(5) . . . . ?
N2 C3 C4 C5 0.5(9) . . . . ?
N2 N1 C5 C4 1.0(8) . . . . ?
C1A N1 C5 C4 176.8(6) . . . . ?
C3 C4 C5 N1 -0.9(9) . . . . ?
C5 N1 C1A C4' -117.0(8) . . . . ?
N2 N1 C1A C4' 58.4(7) . . . . ?
C5' N1' N2' N3' -2.5(7) . . . . ?
C6' N1' N2' N3' -177.9(6) . . . . ?
N1' N2' N3' C4' 2.6(7) . . . . ?
N1' N2' N3' Ir1 -179.2(4) . . . . ?
N2 Ir1 N3' N2' -139.9(5) . . . . ?
C4B Ir1 N3' N2' 43.5(9) . . . . ?
C2B Ir1 N3' N2' 113.2(5) . . . . ?
C5B Ir1 N3' N2' 42.6(6) . . . . ?
C1B Ir1 N3' N2' 75.0(5) . . . . ?
C3B Ir1 N3' N2' 127.0(6) . . . . ?
Cl1 Ir1 N3' N2' -55.6(5) . . . . ?
N2 Ir1 N3' C4' 38.2(5) . . . . ?
C4B Ir1 N3' C4' -138.4(7) . . . . ?
C2B Ir1 N3' C4' -68.7(6) . . . . ?
C5B Ir1 N3' C4' -139.3(5) . . . . ?
C1B Ir1 N3' C4' -106.9(5) . . . . ?
C3B Ir1 N3' C4' -54.9(7) . . . . ?
Cl1 Ir1 N3' C4' 122.5(5) . . . . ?
N2' N3' C4' C5' -1.7(7) . . . . ?
Ir1 N3' C4' C5' 180.0(4) . . . . ?
N2' N3' C4' C1A 176.8(6) . . . . ?
Ir1 N3' C4' C1A -1.5(8) . . . . ?
N1 C1A C4' C5' 123.3(8) . . . . ?
N1 C1A C4' N3' -54.8(8) . . . . ?
N3' C4' C5' N1' 0.1(7) . . . . ?
C1A C4' C5' N1' -178.2(7) . . . . ?
N2' N1' C5' C4' 1.5(7) . . . . ?
C6' N1' C5' C4' 176.5(6) . . . . ?
N2' N1' C6' C7' 147.6(7) . . . . ?
C5' N1' C6' C7' -27.0(11) . . . . ?
N2' N1' C6' C11' -33.3(10) . . . . ?
C5' N1' C6' C11' 152.1(7) . . . . ?
C11' C6' C7' C8' -1.3(12) . . . . ?
N1' C6' C7' C8' 177.9(7) . . . . ?
C6' C7' C8' C9' 1.3(13) . . . . ?
C7' C8' C9' C10' -1.5(14) . . . . ?
C7' C8' C9' C12P 175.9(11) . . . . ?
C7' C8' C9' C12Q -175.5(13) . . . . ?
C8' C9' C10' C11' 1.6(16) . . . . ?
C12P C9' C10' C11' -176.1(11) . . . . ?
C12Q C9' C10' C11' 174.3(16) . . . . ?
C7' C6' C11' C10' 1.3(12) . . . . ?
N1' C6' C11' C10' -177.9(7) . . . . ?
C9' C10' C11' C6' -1.4(14) . . . . ?
C10' C9' C12P F2P 50.3(18) . . . . ?
C8' C9' C12P F2P -127.2(14) . . . . ?
C12Q C9' C12P F2P -155(7) . . . . ?
C10' C9' C12P F3P -72.7(17) . . . . ?
C8' C9' C12P F3P 109.7(15) . . . . ?
C12Q C9' C12P F3P 82(7) . . . . ?
C10' C9' C12P F1P 169.9(14) . . . . ?
C8' C9' C12P F1P -7.6(16) . . . . ?
C12Q C9' C12P F1P -36(6) . . . . ?
C10' C9' C12Q F2Q -168(3) . . . . ?
C8' C9' C12Q F2Q 6(3) . . . . ?
C12P C9' C12Q F2Q 162(7) . . . . ?
C10' C9' C12Q F1Q 70(3) . . . . ?
C8' C9' C12Q F1Q -116(2) . . . . ?
C12P C9' C12Q F1Q 40(6) . . . . ?
C10' C9' C12Q F3Q -42(3) . . . . ?
C8' C9' C12Q F3Q 131(2) . . . . ?
C12P C9' C12Q F3Q -73(6) . . . . ?
N3' Ir1 C1B C5B -129.5(4) . . . . ?
N2 Ir1 C1B C5B 146.0(5) . . . . ?
C4B Ir1 C1B C5B 37.1(4) . . . . ?
C2B Ir1 C1B C5B 117.6(6) . . . . ?
C3B Ir1 C1B C5B 79.4(5) . . . . ?
Cl1 Ir1 C1B C5B -36.1(5) . . . . ?
N3' Ir1 C1B C2B 112.9(4) . . . . ?
N2 Ir1 C1B C2B 28.4(7) . . . . ?
C4B Ir1 C1B C2B -80.6(5) . . . . ?
C5B Ir1 C1B C2B -117.6(6) . . . . ?
C3B Ir1 C1B C2B -38.2(4) . . . . ?
Cl1 Ir1 C1B C2B -153.7(3) . . . . ?
N3' Ir1 C1B C6B -5.8(7) . . . . ?
N2 Ir1 C1B C6B -90.3(7) . . . . ?
C4B Ir1 C1B C6B 160.7(8) . . . . ?
C2B Ir1 C1B C6B -118.7(9) . . . . ?
C5B Ir1 C1B C6B 123.7(8) . . . . ?
C3B Ir1 C1B C6B -157.0(8) . . . . ?
Cl1 Ir1 C1B C6B 87.6(7) . . . . ?
C5B C1B C2B C3B 1.8(8) . . . . ?
C6B C1B C2B C3B -178.3(7) . . . . ?
Ir1 C1B C2B C3B 62.8(5) . . . . ?
C5B C1B C2B C7BC 172.9(7) . . . . ?
C6B C1B C2B C7BC -7.2(12) . . . . ?
Ir1 C1B C2B C7BC -126.0(7) . . . . ?
C5B C1B C2B Ir1 -61.1(5) . . . . ?
C6B C1B C2B Ir1 118.9(8) . . . . ?
N3' Ir1 C2B C3B 167.8(4) . . . . ?
N2 Ir1 C2B C3B 79.8(4) . . . . ?
C4B Ir1 C2B C3B -36.8(4) . . . . ?
C5B Ir1 C2B C3B -79.7(5) . . . . ?
C1B Ir1 C2B C3B -116.8(6) . . . . ?
Cl1 Ir1 C2B C3B -45.5(8) . . . . ?
N3' Ir1 C2B C1B -75.5(5) . . . . ?
N2 Ir1 C2B C1B -163.4(4) . . . . ?
C4B Ir1 C2B C1B 79.9(5) . . . . ?
C5B Ir1 C2B C1B 37.1(5) . . . . ?
C3B Ir1 C2B C1B 116.8(6) . . . . ?
Cl1 Ir1 C2B C1B 71.3(7) . . . . ?
N3' Ir1 C2B C7BC 45.9(7) . . . . ?
N2 Ir1 C2B C7BC -42.0(7) . . . . ?
C4B Ir1 C2B C7BC -158.7(7) . . . . ?
C5B Ir1 C2B C7BC 158.5(7) . . . . ?
C1B Ir1 C2B C7BC 121.4(9) . . . . ?
C3B Ir1 C2B C7BC -121.9(8) . . . . ?
Cl1 Ir1 C2B C7BC -167.3(4) . . . . ?
C1B C2B C3B C4B -3.0(8) . . . . ?
C7BC C2B C3B C4B -174.1(7) . . . . ?
Ir1 C2B C3B C4B 59.5(5) . . . . ?
C1B C2B C3B C8B 178.4(7) . . . . ?
C7BC C2B C3B C8B 7.3(12) . . . . ?
Ir1 C2B C3B C8B -119.1(8) . . . . ?
C1B C2B C3B Ir1 -62.5(5) . . . . ?
C7BC C2B C3B Ir1 126.4(7) . . . . ?
N3' Ir1 C3B C4B -139.7(5) . . . . ?
N2 Ir1 C3B C4B 132.0(5) . . . . ?
C2B Ir1 C3B C4B -118.6(7) . . . . ?
C5B Ir1 C3B C4B -37.7(5) . . . . ?
C1B Ir1 C3B C4B -79.9(5) . . . . ?
Cl1 Ir1 C3B C4B 43.4(5) . . . . ?
N3' Ir1 C3B C2B -21.1(7) . . . . ?
N2 Ir1 C3B C2B -109.4(4) . . . . ?
C4B Ir1 C3B C2B 118.6(7) . . . . ?
C5B Ir1 C3B C2B 80.9(5) . . . . ?
C1B Ir1 C3B C2B 38.7(4) . . . . ?
Cl1 Ir1 C3B C2B 162.0(3) . . . . ?
N3' Ir1 C3B C8B 98.6(8) . . . . ?
N2 Ir1 C3B C8B 10.3(7) . . . . ?
C4B Ir1 C3B C8B -121.7(9) . . . . ?
C2B Ir1 C3B C8B 119.7(8) . . . . ?
C5B Ir1 C3B C8B -159.4(8) . . . . ?
C1B Ir1 C3B C8B 158.4(8) . . . . ?
Cl1 Ir1 C3B C8B -78.3(7) . . . . ?
C2B C3B C4B C5B 3.1(9) . . . . ?
C8B C3B C4B C5B -178.3(8) . . . . ?
Ir1 C3B C4B C5B 62.4(6) . . . . ?
C2B C3B C4B C9B 177.0(8) . . . . ?
C8B C3B C4B C9B -4.4(13) . . . . ?
Ir1 C3B C4B C9B -123.6(9) . . . . ?
C2B C3B C4B Ir1 -59.3(5) . . . . ?
C8B C3B C4B Ir1 119.3(8) . . . . ?
N3' Ir1 C4B C3B 116.6(7) . . . . ?
N2 Ir1 C4B C3B -59.5(5) . . . . ?
C2B Ir1 C4B C3B 37.6(5) . . . . ?
C5B Ir1 C4B C3B 117.9(7) . . . . ?
C1B Ir1 C4B C3B 81.4(5) . . . . ?
Cl1 Ir1 C4B C3B -145.5(4) . . . . ?
N3' Ir1 C4B C5B -1.3(9) . . . . ?
N2 Ir1 C4B C5B -177.4(4) . . . . ?
C2B Ir1 C4B C5B -80.3(5) . . . . ?
C1B Ir1 C4B C5B -36.4(4) . . . . ?
C3B Ir1 C4B C5B -117.9(7) . . . . ?
Cl1 Ir1 C4B C5B 96.6(4) . . . . ?
N3' Ir1 C4B C9B -121.8(9) . . . . ?
N2 Ir1 C4B C9B 62.1(8) . . . . ?
C2B Ir1 C4B C9B 159.2(9) . . . . ?
C5B Ir1 C4B C9B -120.5(10) . . . . ?
C1B Ir1 C4B C9B -157.0(9) . . . . ?
C3B Ir1 C4B C9B 121.6(10) . . . . ?
Cl1 Ir1 C4B C9B -23.9(8) . . . . ?
C2B C1B C5B C4B 0.1(9) . . . . ?
C6B C1B C5B C4B -179.8(8) . . . . ?
Ir1 C1B C5B C4B -60.0(6) . . . . ?
C2B C1B C5B C10B -178.5(8) . . . . ?
C6B C1B C5B C10B 1.6(14) . . . . ?
Ir1 C1B C5B C10B 121.4(9) . . . . ?
C2B C1B C5B Ir1 60.2(5) . . . . ?
C6B C1B C5B Ir1 -119.8(8) . . . . ?
C3B C4B C5B C1B -2.0(9) . . . . ?
C9B C4B C5B C1B -176.0(8) . . . . ?
Ir1 C4B C5B C1B 60.9(6) . . . . ?
C3B C4B C5B C10B 176.6(8) . . . . ?
C9B C4B C5B C10B 2.6(14) . . . . ?
Ir1 C4B C5B C10B -120.5(9) . . . . ?
C3B C4B C5B Ir1 -62.9(5) . . . . ?
C9B C4B C5B Ir1 123.1(8) . . . . ?
N3' Ir1 C5B C1B 60.2(5) . . . . ?
N2 Ir1 C5B C1B -112.7(8) . . . . ?
C4B Ir1 C5B C1B -119.2(6) . . . . ?
C2B Ir1 C5B C1B -38.5(4) . . . . ?
C3B Ir1 C5B C1B -81.9(5) . . . . ?
Cl1 Ir1 C5B C1B 153.1(4) . . . . ?
N3' Ir1 C5B C4B 179.4(4) . . . . ?
N2 Ir1 C5B C4B 6.5(10) . . . . ?
C2B Ir1 C5B C4B 80.7(5) . . . . ?
C1B Ir1 C5B C4B 119.2(6) . . . . ?
C3B Ir1 C5B C4B 37.3(5) . . . . ?
Cl1 Ir1 C5B C4B -87.7(4) . . . . ?
N3' Ir1 C5B C10B -60.6(8) . . . . ?
N2 Ir1 C5B C10B 126.5(9) . . . . ?
C4B Ir1 C5B C10B 120.0(10) . . . . ?
C2B Ir1 C5B C10B -159.3(9) . . . . ?
C1B Ir1 C5B C10B -120.8(10) . . . . ?
C3B Ir1 C5B C10B 157.3(9) . . . . ?
Cl1 Ir1 C5B C10B 32.3(8) . . . . ?
C21B B1C C11C C12C 155.7(6) . . . . ?
C31C B1C C11C C12C -82.2(7) . . . . ?
C41C B1C C11C C12C 38.6(8) . . . . ?
C21B B1C C11C C16C -29.3(9) . . . . ?
C31C B1C C11C C16C 92.8(7) . . . . ?
C41C B1C C11C C16C -146.4(6) . . . . ?
C16C C11C C12C C13C 1.9(10) . . . . ?
B1C C11C C12C C13C 177.2(7) . . . . ?
C11C C12C C13C C14C 0.8(12) . . . . ?
C11C C12C C13C C17C 178.8(8) . . . . ?
C12C C13C C14C C15C -1.7(12) . . . . ?
C17C C13C C14C C15C -179.7(9) . . . . ?
C13C C14C C15C C16C -0.1(12) . . . . ?
C13C C14C C15C C18C 177.0(8) . . . . ?
C14C C15C C16C C11C 2.9(12) . . . . ?
C18C C15C C16C C11C -174.1(7) . . . . ?
C12C C11C C16C C15C -3.8(10) . . . . ?
B1C C11C C16C C15C -179.0(7) . . . . ?
C12C C13C C17C F172 165.0(10) . . . . ?
C14C C13C C17C F172 -17.0(15) . . . . ?
C12C C13C C17C F171 40.5(15) . . . . ?
C14C C13C C17C F171 -141.5(11) . . . . ?
C12C C13C C17C F173 -75.9(12) . . . . ?
C14C C13C C17C F173 102.1(11) . . . . ?
C16C C15C C18C F182 77.2(12) . . . . ?
C14C C15C C18C F182 -99.8(11) . . . . ?
C16C C15C C18C F181 -158.8(8) . . . . ?
C14C C15C C18C F181 24.2(13) . . . . ?
C16C C15C C18C F183 -40.1(11) . . . . ?
C14C C15C C18C F183 142.9(9) . . . . ?
C11C B1C C21B C22B -31.8(9) . . . . ?
C31C B1C C21B C22B -147.8(6) . . . . ?
C41C B1C C21B C22B 90.0(8) . . . . ?
C11C B1C C21B C26C 158.6(6) . . . . ?
C31C B1C C21B C26C 42.7(8) . . . . ?
C41C B1C C21B C26C -79.6(7) . . . . ?
C26C C21B C22B C23C -2.4(10) . . . . ?
B1C C21B C22B C23C -172.6(7) . . . . ?
C21B C22B C23C C24C 2.7(12) . . . . ?
C21B C22B C23C C27C -177.0(7) . . . . ?
C22B C23C C24C C25C -0.5(12) . . . . ?
C27C C23C C24C C25C 179.3(8) . . . . ?
C23C C24C C25C C26C -1.8(12) . . . . ?
C23C C24C C25C C28C 176.8(8) . . . . ?
C24C C25C C26C C21B 2.0(11) . . . . ?
C28C C25C C26C C21B -176.6(7) . . . . ?
C22B C21B C26C C25C 0.0(10) . . . . ?
B1C C21B C26C C25C 170.6(7) . . . . ?
C24C C23C C27C F272 75.7(12) . . . . ?
C22B C23C C27C F272 -104.6(11) . . . . ?
C24C C23C C27C F271 -156.2(8) . . . . ?
C22B C23C C27C F271 23.6(12) . . . . ?
C24C C23C C27C F273 -43.4(11) . . . . ?
C22B C23C C27C F273 136.3(8) . . . . ?
C24C C25C C28C F282 -101.6(9) . . . . ?
C26C C25C C28C F282 76.9(11) . . . . ?
C24C C25C C28C F281 25.4(13) . . . . ?
C26C C25C C28C F281 -156.0(8) . . . . ?
C24C C25C C28C F283 140.2(8) . . . . ?
C26C C25C C28C F283 -41.2(11) . . . . ?
C21B B1C C31C C32C 34.9(9) . . . . ?
C11C B1C C31C C32C -86.4(7) . . . . ?
C41C B1C C31C C32C 152.8(6) . . . . ?
C21B B1C C31C C36C -150.8(6) . . . . ?
C11C B1C C31C C36C 87.9(7) . . . . ?
C41C B1C C31C C36C -32.9(9) . . . . ?
C36C C31C C32C C33C -1.0(10) . . . . ?
B1C C31C C32C C33C 173.7(6) . . . . ?
C31C C32C C33C C34C 0.0(10) . . . . ?
C31C C32C C33C C37C 179.8(6) . . . . ?
C32C C33C C34C C35C 1.3(10) . . . . ?
C37C C33C C34C C35C -178.5(6) . . . . ?
C33C C34C C35C C36C -1.6(11) . . . . ?
C33C C34C C35C C38C 178.8(7) . . . . ?
C34C C35C C36C C31C 0.7(11) . . . . ?
C38C C35C C36C C31C -179.8(7) . . . . ?
C32C C31C C36C C35C 0.6(10) . . . . ?
B1C C31C C36C C35C -174.0(7) . . . . ?
C34C C33C C37C F371 -165.4(6) . . . . ?
C32C C33C C37C F371 14.8(9) . . . . ?
C34C C33C C37C F373 73.7(8) . . . . ?
C32C C33C C37C F373 -106.1(7) . . . . ?
C34C C33C C37C F372 -45.9(9) . . . . ?
C32C C33C C37C F372 134.2(7) . . . . ?
C34C C35C C38C F381 154.2(12) . . . . ?
C36C C35C C38C F381 -25.4(15) . . . . ?
C34C C35C C38C F383 26.9(16) . . . . ?
C36C C35C C38C F383 -152.7(13) . . . . ?
C34C C35C C38C F382 -88.4(14) . . . . ?
C36C C35C C38C F382 92.0(15) . . . . ?
C34C C35C C38C F388 -12.5(15) . . . . ?
C36C C35C C38C F388 167.9(12) . . . . ?
C34C C35C C38C F387 -133.7(15) . . . . ?
C36C C35C C38C F387 46.7(17) . . . . ?
C34C C35C C38C F389 110.0(18) . . . . ?
C36C C35C C38C F389 -69.6(19) . . . . ?
C34C C35C C38C F384 -172.3(13) . . . . ?
C36C C35C C38C F384 8.2(16) . . . . ?
C34C C35C C38C F385 -45.8(16) . . . . ?
C36C C35C C38C F385 134.6(15) . . . . ?
C34C C35C C38C F386 69.1(14) . . . . ?
C36C C35C C38C F386 -110.5(13) . . . . ?
C21B B1C C41C C42C 86.5(7) . . . . ?
C11C B1C C41C C42C -151.8(6) . . . . ?
C31C B1C C41C C42C -36.6(8) . . . . ?
C21B B1C C41C C46C -87.9(7) . . . . ?
C11C B1C C41C C46C 33.7(8) . . . . ?
C31C B1C C41C C46C 149.0(6) . . . . ?
C46C C41C C42C C43C 1.2(10) . . . . ?
B1C C41C C42C C43C -173.6(6) . . . . ?
C41C C42C C43C C44C -0.5(11) . . . . ?
C41C C42C C43C C47C -177.4(7) . . . . ?
C42C C43C C44C C45C -0.2(11) . . . . ?
C47C C43C C44C C45C 176.7(8) . . . . ?
C43C C44C C45C C46C 0.1(11) . . . . ?
C43C C44C C45C C48C -179.3(7) . . . . ?
C42C C41C C46C C45C -1.2(9) . . . . ?
B1C C41C C46C C45C 173.4(6) . . . . ?
C44C C45C C46C C41C 0.6(10) . . . . ?
C48C C45C C46C C41C -180.0(7) . . . . ?
C44C C43C C47C F471 95.7(10) . . . . ?
C42C C43C C47C F471 -87.3(10) . . . . ?
C44C C43C C47C F473 -26.4(13) . . . . ?
C42C C43C C47C F473 150.5(8) . . . . ?
C44C C43C C47C F472 -144.7(8) . . . . ?
C42C C43C C47C F472 32.2(11) . . . . ?
C44C C45C C48C F483 -93.6(11) . . . . ?
C46C C45C C48C F483 87.0(11) . . . . ?
C44C C45C C48C F482 143.0(8) . . . . ?
C46C C45C C48C F482 -36.4(11) . . . . ?
C44C C45C C48C F481 27.0(11) . . . . ?
C46C C45C C48C F481 -152.4(7) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 2.643
_refine_diff_density_min -1.386
_refine_diff_density_rms 0.118
_iucr_refine_instructions_details
;
TITL Chinmin4_C2byc in C2/c
CELL 0.71073 29.5110 13.3179 32.1453 90.000 109.255 90.000
ZERR 8.00 0.0016 0.0007 0.0017 0.000 0.003 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H B N F Cl Ir O
UNIT 440 296 8 40 216 8 8 8
OMIT -2 0 2
OMIT 0 0 2
OMIT 2 0 2
OMIT 2 0 0
OMIT -1 1 2
OMIT 1 1 0
OMIT -1 1 1
OMIT 1 1 1
OMIT -3 50
L.S. 25
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.319 0.101 0.044
CONF
SADI 0.01 C9' C12P C9' C12Q
SADI 0.01 F1Q F2Q F2Q F3Q F3Q F1Q
SADI 0.01 F1P F2P F2P F3P F3P F1P
SADI 0.01 C12Q F1Q C12Q F2Q C12Q F3Q
SADI 0.01 C12P F1P C12P F2P C12P F3P
SADI 0.01 C38C F387 C38C F388 C38C F389
SADI 0.01 C38C F384 C38C F385 C38C F386
SADI 0.01 C38C F381 C38C F382 C38C F383
DELU 0.005 C12P F1P F2P F3P
DELU 0.005 C12Q F1Q F2Q F3Q
DELU 0.005 C38C F381 > F389
WGHT 0.100000 15.000000
FVAR 1.000000
TEMP -103.030
MOLE 1
Ir1 7 0.707075 0.660250 0.811750 11.000000 0.035660 =
0.027250 0.030970 0.002160 0.011540 -0.003320
Cl1 6 0.751381 0.767185 0.779703 11.000000 0.054800 =
0.040800 0.049860 0.009240 0.020230 -0.012260
N1 4 0.760846 0.464754 0.806253 11.000000 0.033410 =
0.033300 0.027080 -0.001470 0.007630 0.002350
N2 4 0.765391 0.560980 0.821235 11.000000 0.045570 =
0.028610 0.035280 -0.000880 0.015790 -0.004100
C3 1 0.812606 0.578147 0.835756 11.000000 0.029730 =
0.046820 0.049750 -0.003360 0.004930 -0.009550
AFIX 43
H3 2 0.826772 0.639892 0.848307 11.000000 -1.200000
AFIX 0
C4 1 0.838390 0.495638 0.830383 11.000000 0.024890 =
0.062080 0.048230 0.008400 0.004200 0.000120
AFIX 43
H4 2 0.872258 0.489504 0.838329 11.000000 -1.200000
AFIX 0
C5 1 0.804584 0.424782 0.811155 11.000000 0.036650 =
0.048390 0.038870 0.002790 0.008090 0.013550
AFIX 43
H5 2 0.810606 0.359100 0.802699 11.000000 -1.200000
AFIX 0
C1A 1 0.713237 0.422067 0.785733 11.000000 0.032780 =
0.030740 0.034160 -0.001050 0.016110 -0.000960
AFIX 23
H1A1 2 0.695808 0.420454 0.807287 11.000000 -1.200000
H1A2 2 0.716118 0.352325 0.776243 11.000000 -1.200000
AFIX 0
N1' 4 0.647009 0.548613 0.684399 11.000000 0.025210 =
0.040600 0.029740 0.005120 0.006410 -0.001030
N2' 4 0.657639 0.626398 0.713221 11.000000 0.028520 =
0.040950 0.031290 0.002810 0.007660 -0.000540
N3' 4 0.680526 0.583436 0.751417 11.000000 0.031670 =
0.033350 0.033040 0.007320 0.012580 0.001420
C4' 1 0.686311 0.483304 0.747283 11.000000 0.027760 =
0.027830 0.030310 0.001650 0.012710 -0.001720
C5' 1 0.664921 0.459875 0.704415 11.000000 0.025750 =
0.028760 0.038010 0.002480 0.008530 -0.003910
AFIX 43
H5' 2 0.662785 0.395629 0.691061 11.000000 -1.200000
AFIX 0
C6' 1 0.623014 0.566404 0.638310 11.000000 0.028960 =
0.045680 0.032100 0.002170 0.002650 -0.010100
C7' 1 0.632284 0.507325 0.608066 11.000000 0.035230 =
0.067720 0.038860 0.003430 0.007130 -0.016670
AFIX 43
H7' 2 0.655535 0.455445 0.617413 11.000000 -1.200000
AFIX 0
C8' 1 0.608199 0.521379 0.563271 11.000000 0.054220 =
0.103880 0.034710 0.003500 0.005870 -0.029070
AFIX 43
H8' 2 0.614231 0.478849 0.541955 11.000000 -1.200000
AFIX 0
C9' 1 0.575629 0.597978 0.550731 11.000000 0.056780 =
0.087290 0.043320 0.024910 -0.007220 -0.029100
C10' 1 0.566353 0.656528 0.580803 11.000000 0.052510 =
0.086370 0.072320 0.039580 -0.004350 0.001620
AFIX 43
H10' 2 0.542997 0.708168 0.571300 11.000000 -1.200000
AFIX 0
C11' 1 0.590293 0.643356 0.625916 11.000000 0.047470 =
0.055690 0.051840 0.019350 0.007050 0.002730
AFIX 43
H11' 2 0.584162 0.685967 0.647158 11.000000 -1.200000
PART 1
AFIX 0
C12P 1 0.548881 0.627793 0.504071 10.500000 0.061350 =
0.080520 0.046110 0.041680 0.005640 -0.023170
F1P 5 0.566443 0.575998 0.477488 10.500000 0.140930 =
0.212420 0.028170 0.002560 0.004440 0.016450
F2P 5 0.551507 0.724018 0.494123 10.500000 0.126650 =
0.096620 0.066490 0.054400 -0.035550 -0.076990
F3P 5 0.502375 0.605760 0.491717 10.500000 0.066630 =
0.085470 0.045360 0.035670 -0.035980 -0.046960
PART 2
C12Q 1 0.551067 0.594793 0.501772 10.500000 0.091570 =
0.146440 0.077490 0.044120 -0.025290 -0.080680
F1Q 5 0.562064 0.674531 0.486478 10.500000 0.325250 =
0.277580 0.089920 0.108180 -0.106220 -0.245100
F2Q 5 0.556161 0.527628 0.476223 10.500000 0.214340 =
0.291890 0.051570 0.001360 -0.029360 -0.014140
F3Q 5 0.506334 0.601089 0.492768 10.500000 0.096230 =
0.274060 0.226460 0.090870 -0.033350 -0.004960
PART 0
C1B 1 0.637775 0.681444 0.819921 11.000000 0.035520 =
0.054220 0.033990 0.008830 0.011550 0.009580
C2B 1 0.667325 0.613529 0.853282 11.000000 0.034490 =
0.037850 0.031560 0.003150 0.018010 -0.000290
C3B 1 0.708729 0.668770 0.879708 11.000000 0.051890 =
0.034980 0.031750 0.000250 0.017330 0.007780
C4B 1 0.705637 0.765719 0.861444 11.000000 0.061830 =
0.032180 0.047950 -0.002890 0.027770 -0.002980
C5B 1 0.661983 0.774000 0.825672 11.000000 0.058650 =
0.016010 0.055610 0.005770 0.019190 0.009880
C6B 1 0.591353 0.654720 0.786898 11.000000 0.038810 =
0.070230 0.054860 0.011960 0.015620 0.005320
AFIX 137
H6B1 2 0.565300 0.671632 0.798258 11.000000 -1.500000
H6B2 2 0.590690 0.582532 0.780815 11.000000 -1.500000
H6B3 2 0.587194 0.692225 0.759658 11.000000 -1.500000
AFIX 0
C7BC 1 0.653128 0.508359 0.863044 11.000000 0.054330 =
0.035730 0.048930 0.003940 0.028760 -0.007680
AFIX 137
H7B1 2 0.636593 0.512357 0.884896 11.000000 -1.500000
H7B2 2 0.681986 0.466859 0.874651 11.000000 -1.500000
H7B3 2 0.631675 0.478232 0.835862 11.000000 -1.500000
AFIX 0
C8B 1 0.748121 0.628311 0.918685 11.000000 0.060730 =
0.054350 0.036170 0.002040 0.008440 -0.004920
AFIX 137
H8B1 2 0.776870 0.669995 0.924176 11.000000 -1.500000
H8B2 2 0.755460 0.559155 0.912658 11.000000 -1.500000
H8B3 2 0.737762 0.629355 0.944680 11.000000 -1.500000
AFIX 0
C9B 1 0.740586 0.851320 0.879944 11.000000 0.107300 =
0.038270 0.066850 -0.009850 0.033880 -0.019530
AFIX 137
H9B1 2 0.745422 0.889293 0.855633 11.000000 -1.500000
H9B2 2 0.771369 0.823952 0.898701 11.000000 -1.500000
H9B3 2 0.727490 0.895880 0.897422 11.000000 -1.500000
AFIX 0
C10B 1 0.643824 0.868137 0.798758 11.000000 0.096660 =
0.037620 0.077950 0.020010 0.032620 0.025510
AFIX 137
H10A 2 0.640077 0.921904 0.818183 11.000000 -1.500000
H10B 2 0.612755 0.854246 0.776266 11.000000 -1.500000
H10C 2 0.666908 0.889068 0.784441 11.000000 -1.500000
AFIX 0
MOLE 2
B1C 3 0.596409 0.146829 0.894231 11.000000 0.033410 =
0.035520 0.022650 0.002510 0.008880 0.005460
C11C 1 0.583894 0.026255 0.892086 11.000000 0.030920 =
0.033940 0.034940 -0.001800 0.017140 0.002060
MOLE 3
C12C 1 0.542134 -0.011225 0.860943 11.000000 0.037960 =
0.038090 0.040170 -0.006020 0.015210 -0.004740
AFIX 43
H12C 2 0.520316 0.034527 0.841826 11.000000 -1.200000
AFIX 0
MOLE 2
C13C 1 0.531496 -0.113155 0.857032 11.000000 0.046090 =
0.051530 0.054330 -0.018490 0.022930 -0.014210
C14C 1 0.562701 -0.181653 0.885086 11.000000 0.071630 =
0.040510 0.065970 -0.005920 0.038080 -0.007680
AFIX 43
H14C 2 0.555298 -0.251279 0.883197 11.000000 -1.200000
AFIX 0
C15C 1 0.604518 -0.146620 0.915639 11.000000 0.053920 =
0.051390 0.044660 -0.005870 0.022650 0.005390
C16C 1 0.615022 -0.045814 0.918166 11.000000 0.039280 =
0.040290 0.035700 -0.006780 0.014830 0.003120
AFIX 43
H16C 2 0.644734 -0.024058 0.938521 11.000000 -1.200000
AFIX 0
C17C 1 0.486582 -0.147959 0.824260 11.000000 0.068800 =
0.054790 0.089570 -0.017990 0.020220 -0.023880
C18C 1 0.636580 -0.216805 0.946867 11.000000 0.085510 =
0.050810 0.062620 -0.002570 0.040280 0.008630
F171 5 0.475420 -0.101518 0.786590 11.000000 0.168480 =
0.213050 0.098810 0.031640 -0.051900 -0.136020
F172 5 0.484295 -0.243270 0.815723 11.000000 0.086110 =
0.078020 0.183120 -0.054620 -0.008030 -0.018520
F173 5 0.448414 -0.131584 0.836114 11.000000 0.059920 =
0.114280 0.192840 -0.059850 0.018940 -0.009120
F181 5 0.633036 -0.311731 0.933781 11.000000 0.149940 =
0.045280 0.106900 0.011520 0.046360 0.036110
F182 5 0.631767 -0.215577 0.986399 11.000000 0.169110 =
0.117330 0.076390 0.046160 0.066380 0.082720
F183 5 0.683607 -0.196244 0.955649 11.000000 0.082050 =
0.076460 0.111840 0.026150 0.025110 0.034320
C21B 1 0.631042 0.180477 0.942084 11.000000 0.017660 =
0.025390 0.028330 0.012080 0.009080 0.011800
C22B 1 0.631346 0.137186 0.981471 11.000000 0.033020 =
0.035230 0.035700 -0.002310 0.009990 -0.002750
AFIX 43
H22C 2 0.612424 0.078792 0.980118 11.000000 -1.200000
AFIX 0
C23C 1 0.657891 0.174580 1.022999 11.000000 0.049780 =
0.033810 0.030460 0.004340 0.012580 0.002620
C24C 1 0.683886 0.259575 1.027026 11.000000 0.044610 =
0.036400 0.026810 0.001150 -0.000840 0.003290
AFIX 43
H24C 2 0.701650 0.284845 1.055355 11.000000 -1.200000
AFIX 0
C25C 1 0.684377 0.309827 0.989183 11.000000 0.038800 =
0.035060 0.030820 0.000910 0.000500 -0.003330
C26C 1 0.659027 0.269642 0.947869 11.000000 0.034940 =
0.047220 0.025380 0.000670 0.002810 0.007020
AFIX 43
H26C 2 0.660559 0.303566 0.922370 11.000000 -1.200000
AFIX 0
C27C 1 0.658202 0.120973 1.063794 11.000000 0.076940 =
0.050210 0.033090 0.000160 0.018310 -0.007830
C28C 1 0.710111 0.405512 0.991798 11.000000 0.061330 =
0.047400 0.041380 0.003000 0.003790 -0.014380
F271 5 0.647912 0.025848 1.057994 11.000000 0.181190 =
0.085950 0.051810 0.027030 0.017830 -0.039490
F272 5 0.633174 0.162256 1.083624 11.000000 0.253550 =
0.226860 0.134320 0.139100 0.160500 0.178620
F273 5 0.702233 0.115334 1.093546 11.000000 0.097190 =
0.115340 0.045960 0.027860 0.007080 0.004870
F281 5 0.746323 0.418583 1.029248 11.000000 0.111130 =
0.096530 0.056340 0.010780 -0.022990 -0.061470
F282 5 0.683199 0.484860 0.984123 11.000000 0.086910 =
0.031120 0.181570 -0.008160 0.031170 -0.003220
F283 5 0.732865 0.411964 0.962099 11.000000 0.086390 =
0.066470 0.078410 0.005750 0.025030 -0.025840
C31C 1 0.620962 0.160204 0.855352 11.000000 0.028200 =
0.029420 0.024300 -0.004580 0.005670 -0.003260
C32C 1 0.669785 0.144478 0.863516 11.000000 0.022860 =
0.032170 0.022140 0.001020 0.003110 0.003770
AFIX 43
H32C 2 0.690029 0.132244 0.892880 11.000000 -1.200000
AFIX 0
C33C 1 0.689781 0.146169 0.829890 11.000000 0.027670 =
0.024120 0.031050 0.002210 0.008490 0.002510
C34C 1 0.662090 0.163490 0.786918 11.000000 0.036260 =
0.038920 0.027350 -0.005170 0.014320 -0.008030
AFIX 43
H34C 2 0.675793 0.163176 0.764005 11.000000 -1.200000
AFIX 0
C35C 1 0.613422 0.181493 0.777947 11.000000 0.028220 =
0.053460 0.029830 0.002080 0.006640 0.004550
C36C 1 0.593319 0.179336 0.811554 11.000000 0.023210 =
0.047610 0.025340 -0.004930 0.002800 0.002490
AFIX 43
H36C 2 0.559883 0.191203 0.804502 11.000000 -1.200000
AFIX 0
C37C 1 0.741976 0.129418 0.839933 11.000000 0.027880 =
0.033660 0.035610 -0.001630 0.010890 0.002680
C38C 1 0.583485 0.202216 0.732114 11.000000 0.054490 =
0.073140 0.041320 0.011490 0.018020 0.008280
F371 5 0.763807 0.091086 0.879684 11.000000 0.027540 =
0.059090 0.049450 0.009530 0.009180 0.014520
F372 5 0.750849 0.064445 0.811309 11.000000 0.040260 =
0.081500 0.066410 -0.024510 0.025420 0.009440
F373 5 0.766026 0.213746 0.837906 11.000000 0.036220 =
0.047060 0.093740 0.018250 0.014190 -0.013430
PART 1
F381 5 0.538126 0.180506 0.721690 10.400000 0.046750
F382 5 0.585086 0.300570 0.726112 10.400000 0.094560
F383 5 0.597574 0.164729 0.700745 10.400000 0.069280
PART 2
F384 5 0.537739 0.231154 0.726619 10.300000 0.031080
F385 5 0.604074 0.270078 0.711511 10.300000 0.054820
F386 5 0.579020 0.115930 0.706549 10.300000 0.054160
PART 3
F387 5 0.555120 0.281511 0.730479 10.300000 0.067010
F388 5 0.607739 0.220873 0.704700 10.300000 0.025280
F389 5 0.553290 0.126587 0.714782 10.300000 0.089510
PART 0
C41C 1 0.548027 0.217486 0.885275 11.000000 0.028860 =
0.035210 0.023280 -0.003500 0.006830 0.004670
C42C 1 0.545652 0.311973 0.867191 11.000000 0.022360 =
0.033160 0.036450 -0.005450 0.007540 0.002450
AFIX 43
H42C 2 0.570827 0.333740 0.857037 11.000000 -1.200000
AFIX 0
C43C 1 0.506975 0.376967 0.863376 11.000000 0.035890 =
0.044060 0.039790 -0.006510 0.007120 0.004400
C44C 1 0.470321 0.347747 0.877291 11.000000 0.025600 =
0.050890 0.055330 -0.021310 0.014720 -0.005400
AFIX 43
H44C 2 0.444259 0.391893 0.874756 11.000000 -1.200000
AFIX 0
C45C 1 0.471280 0.253704 0.895078 11.000000 0.020200 =
0.054480 0.040090 -0.016780 0.008240 -0.008670
C46C 1 0.510172 0.188446 0.898833 11.000000 0.031850 =
0.039220 0.032330 -0.010600 0.005770 -0.006140
AFIX 43
H46C 2 0.510297 0.123311 0.910919 11.000000 -1.200000
AFIX 0
C47C 1 0.505837 0.476444 0.841686 11.000000 0.039470 =
0.049730 0.102780 0.009990 0.028290 0.011700
C48C 1 0.431409 0.219404 0.910066 11.000000 0.043900 =
0.061350 0.070660 -0.016390 0.028140 -0.014880
F471 5 0.529027 0.546140 0.869142 11.000000 0.147310 =
0.034270 0.151290 0.003050 -0.022400 -0.013490
F472 5 0.525572 0.475698 0.809896 11.000000 0.107880 =
0.079660 0.153100 0.055900 0.081840 0.040550
F473 5 0.462119 0.510882 0.821710 11.000000 0.057730 =
0.073800 0.127230 0.038200 0.027100 0.031770
F481 5 0.389672 0.265610 0.887872 11.000000 0.039790 =
0.075400 0.201150 0.010760 0.050370 0.004320
F482 5 0.420922 0.123333 0.902286 11.000000 0.059120 =
0.065670 0.146400 0.003500 0.056410 -0.012210
F483 5 0.438165 0.234554 0.950661 11.000000 0.132300 =
0.268000 0.100930 -0.085270 0.094000 -0.123470
MOLE 3
O1X 8 0.493114 0.056859 0.036378 11.000000 0.216420 =
0.056000 0.142170 0.030860 0.101790 0.012910
HKLF 4
END
Q1 1 0.691700 0.719900 0.809400 11.000000 0.050000 2.640000
Q2 1 0.572600 0.332200 0.734800 11.000000 0.050000 1.400000
Q3 1 0.519800 0.033400 0.007900 11.000000 0.050000 1.160000
Q4 1 0.671100 0.171400 1.097500 11.000000 0.050000 0.980000
Q5 1 0.698900 0.956500 0.812400 11.000000 0.050000 0.940000
Q6 1 0.610200 0.087300 1.055700 11.000000 0.050000 0.880000
Q7 1 0.574800 0.069000 0.714600 11.000000 0.050000 0.730000
Q8 1 0.700300 0.466700 1.028800 11.000000 0.050000 0.710000
Q9 1 0.702600 0.658000 0.778200 11.000000 0.050000 0.680000
Q10 1 0.596300 0.318200 0.724300 11.000000 0.050000 0.660000
Q11 1 0.708700 0.459600 0.959600 11.000000 0.050000 0.600000
Q12 1 0.500300 -0.185700 0.787500 11.000000 0.050000 0.600000
Q13 1 0.643500 0.172200 1.098400 11.000000 0.050000 0.590000
Q14 1 0.589100 0.221300 0.706000 11.000000 0.050000 0.580000
Q15 1 0.532100 0.126500 0.727400 11.000000 0.050000 0.580000
Q16 1 0.548200 0.217600 0.715900 11.000000 0.050000 0.580000
Q17 1 0.712500 0.306200 0.813800 11.000000 0.050000 0.560000
Q18 1 0.411500 0.280000 0.919900 11.000000 0.050000 0.560000
Q19 1 0.712300 0.658300 0.854600 11.000000 0.050000 0.550000
Q20 1 0.718600 0.582600 0.792200 11.000000 0.050000 0.550000
HKLF 4
REM Chinmin4_C2byc in C2/c
REM R1= 0.0509 for 7764 Fo > 4sig(Fo) and 0.0804 for all 10497 data
REM 870 parameters refined using 34 restraints
;
#===END
data_chinmin5_p21byc
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C58 H40 B Cl3 F27 Ir N5'
_chemical_formula_weight 1629.31
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ir' 'Ir' -1.4442 7.9887
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 19.4090(8)
_cell_length_b 17.2163(8)
_cell_length_c 21.6370(10)
_cell_angle_alpha 90.00
_cell_angle_beta 112.133(2)
_cell_angle_gamma 90.00
_cell_volume 6697.3(5)
_cell_formula_units_Z 4
_cell_measurement_temperature 170(2)
_cell_measurement_reflns_used 9789
_cell_measurement_theta_min 2.254
_cell_measurement_theta_max 26.897
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'Yellow'
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.616
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3196
_exptl_absorpt_coefficient_mu 2.229
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.5701
_exptl_absorpt_correction_T_max 0.7411
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 170(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 45958
_diffrn_reflns_av_R_equivalents 0.0238
_diffrn_reflns_av_sigmaI/netI 0.0251
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 25
_diffrn_reflns_theta_min 2.67
_diffrn_reflns_theta_max 25.00
_reflns_number_total 11717
_reflns_number_gt 9929
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 11717
_refine_ls_number_parameters 915
_refine_ls_number_restraints 57
_refine_ls_R_factor_all 0.0618
_refine_ls_R_factor_gt 0.0514
_refine_ls_wR_factor_ref 0.1664
_refine_ls_wR_factor_gt 0.1575
_refine_ls_goodness_of_fit_ref 1.152
_refine_ls_restrained_S_all 1.165
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1E C 0.8505(17) 0.866(2) 0.7123(13) 0.059(8) Uiso 0.25 1 d PDU A 1
C1E' C 0.8983(16) 0.9459(17) 0.7374(12) 0.049(7) Uiso 0.25 1 d PDU A 1
Cl1E Cl 0.8076(7) 0.9437(8) 0.7623(6) 0.081(3) Uiso 0.25 1 d PDU A 1
Cl2E Cl 0.8841(9) 0.9556(10) 0.6657(8) 0.107(5) Uiso 0.25 1 d PDU A 1
Cl3E Cl 0.8186(8) 0.9166(9) 0.7498(7) 0.102(4) Uiso 0.25 1 d PDU A 1
Cl4E Cl 0.8848(7) 0.9839(9) 0.6588(6) 0.085(4) Uiso 0.25 1 d PDU A 1
C1F C 0.8034(8) 0.7926(9) 0.5394(8) 0.052(3) Uiso 0.50 1 d P . .
Cl1F Cl 0.7714(6) 0.7544(6) 0.4640(5) 0.053(2) Uiso 0.25 1 d P B 1
Cl2F Cl 0.7511(12) 0.7766(13) 0.5846(11) 0.062(5) Uiso 0.13 1 d P B 1
Cl2' Cl 0.7401(15) 0.7493(15) 0.5685(13) 0.066(6) Uiso 0.13 1 d P B 1
Cl1' Cl 0.7767(9) 0.7475(9) 0.4447(8) 0.020(3) Uiso 0.10 1 d P B 2
Cl3F Cl 0.7982(6) 0.7668(6) 0.4621(5) 0.040(2) Uiso 0.20 1 d P B 2
Cl4F Cl 0.7203(7) 0.7674(7) 0.5563(6) 0.049(3) Uiso 0.20 1 d P B 2
Ir1 Ir 0.204502(12) 0.526771(15) 0.109597(11) 0.03409(12) Uani 1 1 d . . .
Cl1 Cl 0.12386(11) 0.47643(12) 0.00470(9) 0.0573(5) Uani 1 1 d . . .
N1 N 0.2604(3) 0.3726(3) 0.1841(3) 0.0407(12) Uani 1 1 d . . .
N2 N 0.1985(3) 0.4171(3) 0.1515(2) 0.0397(12) Uani 1 1 d . . .
C3 C 0.1402(4) 0.3773(4) 0.1538(4) 0.0489(17) Uani 1 1 d . . .
C4 C 0.1653(5) 0.3087(5) 0.1880(4) 0.060(2) Uani 1 1 d . . .
H4 H 0.1354 0.2698 0.1969 0.072 Uiso 1 1 calc R . .
C5 C 0.2422(5) 0.3069(4) 0.2071(4) 0.0548(19) Uani 1 1 d . . .
C1A C 0.3331(4) 0.3994(4) 0.1912(3) 0.0419(15) Uani 1 1 d . . .
H1A1 H 0.3700 0.3581 0.2124 0.050 Uiso 1 1 calc R . .
H1A2 H 0.3464 0.4454 0.2209 0.050 Uiso 1 1 calc R . .
N1' N 0.3587(3) 0.4395(3) 0.0366(3) 0.0417(12) Uani 1 1 d . . .
N2' N 0.3019(3) 0.4869(3) 0.0325(3) 0.0427(13) Uani 1 1 d . . .
N3' N 0.2894(3) 0.4750(3) 0.0870(3) 0.0377(12) Uani 1 1 d . . .
C4' C 0.3365(3) 0.4202(4) 0.1258(3) 0.0367(14) Uani 1 1 d . . .
C5' C 0.3803(4) 0.3974(4) 0.0934(3) 0.0404(15) Uani 1 1 d . . .
H5' H 0.4185 0.3593 0.1076 0.049 Uiso 1 1 calc R . .
C6 C 0.0620(5) 0.4032(6) 0.1233(5) 0.069(2) Uani 1 1 d . . .
H6A H 0.0596 0.4526 0.1000 0.103 Uiso 1 1 calc R . .
H6B H 0.0418 0.4102 0.1582 0.103 Uiso 1 1 calc R . .
H6C H 0.0326 0.3641 0.0913 0.103 Uiso 1 1 calc R . .
C7 C 0.2965(6) 0.2460(5) 0.2442(5) 0.072(2) Uani 1 1 d . . .
H7A H 0.3151 0.2191 0.2137 0.108 Uiso 1 1 calc R . .
H7B H 0.2719 0.2085 0.2632 0.108 Uiso 1 1 calc R . .
H7C H 0.3381 0.2702 0.2802 0.108 Uiso 1 1 calc R . .
C8 C 0.3849(4) 0.4370(4) -0.0170(3) 0.0434(15) Uani 1 1 d . . .
C9 C 0.4473(7) 0.4009(9) -0.0105(5) 0.124(6) Uani 1 1 d . . .
H9 H 0.4779 0.3803 0.0316 0.149 Uiso 1 1 calc R . .
C10 C 0.4682(7) 0.3930(8) -0.0637(5) 0.115(5) Uani 1 1 d . . .
H10 H 0.5105 0.3621 -0.0589 0.138 Uiso 1 1 calc R . .
C11 C 0.4326(4) 0.4259(4) -0.1203(4) 0.0506(18) Uani 1 1 d . . .
C12 C 0.3665(6) 0.4658(5) -0.1309(5) 0.073(3) Uani 1 1 d . . .
H12 H 0.3390 0.4890 -0.1727 0.088 Uiso 1 1 calc R . .
C13 C 0.3427(6) 0.4703(5) -0.0786(5) 0.068(3) Uani 1 1 d . . .
H13 H 0.2974 0.4960 -0.0844 0.082 Uiso 1 1 calc R . .
C14 C 0.4588(5) 0.4181(5) -0.1776(5) 0.060(2) Uani 1 1 d . . .
F141 F 0.4718(4) 0.3438(3) -0.1873(3) 0.0862(17) Uani 1 1 d . . .
F142 F 0.5223(3) 0.4558(3) -0.1655(3) 0.0819(16) Uani 1 1 d . . .
F143 F 0.4108(3) 0.4443(4) -0.2350(3) 0.0793(14) Uani 1 1 d . . .
C1B C 0.1686(5) 0.6447(4) 0.0845(4) 0.0535(19) Uani 1 1 d . . .
C2B C 0.1341(4) 0.6133(5) 0.1270(4) 0.0538(19) Uani 1 1 d . . .
C3B C 0.1924(4) 0.5946(4) 0.1886(3) 0.0444(16) Uani 1 1 d . . .
C4B C 0.2617(4) 0.6122(4) 0.1835(3) 0.0391(14) Uani 1 1 d . . .
C5B C 0.2455(4) 0.6444(4) 0.1183(4) 0.0437(16) Uani 1 1 d . . .
C6B C 0.1280(7) 0.6783(6) 0.0142(5) 0.101(4) Uani 1 1 d . . .
H6B1 H 0.1238 0.7348 0.0171 0.152 Uiso 1 1 calc R . .
H6B2 H 0.0782 0.6554 -0.0055 0.152 Uiso 1 1 calc R . .
H6B3 H 0.1563 0.6660 -0.0138 0.152 Uiso 1 1 calc R . .
C7B C 0.0524(5) 0.6119(7) 0.1125(8) 0.105(4) Uani 1 1 d . . .
H7B1 H 0.0430 0.5802 0.1461 0.158 Uiso 1 1 calc R . .
H7B2 H 0.0260 0.5896 0.0682 0.158 Uiso 1 1 calc R . .
H7B3 H 0.0348 0.6650 0.1138 0.158 Uiso 1 1 calc R . .
C8B C 0.1855(7) 0.5625(6) 0.2499(5) 0.087(3) Uani 1 1 d . . .
H8B1 H 0.1903 0.6047 0.2817 0.130 Uiso 1 1 calc R . .
H8B2 H 0.2248 0.5241 0.2703 0.130 Uiso 1 1 calc R . .
H8B3 H 0.1368 0.5376 0.2382 0.130 Uiso 1 1 calc R . .
C9B C 0.3355(5) 0.6100(5) 0.2385(5) 0.079(3) Uani 1 1 d . . .
H9B1 H 0.3459 0.6605 0.2610 0.118 Uiso 1 1 calc R . .
H9B2 H 0.3737 0.5986 0.2204 0.118 Uiso 1 1 calc R . .
H9B3 H 0.3359 0.5696 0.2704 0.118 Uiso 1 1 calc R . .
C10B C 0.3019(6) 0.6751(5) 0.0925(6) 0.081(3) Uani 1 1 d . . .
H10A H 0.2893 0.7288 0.0773 0.121 Uiso 1 1 calc R . .
H10B H 0.3017 0.6429 0.0551 0.121 Uiso 1 1 calc R . .
H10C H 0.3513 0.6737 0.1281 0.121 Uiso 1 1 calc R . .
B1C B 0.2542(3) 0.9587(4) 1.0122(3) 0.0255(13) Uani 1 1 d . . .
C11C C 0.3221(3) 1.0142(3) 1.0114(3) 0.0238(11) Uani 1 1 d . . .
C12C C 0.3545(3) 1.0677(3) 1.0628(3) 0.0263(11) Uani 1 1 d . . .
H12C H 0.3381 1.0688 1.0990 0.032 Uiso 1 1 calc R . .
C13C C 0.4093(3) 1.1190(3) 1.0633(3) 0.0302(12) Uani 1 1 d . . .
C14C C 0.4336(3) 1.1201(4) 1.0106(3) 0.0343(13) Uani 1 1 d . . .
H14C H 0.4714 1.1552 1.0107 0.041 Uiso 1 1 calc R . .
C15C C 0.4020(3) 1.0694(4) 0.9583(3) 0.0327(13) Uani 1 1 d . C .
C16C C 0.3472(3) 1.0172(3) 0.9593(3) 0.0287(12) Uani 1 1 d . . .
H16C H 0.3264 0.9824 0.9229 0.034 Uiso 1 1 calc R . .
C17C C 0.4436(4) 1.1716(4) 1.1210(3) 0.0419(15) Uani 1 1 d . . .
C18C C 0.4258(3) 1.0715(3) 0.9005(3) 0.0496(17) Uani 1 1 d DU . .
F171 F 0.4757(4) 1.2335(3) 1.1069(3) 0.0867(18) Uani 1 1 d . . .
F172 F 0.4939(3) 1.1355(3) 1.1727(3) 0.092(2) Uani 1 1 d . . .
F173 F 0.3956(3) 1.2016(3) 1.1450(3) 0.0748(15) Uani 1 1 d . . .
F181 F 0.4456(6) 1.0002(4) 0.8863(5) 0.047(2) Uiso 0.50 1 d PDU C 1
F182 F 0.4820(5) 1.1203(6) 0.9071(5) 0.062(2) Uiso 0.50 1 d PDU C 1
F183 F 0.3672(4) 1.0930(6) 0.8445(4) 0.0471(19) Uiso 0.50 1 d PDU C 1
F184 F 0.4138(8) 1.0052(7) 0.8660(8) 0.058(4) Uiso 0.30 1 d PDU C 2
F185 F 0.5005(6) 1.0818(8) 0.9210(6) 0.043(3) Uiso 0.30 1 d PDU C 2
F186 F 0.3960(9) 1.1271(8) 0.8568(7) 0.067(4) Uiso 0.30 1 d PDU C 2
F187 F 0.4831(10) 1.0244(11) 0.9028(13) 0.070(7) Uiso 0.20 1 d PDU C 3
F188 F 0.4479(9) 1.1456(8) 0.8899(8) 0.028(3) Uiso 0.20 1 d PDU C 3
F189 F 0.3685(10) 1.0548(12) 0.8408(8) 0.050(5) Uiso 0.20 1 d PDU C 3
C21C C 0.2404(3) 0.8845(3) 0.9619(3) 0.0274(12) Uani 1 1 d . . .
C22C C 0.2996(3) 0.8376(3) 0.9630(3) 0.0296(12) Uani 1 1 d . . .
H22C H 0.3487 0.8521 0.9910 0.036 Uiso 1 1 calc R . .
C23C C 0.2891(4) 0.7700(4) 0.9245(3) 0.0368(14) Uani 1 1 d . D .
C24C C 0.2194(4) 0.7471(4) 0.8838(3) 0.0376(14) Uani 1 1 d . . .
H24C H 0.2123 0.7014 0.8575 0.045 Uiso 1 1 calc R . .
C25C C 0.1590(3) 0.7920(4) 0.8815(3) 0.0336(13) Uani 1 1 d . . .
C26C C 0.1693(3) 0.8583(4) 0.9200(3) 0.0314(12) Uani 1 1 d . . .
H26C H 0.1269 0.8873 0.9181 0.038 Uiso 1 1 calc R . .
C27C C 0.3539(4) 0.7245(3) 0.9276(3) 0.0532(19) Uani 1 1 d DU . .
C28C C 0.0825(4) 0.7686(5) 0.8362(3) 0.0483(18) Uani 1 1 d . . .
F271 F 0.3435(7) 0.6476(6) 0.9208(7) 0.078(4) Uiso 0.40 1 d PDU D 1
F272 F 0.3713(6) 0.7466(7) 0.8736(5) 0.057(3) Uiso 0.40 1 d PDU D 1
F273 F 0.4169(5) 0.7373(7) 0.9806(5) 0.040(3) Uiso 0.40 1 d PDU D 1
F274 F 0.3536(6) 0.6543(6) 0.9595(6) 0.062(3) Uiso 0.40 1 d PDU D 2
F275 F 0.3606(6) 0.7017(8) 0.8715(5) 0.062(3) Uiso 0.40 1 d PDU D 2
F276 F 0.4220(5) 0.7525(6) 0.9656(5) 0.044(3) Uiso 0.40 1 d PDU D 2
F277 F 0.3373(8) 0.6651(9) 0.8831(8) 0.022(3) Uiso 0.20 1 d PDU D 3
F278 F 0.3927(19) 0.6932(15) 0.9880(10) 0.114(11) Uiso 0.20 1 d PDU D 3
F279 F 0.402(2) 0.771(2) 0.9124(16) 0.138(14) Uiso 0.20 1 d PDU D 3
F281 F 0.0761(3) 0.6927(4) 0.8245(3) 0.104(2) Uani 1 1 d . . .
F282 F 0.0327(3) 0.7819(5) 0.8601(3) 0.108(3) Uani 1 1 d . . .
F283 F 0.0643(3) 0.7972(5) 0.7766(3) 0.110(3) Uani 1 1 d . . .
C31C C 0.2741(3) 0.9194(3) 1.0859(3) 0.0275(11) Uani 1 1 d . . .
C32C C 0.3471(3) 0.9087(3) 1.1310(3) 0.0276(12) Uani 1 1 d . . .
H32C H 0.3868 0.9269 1.1194 0.033 Uiso 1 1 calc R . .
C33C C 0.3636(3) 0.8724(3) 1.1922(3) 0.0344(13) Uani 1 1 d . . .
C34C C 0.3076(4) 0.8446(4) 1.2111(3) 0.0376(14) Uani 1 1 d . . .
C35C C 0.2352(4) 0.8521(4) 1.1671(3) 0.0360(14) Uani 1 1 d . . .
C36C C 0.2184(3) 0.8882(4) 1.1056(3) 0.0323(13) Uani 1 1 d . . .
H36C H 0.1679 0.8919 1.0760 0.039 Uiso 1 1 calc R . .
C37C C 0.4427(4) 0.8610(5) 1.2376(3) 0.0503(18) Uani 1 1 d . . .
C38C C 0.1734(4) 0.8250(4) 1.1875(4) 0.0509(18) Uani 1 1 d . . .
F371 F 0.4683(3) 0.7908(3) 1.2336(4) 0.106(2) Uani 1 1 d . . .
F372 F 0.4524(3) 0.8715(4) 1.3021(2) 0.0771(16) Uani 1 1 d . . .
F373 F 0.4896(2) 0.9105(3) 1.2274(2) 0.0660(13) Uani 1 1 d . . .
F381 F 0.1522(4) 0.8781(3) 1.2184(4) 0.122(3) Uani 1 1 d . . .
F382 F 0.1946(3) 0.7643(3) 1.2292(2) 0.0654(12) Uani 1 1 d . . .
F383 F 0.1148(2) 0.8002(3) 1.1365(3) 0.0757(15) Uani 1 1 d . . .
C41C C 0.1817(3) 1.0155(3) 0.9885(3) 0.0275(12) Uani 1 1 d . . .
C42C C 0.1455(3) 1.0446(3) 1.0288(3) 0.0298(12) Uani 1 1 d . . .
H42C H 0.1630 1.0298 1.0744 0.036 Uiso 1 1 calc R . .
C43C C 0.0845(3) 1.0945(4) 1.0041(3) 0.0364(14) Uani 1 1 d . E .
C44C C 0.0582(4) 1.1179(4) 0.9384(3) 0.0445(16) Uani 1 1 d . . .
H44C H 0.0158 1.1507 0.9210 0.053 Uiso 1 1 calc R . .
C45C C 0.0948(4) 1.0926(4) 0.8986(3) 0.0421(15) Uani 1 1 d . . .
C46C C 0.1541(3) 1.0431(4) 0.9231(3) 0.0336(13) Uani 1 1 d . . .
H46C H 0.1778 1.0266 0.8941 0.040 Uiso 1 1 calc R . .
C47C C 0.0466(3) 1.1204(3) 1.0482(3) 0.0541(19) Uani 1 1 d DU . .
C48C C 0.0691(5) 1.1194(6) 0.8279(4) 0.066(2) Uani 1 1 d . . .
F471 F 0.0365(6) 1.0613(5) 1.0874(5) 0.046(2) Uiso 0.40 1 d PDU E 1
F472 F -0.0246(5) 1.1434(7) 1.0147(5) 0.049(2) Uiso 0.40 1 d PDU E 1
F473 F 0.0797(6) 1.1758(6) 1.0905(6) 0.060(3) Uiso 0.40 1 d PDU E 1
F474 F 0.0022(9) 1.1828(8) 1.0235(8) 0.074(5) Uiso 0.30 1 d PDU E 2
F475 F 0.0965(6) 1.1420(8) 1.1090(5) 0.032(2) Uiso 0.30 1 d PDU E 2
F476 F 0.0041(9) 1.0646(8) 1.0597(8) 0.063(4) Uiso 0.30 1 d PDU E 2
F477 F 0.0447(8) 1.2008(6) 1.0468(8) 0.055(3) Uiso 0.30 1 d PD E 3
F478 F -0.0254(6) 1.1011(9) 1.0279(7) 0.057(4) Uiso 0.30 1 d PD E 3
F479 F 0.0771(10) 1.1044(10) 1.1135(7) 0.090(6) Uiso 0.30 1 d PD E 3
F481 F 0.0152(6) 1.0784(7) 0.7887(3) 0.205(6) Uani 1 1 d . . .
F482 F 0.0443(6) 1.1902(5) 0.8190(3) 0.153(4) Uani 1 1 d . . .
F483 F 0.1178(4) 1.1187(6) 0.8023(3) 0.144(4) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.02841(16) 0.04438(18) 0.02659(16) -0.00067(9) 0.00705(11) -0.00006(10)
Cl1 0.0416(10) 0.0860(15) 0.0345(9) -0.0109(8) 0.0032(8) -0.0039(9)
N1 0.048(3) 0.036(3) 0.039(3) -0.003(2) 0.017(3) -0.006(2)
N2 0.042(3) 0.049(3) 0.030(3) -0.002(2) 0.016(2) -0.007(3)
C3 0.052(4) 0.056(5) 0.044(4) -0.012(3) 0.024(3) -0.016(4)
C4 0.083(6) 0.047(5) 0.065(5) -0.014(4) 0.045(5) -0.020(4)
C5 0.083(6) 0.043(4) 0.050(4) -0.004(3) 0.038(4) -0.004(4)
C1A 0.042(4) 0.037(3) 0.042(4) 0.004(3) 0.010(3) 0.003(3)
N1' 0.038(3) 0.048(3) 0.041(3) -0.005(3) 0.017(2) 0.002(3)
N2' 0.035(3) 0.054(4) 0.038(3) -0.002(2) 0.012(2) 0.006(3)
N3' 0.036(3) 0.044(3) 0.034(3) 0.001(2) 0.014(2) -0.001(2)
C4' 0.032(3) 0.035(3) 0.036(3) -0.003(3) 0.006(3) -0.001(3)
C5' 0.036(3) 0.036(3) 0.046(4) -0.002(3) 0.011(3) 0.000(3)
C6 0.054(5) 0.088(7) 0.065(5) -0.003(5) 0.021(4) -0.025(5)
C7 0.098(7) 0.045(5) 0.089(6) 0.016(4) 0.053(6) 0.012(4)
C8 0.037(3) 0.049(4) 0.046(4) -0.006(3) 0.018(3) 0.000(3)
C9 0.111(9) 0.219(16) 0.058(6) 0.063(8) 0.051(6) 0.106(10)
C10 0.111(9) 0.181(13) 0.073(6) 0.046(7) 0.057(6) 0.103(9)
C11 0.055(4) 0.048(4) 0.059(5) -0.010(3) 0.034(4) -0.004(3)
C12 0.086(7) 0.082(7) 0.068(6) 0.024(5) 0.048(5) 0.025(5)
C13 0.083(7) 0.068(6) 0.067(6) 0.017(4) 0.044(5) 0.024(5)
C14 0.059(5) 0.058(5) 0.078(6) -0.011(4) 0.041(5) -0.003(4)
F141 0.138(5) 0.057(3) 0.096(4) -0.007(3) 0.081(4) 0.008(3)
F142 0.078(4) 0.090(4) 0.099(4) -0.005(3) 0.058(3) -0.014(3)
F143 0.082(4) 0.103(4) 0.063(3) 0.007(3) 0.039(3) 0.015(3)
C1B 0.064(5) 0.045(4) 0.039(4) -0.001(3) 0.006(4) 0.005(4)
C2B 0.034(4) 0.059(5) 0.066(5) -0.017(4) 0.016(3) 0.005(3)
C3B 0.060(4) 0.035(4) 0.044(4) -0.004(3) 0.026(3) 0.001(3)
C4B 0.035(3) 0.039(4) 0.038(3) -0.006(3) 0.008(3) 0.002(3)
C5B 0.053(4) 0.032(3) 0.056(4) 0.002(3) 0.031(3) 0.010(3)
C6B 0.131(10) 0.074(7) 0.059(6) 0.020(5) -0.009(6) 0.030(7)
C7B 0.046(5) 0.078(7) 0.188(13) -0.035(8) 0.040(7) 0.003(5)
C8B 0.145(10) 0.073(6) 0.075(6) -0.010(5) 0.079(7) -0.020(6)
C9B 0.052(5) 0.062(5) 0.085(6) -0.022(5) -0.015(4) 0.009(4)
C10B 0.107(8) 0.049(5) 0.122(8) -0.004(5) 0.085(7) -0.010(5)
B1C 0.022(3) 0.029(3) 0.026(3) 0.000(2) 0.008(3) -0.001(2)
C11C 0.022(3) 0.024(3) 0.021(3) 0.003(2) 0.003(2) 0.001(2)
C12C 0.028(3) 0.026(3) 0.026(3) 0.001(2) 0.012(2) 0.004(2)
C13C 0.030(3) 0.030(3) 0.030(3) -0.004(2) 0.010(2) 0.000(2)
C14C 0.034(3) 0.036(3) 0.034(3) -0.001(3) 0.014(3) -0.011(3)
C15C 0.035(3) 0.036(3) 0.031(3) 0.005(2) 0.017(3) -0.001(3)
C16C 0.027(3) 0.033(3) 0.023(3) -0.004(2) 0.007(2) 0.001(2)
C17C 0.039(4) 0.041(4) 0.047(4) -0.015(3) 0.017(3) -0.008(3)
C18C 0.055(4) 0.056(5) 0.046(4) -0.001(3) 0.029(3) -0.017(4)
F171 0.125(5) 0.066(3) 0.095(4) -0.043(3) 0.069(4) -0.052(3)
F172 0.091(4) 0.080(4) 0.058(3) -0.032(3) -0.027(3) 0.023(3)
F173 0.067(3) 0.089(4) 0.077(3) -0.045(3) 0.036(3) -0.009(3)
C21C 0.028(3) 0.033(3) 0.021(3) 0.002(2) 0.009(2) -0.004(2)
C22C 0.028(3) 0.032(3) 0.029(3) -0.004(2) 0.012(2) -0.003(2)
C23C 0.041(4) 0.036(3) 0.040(3) -0.001(3) 0.024(3) 0.000(3)
C24C 0.051(4) 0.035(3) 0.032(3) -0.013(3) 0.022(3) -0.014(3)
C25C 0.036(3) 0.042(3) 0.027(3) -0.008(2) 0.016(3) -0.014(3)
C26C 0.027(3) 0.041(3) 0.027(3) -0.002(2) 0.012(2) -0.002(3)
C27C 0.061(5) 0.039(4) 0.070(5) -0.019(4) 0.036(4) 0.000(3)
C28C 0.045(4) 0.065(5) 0.038(4) -0.023(3) 0.020(3) -0.015(4)
F281 0.075(4) 0.087(4) 0.127(5) -0.047(4) 0.012(3) -0.038(3)
F282 0.044(3) 0.193(7) 0.094(4) -0.084(5) 0.033(3) -0.041(4)
F283 0.061(3) 0.189(7) 0.052(3) 0.025(4) -0.012(2) -0.052(4)
C31C 0.030(3) 0.027(3) 0.027(3) -0.002(2) 0.012(2) -0.004(2)
C32C 0.028(3) 0.026(3) 0.029(3) 0.000(2) 0.013(2) 0.002(2)
C33C 0.036(3) 0.030(3) 0.030(3) 0.001(2) 0.005(3) 0.004(3)
C34C 0.046(4) 0.037(3) 0.029(3) 0.008(3) 0.014(3) 0.003(3)
C35C 0.043(4) 0.040(3) 0.033(3) 0.003(3) 0.024(3) 0.000(3)
C36C 0.032(3) 0.032(3) 0.032(3) 0.002(2) 0.011(3) -0.002(2)
C37C 0.041(4) 0.062(5) 0.038(4) 0.014(3) 0.003(3) 0.003(4)
C38C 0.059(5) 0.052(4) 0.056(4) 0.008(4) 0.039(4) 0.000(4)
F371 0.066(3) 0.070(3) 0.135(5) -0.009(3) -0.018(3) 0.042(3)
F372 0.057(3) 0.123(5) 0.034(2) 0.019(3) -0.001(2) -0.010(3)
F373 0.036(2) 0.097(4) 0.052(2) 0.022(2) 0.0020(19) 0.003(2)
F381 0.174(7) 0.068(4) 0.213(8) -0.014(4) 0.173(7) -0.005(4)
F382 0.076(3) 0.072(3) 0.058(3) 0.019(2) 0.037(2) -0.009(2)
F383 0.042(2) 0.112(4) 0.076(3) 0.037(3) 0.026(2) -0.005(3)
C41C 0.025(3) 0.030(3) 0.025(3) -0.003(2) 0.007(2) -0.005(2)
C42C 0.033(3) 0.029(3) 0.026(3) 0.001(2) 0.010(2) 0.000(2)
C43C 0.035(3) 0.034(3) 0.044(3) -0.004(3) 0.018(3) 0.001(3)
C44C 0.034(3) 0.048(4) 0.045(4) 0.004(3) 0.008(3) 0.015(3)
C45C 0.039(3) 0.050(4) 0.032(3) 0.009(3) 0.007(3) 0.009(3)
C46C 0.031(3) 0.043(4) 0.028(3) 0.003(3) 0.012(3) 0.003(3)
C47C 0.052(4) 0.054(5) 0.057(5) -0.009(4) 0.022(4) 0.011(4)
C48C 0.062(5) 0.088(6) 0.043(4) 0.023(4) 0.014(4) 0.034(5)
F481 0.230(11) 0.277(13) 0.035(3) 0.036(5) -0.035(5) -0.139(10)
F482 0.234(10) 0.135(6) 0.073(4) 0.053(4) 0.039(5) 0.109(7)
F483 0.121(5) 0.259(10) 0.072(4) 0.096(5) 0.058(4) 0.087(6)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1E Cl3E 1.47(3) . ?
C1E C1E' 1.63(4) . ?
C1E Cl2E 2.07(3) . ?
C1E Cl1E 2.08(3) . ?
C1E' Cl2E 1.48(3) . ?
C1E' Cl3E 1.741(18) . ?
C1E' Cl4E 1.748(18) . ?
C1E' Cl1E 2.03(2) . ?
Cl1E Cl3E 0.616(17) . ?
Cl2E Cl4E 0.51(2) . ?
C1F Cl1F 1.648(19) . ?
C1F Cl2F 1.68(2) . ?
C1F Cl3F 1.698(18) . ?
C1F Cl2' 1.74(3) . ?
C1F Cl4F 1.835(19) . ?
C1F Cl1' 2.07(2) . ?
Cl2F Cl2' 0.58(3) . ?
Cl1' Cl3F 0.554(15) . ?
Ir1 N3' 2.086(5) . ?
Ir1 N2 2.118(5) . ?
Ir1 C4B 2.149(6) . ?
Ir1 C2B 2.149(7) . ?
Ir1 C1B 2.149(7) . ?
Ir1 C3B 2.155(6) . ?
Ir1 C5B 2.158(7) . ?
Ir1 Cl1 2.3823(17) . ?
N1 C5 1.335(9) . ?
N1 N2 1.374(8) . ?
N1 C1A 1.438(8) . ?
N2 C3 1.338(9) . ?
C3 C4 1.381(12) . ?
C3 C6 1.479(11) . ?
C4 C5 1.393(12) . ?
C4 H4 0.9500 . ?
C5 C7 1.489(12) . ?
C1A C4' 1.486(9) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.348(8) . ?
N1' C5' 1.350(9) . ?
N1' C8 1.432(8) . ?
N2' N3' 1.307(8) . ?
N3' C4' 1.360(8) . ?
C4' C5' 1.348(9) . ?
C5' H5' 0.9500 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.321(12) . ?
C8 C13 1.397(12) . ?
C9 C10 1.364(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.288(12) . ?
C10 H10 0.9500 . ?
C11 C12 1.396(12) . ?
C11 C14 1.512(10) . ?
C12 C13 1.377(12) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 F143 1.320(10) . ?
C14 F142 1.328(9) . ?
C14 F141 1.336(9) . ?
C1B C5B 1.393(11) . ?
C1B C2B 1.432(12) . ?
C1B C6B 1.538(11) . ?
C2B C3B 1.422(11) . ?
C2B C7B 1.495(11) . ?
C3B C4B 1.424(10) . ?
C3B C8B 1.490(11) . ?
C4B C5B 1.435(10) . ?
C4B C9B 1.478(10) . ?
C5B C10B 1.501(11) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C41C 1.630(8) . ?
B1C C21C 1.634(8) . ?
B1C C11C 1.634(8) . ?
B1C C31C 1.639(8) . ?
C11C C16C 1.385(8) . ?
C11C C12C 1.398(8) . ?
C12C C13C 1.378(8) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.389(8) . ?
C13C C17C 1.482(8) . ?
C14C C15C 1.378(8) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.399(8) . ?
C15C C18C 1.488(9) . ?
C16C H16C 0.9500 . ?
C17C F171 1.327(8) . ?
C17C F172 1.328(9) . ?
C17C F173 1.331(8) . ?
C18C F186 1.317(11) . ?
C18C F184 1.336(11) . ?
C18C F182 1.341(8) . ?
C18C F181 1.356(8) . ?
C18C F185 1.359(10) . ?
C18C F187 1.362(14) . ?
C18C F183 1.364(8) . ?
C18C F189 1.381(14) . ?
C18C F188 1.392(13) . ?
C21C C22C 1.398(8) . ?
C21C C26C 1.409(8) . ?
C22C C23C 1.402(8) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.366(9) . ?
C23C C27C 1.460(9) . ?
C24C C25C 1.389(9) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.382(8) . ?
C25C C28C 1.494(9) . ?
C26C H26C 0.9500 . ?
C27C F275 1.327(9) . ?
C27C F271 1.339(10) . ?
C27C F273 1.343(9) . ?
C27C F278 1.351(16) . ?
C27C F276 1.355(9) . ?
C27C F279 1.357(17) . ?
C27C F277 1.357(14) . ?
C27C F272 1.387(9) . ?
C27C F274 1.393(9) . ?
C28C F282 1.277(8) . ?
C28C F283 1.298(9) . ?
C28C F281 1.328(9) . ?
C31C C32C 1.397(8) . ?
C31C C36C 1.409(8) . ?
C32C C33C 1.388(8) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.384(9) . ?
C33C C37C 1.491(9) . ?
C34C C35C 1.376(9) . ?
C35C C36C 1.390(8) . ?
C35C C38C 1.500(9) . ?
C36C H36C 0.9500 . ?
C37C F371 1.323(9) . ?
C37C F373 1.324(9) . ?
C37C F372 1.348(9) . ?
C38C F381 1.289(9) . ?
C38C F383 1.321(9) . ?
C38C F382 1.340(9) . ?
C41C C46C 1.394(8) . ?
C41C C42C 1.401(8) . ?
C42C C43C 1.395(9) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.376(9) . ?
C43C C47C 1.476(10) . ?
C44C C45C 1.377(10) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.370(9) . ?
C45C C48C 1.493(10) . ?
C46C H46C 0.9500 . ?
C47C F473 1.312(9) . ?
C47C F479 1.339(12) . ?
C47C F478 1.339(11) . ?
C47C F476 1.349(11) . ?
C47C F474 1.355(11) . ?
C47C F472 1.355(9) . ?
C47C F475 1.359(10) . ?
C47C F471 1.384(9) . ?
C47C F477 1.385(11) . ?
C48C F483 1.263(10) . ?
C48C F481 1.283(12) . ?
C48C F482 1.299(11) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl3E C1E C1E' 68.2(16) . . ?
Cl3E C1E Cl2E 96.3(19) . . ?
C1E' C1E Cl2E 45.2(11) . . ?
Cl3E C1E Cl1E 3.9(7) . . ?
C1E' C1E Cl1E 65.0(14) . . ?
Cl2E C1E Cl1E 92.3(14) . . ?
Cl2E C1E' C1E 83.5(17) . . ?
Cl2E C1E' Cl3E 112(2) . . ?
C1E C1E' Cl3E 51.7(10) . . ?
Cl2E C1E' Cl4E 15.6(9) . . ?
C1E C1E' Cl4E 97.6(18) . . ?
Cl3E C1E' Cl4E 116.3(18) . . ?
Cl2E C1E' Cl1E 116.4(18) . . ?
C1E C1E' Cl1E 68.3(11) . . ?
Cl3E C1E' Cl1E 16.7(6) . . ?
Cl4E C1E' Cl1E 116.1(17) . . ?
Cl3E Cl1E C1E' 54.4(18) . . ?
Cl3E Cl1E C1E 9.4(17) . . ?
C1E' Cl1E C1E 46.7(12) . . ?
Cl4E Cl2E C1E' 113(3) . . ?
Cl4E Cl2E C1E 154(3) . . ?
C1E' Cl2E C1E 51.3(14) . . ?
Cl1E Cl3E C1E 167(2) . . ?
Cl1E Cl3E C1E' 109(2) . . ?
C1E Cl3E C1E' 60.1(16) . . ?
Cl2E Cl4E C1E' 51(2) . . ?
Cl1F C1F Cl2F 115.3(12) . . ?
Cl1F C1F Cl3F 19.8(5) . . ?
Cl2F C1F Cl3F 135.1(13) . . ?
Cl1F C1F Cl2' 97.6(13) . . ?
Cl2F C1F Cl2' 19.3(9) . . ?
Cl3F C1F Cl2' 117.1(13) . . ?
Cl1F C1F Cl4F 94.1(9) . . ?
Cl2F C1F Cl4F 22.2(8) . . ?
Cl3F C1F Cl4F 113.9(10) . . ?
Cl2' C1F Cl4F 15.4(8) . . ?
Cl1F C1F Cl1' 7.4(7) . . ?
Cl2F C1F Cl1' 122.4(12) . . ?
Cl3F C1F Cl1' 12.7(6) . . ?
Cl2' C1F Cl1' 104.5(13) . . ?
Cl4F C1F Cl1' 101.4(9) . . ?
Cl2' Cl2F C1F 87(3) . . ?
Cl2F Cl2' C1F 74(3) . . ?
Cl3F Cl1' C1F 42(2) . . ?
Cl1' Cl3F C1F 125(3) . . ?
N3' Ir1 N2 84.0(2) . . ?
N3' Ir1 C4B 103.5(2) . . ?
N2 Ir1 C4B 112.9(2) . . ?
N3' Ir1 C2B 161.4(3) . . ?
N2 Ir1 C2B 113.7(3) . . ?
C4B Ir1 C2B 65.1(3) . . ?
N3' Ir1 C1B 123.6(3) . . ?
N2 Ir1 C1B 152.3(3) . . ?
C4B Ir1 C1B 64.4(3) . . ?
C2B Ir1 C1B 38.9(3) . . ?
N3' Ir1 C3B 138.5(2) . . ?
N2 Ir1 C3B 95.9(2) . . ?
C4B Ir1 C3B 38.6(3) . . ?
C2B Ir1 C3B 38.6(3) . . ?
C1B Ir1 C3B 64.3(3) . . ?
N3' Ir1 C5B 97.1(2) . . ?
N2 Ir1 C5B 151.4(2) . . ?
C4B Ir1 C5B 38.9(3) . . ?
C2B Ir1 C5B 64.6(3) . . ?
C1B Ir1 C5B 37.7(3) . . ?
C3B Ir1 C5B 64.4(3) . . ?
N3' Ir1 Cl1 85.13(16) . . ?
N2 Ir1 Cl1 87.77(15) . . ?
C4B Ir1 Cl1 158.12(19) . . ?
C2B Ir1 Cl1 100.7(2) . . ?
C1B Ir1 Cl1 93.9(2) . . ?
C3B Ir1 Cl1 136.4(2) . . ?
C5B Ir1 Cl1 120.9(2) . . ?
C5 N1 N2 111.2(6) . . ?
C5 N1 C1A 128.1(6) . . ?
N2 N1 C1A 120.7(5) . . ?
C3 N2 N1 106.5(6) . . ?
C3 N2 Ir1 131.0(5) . . ?
N1 N2 Ir1 122.5(4) . . ?
N2 C3 C4 109.0(7) . . ?
N2 C3 C6 124.6(7) . . ?
C4 C3 C6 126.4(7) . . ?
C3 C4 C5 107.4(7) . . ?
C3 C4 H4 126.3 . . ?
C5 C4 H4 126.3 . . ?
N1 C5 C4 105.9(7) . . ?
N1 C5 C7 124.5(8) . . ?
C4 C5 C7 129.6(7) . . ?
N1 C1A C4' 111.7(5) . . ?
N1 C1A H1A1 109.3 . . ?
C4' C1A H1A1 109.3 . . ?
N1 C1A H1A2 109.3 . . ?
C4' C1A H1A2 109.3 . . ?
H1A1 C1A H1A2 107.9 . . ?
N2' N1' C5' 110.5(5) . . ?
N2' N1' C8 119.7(6) . . ?
C5' N1' C8 129.7(6) . . ?
N3' N2' N1' 105.7(5) . . ?
N2' N3' C4' 110.8(5) . . ?
N2' N3' Ir1 125.2(4) . . ?
C4' N3' Ir1 123.9(4) . . ?
C5' C4' N3' 106.9(6) . . ?
C5' C4' C1A 133.5(6) . . ?
N3' C4' C1A 119.6(6) . . ?
C4' C5' N1' 106.1(6) . . ?
C4' C5' H5' 127.0 . . ?
N1' C5' H5' 127.0 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C13 118.7(7) . . ?
C9 C8 N1' 121.3(7) . . ?
C13 C8 N1' 120.0(6) . . ?
C8 C9 C10 120.7(9) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 122.3(9) . . ?
C11 C10 H10 118.9 . . ?
C9 C10 H10 118.9 . . ?
C10 C11 C12 120.2(8) . . ?
C10 C11 C14 121.0(8) . . ?
C12 C11 C14 118.8(8) . . ?
C13 C12 C11 117.8(9) . . ?
C13 C12 H12 121.1 . . ?
C11 C12 H12 121.1 . . ?
C12 C13 C8 120.1(9) . . ?
C12 C13 H13 119.9 . . ?
C8 C13 H13 119.9 . . ?
F143 C14 F142 107.0(7) . . ?
F143 C14 F141 106.7(7) . . ?
F142 C14 F141 106.4(7) . . ?
F143 C14 C11 113.9(7) . . ?
F142 C14 C11 111.6(7) . . ?
F141 C14 C11 110.8(7) . . ?
C5B C1B C2B 109.2(6) . . ?
C5B C1B C6B 124.7(9) . . ?
C2B C1B C6B 126.1(9) . . ?
C5B C1B Ir1 71.4(4) . . ?
C2B C1B Ir1 70.5(4) . . ?
C6B C1B Ir1 126.9(6) . . ?
C3B C2B C1B 106.7(6) . . ?
C3B C2B C7B 126.8(9) . . ?
C1B C2B C7B 125.9(9) . . ?
C3B C2B Ir1 70.9(4) . . ?
C1B C2B Ir1 70.6(4) . . ?
C7B C2B Ir1 130.3(6) . . ?
C2B C3B C4B 108.7(6) . . ?
C2B C3B C8B 127.7(8) . . ?
C4B C3B C8B 123.6(8) . . ?
C2B C3B Ir1 70.5(4) . . ?
C4B C3B Ir1 70.4(4) . . ?
C8B C3B Ir1 125.4(6) . . ?
C3B C4B C5B 107.1(6) . . ?
C3B C4B C9B 126.2(7) . . ?
C5B C4B C9B 126.0(7) . . ?
C3B C4B Ir1 70.9(4) . . ?
C5B C4B Ir1 70.9(4) . . ?
C9B C4B Ir1 130.8(5) . . ?
C1B C5B C4B 108.3(6) . . ?
C1B C5B C10B 126.2(8) . . ?
C4B C5B C10B 125.5(7) . . ?
C1B C5B Ir1 70.8(4) . . ?
C4B C5B Ir1 70.2(4) . . ?
C10B C5B Ir1 126.5(5) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C41C B1C C21C 110.7(5) . . ?
C41C B1C C11C 104.5(4) . . ?
C21C B1C C11C 112.4(5) . . ?
C41C B1C C31C 114.4(5) . . ?
C21C B1C C31C 104.2(4) . . ?
C11C B1C C31C 111.0(4) . . ?
C16C C11C C12C 115.6(5) . . ?
C16C C11C B1C 124.2(5) . . ?
C12C C11C B1C 119.9(5) . . ?
C13C C12C C11C 122.8(5) . . ?
C13C C12C H12C 118.6 . . ?
C11C C12C H12C 118.6 . . ?
C12C C13C C14C 120.2(5) . . ?
C12C C13C C17C 119.9(5) . . ?
C14C C13C C17C 119.9(5) . . ?
C15C C14C C13C 118.8(5) . . ?
C15C C14C H14C 120.6 . . ?
C13C C14C H14C 120.6 . . ?
C14C C15C C16C 120.0(5) . . ?
C14C C15C C18C 119.4(5) . . ?
C16C C15C C18C 120.5(5) . . ?
C11C C16C C15C 122.6(5) . . ?
C11C C16C H16C 118.7 . . ?
C15C C16C H16C 118.7 . . ?
F171 C17C F172 108.0(6) . . ?
F171 C17C F173 103.6(6) . . ?
F172 C17C F173 104.7(6) . . ?
F171 C17C C13C 113.5(6) . . ?
F172 C17C C13C 112.3(6) . . ?
F173 C17C C13C 114.0(5) . . ?
F186 C18C F184 106.4(7) . . ?
F186 C18C F182 75.0(7) . . ?
F184 C18C F182 123.9(9) . . ?
F186 C18C F181 125.5(9) . . ?
F184 C18C F181 26.4(6) . . ?
F182 C18C F181 107.6(6) . . ?
F186 C18C F185 105.4(7) . . ?
F184 C18C F185 103.5(7) . . ?
F182 C18C F185 32.7(5) . . ?
F181 C18C F185 80.4(6) . . ?
F186 C18C F187 126.2(14) . . ?
F184 C18C F187 58.7(9) . . ?
F182 C18C F187 75.4(8) . . ?
F181 C18C F187 34.1(8) . . ?
F185 C18C F187 46.3(8) . . ?
F186 C18C F183 34.0(6) . . ?
F184 C18C F183 79.8(7) . . ?
F182 C18C F183 107.3(6) . . ?
F181 C18C F183 104.8(5) . . ?
F185 C18C F183 133.2(8) . . ?
F187 C18C F183 126.1(12) . . ?
F186 C18C F189 59.9(9) . . ?
F184 C18C F189 52.3(9) . . ?
F182 C18C F189 124.4(10) . . ?
F181 C18C F189 78.2(8) . . ?
F185 C18C F189 135.7(11) . . ?
F187 C18C F189 105.6(9) . . ?
F183 C18C F189 28.0(7) . . ?
F186 C18C F188 45.2(7) . . ?
F184 C18C F188 133.7(11) . . ?
F182 C18C F188 32.3(6) . . ?
F181 C18C F188 131.4(8) . . ?
F185 C18C F188 65.0(7) . . ?
F187 C18C F188 104.6(8) . . ?
F183 C18C F188 79.1(7) . . ?
F189 C18C F188 103.1(8) . . ?
F186 C18C C15C 115.5(9) . . ?
F184 C18C C15C 113.9(8) . . ?
F182 C18C C15C 115.1(6) . . ?
F181 C18C C15C 111.9(6) . . ?
F185 C18C C15C 111.1(7) . . ?
F187 C18C C15C 117.6(12) . . ?
F183 C18C C15C 109.6(6) . . ?
F189 C18C C15C 112.7(10) . . ?
F188 C18C C15C 112.0(8) . . ?
C22C C21C C26C 115.2(5) . . ?
C22C C21C B1C 120.8(5) . . ?
C26C C21C B1C 123.7(5) . . ?
C21C C22C C23C 122.4(5) . . ?
C21C C22C H22C 118.8 . . ?
C23C C22C H22C 118.8 . . ?
C24C C23C C22C 120.6(6) . . ?
C24C C23C C27C 120.1(5) . . ?
C22C C23C C27C 119.3(5) . . ?
C23C C24C C25C 118.7(5) . . ?
C23C C24C H24C 120.7 . . ?
C25C C24C H24C 120.7 . . ?
C26C C25C C24C 120.7(5) . . ?
C26C C25C C28C 120.0(6) . . ?
C24C C25C C28C 119.3(6) . . ?
C25C C26C C21C 122.4(6) . . ?
C25C C26C H26C 118.8 . . ?
C21C C26C H26C 118.8 . . ?
F275 C27C F271 70.7(6) . . ?
F275 C27C F273 117.2(8) . . ?
F271 C27C F273 107.8(7) . . ?
F275 C27C F278 123.7(16) . . ?
F271 C27C F278 73.6(11) . . ?
F273 C27C F278 40.7(12) . . ?
F275 C27C F276 104.6(7) . . ?
F271 C27C F276 119.4(9) . . ?
F273 C27C F276 19.4(5) . . ?
F278 C27C F276 59.6(14) . . ?
F275 C27C F279 68.9(11) . . ?
F271 C27C F279 130.0(18) . . ?
F273 C27C F279 67.9(14) . . ?
F278 C27C F279 106.6(12) . . ?
F276 C27C F279 48.5(14) . . ?
F275 C27C F277 37.6(6) . . ?
F271 C27C F277 36.0(6) . . ?
F273 C27C F277 128.7(9) . . ?
F278 C27C F277 106.4(11) . . ?
F276 C27C F277 128.0(9) . . ?
F279 C27C F277 105.8(11) . . ?
F275 C27C F272 34.1(5) . . ?
F271 C27C F272 104.7(6) . . ?
F273 C27C F272 104.0(6) . . ?
F278 C27C F272 134.5(18) . . ?
F276 C27C F272 85.5(6) . . ?
F279 C27C F272 39.4(11) . . ?
F277 C27C F272 71.2(7) . . ?
F275 C27C F274 102.5(6) . . ?
F271 C27C F274 33.7(6) . . ?
F273 C27C F274 83.7(6) . . ?
F278 C27C F274 43.8(11) . . ?
F276 C27C F274 101.1(6) . . ?
F279 C27C F274 139(2) . . ?
F277 C27C F274 69.7(7) . . ?
F272 C27C F274 134.7(7) . . ?
F275 C27C C23C 119.7(7) . . ?
F271 C27C C23C 115.7(8) . . ?
F273 C27C C23C 116.3(6) . . ?
F278 C27C C23C 114.5(16) . . ?
F276 C27C C23C 117.5(7) . . ?
F279 C27C C23C 109.4(19) . . ?
F277 C27C C23C 113.6(8) . . ?
F272 C27C C23C 107.1(7) . . ?
F274 C27C C23C 108.9(7) . . ?
F282 C28C F283 111.7(8) . . ?
F282 C28C F281 102.9(7) . . ?
F283 C28C F281 102.3(6) . . ?
F282 C28C C25C 113.7(5) . . ?
F283 C28C C25C 112.4(6) . . ?
F281 C28C C25C 112.9(7) . . ?
C32C C31C C36C 115.5(5) . . ?
C32C C31C B1C 122.6(5) . . ?
C36C C31C B1C 121.7(5) . . ?
C33C C32C C31C 122.3(5) . . ?
C33C C32C H32C 118.8 . . ?
C31C C32C H32C 118.8 . . ?
C34C C33C C32C 120.8(5) . . ?
C34C C33C C37C 119.2(6) . . ?
C32C C33C C37C 119.9(6) . . ?
C35C C34C C33C 118.3(5) . . ?
C34C C35C C36C 121.0(6) . . ?
C34C C35C C38C 119.2(6) . . ?
C36C C35C C38C 119.7(6) . . ?
C35C C36C C31C 122.0(6) . . ?
C35C C36C H36C 119.0 . . ?
C31C C36C H36C 119.0 . . ?
F371 C37C F373 106.1(7) . . ?
F371 C37C F372 106.3(6) . . ?
F373 C37C F372 104.6(6) . . ?
F371 C37C C33C 113.3(6) . . ?
F373 C37C C33C 114.0(6) . . ?
F372 C37C C33C 111.9(6) . . ?
F381 C38C F383 108.6(7) . . ?
F381 C38C F382 106.3(6) . . ?
F383 C38C F382 105.1(6) . . ?
F381 C38C C35C 112.3(6) . . ?
F383 C38C C35C 112.7(6) . . ?
F382 C38C C35C 111.4(6) . . ?
C46C C41C C42C 114.8(5) . . ?
C46C C41C B1C 118.6(5) . . ?
C42C C41C B1C 126.5(5) . . ?
C43C C42C C41C 122.3(5) . . ?
C43C C42C H42C 118.9 . . ?
C41C C42C H42C 118.9 . . ?
C44C C43C C42C 120.4(6) . . ?
C44C C43C C47C 119.8(6) . . ?
C42C C43C C47C 119.7(6) . . ?
C43C C44C C45C 118.3(6) . . ?
C43C C44C H44C 120.8 . . ?
C45C C44C H44C 120.8 . . ?
C46C C45C C44C 120.7(6) . . ?
C46C C45C C48C 119.7(6) . . ?
C44C C45C C48C 119.5(6) . . ?
C45C C46C C41C 123.4(6) . . ?
C45C C46C H46C 118.3 . . ?
C41C C46C H46C 118.3 . . ?
F473 C47C F479 60.4(8) . . ?
F473 C47C F478 125.8(10) . . ?
F479 C47C F478 106.6(8) . . ?
F473 C47C F476 124.1(9) . . ?
F479 C47C F476 73.5(8) . . ?
F478 C47C F476 41.4(7) . . ?
F473 C47C F474 76.7(7) . . ?
F479 C47C F474 122.8(12) . . ?
F478 C47C F474 68.7(7) . . ?
F476 C47C F474 107.2(7) . . ?
F473 C47C F472 107.0(6) . . ?
F479 C47C F472 125.4(11) . . ?
F478 C47C F472 33.8(6) . . ?
F476 C47C F472 74.6(7) . . ?
F474 C47C F472 35.8(6) . . ?
F473 C47C F475 30.8(5) . . ?
F479 C47C F475 33.3(7) . . ?
F478 C47C F475 131.3(9) . . ?
F476 C47C F475 106.2(7) . . ?
F474 C47C F475 106.3(7) . . ?
F472 C47C F475 130.4(8) . . ?
F473 C47C F471 104.6(6) . . ?
F479 C47C F471 46.4(7) . . ?
F478 C47C F471 69.4(7) . . ?
F476 C47C F471 29.1(6) . . ?
F474 C47C F471 127.5(10) . . ?
F472 C47C F471 101.0(6) . . ?
F475 C47C F471 79.8(6) . . ?
F473 C47C F477 44.7(6) . . ?
F479 C47C F477 103.0(8) . . ?
F478 C47C F477 103.0(7) . . ?
F476 C47C F477 134.7(10) . . ?
F474 C47C F477 36.0(7) . . ?
F472 C47C F477 71.5(6) . . ?
F475 C47C F477 75.5(7) . . ?
F471 C47C F477 137.6(9) . . ?
F473 C47C C43C 116.0(7) . . ?
F479 C47C C43C 119.4(10) . . ?
F478 C47C C43C 115.2(8) . . ?
F476 C47C C43C 113.2(8) . . ?
F474 C47C C43C 112.5(9) . . ?
F472 C47C C43C 113.6(6) . . ?
F475 C47C C43C 111.1(7) . . ?
F471 C47C C43C 113.2(6) . . ?
F477 C47C C43C 107.6(8) . . ?
F483 C48C F481 105.4(10) . . ?
F483 C48C F482 104.0(9) . . ?
F481 C48C F482 104.7(9) . . ?
F483 C48C C45C 115.6(7) . . ?
F481 C48C C45C 112.4(8) . . ?
F482 C48C C45C 113.8(8) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl3E C1E C1E' Cl2E -124.3(19) . . . . ?
Cl1E C1E C1E' Cl2E -121.7(17) . . . . ?
Cl2E C1E C1E' Cl3E 124.3(19) . . . . ?
Cl1E C1E C1E' Cl3E 2.5(9) . . . . ?
Cl3E C1E C1E' Cl4E -117.6(17) . . . . ?
Cl2E C1E C1E' Cl4E 6.7(9) . . . . ?
Cl1E C1E C1E' Cl4E -115.1(16) . . . . ?
Cl3E C1E C1E' Cl1E -2.5(9) . . . . ?
Cl2E C1E C1E' Cl1E 121.7(17) . . . . ?
Cl2E C1E' Cl1E Cl3E 77(3) . . . . ?
C1E C1E' Cl1E Cl3E 7(3) . . . . ?
Cl4E C1E' Cl1E Cl3E 95(3) . . . . ?
Cl2E C1E' Cl1E C1E 71(2) . . . . ?
Cl3E C1E' Cl1E C1E -7(3) . . . . ?
Cl4E C1E' Cl1E C1E 88(2) . . . . ?
C1E' C1E Cl1E Cl3E -143(13) . . . . ?
Cl2E C1E Cl1E Cl3E 180(100) . . . . ?
Cl3E C1E Cl1E C1E' 143(13) . . . . ?
Cl2E C1E Cl1E C1E' -37.2(12) . . . . ?
C1E C1E' Cl2E Cl4E 155(3) . . . . ?
Cl3E C1E' Cl2E Cl4E 110(3) . . . . ?
Cl1E C1E' Cl2E Cl4E 93(3) . . . . ?
Cl3E C1E' Cl2E C1E -44.3(16) . . . . ?
Cl4E C1E' Cl2E C1E -155(3) . . . . ?
Cl1E C1E' Cl2E C1E -61.9(17) . . . . ?
Cl3E C1E Cl2E Cl4E -12(8) . . . . ?
C1E' C1E Cl2E Cl4E -62(8) . . . . ?
Cl1E C1E Cl2E Cl4E -12(8) . . . . ?
Cl3E C1E Cl2E C1E' 50.5(19) . . . . ?
Cl1E C1E Cl2E C1E' 50.5(17) . . . . ?
C1E' Cl1E Cl3E C1E -32(12) . . . . ?
C1E Cl1E Cl3E C1E' 32(12) . . . . ?
C1E' C1E Cl3E Cl1E 36(13) . . . . ?
Cl2E C1E Cl3E Cl1E 0(13) . . . . ?
Cl2E C1E Cl3E C1E' -36.2(13) . . . . ?
Cl1E C1E Cl3E C1E' -36(13) . . . . ?
Cl2E C1E' Cl3E Cl1E -110(3) . . . . ?
C1E C1E' Cl3E Cl1E -172(3) . . . . ?
Cl4E C1E' Cl3E Cl1E -93(3) . . . . ?
Cl2E C1E' Cl3E C1E 62(2) . . . . ?
Cl4E C1E' Cl3E C1E 78(2) . . . . ?
Cl1E C1E' Cl3E C1E 172(3) . . . . ?
C1E Cl2E Cl4E C1E' 49(6) . . . . ?
C1E C1E' Cl4E Cl2E -25(3) . . . . ?
Cl3E C1E' Cl4E Cl2E -76(4) . . . . ?
Cl1E C1E' Cl4E Cl2E -95(4) . . . . ?
Cl1F C1F Cl2F Cl2' 25(5) . . . . ?
Cl3F C1F Cl2F Cl2' 24(5) . . . . ?
Cl4F C1F Cl2F Cl2' 44(3) . . . . ?
Cl1' C1F Cl2F Cl2' 23(5) . . . . ?
Cl1F C1F Cl2' Cl2F -157(4) . . . . ?
Cl3F C1F Cl2' Cl2F -161(4) . . . . ?
Cl4F C1F Cl2' Cl2F -80(5) . . . . ?
Cl1' C1F Cl2' Cl2F -160(4) . . . . ?
Cl1F C1F Cl1' Cl3F 162(6) . . . . ?
Cl2F C1F Cl1' Cl3F 177(3) . . . . ?
Cl2' C1F Cl1' Cl3F -175(3) . . . . ?
Cl4F C1F Cl1' Cl3F 169(3) . . . . ?
Cl1F C1F Cl3F Cl1' -7(2) . . . . ?
Cl2F C1F Cl3F Cl1' -4(3) . . . . ?
Cl2' C1F Cl3F Cl1' 5(3) . . . . ?
Cl4F C1F Cl3F Cl1' -12(3) . . . . ?
C5 N1 N2 C3 -0.5(7) . . . . ?
C1A N1 N2 C3 -179.4(6) . . . . ?
C5 N1 N2 Ir1 178.8(4) . . . . ?
C1A N1 N2 Ir1 0.0(7) . . . . ?
N3' Ir1 N2 C3 -144.6(6) . . . . ?
C4B Ir1 N2 C3 113.2(6) . . . . ?
C2B Ir1 N2 C3 41.5(6) . . . . ?
C1B Ir1 N2 C3 35.0(8) . . . . ?
C3B Ir1 N2 C3 77.2(6) . . . . ?
C5B Ir1 N2 C3 121.6(6) . . . . ?
Cl1 Ir1 N2 C3 -59.2(6) . . . . ?
N3' Ir1 N2 N1 36.3(4) . . . . ?
C4B Ir1 N2 N1 -65.9(5) . . . . ?
C2B Ir1 N2 N1 -137.7(5) . . . . ?
C1B Ir1 N2 N1 -144.2(5) . . . . ?
C3B Ir1 N2 N1 -102.0(5) . . . . ?
C5B Ir1 N2 N1 -57.6(7) . . . . ?
Cl1 Ir1 N2 N1 121.6(4) . . . . ?
N1 N2 C3 C4 0.4(7) . . . . ?
Ir1 N2 C3 C4 -178.9(5) . . . . ?
N1 N2 C3 C6 -178.6(7) . . . . ?
Ir1 N2 C3 C6 2.1(10) . . . . ?
N2 C3 C4 C5 -0.1(8) . . . . ?
C6 C3 C4 C5 178.8(8) . . . . ?
N2 N1 C5 C4 0.4(8) . . . . ?
C1A N1 C5 C4 179.2(6) . . . . ?
N2 N1 C5 C7 179.6(7) . . . . ?
C1A N1 C5 C7 -1.7(11) . . . . ?
C3 C4 C5 N1 -0.2(8) . . . . ?
C3 C4 C5 C7 -179.3(8) . . . . ?
C5 N1 C1A C4' 127.3(7) . . . . ?
N2 N1 C1A C4' -54.0(8) . . . . ?
C5' N1' N2' N3' 1.2(7) . . . . ?
C8 N1' N2' N3' 178.3(6) . . . . ?
N1' N2' N3' C4' -0.8(7) . . . . ?
N1' N2' N3' Ir1 -176.9(4) . . . . ?
N2 Ir1 N3' N2' 142.5(5) . . . . ?
C4B Ir1 N3' N2' -105.4(5) . . . . ?
C2B Ir1 N3' N2' -55.2(10) . . . . ?
C1B Ir1 N3' N2' -37.3(6) . . . . ?
C3B Ir1 N3' N2' -125.3(5) . . . . ?
C5B Ir1 N3' N2' -66.3(5) . . . . ?
Cl1 Ir1 N3' N2' 54.2(5) . . . . ?
N2 Ir1 N3' C4' -33.1(5) . . . . ?
C4B Ir1 N3' C4' 79.0(5) . . . . ?
C2B Ir1 N3' C4' 129.2(8) . . . . ?
C1B Ir1 N3' C4' 147.1(5) . . . . ?
C3B Ir1 N3' C4' 59.1(6) . . . . ?
C5B Ir1 N3' C4' 118.1(5) . . . . ?
Cl1 Ir1 N3' C4' -121.3(5) . . . . ?
N2' N3' C4' C5' 0.1(7) . . . . ?
Ir1 N3' C4' C5' 176.3(4) . . . . ?
N2' N3' C4' C1A 178.4(6) . . . . ?
Ir1 N3' C4' C1A -5.5(8) . . . . ?
N1 C1A C4' C5' -124.6(8) . . . . ?
N1 C1A C4' N3' 57.7(8) . . . . ?
N3' C4' C5' N1' 0.6(7) . . . . ?
C1A C4' C5' N1' -177.3(7) . . . . ?
N2' N1' C5' C4' -1.1(7) . . . . ?
C8 N1' C5' C4' -177.9(6) . . . . ?
N2' N1' C8 C9 169.4(11) . . . . ?
C5' N1' C8 C9 -14.1(14) . . . . ?
N2' N1' C8 C13 -13.5(10) . . . . ?
C5' N1' C8 C13 163.0(8) . . . . ?
C13 C8 C9 C10 -3(2) . . . . ?
N1' C8 C9 C10 174.1(13) . . . . ?
C8 C9 C10 C11 7(3) . . . . ?
C9 C10 C11 C12 -6(2) . . . . ?
C9 C10 C11 C14 177.9(13) . . . . ?
C10 C11 C12 C13 1.8(16) . . . . ?
C14 C11 C12 C13 178.2(8) . . . . ?
C11 C12 C13 C8 1.4(15) . . . . ?
C9 C8 C13 C12 -0.6(16) . . . . ?
N1' C8 C13 C12 -177.9(8) . . . . ?
C10 C11 C14 F143 169.9(11) . . . . ?
C12 C11 C14 F143 -6.5(11) . . . . ?
C10 C11 C14 F142 -68.9(13) . . . . ?
C12 C11 C14 F142 114.8(9) . . . . ?
C10 C11 C14 F141 49.5(13) . . . . ?
C12 C11 C14 F141 -126.8(9) . . . . ?
N3' Ir1 C1B C5B -51.9(5) . . . . ?
N2 Ir1 C1B C5B 128.6(5) . . . . ?
C4B Ir1 C1B C5B 37.7(4) . . . . ?
C2B Ir1 C1B C5B 119.1(6) . . . . ?
C3B Ir1 C1B C5B 80.8(5) . . . . ?
Cl1 Ir1 C1B C5B -138.7(4) . . . . ?
N3' Ir1 C1B C2B -171.0(4) . . . . ?
N2 Ir1 C1B C2B 9.5(7) . . . . ?
C4B Ir1 C1B C2B -81.4(4) . . . . ?
C3B Ir1 C1B C2B -38.3(4) . . . . ?
C5B Ir1 C1B C2B -119.1(6) . . . . ?
Cl1 Ir1 C1B C2B 102.2(4) . . . . ?
N3' Ir1 C1B C6B 68.0(10) . . . . ?
N2 Ir1 C1B C6B -111.5(9) . . . . ?
C4B Ir1 C1B C6B 157.6(10) . . . . ?
C2B Ir1 C1B C6B -121.0(11) . . . . ?
C3B Ir1 C1B C6B -159.3(10) . . . . ?
C5B Ir1 C1B C6B 119.9(11) . . . . ?
Cl1 Ir1 C1B C6B -18.8(9) . . . . ?
C5B C1B C2B C3B 0.8(8) . . . . ?
C6B C1B C2B C3B -175.8(8) . . . . ?
Ir1 C1B C2B C3B 62.1(5) . . . . ?
C5B C1B C2B C7B 172.5(8) . . . . ?
C6B C1B C2B C7B -4.1(13) . . . . ?
Ir1 C1B C2B C7B -126.2(8) . . . . ?
C5B C1B C2B Ir1 -61.3(5) . . . . ?
C6B C1B C2B Ir1 122.1(8) . . . . ?
N3' Ir1 C2B C3B -92.3(9) . . . . ?
N2 Ir1 C2B C3B 68.4(5) . . . . ?
C4B Ir1 C2B C3B -36.9(4) . . . . ?
C1B Ir1 C2B C3B -116.4(6) . . . . ?
C5B Ir1 C2B C3B -80.1(5) . . . . ?
Cl1 Ir1 C2B C3B 160.7(4) . . . . ?
N3' Ir1 C2B C1B 24.1(10) . . . . ?
N2 Ir1 C2B C1B -175.2(4) . . . . ?
C4B Ir1 C2B C1B 79.5(4) . . . . ?
C3B Ir1 C2B C1B 116.4(6) . . . . ?
C5B Ir1 C2B C1B 36.3(4) . . . . ?
Cl1 Ir1 C2B C1B -82.9(4) . . . . ?
N3' Ir1 C2B C7B 145.1(10) . . . . ?
N2 Ir1 C2B C7B -54.2(11) . . . . ?
C4B Ir1 C2B C7B -159.5(11) . . . . ?
C1B Ir1 C2B C7B 121.0(12) . . . . ?
C3B Ir1 C2B C7B -122.6(12) . . . . ?
C5B Ir1 C2B C7B 157.3(11) . . . . ?
Cl1 Ir1 C2B C7B 38.1(11) . . . . ?
C1B C2B C3B C4B -1.6(8) . . . . ?
C7B C2B C3B C4B -173.1(8) . . . . ?
Ir1 C2B C3B C4B 60.3(5) . . . . ?
C1B C2B C3B C8B 178.0(8) . . . . ?
C7B C2B C3B C8B 6.4(13) . . . . ?
Ir1 C2B C3B C8B -120.2(8) . . . . ?
C1B C2B C3B Ir1 -61.9(5) . . . . ?
C7B C2B C3B Ir1 126.5(9) . . . . ?
N3' Ir1 C3B C2B 151.2(4) . . . . ?
N2 Ir1 C3B C2B -121.1(4) . . . . ?
C4B Ir1 C3B C2B 119.2(6) . . . . ?
C1B Ir1 C3B C2B 38.7(5) . . . . ?
C5B Ir1 C3B C2B 80.7(5) . . . . ?
Cl1 Ir1 C3B C2B -28.1(6) . . . . ?
N3' Ir1 C3B C4B 32.0(5) . . . . ?
N2 Ir1 C3B C4B 119.7(4) . . . . ?
C2B Ir1 C3B C4B -119.2(6) . . . . ?
C1B Ir1 C3B C4B -80.5(4) . . . . ?
C5B Ir1 C3B C4B -38.5(4) . . . . ?
Cl1 Ir1 C3B C4B -147.3(3) . . . . ?
N3' Ir1 C3B C8B -85.8(9) . . . . ?
N2 Ir1 C3B C8B 1.8(8) . . . . ?
C4B Ir1 C3B C8B -117.9(9) . . . . ?
C2B Ir1 C3B C8B 122.9(10) . . . . ?
C1B Ir1 C3B C8B 161.6(9) . . . . ?
C5B Ir1 C3B C8B -156.4(9) . . . . ?
Cl1 Ir1 C3B C8B 94.8(8) . . . . ?
C2B C3B C4B C5B 1.7(8) . . . . ?
C8B C3B C4B C5B -177.8(7) . . . . ?
Ir1 C3B C4B C5B 62.0(4) . . . . ?
C2B C3B C4B C9B 172.5(7) . . . . ?
C8B C3B C4B C9B -7.1(11) . . . . ?
Ir1 C3B C4B C9B -127.2(7) . . . . ?
C2B C3B C4B Ir1 -60.3(5) . . . . ?
C8B C3B C4B Ir1 120.1(7) . . . . ?
N3' Ir1 C4B C3B -158.8(4) . . . . ?
N2 Ir1 C4B C3B -69.7(4) . . . . ?
C2B Ir1 C4B C3B 36.9(4) . . . . ?
C1B Ir1 C4B C3B 80.1(4) . . . . ?
C5B Ir1 C4B C3B 116.7(5) . . . . ?
Cl1 Ir1 C4B C3B 89.8(6) . . . . ?
N3' Ir1 C4B C5B 84.5(4) . . . . ?
N2 Ir1 C4B C5B 173.7(4) . . . . ?
C2B Ir1 C4B C5B -79.8(4) . . . . ?
C1B Ir1 C4B C5B -36.6(4) . . . . ?
C3B Ir1 C4B C5B -116.7(5) . . . . ?
Cl1 Ir1 C4B C5B -26.9(7) . . . . ?
N3' Ir1 C4B C9B -37.0(9) . . . . ?
N2 Ir1 C4B C9B 52.1(9) . . . . ?
C2B Ir1 C4B C9B 158.7(9) . . . . ?
C1B Ir1 C4B C9B -158.1(9) . . . . ?
C3B Ir1 C4B C9B 121.8(10) . . . . ?
C5B Ir1 C4B C9B -121.5(10) . . . . ?
Cl1 Ir1 C4B C9B -148.4(7) . . . . ?
C2B C1B C5B C4B 0.2(8) . . . . ?
C6B C1B C5B C4B 176.9(8) . . . . ?
Ir1 C1B C5B C4B -60.5(5) . . . . ?
C2B C1B C5B C10B -177.6(7) . . . . ?
C6B C1B C5B C10B -0.9(12) . . . . ?
Ir1 C1B C5B C10B 121.7(7) . . . . ?
C2B C1B C5B Ir1 60.7(5) . . . . ?
C6B C1B C5B Ir1 -122.6(8) . . . . ?
C3B C4B C5B C1B -1.2(7) . . . . ?
C9B C4B C5B C1B -172.0(7) . . . . ?
Ir1 C4B C5B C1B 60.9(5) . . . . ?
C3B C4B C5B C10B 176.7(7) . . . . ?
C9B C4B C5B C10B 5.9(11) . . . . ?
Ir1 C4B C5B C10B -121.3(7) . . . . ?
C3B C4B C5B Ir1 -62.1(4) . . . . ?
C9B C4B C5B Ir1 127.1(7) . . . . ?
N3' Ir1 C5B C1B 138.7(4) . . . . ?
N2 Ir1 C5B C1B -130.8(5) . . . . ?
C4B Ir1 C5B C1B -118.6(6) . . . . ?
C2B Ir1 C5B C1B -37.4(5) . . . . ?
C3B Ir1 C5B C1B -80.4(5) . . . . ?
Cl1 Ir1 C5B C1B 50.1(5) . . . . ?
N3' Ir1 C5B C4B -102.7(4) . . . . ?
N2 Ir1 C5B C4B -12.2(7) . . . . ?
C2B Ir1 C5B C4B 81.2(4) . . . . ?
C1B Ir1 C5B C4B 118.6(6) . . . . ?
C3B Ir1 C5B C4B 38.2(4) . . . . ?
Cl1 Ir1 C5B C4B 168.7(3) . . . . ?
N3' Ir1 C5B C10B 17.4(8) . . . . ?
N2 Ir1 C5B C10B 107.9(8) . . . . ?
C4B Ir1 C5B C10B 120.1(9) . . . . ?
C2B Ir1 C5B C10B -158.7(9) . . . . ?
C1B Ir1 C5B C10B -121.3(10) . . . . ?
C3B Ir1 C5B C10B 158.3(9) . . . . ?
Cl1 Ir1 C5B C10B -71.2(8) . . . . ?
C41C B1C C11C C16C -97.7(6) . . . . ?
C21C B1C C11C C16C 22.4(7) . . . . ?
C31C B1C C11C C16C 138.5(5) . . . . ?
C41C B1C C11C C12C 76.6(6) . . . . ?
C21C B1C C11C C12C -163.3(5) . . . . ?
C31C B1C C11C C12C -47.1(7) . . . . ?
C16C C11C C12C C13C -1.7(8) . . . . ?
B1C C11C C12C C13C -176.5(5) . . . . ?
C11C C12C C13C C14C 1.3(9) . . . . ?
C11C C12C C13C C17C -177.1(5) . . . . ?
C12C C13C C14C C15C 0.1(9) . . . . ?
C17C C13C C14C C15C 178.5(6) . . . . ?
C13C C14C C15C C16C -1.0(9) . . . . ?
C13C C14C C15C C18C 178.1(5) . . . . ?
C12C C11C C16C C15C 0.8(8) . . . . ?
B1C C11C C16C C15C 175.4(5) . . . . ?
C14C C15C C16C C11C 0.5(9) . . . . ?
C18C C15C C16C C11C -178.6(5) . . . . ?
C12C C13C C17C F171 -158.8(6) . . . . ?
C14C C13C C17C F171 22.8(9) . . . . ?
C12C C13C C17C F172 78.4(8) . . . . ?
C14C C13C C17C F172 -100.0(7) . . . . ?
C12C C13C C17C F173 -40.5(9) . . . . ?
C14C C13C C17C F173 141.2(6) . . . . ?
C14C C15C C18C F186 -79.5(10) . . . . ?
C16C C15C C18C F186 99.5(9) . . . . ?
C14C C15C C18C F184 156.9(8) . . . . ?
C16C C15C C18C F184 -24.0(10) . . . . ?
C14C C15C C18C F182 5.1(9) . . . . ?
C16C C15C C18C F182 -175.9(7) . . . . ?
C14C C15C C18C F181 128.3(7) . . . . ?
C16C C15C C18C F181 -52.6(8) . . . . ?
C14C C15C C18C F185 40.4(9) . . . . ?
C16C C15C C18C F185 -140.5(8) . . . . ?
C14C C15C C18C F187 91.1(12) . . . . ?
C16C C15C C18C F187 -89.8(12) . . . . ?
C14C C15C C18C F183 -115.9(7) . . . . ?
C16C C15C C18C F183 63.2(8) . . . . ?
C14C C15C C18C F189 -145.8(10) . . . . ?
C16C C15C C18C F189 33.3(11) . . . . ?
C14C C15C C18C F188 -30.1(10) . . . . ?
C16C C15C C18C F188 149.0(9) . . . . ?
C41C B1C C21C C22C 165.6(5) . . . . ?
C11C B1C C21C C22C 49.2(7) . . . . ?
C31C B1C C21C C22C -71.0(6) . . . . ?
C41C B1C C21C C26C -21.0(7) . . . . ?
C11C B1C C21C C26C -137.5(5) . . . . ?
C31C B1C C21C C26C 102.4(6) . . . . ?
C26C C21C C22C C23C 0.9(8) . . . . ?
B1C C21C C22C C23C 174.8(5) . . . . ?
C21C C22C C23C C24C 0.0(9) . . . . ?
C21C C22C C23C C27C 179.1(5) . . . . ?
C22C C23C C24C C25C -0.3(9) . . . . ?
C27C C23C C24C C25C -179.5(5) . . . . ?
C23C C24C C25C C26C -0.3(9) . . . . ?
C23C C24C C25C C28C 178.8(6) . . . . ?
C24C C25C C26C C21C 1.2(9) . . . . ?
C28C C25C C26C C21C -177.9(6) . . . . ?
C22C C21C C26C C25C -1.4(8) . . . . ?
B1C C21C C26C C25C -175.1(5) . . . . ?
C24C C23C C27C F275 47.3(10) . . . . ?
C22C C23C C27C F275 -131.8(8) . . . . ?
C24C C23C C27C F271 -34.2(10) . . . . ?
C22C C23C C27C F271 146.6(8) . . . . ?
C24C C23C C27C F273 -162.2(7) . . . . ?
C22C C23C C27C F273 18.6(9) . . . . ?
C24C C23C C27C F278 -116.9(15) . . . . ?
C22C C23C C27C F278 63.9(15) . . . . ?
C24C C23C C27C F276 176.0(7) . . . . ?
C22C C23C C27C F276 -3.2(9) . . . . ?
C24C C23C C27C F279 123.5(14) . . . . ?
C22C C23C C27C F279 -55.6(14) . . . . ?
C24C C23C C27C F277 5.5(11) . . . . ?
C22C C23C C27C F277 -173.6(9) . . . . ?
C24C C23C C27C F272 82.1(8) . . . . ?
C22C C23C C27C F272 -97.1(8) . . . . ?
C24C C23C C27C F274 -69.9(8) . . . . ?
C22C C23C C27C F274 110.9(8) . . . . ?
C26C C25C C28C F282 -36.9(10) . . . . ?
C24C C25C C28C F282 144.0(7) . . . . ?
C26C C25C C28C F283 91.2(8) . . . . ?
C24C C25C C28C F283 -87.8(9) . . . . ?
C26C C25C C28C F281 -153.6(6) . . . . ?
C24C C25C C28C F281 27.3(9) . . . . ?
C41C B1C C31C C32C -142.0(5) . . . . ?
C21C B1C C31C C32C 97.0(6) . . . . ?
C11C B1C C31C C32C -24.1(7) . . . . ?
C41C B1C C31C C36C 43.5(7) . . . . ?
C21C B1C C31C C36C -77.6(6) . . . . ?
C11C B1C C31C C36C 161.3(5) . . . . ?
C36C C31C C32C C33C -2.3(8) . . . . ?
B1C C31C C32C C33C -177.2(5) . . . . ?
C31C C32C C33C C34C 0.3(9) . . . . ?
C31C C32C C33C C37C 178.6(6) . . . . ?
C32C C33C C34C C35C 1.6(9) . . . . ?
C37C C33C C34C C35C -176.8(6) . . . . ?
C33C C34C C35C C36C -1.3(10) . . . . ?
C33C C34C C35C C38C -177.8(6) . . . . ?
C34C C35C C36C C31C -0.8(10) . . . . ?
C38C C35C C36C C31C 175.7(6) . . . . ?
C32C C31C C36C C35C 2.6(9) . . . . ?
B1C C31C C36C C35C 177.5(6) . . . . ?
C34C C33C C37C F371 80.4(9) . . . . ?
C32C C33C C37C F371 -97.9(8) . . . . ?
C34C C33C C37C F373 -158.1(6) . . . . ?
C32C C33C C37C F373 23.6(9) . . . . ?
C34C C33C C37C F372 -39.7(9) . . . . ?
C32C C33C C37C F372 141.9(6) . . . . ?
C34C C35C C38C F381 87.5(9) . . . . ?
C36C C35C C38C F381 -89.0(9) . . . . ?
C34C C35C C38C F383 -149.4(6) . . . . ?
C36C C35C C38C F383 34.1(9) . . . . ?
C34C C35C C38C F382 -31.6(9) . . . . ?
C36C C35C C38C F382 151.9(6) . . . . ?
C21C B1C C41C C46C -53.9(7) . . . . ?
C11C B1C C41C C46C 67.3(6) . . . . ?
C31C B1C C41C C46C -171.2(5) . . . . ?
C21C B1C C41C C42C 130.5(6) . . . . ?
C11C B1C C41C C42C -108.4(6) . . . . ?
C31C B1C C41C C42C 13.1(8) . . . . ?
C46C C41C C42C C43C 2.7(8) . . . . ?
B1C C41C C42C C43C 178.5(5) . . . . ?
C41C C42C C43C C44C -0.8(10) . . . . ?
C41C C42C C43C C47C 177.2(5) . . . . ?
C42C C43C C44C C45C -1.9(10) . . . . ?
C47C C43C C44C C45C -179.8(6) . . . . ?
C43C C44C C45C C46C 2.4(11) . . . . ?
C43C C44C C45C C48C -177.7(7) . . . . ?
C44C C45C C46C C41C -0.4(11) . . . . ?
C48C C45C C46C C41C 179.8(7) . . . . ?
C42C C41C C46C C45C -2.1(9) . . . . ?
B1C C41C C46C C45C -178.3(6) . . . . ?
C44C C43C C47C F473 -103.6(9) . . . . ?
C42C C43C C47C F473 78.4(9) . . . . ?
C44C C43C C47C F479 -172.8(10) . . . . ?
C42C C43C C47C F479 9.2(12) . . . . ?
C44C C43C C47C F478 58.2(10) . . . . ?
C42C C43C C47C F478 -119.8(9) . . . . ?
C44C C43C C47C F476 103.7(10) . . . . ?
C42C C43C C47C F476 -74.3(10) . . . . ?
C44C C43C C47C F474 -18.0(11) . . . . ?
C42C C43C C47C F474 164.0(9) . . . . ?
C44C C43C C47C F472 21.0(9) . . . . ?
C42C C43C C47C F472 -157.0(7) . . . . ?
C44C C43C C47C F475 -137.0(8) . . . . ?
C42C C43C C47C F475 45.0(9) . . . . ?
C44C C43C C47C F471 135.4(7) . . . . ?
C42C C43C C47C F471 -42.6(8) . . . . ?
C44C C43C C47C F477 -56.1(9) . . . . ?
C42C C43C C47C F477 125.9(8) . . . . ?
C46C C45C C48C F483 -25.1(13) . . . . ?
C44C C45C C48C F483 155.1(9) . . . . ?
C46C C45C C48C F481 95.9(11) . . . . ?
C44C C45C C48C F481 -83.9(12) . . . . ?
C46C C45C C48C F482 -145.3(9) . . . . ?
C44C C45C C48C F482 34.9(13) . . . . ?
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max 1.385
_refine_diff_density_min -0.831
_refine_diff_density_rms 0.124
_iucr_refine_instructions_details
;
TITL Chinmin5_P21byc in P2(1)/c
CELL 0.71073 19.4090 17.2163 21.6370 90.000 112.133 90.000
ZERR 4.00 0.0008 0.0008 0.0010 0.000 0.002 0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H B F Cl Ir N
UNIT 232 160 4 108 12 4 20
OMIT -1 0 2
OMIT -1 1 1
OMIT 1 1 0
OMIT 0 0 2
OMIT 0 1 1
OMIT 1 0 0
OMIT -3 1 3
OMIT 1 2 0
OMIT 0 1 2
OMIT -1 2 1
OMIT -2 0 2
OMIT 1 3 2
OMIT 1 3 0
OMIT 2 0 4
OMIT 0 3 4
OMIT 0 2 2
OMIT 1 1 1
OMIT -3 50
L.S. 25
ACTA
BOND $H
FMAP 2
PLAN 20
SADI 0.01 C18C F181 C18C F182 C18C F183
SADI 0.01 F181 F182 F182 F183 F183 F181
SADI 0.01 C18C F184 C18C F185 C18C F186
SADI 0.01 F184 F185 F185 F186 F186 F184
SADI 0.01 C18C F187 C18C F188 C18C F189
SADI 0.01 F187 F188 F188 F189 F189 F187
SADI 0.01 F277 F278 F278 F279 F279 F277
SADI 0.01 F274 F275 F275 F276 F276 F274
SADI 0.01 F271 F272 F272 F273 F273 F271
SADI 0.01 C27C F277 C27C F278 C27C F279
SADI 0.01 C27C F274 C27C F275 C27C F276
SADI 0.01 C27C F271 C27C F272 C27C F273
SADI 0.01 F474 F475 F475 F476 F476 F474
SADI 0.01 F471 F472 F472 F473 F473 F471
SADI 0.01 F477 F478 F478 F479 F479 F477
SADI 0.01 C47C F477 C47C F478 C47C F479
SADI 0.01 C47C F474 C47C F475 C47C F476
SADI 0.01 C47C F471 C47C F472 C47C F473
SADI 0.01 C1E CL1E C1E CL2E
SADI 0.01 C1E' CL3E C1E' CL4E
SADI 0.01 CL1E CL2E CL3E CL4E
CONF
SIZE 0.284 0.255 0.143
DELU 0.01 C18C F181 > F189
DELU 0.01 C47C F471 > F476
DELU 0.005 C27C F271 > F279
DELU 0.01 C1E C1E' CL1E > CL4E
WGHT 0.100000 15.000000
FVAR 0.050060
TEMP -103.150
PART 1
MOLE 3
C1E 1 0.850485 0.866478 0.712267 10.250000 0.058600
C1E' 1 0.898293 0.945875 0.737404 10.250000 0.049470
Cl1E 5 0.807645 0.943711 0.762344 10.250000 0.081010
Cl2E 5 0.884077 0.955596 0.665682 10.250000 0.107300
Cl3E 5 0.818602 0.916611 0.749820 10.250000 0.101880
Cl4E 5 0.884800 0.983923 0.658808 10.250000 0.084510
PART 0
MOLE 4
C1F 1 0.803437 0.792555 0.539433 10.500000 0.051840
PART 1
Cl1F 5 0.771420 0.754440 0.464021 10.250000 0.052920
Cl2F 5 0.751112 0.776631 0.584650 10.125000 0.062310
Cl2' 5 0.740137 0.749261 0.568513 10.125000 0.066220
PART 2
Cl1' 5 0.776715 0.747531 0.444708 10.100000 0.019630
Cl3F 5 0.798226 0.766776 0.462053 10.200000 0.040290
Cl4F 5 0.720342 0.767379 0.556342 10.200000 0.049250
PART 0
MOLE 1
Ir1 6 0.204502 0.526771 0.109597 11.000000 0.028410 =
0.044380 0.026590 -0.000670 0.007050 -0.000060
Cl1 5 0.123861 0.476431 0.004701 11.000000 0.041550 =
0.086010 0.034550 -0.010930 0.003220 -0.003910
N1 7 0.260355 0.372650 0.184135 11.000000 0.048280 =
0.035640 0.038670 -0.003430 0.016930 -0.005780
N2 7 0.198454 0.417051 0.151523 11.000000 0.041890 =
0.048660 0.030230 -0.002450 0.015620 -0.006510
C3 1 0.140210 0.377298 0.153839 11.000000 0.051730 =
0.055790 0.044200 -0.011580 0.023830 -0.016190
C4 1 0.165260 0.308685 0.188000 11.000000 0.083350 =
0.046770 0.065220 -0.013920 0.044570 -0.020070
AFIX 43
H4 2 0.135449 0.269842 0.196871 11.000000 -1.200000
AFIX 0
C5 1 0.242240 0.306894 0.207053 11.000000 0.082640 =
0.043230 0.050010 -0.004090 0.038050 -0.003570
C1A 1 0.333125 0.399379 0.191214 11.000000 0.042150 =
0.037120 0.041570 0.003550 0.010310 0.003300
AFIX 23
H1A1 2 0.370025 0.358116 0.212368 11.000000 -1.200000
H1A2 2 0.346386 0.445362 0.220864 11.000000 -1.200000
AFIX 0
N1' 7 0.358740 0.439512 0.036627 11.000000 0.037740 =
0.048000 0.041480 -0.005430 0.017400 0.002150
N2' 7 0.301875 0.486858 0.032481 11.000000 0.035300 =
0.053530 0.037910 -0.002040 0.012310 0.005720
N3' 7 0.289407 0.475030 0.087047 11.000000 0.035960 =
0.043850 0.033800 0.000760 0.013670 -0.000580
C4' 1 0.336502 0.420242 0.125793 11.000000 0.032430 =
0.035140 0.036480 -0.002640 0.005920 -0.001500
C5' 1 0.380263 0.397373 0.093370 11.000000 0.036030 =
0.035640 0.045770 -0.002270 0.011020 -0.000220
AFIX 43
H5' 2 0.418494 0.359316 0.107580 11.000000 -1.200000
AFIX 0
C6 1 0.061955 0.403244 0.123260 11.000000 0.053640 =
0.087560 0.064850 -0.002750 0.021370 -0.024520
AFIX 137
H6A 2 0.059590 0.452641 0.100039 11.000000 -1.500000
H6B 2 0.041791 0.410230 0.158156 11.000000 -1.500000
H6C 2 0.032627 0.364055 0.091321 11.000000 -1.500000
AFIX 0
C7 1 0.296484 0.245965 0.244226 11.000000 0.097750 =
0.044730 0.089140 0.016100 0.053490 0.012310
AFIX 137
H7A 2 0.315105 0.219123 0.213696 11.000000 -1.500000
H7B 2 0.271896 0.208481 0.263200 11.000000 -1.500000
H7C 2 0.338150 0.270193 0.280243 11.000000 -1.500000
AFIX 0
C8 1 0.384932 0.437026 -0.016999 11.000000 0.037190 =
0.049100 0.046210 -0.006360 0.018180 0.000490
C9 1 0.447312 0.400938 -0.010527 11.000000 0.111440 =
0.218860 0.058490 0.063480 0.050940 0.106290
AFIX 43
H9 2 0.477940 0.380312 0.031616 11.000000 -1.200000
AFIX 0
C10 1 0.468232 0.392967 -0.063741 11.000000 0.110880 =
0.180790 0.072630 0.045920 0.056690 0.103110
AFIX 43
H10 2 0.510507 0.362070 -0.058908 11.000000 -1.200000
AFIX 0
C11 1 0.432642 0.425887 -0.120305 11.000000 0.055360 =
0.047890 0.059220 -0.010370 0.033590 -0.004260
C12 1 0.366548 0.465766 -0.130858 11.000000 0.085870 =
0.081810 0.068310 0.023900 0.047770 0.024760
AFIX 43
H12 2 0.338956 0.489036 -0.172729 11.000000 -1.200000
AFIX 0
C13 1 0.342661 0.470260 -0.078561 11.000000 0.083450 =
0.068120 0.066960 0.016970 0.043990 0.024500
AFIX 43
H13 2 0.297350 0.496010 -0.084364 11.000000 -1.200000
AFIX 0
C14 1 0.458811 0.418131 -0.177604 11.000000 0.059200 =
0.057770 0.078040 -0.011370 0.041290 -0.002810
F141 4 0.471836 0.343786 -0.187306 11.000000 0.138130 =
0.056800 0.096340 -0.007250 0.081460 0.007650
F142 4 0.522291 0.455811 -0.165536 11.000000 0.077740 =
0.090360 0.099060 -0.004620 0.057730 -0.013660
F143 4 0.410803 0.444334 -0.235002 11.000000 0.082170 =
0.103020 0.063020 0.007430 0.038940 0.014970
C1B 1 0.168556 0.644728 0.084504 11.000000 0.064150 =
0.044790 0.039310 -0.000950 0.005590 0.004880
C2B 1 0.134075 0.613282 0.127022 11.000000 0.033650 =
0.059080 0.066440 -0.017000 0.016190 0.005280
C3B 1 0.192391 0.594608 0.188593 11.000000 0.059980 =
0.035140 0.043930 -0.004470 0.026230 0.000800
C4B 1 0.261729 0.612221 0.183502 11.000000 0.034740 =
0.039390 0.038180 -0.005860 0.008170 0.001740
C5B 1 0.245455 0.644398 0.118344 11.000000 0.053490 =
0.031570 0.055700 0.002120 0.031480 0.009900
C6B 1 0.128030 0.678267 0.014207 11.000000 0.130570 =
0.074110 0.059400 0.019610 -0.008640 0.030290
AFIX 137
H6B1 2 0.123774 0.734753 0.017108 11.000000 -1.500000
H6B2 2 0.078233 0.655408 -0.005537 11.000000 -1.500000
H6B3 2 0.156254 0.666016 -0.013757 11.000000 -1.500000
AFIX 0
C7B 1 0.052436 0.611914 0.112543 11.000000 0.045820 =
0.078070 0.187910 -0.034730 0.040320 0.002750
AFIX 137
H7B1 2 0.042976 0.580239 0.146149 11.000000 -1.500000
H7B2 2 0.026030 0.589603 0.068195 11.000000 -1.500000
H7B3 2 0.034791 0.665003 0.113796 11.000000 -1.500000
AFIX 0
C8B 1 0.185463 0.562517 0.249943 11.000000 0.145350 =
0.073170 0.074690 -0.009710 0.079050 -0.020000
AFIX 137
H8B1 2 0.190279 0.604706 0.281713 11.000000 -1.500000
H8B2 2 0.224785 0.524098 0.270253 11.000000 -1.500000
H8B3 2 0.136766 0.537641 0.238215 11.000000 -1.500000
AFIX 0
C9B 1 0.335539 0.610041 0.238458 11.000000 0.052320 =
0.062060 0.085450 -0.022040 -0.015120 0.008790
AFIX 137
H9B1 2 0.345906 0.660520 0.261039 11.000000 -1.500000
H9B2 2 0.373727 0.598605 0.220351 11.000000 -1.500000
H9B3 2 0.335930 0.569553 0.270425 11.000000 -1.500000
AFIX 0
C10B 1 0.301856 0.675131 0.092464 11.000000 0.107400 =
0.048800 0.122410 -0.004340 0.085300 -0.009610
AFIX 137
H10A 2 0.289315 0.728793 0.077284 11.000000 -1.500000
H10B 2 0.301729 0.642942 0.055065 11.000000 -1.500000
H10C 2 0.351341 0.673721 0.128147 11.000000 -1.500000
AFIX 0
MOLE 2
B1C 3 0.254187 0.958707 1.012233 11.000000 0.021790 =
0.028670 0.025550 0.000130 0.008460 -0.001170
C11C 1 0.322123 1.014230 1.011359 11.000000 0.021920 =
0.024130 0.021190 0.003050 0.003340 0.001430
C12C 1 0.354515 1.067744 1.062800 11.000000 0.027700 =
0.026500 0.026070 0.001350 0.011770 0.004000
AFIX 43
H12C 2 0.338069 1.068813 1.098959 11.000000 -1.200000
AFIX 0
C13C 1 0.409253 1.118983 1.063302 11.000000 0.030310 =
0.029760 0.029610 -0.004330 0.010270 0.000060
C14C 1 0.433636 1.120112 1.010634 11.000000 0.033720 =
0.036260 0.034280 -0.001100 0.014290 -0.010910
AFIX 43
H14C 2 0.471425 1.155215 1.010692 11.000000 -1.200000
AFIX 0
C15C 1 0.401999 1.069379 0.958316 11.000000 0.035260 =
0.036030 0.031090 0.004570 0.017220 -0.000690
C16C 1 0.347190 1.017162 0.959343 11.000000 0.027290 =
0.033270 0.023360 -0.003730 0.006940 0.000630
AFIX 43
H16C 2 0.326363 0.982369 0.922948 11.000000 -1.200000
AFIX 0
C17C 1 0.443623 1.171563 1.121008 11.000000 0.038820 =
0.041050 0.046850 -0.014820 0.017170 -0.008070
C18C 1 0.425803 1.071509 0.900515 11.000000 0.055000 =
0.055860 0.046180 -0.001070 0.028510 -0.016510
F171 4 0.475727 1.233487 1.106915 11.000000 0.124580 =
0.065530 0.094600 -0.043380 0.069320 -0.051980
F172 4 0.493879 1.135545 1.172674 11.000000 0.091200 =
0.079620 0.057700 -0.031980 -0.027010 0.022670
F173 4 0.395562 1.201629 1.144964 11.000000 0.066920 =
0.088920 0.076610 -0.044820 0.036250 -0.009340
PART 1
F181 4 0.445594 1.000181 0.886294 10.500000 0.046870
F182 4 0.482015 1.120315 0.907089 10.500000 0.062050
F183 4 0.367230 1.092959 0.844470 10.500000 0.047140
PART 2
F184 4 0.413787 1.005205 0.865996 10.300000 0.057710
F185 4 0.500522 1.081806 0.921013 10.300000 0.042950
F186 4 0.395975 1.127100 0.856800 10.300000 0.067440
PART 3
F187 4 0.483134 1.024437 0.902814 10.200000 0.070180
F188 4 0.447910 1.145571 0.889883 10.200000 0.028030
F189 4 0.368546 1.054770 0.840770 10.200000 0.050180
PART 0
C21C 1 0.240353 0.884516 0.961911 11.000000 0.027770 =
0.033140 0.021080 0.001660 0.008880 -0.004430
C22C 1 0.299608 0.837623 0.963044 11.000000 0.028480 =
0.032270 0.029240 -0.004440 0.012150 -0.003410
AFIX 43
H22C 2 0.348748 0.852109 0.990950 11.000000 -1.200000
AFIX 0
C23C 1 0.289149 0.770000 0.924499 11.000000 0.041260 =
0.036390 0.040170 -0.001200 0.023620 0.000250
C24C 1 0.219380 0.747107 0.883753 11.000000 0.050730 =
0.035220 0.032000 -0.013350 0.021500 -0.013890
AFIX 43
H24C 2 0.212282 0.701408 0.857464 11.000000 -1.200000
AFIX 0
C25C 1 0.159044 0.792002 0.881548 11.000000 0.035770 =
0.042150 0.026660 -0.008250 0.016070 -0.013690
C26C 1 0.169298 0.858306 0.919974 11.000000 0.027410 =
0.041070 0.027450 -0.002460 0.012400 -0.001960
AFIX 43
H26C 2 0.126888 0.887291 0.918053 11.000000 -1.200000
AFIX 0
C27C 1 0.353876 0.724531 0.927585 11.000000 0.061060 =
0.039230 0.069620 -0.018740 0.036240 0.000260
C28C 1 0.082511 0.768592 0.836201 11.000000 0.045380 =
0.065110 0.038390 -0.023470 0.020250 -0.015440
PART 1
F271 4 0.343486 0.647648 0.920815 10.400000 0.077720
F272 4 0.371349 0.746627 0.873564 10.400000 0.056570
F273 4 0.416878 0.737267 0.980605 10.400000 0.039520
PART 2
F274 4 0.353578 0.654332 0.959477 10.400000 0.062110
F275 4 0.360589 0.701676 0.871526 10.400000 0.062480
F276 4 0.421953 0.752528 0.965631 10.400000 0.044420
PART 3
F277 4 0.337256 0.665092 0.883129 10.200000 0.022400
F278 4 0.392662 0.693184 0.988009 10.200000 0.113790
F279 4 0.401911 0.770767 0.912413 10.200000 0.137570
PART 0
F281 4 0.076107 0.692680 0.824547 11.000000 0.075020 =
0.087340 0.127230 -0.046790 0.011860 -0.038490
F282 4 0.032748 0.781918 0.860139 11.000000 0.043910 =
0.193290 0.094220 -0.084410 0.033390 -0.041160
F283 4 0.064326 0.797179 0.776629 11.000000 0.061070 =
0.188890 0.052330 0.024960 -0.011510 -0.051610
C31C 1 0.274055 0.919384 1.085949 11.000000 0.029850 =
0.026720 0.027170 -0.002150 0.012220 -0.003530
C32C 1 0.347084 0.908699 1.131028 11.000000 0.028440 =
0.026260 0.029470 0.000360 0.012580 0.001550
AFIX 43
H32C 2 0.386798 0.926925 1.119380 11.000000 -1.200000
AFIX 0
C33C 1 0.363643 0.872398 1.192214 11.000000 0.036440 =
0.030140 0.029690 0.000860 0.004680 0.004190
C34C 1 0.307604 0.844578 1.211142 11.000000 0.046200 =
0.037330 0.028990 0.007590 0.013700 0.003460
C35C 1 0.235156 0.852137 1.167062 11.000000 0.043340 =
0.040210 0.032790 0.003450 0.023800 -0.000120
C36C 1 0.218380 0.888189 1.105635 11.000000 0.032080 =
0.031560 0.031960 0.002360 0.010730 -0.001790
AFIX 43
H36C 2 0.167859 0.891905 1.076041 11.000000 -1.200000
AFIX 0
C37C 1 0.442702 0.861047 1.237649 11.000000 0.041300 =
0.061650 0.037600 0.014260 0.003180 0.002840
C38C 1 0.173383 0.824981 1.187485 11.000000 0.059200 =
0.051930 0.056430 0.007530 0.038870 0.000430
F371 4 0.468300 0.790810 1.233618 11.000000 0.066210 =
0.069830 0.134540 -0.009200 -0.017800 0.041520
F372 4 0.452400 0.871502 1.302130 11.000000 0.057260 =
0.123390 0.034310 0.019320 -0.001250 -0.009510
F373 4 0.489551 0.910506 1.227355 11.000000 0.036430 =
0.097260 0.051570 0.021980 0.002020 0.002620
F381 4 0.152157 0.878076 1.218412 11.000000 0.173890 =
0.068120 0.212850 -0.013950 0.172890 -0.005030
F382 4 0.194565 0.764291 1.229173 11.000000 0.075940 =
0.072210 0.058040 0.019170 0.036540 -0.009490
F383 4 0.114815 0.800234 1.136516 11.000000 0.042010 =
0.111820 0.076470 0.036730 0.025940 -0.005290
C41C 1 0.181694 1.015539 0.988549 11.000000 0.025500 =
0.029850 0.024670 -0.002760 0.006570 -0.005120
C42C 1 0.145488 1.044619 1.028750 11.000000 0.033480 =
0.028860 0.026130 0.001020 0.010250 -0.000440
AFIX 43
H42C 2 0.163029 1.029845 1.074392 11.000000 -1.200000
AFIX 0
C43C 1 0.084539 1.094545 1.004078 11.000000 0.034520 =
0.034030 0.043690 -0.003900 0.018120 0.001010
C44C 1 0.058187 1.117907 0.938429 11.000000 0.033560 =
0.048180 0.045420 0.003820 0.007560 0.014660
AFIX 43
H44C 2 0.015827 1.150663 0.921015 11.000000 -1.200000
AFIX 0
C45C 1 0.094761 1.092614 0.898596 11.000000 0.038960 =
0.050340 0.031730 0.008830 0.007320 0.008560
C46C 1 0.154144 1.043079 0.923122 11.000000 0.030740 =
0.042570 0.028470 0.002510 0.012390 0.002970
AFIX 43
H46C 2 0.177765 1.026647 0.894070 11.000000 -1.200000
AFIX 0
C47C 1 0.046610 1.120372 1.048167 11.000000 0.052380 =
0.054010 0.057440 -0.009230 0.022410 0.010690
C48C 1 0.069147 1.119404 0.827872 11.000000 0.061940 =
0.088080 0.043050 0.022990 0.013810 0.034330
PART 1
F471 4 0.036544 1.061334 1.087355 10.400000 0.045900
F472 4 -0.024618 1.143351 1.014744 10.400000 0.048760
F473 4 0.079695 1.175836 1.090509 10.400000 0.060140
PART 2
F474 4 0.002179 1.182768 1.023455 10.300000 0.074210
F475 4 0.096546 1.142024 1.108953 10.300000 0.032020
F476 4 0.004141 1.064582 1.059739 10.300000 0.062550
PART 3
F477 4 0.044731 1.200809 1.046767 10.300000 0.055020
F478 4 -0.025386 1.101099 1.027889 10.300000 0.056910
F479 4 0.077081 1.104437 1.113482 10.300000 0.090300
PART 0
F481 4 0.015166 1.078400 0.788697 11.000000 0.229950 =
0.276730 0.034800 0.035530 -0.035270 -0.138640
F482 4 0.044286 1.190241 0.818995 11.000000 0.234340 =
0.135270 0.072980 0.053150 0.038870 0.109150
F483 4 0.117840 1.118718 0.802272 11.000000 0.121270 =
0.259140 0.071630 0.096150 0.058260 0.087380
HKLF 4
END
Q1 1 0.197400 0.474000 0.120000 11.000000 0.050000 1.390000
Q2 1 0.917700 0.905400 0.699700 11.000000 0.050000 1.130000
Q3 1 0.791200 0.782300 0.489700 11.000000 0.050000 1.110000
Q4 1 0.853900 0.997700 0.662100 11.000000 0.050000 1.080000
Q5 1 0.383400 0.780600 0.867500 11.000000 0.050000 1.030000
Q6 1 0.336900 1.073200 0.832200 11.000000 0.050000 0.960000
Q7 1 0.830600 0.888400 0.727400 11.000000 0.050000 0.960000
Q8 1 0.419200 0.487900 -0.090700 11.000000 0.050000 0.930000
Q9 1 0.036000 0.838600 0.816200 11.000000 0.050000 0.920000
Q10 1 0.399600 1.088100 0.850600 11.000000 0.050000 0.910000
Q11 1 0.428700 0.971800 0.880100 11.000000 0.050000 0.880000
Q12 1 0.367800 0.668300 0.899900 11.000000 0.050000 0.860000
Q13 1 0.027800 1.216300 1.022000 11.000000 0.050000 0.840000
Q14 1 0.151500 0.531200 0.089200 11.000000 0.050000 0.840000
Q15 1 0.396900 0.489900 -0.040100 11.000000 0.050000 0.810000
Q16 1 0.023200 1.031400 1.081100 11.000000 0.050000 0.790000
Q17 1 0.366600 0.656500 0.992400 11.000000 0.050000 0.780000
Q18 1 0.517200 1.185000 1.131900 11.000000 0.050000 0.760000
Q19 1 0.785800 0.948600 0.784000 11.000000 0.050000 0.740000
Q20 1 -0.044200 1.117200 0.998800 11.000000 0.050000 0.740000
HKLF 4
REM Chinmin5_P21byc in P2(1)/c
REM R1= 0.0514 for 9929 Fo > 4sig(Fo) and 0.0618 for all 11717 data
REM 915 parameters refined using 57 restraints
;
#===END
data_chinmin6_p1bar
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C48.75 H26 B Cl1.50 F24 N6 O4 Rh'
_chemical_formula_weight 1382.65
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Rh' 'Rh' -1.1178 0.9187
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'C 2/c '
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 39.396(4)
_cell_length_b 18.3734(16)
_cell_length_c 16.4800(16)
_cell_angle_alpha 90.00
_cell_angle_beta 106.912(5)
_cell_angle_gamma 90.00
_cell_volume 11413.0(19)
_cell_formula_units_Z 8
_cell_measurement_temperature 160(2)
_cell_measurement_reflns_used 9908
_cell_measurement_theta_min 2.494
_cell_measurement_theta_max 30.307
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_max 0.21
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.609
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5472
_exptl_absorpt_coefficient_mu 0.496
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.9026
_exptl_absorpt_correction_T_max 0.9567
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 160(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 123073
_diffrn_reflns_av_R_equivalents 0.0385
_diffrn_reflns_av_sigmaI/netI 0.0169
_diffrn_reflns_limit_h_min -46
_diffrn_reflns_limit_h_max 46
_diffrn_reflns_limit_k_min -21
_diffrn_reflns_limit_k_max 21
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 1.23
_diffrn_reflns_theta_max 25.00
_reflns_number_total 10039
_reflns_number_gt 8611
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1541P)^2^+117.6605P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10039
_refine_ls_number_parameters 819
_refine_ls_number_restraints 36
_refine_ls_R_factor_all 0.0645
_refine_ls_R_factor_gt 0.0557
_refine_ls_wR_factor_ref 0.1830
_refine_ls_wR_factor_gt 0.1646
_refine_ls_goodness_of_fit_ref 0.755
_refine_ls_restrained_S_all 0.775
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.169920(9) 0.110157(16) 0.61679(2) 0.02982(14) Uani 1 1 d . . .
N1 N 0.11965(10) 0.18268(19) 0.7001(2) 0.0334(8) Uani 1 1 d . . .
N2 N 0.12437(10) 0.1227(2) 0.6552(2) 0.0361(8) Uani 1 1 d . . .
C3 C 0.09301(14) 0.0882(3) 0.6327(3) 0.0492(12) Uani 1 1 d . . .
C4 C 0.06866(15) 0.1270(3) 0.6617(4) 0.0568(14) Uani 1 1 d . . .
H4A H 0.0451 0.1146 0.6541 0.068 Uiso 1 1 calc R . .
C5 C 0.08581(13) 0.1872(3) 0.7037(3) 0.0441(11) Uani 1 1 d . . .
C6 C 0.08742(19) 0.0200(4) 0.5810(5) 0.078(2) Uani 1 1 d . . .
H61 H 0.0982 0.0250 0.5361 0.117 Uiso 1 1 calc R . .
H62 H 0.0624 0.0114 0.5573 0.117 Uiso 1 1 calc R . .
H63 H 0.0980 -0.0203 0.6165 0.117 Uiso 1 1 calc R . .
C7 C 0.07331(16) 0.2491(3) 0.7460(4) 0.0594(14) Uani 1 1 d . . .
H72 H 0.0863 0.2498 0.8051 0.089 Uiso 1 1 calc R . .
H71 H 0.0485 0.2433 0.7399 0.089 Uiso 1 1 calc R . .
H73 H 0.0771 0.2940 0.7201 0.089 Uiso 1 1 calc R . .
C1A C 0.14853(11) 0.2349(2) 0.7285(2) 0.0322(9) Uani 1 1 d . . .
H2A H 0.1695 0.2108 0.7644 0.039 Uiso 1 1 calc R . .
H1A H 0.1418 0.2732 0.7611 0.039 Uiso 1 1 calc R . .
N1' N 0.16115(9) 0.32833(17) 0.5456(2) 0.0265(7) Uani 1 1 d . . .
N2' N 0.16850(9) 0.25901(17) 0.5308(2) 0.0285(7) Uani 1 1 d . . .
N3' N 0.16567(9) 0.22202(18) 0.5967(2) 0.0286(7) Uani 1 1 d . . .
C4' C 0.15641(10) 0.2664(2) 0.6528(2) 0.0276(8) Uani 1 1 d . . .
C5' C 0.15346(11) 0.3351(2) 0.6205(2) 0.0283(8) Uani 1 1 d . . .
H5' H 0.1475 0.3773 0.6444 0.034 Uiso 1 1 calc R . .
C6' C 0.15809(11) 0.3823(2) 0.4814(3) 0.0284(8) Uani 1 1 d . . .
C7' C 0.14275(12) 0.4484(2) 0.4894(3) 0.0361(9) Uani 1 1 d . . .
H7' H 0.1360 0.4588 0.5378 0.043 Uiso 1 1 calc R . .
C8' C 0.13746(12) 0.4992(2) 0.4246(3) 0.0372(10) Uani 1 1 d . . .
H8' H 0.1271 0.5441 0.4286 0.045 Uiso 1 1 calc R . .
C9' C 0.14788(11) 0.4815(2) 0.3544(3) 0.0332(9) Uani 1 1 d . . .
C10' C 0.16455(15) 0.4169(3) 0.3476(3) 0.0466(12) Uani 1 1 d . . .
H10' H 0.1720 0.4073 0.3001 0.056 Uiso 1 1 calc R . .
C11' C 0.17001(14) 0.3668(3) 0.4125(3) 0.0436(11) Uani 1 1 d . . .
H11' H 0.1816 0.3231 0.4098 0.052 Uiso 1 1 calc R . .
N4' N 0.13995(11) 0.5331(2) 0.2829(2) 0.0400(9) Uani 1 1 d . . .
O1' O 0.14400(11) 0.5123(2) 0.2159(2) 0.0527(9) Uani 1 1 d . . .
O2' O 0.12933(11) 0.59398(19) 0.2937(2) 0.0528(9) Uani 1 1 d . . .
C1B C 0.17452(14) 0.0112(3) 0.6445(3) 0.0424(11) Uani 1 1 d . . .
O1B O 0.17812(13) -0.04832(19) 0.6618(3) 0.0644(11) Uani 1 1 d . . .
C2B C 0.21041(14) 0.1008(2) 0.5817(3) 0.0366(10) Uani 1 1 d . . .
O2B O 0.23541(10) 0.0924(2) 0.5614(2) 0.0515(9) Uani 1 1 d . . .
B1C B 0.13934(11) 0.2683(2) 0.0701(3) 0.0255(9) Uani 1 1 d . . .
C11C C 0.12680(10) 0.2005(2) 0.0032(2) 0.0268(8) Uani 1 1 d . . .
C12C C 0.15139(10) 0.1583(2) -0.0222(2) 0.0277(8) Uani 1 1 d . . .
H12C H 0.1754 0.1686 0.0001 0.033 Uiso 1 1 calc R . .
C13C C 0.14104(11) 0.1012(2) -0.0801(3) 0.0299(9) Uani 1 1 d . . .
C14C C 0.10594(11) 0.0813(2) -0.1117(3) 0.0338(9) Uani 1 1 d . . .
H14C H 0.0991 0.0432 -0.1501 0.041 Uiso 1 1 calc R . .
C15C C 0.08104(11) 0.1200(2) -0.0845(3) 0.0355(9) Uani 1 1 d . . .
C16C C 0.09130(11) 0.1783(2) -0.0283(3) 0.0317(9) Uani 1 1 d . . .
H16C H 0.0740 0.2032 -0.0112 0.038 Uiso 1 1 calc R . .
C17C C 0.16925(12) 0.0623(2) -0.1078(3) 0.0340(9) Uani 1 1 d . . .
C18C C 0.04262(13) 0.1010(3) -0.1171(4) 0.0493(12) Uani 1 1 d . . .
F171 F 0.19171(8) 0.10878(14) -0.1283(2) 0.0472(7) Uani 1 1 d . . .
F172 F 0.18957(8) 0.01979(16) -0.04701(18) 0.0496(7) Uani 1 1 d . . .
F173 F 0.15620(8) 0.02030(18) -0.1760(2) 0.0580(8) Uani 1 1 d . . .
F181 F 0.03580(11) 0.0493(3) -0.1745(4) 0.140(3) Uani 1 1 d . . .
F182 F 0.02284(9) 0.1561(3) -0.1562(3) 0.0925(14) Uani 1 1 d . . .
F183 F 0.02851(9) 0.0832(3) -0.0569(3) 0.0854(13) Uani 1 1 d . . .
C21C C 0.10557(10) 0.3224(2) 0.0650(2) 0.0269(8) Uani 1 1 d . . .
C22C C 0.08493(11) 0.3476(2) -0.0143(3) 0.0331(9) Uani 1 1 d . . .
H22C H 0.0910 0.3338 -0.0625 0.040 Uiso 1 1 calc R . .
C23C C 0.05556(13) 0.3925(2) -0.0234(3) 0.0395(10) Uani 1 1 d . A .
C24C C 0.04617(12) 0.4149(3) 0.0473(3) 0.0409(10) Uani 1 1 d . . .
H24C H 0.0266 0.4449 0.0418 0.049 Uiso 1 1 calc R . .
C25C C 0.06653(12) 0.3918(2) 0.1260(3) 0.0367(10) Uani 1 1 d . . .
C26C C 0.09565(11) 0.3470(2) 0.1346(3) 0.0324(9) Uani 1 1 d . . .
H26C H 0.1090 0.3329 0.1887 0.039 Uiso 1 1 calc R . .
C27C C 0.03458(13) 0.4154(3) -0.1092(4) 0.0655(17) Uani 1 1 d DU . .
C28C C 0.05670(14) 0.4164(3) 0.2027(3) 0.0556(14) Uani 1 1 d . . .
F271 F 0.0529(2) 0.4188(5) -0.1658(5) 0.058(2) Uiso 0.40 1 d PDU A 1
F272 F 0.0101(3) 0.3594(5) -0.1440(6) 0.080(3) Uiso 0.40 1 d PDU A 1
F273 F 0.0144(3) 0.4733(5) -0.1176(7) 0.082(3) Uiso 0.40 1 d PDU A 1
F274 F 0.0440(2) 0.3910(5) -0.1751(5) 0.0462(18) Uiso 0.40 1 d PDU A 2
F275 F 0.0000(2) 0.4103(7) -0.1263(7) 0.087(3) Uiso 0.40 1 d PDU A 2
F276 F 0.0397(3) 0.4907(5) -0.1157(6) 0.078(3) Uiso 0.40 1 d PDU A 2
F277 F 0.0282(4) 0.3615(8) -0.1664(10) 0.061(4) Uiso 0.20 1 d PDU A 3
F278 F 0.0029(2) 0.4436(6) -0.1102(6) 0.0153(19) Uiso 0.20 1 d PDU A 3
F279 F 0.0522(5) 0.4677(9) -0.1375(15) 0.094(6) Uiso 0.20 1 d PDU A 3
F281 F 0.02235(9) 0.4116(3) 0.1936(2) 0.0779(11) Uani 1 1 d . . .
F282 F 0.06454(12) 0.4871(2) 0.2200(3) 0.0923(13) Uani 1 1 d . . .
F283 F 0.07422(12) 0.3826(3) 0.2733(2) 0.0997(17) Uani 1 1 d . . .
C31C C 0.15371(10) 0.2311(2) 0.1650(2) 0.0252(8) Uani 1 1 d . . .
C32C C 0.12962(11) 0.1971(2) 0.2009(3) 0.0298(8) Uani 1 1 d . . .
H32C H 0.1058 0.1949 0.1696 0.036 Uiso 1 1 calc R . .
C33C C 0.14007(12) 0.1666(2) 0.2819(3) 0.0340(9) Uani 1 1 d . . .
C34C C 0.17528(12) 0.1665(2) 0.3297(3) 0.0340(9) Uani 1 1 d . . .
H34C H 0.1824 0.1462 0.3837 0.041 Uiso 1 1 calc R . .
C35C C 0.19953(11) 0.1975(2) 0.2947(3) 0.0303(8) Uani 1 1 d . . .
C36C C 0.18914(10) 0.2293(2) 0.2141(2) 0.0275(8) Uani 1 1 d . . .
H36C H 0.2063 0.2498 0.1926 0.033 Uiso 1 1 calc R . .
C37C C 0.11198(14) 0.1362(3) 0.3164(4) 0.0503(13) Uani 1 1 d . . .
C38C C 0.23787(12) 0.2020(3) 0.3452(3) 0.0415(11) Uani 1 1 d . . .
F371 F 0.09369(9) 0.0823(2) 0.2684(2) 0.0746(11) Uani 1 1 d . . .
F372 F 0.08821(12) 0.1863(3) 0.3203(3) 0.1039(17) Uani 1 1 d . . .
F373 F 0.12456(10) 0.1085(2) 0.3944(2) 0.0680(10) Uani 1 1 d . . .
F381 F 0.24717(10) 0.1545(3) 0.4083(2) 0.0858(13) Uani 1 1 d . . .
F382 F 0.24582(12) 0.2649(2) 0.3812(5) 0.153(3) Uani 1 1 d . . .
F383 F 0.25966(9) 0.1868(3) 0.3008(2) 0.0958(16) Uani 1 1 d . . .
C41C C 0.17026(10) 0.3203(2) 0.0514(2) 0.0257(8) Uani 1 1 d . . .
C42C C 0.18515(11) 0.3751(2) 0.1100(3) 0.0290(8) Uani 1 1 d . . .
H42C H 0.1767 0.3811 0.1567 0.035 Uiso 1 1 calc R . .
C43C C 0.21194(10) 0.4209(2) 0.1017(3) 0.0299(8) Uani 1 1 d . . .
C44C C 0.22462(11) 0.4153(2) 0.0316(3) 0.0339(9) Uani 1 1 d . . .
H44C H 0.2424 0.4461 0.0254 0.041 Uiso 1 1 calc R . .
C45C C 0.21008(11) 0.3628(2) -0.0286(3) 0.0323(9) Uani 1 1 d . B .
C46C C 0.18320(10) 0.3166(2) -0.0187(2) 0.0278(8) Uani 1 1 d . . .
H46C H 0.1736 0.2823 -0.0605 0.033 Uiso 1 1 calc R . .
C47C C 0.22717(12) 0.4771(2) 0.1683(3) 0.0385(10) Uani 1 1 d . . .
C48C C 0.22421(9) 0.3536(2) -0.1020(3) 0.0425(11) Uani 1 1 d DU . .
F471 F 0.22984(11) 0.45269(19) 0.24700(18) 0.0704(10) Uani 1 1 d . . .
F472 F 0.20724(8) 0.53657(16) 0.1595(2) 0.0559(8) Uani 1 1 d . . .
F473 F 0.25933(8) 0.49946(18) 0.1694(2) 0.0638(9) Uani 1 1 d . . .
F481 F 0.25685(15) 0.3777(4) -0.0928(4) 0.0364(14) Uiso 0.40 1 d PDU B 1
F482 F 0.22663(19) 0.2787(3) -0.1221(5) 0.0433(15) Uiso 0.40 1 d PDU B 1
F483 F 0.20260(18) 0.3792(5) -0.1760(4) 0.0561(18) Uiso 0.45 1 d PDU B 1
F484 F 0.25884(18) 0.3431(5) -0.0798(5) 0.0360(19) Uiso 0.30 1 d PDU B 2
F485 F 0.2092(2) 0.3032(5) -0.1566(6) 0.046(2) Uiso 0.30 1 d PDU B 2
F486 F 0.2188(3) 0.4176(5) -0.1460(7) 0.062(3) Uiso 0.30 1 d PDU B 2
F487 F 0.2464(3) 0.2972(6) -0.0909(8) 0.076(3) Uiso 0.30 1 d PDU B 3
F488 F 0.20002(19) 0.3435(5) -0.1757(4) 0.0309(17) Uiso 0.30 1 d PDU B 3
F489 F 0.2437(3) 0.4110(5) -0.1133(7) 0.073(3) Uiso 0.35 1 d PDU B 3
C1D C 0.9460(6) 0.3377(13) 0.0188(15) 0.119(6) Uiso 0.50 1 d P . .
Cl2D Cl 0.92431(11) 0.2633(3) 0.0213(3) 0.1068(16) Uani 0.50 1 d P . .
Cl1D Cl 0.93628(10) 0.3949(2) -0.0557(3) 0.0853(11) Uani 0.50 1 d P . .
C1E C 0.0032(10) 0.162(2) 0.173(3) 0.103(11) Uiso 0.25 1 d P . .
Cl1E Cl 0.0231(4) 0.2199(8) 0.1045(9) 0.074(3) Uiso 0.13 1 d P . .
Cl2E Cl 0.0022(6) 0.0876(14) 0.1319(15) 0.120(6) Uiso 0.13 1 d P . .
Cl3E Cl 0.0128(9) 0.136(2) 0.103(2) 0.159(10) Uiso 0.13 1 d P . .
Cl4E Cl 0.0063(8) 0.2344(16) 0.2132(18) 0.145(9) Uiso 0.13 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0396(2) 0.0209(2) 0.0283(2) -0.00009(11) 0.00894(15) -0.00146(12)
N1 0.041(2) 0.0323(18) 0.0304(18) 0.0010(14) 0.0150(15) -0.0039(15)
N2 0.041(2) 0.0329(19) 0.0347(19) -0.0033(15) 0.0111(16) -0.0070(16)
C3 0.045(3) 0.053(3) 0.049(3) -0.008(2) 0.014(2) -0.020(2)
C4 0.040(3) 0.073(4) 0.058(3) -0.005(3) 0.016(2) -0.018(3)
C5 0.043(3) 0.053(3) 0.040(2) 0.005(2) 0.018(2) -0.001(2)
C6 0.076(4) 0.075(4) 0.086(5) -0.038(4) 0.028(4) -0.043(4)
C7 0.062(3) 0.062(3) 0.066(4) 0.001(3) 0.037(3) 0.006(3)
C1A 0.041(2) 0.031(2) 0.0232(19) 0.0003(16) 0.0062(17) -0.0033(17)
N1' 0.0333(17) 0.0226(16) 0.0244(16) 0.0016(13) 0.0096(13) 0.0012(13)
N2' 0.0367(18) 0.0216(16) 0.0287(17) 0.0017(13) 0.0121(14) 0.0027(13)
N3' 0.0332(17) 0.0239(17) 0.0281(16) -0.0002(13) 0.0078(14) -0.0001(13)
C4' 0.031(2) 0.0260(19) 0.0234(18) 0.0005(15) 0.0049(15) -0.0009(15)
C5' 0.036(2) 0.0253(19) 0.0259(19) -0.0028(15) 0.0127(16) 0.0000(16)
C6' 0.033(2) 0.0255(19) 0.028(2) 0.0025(15) 0.0115(17) -0.0007(15)
C7' 0.051(3) 0.029(2) 0.031(2) 0.0024(17) 0.0172(19) 0.0060(19)
C8' 0.050(3) 0.025(2) 0.039(2) 0.0019(17) 0.018(2) 0.0059(18)
C9' 0.034(2) 0.031(2) 0.035(2) 0.0081(17) 0.0106(17) -0.0038(17)
C10' 0.073(3) 0.039(3) 0.040(3) 0.009(2) 0.034(2) 0.010(2)
C11' 0.062(3) 0.033(2) 0.043(3) 0.008(2) 0.029(2) 0.013(2)
N4' 0.048(2) 0.036(2) 0.038(2) 0.0105(16) 0.0141(17) -0.0049(17)
O1' 0.074(2) 0.050(2) 0.0410(19) 0.0139(16) 0.0289(18) 0.0003(18)
O2' 0.071(2) 0.0339(18) 0.054(2) 0.0145(16) 0.0201(19) 0.0050(17)
C1B 0.061(3) 0.032(3) 0.039(2) -0.0027(19) 0.020(2) -0.003(2)
O1B 0.102(3) 0.0237(18) 0.072(3) 0.0059(17) 0.032(2) -0.0012(18)
C2B 0.052(3) 0.023(2) 0.035(2) -0.0017(17) 0.012(2) -0.0017(18)
O2B 0.054(2) 0.049(2) 0.057(2) -0.0081(17) 0.0269(18) -0.0018(17)
B1C 0.024(2) 0.029(2) 0.026(2) -0.0002(17) 0.0090(17) 0.0026(17)
C11C 0.0281(19) 0.029(2) 0.0236(18) 0.0034(15) 0.0082(15) 0.0021(15)
C12C 0.0265(19) 0.0276(19) 0.0277(19) 0.0020(16) 0.0057(15) 0.0034(15)
C13C 0.035(2) 0.028(2) 0.027(2) 0.0030(15) 0.0082(17) 0.0051(16)
C14C 0.035(2) 0.031(2) 0.032(2) -0.0049(17) 0.0044(17) -0.0001(17)
C15C 0.030(2) 0.036(2) 0.038(2) -0.0007(18) 0.0052(18) -0.0014(17)
C16C 0.027(2) 0.034(2) 0.035(2) -0.0015(17) 0.0096(17) 0.0031(16)
C17C 0.042(2) 0.028(2) 0.034(2) 0.0016(17) 0.0137(18) 0.0065(18)
C18C 0.034(3) 0.052(3) 0.055(3) -0.007(2) 0.004(2) -0.007(2)
F171 0.0512(16) 0.0394(15) 0.0623(18) 0.0088(12) 0.0341(15) 0.0094(12)
F172 0.0533(16) 0.0475(16) 0.0534(16) 0.0190(13) 0.0241(13) 0.0253(13)
F173 0.0589(18) 0.0643(19) 0.0535(17) -0.0280(15) 0.0203(14) 0.0034(15)
F181 0.048(2) 0.168(5) 0.196(6) -0.130(5) 0.022(3) -0.037(3)
F182 0.0331(17) 0.111(3) 0.111(3) 0.045(3) -0.0151(18) -0.0062(18)
F183 0.0371(17) 0.127(3) 0.086(3) 0.036(3) 0.0087(17) -0.020(2)
C21C 0.0264(19) 0.0271(19) 0.0278(19) 0.0009(15) 0.0091(15) 0.0005(15)
C22C 0.037(2) 0.034(2) 0.031(2) 0.0043(17) 0.0153(18) 0.0060(18)
C23C 0.038(2) 0.039(3) 0.043(3) 0.0080(19) 0.014(2) 0.0097(18)
C24C 0.036(2) 0.040(2) 0.048(3) 0.004(2) 0.015(2) 0.0140(19)
C25C 0.036(2) 0.038(2) 0.038(2) -0.0047(18) 0.0142(19) 0.0068(18)
C26C 0.031(2) 0.035(2) 0.032(2) -0.0021(17) 0.0099(17) 0.0048(17)
C27C 0.057(3) 0.081(4) 0.060(4) 0.028(3) 0.019(3) 0.036(3)
C28C 0.049(3) 0.072(4) 0.047(3) -0.008(3) 0.017(2) 0.026(3)
F281 0.0512(19) 0.124(3) 0.069(2) -0.016(2) 0.0353(17) 0.010(2)
F282 0.102(3) 0.088(3) 0.099(3) -0.049(2) 0.048(3) 0.000(2)
F283 0.105(3) 0.158(4) 0.042(2) 0.006(2) 0.032(2) 0.072(3)
C31C 0.0272(19) 0.0208(18) 0.0279(19) -0.0035(15) 0.0087(15) 0.0029(14)
C32C 0.0269(19) 0.030(2) 0.033(2) 0.0025(16) 0.0091(16) 0.0004(16)
C33C 0.040(2) 0.030(2) 0.037(2) 0.0036(17) 0.0186(19) 0.0011(18)
C34C 0.046(2) 0.029(2) 0.027(2) 0.0029(16) 0.0109(18) 0.0055(18)
C35C 0.032(2) 0.028(2) 0.029(2) -0.0030(16) 0.0059(17) 0.0050(16)
C36C 0.0283(19) 0.0251(19) 0.030(2) -0.0015(15) 0.0094(16) 0.0016(15)
C37C 0.049(3) 0.053(3) 0.057(3) 0.024(3) 0.027(2) 0.006(2)
C38C 0.038(2) 0.038(2) 0.041(2) 0.000(2) 0.000(2) 0.0058(19)
F371 0.058(2) 0.090(3) 0.070(2) 0.029(2) 0.0084(17) -0.0299(19)
F372 0.099(3) 0.096(3) 0.157(4) 0.060(3) 0.101(3) 0.043(2)
F373 0.075(2) 0.087(3) 0.0480(18) 0.0227(16) 0.0267(17) -0.0126(18)
F381 0.055(2) 0.122(3) 0.065(2) 0.043(2) -0.0061(17) 0.004(2)
F382 0.066(3) 0.068(3) 0.252(7) -0.074(4) -0.066(4) 0.011(2)
F383 0.0351(17) 0.192(5) 0.059(2) 0.020(3) 0.0108(15) 0.017(2)
C41C 0.0244(18) 0.0276(19) 0.0250(18) 0.0016(15) 0.0069(15) 0.0033(15)
C42C 0.031(2) 0.0277(19) 0.030(2) 0.0008(16) 0.0117(17) 0.0049(16)
C43C 0.0281(19) 0.028(2) 0.032(2) 0.0004(16) 0.0068(16) 0.0026(16)
C44C 0.026(2) 0.038(2) 0.037(2) 0.0055(18) 0.0078(17) -0.0027(17)
C45C 0.027(2) 0.041(2) 0.030(2) 0.0047(18) 0.0084(16) 0.0007(17)
C46C 0.0257(19) 0.033(2) 0.0241(19) 0.0003(16) 0.0060(15) 0.0024(16)
C47C 0.035(2) 0.035(2) 0.043(2) -0.0009(19) 0.0079(19) -0.0025(18)
C48C 0.032(2) 0.061(3) 0.037(2) 0.000(2) 0.0142(19) -0.007(2)
F471 0.106(3) 0.060(2) 0.0340(15) -0.0053(14) 0.0040(16) -0.0266(19)
F472 0.0496(16) 0.0443(16) 0.072(2) -0.0189(14) 0.0142(15) 0.0061(13)
F473 0.0397(16) 0.065(2) 0.089(2) -0.0373(18) 0.0212(15) -0.0173(14)
Cl2D 0.073(2) 0.109(3) 0.106(3) 0.045(3) -0.024(2) -0.016(2)
Cl1D 0.074(2) 0.081(2) 0.110(3) 0.000(2) 0.040(2) -0.0153(17)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 C2B 1.856(5) . ?
Rh1 C1B 1.870(5) . ?
Rh1 N3' 2.081(3) . ?
Rh1 N2 2.082(4) . ?
N1 C5 1.354(6) . ?
N1 N2 1.370(5) . ?
N1 C1A 1.457(5) . ?
N2 C3 1.342(6) . ?
C3 C4 1.388(8) . ?
C3 C6 1.494(8) . ?
C4 C5 1.374(8) . ?
C4 H4A 0.9300 . ?
C5 C7 1.490(8) . ?
C6 H61 0.9600 . ?
C6 H62 0.9600 . ?
C6 H63 0.9600 . ?
C7 H72 0.9600 . ?
C7 H71 0.9600 . ?
C7 H73 0.9600 . ?
C1A C4' 1.487(5) . ?
C1A H2A 0.9700 . ?
C1A H1A 0.9700 . ?
N1' N2' 1.344(4) . ?
N1' C5' 1.359(5) . ?
N1' C6' 1.429(5) . ?
N2' N3' 1.313(5) . ?
N3' C4' 1.359(5) . ?
C4' C5' 1.362(6) . ?
C5' H5' 0.9300 . ?
C6' C7' 1.379(6) . ?
C6' C11' 1.380(6) . ?
C7' C8' 1.388(6) . ?
C7' H7' 0.9300 . ?
C8' C9' 1.375(6) . ?
C8' H8' 0.9300 . ?
C9' C10' 1.377(7) . ?
C9' N4' 1.472(5) . ?
C10' C11' 1.381(7) . ?
C10' H10' 0.9300 . ?
C11' H11' 0.9300 . ?
N4' O1' 1.223(5) . ?
N4' O2' 1.225(5) . ?
C1B O1B 1.129(6) . ?
C2B O2B 1.139(6) . ?
B1C C11C 1.641(6) . ?
B1C C21C 1.643(5) . ?
B1C C41C 1.646(6) . ?
B1C C31C 1.649(6) . ?
C11C C12C 1.397(5) . ?
C11C C16C 1.404(6) . ?
C12C C13C 1.397(6) . ?
C12C H12C 0.9300 . ?
C13C C14C 1.378(6) . ?
C13C C17C 1.499(6) . ?
C14C C15C 1.387(6) . ?
C14C H14C 0.9300 . ?
C15C C16C 1.396(6) . ?
C15C C18C 1.493(6) . ?
C16C H16C 0.9300 . ?
C17C F172 1.337(5) . ?
C17C F173 1.337(5) . ?
C17C F171 1.342(5) . ?
C18C F181 1.312(7) . ?
C18C F183 1.312(7) . ?
C18C F182 1.324(7) . ?
C21C C26C 1.391(6) . ?
C21C C22C 1.402(6) . ?
C22C C23C 1.393(6) . ?
C22C H22C 0.9300 . ?
C23C C24C 1.383(7) . ?
C23C C27C 1.476(7) . ?
C24C C25C 1.379(7) . ?
C24C H24C 0.9300 . ?
C25C C26C 1.385(6) . ?
C25C C28C 1.496(7) . ?
C26C H26C 0.9300 . ?
C27C F273 1.311(8) . ?
C27C F275 1.313(8) . ?
C27C F274 1.324(7) . ?
C27C F271 1.338(8) . ?
C27C F277 1.339(11) . ?
C27C F278 1.347(9) . ?
C27C F279 1.347(12) . ?
C27C F276 1.408(8) . ?
C27C F272 1.412(8) . ?
C28C F281 1.320(7) . ?
C28C F283 1.322(7) . ?
C28C F282 1.348(8) . ?
C31C C36C 1.395(5) . ?
C31C C32C 1.403(6) . ?
C32C C33C 1.395(6) . ?
C32C H32C 0.9300 . ?
C33C C34C 1.381(6) . ?
C33C C37C 1.492(6) . ?
C34C C35C 1.375(6) . ?
C34C H34C 0.9300 . ?
C35C C36C 1.398(6) . ?
C35C C38C 1.500(6) . ?
C36C H36C 0.9300 . ?
C37C F372 1.328(6) . ?
C37C F373 1.336(6) . ?
C37C F371 1.339(7) . ?
C38C F382 1.295(6) . ?
C38C F383 1.310(6) . ?
C38C F381 1.324(6) . ?
C41C C46C 1.393(5) . ?
C41C C42C 1.401(6) . ?
C42C C43C 1.387(6) . ?
C42C H42C 0.9300 . ?
C43C C44C 1.388(6) . ?
C43C C47C 1.499(6) . ?
C44C C45C 1.384(6) . ?
C44C H44C 0.9300 . ?
C45C C46C 1.403(6) . ?
C45C C48C 1.481(6) . ?
C46C H46C 0.9300 . ?
C47C F473 1.327(5) . ?
C47C F472 1.329(5) . ?
C47C F471 1.348(6) . ?
C48C F485 1.307(8) . ?
C48C F488 1.320(7) . ?
C48C F484 1.320(7) . ?
C48C F481 1.326(6) . ?
C48C F487 1.333(9) . ?
C48C F489 1.348(8) . ?
C48C F483 1.352(6) . ?
C48C F486 1.365(8) . ?
C48C F482 1.426(6) . ?
C1D Cl1D 1.58(2) . ?
C1D Cl2D 1.62(2) . ?
C1E Cl3E 1.40(5) . ?
C1E Cl4E 1.47(5) . ?
C1E Cl2E 1.52(5) . ?
C1E Cl1E 1.88(4) . ?
Cl1E Cl3E 1.60(4) . ?
Cl1E Cl4E 2.10(3) . ?
Cl2E Cl3E 1.14(4) . ?
Cl4E Cl4E 1.44(5) 2 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2B Rh1 C1B 87.4(2) . . ?
C2B Rh1 N3' 94.54(16) . . ?
C1B Rh1 N3' 175.23(17) . . ?
C2B Rh1 N2 178.89(17) . . ?
C1B Rh1 N2 93.71(19) . . ?
N3' Rh1 N2 84.38(14) . . ?
C5 N1 N2 111.3(4) . . ?
C5 N1 C1A 129.2(4) . . ?
N2 N1 C1A 119.1(3) . . ?
C3 N2 N1 105.7(4) . . ?
C3 N2 Rh1 132.0(3) . . ?
N1 N2 Rh1 121.2(3) . . ?
N2 C3 C4 109.6(5) . . ?
N2 C3 C6 121.7(5) . . ?
C4 C3 C6 128.7(5) . . ?
C5 C4 C3 107.4(5) . . ?
C5 C4 H4A 126.3 . . ?
C3 C4 H4A 126.3 . . ?
N1 C5 C4 106.0(4) . . ?
N1 C5 C7 122.0(5) . . ?
C4 C5 C7 132.0(5) . . ?
C3 C6 H61 109.5 . . ?
C3 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
C3 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
C5 C7 H72 109.5 . . ?
C5 C7 H71 109.5 . . ?
H72 C7 H71 109.5 . . ?
C5 C7 H73 109.5 . . ?
H72 C7 H73 109.5 . . ?
H71 C7 H73 109.5 . . ?
N1 C1A C4' 108.7(3) . . ?
N1 C1A H2A 109.9 . . ?
C4' C1A H2A 109.9 . . ?
N1 C1A H1A 109.9 . . ?
C4' C1A H1A 109.9 . . ?
H2A C1A H1A 108.3 . . ?
N2' N1' C5' 111.6(3) . . ?
N2' N1' C6' 120.0(3) . . ?
C5' N1' C6' 128.0(3) . . ?
N3' N2' N1' 105.4(3) . . ?
N2' N3' C4' 110.9(3) . . ?
N2' N3' Rh1 128.4(3) . . ?
C4' N3' Rh1 120.6(3) . . ?
N3' C4' C5' 107.4(3) . . ?
N3' C4' C1A 120.0(4) . . ?
C5' C4' C1A 132.3(4) . . ?
N1' C5' C4' 104.7(3) . . ?
N1' C5' H5' 127.6 . . ?
C4' C5' H5' 127.6 . . ?
C7' C6' C11' 121.6(4) . . ?
C7' C6' N1' 119.1(4) . . ?
C11' C6' N1' 119.3(4) . . ?
C6' C7' C8' 119.4(4) . . ?
C6' C7' H7' 120.3 . . ?
C8' C7' H7' 120.3 . . ?
C9' C8' C7' 118.3(4) . . ?
C9' C8' H8' 120.9 . . ?
C7' C8' H8' 120.9 . . ?
C8' C9' C10' 122.6(4) . . ?
C8' C9' N4' 118.4(4) . . ?
C10' C9' N4' 119.0(4) . . ?
C9' C10' C11' 118.9(4) . . ?
C9' C10' H10' 120.6 . . ?
C11' C10' H10' 120.6 . . ?
C6' C11' C10' 119.1(4) . . ?
C6' C11' H11' 120.4 . . ?
C10' C11' H11' 120.4 . . ?
O1' N4' O2' 123.8(4) . . ?
O1' N4' C9' 117.9(4) . . ?
O2' N4' C9' 118.3(4) . . ?
O1B C1B Rh1 178.4(5) . . ?
O2B C2B Rh1 177.4(4) . . ?
C11C B1C C21C 110.1(3) . . ?
C11C B1C C41C 114.1(3) . . ?
C21C B1C C41C 105.8(3) . . ?
C11C B1C C31C 106.0(3) . . ?
C21C B1C C31C 110.4(3) . . ?
C41C B1C C31C 110.5(3) . . ?
C12C C11C C16C 115.5(4) . . ?
C12C C11C B1C 121.5(3) . . ?
C16C C11C B1C 122.9(3) . . ?
C13C C12C C11C 122.1(4) . . ?
C13C C12C H12C 118.9 . . ?
C11C C12C H12C 118.9 . . ?
C14C C13C C12C 121.2(4) . . ?
C14C C13C C17C 120.7(4) . . ?
C12C C13C C17C 118.1(4) . . ?
C13C C14C C15C 117.9(4) . . ?
C13C C14C H14C 121.0 . . ?
C15C C14C H14C 121.0 . . ?
C14C C15C C16C 120.8(4) . . ?
C14C C15C C18C 120.2(4) . . ?
C16C C15C C18C 119.0(4) . . ?
C15C C16C C11C 122.3(4) . . ?
C15C C16C H16C 118.9 . . ?
C11C C16C H16C 118.9 . . ?
F172 C17C F173 107.0(3) . . ?
F172 C17C F171 105.4(4) . . ?
F173 C17C F171 106.0(4) . . ?
F172 C17C C13C 112.7(3) . . ?
F173 C17C C13C 113.1(4) . . ?
F171 C17C C13C 112.0(3) . . ?
F181 C18C F183 108.8(5) . . ?
F181 C18C F182 103.5(5) . . ?
F183 C18C F182 103.8(5) . . ?
F181 C18C C15C 113.7(5) . . ?
F183 C18C C15C 113.2(4) . . ?
F182 C18C C15C 112.8(4) . . ?
C26C C21C C22C 115.8(4) . . ?
C26C C21C B1C 124.9(3) . . ?
C22C C21C B1C 119.2(3) . . ?
C23C C22C C21C 122.2(4) . . ?
C23C C22C H22C 118.9 . . ?
C21C C22C H22C 118.9 . . ?
C24C C23C C22C 120.2(4) . . ?
C24C C23C C27C 120.6(4) . . ?
C22C C23C C27C 119.2(4) . . ?
C25C C24C C23C 118.4(4) . . ?
C25C C24C H24C 120.8 . . ?
C23C C24C H24C 120.8 . . ?
C24C C25C C26C 121.1(4) . . ?
C24C C25C C28C 118.7(4) . . ?
C26C C25C C28C 120.2(4) . . ?
C25C C26C C21C 122.1(4) . . ?
C25C C26C H26C 118.9 . . ?
C21C C26C H26C 118.9 . . ?
F273 C27C F275 58.4(6) . . ?
F273 C27C F274 119.6(7) . . ?
F275 C27C F274 108.8(6) . . ?
F273 C27C F271 108.7(6) . . ?
F275 C27C F271 126.3(7) . . ?
F274 C27C F271 26.7(4) . . ?
F273 C27C F277 122.8(9) . . ?
F275 C27C F277 80.0(7) . . ?
F274 C27C F277 38.0(7) . . ?
F271 C27C F277 64.7(7) . . ?
F273 C27C F278 32.4(5) . . ?
F275 C27C F278 28.8(5) . . ?
F274 C27C F278 126.8(7) . . ?
F271 C27C F278 131.2(7) . . ?
F277 C27C F278 107.0(7) . . ?
F273 C27C F279 75.0(8) . . ?
F275 C27C F279 125.7(10) . . ?
F274 C27C F279 70.2(8) . . ?
F271 C27C F279 44.5(7) . . ?
F277 C27C F279 107.1(8) . . ?
F278 C27C F279 106.8(7) . . ?
F273 C27C F276 44.7(5) . . ?
F275 C27C F276 102.5(6) . . ?
F274 C27C F276 100.9(5) . . ?
F271 C27C F276 77.4(5) . . ?
F277 C27C F276 132.4(9) . . ?
F278 C27C F276 76.9(5) . . ?
F279 C27C F276 34.0(7) . . ?
F273 C27C F272 103.2(6) . . ?
F275 C27C F272 47.0(5) . . ?
F274 C27C F272 75.0(5) . . ?
F271 C27C F272 101.2(5) . . ?
F277 C27C F272 37.8(6) . . ?
F278 C27C F272 75.9(5) . . ?
F279 C27C F272 137.6(11) . . ?
F276 C27C F272 141.4(7) . . ?
F273 C27C C23C 119.0(6) . . ?
F275 C27C C23C 116.3(7) . . ?
F274 C27C C23C 118.5(5) . . ?
F271 C27C C23C 114.6(5) . . ?
F277 C27C C23C 113.7(8) . . ?
F278 C27C C23C 112.4(6) . . ?
F279 C27C C23C 109.5(11) . . ?
F276 C27C C23C 107.5(6) . . ?
F272 C27C C23C 108.0(6) . . ?
F281 C28C F283 108.9(5) . . ?
F281 C28C F282 104.6(4) . . ?
F283 C28C F282 103.7(5) . . ?
F281 C28C C25C 113.1(5) . . ?
F283 C28C C25C 113.9(4) . . ?
F282 C28C C25C 111.7(5) . . ?
C36C C31C C32C 115.4(4) . . ?
C36C C31C B1C 124.7(3) . . ?
C32C C31C B1C 119.8(3) . . ?
C33C C32C C31C 122.4(4) . . ?
C33C C32C H32C 118.8 . . ?
C31C C32C H32C 118.8 . . ?
C34C C33C C32C 120.9(4) . . ?
C34C C33C C37C 121.1(4) . . ?
C32C C33C C37C 118.0(4) . . ?
C35C C34C C33C 117.8(4) . . ?
C35C C34C H34C 121.1 . . ?
C33C C34C H34C 121.1 . . ?
C34C C35C C36C 121.6(4) . . ?
C34C C35C C38C 120.0(4) . . ?
C36C C35C C38C 118.3(4) . . ?
C31C C36C C35C 121.9(4) . . ?
C31C C36C H36C 119.1 . . ?
C35C C36C H36C 119.1 . . ?
F372 C37C F373 106.7(5) . . ?
F372 C37C F371 106.0(5) . . ?
F373 C37C F371 105.8(4) . . ?
F372 C37C C33C 111.7(4) . . ?
F373 C37C C33C 113.6(4) . . ?
F371 C37C C33C 112.6(4) . . ?
F382 C38C F383 109.6(6) . . ?
F382 C38C F381 104.7(5) . . ?
F383 C38C F381 102.8(4) . . ?
F382 C38C C35C 111.9(4) . . ?
F383 C38C C35C 113.3(4) . . ?
F381 C38C C35C 113.8(4) . . ?
C46C C41C C42C 115.2(4) . . ?
C46C C41C B1C 126.7(3) . . ?
C42C C41C B1C 118.2(3) . . ?
C43C C42C C41C 123.1(4) . . ?
C43C C42C H42C 118.5 . . ?
C41C C42C H42C 118.5 . . ?
C42C C43C C44C 120.4(4) . . ?
C42C C43C C47C 119.9(4) . . ?
C44C C43C C47C 119.7(4) . . ?
C45C C44C C43C 118.3(4) . . ?
C45C C44C H44C 120.8 . . ?
C43C C44C H44C 120.8 . . ?
C44C C45C C46C 120.4(4) . . ?
C44C C45C C48C 119.4(4) . . ?
C46C C45C C48C 120.2(4) . . ?
C41C C46C C45C 122.6(4) . . ?
C41C C46C H46C 118.7 . . ?
C45C C46C H46C 118.7 . . ?
F473 C47C F472 106.1(4) . . ?
F473 C47C F471 106.4(4) . . ?
F472 C47C F471 104.8(4) . . ?
F473 C47C C43C 113.6(4) . . ?
F472 C47C C43C 112.9(4) . . ?
F471 C47C C43C 112.3(4) . . ?
F485 C48C F488 37.5(4) . . ?
F485 C48C F484 108.2(5) . . ?
F488 C48C F484 130.3(6) . . ?
F485 C48C F481 123.0(6) . . ?
F488 C48C F481 124.7(5) . . ?
F484 C48C F481 29.2(4) . . ?
F485 C48C F487 72.0(6) . . ?
F488 C48C F487 106.7(6) . . ?
F484 C48C F487 42.7(5) . . ?
F481 C48C F487 70.7(5) . . ?
F485 C48C F489 128.5(7) . . ?
F488 C48C F489 105.7(5) . . ?
F484 C48C F489 64.5(5) . . ?
F481 C48C F489 35.3(4) . . ?
F487 C48C F489 104.6(6) . . ?
F485 C48C F483 65.5(5) . . ?
F488 C48C F483 28.7(4) . . ?
F484 C48C F483 129.1(6) . . ?
F481 C48C F483 108.8(5) . . ?
F487 C48C F483 127.6(7) . . ?
F489 C48C F483 80.7(5) . . ?
F485 C48C F486 106.0(5) . . ?
F488 C48C F486 70.9(5) . . ?
F484 C48C F486 105.2(5) . . ?
F481 C48C F486 76.7(5) . . ?
F487 C48C F486 137.5(8) . . ?
F489 C48C F486 42.3(5) . . ?
F483 C48C F486 42.4(4) . . ?
F485 C48C F482 37.2(4) . . ?
F488 C48C F482 74.4(4) . . ?
F484 C48C F482 77.8(4) . . ?
F481 C48C F482 102.7(4) . . ?
F487 C48C F482 36.5(5) . . ?
F489 C48C F482 130.2(6) . . ?
F483 C48C F482 101.2(4) . . ?
F486 C48C F482 136.0(6) . . ?
F485 C48C C45C 116.1(5) . . ?
F488 C48C C45C 115.1(5) . . ?
F484 C48C C45C 113.2(5) . . ?
F481 C48C C45C 116.8(4) . . ?
F487 C48C C45C 111.3(6) . . ?
F489 C48C C45C 112.8(6) . . ?
F483 C48C C45C 114.1(4) . . ?
F486 C48C C45C 107.4(6) . . ?
F482 C48C C45C 111.5(4) . . ?
Cl1D C1D Cl2D 124.9(15) . . ?
Cl3E C1E Cl4E 133(4) . . ?
Cl3E C1E Cl2E 46(2) . . ?
Cl4E C1E Cl2E 177(3) . . ?
Cl3E C1E Cl1E 56(2) . . ?
Cl4E C1E Cl1E 77(2) . . ?
Cl2E C1E Cl1E 102(2) . . ?
Cl3E Cl1E C1E 46.7(17) . . ?
Cl3E Cl1E Cl4E 89.7(16) . . ?
C1E Cl1E Cl4E 43.0(14) . . ?
Cl3E Cl2E C1E 62(3) . . ?
Cl2E Cl3E C1E 73(3) . . ?
Cl2E Cl3E Cl1E 150(3) . . ?
C1E Cl3E Cl1E 77(2) . . ?
Cl4E Cl4E C1E 112(2) 2 . ?
Cl4E Cl4E Cl1E 172.5(12) 2 . ?
C1E Cl4E Cl1E 60.5(19) . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 C3 -1.9(5) . . . . ?
C1A N1 N2 C3 -175.6(4) . . . . ?
C5 N1 N2 Rh1 167.7(3) . . . . ?
C1A N1 N2 Rh1 -6.0(5) . . . . ?
C2B Rh1 N2 C3 116(9) . . . . ?
C1B Rh1 N2 C3 -55.5(5) . . . . ?
N3' Rh1 N2 C3 128.9(5) . . . . ?
C2B Rh1 N2 N1 -51(9) . . . . ?
C1B Rh1 N2 N1 138.0(3) . . . . ?
N3' Rh1 N2 N1 -37.6(3) . . . . ?
N1 N2 C3 C4 1.3(6) . . . . ?
Rh1 N2 C3 C4 -166.7(4) . . . . ?
N1 N2 C3 C6 179.1(5) . . . . ?
Rh1 N2 C3 C6 11.0(8) . . . . ?
N2 C3 C4 C5 -0.3(7) . . . . ?
C6 C3 C4 C5 -177.8(6) . . . . ?
N2 N1 C5 C4 1.7(5) . . . . ?
C1A N1 C5 C4 174.6(4) . . . . ?
N2 N1 C5 C7 -177.4(4) . . . . ?
C1A N1 C5 C7 -4.6(7) . . . . ?
C3 C4 C5 N1 -0.9(6) . . . . ?
C3 C4 C5 C7 178.2(6) . . . . ?
C5 N1 C1A C4' -110.6(5) . . . . ?
N2 N1 C1A C4' 61.7(5) . . . . ?
C5' N1' N2' N3' -0.4(4) . . . . ?
C6' N1' N2' N3' -173.2(3) . . . . ?
N1' N2' N3' C4' 0.5(4) . . . . ?
N1' N2' N3' Rh1 175.7(3) . . . . ?
C2B Rh1 N3' N2' 45.7(4) . . . . ?
C1B Rh1 N3' N2' 159(2) . . . . ?
N2 Rh1 N3' N2' -134.0(3) . . . . ?
C2B Rh1 N3' C4' -139.5(3) . . . . ?
C1B Rh1 N3' C4' -26(2) . . . . ?
N2 Rh1 N3' C4' 40.8(3) . . . . ?
N2' N3' C4' C5' -0.4(5) . . . . ?
Rh1 N3' C4' C5' -176.0(3) . . . . ?
N2' N3' C4' C1A 174.5(3) . . . . ?
Rh1 N3' C4' C1A -1.2(5) . . . . ?
N1 C1A C4' N3' -58.0(5) . . . . ?
N1 C1A C4' C5' 115.3(5) . . . . ?
N2' N1' C5' C4' 0.2(4) . . . . ?
C6' N1' C5' C4' 172.3(4) . . . . ?
N3' C4' C5' N1' 0.1(4) . . . . ?
C1A C4' C5' N1' -173.8(4) . . . . ?
N2' N1' C6' C7' 165.2(4) . . . . ?
C5' N1' C6' C7' -6.3(6) . . . . ?
N2' N1' C6' C11' -13.8(6) . . . . ?
C5' N1' C6' C11' 174.7(4) . . . . ?
C11' C6' C7' C8' 3.4(7) . . . . ?
N1' C6' C7' C8' -175.6(4) . . . . ?
C6' C7' C8' C9' -0.1(7) . . . . ?
C7' C8' C9' C10' -2.7(7) . . . . ?
C7' C8' C9' N4' 175.6(4) . . . . ?
C8' C9' C10' C11' 2.2(8) . . . . ?
N4' C9' C10' C11' -176.1(5) . . . . ?
C7' C6' C11' C10' -3.9(8) . . . . ?
N1' C6' C11' C10' 175.1(5) . . . . ?
C9' C10' C11' C6' 1.1(8) . . . . ?
C8' C9' N4' O1' -168.4(4) . . . . ?
C10' C9' N4' O1' 10.0(6) . . . . ?
C8' C9' N4' O2' 10.8(6) . . . . ?
C10' C9' N4' O2' -170.8(5) . . . . ?
C2B Rh1 C1B O1B 37(17) . . . . ?
N3' Rh1 C1B O1B -77(18) . . . . ?
N2 Rh1 C1B O1B -143(17) . . . . ?
C1B Rh1 C2B O2B -8(10) . . . . ?
N3' Rh1 C2B O2B 168(10) . . . . ?
N2 Rh1 C2B O2B -179(100) . . . . ?
C21C B1C C11C C12C 162.3(3) . . . . ?
C41C B1C C11C C12C 43.5(5) . . . . ?
C31C B1C C11C C12C -78.3(4) . . . . ?
C21C B1C C11C C16C -21.5(5) . . . . ?
C41C B1C C11C C16C -140.3(4) . . . . ?
C31C B1C C11C C16C 97.9(4) . . . . ?
C16C C11C C12C C13C 4.6(6) . . . . ?
B1C C11C C12C C13C -179.0(4) . . . . ?
C11C C12C C13C C14C -3.4(6) . . . . ?
C11C C12C C13C C17C 176.0(4) . . . . ?
C12C C13C C14C C15C 0.3(6) . . . . ?
C17C C13C C14C C15C -179.2(4) . . . . ?
C13C C14C C15C C16C 1.4(7) . . . . ?
C13C C14C C15C C18C 179.7(4) . . . . ?
C14C C15C C16C C11C 0.0(7) . . . . ?
C18C C15C C16C C11C -178.3(4) . . . . ?
C12C C11C C16C C15C -2.9(6) . . . . ?
B1C C11C C16C C15C -179.3(4) . . . . ?
C14C C13C C17C F172 -108.2(5) . . . . ?
C12C C13C C17C F172 72.4(5) . . . . ?
C14C C13C C17C F173 13.4(6) . . . . ?
C12C C13C C17C F173 -166.1(4) . . . . ?
C14C C13C C17C F171 133.1(4) . . . . ?
C12C C13C C17C F171 -46.3(5) . . . . ?
C14C C15C C18C F181 -3.5(8) . . . . ?
C16C C15C C18C F181 174.8(6) . . . . ?
C14C C15C C18C F183 121.4(5) . . . . ?
C16C C15C C18C F183 -60.3(6) . . . . ?
C14C C15C C18C F182 -121.0(5) . . . . ?
C16C C15C C18C F182 57.3(7) . . . . ?
C11C B1C C21C C26C 130.7(4) . . . . ?
C41C B1C C21C C26C -105.6(4) . . . . ?
C31C B1C C21C C26C 14.0(5) . . . . ?
C11C B1C C21C C22C -50.3(5) . . . . ?
C41C B1C C21C C22C 73.5(4) . . . . ?
C31C B1C C21C C22C -167.0(3) . . . . ?
C26C C21C C22C C23C -2.0(6) . . . . ?
B1C C21C C22C C23C 178.8(4) . . . . ?
C21C C22C C23C C24C 1.1(7) . . . . ?
C21C C22C C23C C27C -178.5(4) . . . . ?
C22C C23C C24C C25C 0.1(7) . . . . ?
C27C C23C C24C C25C 179.7(5) . . . . ?
C23C C24C C25C C26C -0.2(7) . . . . ?
C23C C24C C25C C28C 179.5(5) . . . . ?
C24C C25C C26C C21C -0.8(7) . . . . ?
C28C C25C C26C C21C 179.5(5) . . . . ?
C22C C21C C26C C25C 1.9(6) . . . . ?
B1C C21C C26C C25C -179.1(4) . . . . ?
C24C C23C C27C F273 21.1(9) . . . . ?
C22C C23C C27C F273 -159.3(7) . . . . ?
C24C C23C C27C F275 -45.7(8) . . . . ?
C22C C23C C27C F275 134.0(7) . . . . ?
C24C C23C C27C F274 -178.2(6) . . . . ?
C22C C23C C27C F274 1.4(8) . . . . ?
C24C C23C C27C F271 152.2(6) . . . . ?
C22C C23C C27C F271 -28.2(8) . . . . ?
C24C C23C C27C F277 -136.0(9) . . . . ?
C22C C23C C27C F277 43.7(10) . . . . ?
C24C C23C C27C F278 -14.2(8) . . . . ?
C22C C23C C27C F278 165.4(6) . . . . ?
C24C C23C C27C F279 104.3(10) . . . . ?
C22C C23C C27C F279 -76.1(10) . . . . ?
C24C C23C C27C F276 68.4(7) . . . . ?
C22C C23C C27C F276 -111.9(6) . . . . ?
C24C C23C C27C F272 -95.9(7) . . . . ?
C22C C23C C27C F272 83.7(7) . . . . ?
C24C C25C C28C F281 44.9(7) . . . . ?
C26C C25C C28C F281 -135.4(5) . . . . ?
C24C C25C C28C F283 170.0(5) . . . . ?
C26C C25C C28C F283 -10.2(8) . . . . ?
C24C C25C C28C F282 -72.8(6) . . . . ?
C26C C25C C28C F282 106.9(5) . . . . ?
C11C B1C C31C C36C 110.0(4) . . . . ?
C21C B1C C31C C36C -130.8(4) . . . . ?
C41C B1C C31C C36C -14.1(5) . . . . ?
C11C B1C C31C C32C -69.0(4) . . . . ?
C21C B1C C31C C32C 50.2(5) . . . . ?
C41C B1C C31C C32C 166.9(3) . . . . ?
C36C C31C C32C C33C 2.9(6) . . . . ?
B1C C31C C32C C33C -178.1(4) . . . . ?
C31C C32C C33C C34C -2.1(6) . . . . ?
C31C C32C C33C C37C 176.0(4) . . . . ?
C32C C33C C34C C35C 0.0(6) . . . . ?
C37C C33C C34C C35C -178.1(4) . . . . ?
C33C C34C C35C C36C 1.1(6) . . . . ?
C33C C34C C35C C38C 177.2(4) . . . . ?
C32C C31C C36C C35C -1.8(5) . . . . ?
B1C C31C C36C C35C 179.2(4) . . . . ?
C34C C35C C36C C31C -0.2(6) . . . . ?
C38C C35C C36C C31C -176.4(4) . . . . ?
C34C C33C C37C F372 119.1(5) . . . . ?
C32C C33C C37C F372 -59.0(7) . . . . ?
C34C C33C C37C F373 -1.6(7) . . . . ?
C32C C33C C37C F373 -179.7(4) . . . . ?
C34C C33C C37C F371 -121.7(5) . . . . ?
C32C C33C C37C F371 60.1(6) . . . . ?
C34C C35C C38C F382 -96.9(6) . . . . ?
C36C C35C C38C F382 79.4(6) . . . . ?
C34C C35C C38C F383 138.6(5) . . . . ?
C36C C35C C38C F383 -45.1(6) . . . . ?
C34C C35C C38C F381 21.6(6) . . . . ?
C36C C35C C38C F381 -162.1(4) . . . . ?
C11C B1C C41C C46C 7.5(5) . . . . ?
C21C B1C C41C C46C -113.7(4) . . . . ?
C31C B1C C41C C46C 126.8(4) . . . . ?
C11C B1C C41C C42C -173.8(3) . . . . ?
C21C B1C C41C C42C 65.0(4) . . . . ?
C31C B1C C41C C42C -54.5(4) . . . . ?
C46C C41C C42C C43C -2.7(6) . . . . ?
B1C C41C C42C C43C 178.4(4) . . . . ?
C41C C42C C43C C44C 2.0(6) . . . . ?
C41C C42C C43C C47C -178.4(4) . . . . ?
C42C C43C C44C C45C -0.6(6) . . . . ?
C47C C43C C44C C45C 179.9(4) . . . . ?
C43C C44C C45C C46C 0.1(6) . . . . ?
C43C C44C C45C C48C -177.4(4) . . . . ?
C42C C41C C46C C45C 2.1(6) . . . . ?
B1C C41C C46C C45C -179.1(4) . . . . ?
C44C C45C C46C C41C -0.9(6) . . . . ?
C48C C45C C46C C41C 176.5(4) . . . . ?
C42C C43C C47C F473 158.2(4) . . . . ?
C44C C43C C47C F473 -22.2(6) . . . . ?
C42C C43C C47C F472 -80.8(5) . . . . ?
C44C C43C C47C F472 98.7(5) . . . . ?
C42C C43C C47C F471 37.4(6) . . . . ?
C44C C43C C47C F471 -143.0(4) . . . . ?
C44C C45C C48C F485 -179.8(6) . . . . ?
C46C C45C C48C F485 2.8(7) . . . . ?
C44C C45C C48C F488 -138.1(6) . . . . ?
C46C C45C C48C F488 44.5(7) . . . . ?
C44C C45C C48C F484 54.2(7) . . . . ?
C46C C45C C48C F484 -123.2(6) . . . . ?
C44C C45C C48C F481 22.1(7) . . . . ?
C46C C45C C48C F481 -155.3(5) . . . . ?
C44C C45C C48C F487 100.5(7) . . . . ?
C46C C45C C48C F487 -77.0(7) . . . . ?
C44C C45C C48C F489 -16.7(7) . . . . ?
C46C C45C C48C F489 165.9(6) . . . . ?
C44C C45C C48C F483 -106.4(6) . . . . ?
C46C C45C C48C F483 76.2(6) . . . . ?
C44C C45C C48C F486 -61.4(6) . . . . ?
C46C C45C C48C F486 121.1(6) . . . . ?
C44C C45C C48C F482 139.7(5) . . . . ?
C46C C45C C48C F482 -37.7(6) . . . . ?
Cl4E C1E Cl1E Cl3E 178(3) . . . . ?
Cl2E C1E Cl1E Cl3E 1(2) . . . . ?
Cl3E C1E Cl1E Cl4E -178(3) . . . . ?
Cl2E C1E Cl1E Cl4E -177(3) . . . . ?
Cl4E C1E Cl2E Cl3E -57(63) . . . . ?
Cl1E C1E Cl2E Cl3E -1(2) . . . . ?
C1E Cl2E Cl3E Cl1E 3(6) . . . . ?
Cl4E C1E Cl3E Cl2E 176(5) . . . . ?
Cl1E C1E Cl3E Cl2E 179(3) . . . . ?
Cl4E C1E Cl3E Cl1E -2(4) . . . . ?
Cl2E C1E Cl3E Cl1E -179(3) . . . . ?
C1E Cl1E Cl3E Cl2E -3(5) . . . . ?
Cl4E Cl1E Cl3E Cl2E -1(6) . . . . ?
Cl4E Cl1E Cl3E C1E 1(2) . . . . ?
Cl3E C1E Cl4E Cl4E -178(4) . . . 2 ?
Cl2E C1E Cl4E Cl4E -124(62) . . . 2 ?
Cl1E C1E Cl4E Cl4E -180(3) . . . 2 ?
Cl3E C1E Cl4E Cl1E 2(4) . . . . ?
Cl2E C1E Cl4E Cl1E 56(62) . . . . ?
Cl3E Cl1E Cl4E Cl4E 0(24) . . . 2 ?
C1E Cl1E Cl4E Cl4E 1(23) . . . 2 ?
Cl3E Cl1E Cl4E C1E -1(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.249
_refine_diff_density_min -0.990
_refine_diff_density_rms 0.106
_iucr_refine_instructions_details
;
TITL cHINMIN6_p1BAR in P-1 New: C2/c
CELL 0.71073 39.3960 18.3734 16.4800 90.000 106.912 90.000
ZERR 8 0.0040 0.0016 0.0016 0.000 0.005 0.000
LATT 7
SYMM - X , Y , 0.50000 - Z
SFAC C H B F N O Rh Cl
UNIT 390 208 8 192 48 32 8 12
OMIT 2 0 0
OMIT 0 0 2
OMIT 2 0 2
OMIT 4 2 1
OMIT -2 2 2
OMIT 4 2 0
OMIT -1 1 2
OMIT 0 2 2
OMIT -1 1 1
OMIT 1 1 3
OMIT 2 2 0
OMIT -3 50
L.S. 25
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.211 0.205 0.090
SADI 0.01 F487 F488 F488 F489 F489 F487
SADI 0.01 C48C F487 C48C F488 C48C F489
SADI 0.01 F484 F485 F485 F486 F486 F484
SADI 0.01 C48C F484 C48C F485 C48C F486
SADI 0.01 F481 F482 F482 F483 F483 F481
SADI 0.01 C48C F481 C48C F482 C48C F483
SADI 0.01 F277 F278 F278 F279 F279 F277
SADI 0.01 C27C F277 C27C F278 C27C F279
SADI 0.01 F274 F275 F275 F276 F276 F274
SADI 0.01 C27C F274 C27C F275 C27C F276
SADI 0.01 F271 F272 F272 F273 F273 F271
SADI 0.01 C27C F271 C27C F272 C27C F273
CONF
DELU 0.01 C27C F271 > F279
DELU 0.01 C48C F481 > F489
WGHT 0.154100 117.660500
FVAR 0.03855
MOLE 1
RH1 7 0.169920 0.110157 0.616792 11.00000 0.03963 0.02090 =
0.02834 -0.00009 0.00894 -0.00146
N1 5 0.119651 0.182675 0.700142 11.00000 0.04054 0.03232 =
0.03043 0.00096 0.01496 -0.00385
N2 5 0.124370 0.122730 0.655150 11.00000 0.04088 0.03291 =
0.03467 -0.00331 0.01107 -0.00700
C3 1 0.093014 0.088154 0.632673 11.00000 0.04513 0.05348 =
0.04914 -0.00827 0.01375 -0.01969
C4 1 0.068657 0.126989 0.661706 11.00000 0.04043 0.07320 =
0.05778 -0.00464 0.01610 -0.01802
AFIX 43
H4A 2 0.045053 0.114551 0.654105 11.00000 -1.20000
AFIX 0
C5 1 0.085813 0.187168 0.703728 11.00000 0.04338 0.05303 =
0.03976 0.00486 0.01827 -0.00125
C6 1 0.087418 0.019969 0.581029 11.00000 0.07637 0.07471 =
0.08617 -0.03802 0.02846 -0.04300
AFIX 137
H61 2 0.098237 0.025000 0.536117 11.00000 -1.50000
H62 2 0.062447 0.011423 0.557266 11.00000 -1.50000
H63 2 0.097974 -0.020319 0.616530 11.00000 -1.50000
AFIX 0
C7 1 0.073309 0.249068 0.745956 11.00000 0.06213 0.06194 =
0.06585 0.00061 0.03713 0.00583
AFIX 137
H72 2 0.086307 0.249784 0.805084 11.00000 -1.50000
H71 2 0.048474 0.243337 0.739918 11.00000 -1.50000
H73 2 0.077089 0.293967 0.720073 11.00000 -1.50000
AFIX 0
C1A 1 0.148531 0.234887 0.728484 11.00000 0.04057 0.03084 =
0.02322 0.00029 0.00625 -0.00327
AFIX 23
H2A 2 0.169451 0.210829 0.764380 11.00000 -1.20000
H1A 2 0.141764 0.273241 0.761146 11.00000 -1.20000
AFIX 0
N1' 5 0.161152 0.328328 0.545630 11.00000 0.03330 0.02255 =
0.02445 0.00164 0.00957 0.00120
N2' 5 0.168496 0.259005 0.530811 11.00000 0.03670 0.02160 =
0.02874 0.00170 0.01208 0.00266
N3' 5 0.165669 0.222016 0.596699 11.00000 0.03319 0.02385 =
0.02810 -0.00022 0.00785 -0.00013
C4' 1 0.156408 0.266352 0.652797 11.00000 0.03141 0.02601 =
0.02338 0.00045 0.00490 -0.00090
C5' 1 0.153463 0.335092 0.620476 11.00000 0.03606 0.02531 =
0.02585 -0.00279 0.01267 0.00001
AFIX 43
H5' 2 0.147509 0.377295 0.644357 11.00000 -1.20000
AFIX 0
C6' 1 0.158088 0.382323 0.481445 11.00000 0.03347 0.02546 =
0.02778 0.00249 0.01147 -0.00067
C7' 1 0.142749 0.448412 0.489404 11.00000 0.05144 0.02936 =
0.03079 0.00240 0.01719 0.00598
AFIX 43
H7' 2 0.136013 0.458817 0.537754 11.00000 -1.20000
AFIX 0
C8' 1 0.137460 0.499234 0.424611 11.00000 0.05027 0.02544 =
0.03877 0.00187 0.01767 0.00586
AFIX 43
H8' 2 0.127136 0.544102 0.428597 11.00000 -1.20000
AFIX 0
C9' 1 0.147878 0.481540 0.354382 11.00000 0.03394 0.03144 =
0.03467 0.00811 0.01057 -0.00383
C10' 1 0.164551 0.416948 0.347572 11.00000 0.07284 0.03898 =
0.03955 0.00891 0.03439 0.01003
AFIX 43
H10' 2 0.172009 0.407269 0.300059 11.00000 -1.20000
AFIX 0
C11' 1 0.170012 0.366786 0.412482 11.00000 0.06243 0.03331 =
0.04341 0.00786 0.02865 0.01302
AFIX 43
H11' 2 0.181568 0.323117 0.409769 11.00000 -1.20000
AFIX 0
N4' 5 0.139951 0.533117 0.282943 11.00000 0.04780 0.03573 =
0.03755 0.01050 0.01408 -0.00487
O1' 6 0.143999 0.512262 0.215895 11.00000 0.07436 0.05037 =
0.04104 0.01395 0.02895 0.00034
O2' 6 0.129326 0.593981 0.293710 11.00000 0.07143 0.03392 =
0.05417 0.01445 0.02006 0.00502
C1B 1 0.174523 0.011235 0.644490 11.00000 0.06057 0.03152 =
0.03868 -0.00267 0.01985 -0.00259
O1B 6 0.178119 -0.048322 0.661827 11.00000 0.10196 0.02374 =
0.07155 0.00593 0.03166 -0.00123
C2B 1 0.210408 0.100750 0.581710 11.00000 0.05157 0.02301 =
0.03509 -0.00173 0.01222 -0.00175
O2B 6 0.235413 0.092404 0.561382 11.00000 0.05445 0.04936 =
0.05743 -0.00812 0.02688 -0.00180
MOLE 2
B1C 3 0.139339 0.268335 0.070098 11.00000 0.02360 0.02854 =
0.02561 -0.00017 0.00899 0.00263
C11C 1 0.126798 0.200545 0.003213 11.00000 0.02805 0.02901 =
0.02363 0.00336 0.00821 0.00214
C12C 1 0.151394 0.158332 -0.022216 11.00000 0.02653 0.02758 =
0.02766 0.00204 0.00574 0.00338
AFIX 43
H12C 2 0.175430 0.168585 0.000129 11.00000 -1.20000
AFIX 0
C13C 1 0.141040 0.101207 -0.080142 11.00000 0.03457 0.02808 =
0.02654 0.00300 0.00819 0.00505
C14C 1 0.105937 0.081336 -0.111729 11.00000 0.03512 0.03074 =
0.03214 -0.00492 0.00438 -0.00015
AFIX 43
H14C 2 0.099144 0.043166 -0.150102 11.00000 -1.20000
AFIX 0
C15C 1 0.081040 0.120018 -0.084533 11.00000 0.02957 0.03638 =
0.03772 -0.00073 0.00519 -0.00139
C16C 1 0.091296 0.178280 -0.028316 11.00000 0.02675 0.03390 =
0.03487 -0.00149 0.00960 0.00308
AFIX 43
H16C 2 0.074012 0.203192 -0.011170 11.00000 -1.20000
AFIX 0
C17C 1 0.169251 0.062333 -0.107765 11.00000 0.04216 0.02794 =
0.03351 0.00163 0.01371 0.00654
C18C 1 0.042618 0.101000 -0.117092 11.00000 0.03442 0.05225 =
0.05541 -0.00745 0.00385 -0.00667
F171 4 0.191713 0.108784 -0.128337 11.00000 0.05119 0.03942 =
0.06233 0.00881 0.03411 0.00943
F172 4 0.189566 0.019789 -0.047014 11.00000 0.05329 0.04752 =
0.05336 0.01898 0.02412 0.02533
F173 4 0.156204 0.020299 -0.175989 11.00000 0.05887 0.06426 =
0.05353 -0.02800 0.02032 0.00340
F181 4 0.035798 0.049327 -0.174497 11.00000 0.04757 0.16812 =
0.19599 -0.13030 0.02207 -0.03740
F182 4 0.022841 0.156071 -0.156180 11.00000 0.03306 0.11073 =
0.11073 0.04532 -0.01511 -0.00619
F183 4 0.028507 0.083247 -0.056853 11.00000 0.03706 0.12749 =
0.08578 0.03630 0.00870 -0.01965
C21C 1 0.105574 0.322413 0.065004 11.00000 0.02641 0.02711 =
0.02779 0.00090 0.00907 0.00047
C22C 1 0.084929 0.347575 -0.014324 11.00000 0.03733 0.03440 =
0.03086 0.00434 0.01529 0.00604
AFIX 43
H22C 2 0.091043 0.333813 -0.062547 11.00000 -1.20000
AFIX 0
C23C 1 0.055562 0.392496 -0.023376 11.00000 0.03776 0.03943 =
0.04254 0.00798 0.01353 0.00966
C24C 1 0.046170 0.414918 0.047266 11.00000 0.03599 0.04023 =
0.04838 0.00411 0.01511 0.01404
AFIX 43
H24C 2 0.026598 0.444860 0.041808 11.00000 -1.20000
AFIX 0
C25C 1 0.066527 0.391803 0.125990 11.00000 0.03648 0.03818 =
0.03761 -0.00467 0.01423 0.00683
C26C 1 0.095645 0.347004 0.134620 11.00000 0.03131 0.03469 =
0.03153 -0.00211 0.00988 0.00475
AFIX 43
H26C 2 0.108984 0.332916 0.188698 11.00000 -1.20000
AFIX 0
C27C 1 0.034582 0.415355 -0.109175 11.00000 0.05676 0.08066 =
0.06025 0.02843 0.01874 0.03614
C28C 1 0.056699 0.416362 0.202721 11.00000 0.04927 0.07200 =
0.04739 -0.00812 0.01710 0.02560
PART 1
F271 4 0.052939 0.418813 -0.165811 10.40000 0.05757
F272 4 0.010133 0.359400 -0.144029 10.40000 0.08006
F273 4 0.014434 0.473326 -0.117552 10.40000 0.08168
PART 2
F274 4 0.044004 0.390952 -0.175099 10.40000 0.04616
F275 4 -0.000038 0.410317 -0.126253 10.40000 0.08681
F276 4 0.039717 0.490716 -0.115697 10.40000 0.07822
PART 3
F277 4 0.028209 0.361478 -0.166372 10.20000 0.06059
F278 4 0.002919 0.443623 -0.110237 10.20000 0.01527
F279 4 0.052210 0.467721 -0.137532 10.20000 0.09430
PART 0
F281 4 0.022346 0.411609 0.193629 11.00000 0.05120 0.12446 =
0.06945 -0.01568 0.03533 0.00956
F282 4 0.064545 0.487144 0.220029 11.00000 0.10208 0.08788 =
0.09872 -0.04910 0.04775 0.00050
F283 4 0.074223 0.382620 0.273338 11.00000 0.10463 0.15848 =
0.04247 0.00553 0.03166 0.07216
C31C 1 0.153713 0.231087 0.164958 11.00000 0.02715 0.02081 =
0.02795 -0.00350 0.00873 0.00290
C32C 1 0.129619 0.197123 0.200930 11.00000 0.02690 0.02977 =
0.03299 0.00251 0.00909 0.00041
AFIX 43
H32C 2 0.105827 0.194876 0.169643 11.00000 -1.20000
AFIX 0
C33C 1 0.140072 0.166605 0.281941 11.00000 0.04048 0.02963 =
0.03672 0.00356 0.01862 0.00107
C34C 1 0.175285 0.166542 0.329669 11.00000 0.04605 0.02936 =
0.02671 0.00291 0.01086 0.00549
AFIX 43
H34C 2 0.182352 0.146221 0.383676 11.00000 -1.20000
AFIX 0
C35C 1 0.199531 0.197524 0.294658 11.00000 0.03196 0.02794 =
0.02912 -0.00302 0.00589 0.00498
C36C 1 0.189142 0.229288 0.214097 11.00000 0.02833 0.02507 =
0.02976 -0.00146 0.00940 0.00157
AFIX 43
H36C 2 0.206331 0.249802 0.192646 11.00000 -1.20000
AFIX 0
C37C 1 0.111975 0.136174 0.316387 11.00000 0.04867 0.05258 =
0.05703 0.02375 0.02699 0.00582
C38C 1 0.237872 0.201956 0.345243 11.00000 0.03841 0.03819 =
0.04070 -0.00041 0.00030 0.00575
F371 4 0.093688 0.082271 0.268448 11.00000 0.05809 0.08954 =
0.06971 0.02887 0.00843 -0.02994
F372 4 0.088211 0.186262 0.320296 11.00000 0.09903 0.09620 =
0.15713 0.06018 0.10131 0.04320
F373 4 0.124564 0.108517 0.394376 11.00000 0.07451 0.08704 =
0.04796 0.02272 0.02666 -0.01259
F381 4 0.247170 0.154481 0.408316 11.00000 0.05549 0.12248 =
0.06450 0.04251 -0.00608 0.00353
F382 4 0.245820 0.264886 0.381163 11.00000 0.06621 0.06776 =
0.25241 -0.07378 -0.06578 0.01085
F383 4 0.259656 0.186756 0.300841 11.00000 0.03507 0.19205 =
0.05852 0.02017 0.01080 0.01683
C41C 1 0.170260 0.320272 0.051371 11.00000 0.02435 0.02761 =
0.02496 0.00165 0.00688 0.00330
C42C 1 0.185151 0.375121 0.109985 11.00000 0.03088 0.02766 =
0.03013 0.00081 0.01165 0.00489
AFIX 43
H42C 2 0.176675 0.381130 0.156663 11.00000 -1.20000
AFIX 0
C43C 1 0.211945 0.420881 0.101653 11.00000 0.02813 0.02819 =
0.03200 0.00036 0.00676 0.00255
C44C 1 0.224618 0.415328 0.031642 11.00000 0.02611 0.03794 =
0.03667 0.00553 0.00780 -0.00272
AFIX 43
H44C 2 0.242427 0.446119 0.025397 11.00000 -1.20000
AFIX 0
C45C 1 0.210080 0.362799 -0.028649 11.00000 0.02671 0.04070 =
0.02958 0.00468 0.00835 0.00069
C46C 1 0.183197 0.316648 -0.018697 11.00000 0.02574 0.03296 =
0.02406 0.00027 0.00602 0.00239
AFIX 43
H46C 2 0.173639 0.282280 -0.060537 11.00000 -1.20000
AFIX 0
C47C 1 0.227171 0.477067 0.168252 11.00000 0.03542 0.03501 =
0.04281 -0.00092 0.00791 -0.00248
C48C 1 0.224208 0.353603 -0.102048 11.00000 0.03223 0.06106 =
0.03691 0.00017 0.01422 -0.00674
F471 4 0.229843 0.452689 0.247002 11.00000 0.10645 0.06040 =
0.03396 -0.00526 0.00395 -0.02659
F472 4 0.207238 0.536574 0.159503 11.00000 0.04957 0.04429 =
0.07172 -0.01889 0.01423 0.00606
F473 4 0.259326 0.499460 0.169407 11.00000 0.03974 0.06457 =
0.08855 -0.03731 0.02116 -0.01731
PART 1
F481 4 0.256850 0.377674 -0.092839 10.40000 0.03636
F482 4 0.226632 0.278666 -0.122075 10.40000 0.04333
F483 4 0.202597 0.379205 -0.175998 10.45000 0.05614
PART 2
F484 4 0.258842 0.343089 -0.079829 10.30000 0.03603
F485 4 0.209189 0.303168 -0.156613 10.30000 0.04601
F486 4 0.218822 0.417577 -0.146048 10.30000 0.06222
PART 3
F487 4 0.246372 0.297215 -0.090869 10.30000 0.07611
F488 4 0.200019 0.343523 -0.175671 10.30000 0.03095
F489 4 0.243663 0.411022 -0.113289 10.35000 0.07326
PART 0
MOLE 3
C1D 1 0.946021 0.337667 0.018823 10.50000 0.11948
CL2D 8 0.924315 0.263290 0.021316 10.50000 0.07336 0.10948 =
0.10588 0.04536 -0.02356 -0.01592
CL1D 8 0.936280 0.394919 -0.055693 10.50000 0.07382 0.08054 =
0.10988 -0.00042 0.03979 -0.01532
MOLE 4
C1E 1 0.003200 0.162151 0.172919 10.25000 0.10280
CL1E 8 0.023144 0.219863 0.104526 10.12500 0.07386
CL2E 8 0.002170 0.087632 0.131887 10.12500 0.11977
CL3E 8 0.012770 0.135692 0.102920 10.12500 0.15937
CL4E 8 0.006316 0.234402 0.213162 10.12500 0.14538
HKLF 4 1 0.0000 -1.0000 -2.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 0.0000
REM cHINMIN6_p1BAR in P-1 New: C2/c
REM R1 = 0.0557 for 8611 Fo > 4sig(Fo) and 0.0645 for all 10039 data
REM 819 parameters refined using 36 restraints
END
WGHT 0.0906 66.6327
REM Highest difference peak 1.249, deepest hole -0.990, 1-sigma level 0.106
Q1 1 0.2560 0.2558 0.3141 11.00000 0.05 1.25
Q2 1 0.0261 0.2286 0.1441 11.00000 0.05 1.20
Q3 1 0.0132 0.3302 -0.1539 11.00000 0.05 1.19
Q4 1 0.0087 0.2278 0.0543 11.00000 0.05 1.15
Q5 1 0.9333 0.3019 -0.0118 11.00000 0.05 1.07
Q6 1 0.9453 0.3511 0.0456 11.00000 0.05 0.96
Q7 1 0.0531 0.5014 -0.1113 11.00000 0.05 0.95
Q8 1 0.9435 0.3534 -0.0278 11.00000 0.05 0.93
Q9 1 0.2302 0.4398 -0.1215 11.00000 0.05 0.89
Q10 1 0.2432 0.2172 0.4231 11.00000 0.05 0.85
Q11 1 0.0192 0.1776 0.1101 11.00000 0.05 0.81
Q12 1 -0.0071 0.4233 -0.0976 11.00000 0.05 0.79
Q13 1 0.2365 0.2620 -0.0954 11.00000 0.05 0.77
Q14 1 -0.0183 0.1787 0.0728 11.00000 0.05 0.74
Q15 1 0.9451 0.2524 0.0019 11.00000 0.05 0.74
Q16 1 -0.0156 0.0984 0.0989 11.00000 0.05 0.73
Q17 1 0.0417 0.0248 -0.1101 11.00000 0.05 0.71
Q18 1 0.9716 0.2631 0.0649 11.00000 0.05 0.67
Q19 1 0.0012 0.0941 0.1778 11.00000 0.05 0.66
Q20 1 0.2536 0.1506 0.3485 11.00000 0.05 0.65
;
#===END
data_carol4_p1bar
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'(C32 H12 B F23.97), (C23 H28 Cl Ir N5), 0.5(C H2 Cl2)'
_chemical_formula_sum
'C55.50 H41 B Cl2 F24 Ir N5'
_chemical_formula_weight 1507.84
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ir' 'Ir' -1.4442 7.9887
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Triclinic'
_symmetry_space_group_name_H-M 'P-1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.5013(14)
_cell_length_b 16.3750(8)
_cell_length_c 16.9370(8)
_cell_angle_alpha 117.541(2)
_cell_angle_beta 96.775(2)
_cell_angle_gamma 101.575(2)
_cell_volume 2921.7(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 151(2)
_cell_measurement_reflns_used 9611
_cell_measurement_theta_min 2.30
_cell_measurement_theta_max 30.47
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'Yellow'
_exptl_crystal_size_max 0.41
_exptl_crystal_size_mid 0.38
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.714
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1482
_exptl_absorpt_coefficient_mu 2.496
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.4255
_exptl_absorpt_correction_T_max 0.6850
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 151(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 37589
_diffrn_reflns_av_R_equivalents 0.0277
_diffrn_reflns_av_sigmaI/netI 0.0231
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -17
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.94
_diffrn_reflns_theta_max 25.00
_reflns_number_total 10113
_reflns_number_gt 9804
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
One of the CF3 groups showed orientational disorder, which is modelled over
three equally occupied sites. Restraints were applied on all C-F bond lengths
to be equal (SADI) and on temperatures factors (DELU and SIMU) to be within
reasonable limits. A solvent molecule of Dichloromethane was also located in
the difference Fourier map, which is disordered over two equally occupied
sites.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+2.9979P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10113
_refine_ls_number_parameters 876
_refine_ls_number_restraints 204
_refine_ls_R_factor_all 0.0195
_refine_ls_R_factor_gt 0.0186
_refine_ls_wR_factor_ref 0.0474
_refine_ls_wR_factor_gt 0.0467
_refine_ls_goodness_of_fit_ref 1.044
_refine_ls_restrained_S_all 1.045
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir -0.126123(6) 0.836259(5) 0.621563(5) 0.01527(4) Uani 1 1 d . . .
N1 N -0.06006(16) 1.05833(13) 0.74733(12) 0.0213(4) Uani 1 1 d . . .
N2 N -0.14438(15) 0.97399(13) 0.70525(13) 0.0203(4) Uani 1 1 d . . .
C3 C -0.2381(2) 0.99839(18) 0.72345(17) 0.0281(5) Uani 1 1 d . . .
H3 H -0.3110 0.9542 0.7022 0.034 Uiso 1 1 calc R . .
C4 C -0.2137(2) 1.09760(19) 0.77790(19) 0.0343(6) Uani 1 1 d . . .
H4 H -0.2650 1.1331 0.8010 0.041 Uiso 1 1 calc R . .
C5 C -0.1005(2) 1.13339(17) 0.79132(17) 0.0297(6) Uani 1 1 d . . .
H5 H -0.0579 1.1993 0.8255 0.036 Uiso 1 1 calc R . .
C1A C 0.05623(19) 1.05862(16) 0.74457(15) 0.0226(5) Uani 1 1 d . . .
H1A1 H 0.0827 1.0294 0.7800 0.027 Uiso 1 1 calc R . .
H2A1 H 0.1044 1.1259 0.7739 0.027 Uiso 1 1 calc R . .
N1' N 0.11140(15) 0.94332(13) 0.51805(13) 0.0198(4) Uani 1 1 d . . .
N2' N 0.02746(15) 0.87437(13) 0.51175(12) 0.0190(4) Uani 1 1 d . . .
N3' N 0.00091(15) 0.91195(12) 0.59139(12) 0.0172(4) Uani 1 1 d . . .
C4' C 0.06774(18) 1.00395(15) 0.64825(15) 0.0191(4) Uani 1 1 d . . .
C5' C 0.13885(19) 1.02445(16) 0.60048(16) 0.0229(5) Uani 1 1 d . . .
H6A H 0.1953 1.0830 0.6208 0.027 Uiso 1 1 calc R . .
C6' C 0.1683(2) 0.92089(16) 0.44204(16) 0.0229(5) Uani 1 1 d . . .
H16' H 0.1977 0.9800 0.4392 0.028 Uiso 1 1 calc R . .
H26' H 0.1131 0.8732 0.3832 0.028 Uiso 1 1 calc R . .
C7' C 0.26395(19) 0.88117(16) 0.45453(15) 0.0216(5) Uani 1 1 d . . .
C8' C 0.2499(2) 0.78321(18) 0.40772(18) 0.0297(5) Uani 1 1 d . . .
H8' H 0.1794 0.7404 0.3674 0.036 Uiso 1 1 calc R . .
C9' C 0.3378(2) 0.7470(2) 0.4192(2) 0.0365(6) Uani 1 1 d . . .
H9' H 0.3272 0.6795 0.3868 0.044 Uiso 1 1 calc R . .
C10' C 0.4402(2) 0.8082(2) 0.4773(2) 0.0373(6) Uani 1 1 d . . .
H10' H 0.5010 0.7833 0.4841 0.045 Uiso 1 1 calc R . .
C11' C 0.4545(2) 0.9060(2) 0.52569(19) 0.0379(6) Uani 1 1 d . . .
H11' H 0.5248 0.9483 0.5669 0.046 Uiso 1 1 calc R . .
C12' C 0.3672(2) 0.94270(19) 0.51463(17) 0.0315(6) Uani 1 1 d . . .
H12' H 0.3776 1.0101 0.5481 0.038 Uiso 1 1 calc R . .
C1B C -0.23017(19) 0.70722(16) 0.61123(17) 0.0249(5) Uani 1 1 d . . .
C2B C -0.1752(2) 0.77337(17) 0.70437(17) 0.0253(5) Uani 1 1 d . . .
C3B C -0.0546(2) 0.79362(16) 0.71369(16) 0.0238(5) Uani 1 1 d . . .
C4B C -0.03816(19) 0.73601(16) 0.62355(16) 0.0222(5) Uani 1 1 d . . .
C5B C -0.1451(2) 0.68519(15) 0.56000(16) 0.0232(5) Uani 1 1 d . . .
C6B C -0.3554(2) 0.6645(2) 0.5714(2) 0.0450(7) Uani 1 1 d . . .
H6B1 H -0.3789 0.6004 0.5648 0.068 Uiso 1 1 calc R . .
H6B2 H -0.3741 0.6592 0.5111 0.068 Uiso 1 1 calc R . .
H6B3 H -0.3945 0.7060 0.6124 0.068 Uiso 1 1 calc R . .
C7B C -0.2313(3) 0.8158(2) 0.7813(2) 0.0451(7) Uani 1 1 d . . .
H7B1 H -0.3033 0.8213 0.7576 0.068 Uiso 1 1 calc R . .
H7B2 H -0.1827 0.8798 0.8284 0.068 Uiso 1 1 calc R . .
H7B3 H -0.2447 0.7741 0.8081 0.068 Uiso 1 1 calc R . .
C8B C 0.0349(3) 0.8522(2) 0.80103(19) 0.0402(7) Uani 1 1 d . . .
H8B1 H 0.0094 0.9038 0.8457 0.060 Uiso 1 1 calc R . .
H8B2 H 0.1037 0.8803 0.7891 0.060 Uiso 1 1 calc R . .
H8B3 H 0.0502 0.8109 0.8257 0.060 Uiso 1 1 calc R . .
C9B C 0.0736(2) 0.7323(2) 0.6014(2) 0.0385(7) Uani 1 1 d . . .
H9B1 H 0.0977 0.6835 0.6109 0.058 Uiso 1 1 calc R . .
H9B2 H 0.1291 0.7953 0.6415 0.058 Uiso 1 1 calc R . .
H9B3 H 0.0673 0.7157 0.5372 0.058 Uiso 1 1 calc R . .
C10B C -0.1661(3) 0.61482(19) 0.45957(18) 0.0416(7) Uani 1 1 d . . .
H10B H -0.1016 0.6317 0.4367 0.062 Uiso 1 1 calc R . .
H10C H -0.2340 0.6170 0.4261 0.062 Uiso 1 1 calc R . .
H10D H -0.1765 0.5498 0.4503 0.062 Uiso 1 1 calc R . .
Cl1A Cl -0.25467(5) 0.82954(4) 0.50036(4) 0.02473(12) Uani 1 1 d . . .
B1C B 0.7525(2) 0.32304(17) 0.10332(17) 0.0170(5) Uani 1 1 d . . .
C11C C 0.71695(18) 0.30314(15) -0.00160(15) 0.0173(4) Uani 1 1 d . . .
C12C C 0.61218(18) 0.24412(15) -0.06211(15) 0.0199(5) Uani 1 1 d . . .
H12C H 0.5617 0.2070 -0.0450 0.024 Uiso 1 1 calc R . .
C13C C 0.57967(19) 0.23817(16) -0.14674(16) 0.0225(5) Uani 1 1 d . . .
C14C C 0.6499(2) 0.29181(16) -0.17417(16) 0.0239(5) Uani 1 1 d . . .
H14C H 0.6275 0.2881 -0.2316 0.029 Uiso 1 1 calc R . .
C15C C 0.75391(19) 0.35110(16) -0.11503(15) 0.0214(5) Uani 1 1 d . . .
C16C C 0.78668(19) 0.35575(15) -0.03154(15) 0.0198(5) Uani 1 1 d . . .
H16C H 0.8591 0.3961 0.0068 0.024 Uiso 1 1 calc R . .
C17C C 0.4695(2) 0.1693(2) -0.21001(18) 0.0360(6) Uani 1 1 d . . .
C18C C 0.8351(2) 0.41056(19) -0.14012(18) 0.0329(6) Uani 1 1 d . . .
F1C F 0.38706(15) 0.16671(18) -0.16769(13) 0.0750(7) Uani 1 1 d . . .
F2C F 0.47480(19) 0.07865(13) -0.25224(15) 0.0776(7) Uani 1 1 d . . .
F3C F 0.43327(15) 0.18597(14) -0.27654(12) 0.0572(5) Uani 1 1 d . . .
F4C F 0.78819(15) 0.41914(13) -0.20912(12) 0.0495(4) Uani 1 1 d . . .
F5C F 0.91720(17) 0.37086(18) -0.16817(19) 0.0780(7) Uani 1 1 d . . .
F6C F 0.88610(19) 0.49793(13) -0.07101(12) 0.0695(6) Uani 1 1 d . . .
C21C C 0.88859(18) 0.34302(14) 0.13610(15) 0.0176(4) Uani 1 1 d . . .
C22C C 0.95071(18) 0.29522(16) 0.07544(15) 0.0194(4) Uani 1 1 d . . .
H22C H 0.9137 0.2522 0.0126 0.023 Uiso 1 1 calc R . .
C23C C 1.06515(19) 0.30875(16) 0.10426(16) 0.0211(5) Uani 1 1 d . . .
C24C C 1.12259(19) 0.37073(16) 0.19513(16) 0.0220(5) Uani 1 1 d . . .
H24C H 1.2009 0.3809 0.2147 0.026 Uiso 1 1 calc R . .
C25C C 1.06215(19) 0.41747(16) 0.25661(16) 0.0212(5) Uani 1 1 d . . .
C26C C 0.94785(18) 0.40354(15) 0.22765(15) 0.0194(4) Uani 1 1 d . . .
H26C H 0.9088 0.4363 0.2716 0.023 Uiso 1 1 calc R . .
C27C C 1.1244(2) 0.2554(2) 0.03362(18) 0.0307(6) Uani 1 1 d . . .
C28C C 1.1188(2) 0.48825(17) 0.35512(17) 0.0266(5) Uani 1 1 d . . .
F7C F 1.07628(15) 0.15992(12) -0.01055(13) 0.0550(5) Uani 1 1 d . . .
F8C F 1.12112(15) 0.27881(15) -0.03226(11) 0.0517(5) Uani 1 1 d . . .
F9C F 1.23213(13) 0.26980(13) 0.06798(11) 0.0453(4) Uani 1 1 d . . .
F10C F 1.22485(13) 0.48905(13) 0.37872(11) 0.0500(4) Uani 1 1 d . . .
F11C F 1.12112(14) 0.57845(10) 0.37667(10) 0.0393(4) Uani 1 1 d . . .
F12C F 1.06508(13) 0.47177(11) 0.41286(10) 0.0379(4) Uani 1 1 d . . .
C31C C 0.71560(18) 0.42023(15) 0.16404(14) 0.0176(4) Uani 1 1 d . . .
C32C C 0.78324(18) 0.51019(15) 0.18465(14) 0.0188(4) Uani 1 1 d . . .
H32C H 0.8535 0.5143 0.1684 0.023 Uiso 1 1 calc R . .
C33C C 0.75122(19) 0.59344(15) 0.22796(15) 0.0205(5) Uani 1 1 d . . .
C34C C 0.6512(2) 0.59204(16) 0.25498(16) 0.0238(5) Uani 1 1 d . . .
H34C H 0.6301 0.6494 0.2857 0.029 Uiso 1 1 calc R . .
C35C C 0.58245(19) 0.50371(17) 0.23559(16) 0.0230(5) Uani 1 1 d . A .
C36C C 0.61321(18) 0.41981(16) 0.18957(15) 0.0203(5) Uani 1 1 d . . .
H36C H 0.5629 0.3602 0.1750 0.024 Uiso 1 1 calc R . .
C37C C 0.8282(2) 0.68537(17) 0.24497(17) 0.0299(6) Uani 1 1 d . . .
C38C C 0.4746(2) 0.50003(19) 0.2658(2) 0.0378(6) Uani 1 1 d DU . .
F13C F 0.86558(15) 0.67763(11) 0.17211(11) 0.0462(4) Uani 1 1 d . . .
F14C F 0.92068(17) 0.71777(14) 0.31041(14) 0.0723(7) Uani 1 1 d . . .
F15C F 0.78038(19) 0.75617(12) 0.26894(18) 0.0757(7) Uani 1 1 d . . .
F16A F 0.4163(15) 0.4116(9) 0.2445(13) 0.039(4) Uani 0.33 1 d PDU A 1
F17A F 0.4898(15) 0.5526(15) 0.3554(7) 0.069(6) Uani 0.33 1 d PDU A 1
F18A F 0.4026(12) 0.5295(13) 0.2276(13) 0.062(4) Uani 0.33 1 d PDU A 1
F16B F 0.3947(10) 0.4234(11) 0.2099(10) 0.077(5) Uani 0.33 1 d PDU A 2
F17B F 0.4930(10) 0.4945(17) 0.3446(10) 0.075(3) Uani 0.33 1 d PDU A 2
F18B F 0.4445(14) 0.5774(11) 0.2902(19) 0.087(5) Uani 0.33 1 d PDU A 2
F16C F 0.438(2) 0.4294(12) 0.2799(15) 0.061(6) Uani 0.33 1 d PU A 3
F17C F 0.4765(18) 0.5801(12) 0.3379(14) 0.071(7) Uani 0.33 1 d PU A 3
F18C F 0.3870(14) 0.4856(15) 0.1966(11) 0.066(4) Uani 0.33 1 d PU A 3
C41C C 0.69816(17) 0.23147(15) 0.11592(15) 0.0175(4) Uani 1 1 d . . .
C42C C 0.67213(18) 0.24237(16) 0.19791(15) 0.0200(5) Uani 1 1 d . . .
H42C H 0.6772 0.3049 0.2456 0.024 Uiso 1 1 calc R . .
C43C C 0.63916(19) 0.16450(17) 0.21148(16) 0.0236(5) Uani 1 1 d . . .
C44C C 0.63337(19) 0.07223(17) 0.14464(17) 0.0253(5) Uani 1 1 d . . .
H44C H 0.6113 0.0191 0.1541 0.030 Uiso 1 1 calc R . .
C45C C 0.66071(19) 0.05998(16) 0.06377(17) 0.0233(5) Uani 1 1 d . . .
C46C C 0.69150(18) 0.13768(16) 0.04964(15) 0.0197(4) Uani 1 1 d . . .
H46C H 0.7086 0.1267 -0.0070 0.024 Uiso 1 1 calc R . .
C47C C 0.6091(2) 0.1782(2) 0.29875(18) 0.0329(6) Uani 1 1 d . . .
C48C C 0.6650(2) -0.03677(18) -0.00662(19) 0.0325(6) Uani 1 1 d . . .
F19C F 0.6395(2) 0.26912(14) 0.36502(13) 0.0740(7) Uani 1 1 d . . .
F20C F 0.65981(15) 0.13359(15) 0.33394(12) 0.0530(5) Uani 1 1 d . . .
F21C F 0.49985(14) 0.14114(18) 0.28710(13) 0.0677(6) Uani 1 1 d . . .
F22C F 0.5970(2) -0.10905(12) -0.00470(16) 0.0727(7) Uani 1 1 d . . .
F23C F 0.76789(15) -0.04570(13) 0.00173(14) 0.0634(6) Uani 1 1 d . . .
F24C F 0.63370(16) -0.05425(12) -0.09262(11) 0.0520(5) Uani 1 1 d . . .
C1D C 0.4681(9) 0.5320(8) 0.0114(5) 0.070(2) Uani 0.50 1 d PDU . .
H1D H 0.410(4) 0.553(4) -0.023(3) 0.060 Uiso 0.50 1 d PD . .
H2D H 0.443(5) 0.543(5) 0.074(3) 0.060 Uiso 0.50 1 d PD . .
Cl1D Cl 0.6049(3) 0.5573(5) -0.0008(3) 0.1397(18) Uani 0.50 1 d PU . .
Cl2D Cl 0.5765(4) 0.5978(2) 0.0275(2) 0.1006(13) Uani 0.50 1 d PU . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.01552(5) 0.01487(5) 0.01955(5) 0.01104(4) 0.00574(3) 0.00561(3)
N1 0.0276(10) 0.0168(9) 0.0192(9) 0.0076(8) 0.0086(8) 0.0074(8)
N2 0.0217(10) 0.0180(9) 0.0253(10) 0.0125(8) 0.0095(8) 0.0075(8)
C3 0.0276(13) 0.0317(13) 0.0356(14) 0.0204(12) 0.0152(11) 0.0163(11)
C4 0.0431(16) 0.0336(14) 0.0394(15) 0.0198(12) 0.0229(12) 0.0260(12)
C5 0.0451(15) 0.0211(12) 0.0269(13) 0.0110(10) 0.0165(11) 0.0161(11)
C1A 0.0241(12) 0.0191(11) 0.0210(11) 0.0084(10) 0.0056(9) 0.0032(9)
N1' 0.0230(10) 0.0169(9) 0.0233(10) 0.0119(8) 0.0100(8) 0.0058(8)
N2' 0.0209(9) 0.0176(9) 0.0199(9) 0.0099(8) 0.0077(8) 0.0055(8)
N3' 0.0193(9) 0.0154(9) 0.0195(9) 0.0098(8) 0.0062(7) 0.0065(7)
C4' 0.0192(11) 0.0144(10) 0.0225(11) 0.0085(9) 0.0053(9) 0.0042(9)
C5' 0.0247(12) 0.0143(10) 0.0260(12) 0.0077(10) 0.0088(10) 0.0028(9)
C6' 0.0307(13) 0.0221(11) 0.0240(12) 0.0151(10) 0.0149(10) 0.0098(10)
C7' 0.0239(12) 0.0257(12) 0.0219(11) 0.0156(10) 0.0127(9) 0.0068(9)
C8' 0.0253(13) 0.0257(12) 0.0350(14) 0.0125(11) 0.0091(11) 0.0068(10)
C9' 0.0365(15) 0.0322(14) 0.0478(16) 0.0206(13) 0.0183(13) 0.0176(12)
C10' 0.0298(14) 0.0576(18) 0.0467(16) 0.0375(15) 0.0201(12) 0.0220(13)
C11' 0.0229(13) 0.0542(18) 0.0378(15) 0.0290(14) 0.0027(11) 0.0009(12)
C12' 0.0326(14) 0.0283(13) 0.0300(13) 0.0145(11) 0.0079(11) 0.0019(11)
C1B 0.0219(12) 0.0225(11) 0.0402(14) 0.0239(11) 0.0075(10) 0.0051(9)
C2B 0.0326(13) 0.0264(12) 0.0345(13) 0.0246(11) 0.0168(11) 0.0153(10)
C3B 0.0288(12) 0.0213(11) 0.0282(12) 0.0175(10) 0.0057(10) 0.0090(10)
C4B 0.0263(12) 0.0200(11) 0.0327(13) 0.0200(10) 0.0108(10) 0.0124(9)
C5B 0.0305(13) 0.0139(10) 0.0268(12) 0.0118(10) 0.0041(10) 0.0074(9)
C6B 0.0238(14) 0.0407(16) 0.077(2) 0.0409(17) 0.0025(14) -0.0005(12)
C7B 0.064(2) 0.0586(19) 0.0490(18) 0.0416(16) 0.0388(16) 0.0386(16)
C8B 0.0499(17) 0.0348(15) 0.0322(14) 0.0206(13) -0.0093(12) 0.0063(13)
C9B 0.0302(14) 0.0440(16) 0.0626(19) 0.0365(15) 0.0216(13) 0.0227(12)
C10B 0.069(2) 0.0229(13) 0.0296(14) 0.0109(12) 0.0046(13) 0.0168(13)
Cl1A 0.0225(3) 0.0257(3) 0.0293(3) 0.0185(2) 0.0002(2) 0.0049(2)
B1C 0.0181(12) 0.0162(11) 0.0193(12) 0.0100(10) 0.0065(10) 0.0062(10)
C11C 0.0211(11) 0.0140(10) 0.0214(11) 0.0100(9) 0.0083(9) 0.0093(9)
C12C 0.0217(11) 0.0170(10) 0.0243(11) 0.0117(9) 0.0081(9) 0.0075(9)
C13C 0.0253(12) 0.0186(11) 0.0244(12) 0.0110(10) 0.0048(9) 0.0079(9)
C14C 0.0337(13) 0.0226(11) 0.0209(11) 0.0129(10) 0.0080(10) 0.0133(10)
C15C 0.0276(12) 0.0190(11) 0.0250(12) 0.0140(10) 0.0111(10) 0.0109(9)
C16C 0.0215(11) 0.0173(10) 0.0231(11) 0.0109(9) 0.0066(9) 0.0080(9)
C17C 0.0361(15) 0.0355(15) 0.0325(14) 0.0196(12) -0.0015(12) 0.0018(12)
C18C 0.0371(15) 0.0358(14) 0.0367(15) 0.0266(13) 0.0107(12) 0.0098(12)
F1C 0.0315(10) 0.1137(18) 0.0521(12) 0.0384(12) -0.0040(8) -0.0189(10)
F2C 0.0797(15) 0.0276(9) 0.0766(14) 0.0059(10) -0.0309(12) -0.0026(9)
F3C 0.0473(10) 0.0662(12) 0.0523(11) 0.0414(10) -0.0189(8) -0.0072(9)
F4C 0.0569(11) 0.0591(11) 0.0484(10) 0.0456(9) 0.0078(8) 0.0039(9)
F5C 0.0602(13) 0.1097(18) 0.141(2) 0.1037(18) 0.0694(14) 0.0497(13)
F6C 0.0963(16) 0.0448(11) 0.0443(10) 0.0257(9) 0.0061(10) -0.0283(10)
C21C 0.0196(11) 0.0159(10) 0.0249(11) 0.0147(9) 0.0085(9) 0.0070(9)
C22C 0.0227(11) 0.0202(11) 0.0224(11) 0.0148(10) 0.0080(9) 0.0084(9)
C23C 0.0229(11) 0.0241(11) 0.0291(12) 0.0200(10) 0.0123(10) 0.0122(9)
C24C 0.0179(11) 0.0236(11) 0.0325(13) 0.0197(10) 0.0074(9) 0.0069(9)
C25C 0.0248(12) 0.0176(11) 0.0263(12) 0.0148(10) 0.0061(9) 0.0063(9)
C26C 0.0225(11) 0.0188(11) 0.0229(11) 0.0131(9) 0.0091(9) 0.0093(9)
C27C 0.0272(13) 0.0425(15) 0.0343(14) 0.0235(13) 0.0144(11) 0.0189(11)
C28C 0.0263(13) 0.0220(12) 0.0311(13) 0.0138(11) 0.0032(10) 0.0071(10)
F7C 0.0536(11) 0.0374(9) 0.0665(12) 0.0116(9) 0.0313(9) 0.0249(8)
F8C 0.0603(11) 0.0875(13) 0.0439(10) 0.0467(10) 0.0345(9) 0.0467(10)
F9C 0.0287(8) 0.0752(12) 0.0433(9) 0.0301(9) 0.0187(7) 0.0309(8)
F10C 0.0297(8) 0.0542(10) 0.0425(9) 0.0086(8) -0.0086(7) 0.0144(8)
F11C 0.0556(10) 0.0180(7) 0.0365(8) 0.0116(6) 0.0034(7) 0.0046(7)
F12C 0.0512(9) 0.0349(8) 0.0250(7) 0.0172(7) 0.0041(7) 0.0044(7)
C31C 0.0192(11) 0.0179(10) 0.0168(10) 0.0096(9) 0.0032(8) 0.0062(9)
C32C 0.0192(11) 0.0200(11) 0.0192(11) 0.0110(9) 0.0053(9) 0.0065(9)
C33C 0.0253(12) 0.0175(11) 0.0182(11) 0.0093(9) 0.0034(9) 0.0056(9)
C34C 0.0284(12) 0.0192(11) 0.0239(12) 0.0086(10) 0.0068(10) 0.0125(10)
C35C 0.0187(11) 0.0250(12) 0.0248(12) 0.0106(10) 0.0054(9) 0.0099(9)
C36C 0.0165(11) 0.0190(11) 0.0246(12) 0.0112(10) 0.0034(9) 0.0041(9)
C37C 0.0382(14) 0.0178(11) 0.0296(13) 0.0092(10) 0.0113(11) 0.0052(10)
C38C 0.0270(14) 0.0327(14) 0.0502(17) 0.0145(13) 0.0167(12) 0.0133(12)
F13C 0.0652(11) 0.0308(8) 0.0428(9) 0.0211(7) 0.0235(8) 0.0016(8)
F14C 0.0677(13) 0.0574(12) 0.0574(12) 0.0326(10) -0.0266(10) -0.0368(10)
F15C 0.0869(15) 0.0223(8) 0.132(2) 0.0362(11) 0.0684(15) 0.0261(9)
F16A 0.016(6) 0.034(4) 0.055(11) 0.013(6) 0.014(7) 0.005(3)
F17A 0.041(7) 0.073(12) 0.041(4) -0.012(7) 0.024(4) 0.004(10)
F18A 0.025(8) 0.073(10) 0.117(13) 0.062(9) 0.021(8) 0.030(9)
F16B 0.017(5) 0.082(8) 0.065(7) -0.008(5) 0.011(5) -0.004(5)
F17B 0.050(5) 0.127(11) 0.059(6) 0.050(7) 0.036(5) 0.024(8)
F18B 0.040(10) 0.064(7) 0.178(18) 0.058(9) 0.059(10) 0.042(7)
F16C 0.062(15) 0.067(10) 0.100(17) 0.060(11) 0.063(11) 0.038(9)
F17C 0.036(9) 0.048(7) 0.093(11) -0.001(7) 0.036(8) 0.021(5)
F18C 0.021(4) 0.098(12) 0.093(8) 0.058(9) 0.011(5) 0.016(8)
C41C 0.0143(10) 0.0199(11) 0.0225(11) 0.0128(9) 0.0055(8) 0.0070(8)
C42C 0.0202(11) 0.0207(11) 0.0222(11) 0.0119(10) 0.0068(9) 0.0078(9)
C43C 0.0208(11) 0.0301(12) 0.0286(12) 0.0200(11) 0.0093(10) 0.0094(10)
C44C 0.0237(12) 0.0244(12) 0.0387(14) 0.0234(11) 0.0110(10) 0.0071(10)
C45C 0.0193(11) 0.0203(11) 0.0330(13) 0.0144(10) 0.0078(10) 0.0072(9)
C46C 0.0195(11) 0.0211(11) 0.0222(11) 0.0125(10) 0.0079(9) 0.0076(9)
C47C 0.0360(14) 0.0398(15) 0.0371(15) 0.0284(13) 0.0174(12) 0.0116(12)
C48C 0.0317(14) 0.0230(12) 0.0432(16) 0.0159(12) 0.0120(12) 0.0090(11)
F19C 0.139(2) 0.0482(11) 0.0412(10) 0.0228(9) 0.0513(12) 0.0226(12)
F20C 0.0535(11) 0.0852(13) 0.0523(11) 0.0551(11) 0.0217(9) 0.0266(10)
F21C 0.0295(9) 0.137(2) 0.0575(12) 0.0649(13) 0.0222(8) 0.0184(11)
F22C 0.1034(17) 0.0199(8) 0.0901(15) 0.0214(9) 0.0510(13) 0.0080(9)
F23C 0.0474(11) 0.0454(10) 0.0704(13) 0.0028(9) 0.0004(9) 0.0337(9)
F24C 0.0688(12) 0.0365(9) 0.0363(9) 0.0045(8) 0.0075(8) 0.0243(9)
C1D 0.080(5) 0.095(6) 0.056(4) 0.036(4) 0.021(4) 0.070(4)
Cl1D 0.077(2) 0.212(6) 0.106(3) 0.067(4) 0.0165(19) 0.028(3)
Cl2D 0.139(4) 0.0742(17) 0.079(2) 0.0292(15) 0.0038(19) 0.0490(18)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N3' 2.0753(18) . ?
Ir1 N2 2.1153(18) . ?
Ir1 C5B 2.141(2) . ?
Ir1 C3B 2.157(2) . ?
Ir1 C4B 2.162(2) . ?
Ir1 C1B 2.165(2) . ?
Ir1 C2B 2.166(2) . ?
Ir1 Cl1A 2.3981(6) . ?
N1 C5 1.346(3) . ?
N1 N2 1.362(3) . ?
N1 C1A 1.459(3) . ?
N2 C3 1.336(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.497(3) . ?
C1A H1A1 0.9900 . ?
C1A H2A1 0.9900 . ?
N1' N2' 1.332(3) . ?
N1' C5' 1.349(3) . ?
N1' C6' 1.477(3) . ?
N2' N3' 1.315(2) . ?
N3' C4' 1.363(3) . ?
C4' C5' 1.363(3) . ?
C5' H6A 0.9500 . ?
C6' C7' 1.509(3) . ?
C6' H16' 0.9900 . ?
C6' H26' 0.9900 . ?
C7' C8' 1.382(3) . ?
C7' C12' 1.392(3) . ?
C8' C9' 1.383(4) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.375(4) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.380(4) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.381(4) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
C1B C2B 1.414(4) . ?
C1B C5B 1.448(3) . ?
C1B C6B 1.506(3) . ?
C2B C3B 1.451(3) . ?
C2B C7B 1.498(3) . ?
C3B C4B 1.443(3) . ?
C3B C8B 1.492(3) . ?
C4B C5B 1.423(3) . ?
C4B C9B 1.494(3) . ?
C5B C10B 1.500(3) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
C10B H10D 0.9800 . ?
B1C C41C 1.636(3) . ?
B1C C11C 1.638(3) . ?
B1C C21C 1.642(3) . ?
B1C C31C 1.642(3) . ?
C11C C12C 1.400(3) . ?
C11C C16C 1.402(3) . ?
C12C C13C 1.395(3) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.387(3) . ?
C13C C17C 1.493(3) . ?
C14C C15C 1.387(3) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.387(3) . ?
C15C C18C 1.499(3) . ?
C16C H16C 0.9500 . ?
C17C F1C 1.327(3) . ?
C17C F3C 1.328(3) . ?
C17C F2C 1.338(3) . ?
C18C F6C 1.316(3) . ?
C18C F4C 1.324(3) . ?
C18C F5C 1.342(3) . ?
C21C C26C 1.396(3) . ?
C21C C22C 1.400(3) . ?
C22C C23C 1.394(3) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.385(3) . ?
C23C C27C 1.498(3) . ?
C24C C25C 1.386(3) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.391(3) . ?
C25C C28C 1.494(3) . ?
C26C H26C 0.9500 . ?
C27C F9C 1.330(3) . ?
C27C F8C 1.335(3) . ?
C27C F7C 1.342(3) . ?
C28C F10C 1.335(3) . ?
C28C F11C 1.341(3) . ?
C28C F12C 1.344(3) . ?
C31C C36C 1.398(3) . ?
C31C C32C 1.401(3) . ?
C32C C33C 1.386(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.380(3) . ?
C33C C37C 1.492(3) . ?
C34C C35C 1.391(3) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.391(3) . ?
C35C C38C 1.497(3) . ?
C36C H36C 0.9500 . ?
C37C F14C 1.325(3) . ?
C37C F15C 1.329(3) . ?
C37C F13C 1.332(3) . ?
C38C F16B 1.283(9) . ?
C38C F18B 1.290(10) . ?
C38C F16C 1.293(15) . ?
C38C F17C 1.308(15) . ?
C38C F17A 1.319(11) . ?
C38C F18A 1.336(10) . ?
C38C F16A 1.337(12) . ?
C38C F17B 1.375(8) . ?
C38C F18C 1.402(14) . ?
C41C C46C 1.399(3) . ?
C41C C42C 1.402(3) . ?
C42C C43C 1.390(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.387(3) . ?
C43C C47C 1.495(3) . ?
C44C C45C 1.385(3) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.390(3) . ?
C45C C48C 1.495(3) . ?
C46C H46C 0.9500 . ?
C47C F19C 1.322(3) . ?
C47C F21C 1.328(3) . ?
C47C F20C 1.338(3) . ?
C48C F23C 1.322(3) . ?
C48C F22C 1.327(3) . ?
C48C F24C 1.339(3) . ?
C1D C1D 1.385(13) 2_665 ?
C1D Cl2D 1.459(12) . ?
C1D Cl1D 1.478(12) 2_665 ?
C1D Cl1D 1.738(11) . ?
C1D Cl2D 1.846(12) 2_665 ?
C1D H1D 1.089(2) . ?
C1D H2D 1.089(2) . ?
Cl1D Cl2D 0.798(5) . ?
Cl1D C1D 1.478(12) 2_665 ?
Cl2D C1D 1.846(12) 2_665 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3' Ir1 N2 83.62(7) . . ?
N3' Ir1 C5B 114.87(8) . . ?
N2 Ir1 C5B 161.26(8) . . ?
N3' Ir1 C3B 110.13(8) . . ?
N2 Ir1 C3B 106.30(8) . . ?
C5B Ir1 C3B 65.69(9) . . ?
N3' Ir1 C4B 95.16(8) . . ?
N2 Ir1 C4B 142.36(8) . . ?
C5B Ir1 C4B 38.62(9) . . ?
C3B Ir1 C4B 39.05(9) . . ?
N3' Ir1 C1B 154.12(8) . . ?
N2 Ir1 C1B 122.26(8) . . ?
C5B Ir1 C1B 39.29(9) . . ?
C3B Ir1 C1B 65.16(9) . . ?
C4B Ir1 C1B 64.73(9) . . ?
N3' Ir1 C2B 148.56(8) . . ?
N2 Ir1 C2B 97.67(8) . . ?
C5B Ir1 C2B 65.15(9) . . ?
C3B Ir1 C2B 39.22(9) . . ?
C4B Ir1 C2B 64.86(9) . . ?
C1B Ir1 C2B 38.11(9) . . ?
N3' Ir1 Cl1A 87.31(5) . . ?
N2 Ir1 Cl1A 85.96(5) . . ?
C5B Ir1 Cl1A 97.45(6) . . ?
C3B Ir1 Cl1A 159.37(6) . . ?
C4B Ir1 Cl1A 131.65(7) . . ?
C1B Ir1 Cl1A 94.32(7) . . ?
C2B Ir1 Cl1A 124.13(7) . . ?
C5 N1 N2 110.60(19) . . ?
C5 N1 C1A 128.7(2) . . ?
N2 N1 C1A 120.67(17) . . ?
C3 N2 N1 105.67(18) . . ?
C3 N2 Ir1 128.89(16) . . ?
N1 N2 Ir1 125.32(14) . . ?
N2 C3 C4 110.4(2) . . ?
N2 C3 H3 124.8 . . ?
C4 C3 H3 124.8 . . ?
C5 C4 C3 105.7(2) . . ?
C5 C4 H4 127.2 . . ?
C3 C4 H4 127.2 . . ?
N1 C5 C4 107.6(2) . . ?
N1 C5 H5 126.2 . . ?
C4 C5 H5 126.2 . . ?
N1 C1A C4' 111.69(18) . . ?
N1 C1A H1A1 109.3 . . ?
C4' C1A H1A1 109.3 . . ?
N1 C1A H2A1 109.3 . . ?
C4' C1A H2A1 109.3 . . ?
H1A1 C1A H2A1 107.9 . . ?
N2' N1' C5' 112.23(18) . . ?
N2' N1' C6' 118.90(17) . . ?
C5' N1' C6' 128.58(19) . . ?
N3' N2' N1' 105.27(16) . . ?
N2' N3' C4' 110.83(17) . . ?
N2' N3' Ir1 122.54(13) . . ?
C4' N3' Ir1 126.63(14) . . ?
N3' C4' C5' 106.80(19) . . ?
N3' C4' C1A 119.79(19) . . ?
C5' C4' C1A 133.3(2) . . ?
N1' C5' C4' 104.87(19) . . ?
N1' C5' H6A 127.6 . . ?
C4' C5' H6A 127.6 . . ?
N1' C6' C7' 111.33(18) . . ?
N1' C6' H16' 109.4 . . ?
C7' C6' H16' 109.4 . . ?
N1' C6' H26' 109.4 . . ?
C7' C6' H26' 109.4 . . ?
H16' C6' H26' 108.0 . . ?
C8' C7' C12' 119.0(2) . . ?
C8' C7' C6' 120.6(2) . . ?
C12' C7' C6' 120.4(2) . . ?
C7' C8' C9' 120.5(2) . . ?
C7' C8' H8' 119.7 . . ?
C9' C8' H8' 119.7 . . ?
C10' C9' C8' 120.3(3) . . ?
C10' C9' H9' 119.9 . . ?
C8' C9' H9' 119.9 . . ?
C9' C10' C11' 119.7(2) . . ?
C9' C10' H10' 120.2 . . ?
C11' C10' H10' 120.2 . . ?
C10' C11' C12' 120.4(2) . . ?
C10' C11' H11' 119.8 . . ?
C12' C11' H11' 119.8 . . ?
C11' C12' C7' 120.1(2) . . ?
C11' C12' H12' 119.9 . . ?
C7' C12' H12' 119.9 . . ?
C2B C1B C5B 108.2(2) . . ?
C2B C1B C6B 126.5(2) . . ?
C5B C1B C6B 125.3(2) . . ?
C2B C1B Ir1 70.95(13) . . ?
C5B C1B Ir1 69.45(12) . . ?
C6B C1B Ir1 126.40(17) . . ?
C1B C2B C3B 108.7(2) . . ?
C1B C2B C7B 126.1(2) . . ?
C3B C2B C7B 125.3(2) . . ?
C1B C2B Ir1 70.94(13) . . ?
C3B C2B Ir1 70.06(12) . . ?
C7B C2B Ir1 125.00(17) . . ?
C4B C3B C2B 106.6(2) . . ?
C4B C3B C8B 126.2(2) . . ?
C2B C3B C8B 126.7(2) . . ?
C4B C3B Ir1 70.66(13) . . ?
C2B C3B Ir1 70.73(13) . . ?
C8B C3B Ir1 129.52(17) . . ?
C5B C4B C3B 108.8(2) . . ?
C5B C4B C9B 126.1(2) . . ?
C3B C4B C9B 125.1(2) . . ?
C5B C4B Ir1 69.91(12) . . ?
C3B C4B Ir1 70.29(12) . . ?
C9B C4B Ir1 125.07(16) . . ?
C4B C5B C1B 107.6(2) . . ?
C4B C5B C10B 126.1(2) . . ?
C1B C5B C10B 126.1(2) . . ?
C4B C5B Ir1 71.47(12) . . ?
C1B C5B Ir1 71.26(12) . . ?
C10B C5B Ir1 126.71(17) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C5B C10B H10D 109.5 . . ?
H10B C10B H10D 109.5 . . ?
H10C C10B H10D 109.5 . . ?
C41C B1C C11C 114.19(18) . . ?
C41C B1C C21C 103.28(17) . . ?
C11C B1C C21C 111.16(17) . . ?
C41C B1C C31C 114.77(17) . . ?
C11C B1C C31C 103.10(17) . . ?
C21C B1C C31C 110.55(17) . . ?
C12C C11C C16C 115.7(2) . . ?
C12C C11C B1C 123.63(19) . . ?
C16C C11C B1C 120.18(19) . . ?
C13C C12C C11C 122.0(2) . . ?
C13C C12C H12C 119.0 . . ?
C11C C12C H12C 119.0 . . ?
C14C C13C C12C 121.1(2) . . ?
C14C C13C C17C 119.9(2) . . ?
C12C C13C C17C 118.9(2) . . ?
C13C C14C C15C 117.8(2) . . ?
C13C C14C H14C 121.1 . . ?
C15C C14C H14C 121.1 . . ?
C14C C15C C16C 120.9(2) . . ?
C14C C15C C18C 121.1(2) . . ?
C16C C15C C18C 118.0(2) . . ?
C15C C16C C11C 122.5(2) . . ?
C15C C16C H16C 118.8 . . ?
C11C C16C H16C 118.8 . . ?
F1C C17C F3C 106.9(2) . . ?
F1C C17C F2C 104.3(2) . . ?
F3C C17C F2C 105.7(2) . . ?
F1C C17C C13C 113.6(2) . . ?
F3C C17C C13C 113.9(2) . . ?
F2C C17C C13C 111.7(2) . . ?
F6C C18C F4C 107.5(2) . . ?
F6C C18C F5C 105.8(2) . . ?
F4C C18C F5C 104.8(2) . . ?
F6C C18C C15C 113.1(2) . . ?
F4C C18C C15C 113.4(2) . . ?
F5C C18C C15C 111.5(2) . . ?
C26C C21C C22C 115.8(2) . . ?
C26C C21C B1C 121.87(18) . . ?
C22C C21C B1C 122.13(19) . . ?
C23C C22C C21C 122.1(2) . . ?
C23C C22C H22C 118.9 . . ?
C21C C22C H22C 118.9 . . ?
C24C C23C C22C 121.0(2) . . ?
C24C C23C C27C 121.1(2) . . ?
C22C C23C C27C 118.0(2) . . ?
C23C C24C C25C 117.8(2) . . ?
C23C C24C H24C 121.1 . . ?
C25C C24C H24C 121.1 . . ?
C24C C25C C26C 121.0(2) . . ?
C24C C25C C28C 121.1(2) . . ?
C26C C25C C28C 117.8(2) . . ?
C25C C26C C21C 122.2(2) . . ?
C25C C26C H26C 118.9 . . ?
C21C C26C H26C 118.9 . . ?
F9C C27C F8C 106.9(2) . . ?
F9C C27C F7C 106.3(2) . . ?
F8C C27C F7C 105.0(2) . . ?
F9C C27C C23C 113.7(2) . . ?
F8C C27C C23C 112.3(2) . . ?
F7C C27C C23C 112.1(2) . . ?
F10C C28C F11C 106.97(19) . . ?
F10C C28C F12C 106.4(2) . . ?
F11C C28C F12C 104.73(19) . . ?
F10C C28C C25C 113.4(2) . . ?
F11C C28C C25C 112.1(2) . . ?
F12C C28C C25C 112.64(19) . . ?
C36C C31C C32C 115.58(19) . . ?
C36C C31C B1C 124.37(19) . . ?
C32C C31C B1C 119.68(19) . . ?
C33C C32C C31C 122.3(2) . . ?
C33C C32C H32C 118.9 . . ?
C31C C32C H32C 118.9 . . ?
C34C C33C C32C 121.3(2) . . ?
C34C C33C C37C 120.6(2) . . ?
C32C C33C C37C 118.1(2) . . ?
C33C C34C C35C 117.7(2) . . ?
C33C C34C H34C 121.2 . . ?
C35C C34C H34C 121.2 . . ?
C34C C35C C36C 120.9(2) . . ?
C34C C35C C38C 119.0(2) . . ?
C36C C35C C38C 120.1(2) . . ?
C35C C36C C31C 122.2(2) . . ?
C35C C36C H36C 118.9 . . ?
C31C C36C H36C 118.9 . . ?
F14C C37C F15C 106.6(2) . . ?
F14C C37C F13C 104.4(2) . . ?
F15C C37C F13C 105.6(2) . . ?
F14C C37C C33C 113.0(2) . . ?
F15C C37C C33C 113.2(2) . . ?
F13C C37C C33C 113.32(19) . . ?
F16B C38C F18B 112.9(9) . . ?
F16B C38C F16C 55.3(9) . . ?
F18B C38C F16C 129.2(12) . . ?
F16B C38C F17C 132.2(11) . . ?
F18B C38C F17C 37.5(8) . . ?
F16C C38C F17C 108.5(13) . . ?
F16B C38C F17A 127.4(10) . . ?
F18B C38C F17A 66.8(10) . . ?
F16C C38C F17A 83.4(11) . . ?
F17C C38C F17A 29.9(10) . . ?
F16B C38C F18A 75.3(8) . . ?
F18B C38C F18A 43.5(8) . . ?
F16C C38C F18A 120.5(11) . . ?
F17C C38C F18A 79.8(9) . . ?
F17A C38C F18A 106.6(9) . . ?
F16B C38C F16A 32.5(7) . . ?
F18B C38C F16A 130.7(11) . . ?
F16C C38C F16A 23.5(9) . . ?
F17C C38C F16A 125.5(12) . . ?
F17A C38C F16A 104.9(10) . . ?
F18A C38C F16A 104.4(9) . . ?
F16B C38C F17B 103.8(8) . . ?
F18B C38C F17B 104.1(9) . . ?
F16C C38C F17B 49.5(8) . . ?
F17C C38C F17B 68.4(9) . . ?
F17A C38C F17B 38.6(7) . . ?
F18A C38C F17B 135.7(9) . . ?
F16A C38C F17B 73.0(7) . . ?
F16B C38C F18C 51.0(8) . . ?
F18B C38C F18C 69.8(9) . . ?
F16C C38C F18C 103.3(10) . . ?
F17C C38C F18C 104.9(9) . . ?
F17A C38C F18C 127.9(10) . . ?
F18A C38C F18C 26.6(7) . . ?
F16A C38C F18C 82.7(9) . . ?
F17B C38C F18C 141.2(9) . . ?
F16B C38C C35C 113.6(6) . . ?
F18B C38C C35C 113.9(7) . . ?
F16C C38C C35C 115.5(11) . . ?
F17C C38C C35C 113.6(10) . . ?
F17A C38C C35C 113.0(8) . . ?
F18A C38C C35C 113.4(8) . . ?
F16A C38C C35C 113.7(9) . . ?
F17B C38C C35C 107.4(5) . . ?
F18C C38C C35C 110.0(8) . . ?
C46C C41C C42C 115.8(2) . . ?
C46C C41C B1C 120.76(19) . . ?
C42C C41C B1C 122.74(19) . . ?
C43C C42C C41C 122.0(2) . . ?
C43C C42C H42C 119.0 . . ?
C41C C42C H42C 119.0 . . ?
C44C C43C C42C 121.0(2) . . ?
C44C C43C C47C 118.3(2) . . ?
C42C C43C C47C 120.7(2) . . ?
C45C C44C C43C 118.0(2) . . ?
C45C C44C H44C 121.0 . . ?
C43C C44C H44C 121.0 . . ?
C44C C45C C46C 120.9(2) . . ?
C44C C45C C48C 119.6(2) . . ?
C46C C45C C48C 119.4(2) . . ?
C45C C46C C41C 122.3(2) . . ?
C45C C46C H46C 118.9 . . ?
C41C C46C H46C 118.9 . . ?
F19C C47C F21C 108.2(2) . . ?
F19C C47C F20C 104.8(2) . . ?
F21C C47C F20C 104.7(2) . . ?
F19C C47C C43C 113.7(2) . . ?
F21C C47C C43C 112.7(2) . . ?
F20C C47C C43C 112.0(2) . . ?
F23C C48C F22C 108.1(2) . . ?
F23C C48C F24C 105.0(2) . . ?
F22C C48C F24C 104.9(2) . . ?
F23C C48C C45C 112.1(2) . . ?
F22C C48C C45C 113.3(2) . . ?
F24C C48C C45C 112.9(2) . . ?
C1D C1D Cl2D 80.9(9) 2_665 . ?
C1D C1D Cl1D 74.6(9) 2_665 2_665 ?
Cl2D C1D Cl1D 153.8(6) . 2_665 ?
C1D C1D Cl1D 55.1(7) 2_665 . ?
Cl2D C1D Cl1D 27.2(3) . . ?
Cl1D C1D Cl1D 129.8(5) 2_665 . ?
C1D C1D Cl2D 51.3(8) 2_665 2_665 ?
Cl2D C1D Cl2D 132.2(4) . 2_665 ?
Cl1D C1D Cl2D 24.8(2) 2_665 2_665 ?
Cl1D C1D Cl2D 105.9(4) . 2_665 ?
C1D C1D H1D 138(3) 2_665 . ?
Cl2D C1D H1D 103(3) . . ?
Cl1D C1D H1D 102(3) 2_665 . ?
Cl1D C1D H1D 115(3) . . ?
Cl2D C1D H1D 113(3) 2_665 . ?
C1D C1D H2D 110(3) 2_665 . ?
Cl2D C1D H2D 113(4) . . ?
Cl1D C1D H2D 68(4) 2_665 . ?
Cl1D C1D H2D 126(3) . . ?
Cl2D C1D H2D 87(4) 2_665 . ?
H1D C1D H2D 106.7(3) . . ?
Cl2D Cl1D C1D 104.3(7) . 2_665 ?
Cl2D Cl1D C1D 56.6(6) . . ?
C1D Cl1D C1D 50.2(5) 2_665 . ?
Cl1D Cl2D C1D 96.2(7) . . ?
Cl1D Cl2D C1D 50.9(6) . 2_665 ?
C1D Cl2D C1D 47.8(4) . 2_665 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 C3 0.5(3) . . . . ?
C1A N1 N2 C3 177.7(2) . . . . ?
C5 N1 N2 Ir1 176.62(16) . . . . ?
C1A N1 N2 Ir1 -6.2(3) . . . . ?
N3' Ir1 N2 C3 145.2(2) . . . . ?
C5B Ir1 N2 C3 -43.8(4) . . . . ?
C3B Ir1 N2 C3 -105.6(2) . . . . ?
C4B Ir1 N2 C3 -124.6(2) . . . . ?
C1B Ir1 N2 C3 -35.1(2) . . . . ?
C2B Ir1 N2 C3 -66.4(2) . . . . ?
Cl1A Ir1 N2 C3 57.5(2) . . . . ?
N3' Ir1 N2 N1 -29.96(17) . . . . ?
C5B Ir1 N2 N1 141.0(2) . . . . ?
C3B Ir1 N2 N1 79.19(18) . . . . ?
C4B Ir1 N2 N1 60.2(2) . . . . ?
C1B Ir1 N2 N1 149.74(16) . . . . ?
C2B Ir1 N2 N1 118.37(18) . . . . ?
Cl1A Ir1 N2 N1 -117.70(17) . . . . ?
N1 N2 C3 C4 -0.8(3) . . . . ?
Ir1 N2 C3 C4 -176.78(17) . . . . ?
N2 C3 C4 C5 0.9(3) . . . . ?
N2 N1 C5 C4 0.0(3) . . . . ?
C1A N1 C5 C4 -176.9(2) . . . . ?
C3 C4 C5 N1 -0.5(3) . . . . ?
C5 N1 C1A C4' -129.2(2) . . . . ?
N2 N1 C1A C4' 54.1(3) . . . . ?
C5' N1' N2' N3' -0.1(2) . . . . ?
C6' N1' N2' N3' 174.34(18) . . . . ?
N1' N2' N3' C4' -0.3(2) . . . . ?
N1' N2' N3' Ir1 -179.91(13) . . . . ?
N2 Ir1 N3' N2' -149.24(17) . . . . ?
C5B Ir1 N3' N2' 33.96(19) . . . . ?
C3B Ir1 N3' N2' 105.70(17) . . . . ?
C4B Ir1 N3' N2' 68.58(17) . . . . ?
C1B Ir1 N3' N2' 31.3(3) . . . . ?
C2B Ir1 N3' N2' 116.49(19) . . . . ?
Cl1A Ir1 N3' N2' -63.01(16) . . . . ?
N2 Ir1 N3' C4' 31.23(18) . . . . ?
C5B Ir1 N3' C4' -145.57(18) . . . . ?
C3B Ir1 N3' C4' -73.83(19) . . . . ?
C4B Ir1 N3' C4' -110.95(19) . . . . ?
C1B Ir1 N3' C4' -148.2(2) . . . . ?
C2B Ir1 N3' C4' -63.0(2) . . . . ?
Cl1A Ir1 N3' C4' 117.46(18) . . . . ?
N2' N3' C4' C5' 0.6(3) . . . . ?
Ir1 N3' C4' C5' -179.85(15) . . . . ?
N2' N3' C4' C1A -176.63(19) . . . . ?
Ir1 N3' C4' C1A 3.0(3) . . . . ?
N1 C1A C4' N3' -52.7(3) . . . . ?
N1 C1A C4' C5' 131.0(3) . . . . ?
N2' N1' C5' C4' 0.4(3) . . . . ?
C6' N1' C5' C4' -173.3(2) . . . . ?
N3' C4' C5' N1' -0.6(3) . . . . ?
C1A C4' C5' N1' 176.1(2) . . . . ?
N2' N1' C6' C7' -87.8(2) . . . . ?
C5' N1' C6' C7' 85.6(3) . . . . ?
N1' C6' C7' C8' 99.6(2) . . . . ?
N1' C6' C7' C12' -79.3(3) . . . . ?
C12' C7' C8' C9' -1.1(4) . . . . ?
C6' C7' C8' C9' 179.9(2) . . . . ?
C7' C8' C9' C10' -0.1(4) . . . . ?
C8' C9' C10' C11' 1.3(4) . . . . ?
C9' C10' C11' C12' -1.3(4) . . . . ?
C10' C11' C12' C7' 0.1(4) . . . . ?
C8' C7' C12' C11' 1.2(4) . . . . ?
C6' C7' C12' C11' -179.9(2) . . . . ?
N3' Ir1 C1B C2B 122.62(19) . . . . ?
N2 Ir1 C1B C2B -56.70(16) . . . . ?
C5B Ir1 C1B C2B 118.87(19) . . . . ?
C3B Ir1 C1B C2B 37.53(14) . . . . ?
C4B Ir1 C1B C2B 80.83(15) . . . . ?
Cl1A Ir1 C1B C2B -144.64(13) . . . . ?
N3' Ir1 C1B C5B 3.7(3) . . . . ?
N2 Ir1 C1B C5B -175.57(12) . . . . ?
C3B Ir1 C1B C5B -81.35(14) . . . . ?
C4B Ir1 C1B C5B -38.05(13) . . . . ?
C2B Ir1 C1B C5B -118.87(19) . . . . ?
Cl1A Ir1 C1B C5B 96.49(13) . . . . ?
N3' Ir1 C1B C6B -115.6(3) . . . . ?
N2 Ir1 C1B C6B 65.1(3) . . . . ?
C5B Ir1 C1B C6B -119.3(3) . . . . ?
C3B Ir1 C1B C6B 159.3(3) . . . . ?
C4B Ir1 C1B C6B -157.4(3) . . . . ?
C2B Ir1 C1B C6B 121.8(3) . . . . ?
Cl1A Ir1 C1B C6B -22.8(2) . . . . ?
C5B C1B C2B C3B -0.5(2) . . . . ?
C6B C1B C2B C3B 178.1(2) . . . . ?
Ir1 C1B C2B C3B -60.16(15) . . . . ?
C5B C1B C2B C7B 179.6(2) . . . . ?
C6B C1B C2B C7B -1.8(4) . . . . ?
Ir1 C1B C2B C7B 119.9(2) . . . . ?
C5B C1B C2B Ir1 59.69(15) . . . . ?
C6B C1B C2B Ir1 -121.7(2) . . . . ?
N3' Ir1 C2B C1B -135.19(16) . . . . ?
N2 Ir1 C2B C1B 134.51(13) . . . . ?
C5B Ir1 C2B C1B -37.67(13) . . . . ?
C3B Ir1 C2B C1B -119.05(19) . . . . ?
C4B Ir1 C2B C1B -80.46(14) . . . . ?
Cl1A Ir1 C2B C1B 44.20(15) . . . . ?
N3' Ir1 C2B C3B -16.1(2) . . . . ?
N2 Ir1 C2B C3B -106.44(13) . . . . ?
C5B Ir1 C2B C3B 81.38(14) . . . . ?
C4B Ir1 C2B C3B 38.59(13) . . . . ?
C1B Ir1 C2B C3B 119.05(19) . . . . ?
Cl1A Ir1 C2B C3B 163.25(11) . . . . ?
N3' Ir1 C2B C7B 103.6(3) . . . . ?
N2 Ir1 C2B C7B 13.3(2) . . . . ?
C5B Ir1 C2B C7B -158.9(3) . . . . ?
C3B Ir1 C2B C7B 119.7(3) . . . . ?
C4B Ir1 C2B C7B 158.3(3) . . . . ?
C1B Ir1 C2B C7B -121.3(3) . . . . ?
Cl1A Ir1 C2B C7B -77.1(2) . . . . ?
C1B C2B C3B C4B -1.2(2) . . . . ?
C7B C2B C3B C4B 178.7(2) . . . . ?
Ir1 C2B C3B C4B -61.94(15) . . . . ?
C1B C2B C3B C8B -173.8(2) . . . . ?
C7B C2B C3B C8B 6.1(4) . . . . ?
Ir1 C2B C3B C8B 125.5(2) . . . . ?
C1B C2B C3B Ir1 60.71(16) . . . . ?
C7B C2B C3B Ir1 -119.4(2) . . . . ?
N3' Ir1 C3B C4B -72.55(14) . . . . ?
N2 Ir1 C3B C4B -161.62(12) . . . . ?
C5B Ir1 C3B C4B 36.47(13) . . . . ?
C1B Ir1 C3B C4B 79.86(14) . . . . ?
C2B Ir1 C3B C4B 116.34(19) . . . . ?
Cl1A Ir1 C3B C4B 73.7(2) . . . . ?
N3' Ir1 C3B C2B 171.11(13) . . . . ?
N2 Ir1 C3B C2B 82.03(14) . . . . ?
C5B Ir1 C3B C2B -79.87(14) . . . . ?
C4B Ir1 C3B C2B -116.34(19) . . . . ?
C1B Ir1 C3B C2B -36.48(13) . . . . ?
Cl1A Ir1 C3B C2B -42.6(3) . . . . ?
N3' Ir1 C3B C8B 49.0(3) . . . . ?
N2 Ir1 C3B C8B -40.1(3) . . . . ?
C5B Ir1 C3B C8B 158.0(3) . . . . ?
C4B Ir1 C3B C8B 121.5(3) . . . . ?
C1B Ir1 C3B C8B -158.6(3) . . . . ?
C2B Ir1 C3B C8B -122.1(3) . . . . ?
Cl1A Ir1 C3B C8B -164.75(18) . . . . ?
C2B C3B C4B C5B 2.5(2) . . . . ?
C8B C3B C4B C5B 175.1(2) . . . . ?
Ir1 C3B C4B C5B -59.48(15) . . . . ?
C2B C3B C4B C9B -178.4(2) . . . . ?
C8B C3B C4B C9B -5.8(4) . . . . ?
Ir1 C3B C4B C9B 119.6(2) . . . . ?
C2B C3B C4B Ir1 61.98(15) . . . . ?
C8B C3B C4B Ir1 -125.4(2) . . . . ?
N3' Ir1 C4B C5B -124.31(13) . . . . ?
N2 Ir1 C4B C5B 149.46(14) . . . . ?
C3B Ir1 C4B C5B 119.76(19) . . . . ?
C1B Ir1 C4B C5B 38.71(14) . . . . ?
C2B Ir1 C4B C5B 81.01(15) . . . . ?
Cl1A Ir1 C4B C5B -33.32(16) . . . . ?
N3' Ir1 C4B C3B 115.93(13) . . . . ?
N2 Ir1 C4B C3B 29.70(19) . . . . ?
C5B Ir1 C4B C3B -119.76(19) . . . . ?
C1B Ir1 C4B C3B -81.05(14) . . . . ?
C2B Ir1 C4B C3B -38.75(14) . . . . ?
Cl1A Ir1 C4B C3B -153.09(11) . . . . ?
N3' Ir1 C4B C9B -3.7(2) . . . . ?
N2 Ir1 C4B C9B -89.9(2) . . . . ?
C5B Ir1 C4B C9B 120.6(3) . . . . ?
C3B Ir1 C4B C9B -119.6(3) . . . . ?
C1B Ir1 C4B C9B 159.3(3) . . . . ?
C2B Ir1 C4B C9B -158.3(3) . . . . ?
Cl1A Ir1 C4B C9B 87.3(2) . . . . ?
C3B C4B C5B C1B -2.8(2) . . . . ?
C9B C4B C5B C1B 178.1(2) . . . . ?
Ir1 C4B C5B C1B -62.52(15) . . . . ?
C3B C4B C5B C10B -177.9(2) . . . . ?
C9B C4B C5B C10B 3.0(4) . . . . ?
Ir1 C4B C5B C10B 122.4(2) . . . . ?
C3B C4B C5B Ir1 59.71(15) . . . . ?
C9B C4B C5B Ir1 -119.4(2) . . . . ?
C2B C1B C5B C4B 2.0(2) . . . . ?
C6B C1B C5B C4B -176.6(2) . . . . ?
Ir1 C1B C5B C4B 62.65(15) . . . . ?
C2B C1B C5B C10B 177.1(2) . . . . ?
C6B C1B C5B C10B -1.5(4) . . . . ?
Ir1 C1B C5B C10B -122.3(2) . . . . ?
C2B C1B C5B Ir1 -60.63(15) . . . . ?
C6B C1B C5B Ir1 120.7(2) . . . . ?
N3' Ir1 C5B C4B 65.06(15) . . . . ?
N2 Ir1 C5B C4B -105.0(3) . . . . ?
C3B Ir1 C5B C4B -36.88(13) . . . . ?
C1B Ir1 C5B C4B -116.74(19) . . . . ?
C2B Ir1 C5B C4B -80.19(14) . . . . ?
Cl1A Ir1 C5B C4B 155.54(12) . . . . ?
N3' Ir1 C5B C1B -178.20(12) . . . . ?
N2 Ir1 C5B C1B 11.7(3) . . . . ?
C3B Ir1 C5B C1B 79.86(14) . . . . ?
C4B Ir1 C5B C1B 116.74(19) . . . . ?
C2B Ir1 C5B C1B 36.56(14) . . . . ?
Cl1A Ir1 C5B C1B -87.71(13) . . . . ?
N3' Ir1 C5B C10B -56.7(2) . . . . ?
N2 Ir1 C5B C10B 133.3(3) . . . . ?
C3B Ir1 C5B C10B -158.6(3) . . . . ?
C4B Ir1 C5B C10B -121.7(3) . . . . ?
C1B Ir1 C5B C10B 121.5(3) . . . . ?
C2B Ir1 C5B C10B 158.1(3) . . . . ?
Cl1A Ir1 C5B C10B 33.8(2) . . . . ?
C41C B1C C11C C12C 33.5(3) . . . . ?
C21C B1C C11C C12C 149.89(19) . . . . ?
C31C B1C C11C C12C -91.7(2) . . . . ?
C41C B1C C11C C16C -154.97(19) . . . . ?
C21C B1C C11C C16C -38.6(3) . . . . ?
C31C B1C C11C C16C 79.9(2) . . . . ?
C16C C11C C12C C13C 0.1(3) . . . . ?
B1C C11C C12C C13C 171.9(2) . . . . ?
C11C C12C C13C C14C -0.8(3) . . . . ?
C11C C12C C13C C17C 176.4(2) . . . . ?
C12C C13C C14C C15C 0.5(3) . . . . ?
C17C C13C C14C C15C -176.7(2) . . . . ?
C13C C14C C15C C16C 0.5(3) . . . . ?
C13C C14C C15C C18C 179.4(2) . . . . ?
C14C C15C C16C C11C -1.3(3) . . . . ?
C18C C15C C16C C11C 179.9(2) . . . . ?
C12C C11C C16C C15C 0.9(3) . . . . ?
B1C C11C C16C C15C -171.2(2) . . . . ?
C14C C13C C17C F1C -141.8(2) . . . . ?
C12C C13C C17C F1C 40.9(3) . . . . ?
C14C C13C C17C F3C -19.1(4) . . . . ?
C12C C13C C17C F3C 163.7(2) . . . . ?
C14C C13C C17C F2C 100.5(3) . . . . ?
C12C C13C C17C F2C -76.7(3) . . . . ?
C14C C15C C18C F6C 138.7(2) . . . . ?
C16C C15C C18C F6C -42.4(3) . . . . ?
C14C C15C C18C F4C 15.9(3) . . . . ?
C16C C15C C18C F4C -165.2(2) . . . . ?
C14C C15C C18C F5C -102.1(3) . . . . ?
C16C C15C C18C F5C 76.7(3) . . . . ?
C41C B1C C21C C26C -88.2(2) . . . . ?
C11C B1C C21C C26C 148.92(19) . . . . ?
C31C B1C C21C C26C 35.1(3) . . . . ?
C41C B1C C21C C22C 87.1(2) . . . . ?
C11C B1C C21C C22C -35.8(3) . . . . ?
C31C B1C C21C C22C -149.69(19) . . . . ?
C26C C21C C22C C23C -1.3(3) . . . . ?
B1C C21C C22C C23C -176.84(19) . . . . ?
C21C C22C C23C C24C 0.0(3) . . . . ?
C21C C22C C23C C27C -179.0(2) . . . . ?
C22C C23C C24C C25C 1.1(3) . . . . ?
C27C C23C C24C C25C -179.9(2) . . . . ?
C23C C24C C25C C26C -0.9(3) . . . . ?
C23C C24C C25C C28C -177.7(2) . . . . ?
C24C C25C C26C C21C -0.5(3) . . . . ?
C28C C25C C26C C21C 176.4(2) . . . . ?
C22C C21C C26C C25C 1.5(3) . . . . ?
B1C C21C C26C C25C 177.1(2) . . . . ?
C24C C23C C27C F9C 3.5(3) . . . . ?
C22C C23C C27C F9C -177.5(2) . . . . ?
C24C C23C C27C F8C -118.1(2) . . . . ?
C22C C23C C27C F8C 60.9(3) . . . . ?
C24C C23C C27C F7C 124.0(2) . . . . ?
C22C C23C C27C F7C -56.9(3) . . . . ?
C24C C25C C28C F10C -10.0(3) . . . . ?
C26C C25C C28C F10C 173.1(2) . . . . ?
C24C C25C C28C F11C 111.3(2) . . . . ?
C26C C25C C28C F11C -65.6(3) . . . . ?
C24C C25C C28C F12C -130.9(2) . . . . ?
C26C C25C C28C F12C 52.2(3) . . . . ?
C41C B1C C31C C36C -29.4(3) . . . . ?
C11C B1C C31C C36C 95.4(2) . . . . ?
C21C B1C C31C C36C -145.7(2) . . . . ?
C41C B1C C31C C32C 157.89(19) . . . . ?
C11C B1C C31C C32C -77.3(2) . . . . ?
C21C B1C C31C C32C 41.6(3) . . . . ?
C36C C31C C32C C33C 0.4(3) . . . . ?
B1C C31C C32C C33C 173.7(2) . . . . ?
C31C C32C C33C C34C 1.5(3) . . . . ?
C31C C32C C33C C37C -178.6(2) . . . . ?
C32C C33C C34C C35C -1.3(3) . . . . ?
C37C C33C C34C C35C 178.9(2) . . . . ?
C33C C34C C35C C36C -0.8(3) . . . . ?
C33C C34C C35C C38C 178.7(2) . . . . ?
C34C C35C C36C C31C 2.7(4) . . . . ?
C38C C35C C36C C31C -176.8(2) . . . . ?
C32C C31C C36C C35C -2.4(3) . . . . ?
B1C C31C C36C C35C -175.4(2) . . . . ?
C34C C33C C37C F14C 108.0(3) . . . . ?
C32C C33C C37C F14C -71.8(3) . . . . ?
C34C C33C C37C F15C -13.2(3) . . . . ?
C32C C33C C37C F15C 166.9(2) . . . . ?
C34C C33C C37C F13C -133.5(2) . . . . ?
C32C C33C C37C F13C 46.7(3) . . . . ?
C34C C35C C38C F16B 145.3(12) . . . . ?
C36C C35C C38C F16B -35.2(13) . . . . ?
C34C C35C C38C F18B 14.1(14) . . . . ?
C36C C35C C38C F18B -166.5(14) . . . . ?
C34C C35C C38C F16C -153.4(11) . . . . ?
C36C C35C C38C F16C 26.1(11) . . . . ?
C34C C35C C38C F17C -27.1(13) . . . . ?
C36C C35C C38C F17C 152.4(12) . . . . ?
C34C C35C C38C F17A -59.7(12) . . . . ?
C36C C35C C38C F17A 119.7(12) . . . . ?
C34C C35C C38C F18A 61.8(10) . . . . ?
C36C C35C C38C F18A -118.8(9) . . . . ?
C34C C35C C38C F16A -179.2(9) . . . . ?
C36C C35C C38C F16A 0.3(10) . . . . ?
C34C C35C C38C F17B -100.6(11) . . . . ?
C36C C35C C38C F17B 78.9(11) . . . . ?
C34C C35C C38C F18C 90.2(10) . . . . ?
C36C C35C C38C F18C -90.4(10) . . . . ?
C11C B1C C41C C46C 40.7(3) . . . . ?
C21C B1C C41C C46C -80.2(2) . . . . ?
C31C B1C C41C C46C 159.40(19) . . . . ?
C11C B1C C41C C42C -149.4(2) . . . . ?
C21C B1C C41C C42C 89.7(2) . . . . ?
C31C B1C C41C C42C -30.7(3) . . . . ?
C46C C41C C42C C43C -1.5(3) . . . . ?
B1C C41C C42C C43C -171.9(2) . . . . ?
C41C C42C C43C C44C 1.7(4) . . . . ?
C41C C42C C43C C47C -178.4(2) . . . . ?
C42C C43C C44C C45C -0.4(3) . . . . ?
C47C C43C C44C C45C 179.6(2) . . . . ?
C43C C44C C45C C46C -0.9(3) . . . . ?
C43C C44C C45C C48C 174.8(2) . . . . ?
C44C C45C C46C C41C 1.0(4) . . . . ?
C48C C45C C46C C41C -174.7(2) . . . . ?
C42C C41C C46C C45C 0.2(3) . . . . ?
B1C C41C C46C C45C 170.8(2) . . . . ?
C44C C43C C47C F19C 166.4(2) . . . . ?
C42C C43C C47C F19C -13.6(4) . . . . ?
C44C C43C C47C F21C -69.9(3) . . . . ?
C42C C43C C47C F21C 110.1(3) . . . . ?
C44C C43C C47C F20C 47.8(3) . . . . ?
C42C C43C C47C F20C -132.1(2) . . . . ?
C44C C45C C48C F23C -94.6(3) . . . . ?
C46C C45C C48C F23C 81.1(3) . . . . ?
C44C C45C C48C F22C 28.1(3) . . . . ?
C46C C45C C48C F22C -156.1(2) . . . . ?
C44C C45C C48C F24C 147.1(2) . . . . ?
C46C C45C C48C F24C -37.1(3) . . . . ?
C1D C1D Cl1D Cl2D -159.2(10) 2_665 . . . ?
Cl1D C1D Cl1D Cl2D -159.2(10) 2_665 . . . ?
Cl2D C1D Cl1D Cl2D -166.9(7) 2_665 . . . ?
Cl2D C1D Cl1D C1D 159.2(10) . . . 2_665 ?
Cl1D C1D Cl1D C1D 0.0 2_665 . . 2_665 ?
Cl2D C1D Cl1D C1D -7.7(4) 2_665 . . 2_665 ?
C1D Cl1D Cl2D C1D -16.4(8) 2_665 . . . ?
C1D Cl1D Cl2D C1D 16.4(8) . . . 2_665 ?
C1D C1D Cl2D Cl1D 17.2(9) 2_665 . . . ?
Cl1D C1D Cl2D Cl1D 38.2(17) 2_665 . . . ?
Cl2D C1D Cl2D Cl1D 17.2(9) 2_665 . . . ?
Cl1D C1D Cl2D C1D 21.0(9) 2_665 . . 2_665 ?
Cl1D C1D Cl2D C1D -17.2(9) . . . 2_665 ?
Cl2D C1D Cl2D C1D 0.0 2_665 . . 2_665 ?
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max 0.614
_refine_diff_density_min -0.865
_refine_diff_density_rms 0.063
_iucr_refine_instructions_details
;
TITL Carol4_P1bar in P-1
CELL 0.71073 12.5013 16.3750 16.9370 117.541 96.775 101.575
ZERR 2.00 0.0014 0.0008 0.0008 0.002 0.002 0.002
LATT 1
SFAC C H N Cl Ir F B
UNIT 111 82 10 4 2 48 2
OMIT 0 1 2
OMIT -1 1 1
OMIT 1 0 1
OMIT 0 1 1
OMIT 1 0 0
OMIT -1 -1 2
OMIT 0 -2 1
OMIT 1 -1 1
OMIT 1 1 0
OMIT 0 1 0
OMIT -1 1 0
OMIT 0 0 1
OMIT 0 0 2
OMIT -1 0 2
OMIT -1 -1 1
OMIT 0 -1 2
OMIT 2 -2 1
OMIT -1 -2 3
OMIT -1 0 1
OMIT -1 2 1
OMIT 0 -3 1
OMIT -3 50
L.S. 20
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.413 0.376 0.164
CONF
SADI C38C F16A C38C F17A C38C F18A C38C F16B C38C F17B C38C F18B C38C F16C C38C
DFIX 1.089 0.002 C1D H1D C1D H2D
DFIX 1.746 0.002 H1D H2D
DELU 0.02 CL1D CL2D C1D
DELU C38C F16A F17A F18A F16B F17B F18B F16C F17C F18C
SIMU 0.02 CL1D CL2D C1D
SIMU C38C F16A F17A F18A F16B F17B F18B F16C F17C F18C
TEMP -122.340
WGHT 0.019100 2.997900
FVAR 0.11089
MOLE 1
IR1 5 -0.126123 0.836259 0.621563 11.00000 0.01552 0.01487 =
0.01955 0.01104 0.00574 0.00561
N1 3 -0.060057 1.058332 0.747334 11.00000 0.02760 0.01679 =
0.01917 0.00763 0.00862 0.00744
N2 3 -0.144376 0.973991 0.705253 11.00000 0.02170 0.01804 =
0.02531 0.01247 0.00952 0.00749
C3 1 -0.238069 0.998388 0.723447 11.00000 0.02762 0.03168 =
0.03558 0.02036 0.01516 0.01632
AFIX 43
H3 2 -0.311049 0.954173 0.702169 11.00000 -1.20000
AFIX 0
C4 1 -0.213665 1.097598 0.777904 11.00000 0.04307 0.03360 =
0.03937 0.01983 0.02286 0.02595
AFIX 43
H4 2 -0.265031 1.133126 0.800989 11.00000 -1.20000
AFIX 0
C5 1 -0.100455 1.133391 0.791324 11.00000 0.04508 0.02112 =
0.02693 0.01095 0.01650 0.01611
AFIX 43
H5 2 -0.057932 1.199326 0.825518 11.00000 -1.20000
AFIX 0
C1A 1 0.056228 1.058621 0.744573 11.00000 0.02413 0.01912 =
0.02099 0.00838 0.00557 0.00321
AFIX 23
H1A1 2 0.082702 1.029447 0.780024 11.00000 -1.20000
H2A1 2 0.104431 1.125885 0.773904 11.00000 -1.20000
AFIX 0
N1' 3 0.111401 0.943325 0.518051 11.00000 0.02297 0.01692 =
0.02327 0.01189 0.00998 0.00581
N2' 3 0.027456 0.874372 0.511745 11.00000 0.02091 0.01757 =
0.01992 0.00994 0.00771 0.00551
N3' 3 0.000915 0.911949 0.591391 11.00000 0.01925 0.01543 =
0.01946 0.00975 0.00624 0.00650
C4' 1 0.067738 1.003951 0.648252 11.00000 0.01924 0.01437 =
0.02249 0.00852 0.00531 0.00422
C5' 1 0.138846 1.024454 0.600483 11.00000 0.02472 0.01428 =
0.02603 0.00767 0.00882 0.00276
AFIX 43
H6A 2 0.195330 1.083016 0.620781 11.00000 -1.20000
AFIX 0
C6' 1 0.168254 0.920889 0.442044 11.00000 0.03070 0.02214 =
0.02396 0.01514 0.01486 0.00975
AFIX 23
H16' 2 0.197717 0.980049 0.439228 11.00000 -1.20000
H26' 2 0.113107 0.873199 0.383222 11.00000 -1.20000
AFIX 0
C7' 1 0.263946 0.881173 0.454531 11.00000 0.02386 0.02569 =
0.02185 0.01558 0.01272 0.00681
C8' 1 0.249917 0.783208 0.407721 11.00000 0.02532 0.02572 =
0.03496 0.01251 0.00906 0.00675
AFIX 43
H8' 2 0.179389 0.740425 0.367361 11.00000 -1.20000
AFIX 0
C9' 1 0.337760 0.746990 0.419188 11.00000 0.03649 0.03222 =
0.04781 0.02057 0.01835 0.01758
AFIX 43
H9' 2 0.327227 0.679539 0.386777 11.00000 -1.20000
AFIX 0
C10' 1 0.440240 0.808198 0.477291 11.00000 0.02977 0.05762 =
0.04672 0.03745 0.02006 0.02202
AFIX 43
H10' 2 0.500955 0.783304 0.484096 11.00000 -1.20000
AFIX 0
C11' 1 0.454523 0.905978 0.525695 11.00000 0.02291 0.05421 =
0.03781 0.02896 0.00269 0.00087
AFIX 43
H11' 2 0.524814 0.948271 0.566851 11.00000 -1.20000
AFIX 0
C12' 1 0.367177 0.942698 0.514634 11.00000 0.03261 0.02835 =
0.03003 0.01452 0.00789 0.00190
AFIX 43
H12' 2 0.377604 1.010090 0.548128 11.00000 -1.20000
AFIX 0
C1B 1 -0.230170 0.707223 0.611231 11.00000 0.02192 0.02247 =
0.04016 0.02387 0.00748 0.00512
C2B 1 -0.175231 0.773369 0.704369 11.00000 0.03265 0.02639 =
0.03449 0.02460 0.01681 0.01534
C3B 1 -0.054595 0.793624 0.713693 11.00000 0.02882 0.02126 =
0.02825 0.01750 0.00565 0.00900
C4B 1 -0.038160 0.736008 0.623555 11.00000 0.02626 0.02000 =
0.03275 0.02000 0.01077 0.01238
C5B 1 -0.145101 0.685193 0.560003 11.00000 0.03046 0.01392 =
0.02683 0.01182 0.00406 0.00742
C6B 1 -0.355358 0.664458 0.571397 11.00000 0.02384 0.04073 =
0.07725 0.04087 0.00246 -0.00053
AFIX 137
H6B1 2 -0.378890 0.600384 0.564840 11.00000 -1.50000
H6B2 2 -0.374140 0.659190 0.511068 11.00000 -1.50000
H6B3 2 -0.394491 0.705979 0.612369 11.00000 -1.50000
AFIX 0
C7B 1 -0.231340 0.815825 0.781251 11.00000 0.06404 0.05859 =
0.04896 0.04155 0.03881 0.03857
AFIX 137
H7B1 2 -0.303338 0.821347 0.757551 11.00000 -1.50000
H7B2 2 -0.182724 0.879780 0.828386 11.00000 -1.50000
H7B3 2 -0.244656 0.774118 0.808101 11.00000 -1.50000
AFIX 0
C8B 1 0.034858 0.852163 0.801025 11.00000 0.04989 0.03482 =
0.03217 0.02064 -0.00934 0.00631
AFIX 137
H8B1 2 0.009441 0.903767 0.845676 11.00000 -1.50000
H8B2 2 0.103681 0.880253 0.789118 11.00000 -1.50000
H8B3 2 0.050214 0.810924 0.825650 11.00000 -1.50000
AFIX 0
C9B 1 0.073594 0.732301 0.601379 11.00000 0.03024 0.04400 =
0.06262 0.03650 0.02160 0.02270
AFIX 137
H9B1 2 0.097666 0.683492 0.610945 11.00000 -1.50000
H9B2 2 0.129106 0.795287 0.641475 11.00000 -1.50000
H9B3 2 0.067294 0.715693 0.537174 11.00000 -1.50000
AFIX 0
C10B 1 -0.166141 0.614820 0.459567 11.00000 0.06916 0.02289 =
0.02958 0.01091 0.00464 0.01681
AFIX 137
H10B 2 -0.101598 0.631690 0.436708 11.00000 -1.50000
H10C 2 -0.234027 0.617013 0.426098 11.00000 -1.50000
H10D 2 -0.176540 0.549790 0.450288 11.00000 -1.50000
AFIX 0
CL1A 4 -0.254675 0.829543 0.500356 11.00000 0.02249 0.02570 =
0.02929 0.01853 0.00016 0.00494
MOLE 2
B1C 7 0.752499 0.323040 0.103324 11.00000 0.01807 0.01619 =
0.01934 0.01002 0.00646 0.00617
C11C 1 0.716945 0.303139 -0.001604 11.00000 0.02114 0.01401 =
0.02136 0.01000 0.00830 0.00930
C12C 1 0.612177 0.244121 -0.062109 11.00000 0.02174 0.01700 =
0.02426 0.01172 0.00810 0.00747
AFIX 43
H12C 2 0.561701 0.207015 -0.045043 11.00000 -1.20000
AFIX 0
C13C 1 0.579672 0.238165 -0.146735 11.00000 0.02530 0.01860 =
0.02442 0.01104 0.00481 0.00788
C14C 1 0.649892 0.291815 -0.174172 11.00000 0.03368 0.02264 =
0.02091 0.01288 0.00804 0.01333
AFIX 43
H14C 2 0.627482 0.288087 -0.231610 11.00000 -1.20000
AFIX 0
C15C 1 0.753909 0.351096 -0.115032 11.00000 0.02763 0.01895 =
0.02496 0.01402 0.01112 0.01086
C16C 1 0.786682 0.355747 -0.031539 11.00000 0.02148 0.01727 =
0.02311 0.01085 0.00656 0.00802
AFIX 43
H16C 2 0.859109 0.396099 0.006802 11.00000 -1.20000
AFIX 0
C17C 1 0.469464 0.169315 -0.210005 11.00000 0.03609 0.03552 =
0.03248 0.01955 -0.00154 0.00179
C18C 1 0.835054 0.410555 -0.140121 11.00000 0.03713 0.03581 =
0.03666 0.02661 0.01069 0.00981
F1C 6 0.387065 0.166707 -0.167695 11.00000 0.03147 0.11369 =
0.05205 0.03841 -0.00395 -0.01895
F2C 6 0.474801 0.078655 -0.252239 11.00000 0.07968 0.02764 =
0.07659 0.00595 -0.03094 -0.00256
F3C 6 0.433269 0.185966 -0.276543 11.00000 0.04731 0.06622 =
0.05233 0.04139 -0.01887 -0.00717
F4C 6 0.788190 0.419137 -0.209115 11.00000 0.05695 0.05905 =
0.04840 0.04556 0.00776 0.00386
F5C 6 0.917198 0.370860 -0.168173 11.00000 0.06020 0.10973 =
0.14138 0.10373 0.06938 0.04971
F6C 6 0.886098 0.497930 -0.071015 11.00000 0.09629 0.04484 =
0.04432 0.02570 0.00613 -0.02832
C21C 1 0.888586 0.343021 0.136105 11.00000 0.01959 0.01594 =
0.02493 0.01473 0.00851 0.00697
C22C 1 0.950706 0.295220 0.075438 11.00000 0.02274 0.02015 =
0.02237 0.01482 0.00801 0.00837
AFIX 43
H22C 2 0.913664 0.252184 0.012619 11.00000 -1.20000
AFIX 0
C23C 1 1.065147 0.308755 0.104258 11.00000 0.02286 0.02415 =
0.02911 0.01996 0.01232 0.01222
C24C 1 1.122593 0.370729 0.195133 11.00000 0.01786 0.02356 =
0.03251 0.01969 0.00742 0.00692
AFIX 43
H24C 2 1.200879 0.380893 0.214717 11.00000 -1.20000
AFIX 0
C25C 1 1.062146 0.417468 0.256615 11.00000 0.02477 0.01762 =
0.02627 0.01484 0.00614 0.00628
C26C 1 0.947849 0.403540 0.227652 11.00000 0.02254 0.01880 =
0.02287 0.01305 0.00914 0.00926
AFIX 43
H26C 2 0.908811 0.436312 0.271648 11.00000 -1.20000
AFIX 0
C27C 1 1.124390 0.255435 0.033616 11.00000 0.02724 0.04253 =
0.03428 0.02351 0.01437 0.01885
C28C 1 1.118763 0.488247 0.355124 11.00000 0.02635 0.02202 =
0.03114 0.01377 0.00316 0.00714
F7C 6 1.076276 0.159921 -0.010550 11.00000 0.05363 0.03741 =
0.06651 0.01162 0.03130 0.02486
F8C 6 1.121120 0.278810 -0.032255 11.00000 0.06025 0.08745 =
0.04386 0.04669 0.03449 0.04666
F9C 6 1.232126 0.269805 0.067979 11.00000 0.02866 0.07525 =
0.04327 0.03011 0.01874 0.03087
F10C 6 1.224852 0.489055 0.378715 11.00000 0.02974 0.05419 =
0.04254 0.00860 -0.00863 0.01435
F11C 6 1.121116 0.578454 0.376666 11.00000 0.05559 0.01805 =
0.03649 0.01155 0.00341 0.00458
F12C 6 1.065084 0.471770 0.412859 11.00000 0.05118 0.03491 =
0.02496 0.01717 0.00411 0.00443
C31C 1 0.715599 0.420228 0.164036 11.00000 0.01923 0.01787 =
0.01680 0.00960 0.00320 0.00615
C32C 1 0.783242 0.510194 0.184652 11.00000 0.01918 0.01999 =
0.01924 0.01100 0.00531 0.00649
AFIX 43
H32C 2 0.853503 0.514280 0.168382 11.00000 -1.20000
AFIX 0
C33C 1 0.751216 0.593443 0.227961 11.00000 0.02528 0.01751 =
0.01824 0.00926 0.00338 0.00563
C34C 1 0.651231 0.592040 0.254981 11.00000 0.02844 0.01917 =
0.02388 0.00856 0.00683 0.01254
AFIX 43
H34C 2 0.630142 0.649403 0.285746 11.00000 -1.20000
AFIX 0
C35C 1 0.582449 0.503714 0.235588 11.00000 0.01874 0.02498 =
0.02475 0.01060 0.00542 0.00990
C36C 1 0.613206 0.419810 0.189567 11.00000 0.01648 0.01902 =
0.02464 0.01118 0.00338 0.00413
AFIX 43
H36C 2 0.562948 0.360219 0.174994 11.00000 -1.20000
AFIX 0
C37C 1 0.828155 0.685371 0.244971 11.00000 0.03818 0.01780 =
0.02964 0.00917 0.01128 0.00517
C38C 1 0.474632 0.500030 0.265762 11.00000 0.02697 0.03274 =
0.05018 0.01451 0.01667 0.01334
F13C 6 0.865581 0.677628 0.172115 11.00000 0.06525 0.03077 =
0.04281 0.02110 0.02346 0.00157
F14C 6 0.920677 0.717775 0.310414 11.00000 0.06770 0.05735 =
0.05738 0.03257 -0.02656 -0.03684
F15C 6 0.780380 0.756175 0.268936 11.00000 0.08686 0.02228 =
0.13221 0.03622 0.06845 0.02614
PART 1
F16A 6 0.416344 0.411628 0.244451 10.33333 0.01605 0.03409 =
0.05545 0.01325 0.01402 0.00540
F17A 6 0.489772 0.552643 0.355396 10.33333 0.04077 0.07336 =
0.04081 -0.01167 0.02414 0.00388
F18A 6 0.402604 0.529493 0.227646 10.33333 0.02451 0.07290 =
0.11710 0.06194 0.02074 0.03002
PART 2
F16B 6 0.394656 0.423361 0.209943 10.33333 0.01705 0.08249 =
0.06471 -0.00812 0.01066 -0.00375
F17B 6 0.492962 0.494516 0.344580 10.33333 0.05008 0.12674 =
0.05925 0.05012 0.03617 0.02386
F18B 6 0.444468 0.577446 0.290163 10.33333 0.04004 0.06364 =
0.17781 0.05766 0.05915 0.04243
PART 3
F16C 6 0.438284 0.429409 0.279916 10.33333 0.06181 0.06653 =
0.09968 0.06043 0.06293 0.03801
F17C 6 0.476505 0.580117 0.337879 10.33333 0.03558 0.04797 =
0.09284 -0.00081 0.03625 0.02096
F18C 6 0.387018 0.485621 0.196568 10.33333 0.02058 0.09776 =
0.09316 0.05849 0.01077 0.01583
PART 0
C41C 1 0.698155 0.231474 0.115921 11.00000 0.01432 0.01986 =
0.02247 0.01279 0.00550 0.00701
C42C 1 0.672128 0.242370 0.197911 11.00000 0.02015 0.02066 =
0.02222 0.01190 0.00679 0.00780
AFIX 43
H42C 2 0.677187 0.304906 0.245638 11.00000 -1.20000
AFIX 0
C43C 1 0.639165 0.164501 0.211480 11.00000 0.02084 0.03007 =
0.02863 0.02001 0.00927 0.00939
C44C 1 0.633372 0.072229 0.144645 11.00000 0.02367 0.02444 =
0.03868 0.02342 0.01103 0.00711
AFIX 43
H44C 2 0.611313 0.019054 0.154080 11.00000 -1.20000
AFIX 0
C45C 1 0.660713 0.059981 0.063767 11.00000 0.01930 0.02026 =
0.03296 0.01437 0.00775 0.00721
C46C 1 0.691504 0.137675 0.049641 11.00000 0.01950 0.02114 =
0.02223 0.01253 0.00788 0.00758
AFIX 43
H46C 2 0.708634 0.126742 -0.006975 11.00000 -1.20000
AFIX 0
C47C 1 0.609075 0.178201 0.298745 11.00000 0.03604 0.03978 =
0.03714 0.02838 0.01739 0.01165
C48C 1 0.664974 -0.036768 -0.006617 11.00000 0.03174 0.02299 =
0.04318 0.01590 0.01198 0.00897
F19C 6 0.639526 0.269118 0.365020 11.00000 0.13912 0.04823 =
0.04123 0.02275 0.05132 0.02258
F20C 6 0.659813 0.133591 0.333938 11.00000 0.05351 0.08524 =
0.05227 0.05508 0.02174 0.02659
F21C 6 0.499852 0.141144 0.287099 11.00000 0.02951 0.13714 =
0.05747 0.06491 0.02220 0.01838
F22C 6 0.597043 -0.109054 -0.004702 11.00000 0.10341 0.01992 =
0.09008 0.02135 0.05101 0.00803
F23C 6 0.767890 -0.045701 0.001726 11.00000 0.04737 0.04545 =
0.07040 0.00280 0.00045 0.03365
F24C 6 0.633699 -0.054251 -0.092621 11.00000 0.06880 0.03649 =
0.03628 0.00450 0.00751 0.02430
MOLE 3
C1D 1 0.468081 0.532003 0.011437 10.50000 0.07997 0.09454 =
0.05604 0.03626 0.02059 0.06962
H1D 2 0.409844 0.552993 -0.023487 10.50000 10.06000
H2D 2 0.443186 0.543366 0.074346 10.50000 10.06000
CL1D 4 0.604918 0.557308 -0.000771 10.50000 0.07670 0.21202 =
0.10646 0.06744 0.01655 0.02766
CL2D 4 0.576543 0.597841 0.027549 10.50000 0.13909 0.07416 =
0.07943 0.02916 0.00382 0.04901
HKLF 4
REM Carol4_P1bar in P-1
REM R1 = 0.0186 for 9804 Fo > 4sig(Fo) and 0.0195 for all 10113 data
REM 876 parameters refined using 204 restraints
END
WGHT 0.0191 2.9993
REM Highest difference peak 0.614, deepest hole -0.865, 1-sigma level 0.063
Q1 1 0.5546 0.2536 0.3301 11.00000 0.05 0.61
Q2 1 0.6783 0.2060 0.3672 11.00000 0.05 0.61
Q3 1 0.6786 -0.0921 0.0337 11.00000 0.05 0.60
Q4 1 0.9258 0.4329 -0.1068 11.00000 0.05 0.54
Q5 1 0.8047 0.5038 -0.0914 11.00000 0.05 0.49
Q6 1 0.5027 0.5779 0.0245 11.00000 0.05 0.45
Q7 1 0.4262 0.1062 -0.2127 11.00000 0.05 0.42
Q8 1 0.8394 0.7655 0.3200 11.00000 0.05 0.42
Q9 1 0.4043 0.2298 -0.2221 11.00000 0.05 0.37
Q10 1 -0.1260 0.7722 0.5410 11.00000 0.05 0.37
Q11 1 0.7556 -0.0515 0.0613 11.00000 0.05 0.37
Q12 1 0.7374 0.3764 0.1366 11.00000 0.05 0.36
Q13 1 -0.1167 0.8950 0.6891 11.00000 0.05 0.36
Q14 1 0.5000 0.5000 0.0000 10.50000 0.05 0.35
Q15 1 0.7605 0.4657 -0.1616 11.00000 0.05 0.35
Q16 1 0.5003 0.1122 -0.2815 11.00000 0.05 0.33
Q17 1 0.8211 0.3370 0.1202 11.00000 0.05 0.32
Q18 1 0.6622 0.5665 -0.0070 11.00000 0.05 0.31
Q19 1 1.1833 0.3374 0.0171 11.00000 0.05 0.31
Q20 1 0.7073 -0.0429 -0.0656 11.00000 0.05 0.31
;
#===END
data_carol13_p21byn
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C46 H46 B Cl Ir N5'
_chemical_formula_weight 907.34
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ir' 'Ir' -1.4442 7.9887
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'P2(1)/n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.0829(5)
_cell_length_b 24.4058(10)
_cell_length_c 13.3522(5)
_cell_angle_alpha 90.00
_cell_angle_beta 93.701(2)
_cell_angle_gamma 90.00
_cell_volume 3929.3(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 156(2)
_cell_measurement_reflns_used 9743
_cell_measurement_theta_min 2.375
_cell_measurement_theta_max 30.457
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'Yellow'
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.21
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.534
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1824
_exptl_absorpt_coefficient_mu 3.506
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.3733
_exptl_absorpt_correction_T_max 0.5222
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 156(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 29202
_diffrn_reflns_av_R_equivalents 0.0255
_diffrn_reflns_av_sigmaI/netI 0.0198
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 28
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 3.68
_diffrn_reflns_theta_max 25.00
_reflns_number_total 6884
_reflns_number_gt 6549
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0148P)^2^+3.7404P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6884
_refine_ls_number_parameters 492
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0182
_refine_ls_R_factor_gt 0.0167
_refine_ls_wR_factor_ref 0.0416
_refine_ls_wR_factor_gt 0.0408
_refine_ls_goodness_of_fit_ref 1.066
_refine_ls_restrained_S_all 1.066
_refine_ls_shift/su_max 0.007
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ir1 Ir 0.772855(7) 0.922999(3) 0.246430(6) 0.01621(4) Uani 1 1 d . . .
N1 N 0.77441(16) 0.85787(7) 0.44525(13) 0.0223(4) Uani 1 1 d . . .
N2 N 0.83333(15) 0.88924(7) 0.38330(13) 0.0200(4) Uani 1 1 d . . .
C3 C 0.93519(19) 0.89205(10) 0.42622(17) 0.0248(5) Uani 1 1 d . . .
H3 H 0.9945 0.9118 0.3998 0.030 Uiso 1 1 calc R . .
C4 C 0.9436(2) 0.86219(10) 0.51511(17) 0.0274(5) Uani 1 1 d . . .
H4 H 1.0076 0.8575 0.5595 0.033 Uiso 1 1 calc R . .
C5 C 0.8403(2) 0.84097(10) 0.52484(17) 0.0269(5) Uani 1 1 d . . .
H5 H 0.8186 0.8184 0.5781 0.032 Uiso 1 1 calc R . .
C1A C 0.65933(19) 0.84341(9) 0.41896(17) 0.0242(5) Uani 1 1 d . . .
H1A1 H 0.6274 0.8259 0.4775 0.029 Uiso 1 1 calc R . .
H2A1 H 0.6564 0.8165 0.3634 0.029 Uiso 1 1 calc R . .
N1' N 0.46593(15) 0.95325(7) 0.35406(13) 0.0201(4) Uani 1 1 d . . .
N2' N 0.54943(16) 0.96548(8) 0.29637(13) 0.0224(4) Uani 1 1 d . . .
N3' N 0.62522(16) 0.92771(7) 0.31716(13) 0.0196(4) Uani 1 1 d . . .
C4' C 0.59128(18) 0.89235(9) 0.38769(15) 0.0191(4) Uani 1 1 d . . .
C5' C 0.48865(19) 0.90855(9) 0.41225(16) 0.0207(5) Uani 1 1 d . . .
H5' H 0.4432 0.8922 0.4595 0.025 Uiso 1 1 calc R . .
C6' C 0.36505(18) 0.98444(8) 0.34394(16) 0.0206(5) Uani 1 1 d . . .
C7' C 0.3310(2) 1.00509(9) 0.25048(17) 0.0254(5) Uani 1 1 d . . .
H7' H 0.3748 0.9998 0.1947 0.030 Uiso 1 1 calc R . .
C8' C 0.2322(2) 1.03346(10) 0.23990(18) 0.0291(5) Uani 1 1 d . . .
H8' H 0.2085 1.0486 0.1766 0.035 Uiso 1 1 calc R . .
C9' C 0.1674(2) 1.04007(10) 0.32102(18) 0.0310(5) Uani 1 1 d . . .
H9' H 0.0985 1.0588 0.3129 0.037 Uiso 1 1 calc R . .
C10' C 0.2034(2) 1.01936(10) 0.41376(19) 0.0323(6) Uani 1 1 d . . .
H10' H 0.1590 1.0241 0.4693 0.039 Uiso 1 1 calc R . .
C11' C 0.3035(2) 0.99181(9) 0.42652(17) 0.0259(5) Uani 1 1 d . . .
H11' H 0.3292 0.9783 0.4906 0.031 Uiso 1 1 calc R . .
C1B C 0.7486(2) 0.85948(9) 0.13474(16) 0.0250(5) Uani 1 1 d . . .
C2B C 0.8655(2) 0.86882(10) 0.15436(17) 0.0283(5) Uani 1 1 d . . .
C3B C 0.8890(2) 0.92439(10) 0.13215(18) 0.0316(6) Uani 1 1 d . . .
C4B C 0.7867(2) 0.94988(10) 0.09455(16) 0.0314(6) Uani 1 1 d . . .
C5B C 0.7017(2) 0.91003(10) 0.09525(16) 0.0275(5) Uani 1 1 d . . .
C6B C 0.6904(3) 0.80579(11) 0.1413(2) 0.0452(7) Uani 1 1 d . . .
H6B1 H 0.6912 0.7867 0.0768 0.068 Uiso 1 1 calc R . .
H6B2 H 0.6135 0.8120 0.1577 0.068 Uiso 1 1 calc R . .
H6B3 H 0.7283 0.7833 0.1938 0.068 Uiso 1 1 calc R . .
C7B C 0.9481(3) 0.82790(13) 0.1936(2) 0.0524(8) Uani 1 1 d . . .
H7B1 H 0.9759 0.8072 0.1376 0.079 Uiso 1 1 calc R . .
H7B2 H 0.9129 0.8027 0.2392 0.079 Uiso 1 1 calc R . .
H7B3 H 1.0099 0.8468 0.2301 0.079 Uiso 1 1 calc R . .
C8B C 0.9999(3) 0.95207(16) 0.1388(2) 0.0609(10) Uani 1 1 d . . .
H8B1 H 1.0521 0.9306 0.1823 0.091 Uiso 1 1 calc R . .
H8B2 H 0.9926 0.9889 0.1670 0.091 Uiso 1 1 calc R . .
H8B3 H 1.0277 0.9548 0.0716 0.091 Uiso 1 1 calc R . .
C9B C 0.7720(3) 1.00795(12) 0.0584(2) 0.0563(9) Uani 1 1 d . . .
H9B1 H 0.7847 1.0098 -0.0133 0.085 Uiso 1 1 calc R . .
H9B2 H 0.8253 1.0317 0.0959 0.085 Uiso 1 1 calc R . .
H9B3 H 0.6964 1.0202 0.0690 0.085 Uiso 1 1 calc R . .
C10B C 0.5829(3) 0.91788(14) 0.0608(2) 0.0522(8) Uani 1 1 d . . .
H10B H 0.5620 0.9563 0.0701 0.078 Uiso 1 1 calc R . .
H10C H 0.5364 0.8942 0.1000 0.078 Uiso 1 1 calc R . .
H10D H 0.5722 0.9083 -0.0105 0.078 Uiso 1 1 calc R . .
Cl1 Cl 0.82087(5) 1.00984(2) 0.31929(4) 0.02828(13) Uani 1 1 d . . .
B1C B 0.7669(2) 0.74974(10) 0.82248(18) 0.0191(5) Uani 1 1 d . . .
C11C C 0.74988(17) 0.71330(9) 0.71863(16) 0.0189(4) Uani 1 1 d . . .
C12C C 0.8020(2) 0.66269(10) 0.70705(18) 0.0274(5) Uani 1 1 d . . .
H12C H 0.8462 0.6482 0.7622 0.033 Uiso 1 1 calc R . .
C13C C 0.7919(2) 0.63272(10) 0.61839(18) 0.0306(5) Uani 1 1 d . . .
H13C H 0.8282 0.5983 0.6143 0.037 Uiso 1 1 calc R . .
C14C C 0.72939(19) 0.65270(10) 0.53620(17) 0.0252(5) Uani 1 1 d . . .
H14C H 0.7225 0.6324 0.4754 0.030 Uiso 1 1 calc R . .
C15C C 0.6771(2) 0.70251(10) 0.54382(16) 0.0252(5) Uani 1 1 d . . .
H15C H 0.6341 0.7169 0.4878 0.030 Uiso 1 1 calc R . .
C16C C 0.68718(18) 0.73183(9) 0.63371(16) 0.0212(4) Uani 1 1 d . . .
H16C H 0.6497 0.7659 0.6373 0.025 Uiso 1 1 calc R . .
C21C C 0.65305(18) 0.78572(9) 0.83668(15) 0.0207(5) Uani 1 1 d . . .
C22C C 0.56556(19) 0.76763(10) 0.89167(17) 0.0264(5) Uani 1 1 d . . .
H22C H 0.5737 0.7339 0.9269 0.032 Uiso 1 1 calc R . .
C23C C 0.4672(2) 0.79671(11) 0.89732(18) 0.0314(5) Uani 1 1 d . . .
H23C H 0.4101 0.7826 0.9356 0.038 Uiso 1 1 calc R . .
C24C C 0.4521(2) 0.84602(10) 0.84772(18) 0.0310(6) Uani 1 1 d . . .
H24C H 0.3849 0.8659 0.8512 0.037 Uiso 1 1 calc R . .
C25C C 0.5365(2) 0.86593(10) 0.79292(17) 0.0282(5) Uani 1 1 d . . .
H25C H 0.5276 0.8998 0.7584 0.034 Uiso 1 1 calc R . .
C26C C 0.63457(19) 0.83641(9) 0.78825(17) 0.0239(5) Uani 1 1 d . . .
H26C H 0.6917 0.8512 0.7506 0.029 Uiso 1 1 calc R . .
C31C C 0.87420(18) 0.79054(9) 0.81358(15) 0.0187(4) Uani 1 1 d . . .
C32C C 0.88850(19) 0.83799(9) 0.87298(16) 0.0229(5) Uani 1 1 d . . .
H32C H 0.8334 0.8470 0.9179 0.027 Uiso 1 1 calc R . .
C33C C 0.9798(2) 0.87202(9) 0.86849(17) 0.0274(5) Uani 1 1 d . . .
H33C H 0.9859 0.9037 0.9097 0.033 Uiso 1 1 calc R . .
C34C C 1.0621(2) 0.86021(10) 0.80448(17) 0.0279(5) Uani 1 1 d . . .
H34C H 1.1240 0.8839 0.8003 0.033 Uiso 1 1 calc R . .
C35C C 1.0526(2) 0.81322(10) 0.74670(17) 0.0274(5) Uani 1 1 d . . .
H35C H 1.1094 0.8038 0.7038 0.033 Uiso 1 1 calc R . .
C36C C 0.96012(19) 0.77971(9) 0.75133(16) 0.0235(5) Uani 1 1 d . . .
H36C H 0.9551 0.7479 0.7102 0.028 Uiso 1 1 calc R . .
C41C C 0.79062(18) 0.70913(9) 0.92011(15) 0.0196(4) Uani 1 1 d . . .
C42C C 0.87157(19) 0.71953(9) 0.99764(16) 0.0222(5) Uani 1 1 d . . .
H42C H 0.9202 0.7497 0.9909 0.027 Uiso 1 1 calc R . .
C43C C 0.8841(2) 0.68760(10) 1.08430(17) 0.0263(5) Uani 1 1 d . . .
H43C H 0.9399 0.6964 1.1351 0.032 Uiso 1 1 calc R . .
C44C C 0.8151(2) 0.64312(10) 1.09622(17) 0.0271(5) Uani 1 1 d . . .
H44C H 0.8220 0.6216 1.1556 0.032 Uiso 1 1 calc R . .
C45C C 0.7359(2) 0.63042(9) 1.02036(18) 0.0269(5) Uani 1 1 d . . .
H45C H 0.6888 0.5996 1.0271 0.032 Uiso 1 1 calc R . .
C46C C 0.72493(19) 0.66257(9) 0.93418(17) 0.0241(5) Uani 1 1 d . . .
H46C H 0.6707 0.6526 0.8827 0.029 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.01753(6) 0.01577(5) 0.01568(5) -0.00034(3) 0.00379(3) -0.00021(3)
N1 0.0212(10) 0.0215(10) 0.0247(9) 0.0072(8) 0.0049(8) 0.0037(8)
N2 0.0225(10) 0.0182(9) 0.0198(9) 0.0027(7) 0.0058(7) 0.0015(7)
C3 0.0185(12) 0.0285(13) 0.0279(12) -0.0003(10) 0.0046(9) 0.0025(9)
C4 0.0229(12) 0.0338(13) 0.0254(12) 0.0032(10) 0.0003(9) 0.0091(10)
C5 0.0282(13) 0.0286(13) 0.0242(11) 0.0083(10) 0.0036(9) 0.0086(10)
C1A 0.0225(12) 0.0199(11) 0.0303(12) 0.0072(9) 0.0030(9) 0.0006(9)
N1' 0.0193(10) 0.0184(10) 0.0229(9) 0.0029(7) 0.0047(7) 0.0014(7)
N2' 0.0214(10) 0.0224(10) 0.0242(9) 0.0040(8) 0.0068(8) 0.0043(8)
N3' 0.0200(10) 0.0195(10) 0.0197(9) 0.0025(7) 0.0035(7) 0.0021(7)
C4' 0.0213(11) 0.0154(11) 0.0210(10) 0.0021(8) 0.0034(8) -0.0020(8)
C5' 0.0221(12) 0.0194(11) 0.0209(11) 0.0048(9) 0.0039(9) -0.0011(9)
C6' 0.0190(11) 0.0149(11) 0.0279(11) -0.0007(9) 0.0023(9) 0.0006(8)
C7' 0.0287(13) 0.0233(12) 0.0246(11) -0.0003(9) 0.0052(10) 0.0012(10)
C8' 0.0331(14) 0.0240(13) 0.0296(12) 0.0001(10) -0.0032(10) 0.0050(10)
C9' 0.0265(13) 0.0285(13) 0.0376(13) -0.0072(11) -0.0015(10) 0.0105(10)
C10' 0.0322(14) 0.0338(14) 0.0321(13) -0.0036(11) 0.0101(11) 0.0102(11)
C11' 0.0300(13) 0.0236(12) 0.0243(11) 0.0010(9) 0.0048(10) 0.0053(10)
C1B 0.0306(13) 0.0247(12) 0.0203(11) -0.0081(9) 0.0057(9) -0.0030(10)
C2B 0.0271(13) 0.0350(14) 0.0232(11) -0.0133(10) 0.0054(9) 0.0074(10)
C3B 0.0316(14) 0.0419(15) 0.0228(12) -0.0148(10) 0.0145(10) -0.0135(11)
C4B 0.0525(17) 0.0285(13) 0.0137(10) -0.0009(9) 0.0053(10) -0.0084(11)
C5B 0.0316(14) 0.0336(13) 0.0170(11) -0.0066(9) -0.0003(9) 0.0016(10)
C6B 0.062(2) 0.0309(15) 0.0437(16) -0.0142(12) 0.0136(14) -0.0201(13)
C7B 0.0485(18) 0.055(2) 0.0521(18) -0.0267(15) -0.0075(14) 0.0274(15)
C8B 0.0455(19) 0.093(3) 0.0469(18) -0.0305(18) 0.0273(15) -0.0395(18)
C9B 0.107(3) 0.0343(17) 0.0284(14) 0.0091(12) 0.0091(16) -0.0080(17)
C10B 0.0411(18) 0.070(2) 0.0438(17) -0.0181(15) -0.0151(14) 0.0137(15)
Cl1 0.0429(3) 0.0175(3) 0.0251(3) -0.0045(2) 0.0078(2) -0.0051(2)
B1C 0.0187(12) 0.0181(12) 0.0204(12) 0.0005(9) -0.0002(9) -0.0015(9)
C11C 0.0147(10) 0.0208(11) 0.0214(10) 0.0001(9) 0.0022(8) -0.0042(8)
C12C 0.0291(13) 0.0252(12) 0.0271(12) -0.0013(10) -0.0052(10) 0.0049(10)
C13C 0.0318(14) 0.0229(12) 0.0368(13) -0.0067(10) -0.0001(11) 0.0066(10)
C14C 0.0256(12) 0.0262(13) 0.0242(11) -0.0085(9) 0.0037(9) -0.0050(9)
C15C 0.0271(13) 0.0288(13) 0.0194(11) 0.0030(9) -0.0006(9) -0.0033(10)
C16C 0.0236(12) 0.0177(11) 0.0223(11) 0.0002(9) 0.0025(9) -0.0016(9)
C21C 0.0205(11) 0.0216(12) 0.0194(10) -0.0044(8) -0.0029(8) -0.0014(9)
C22C 0.0245(12) 0.0268(12) 0.0282(12) -0.0015(10) 0.0027(9) -0.0002(10)
C23C 0.0239(13) 0.0374(14) 0.0335(13) -0.0055(11) 0.0055(10) -0.0017(11)
C24C 0.0240(13) 0.0356(14) 0.0329(13) -0.0130(11) -0.0027(10) 0.0080(10)
C25C 0.0303(14) 0.0236(12) 0.0294(12) -0.0070(10) -0.0067(10) 0.0055(10)
C26C 0.0245(12) 0.0224(12) 0.0244(11) -0.0034(9) -0.0010(9) -0.0015(9)
C31C 0.0217(11) 0.0164(11) 0.0175(10) 0.0038(8) -0.0038(8) 0.0006(8)
C32C 0.0235(12) 0.0222(11) 0.0226(11) 0.0014(9) -0.0010(9) 0.0012(9)
C33C 0.0319(13) 0.0200(12) 0.0290(12) 0.0016(9) -0.0089(10) -0.0043(10)
C34C 0.0241(13) 0.0272(13) 0.0311(12) 0.0110(10) -0.0065(10) -0.0085(10)
C35C 0.0222(12) 0.0328(13) 0.0275(12) 0.0083(10) 0.0026(9) -0.0009(10)
C36C 0.0249(12) 0.0221(12) 0.0233(11) 0.0015(9) 0.0003(9) 0.0000(9)
C41C 0.0200(11) 0.0198(11) 0.0193(10) 0.0004(8) 0.0044(8) 0.0020(8)
C42C 0.0269(12) 0.0168(11) 0.0229(11) -0.0020(9) 0.0025(9) 0.0000(9)
C43C 0.0321(13) 0.0250(12) 0.0216(11) -0.0013(9) -0.0004(9) 0.0063(10)
C44C 0.0335(14) 0.0262(12) 0.0225(11) 0.0051(9) 0.0096(10) 0.0072(10)
C45C 0.0245(12) 0.0211(12) 0.0363(13) 0.0072(10) 0.0125(10) 0.0024(9)
C46C 0.0196(11) 0.0237(12) 0.0289(12) 0.0025(9) 0.0016(9) -0.0004(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 N3' 2.0748(19) . ?
Ir1 N2 2.0929(17) . ?
Ir1 C3B 2.139(2) . ?
Ir1 C4B 2.148(2) . ?
Ir1 C1B 2.158(2) . ?
Ir1 C5B 2.166(2) . ?
Ir1 C2B 2.166(2) . ?
Ir1 Cl1 2.3880(5) . ?
N1 C5 1.350(3) . ?
N1 N2 1.361(2) . ?
N1 C1A 1.455(3) . ?
N2 C3 1.325(3) . ?
C3 C4 1.391(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.494(3) . ?
C1A H1A1 0.9900 . ?
C1A H2A1 0.9900 . ?
N1' N2' 1.342(3) . ?
N1' C5' 1.357(3) . ?
N1' C6' 1.436(3) . ?
N2' N3' 1.316(3) . ?
N3' C4' 1.360(3) . ?
C4' C5' 1.362(3) . ?
C5' H5' 0.9500 . ?
C6' C11' 1.381(3) . ?
C6' C7' 1.384(3) . ?
C7' C8' 1.379(3) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.386(3) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.381(4) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.385(3) . ?
C10' H10' 0.9500 . ?
C11' H11' 0.9500 . ?
C1B C2B 1.439(3) . ?
C1B C5B 1.443(3) . ?
C1B C6B 1.492(3) . ?
C2B C3B 1.421(4) . ?
C2B C7B 1.483(4) . ?
C3B C4B 1.444(4) . ?
C3B C8B 1.499(4) . ?
C4B C5B 1.415(4) . ?
C4B C9B 1.504(4) . ?
C5B C10B 1.492(4) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
C10B H10D 0.9800 . ?
B1C C31C 1.645(3) . ?
B1C C41C 1.648(3) . ?
B1C C11C 1.649(3) . ?
B1C C21C 1.654(3) . ?
C11C C16C 1.398(3) . ?
C11C C12C 1.399(3) . ?
C12C C13C 1.390(3) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.381(3) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.377(3) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.396(3) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C22C 1.397(3) . ?
C21C C26C 1.407(3) . ?
C22C C23C 1.390(3) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.380(4) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.381(4) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.391(3) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C36C 1.396(3) . ?
C31C C32C 1.408(3) . ?
C32C C33C 1.385(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.384(4) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.383(3) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.389(3) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C42C 1.401(3) . ?
C41C C46C 1.406(3) . ?
C42C C43C 1.395(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.384(3) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.383(4) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.392(3) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3' Ir1 N2 83.47(7) . . ?
N3' Ir1 C3B 161.21(9) . . ?
N2 Ir1 C3B 114.90(9) . . ?
N3' Ir1 C4B 122.31(9) . . ?
N2 Ir1 C4B 154.21(9) . . ?
C3B Ir1 C4B 39.37(11) . . ?
N3' Ir1 C1B 105.77(8) . . ?
N2 Ir1 C1B 110.17(8) . . ?
C3B Ir1 C1B 65.45(9) . . ?
C4B Ir1 C1B 65.32(9) . . ?
N3' Ir1 C5B 97.54(9) . . ?
N2 Ir1 C5B 148.39(8) . . ?
C3B Ir1 C5B 64.94(10) . . ?
C4B Ir1 C5B 38.29(10) . . ?
C1B Ir1 C5B 39.00(9) . . ?
N3' Ir1 C2B 141.57(8) . . ?
N2 Ir1 C2B 95.23(8) . . ?
C3B Ir1 C2B 38.53(9) . . ?
C4B Ir1 C2B 64.91(10) . . ?
C1B Ir1 C2B 38.86(9) . . ?
C5B Ir1 C2B 64.55(9) . . ?
N3' Ir1 Cl1 87.64(5) . . ?
N2 Ir1 Cl1 86.08(5) . . ?
C3B Ir1 Cl1 97.08(6) . . ?
C4B Ir1 Cl1 94.70(7) . . ?
C1B Ir1 Cl1 159.68(6) . . ?
C5B Ir1 Cl1 125.51(7) . . ?
C2B Ir1 Cl1 130.71(7) . . ?
C5 N1 N2 110.19(19) . . ?
C5 N1 C1A 128.40(19) . . ?
N2 N1 C1A 121.25(17) . . ?
C3 N2 N1 105.89(17) . . ?
C3 N2 Ir1 128.27(15) . . ?
N1 N2 Ir1 125.81(14) . . ?
N2 C3 C4 110.9(2) . . ?
N2 C3 H3 124.6 . . ?
C4 C3 H3 124.6 . . ?
C5 C4 C3 105.2(2) . . ?
C5 C4 H4 127.4 . . ?
C3 C4 H4 127.4 . . ?
N1 C5 C4 107.8(2) . . ?
N1 C5 H5 126.1 . . ?
C4 C5 H5 126.1 . . ?
N1 C1A C4' 111.94(18) . . ?
N1 C1A H1A1 109.2 . . ?
C4' C1A H1A1 109.2 . . ?
N1 C1A H2A1 109.2 . . ?
C4' C1A H2A1 109.2 . . ?
H1A1 C1A H2A1 107.9 . . ?
N2' N1' C5' 112.07(18) . . ?
N2' N1' C6' 119.54(17) . . ?
C5' N1' C6' 128.25(18) . . ?
N3' N2' N1' 105.17(17) . . ?
N2' N3' C4' 110.71(18) . . ?
N2' N3' Ir1 123.35(14) . . ?
C4' N3' Ir1 125.91(14) . . ?
N3' C4' C5' 107.60(19) . . ?
N3' C4' C1A 121.04(19) . . ?
C5' C4' C1A 131.2(2) . . ?
N1' C5' C4' 104.43(18) . . ?
N1' C5' H5' 127.8 . . ?
C4' C5' H5' 127.8 . . ?
C11' C6' C7' 121.9(2) . . ?
C11' C6' N1' 119.43(19) . . ?
C7' C6' N1' 118.64(19) . . ?
C8' C7' C6' 118.7(2) . . ?
C8' C7' H7' 120.6 . . ?
C6' C7' H7' 120.6 . . ?
C7' C8' C9' 120.5(2) . . ?
C7' C8' H8' 119.8 . . ?
C9' C8' H8' 119.8 . . ?
C10' C9' C8' 119.8(2) . . ?
C10' C9' H9' 120.1 . . ?
C8' C9' H9' 120.1 . . ?
C9' C10' C11' 120.6(2) . . ?
C9' C10' H10' 119.7 . . ?
C11' C10' H10' 119.7 . . ?
C6' C11' C10' 118.4(2) . . ?
C6' C11' H11' 120.8 . . ?
C10' C11' H11' 120.8 . . ?
C2B C1B C5B 106.8(2) . . ?
C2B C1B C6B 126.1(2) . . ?
C5B C1B C6B 126.7(2) . . ?
C2B C1B Ir1 70.86(12) . . ?
C5B C1B Ir1 70.78(12) . . ?
C6B C1B Ir1 129.32(16) . . ?
C3B C2B C1B 108.7(2) . . ?
C3B C2B C7B 125.3(3) . . ?
C1B C2B C7B 126.0(3) . . ?
C3B C2B Ir1 69.70(13) . . ?
C1B C2B Ir1 70.27(12) . . ?
C7B C2B Ir1 124.80(17) . . ?
C2B C3B C4B 107.8(2) . . ?
C2B C3B C8B 127.4(3) . . ?
C4B C3B C8B 124.6(3) . . ?
C2B C3B Ir1 71.77(13) . . ?
C4B C3B Ir1 70.67(13) . . ?
C8B C3B Ir1 126.16(17) . . ?
C5B C4B C3B 107.9(2) . . ?
C5B C4B C9B 125.4(3) . . ?
C3B C4B C9B 126.7(3) . . ?
C5B C4B Ir1 71.52(13) . . ?
C3B C4B Ir1 69.96(13) . . ?
C9B C4B Ir1 125.17(17) . . ?
C4B C5B C1B 108.8(2) . . ?
C4B C5B C10B 126.5(3) . . ?
C1B C5B C10B 124.7(2) . . ?
C4B C5B Ir1 70.19(13) . . ?
C1B C5B Ir1 70.22(13) . . ?
C10B C5B Ir1 125.82(18) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C5B C10B H10D 109.5 . . ?
H10B C10B H10D 109.5 . . ?
H10C C10B H10D 109.5 . . ?
C31C B1C C41C 108.89(17) . . ?
C31C B1C C11C 108.79(17) . . ?
C41C B1C C11C 110.29(18) . . ?
C31C B1C C21C 110.62(17) . . ?
C41C B1C C21C 109.39(17) . . ?
C11C B1C C21C 108.85(17) . . ?
C16C C11C C12C 114.8(2) . . ?
C16C C11C B1C 122.65(19) . . ?
C12C C11C B1C 122.43(19) . . ?
C13C C12C C11C 122.9(2) . . ?
C13C C12C H12C 118.5 . . ?
C11C C12C H12C 118.5 . . ?
C14C C13C C12C 120.3(2) . . ?
C14C C13C H13C 119.9 . . ?
C12C C13C H13C 119.9 . . ?
C15C C14C C13C 118.9(2) . . ?
C15C C14C H14C 120.6 . . ?
C13C C14C H14C 120.6 . . ?
C14C C15C C16C 120.1(2) . . ?
C14C C15C H15C 120.0 . . ?
C16C C15C H15C 120.0 . . ?
C15C C16C C11C 123.0(2) . . ?
C15C C16C H16C 118.5 . . ?
C11C C16C H16C 118.5 . . ?
C22C C21C C26C 114.6(2) . . ?
C22C C21C B1C 123.8(2) . . ?
C26C C21C B1C 121.51(19) . . ?
C23C C22C C21C 123.1(2) . . ?
C23C C22C H22C 118.5 . . ?
C21C C22C H22C 118.5 . . ?
C24C C23C C22C 120.4(2) . . ?
C24C C23C H23C 119.8 . . ?
C22C C23C H23C 119.8 . . ?
C23C C24C C25C 118.8(2) . . ?
C23C C24C H24C 120.6 . . ?
C25C C24C H24C 120.6 . . ?
C24C C25C C26C 120.1(2) . . ?
C24C C25C H25C 120.0 . . ?
C26C C25C H25C 120.0 . . ?
C25C C26C C21C 123.0(2) . . ?
C25C C26C H26C 118.5 . . ?
C21C C26C H26C 118.5 . . ?
C36C C31C C32C 115.0(2) . . ?
C36C C31C B1C 123.23(19) . . ?
C32C C31C B1C 121.73(19) . . ?
C33C C32C C31C 122.5(2) . . ?
C33C C32C H32C 118.7 . . ?
C31C C32C H32C 118.7 . . ?
C34C C33C C32C 120.6(2) . . ?
C34C C33C H33C 119.7 . . ?
C32C C33C H33C 119.7 . . ?
C35C C34C C33C 118.7(2) . . ?
C35C C34C H34C 120.7 . . ?
C33C C34C H34C 120.7 . . ?
C34C C35C C36C 120.1(2) . . ?
C34C C35C H35C 119.9 . . ?
C36C C35C H35C 119.9 . . ?
C35C C36C C31C 123.1(2) . . ?
C35C C36C H36C 118.5 . . ?
C31C C36C H36C 118.5 . . ?
C42C C41C C46C 114.90(19) . . ?
C42C C41C B1C 123.58(19) . . ?
C46C C41C B1C 121.41(19) . . ?
C43C C42C C41C 123.0(2) . . ?
C43C C42C H42C 118.5 . . ?
C41C C42C H42C 118.5 . . ?
C44C C43C C42C 120.0(2) . . ?
C44C C43C H43C 120.0 . . ?
C42C C43C H43C 120.0 . . ?
C45C C44C C43C 119.0(2) . . ?
C45C C44C H44C 120.5 . . ?
C43C C44C H44C 120.5 . . ?
C44C C45C C46C 120.2(2) . . ?
C44C C45C H45C 119.9 . . ?
C46C C45C H45C 119.9 . . ?
C45C C46C C41C 122.8(2) . . ?
C45C C46C H46C 118.6 . . ?
C41C C46C H46C 118.6 . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.669
_refine_diff_density_min -0.619
_refine_diff_density_rms 0.058
_iucr_refine_instructions_details
;
TITL Carol13_P21byn in P2(1)/n
CELL 0.71073 12.0829 24.4058 13.3522 90.000 93.701 90.000
ZERR 4.00 0.0005 0.0010 0.0005 0.000 0.002 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H B N Cl Ir
UNIT 184 184 4 20 4 4
OMIT 2 0 0
OMIT 1 4 0
OMIT 0 0 2
OMIT 1 2 0
OMIT 0 2 1
OMIT 1 0 1
OMIT 1 2 1
OMIT -1 2 1
OMIT -1 0 1
OMIT 0 2 0
OMIT 2 1 0
OMIT 0 1 1
OMIT -1 1 1
OMIT 1 1 0
OMIT 1 1 1
OMIT -2 2 1
OMIT -1 1 2
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.350 0.246 0.213
TEMP -117.110
WGHT 0.014800 3.740400
FVAR 0.09246
MOLE 1
IR1 6 0.772855 0.922999 0.246430 11.00000 0.01753 0.01577 =
0.01568 -0.00034 0.00379 -0.00021
N1 4 0.774408 0.857868 0.445251 11.00000 0.02121 0.02148 =
0.02471 0.00722 0.00491 0.00370
N2 4 0.833333 0.889239 0.383301 11.00000 0.02254 0.01819 =
0.01981 0.00272 0.00581 0.00145
C3 1 0.935188 0.892049 0.426225 11.00000 0.01852 0.02853 =
0.02789 -0.00032 0.00460 0.00245
AFIX 43
H3 2 0.994471 0.911808 0.399824 11.00000 -1.20000
AFIX 0
C4 1 0.943625 0.862186 0.515110 11.00000 0.02292 0.03380 =
0.02538 0.00316 0.00034 0.00909
AFIX 43
H4 2 1.007570 0.857537 0.559532 11.00000 -1.20000
AFIX 0
C5 1 0.840262 0.840975 0.524835 11.00000 0.02819 0.02855 =
0.02425 0.00835 0.00362 0.00858
AFIX 43
H5 2 0.818576 0.818373 0.578084 11.00000 -1.20000
AFIX 0
C1A 1 0.659330 0.843412 0.418962 11.00000 0.02255 0.01989 =
0.03028 0.00716 0.00305 0.00064
AFIX 23
H1A1 2 0.627381 0.825934 0.477466 11.00000 -1.20000
H2A1 2 0.656384 0.816460 0.363441 11.00000 -1.20000
AFIX 0
N1' 4 0.465934 0.953250 0.354058 11.00000 0.01934 0.01837 =
0.02288 0.00287 0.00471 0.00138
N2' 4 0.549429 0.965485 0.296368 11.00000 0.02142 0.02240 =
0.02415 0.00402 0.00682 0.00427
N3' 4 0.625223 0.927712 0.317158 11.00000 0.02002 0.01952 =
0.01970 0.00249 0.00354 0.00205
C4' 1 0.591277 0.892346 0.387691 11.00000 0.02132 0.01537 =
0.02096 0.00206 0.00341 -0.00200
C5' 1 0.488646 0.908550 0.412252 11.00000 0.02213 0.01939 =
0.02089 0.00479 0.00388 -0.00113
AFIX 43
H5' 2 0.443190 0.892240 0.459480 11.00000 -1.20000
AFIX 0
C6' 1 0.365047 0.984445 0.343941 11.00000 0.01899 0.01490 =
0.02794 -0.00069 0.00233 0.00060
C7' 1 0.330972 1.005092 0.250478 11.00000 0.02869 0.02334 =
0.02461 -0.00035 0.00523 0.00115
AFIX 43
H7' 2 0.374760 0.999820 0.194677 11.00000 -1.20000
AFIX 0
C8' 1 0.232248 1.033461 0.239897 11.00000 0.03305 0.02401 =
0.02960 0.00007 -0.00321 0.00501
AFIX 43
H8' 2 0.208458 1.048589 0.176570 11.00000 -1.20000
AFIX 0
C9' 1 0.167446 1.040070 0.321019 11.00000 0.02652 0.02848 =
0.03758 -0.00716 -0.00145 0.01050
AFIX 43
H9' 2 0.098513 1.058784 0.312853 11.00000 -1.20000
AFIX 0
C10' 1 0.203404 1.019362 0.413762 11.00000 0.03215 0.03378 =
0.03212 -0.00359 0.01013 0.01021
AFIX 43
H10' 2 0.159029 1.024067 0.469328 11.00000 -1.20000
AFIX 0
C11' 1 0.303517 0.991808 0.426521 11.00000 0.03004 0.02362 =
0.02433 0.00100 0.00478 0.00531
AFIX 43
H11' 2 0.329249 0.978293 0.490570 11.00000 -1.20000
AFIX 0
C1B 1 0.748573 0.859476 0.134744 11.00000 0.03063 0.02469 =
0.02030 -0.00814 0.00574 -0.00305
C2B 1 0.865516 0.868819 0.154357 11.00000 0.02712 0.03503 =
0.02319 -0.01328 0.00541 0.00743
C3B 1 0.888960 0.924385 0.132152 11.00000 0.03163 0.04189 =
0.02283 -0.01481 0.01449 -0.01354
C4B 1 0.786723 0.949875 0.094555 11.00000 0.05253 0.02846 =
0.01373 -0.00091 0.00532 -0.00845
C5B 1 0.701715 0.910034 0.095253 11.00000 0.03156 0.03357 =
0.01705 -0.00662 -0.00033 0.00164
C6B 1 0.690437 0.805792 0.141337 11.00000 0.06224 0.03089 =
0.04367 -0.01423 0.01356 -0.02009
AFIX 137
H6B1 2 0.691231 0.786743 0.076776 11.00000 -1.50000
H6B2 2 0.613548 0.812037 0.157716 11.00000 -1.50000
H6B3 2 0.728342 0.783333 0.193850 11.00000 -1.50000
AFIX 0
C7B 1 0.948056 0.827902 0.193647 11.00000 0.04847 0.05515 =
0.05212 -0.02667 -0.00751 0.02739
AFIX 137
H7B1 2 0.975865 0.807183 0.137634 11.00000 -1.50000
H7B2 2 0.912934 0.802725 0.239168 11.00000 -1.50000
H7B3 2 1.009911 0.846761 0.230103 11.00000 -1.50000
AFIX 0
C8B 1 0.999947 0.952071 0.138841 11.00000 0.04548 0.09339 =
0.04695 -0.03050 0.02735 -0.03954
AFIX 137
H8B1 2 1.052126 0.930621 0.182256 11.00000 -1.50000
H8B2 2 0.992617 0.988877 0.167000 11.00000 -1.50000
H8B3 2 1.027651 0.954814 0.071641 11.00000 -1.50000
AFIX 0
C9B 1 0.772019 1.007946 0.058381 11.00000 0.10692 0.03428 =
0.02841 0.00910 0.00906 -0.00796
AFIX 137
H9B1 2 0.784693 1.009751 -0.013302 11.00000 -1.50000
H9B2 2 0.825341 1.031705 0.095879 11.00000 -1.50000
H9B3 2 0.696441 1.020215 0.068996 11.00000 -1.50000
AFIX 0
C10B 1 0.582879 0.917879 0.060766 11.00000 0.04111 0.06955 =
0.04377 -0.01808 -0.01509 0.01365
AFIX 137
H10B 2 0.562041 0.956255 0.070149 11.00000 -1.50000
H10C 2 0.536370 0.894244 0.099963 11.00000 -1.50000
H10D 2 0.572153 0.908290 -0.010472 11.00000 -1.50000
AFIX 0
CL1 5 0.820874 1.009841 0.319291 11.00000 0.04291 0.01754 =
0.02512 -0.00450 0.00779 -0.00509
MOLE 2
B1C 3 0.766932 0.749739 0.822478 11.00000 0.01866 0.01813 =
0.02038 0.00055 -0.00018 -0.00155
C11C 1 0.749879 0.713296 0.718626 11.00000 0.01472 0.02075 =
0.02143 0.00005 0.00223 -0.00418
C12C 1 0.801971 0.662692 0.707046 11.00000 0.02908 0.02518 =
0.02711 -0.00134 -0.00522 0.00491
AFIX 43
H12C 2 0.846161 0.648172 0.762214 11.00000 -1.20000
AFIX 0
C13C 1 0.791922 0.632722 0.618386 11.00000 0.03182 0.02294 =
0.03676 -0.00671 -0.00008 0.00656
AFIX 43
H13C 2 0.828248 0.598347 0.614338 11.00000 -1.20000
AFIX 0
C14C 1 0.729385 0.652697 0.536196 11.00000 0.02564 0.02617 =
0.02419 -0.00847 0.00369 -0.00503
AFIX 43
H14C 2 0.722536 0.632409 0.475390 11.00000 -1.20000
AFIX 0
C15C 1 0.677105 0.702512 0.543822 11.00000 0.02709 0.02884 =
0.01938 0.00305 -0.00061 -0.00326
AFIX 43
H15C 2 0.634122 0.716948 0.487839 11.00000 -1.20000
AFIX 0
C16C 1 0.687184 0.731826 0.633706 11.00000 0.02364 0.01771 =
0.02226 0.00019 0.00254 -0.00156
AFIX 43
H16C 2 0.649724 0.765923 0.637323 11.00000 -1.20000
AFIX 0
C21C 1 0.653045 0.785717 0.836676 11.00000 0.02052 0.02162 =
0.01939 -0.00444 -0.00291 -0.00136
C22C 1 0.565565 0.767635 0.891671 11.00000 0.02446 0.02679 =
0.02821 -0.00145 0.00273 -0.00019
AFIX 43
H22C 2 0.573650 0.733891 0.926853 11.00000 -1.20000
AFIX 0
C23C 1 0.467219 0.796714 0.897324 11.00000 0.02385 0.03741 =
0.03352 -0.00553 0.00548 -0.00168
AFIX 43
H23C 2 0.410061 0.782558 0.935561 11.00000 -1.20000
AFIX 0
C24C 1 0.452147 0.846018 0.847717 11.00000 0.02398 0.03557 =
0.03295 -0.01298 -0.00275 0.00804
AFIX 43
H24C 2 0.384920 0.865908 0.851195 11.00000 -1.20000
AFIX 0
C25C 1 0.536532 0.865934 0.792922 11.00000 0.03033 0.02362 =
0.02941 -0.00696 -0.00672 0.00552
AFIX 43
H25C 2 0.527625 0.899835 0.758376 11.00000 -1.20000
AFIX 0
C26C 1 0.634574 0.836409 0.788251 11.00000 0.02447 0.02245 =
0.02443 -0.00338 -0.00101 -0.00149
AFIX 43
H26C 2 0.691673 0.851154 0.750634 11.00000 -1.20000
AFIX 0
C31C 1 0.874199 0.790543 0.813582 11.00000 0.02166 0.01635 =
0.01754 0.00377 -0.00375 0.00063
C32C 1 0.888498 0.837993 0.872982 11.00000 0.02351 0.02216 =
0.02258 0.00140 -0.00100 0.00124
AFIX 43
H32C 2 0.833408 0.847018 0.917880 11.00000 -1.20000
AFIX 0
C33C 1 0.979760 0.872017 0.868489 11.00000 0.03187 0.02004 =
0.02899 0.00161 -0.00886 -0.00434
AFIX 43
H33C 2 0.985851 0.903737 0.909713 11.00000 -1.20000
AFIX 0
C34C 1 1.062146 0.860212 0.804480 11.00000 0.02409 0.02725 =
0.03114 0.01103 -0.00652 -0.00848
AFIX 43
H34C 2 1.124042 0.883916 0.800306 11.00000 -1.20000
AFIX 0
C35C 1 1.052597 0.813222 0.746704 11.00000 0.02218 0.03281 =
0.02747 0.00828 0.00260 -0.00086
AFIX 43
H35C 2 1.109374 0.803837 0.703771 11.00000 -1.20000
AFIX 0
C36C 1 0.960121 0.779712 0.751328 11.00000 0.02492 0.02209 =
0.02326 0.00146 0.00028 -0.00003
AFIX 43
H36C 2 0.955102 0.747932 0.710202 11.00000 -1.20000
AFIX 0
C41C 1 0.790623 0.709128 0.920110 11.00000 0.02004 0.01979 =
0.01926 0.00039 0.00438 0.00195
C42C 1 0.871570 0.719525 0.997636 11.00000 0.02692 0.01683 =
0.02289 -0.00198 0.00252 0.00002
AFIX 43
H42C 2 0.920201 0.749699 0.990896 11.00000 -1.20000
AFIX 0
C43C 1 0.884051 0.687602 1.084295 11.00000 0.03206 0.02502 =
0.02158 -0.00133 -0.00040 0.00625
AFIX 43
H43C 2 0.939885 0.696392 1.135116 11.00000 -1.20000
AFIX 0
C44C 1 0.815071 0.643119 1.096218 11.00000 0.03348 0.02624 =
0.02251 0.00511 0.00957 0.00724
AFIX 43
H44C 2 0.822023 0.621634 1.155621 11.00000 -1.20000
AFIX 0
C45C 1 0.735878 0.630418 1.020361 11.00000 0.02454 0.02110 =
0.03631 0.00716 0.01248 0.00240
AFIX 43
H45C 2 0.688787 0.599644 1.027089 11.00000 -1.20000
AFIX 0
C46C 1 0.724928 0.662571 0.934181 11.00000 0.01964 0.02368 =
0.02888 0.00247 0.00160 -0.00040
AFIX 43
H46C 2 0.670739 0.652623 0.882675 11.00000 -1.20000
HKLF 4
REM Carol13_P21byn in P2(1)/n
REM R1 = 0.0167 for 6549 Fo > 4sig(Fo) and 0.0182 for all 6884 data
REM 492 parameters refined using 0 restraints
END
WGHT 0.0148 3.7414
REM Highest difference peak 0.669, deepest hole -0.619, 1-sigma level 0.058
Q1 1 0.7037 0.9057 0.2180 11.00000 0.05 0.67
Q2 1 0.8574 0.9227 0.2415 11.00000 0.05 0.62
Q3 1 0.8226 0.8977 0.2745 11.00000 0.05 0.59
Q4 1 0.7012 0.9395 0.2157 11.00000 0.05 0.54
Q5 1 0.8389 0.9373 0.2742 11.00000 0.05 0.51
Q6 1 0.7071 0.9055 0.2747 11.00000 0.05 0.39
Q7 1 0.8566 1.0011 0.0674 11.00000 0.05 0.36
Q8 1 1.0252 0.9176 0.1711 11.00000 0.05 0.34
Q9 1 0.7101 0.9266 0.2984 11.00000 0.05 0.34
Q10 1 0.7614 0.7305 0.7655 11.00000 0.05 0.31
Q11 1 0.7136 0.7697 0.8327 11.00000 0.05 0.28
Q12 1 0.4095 0.9686 0.3455 11.00000 0.05 0.27
Q13 1 0.8258 0.7700 0.8138 11.00000 0.05 0.27
Q14 1 1.0585 0.9304 0.0946 11.00000 0.05 0.27
Q15 1 0.8999 0.8016 0.2159 11.00000 0.05 0.26
Q16 1 0.8780 0.8120 0.8409 11.00000 0.05 0.26
Q17 1 0.8164 0.8631 0.1177 11.00000 0.05 0.25
Q18 1 0.7220 0.8454 0.4270 11.00000 0.05 0.25
Q19 1 0.8382 0.9296 0.0878 11.00000 0.05 0.25
Q20 1 0.5588 0.9044 0.4253 11.00000 0.05 0.25
;
#===END
data_chinmin1_c2byc
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'(C32 H12 B F23.97), (C17 H23 Cl Ir N4), 0.375(C Cl2)'
_chemical_formula_sum
'C49.38 H35 B Cl1.75 F24 Ir N4'
_chemical_formula_weight 1405.36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Ir' 'Ir' -1.4442 7.9887
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 28.8655(12)
_cell_length_b 12.9022(5)
_cell_length_c 29.8343(12)
_cell_angle_alpha 90.00
_cell_angle_beta 104.7220(10)
_cell_angle_gamma 90.00
_cell_volume 10746.4(7)
_cell_formula_units_Z 8
_cell_measurement_temperature 155(2)
_cell_measurement_reflns_used 9566
_cell_measurement_theta_min 2.354
_cell_measurement_theta_max 30.458
_exptl_crystal_description ?
_exptl_crystal_colour ?
_exptl_crystal_size_max 0.36
_exptl_crystal_size_mid 0.26
_exptl_crystal_size_min 0.18
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.737
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5496
_exptl_absorpt_coefficient_mu 2.695
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.4404
_exptl_absorpt_correction_T_max 0.6484
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 155(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 38085
_diffrn_reflns_av_R_equivalents 0.0230
_diffrn_reflns_av_sigmaI/netI 0.0186
_diffrn_reflns_limit_h_min -32
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_theta_min 2.59
_diffrn_reflns_theta_max 25.00
_reflns_number_total 9435
_reflns_number_gt 8380
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The CF3 groups of the anion exhibited extensive rotational disorder over
two and (in some cases) three positions. The solvent dichloromethane (DCM)
also showed orientational disorder over several positions. Modelling these
disorders was handled using SADI (0.01) to keep the C-F bond distances
similar and also the F...F distances to be same. The DELU and SIMU
restraints were used to keep the atomic displacement paramters similar
and within reasonable limits. The same strategy was applied to DCM as well.
A single alert at level A arises due to this structural feature (CF3
disorder).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9435
_refine_ls_number_parameters 962
_refine_ls_number_restraints 341
_refine_ls_R_factor_all 0.0374
_refine_ls_R_factor_gt 0.0310
_refine_ls_wR_factor_ref 0.1323
_refine_ls_wR_factor_gt 0.1203
_refine_ls_goodness_of_fit_ref 1.182
_refine_ls_restrained_S_all 1.245
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1D C 0.4920(7) 0.015(2) 0.5188(10) 0.081(8) Uiso 0.25 1 d PDU . -1
Cl1D Cl 0.5433(5) 0.0274(13) 0.5039(6) 0.127(5) Uiso 0.25 1 d PDU . -1
Cl2D Cl 0.4493(5) -0.0710(11) 0.4997(5) 0.111(4) Uiso 0.25 1 d PDU . -1
Ir1 Ir 0.747758(5) 0.125787(13) 0.696814(5) 0.02397(11) Uani 1 1 d . . .
N1 N 0.83300(17) 0.1281(3) 0.78149(16) 0.0385(11) Uani 1 1 d . . .
N2 N 0.81421(13) 0.1712(3) 0.73977(12) 0.0319(8) Uani 1 1 d . . .
C3 C 0.84600(16) 0.2417(4) 0.73374(17) 0.0398(11) Uani 1 1 d . . .
H3 H 0.8426 0.2849 0.7073 0.048 Uiso 1 1 calc R . .
C4 C 0.88490(18) 0.2416(4) 0.7726(2) 0.0521(15) Uani 1 1 d . . .
H4 H 0.9124 0.2849 0.7774 0.063 Uiso 1 1 calc R . .
C5 C 0.87666(17) 0.1700(4) 0.80193(19) 0.0452(13) Uani 1 1 d . . .
H5 H 0.8971 0.1518 0.8312 0.054 Uiso 1 1 calc R . .
C1A C 0.80941(18) 0.0415(4) 0.79706(16) 0.0423(12) Uani 1 1 d . . .
H1A1 H 0.8079 -0.0176 0.7756 0.051 Uiso 1 1 calc R . .
H1A2 H 0.8280 0.0196 0.8282 0.051 Uiso 1 1 calc R . .
N1' N 0.76191(17) 0.0700(3) 0.79879(12) 0.0420(10) Uani 1 1 d . . .
N2' N 0.72928(16) 0.1037(3) 0.75946(14) 0.0363(9) Uani 1 1 d . . .
C3' C 0.6877(2) 0.1137(4) 0.7707(2) 0.0476(15) Uani 1 1 d . . .
H3' H 0.6588 0.1381 0.7505 0.057 Uiso 1 1 calc R . .
C4' C 0.6927(3) 0.0835(5) 0.8163(2) 0.0637(18) Uani 1 1 d . . .
H4' H 0.6682 0.0815 0.8325 0.076 Uiso 1 1 calc R . .
C5' C 0.7393(2) 0.0572(4) 0.83338(19) 0.0552(15) Uani 1 1 d . . .
H5' H 0.7537 0.0340 0.8640 0.066 Uiso 1 1 calc R . .
C1B C 0.77338(14) 0.0695(4) 0.63927(14) 0.0291(9) Uani 1 1 d . . .
C2B C 0.73043(17) 0.1251(3) 0.62167(16) 0.0295(10) Uani 1 1 d . . .
C3B C 0.69285(15) 0.0752(3) 0.63819(14) 0.0296(9) Uani 1 1 d . . .
C4B C 0.71360(15) -0.0135(3) 0.66450(14) 0.0279(9) Uani 1 1 d . . .
C5B C 0.76377(14) -0.0165(3) 0.66721(13) 0.0287(9) Uani 1 1 d . . .
C6B C 0.82173(18) 0.0925(5) 0.63163(19) 0.0422(12) Uani 1 1 d . . .
H6B1 H 0.8276 0.0463 0.6076 0.063 Uiso 1 1 calc R . .
H6B2 H 0.8464 0.0814 0.6606 0.063 Uiso 1 1 calc R . .
H6B3 H 0.8227 0.1647 0.6218 0.063 Uiso 1 1 calc R . .
C7B C 0.72359(19) 0.2173(4) 0.59040(17) 0.0451(12) Uani 1 1 d . . .
H7B1 H 0.7538 0.2558 0.5956 0.068 Uiso 1 1 calc R . .
H7B2 H 0.6988 0.2623 0.5970 0.068 Uiso 1 1 calc R . .
H7B3 H 0.7137 0.1944 0.5580 0.068 Uiso 1 1 calc R . .
C8B C 0.64080(19) 0.1063(5) 0.6255(2) 0.0510(15) Uani 1 1 d . . .
H8B1 H 0.6259 0.0854 0.5935 0.076 Uiso 1 1 calc R . .
H8B2 H 0.6383 0.1817 0.6283 0.076 Uiso 1 1 calc R . .
H8B3 H 0.6244 0.0722 0.6465 0.076 Uiso 1 1 calc R . .
C9B C 0.68662(18) -0.0890(4) 0.68670(17) 0.0375(10) Uani 1 1 d . . .
H9B1 H 0.6717 -0.1419 0.6640 0.056 Uiso 1 1 calc R . .
H9B2 H 0.6618 -0.0521 0.6974 0.056 Uiso 1 1 calc R . .
H9B3 H 0.7088 -0.1223 0.7131 0.056 Uiso 1 1 calc R . .
C10B C 0.7984(2) -0.0992(4) 0.68843(17) 0.0449(13) Uani 1 1 d . . .
H10A H 0.7864 -0.1364 0.7118 0.067 Uiso 1 1 calc R . .
H10B H 0.8295 -0.0678 0.7031 0.067 Uiso 1 1 calc R . .
H10C H 0.8021 -0.1478 0.6643 0.067 Uiso 1 1 calc R . .
Cl1 Cl 0.72435(5) 0.30241(9) 0.70038(4) 0.0434(3) Uani 1 1 d . . .
B1C B 0.58965(17) 0.7033(4) 0.40613(16) 0.0274(10) Uani 1 1 d . . .
C11C C 0.64405(17) 0.6653(3) 0.43188(14) 0.0296(10) Uani 1 1 d . . .
C12C C 0.68611(15) 0.7059(3) 0.42299(14) 0.0295(9) Uani 1 1 d . . .
H12C H 0.6836 0.7648 0.4034 0.035 Uiso 1 1 calc R . .
C13C C 0.73054(16) 0.6639(4) 0.44139(15) 0.0340(10) Uani 1 1 d . A .
C14C C 0.73633(17) 0.5760(4) 0.46934(15) 0.0377(11) Uani 1 1 d . . .
H14C H 0.7671 0.5466 0.4818 0.045 Uiso 1 1 calc R . .
C15C C 0.69524(16) 0.5326(4) 0.47847(15) 0.0369(11) Uani 1 1 d . . .
C16C C 0.65135(17) 0.5773(4) 0.46082(14) 0.0330(10) Uani 1 1 d . . .
H16C H 0.6243 0.5472 0.4685 0.040 Uiso 1 1 calc R . .
C17C C 0.6995(2) 0.4362(5) 0.50736(18) 0.0507(14) Uani 1 1 d . . .
C18C C 0.77452(17) 0.7109(4) 0.43265(16) 0.0491(9) Uani 1 1 d DU . .
F181 F 0.7660(5) 0.7233(9) 0.3827(4) 0.0470(13) Uani 0.33 1 d PDU A 1
F182 F 0.8145(3) 0.6583(9) 0.4455(4) 0.0532(13) Uani 0.33 1 d PDU A 1
F183 F 0.7819(4) 0.8126(9) 0.4465(4) 0.0502(13) Uani 0.33 1 d PDU A 1
F184 F 0.7705(5) 0.7540(10) 0.3918(4) 0.061(2) Uani 0.33 1 d PDU A 2
F185 F 0.8042(4) 0.6329(7) 0.4249(4) 0.050(2) Uani 0.33 1 d PDU A 2
F186 F 0.8007(4) 0.7677(12) 0.4653(4) 0.057(2) Uani 0.33 1 d PDU A 2
F187 F 0.7832(4) 0.6897(11) 0.3943(4) 0.056(2) Uani 0.33 1 d PDU A 3
F188 F 0.8115(3) 0.7077(9) 0.4699(3) 0.0431(19) Uani 0.33 1 d PDU A 3
F189 F 0.7679(3) 0.8161(7) 0.4273(4) 0.051(2) Uani 0.33 1 d PDU A 3
F171 F 0.66153(18) 0.3737(2) 0.49421(17) 0.0810(13) Uani 1 1 d . . .
F172 F 0.73474(16) 0.3756(3) 0.50356(19) 0.0873(15) Uani 1 1 d . . .
F173 F 0.7009(2) 0.4548(3) 0.55024(12) 0.1007(17) Uani 1 1 d . . .
C21C C 0.55466(17) 0.6854(3) 0.44086(16) 0.0364(10) Uani 1 1 d DU . .
C22C C 0.5715(2) 0.7143(4) 0.48794(18) 0.0575(14) Uani 1 1 d DU . .
H22C H 0.6032 0.7393 0.4994 0.069 Uiso 1 1 calc R . .
C23C C 0.5413(3) 0.7059(6) 0.5172(2) 0.0836(18) Uani 1 1 d DU B .
C24C C 0.4947(3) 0.6686(7) 0.5027(3) 0.0857(18) Uani 1 1 d DU . .
H24C H 0.4751 0.6620 0.5238 0.103 Uiso 1 1 calc R . .
C25C C 0.4776(3) 0.6411(5) 0.4560(3) 0.0748(18) Uani 1 1 d DU C .
C26C C 0.5073(2) 0.6503(5) 0.4256(2) 0.0482(12) Uani 1 1 d DU . .
H26C H 0.4950 0.6324 0.3939 0.058 Uiso 1 1 calc R . .
C27C C 0.5598(4) 0.7398(10) 0.5677(3) 0.119(3) Uani 1 1 d DU . .
C28C C 0.4264(3) 0.6008(9) 0.4363(4) 0.101(3) Uani 1 1 d DU . .
F271 F 0.6117(3) 0.6981(8) 0.5878(3) 0.074(3) Uani 0.50 1 d PDU B 1
F272 F 0.5433(4) 0.7359(11) 0.5986(3) 0.105(3) Uani 0.50 1 d PDU B 1
F273 F 0.5823(4) 0.8492(8) 0.5718(3) 0.107(3) Uani 0.50 1 d PDU B 1
F274 F 0.5404(5) 0.6368(9) 0.5917(4) 0.126(5) Uani 0.50 1 d PDU B 2
F275 F 0.5233(4) 0.7920(10) 0.5774(4) 0.128(4) Uani 0.50 1 d PDU B 2
F276 F 0.5919(5) 0.7380(12) 0.5798(4) 0.115(4) Uani 0.50 1 d PDU B 2
F281 F 0.4084(5) 0.5211(13) 0.4601(6) 0.074(4) Uani 0.50 1 d P C 1
F282 F 0.3922(7) 0.6598(17) 0.4228(9) 0.127(10) Uani 0.50 1 d P C 1
F283 F 0.4268(7) 0.5199(15) 0.4024(9) 0.151(7) Uani 0.50 1 d P C 1
F284 F 0.4222(6) 0.5451(16) 0.4692(10) 0.119(8) Uani 0.50 1 d P C 2
F285 F 0.4001(6) 0.6959(15) 0.4495(7) 0.107(6) Uani 0.50 1 d P C 2
F286 F 0.4137(5) 0.593(2) 0.3953(6) 0.131(8) Uani 0.50 1 d P C 2
C31C C 0.58344(15) 0.8271(3) 0.39384(14) 0.0289(9) Uani 1 1 d D . .
C32C C 0.61457(18) 0.9046(4) 0.41683(17) 0.0443(12) Uani 1 1 d D . .
H32C H 0.6433 0.8852 0.4387 0.053 Uiso 1 1 calc R . .
C33C C 0.60433(19) 1.0103(4) 0.4083(2) 0.0601(17) Uani 1 1 d D D .
C34C C 0.5626(2) 1.0411(4) 0.3770(2) 0.0548(15) Uani 1 1 d D . .
H34C H 0.5556 1.1126 0.3713 0.066 Uiso 1 1 calc R . .
C35C C 0.53118(16) 0.9665(4) 0.35425(16) 0.0357(10) Uani 1 1 d D E .
C36C C 0.54165(18) 0.8626(3) 0.36249(16) 0.0299(10) Uani 1 1 d D . .
H36C H 0.5194 0.8128 0.3461 0.036 Uiso 1 1 calc R . .
C37C C 0.6396(4) 1.0884(6) 0.4334(4) 0.119(5) Uani 1 1 d D . .
C38C C 0.48496(19) 0.9999(4) 0.32168(19) 0.0488(13) Uani 1 1 d D . .
F371 F 0.6570(12) 1.054(3) 0.4780(10) 0.097(6) Uani 0.50 1 d PDU D 1
F372 F 0.6092(4) 1.1743(8) 0.4477(5) 0.123(5) Uani 0.50 1 d PDU D 1
F373 F 0.6633(5) 1.1253(11) 0.4156(6) 0.122(4) Uani 0.50 1 d PDU D 1
F374 F 0.6612(12) 1.075(3) 0.4762(10) 0.086(5) Uani 0.50 1 d PDU D 2
F375 F 0.6322(5) 1.1823(9) 0.4219(5) 0.109(4) Uani 0.50 1 d PDU D 2
F376 F 0.6857(3) 1.0737(9) 0.4142(4) 0.100(3) Uani 0.50 1 d PDU D 2
F381 F 0.4865(9) 1.077(2) 0.2938(8) 0.067(5) Uani 0.50 1 d PU E 1
F382 F 0.4546(6) 1.0449(10) 0.3479(6) 0.079(4) Uani 0.50 1 d PU E 1
F383 F 0.4564(3) 0.9296(12) 0.2979(7) 0.093(5) Uani 0.50 1 d PU E 1
F384 F 0.4892(9) 1.0907(17) 0.3054(8) 0.081(6) Uani 0.50 1 d PU E 2
F385 F 0.4506(6) 0.9961(12) 0.3384(6) 0.097(5) Uani 0.50 1 d PU E 2
F386 F 0.4760(4) 0.9352(13) 0.2856(6) 0.093(5) Uani 0.50 1 d PU E 2
C41C C 0.57484(15) 0.6313(3) 0.35986(16) 0.0265(10) Uani 1 1 d . . .
C42C C 0.57892(13) 0.6643(3) 0.31649(14) 0.0249(8) Uani 1 1 d . . .
H42C H 0.5876 0.7343 0.3128 0.030 Uiso 1 1 calc R . .
C43C C 0.57061(15) 0.5975(4) 0.27798(15) 0.0282(9) Uani 1 1 d . F .
C44C C 0.55758(14) 0.4959(4) 0.28141(16) 0.0312(10) Uani 1 1 d . . .
H44C H 0.5514 0.4512 0.2552 0.037 Uiso 1 1 calc R . .
C45C C 0.55364(14) 0.4601(3) 0.32469(16) 0.0285(10) Uani 1 1 d . G .
C46C C 0.56217(14) 0.5266(3) 0.36250(15) 0.0294(9) Uani 1 1 d . . .
H46C H 0.5593 0.5002 0.3914 0.035 Uiso 1 1 calc R . .
C47C C 0.57482(17) 0.6373(3) 0.23224(17) 0.0341(11) Uani 1 1 d . . .
C48C C 0.53922(19) 0.3514(4) 0.3298(2) 0.0421(12) Uani 1 1 d . . .
F471 F 0.5986(6) 0.7316(9) 0.2350(5) 0.058(4) Uani 0.50 1 d PU F 1
F472 F 0.5351(7) 0.6489(16) 0.2015(8) 0.076(5) Uani 0.50 1 d PU F 1
F473 F 0.6024(3) 0.5775(10) 0.2135(3) 0.059(3) Uani 0.50 1 d PU F 1
F474 F 0.6107(6) 0.6916(12) 0.2341(6) 0.085(5) Uani 0.50 1 d PU F 2
F475 F 0.5372(7) 0.6869(15) 0.2105(7) 0.081(6) Uani 0.50 1 d PU F 2
F476 F 0.5763(5) 0.5620(10) 0.2031(4) 0.094(4) Uani 0.50 1 d PU F 2
F481 F 0.5486(6) 0.3219(14) 0.3767(5) 0.058(3) Uani 0.50 1 d PU G 1
F482 F 0.4930(5) 0.3355(14) 0.3144(5) 0.075(5) Uani 0.50 1 d PU G 1
F483 F 0.5638(4) 0.2834(10) 0.3132(6) 0.072(4) Uani 0.50 1 d PU G 1
F484 F 0.5613(6) 0.3081(15) 0.3665(6) 0.102(6) Uani 0.50 1 d PU G 2
F485 F 0.4951(5) 0.3408(15) 0.3276(6) 0.074(4) Uani 0.50 1 d PU G 2
F486 F 0.5415(7) 0.2944(12) 0.2935(7) 0.121(6) Uani 0.50 1 d PU G 2
C1E C 0.5332(13) 0.032(3) 0.4793(13) 0.027(7) Uiso 0.13 1 d P . .
Cl1E Cl 0.5205(6) 0.0589(13) 0.5374(5) 0.156(5) Uiso 0.25 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ir1 0.02353(15) 0.02255(15) 0.02582(15) -0.00100(5) 0.00623(9) 0.00005(5)
N1 0.041(3) 0.033(2) 0.034(2) -0.0111(15) -0.004(2) 0.0009(16)
N2 0.032(2) 0.028(2) 0.034(2) -0.0089(16) 0.0047(16) 0.0001(16)
C3 0.033(2) 0.037(3) 0.051(3) -0.016(2) 0.014(2) -0.011(2)
C4 0.033(3) 0.047(3) 0.069(4) -0.033(3) 0.000(2) -0.004(2)
C5 0.033(3) 0.039(3) 0.052(3) -0.018(3) -0.010(2) 0.003(2)
C1A 0.054(3) 0.036(3) 0.029(2) 0.0011(19) -0.004(2) 0.008(2)
N1' 0.069(3) 0.030(2) 0.027(2) -0.0014(16) 0.011(2) 0.001(2)
N2' 0.043(2) 0.032(2) 0.037(2) -0.0044(17) 0.0148(19) -0.0025(18)
C3' 0.051(4) 0.041(3) 0.062(4) -0.008(2) 0.035(3) -0.001(2)
C4' 0.102(6) 0.049(4) 0.063(4) -0.006(3) 0.062(4) -0.007(4)
C5' 0.086(5) 0.048(3) 0.037(3) -0.006(2) 0.024(3) -0.005(3)
C1B 0.024(2) 0.037(3) 0.025(2) -0.0075(18) 0.0035(16) -0.0055(19)
C2B 0.027(2) 0.031(3) 0.027(2) 0.0004(15) 0.0011(19) 0.0002(16)
C3B 0.027(2) 0.033(2) 0.026(2) 0.0012(17) 0.0001(16) -0.0014(19)
C4B 0.031(2) 0.024(2) 0.027(2) -0.0001(17) 0.0044(17) -0.0061(18)
C5B 0.029(2) 0.031(2) 0.0225(19) -0.0103(17) 0.0010(16) 0.0029(18)
C6B 0.031(3) 0.061(3) 0.039(3) -0.011(3) 0.017(2) -0.010(3)
C7B 0.046(3) 0.045(3) 0.043(3) 0.012(2) 0.008(2) -0.004(2)
C8B 0.031(3) 0.062(3) 0.057(4) 0.018(3) 0.004(3) 0.006(2)
C9B 0.041(3) 0.032(2) 0.040(3) 0.001(2) 0.011(2) -0.009(2)
C10B 0.060(4) 0.039(3) 0.032(3) -0.007(2) 0.005(2) 0.023(3)
Cl1 0.0539(7) 0.0286(6) 0.0475(7) -0.0011(5) 0.0123(6) 0.0116(5)
B1C 0.032(2) 0.023(2) 0.027(2) -0.0003(19) 0.0063(19) 0.000(2)
C11C 0.043(3) 0.023(2) 0.020(2) -0.0047(17) 0.0035(18) 0.003(2)
C12C 0.036(2) 0.029(2) 0.0215(19) 0.0015(16) 0.0043(17) 0.0011(19)
C13C 0.036(2) 0.033(2) 0.029(2) -0.0065(19) -0.0008(19) -0.001(2)
C14C 0.034(2) 0.049(3) 0.026(2) 0.004(2) -0.0004(18) 0.007(2)
C15C 0.042(3) 0.040(3) 0.029(2) 0.0056(19) 0.0094(19) 0.013(2)
C16C 0.040(2) 0.029(2) 0.029(2) -0.0008(18) 0.0081(19) 0.002(2)
C17C 0.050(3) 0.059(4) 0.043(3) 0.014(3) 0.011(2) 0.020(3)
C18C 0.0371(19) 0.059(2) 0.047(2) -0.0157(17) 0.0037(16) -0.0114(18)
F181 0.037(3) 0.055(3) 0.046(2) -0.019(2) 0.005(2) -0.010(3)
F182 0.037(2) 0.065(3) 0.053(3) -0.012(2) 0.002(2) -0.011(2)
F183 0.038(3) 0.062(3) 0.046(3) -0.021(2) 0.003(2) -0.016(2)
F184 0.046(5) 0.075(5) 0.061(4) 0.005(4) 0.011(4) -0.030(5)
F185 0.042(4) 0.060(4) 0.050(5) -0.035(3) 0.016(4) -0.019(3)
F186 0.048(4) 0.064(5) 0.062(4) -0.035(4) 0.018(4) -0.018(4)
F187 0.034(5) 0.079(6) 0.053(4) -0.023(4) 0.010(4) -0.022(4)
F188 0.033(4) 0.040(4) 0.050(4) -0.010(4) -0.001(3) -0.013(4)
F189 0.035(4) 0.054(4) 0.055(5) -0.002(4) -0.006(3) -0.026(3)
F171 0.101(3) 0.048(2) 0.088(3) 0.0257(17) 0.012(3) -0.0038(18)
F172 0.072(3) 0.065(3) 0.131(4) 0.041(2) 0.037(3) 0.0377(19)
F173 0.201(5) 0.061(2) 0.0328(18) 0.0123(16) 0.017(2) -0.008(3)
C21C 0.044(2) 0.031(2) 0.037(2) 0.0119(18) 0.0171(19) 0.0141(19)
C22C 0.073(3) 0.062(3) 0.044(3) 0.009(2) 0.027(2) 0.026(3)
C23C 0.113(4) 0.102(5) 0.054(3) 0.023(3) 0.053(3) 0.047(4)
C24C 0.096(4) 0.101(5) 0.086(4) 0.043(4) 0.072(3) 0.043(4)
C25C 0.063(3) 0.084(4) 0.096(4) 0.048(3) 0.053(3) 0.032(3)
C26C 0.043(3) 0.048(3) 0.059(3) 0.027(3) 0.025(2) 0.014(2)
C27C 0.153(8) 0.156(8) 0.060(5) 0.018(5) 0.050(5) 0.054(7)
C28C 0.060(4) 0.123(7) 0.140(7) 0.067(6) 0.062(4) 0.014(4)
F271 0.067(6) 0.119(8) 0.035(4) 0.003(4) 0.008(4) 0.027(5)
F272 0.091(6) 0.186(11) 0.045(5) -0.006(6) 0.033(4) 0.018(7)
F273 0.170(10) 0.096(7) 0.060(5) -0.023(5) 0.038(6) -0.012(7)
F274 0.168(11) 0.173(13) 0.043(5) -0.002(6) 0.039(6) 0.024(8)
F275 0.171(11) 0.149(11) 0.070(7) -0.034(6) 0.040(7) 0.044(8)
F276 0.114(9) 0.188(11) 0.038(6) -0.015(7) 0.014(7) 0.013(9)
F281 0.053(9) 0.055(8) 0.136(9) 0.043(6) 0.064(8) 0.002(6)
F282 0.056(7) 0.109(15) 0.20(2) 0.094(15) 0.006(13) 0.008(9)
F283 0.113(14) 0.156(16) 0.22(2) -0.017(15) 0.110(14) -0.060(11)
F284 0.044(8) 0.077(10) 0.25(2) 0.075(10) 0.065(9) -0.015(6)
F285 0.054(9) 0.096(12) 0.180(18) 0.063(11) 0.049(10) 0.026(8)
F286 0.039(6) 0.25(2) 0.103(9) 0.058(14) 0.021(6) -0.034(11)
C31C 0.035(2) 0.025(2) 0.027(2) -0.0015(17) 0.0075(18) 0.0012(19)
C32C 0.045(3) 0.026(2) 0.050(3) 0.001(2) -0.008(2) 0.007(2)
C33C 0.054(3) 0.026(3) 0.077(4) 0.001(3) -0.027(3) -0.006(2)
C34C 0.055(3) 0.025(3) 0.071(4) 0.007(2) -0.009(3) 0.011(2)
C35C 0.036(2) 0.026(2) 0.041(2) 0.0063(19) 0.004(2) 0.0017(19)
C36C 0.037(3) 0.024(2) 0.029(2) 0.0013(16) 0.009(2) 0.0004(18)
C37C 0.107(7) 0.035(4) 0.162(10) 0.012(5) -0.064(7) -0.009(5)
C38C 0.044(3) 0.038(3) 0.057(3) 0.010(3) -0.001(2) -0.001(2)
F371 0.083(8) 0.051(12) 0.115(7) -0.029(5) -0.050(5) 0.003(10)
F372 0.107(9) 0.035(5) 0.172(11) -0.027(7) -0.066(7) 0.006(6)
F373 0.090(9) 0.073(8) 0.179(8) -0.004(7) -0.007(8) -0.034(5)
F374 0.079(6) 0.047(11) 0.102(6) -0.022(6) -0.035(5) -0.014(7)
F375 0.093(8) 0.027(4) 0.165(9) 0.004(6) -0.043(6) -0.017(5)
F376 0.057(6) 0.094(8) 0.153(7) -0.035(7) 0.035(6) -0.037(5)
F381 0.062(8) 0.076(11) 0.057(8) 0.040(7) 0.003(7) 0.007(7)
F382 0.052(6) 0.094(10) 0.089(6) -0.016(6) 0.014(5) 0.025(7)
F383 0.034(6) 0.045(5) 0.164(11) -0.019(6) -0.041(7) 0.016(6)
F384 0.075(7) 0.031(5) 0.102(14) 0.023(7) -0.043(8) 0.009(5)
F385 0.035(5) 0.133(13) 0.127(11) 0.042(9) 0.027(7) 0.008(9)
F386 0.058(7) 0.067(6) 0.113(9) -0.016(6) -0.054(7) 0.033(7)
C41C 0.020(2) 0.027(2) 0.031(2) 0.0036(16) 0.0040(18) 0.0020(15)
C42C 0.0185(19) 0.022(2) 0.032(2) 0.0035(17) 0.0017(16) 0.0003(17)
C43C 0.020(2) 0.032(2) 0.030(2) -0.0002(19) 0.0021(17) 0.0011(18)
C44C 0.018(2) 0.030(2) 0.042(2) -0.008(2) 0.0010(18) 0.0008(18)
C45C 0.0147(19) 0.025(2) 0.043(2) 0.0009(19) 0.0029(17) -0.0012(17)
C46C 0.023(2) 0.028(2) 0.037(2) 0.0060(18) 0.0058(17) 0.0020(17)
C47C 0.028(3) 0.037(3) 0.034(3) -0.0029(19) 0.002(2) -0.002(2)
C48C 0.038(3) 0.027(2) 0.058(3) -0.002(2) 0.006(3) 0.002(2)
F471 0.101(10) 0.047(5) 0.032(4) -0.006(4) 0.030(5) -0.031(5)
F472 0.036(6) 0.134(13) 0.048(7) 0.029(7) -0.009(5) -0.025(8)
F473 0.063(5) 0.085(7) 0.038(5) 0.015(4) 0.029(4) 0.039(5)
F474 0.064(7) 0.132(12) 0.049(6) 0.030(8) -0.002(5) -0.042(9)
F475 0.055(8) 0.129(13) 0.062(10) 0.062(9) 0.020(7) 0.048(9)
F476 0.180(11) 0.054(5) 0.059(6) -0.007(4) 0.052(8) 0.010(8)
F481 0.090(8) 0.030(6) 0.060(5) 0.012(4) 0.027(5) -0.005(5)
F482 0.042(6) 0.049(6) 0.096(8) 0.030(6) -0.051(6) -0.027(5)
F483 0.083(6) 0.013(3) 0.151(12) -0.002(6) 0.085(7) 0.006(4)
F484 0.093(10) 0.036(6) 0.136(12) 0.026(8) -0.048(8) -0.011(7)
F485 0.053(8) 0.055(6) 0.137(12) 0.002(8) 0.063(8) -0.019(6)
F486 0.214(17) 0.041(7) 0.150(14) -0.045(8) 0.121(12) -0.045(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1D C1E 0.96(4) 5_656 ?
C1D Cl1E 1.04(2) . ?
C1D Cl2D 1.645(11) . ?
C1D Cl1D 1.659(10) . ?
C1D Cl1E 1.88(3) 5_656 ?
C1D C1E 1.89(4) . ?
Cl1D C1E 0.72(3) . ?
Cl1D Cl1E 1.391(19) . ?
Cl1D Cl1E 2.23(2) 5_656 ?
Cl2D C1E 0.86(4) 5_656 ?
Cl2D Cl1E 1.58(2) 5_656 ?
Ir1 N2' 2.089(4) . ?
Ir1 N2 2.101(3) . ?
Ir1 C5B 2.138(4) . ?
Ir1 C3B 2.142(4) . ?
Ir1 C4B 2.156(4) . ?
Ir1 C1B 2.160(4) . ?
Ir1 C2B 2.170(5) . ?
Ir1 Cl1 2.3869(12) . ?
N1 N2 1.345(6) . ?
N1 C5 1.364(6) . ?
N1 C1A 1.444(7) . ?
N2 C3 1.337(6) . ?
C3 C4 1.394(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.335(8) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A N1' 1.433(7) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' C5' 1.363(6) . ?
N1' N2' 1.375(6) . ?
N2' C3' 1.333(7) . ?
C3' C4' 1.388(9) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.357(9) . ?
C4' H4' 0.9500 . ?
C5' H5' 0.9500 . ?
C1B C2B 1.412(6) . ?
C1B C5B 1.456(6) . ?
C1B C6B 1.500(6) . ?
C2B C3B 1.451(6) . ?
C2B C7B 1.494(6) . ?
C3B C4B 1.431(6) . ?
C3B C8B 1.508(7) . ?
C4B C5B 1.430(6) . ?
C4B C9B 1.502(6) . ?
C5B C10B 1.489(6) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C41C 1.628(6) . ?
B1C C21C 1.637(7) . ?
B1C C31C 1.638(6) . ?
B1C C11C 1.638(6) . ?
C11C C12C 1.408(7) . ?
C11C C16C 1.410(6) . ?
C12C C13C 1.372(6) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.392(7) . ?
C13C C18C 1.489(7) . ?
C14C C15C 1.400(7) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.370(6) . ?
C15C C17C 1.500(7) . ?
C16C H16C 0.9500 . ?
C17C F173 1.292(6) . ?
C17C F172 1.311(7) . ?
C17C F171 1.337(7) . ?
C18C F187 1.262(8) . ?
C18C F186 1.298(8) . ?
C18C F182 1.310(11) . ?
C18C F184 1.318(9) . ?
C18C F188 1.332(8) . ?
C18C F189 1.375(8) . ?
C18C F183 1.377(12) . ?
C18C F185 1.379(8) . ?
C18C F181 1.456(14) . ?
C21C C26C 1.402(8) . ?
C21C C22C 1.414(7) . ?
C22C C23C 1.384(9) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.391(11) . ?
C23C C27C 1.527(11) . ?
C24C C25C 1.401(11) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.403(8) . ?
C25C C28C 1.535(11) . ?
C26C H26C 0.9500 . ?
C27C F276 0.906(13) . ?
C27C F272 1.142(12) . ?
C27C F275 1.342(14) . ?
C27C F273 1.546(16) . ?
C27C F271 1.562(13) . ?
C27C F274 1.673(17) . ?
C28C F286 1.19(2) . ?
C28C F282 1.23(2) . ?
C28C F284 1.25(3) . ?
C28C F281 1.422(16) . ?
C28C F283 1.46(2) . ?
C28C F285 1.55(2) . ?
C31C C32C 1.402(7) . ?
C31C C36C 1.402(6) . ?
C32C C33C 1.405(7) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.383(7) . ?
C33C C37C 1.491(9) . ?
C34C C35C 1.378(7) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.382(6) . ?
C35C C38C 1.500(7) . ?
C36C H36C 0.9500 . ?
C37C F373 1.079(18) . ?
C37C F375 1.262(15) . ?
C37C F374 1.28(3) . ?
C37C F371 1.37(2) . ?
C37C F372 1.540(18) . ?
C37C F376 1.589(18) . ?
C38C F385 1.219(17) . ?
C38C F384 1.29(2) . ?
C38C F383 1.306(16) . ?
C38C F381 1.31(2) . ?
C38C F386 1.334(17) . ?
C38C F382 1.437(17) . ?
C41C C42C 1.395(6) . ?
C41C C46C 1.408(6) . ?
C42C C43C 1.407(6) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.375(7) . ?
C43C C47C 1.491(7) . ?
C44C C45C 1.403(7) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.389(6) . ?
C45C C48C 1.482(7) . ?
C46C H46C 0.9500 . ?
C47C F474 1.241(17) . ?
C47C F472 1.281(19) . ?
C47C F475 1.284(17) . ?
C47C F476 1.312(12) . ?
C47C F473 1.330(11) . ?
C47C F471 1.388(14) . ?
C48C F484 1.250(18) . ?
C48C F485 1.265(13) . ?
C48C F483 1.303(14) . ?
C48C F482 1.313(13) . ?
C48C F486 1.325(18) . ?
C48C F481 1.408(15) . ?
C1E Cl2D 0.86(4) 5_656 ?
C1E C1D 0.96(4) 5_656 ?
C1E Cl1E 1.89(4) . ?
C1E Cl1E 1.91(4) 5_656 ?
Cl1E Cl2D 1.58(2) 5_656 ?
Cl1E C1D 1.88(3) 5_656 ?
Cl1E C1E 1.91(4) 5_656 ?
Cl1E Cl1D 2.23(2) 5_656 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1E C1D Cl1E 145(4) 5_656 . ?
C1E C1D Cl2D 24(2) 5_656 . ?
Cl1E C1D Cl2D 167(3) . . ?
C1E C1D Cl1D 145(3) 5_656 . ?
Cl1E C1D Cl1D 56.6(12) . . ?
Cl2D C1D Cl1D 128.1(16) . . ?
C1E C1D Cl1E 76(3) 5_656 5_656 ?
Cl1E C1D Cl1E 134.6(16) . 5_656 ?
Cl2D C1D Cl1E 52.9(10) . 5_656 ?
Cl1D C1D Cl1E 78.1(12) . 5_656 ?
C1E C1D C1E 136(2) 5_656 . ?
Cl1E C1D C1E 74.3(19) . . ?
Cl2D C1D C1E 113.7(17) . . ?
Cl1D C1D C1E 22.3(12) . . ?
Cl1E C1D C1E 60.9(13) 5_656 . ?
C1E Cl1D Cl1E 124(4) . . ?
C1E Cl1D C1D 97(4) . . ?
Cl1E Cl1D C1D 38.6(9) . . ?
C1E Cl1D Cl1E 54(4) . 5_656 ?
Cl1E Cl1D Cl1E 93.8(11) . 5_656 ?
C1D Cl1D Cl1E 55.3(11) . 5_656 ?
C1E Cl2D Cl1E 97(3) 5_656 5_656 ?
C1E Cl2D C1D 27(3) 5_656 . ?
Cl1E Cl2D C1D 71.2(13) 5_656 . ?
N2' Ir1 N2 83.88(16) . . ?
N2' Ir1 C5B 112.55(16) . . ?
N2 Ir1 C5B 103.39(14) . . ?
N2' Ir1 C3B 112.63(17) . . ?
N2 Ir1 C3B 162.61(16) . . ?
C5B Ir1 C3B 66.05(16) . . ?
N2' Ir1 C4B 95.43(16) . . ?
N2 Ir1 C4B 138.41(15) . . ?
C5B Ir1 C4B 38.91(16) . . ?
C3B Ir1 C4B 38.89(16) . . ?
N2' Ir1 C1B 151.86(18) . . ?
N2 Ir1 C1B 97.74(14) . . ?
C5B Ir1 C1B 39.60(17) . . ?
C3B Ir1 C1B 65.19(15) . . ?
C4B Ir1 C1B 64.81(16) . . ?
N2' Ir1 C2B 151.59(19) . . ?
N2 Ir1 C2B 124.50(16) . . ?
C5B Ir1 C2B 65.59(15) . . ?
C3B Ir1 C2B 39.32(17) . . ?
C4B Ir1 C2B 64.86(15) . . ?
C1B Ir1 C2B 38.08(16) . . ?
N2' Ir1 Cl1 87.19(12) . . ?
N2 Ir1 Cl1 86.07(11) . . ?
C5B Ir1 Cl1 158.67(11) . . ?
C3B Ir1 Cl1 99.67(12) . . ?
C4B Ir1 Cl1 135.51(12) . . ?
C1B Ir1 Cl1 120.95(13) . . ?
C2B Ir1 Cl1 93.25(11) . . ?
N2 N1 C5 111.0(4) . . ?
N2 N1 C1A 120.3(4) . . ?
C5 N1 C1A 128.3(4) . . ?
C3 N2 N1 106.1(4) . . ?
C3 N2 Ir1 131.2(3) . . ?
N1 N2 Ir1 122.7(3) . . ?
N2 C3 C4 108.8(5) . . ?
N2 C3 H3 125.6 . . ?
C4 C3 H3 125.6 . . ?
C5 C4 C3 107.8(5) . . ?
C5 C4 H4 126.1 . . ?
C3 C4 H4 126.1 . . ?
C4 C5 N1 106.2(4) . . ?
C4 C5 H5 126.9 . . ?
N1 C5 H5 126.9 . . ?
N1' C1A N1 110.3(4) . . ?
N1' C1A H1A1 109.6 . . ?
N1 C1A H1A1 109.6 . . ?
N1' C1A H1A2 109.6 . . ?
N1 C1A H1A2 109.6 . . ?
H1A1 C1A H1A2 108.1 . . ?
C5' N1' N2' 109.2(5) . . ?
C5' N1' C1A 129.9(4) . . ?
N2' N1' C1A 120.3(4) . . ?
C3' N2' N1' 106.3(5) . . ?
C3' N2' Ir1 131.6(4) . . ?
N1' N2' Ir1 122.1(3) . . ?
N2' C3' C4' 110.1(6) . . ?
N2' C3' H3' 124.9 . . ?
C4' C3' H3' 124.9 . . ?
C5' C4' C3' 106.5(5) . . ?
C5' C4' H4' 126.8 . . ?
C3' C4' H4' 126.8 . . ?
C4' C5' N1' 107.8(5) . . ?
C4' C5' H5' 126.1 . . ?
N1' C5' H5' 126.1 . . ?
C2B C1B C5B 108.8(4) . . ?
C2B C1B C6B 127.3(5) . . ?
C5B C1B C6B 123.9(4) . . ?
C2B C1B Ir1 71.3(3) . . ?
C5B C1B Ir1 69.4(2) . . ?
C6B C1B Ir1 125.0(3) . . ?
C1B C2B C3B 108.1(4) . . ?
C1B C2B C7B 126.9(4) . . ?
C3B C2B C7B 125.0(4) . . ?
C1B C2B Ir1 70.6(2) . . ?
C3B C2B Ir1 69.3(2) . . ?
C7B C2B Ir1 126.9(3) . . ?
C4B C3B C2B 107.2(4) . . ?
C4B C3B C8B 127.0(4) . . ?
C2B C3B C8B 125.5(4) . . ?
C4B C3B Ir1 71.1(2) . . ?
C2B C3B Ir1 71.4(2) . . ?
C8B C3B Ir1 127.4(4) . . ?
C5B C4B C3B 109.2(4) . . ?
C5B C4B C9B 126.1(4) . . ?
C3B C4B C9B 124.7(4) . . ?
C5B C4B Ir1 69.9(2) . . ?
C3B C4B Ir1 70.0(2) . . ?
C9B C4B Ir1 125.0(3) . . ?
C4B C5B C1B 106.5(4) . . ?
C4B C5B C10B 127.2(4) . . ?
C1B C5B C10B 125.8(4) . . ?
C4B C5B Ir1 71.2(2) . . ?
C1B C5B Ir1 71.0(2) . . ?
C10B C5B Ir1 129.2(3) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C41C B1C C21C 112.6(4) . . ?
C41C B1C C31C 112.1(3) . . ?
C21C B1C C31C 103.3(3) . . ?
C41C B1C C11C 103.9(3) . . ?
C21C B1C C11C 109.4(4) . . ?
C31C B1C C11C 115.7(4) . . ?
C12C C11C C16C 114.4(4) . . ?
C12C C11C B1C 124.7(4) . . ?
C16C C11C B1C 120.3(4) . . ?
C13C C12C C11C 122.7(4) . . ?
C13C C12C H12C 118.6 . . ?
C11C C12C H12C 118.6 . . ?
C12C C13C C14C 121.3(4) . . ?
C12C C13C C18C 121.4(4) . . ?
C14C C13C C18C 117.3(4) . . ?
C13C C14C C15C 117.6(4) . . ?
C13C C14C H14C 121.2 . . ?
C15C C14C H14C 121.2 . . ?
C16C C15C C14C 120.2(4) . . ?
C16C C15C C17C 120.2(4) . . ?
C14C C15C C17C 119.6(4) . . ?
C15C C16C C11C 123.6(4) . . ?
C15C C16C H16C 118.2 . . ?
C11C C16C H16C 118.2 . . ?
F173 C17C F172 111.5(5) . . ?
F173 C17C F171 102.7(5) . . ?
F172 C17C F171 102.2(5) . . ?
F173 C17C C15C 113.1(5) . . ?
F172 C17C C15C 113.4(5) . . ?
F171 C17C C15C 112.9(4) . . ?
F187 C18C F186 126.1(8) . . ?
F187 C18C F182 77.8(8) . . ?
F186 C18C F182 76.8(7) . . ?
F187 C18C F184 40.9(8) . . ?
F186 C18C F184 110.6(10) . . ?
F182 C18C F184 110.6(10) . . ?
F187 C18C F188 116.6(8) . . ?
F186 C18C F188 36.9(6) . . ?
F182 C18C F188 44.0(6) . . ?
F184 C18C F188 130.4(8) . . ?
F187 C18C F189 99.4(9) . . ?
F186 C18C F189 64.3(8) . . ?
F182 C18C F189 129.2(7) . . ?
F184 C18C F189 59.9(8) . . ?
F188 C18C F189 100.7(7) . . ?
F187 C18C F183 115.3(9) . . ?
F186 C18C F183 38.7(6) . . ?
F182 C18C F183 110.4(7) . . ?
F184 C18C F183 81.2(8) . . ?
F188 C18C F183 75.5(6) . . ?
F189 C18C F183 25.8(5) . . ?
F187 C18C F185 54.1(8) . . ?
F186 C18C F185 105.6(8) . . ?
F182 C18C F185 29.7(5) . . ?
F184 C18C F185 93.7(9) . . ?
F188 C18C F185 73.6(7) . . ?
F189 C18C F185 140.8(8) . . ?
F183 C18C F185 133.7(7) . . ?
F187 C18C F181 28.0(7) . . ?
F186 C18C F181 128.3(9) . . ?
F182 C18C F181 105.3(7) . . ?
F184 C18C F181 19.0(7) . . ?
F188 C18C F181 138.6(8) . . ?
F189 C18C F181 77.9(7) . . ?
F183 C18C F181 100.1(7) . . ?
F185 C18C F181 82.0(7) . . ?
F187 C18C C13C 116.5(6) . . ?
F186 C18C C13C 117.4(6) . . ?
F182 C18C C13C 117.8(6) . . ?
F184 C18C C13C 117.1(7) . . ?
F188 C18C C13C 112.3(6) . . ?
F189 C18C C13C 108.8(6) . . ?
F183 C18C C13C 114.1(6) . . ?
F185 C18C C13C 109.1(6) . . ?
F181 C18C C13C 107.1(6) . . ?
C26C C21C C22C 117.9(5) . . ?
C26C C21C B1C 123.2(4) . . ?
C22C C21C B1C 118.7(5) . . ?
C23C C22C C21C 119.6(6) . . ?
C23C C22C H22C 120.2 . . ?
C21C C22C H22C 120.2 . . ?
C22C C23C C24C 122.9(7) . . ?
C22C C23C C27C 118.9(8) . . ?
C24C C23C C27C 118.2(6) . . ?
C23C C24C C25C 117.8(6) . . ?
C23C C24C H24C 121.1 . . ?
C25C C24C H24C 121.1 . . ?
C24C C25C C26C 120.1(7) . . ?
C24C C25C C28C 122.0(7) . . ?
C26C C25C C28C 117.9(8) . . ?
C21C C26C C25C 121.6(6) . . ?
C21C C26C H26C 119.2 . . ?
C25C C26C H26C 119.2 . . ?
F276 C27C F272 105.7(13) . . ?
F276 C27C F275 134.9(15) . . ?
F272 C27C F275 48.4(7) . . ?
F276 C27C C23C 116.8(12) . . ?
F272 C27C C23C 132.2(11) . . ?
F275 C27C C23C 105.1(9) . . ?
F276 C27C F273 67.9(14) . . ?
F272 C27C F273 103.2(11) . . ?
F275 C27C F273 82.1(10) . . ?
C23C C27C F273 112.0(8) . . ?
F276 C27C F271 18.7(12) . . ?
F272 C27C F271 103.3(9) . . ?
F275 C27C F271 144.9(10) . . ?
C23C C27C F271 109.9(8) . . ?
F273 C27C F271 86.6(8) . . ?
F276 C27C F274 103.1(13) . . ?
F272 C27C F274 50.5(8) . . ?
F275 C27C F274 86.6(8) . . ?
C23C C27C F274 97.2(8) . . ?
F273 C27C F274 150.5(8) . . ?
F271 C27C F274 87.3(8) . . ?
F286 C28C F282 72.7(16) . . ?
F286 C28C F284 134.1(19) . . ?
F282 C28C F284 112.5(17) . . ?
F286 C28C F281 113.4(16) . . ?
F282 C28C F281 104.2(14) . . ?
F284 C28C F281 21.4(15) . . ?
F286 C28C F283 43.9(12) . . ?
F282 C28C F283 111.4(17) . . ?
F284 C28C F283 98.8(17) . . ?
F281 C28C F283 84.1(13) . . ?
F286 C28C C25C 116.0(9) . . ?
F282 C28C C25C 122.0(14) . . ?
F284 C28C C25C 99.8(11) . . ?
F281 C28C C25C 119.5(11) . . ?
F283 C28C C25C 109.4(10) . . ?
F286 C28C F285 106.6(16) . . ?
F282 C28C F285 35.6(12) . . ?
F284 C28C F285 95.9(16) . . ?
F281 C28C F285 100.4(12) . . ?
F283 C28C F285 147.0(15) . . ?
C25C C28C F285 96.9(10) . . ?
C32C C31C C36C 115.4(4) . . ?
C32C C31C B1C 124.5(4) . . ?
C36C C31C B1C 119.6(4) . . ?
C31C C32C C33C 121.7(4) . . ?
C31C C32C H32C 119.2 . . ?
C33C C32C H32C 119.2 . . ?
C34C C33C C32C 120.6(5) . . ?
C34C C33C C37C 120.7(5) . . ?
C32C C33C C37C 118.7(5) . . ?
C35C C34C C33C 118.9(5) . . ?
C35C C34C H34C 120.6 . . ?
C33C C34C H34C 120.6 . . ?
C34C C35C C36C 120.2(4) . . ?
C34C C35C C38C 118.9(4) . . ?
C36C C35C C38C 120.8(4) . . ?
C35C C36C C31C 123.2(4) . . ?
C35C C36C H36C 118.4 . . ?
C31C C36C H36C 118.4 . . ?
F373 C37C F375 61.8(8) . . ?
F373 C37C F374 110(2) . . ?
F375 C37C F374 114.1(18) . . ?
F373 C37C F371 120.0(18) . . ?
F375 C37C F371 124.8(19) . . ?
F374 C37C F371 13(4) . . ?
F373 C37C C33C 119.3(15) . . ?
F375 C37C C33C 117.8(8) . . ?
F374 C37C C33C 120(2) . . ?
F371 C37C C33C 108(2) . . ?
F373 C37C F372 107.3(10) . . ?
F375 C37C F372 46.8(8) . . ?
F374 C37C F372 89.5(14) . . ?
F371 C37C F372 93.4(13) . . ?
C33C C37C F372 105.1(9) . . ?
F373 C37C F376 34.9(11) . . ?
F375 C37C F376 96.6(11) . . ?
F374 C37C F376 95.9(12) . . ?
F371 C37C F376 100.2(13) . . ?
C33C C37C F376 105.5(9) . . ?
F372 C37C F376 140.8(9) . . ?
F385 C38C F384 110.8(15) . . ?
F385 C38C F383 74.2(11) . . ?
F384 C38C F383 122.3(14) . . ?
F385 C38C F381 116.9(14) . . ?
F384 C38C F381 17(2) . . ?
F383 C38C F381 107.6(15) . . ?
F385 C38C F386 107.1(11) . . ?
F384 C38C F386 106.5(14) . . ?
F383 C38C F386 33.0(10) . . ?
F381 C38C F386 89.8(14) . . ?
F385 C38C F382 28.6(10) . . ?
F384 C38C F382 88.0(14) . . ?
F383 C38C F382 100.9(10) . . ?
F381 C38C F382 99.2(13) . . ?
F386 C38C F382 132.3(9) . . ?
F385 C38C C35C 113.9(9) . . ?
F384 C38C C35C 110.6(12) . . ?
F383 C38C C35C 119.1(7) . . ?
F381 C38C C35C 117.6(11) . . ?
F386 C38C C35C 107.5(7) . . ?
F382 C38C C35C 109.2(8) . . ?
C42C C41C C46C 115.4(4) . . ?
C42C C41C B1C 123.1(4) . . ?
C46C C41C B1C 121.1(4) . . ?
C41C C42C C43C 122.2(4) . . ?
C41C C42C H42C 118.9 . . ?
C43C C42C H42C 118.9 . . ?
C44C C43C C42C 121.1(4) . . ?
C44C C43C C47C 118.9(4) . . ?
C42C C43C C47C 120.0(4) . . ?
C43C C44C C45C 118.1(4) . . ?
C43C C44C H44C 121.0 . . ?
C45C C44C H44C 121.0 . . ?
C46C C45C C44C 120.3(4) . . ?
C46C C45C C48C 119.8(4) . . ?
C44C C45C C48C 119.8(4) . . ?
C45C C46C C41C 122.9(4) . . ?
C45C C46C H46C 118.6 . . ?
C41C C46C H46C 118.6 . . ?
F474 C47C F472 123.4(13) . . ?
F474 C47C F475 109.3(13) . . ?
F472 C47C F475 25.0(14) . . ?
F474 C47C F476 106.2(11) . . ?
F472 C47C F476 77.6(12) . . ?
F475 C47C F476 101.5(11) . . ?
F474 C47C F473 76.3(10) . . ?
F472 C47C F473 106.8(12) . . ?
F475 C47C F473 126.6(11) . . ?
F476 C47C F473 33.7(6) . . ?
F474 C47C F471 27.0(10) . . ?
F472 C47C F471 106.2(12) . . ?
F475 C47C F471 86.3(12) . . ?
F476 C47C F471 126.2(9) . . ?
F473 C47C F471 101.2(9) . . ?
F474 C47C C43C 114.6(8) . . ?
F472 C47C C43C 115.4(12) . . ?
F475 C47C C43C 112.2(11) . . ?
F476 C47C C43C 112.0(7) . . ?
F473 C47C C43C 112.4(6) . . ?
F471 C47C C43C 113.6(7) . . ?
F484 C48C F485 106.3(13) . . ?
F484 C48C F483 80.0(11) . . ?
F485 C48C F483 123.0(11) . . ?
F484 C48C F482 119.0(11) . . ?
F485 C48C F482 17.1(13) . . ?
F483 C48C F482 111.5(11) . . ?
F484 C48C F486 110.4(12) . . ?
F485 C48C F486 98.9(12) . . ?
F483 C48C F486 33.9(9) . . ?
F482 C48C F486 83.4(12) . . ?
F484 C48C F481 23.5(12) . . ?
F485 C48C F481 87.7(11) . . ?
F483 C48C F481 102.2(10) . . ?
F482 C48C F481 103.1(10) . . ?
F486 C48C F481 128.8(11) . . ?
F484 C48C C45C 114.7(10) . . ?
F485 C48C C45C 113.7(10) . . ?
F483 C48C C45C 113.8(7) . . ?
F482 C48C C45C 113.5(9) . . ?
F486 C48C C45C 111.5(9) . . ?
F481 C48C C45C 111.7(8) . . ?
Cl1D C1E Cl2D 45(3) . 5_656 ?
Cl1D C1E C1D 90(4) . 5_656 ?
Cl2D C1E C1D 130(5) 5_656 5_656 ?
Cl1D C1E C1D 61(3) . . ?
Cl2D C1E C1D 88(3) 5_656 . ?
C1D C1E C1D 44(2) 5_656 . ?
Cl1D C1E Cl1E 38(3) . . ?
Cl2D C1E Cl1E 56(2) 5_656 . ?
C1D C1E Cl1E 74(3) 5_656 . ?
C1D C1E Cl1E 31.9(9) . . ?
Cl1D C1E Cl1E 108(4) . 5_656 ?
Cl2D C1E Cl1E 147(4) 5_656 5_656 ?
C1D C1E Cl1E 18(2) 5_656 5_656 ?
C1D C1E Cl1E 59.3(14) . 5_656 ?
Cl1E C1E Cl1E 91.0(17) . 5_656 ?
C1D Cl1E Cl1D 84.8(14) . . ?
C1D Cl1E Cl2D 100.4(17) . 5_656 ?
Cl1D Cl1E Cl2D 22.9(8) . 5_656 ?
C1D Cl1E C1D 45.4(16) . 5_656 ?
Cl1D Cl1E C1D 39.7(10) . 5_656 ?
Cl2D Cl1E C1D 56.0(8) 5_656 5_656 ?
C1D Cl1E C1E 74(2) . . ?
Cl1D Cl1E C1E 18.4(12) . . ?
Cl2D Cl1E C1E 26.7(11) 5_656 . ?
C1D Cl1E C1E 29.5(11) 5_656 . ?
C1D Cl1E C1E 17(2) . 5_656 ?
Cl1D Cl1E C1E 97.7(15) . 5_656 ?
Cl2D Cl1E C1E 115.7(15) 5_656 5_656 ?
C1D Cl1E C1E 59.8(13) 5_656 5_656 ?
C1E Cl1E C1E 89.0(17) . 5_656 ?
C1D Cl1E Cl1D 3.6(19) . 5_656 ?
Cl1D Cl1E Cl1D 86.2(11) . 5_656 ?
Cl2D Cl1E Cl1D 100.8(11) 5_656 5_656 ?
C1D Cl1E Cl1D 46.6(6) 5_656 5_656 ?
C1E Cl1E Cl1D 74.3(13) . 5_656 ?
C1E Cl1E Cl1D 17.9(11) 5_656 5_656 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1E C1D Cl1D C1E 80(7) 5_656 . . . ?
Cl1E C1D Cl1D C1E -139(4) . . . . ?
Cl2D C1D Cl1D C1E 56(4) . . . . ?
Cl1E C1D Cl1D C1E 37(4) 5_656 . . . ?
C1E C1D Cl1D Cl1E -141(7) 5_656 . . . ?
Cl2D C1D Cl1D Cl1E -166(4) . . . . ?
Cl1E C1D Cl1D Cl1E 176(2) 5_656 . . . ?
C1E C1D Cl1D Cl1E 139(4) . . . . ?
C1E C1D Cl1D Cl1E 43(6) 5_656 . . 5_656 ?
Cl1E C1D Cl1D Cl1E -176(2) . . . 5_656 ?
Cl2D C1D Cl1D Cl1E 18(2) . . . 5_656 ?
C1E C1D Cl1D Cl1E -37(4) . . . 5_656 ?
Cl1E C1D Cl2D C1E 37(10) . . . 5_656 ?
Cl1D C1D Cl2D C1E 144(7) . . . 5_656 ?
Cl1E C1D Cl2D C1E 167(6) 5_656 . . 5_656 ?
C1E C1D Cl2D C1E 164(6) . . . 5_656 ?
C1E C1D Cl2D Cl1E -167(6) 5_656 . . 5_656 ?
Cl1E C1D Cl2D Cl1E -130(10) . . . 5_656 ?
Cl1D C1D Cl2D Cl1E -23(2) . . . 5_656 ?
C1E C1D Cl2D Cl1E -2.8(19) . . . 5_656 ?
C5 N1 N2 C3 -0.5(5) . . . . ?
C1A N1 N2 C3 -174.5(4) . . . . ?
C5 N1 N2 Ir1 178.9(3) . . . . ?
C1A N1 N2 Ir1 4.9(6) . . . . ?
N2' Ir1 N2 C3 -146.5(4) . . . . ?
C5B Ir1 N2 C3 101.7(4) . . . . ?
C3B Ir1 N2 C3 51.2(7) . . . . ?
C4B Ir1 N2 C3 122.2(4) . . . . ?
C1B Ir1 N2 C3 61.8(4) . . . . ?
C2B Ir1 N2 C3 32.3(5) . . . . ?
Cl1 Ir1 N2 C3 -58.9(4) . . . . ?
N2' Ir1 N2 N1 34.2(3) . . . . ?
C5B Ir1 N2 N1 -77.5(4) . . . . ?
C3B Ir1 N2 N1 -128.0(5) . . . . ?
C4B Ir1 N2 N1 -57.1(4) . . . . ?
C1B Ir1 N2 N1 -117.5(4) . . . . ?
C2B Ir1 N2 N1 -146.9(3) . . . . ?
Cl1 Ir1 N2 N1 121.8(3) . . . . ?
N1 N2 C3 C4 -0.1(5) . . . . ?
Ir1 N2 C3 C4 -179.4(3) . . . . ?
N2 C3 C4 C5 0.6(6) . . . . ?
C3 C4 C5 N1 -0.9(6) . . . . ?
N2 N1 C5 C4 0.8(6) . . . . ?
C1A N1 C5 C4 174.3(5) . . . . ?
N2 N1 C1A N1' -59.4(6) . . . . ?
C5 N1 C1A N1' 127.8(5) . . . . ?
N1 C1A N1' C5' -130.7(5) . . . . ?
N1 C1A N1' N2' 59.0(6) . . . . ?
C5' N1' N2' C3' 1.6(5) . . . . ?
C1A N1' N2' C3' 173.7(4) . . . . ?
C5' N1' N2' Ir1 -176.6(3) . . . . ?
C1A N1' N2' Ir1 -4.5(6) . . . . ?
N2 Ir1 N2' C3' 148.0(5) . . . . ?
C5B Ir1 N2' C3' -110.0(4) . . . . ?
C3B Ir1 N2' C3' -37.6(5) . . . . ?
C4B Ir1 N2' C3' -73.8(5) . . . . ?
C1B Ir1 N2' C3' -117.0(5) . . . . ?
C2B Ir1 N2' C3' -30.0(6) . . . . ?
Cl1 Ir1 N2' C3' 61.7(4) . . . . ?
N2 Ir1 N2' N1' -34.2(4) . . . . ?
C5B Ir1 N2' N1' 67.8(4) . . . . ?
C3B Ir1 N2' N1' 140.1(3) . . . . ?
C4B Ir1 N2' N1' 104.0(4) . . . . ?
C1B Ir1 N2' N1' 60.8(5) . . . . ?
C2B Ir1 N2' N1' 147.8(3) . . . . ?
Cl1 Ir1 N2' N1' -120.6(4) . . . . ?
N1' N2' C3' C4' -2.1(6) . . . . ?
Ir1 N2' C3' C4' 176.0(4) . . . . ?
N2' C3' C4' C5' 1.8(7) . . . . ?
C3' C4' C5' N1' -0.7(7) . . . . ?
N2' N1' C5' C4' -0.5(6) . . . . ?
C1A N1' C5' C4' -171.7(5) . . . . ?
N2' Ir1 C1B C2B 129.6(4) . . . . ?
N2 Ir1 C1B C2B -138.9(2) . . . . ?
C5B Ir1 C1B C2B 119.4(3) . . . . ?
C3B Ir1 C1B C2B 37.6(2) . . . . ?
C4B Ir1 C1B C2B 80.7(3) . . . . ?
Cl1 Ir1 C1B C2B -48.8(3) . . . . ?
N2' Ir1 C1B C5B 10.2(4) . . . . ?
N2 Ir1 C1B C5B 101.7(2) . . . . ?
C3B Ir1 C1B C5B -81.8(2) . . . . ?
C4B Ir1 C1B C5B -38.7(2) . . . . ?
C2B Ir1 C1B C5B -119.4(3) . . . . ?
Cl1 Ir1 C1B C5B -168.27(18) . . . . ?
N2' Ir1 C1B C6B -107.4(5) . . . . ?
N2 Ir1 C1B C6B -15.9(5) . . . . ?
C5B Ir1 C1B C6B -117.6(5) . . . . ?
C3B Ir1 C1B C6B 160.6(5) . . . . ?
C4B Ir1 C1B C6B -156.3(5) . . . . ?
C2B Ir1 C1B C6B 123.0(5) . . . . ?
Cl1 Ir1 C1B C6B 74.1(4) . . . . ?
C5B C1B C2B C3B 0.0(5) . . . . ?
C6B C1B C2B C3B -179.7(4) . . . . ?
Ir1 C1B C2B C3B -59.4(3) . . . . ?
C5B C1B C2B C7B -178.4(4) . . . . ?
C6B C1B C2B C7B 1.9(8) . . . . ?
Ir1 C1B C2B C7B 122.2(5) . . . . ?
C5B C1B C2B Ir1 59.5(3) . . . . ?
C6B C1B C2B Ir1 -120.3(5) . . . . ?
N2' Ir1 C2B C1B -130.2(4) . . . . ?
N2 Ir1 C2B C1B 52.2(3) . . . . ?
C5B Ir1 C2B C1B -37.6(2) . . . . ?
C3B Ir1 C2B C1B -119.0(3) . . . . ?
C4B Ir1 C2B C1B -80.6(3) . . . . ?
Cl1 Ir1 C2B C1B 139.7(2) . . . . ?
N2' Ir1 C2B C3B -11.2(4) . . . . ?
N2 Ir1 C2B C3B 171.2(2) . . . . ?
C5B Ir1 C2B C3B 81.4(3) . . . . ?
C4B Ir1 C2B C3B 38.4(2) . . . . ?
C1B Ir1 C2B C3B 119.0(3) . . . . ?
Cl1 Ir1 C2B C3B -101.3(2) . . . . ?
N2' Ir1 C2B C7B 107.7(5) . . . . ?
N2 Ir1 C2B C7B -69.9(5) . . . . ?
C5B Ir1 C2B C7B -159.7(5) . . . . ?
C3B Ir1 C2B C7B 118.9(5) . . . . ?
C4B Ir1 C2B C7B 157.3(5) . . . . ?
C1B Ir1 C2B C7B -122.1(5) . . . . ?
Cl1 Ir1 C2B C7B 17.6(4) . . . . ?
C1B C2B C3B C4B -2.2(5) . . . . ?
C7B C2B C3B C4B 176.2(4) . . . . ?
Ir1 C2B C3B C4B -62.4(3) . . . . ?
C1B C2B C3B C8B -176.7(5) . . . . ?
C7B C2B C3B C8B 1.8(7) . . . . ?
Ir1 C2B C3B C8B 123.1(5) . . . . ?
C1B C2B C3B Ir1 60.2(3) . . . . ?
C7B C2B C3B Ir1 -121.3(5) . . . . ?
N2' Ir1 C3B C4B -69.3(3) . . . . ?
N2 Ir1 C3B C4B 91.6(6) . . . . ?
C5B Ir1 C3B C4B 36.3(2) . . . . ?
C1B Ir1 C3B C4B 80.0(3) . . . . ?
C2B Ir1 C3B C4B 116.5(4) . . . . ?
Cl1 Ir1 C3B C4B -160.3(2) . . . . ?
N2' Ir1 C3B C2B 174.2(2) . . . . ?
N2 Ir1 C3B C2B -24.9(6) . . . . ?
C5B Ir1 C3B C2B -80.1(3) . . . . ?
C4B Ir1 C3B C2B -116.5(4) . . . . ?
C1B Ir1 C3B C2B -36.5(2) . . . . ?
Cl1 Ir1 C3B C2B 83.3(2) . . . . ?
N2' Ir1 C3B C8B 53.4(5) . . . . ?
N2 Ir1 C3B C8B -145.8(5) . . . . ?
C5B Ir1 C3B C8B 159.0(5) . . . . ?
C4B Ir1 C3B C8B 122.7(5) . . . . ?
C1B Ir1 C3B C8B -157.3(5) . . . . ?
C2B Ir1 C3B C8B -120.9(5) . . . . ?
Cl1 Ir1 C3B C8B -37.6(4) . . . . ?
C2B C3B C4B C5B 3.6(5) . . . . ?
C8B C3B C4B C5B 177.9(5) . . . . ?
Ir1 C3B C4B C5B -59.0(3) . . . . ?
C2B C3B C4B C9B -178.1(4) . . . . ?
C8B C3B C4B C9B -3.7(7) . . . . ?
Ir1 C3B C4B C9B 119.3(4) . . . . ?
C2B C3B C4B Ir1 62.6(3) . . . . ?
C8B C3B C4B Ir1 -123.1(5) . . . . ?
N2' Ir1 C4B C5B -119.7(2) . . . . ?
N2 Ir1 C4B C5B -32.8(3) . . . . ?
C3B Ir1 C4B C5B 120.4(3) . . . . ?
C1B Ir1 C4B C5B 39.4(2) . . . . ?
C2B Ir1 C4B C5B 81.6(3) . . . . ?
Cl1 Ir1 C4B C5B 148.8(2) . . . . ?
N2' Ir1 C4B C3B 119.9(3) . . . . ?
N2 Ir1 C4B C3B -153.3(3) . . . . ?
C5B Ir1 C4B C3B -120.4(3) . . . . ?
C1B Ir1 C4B C3B -81.1(3) . . . . ?
C2B Ir1 C4B C3B -38.8(3) . . . . ?
Cl1 Ir1 C4B C3B 28.3(3) . . . . ?
N2' Ir1 C4B C9B 0.9(4) . . . . ?
N2 Ir1 C4B C9B 87.8(4) . . . . ?
C5B Ir1 C4B C9B 120.6(5) . . . . ?
C3B Ir1 C4B C9B -119.0(5) . . . . ?
C1B Ir1 C4B C9B 160.0(4) . . . . ?
C2B Ir1 C4B C9B -157.8(4) . . . . ?
Cl1 Ir1 C4B C9B -90.6(4) . . . . ?
C3B C4B C5B C1B -3.5(4) . . . . ?
C9B C4B C5B C1B 178.1(4) . . . . ?
Ir1 C4B C5B C1B -62.7(3) . . . . ?
C3B C4B C5B C10B -175.4(4) . . . . ?
C9B C4B C5B C10B 6.3(7) . . . . ?
Ir1 C4B C5B C10B 125.5(4) . . . . ?
C3B C4B C5B Ir1 59.1(3) . . . . ?
C9B C4B C5B Ir1 -119.2(4) . . . . ?
C2B C1B C5B C4B 2.1(4) . . . . ?
C6B C1B C5B C4B -178.1(4) . . . . ?
Ir1 C1B C5B C4B 62.8(3) . . . . ?
C2B C1B C5B C10B 174.2(4) . . . . ?
C6B C1B C5B C10B -6.1(7) . . . . ?
Ir1 C1B C5B C10B -125.2(4) . . . . ?
C2B C1B C5B Ir1 -60.7(3) . . . . ?
C6B C1B C5B Ir1 119.1(4) . . . . ?
N2' Ir1 C5B C4B 69.4(3) . . . . ?
N2 Ir1 C5B C4B 158.3(2) . . . . ?
C3B Ir1 C5B C4B -36.3(2) . . . . ?
C1B Ir1 C5B C4B -115.8(3) . . . . ?
C2B Ir1 C5B C4B -79.6(3) . . . . ?
Cl1 Ir1 C5B C4B -87.1(4) . . . . ?
N2' Ir1 C5B C1B -174.8(2) . . . . ?
N2 Ir1 C5B C1B -85.9(2) . . . . ?
C3B Ir1 C5B C1B 79.4(2) . . . . ?
C4B Ir1 C5B C1B 115.8(3) . . . . ?
C2B Ir1 C5B C1B 36.2(2) . . . . ?
Cl1 Ir1 C5B C1B 28.7(4) . . . . ?
N2' Ir1 C5B C10B -53.7(5) . . . . ?
N2 Ir1 C5B C10B 35.2(5) . . . . ?
C3B Ir1 C5B C10B -159.4(5) . . . . ?
C4B Ir1 C5B C10B -123.1(6) . . . . ?
C1B Ir1 C5B C10B 121.1(5) . . . . ?
C2B Ir1 C5B C10B 157.3(5) . . . . ?
Cl1 Ir1 C5B C10B 149.8(4) . . . . ?
C41C B1C C11C C12C 87.7(5) . . . . ?
C21C B1C C11C C12C -151.8(4) . . . . ?
C31C B1C C11C C12C -35.6(6) . . . . ?
C41C B1C C11C C16C -83.4(5) . . . . ?
C21C B1C C11C C16C 37.1(5) . . . . ?
C31C B1C C11C C16C 153.2(4) . . . . ?
C16C C11C C12C C13C -0.7(6) . . . . ?
B1C C11C C12C C13C -172.3(4) . . . . ?
C11C C12C C13C C14C 1.6(7) . . . . ?
C11C C12C C13C C18C -177.8(4) . . . . ?
C12C C13C C14C C15C -0.7(7) . . . . ?
C18C C13C C14C C15C 178.8(4) . . . . ?
C13C C14C C15C C16C -1.1(7) . . . . ?
C13C C14C C15C C17C 178.4(4) . . . . ?
C14C C15C C16C C11C 2.1(7) . . . . ?
C17C C15C C16C C11C -177.4(4) . . . . ?
C12C C11C C16C C15C -1.2(6) . . . . ?
B1C C11C C16C C15C 170.9(4) . . . . ?
C16C C15C C17C F173 -82.6(6) . . . . ?
C14C C15C C17C F173 97.9(6) . . . . ?
C16C C15C C17C F172 149.1(5) . . . . ?
C14C C15C C17C F172 -30.4(7) . . . . ?
C16C C15C C17C F171 33.4(7) . . . . ?
C14C C15C C17C F171 -146.0(5) . . . . ?
C12C C13C C18C F187 -80.3(10) . . . . ?
C14C C13C C18C F187 100.2(9) . . . . ?
C12C C13C C18C F186 101.0(10) . . . . ?
C14C C13C C18C F186 -78.5(11) . . . . ?
C12C C13C C18C F182 -170.0(7) . . . . ?
C14C C13C C18C F182 10.5(9) . . . . ?
C12C C13C C18C F184 -34.3(10) . . . . ?
C14C C13C C18C F184 146.2(8) . . . . ?
C12C C13C C18C F188 141.5(7) . . . . ?
C14C C13C C18C F188 -38.0(8) . . . . ?
C12C C13C C18C F189 30.9(7) . . . . ?
C14C C13C C18C F189 -148.6(6) . . . . ?
C12C C13C C18C F183 58.0(8) . . . . ?
C14C C13C C18C F183 -121.5(7) . . . . ?
C12C C13C C18C F185 -139.0(7) . . . . ?
C14C C13C C18C F185 41.5(8) . . . . ?
C12C C13C C18C F181 -51.8(7) . . . . ?
C14C C13C C18C F181 128.7(6) . . . . ?
C41C B1C C21C C26C -26.0(6) . . . . ?
C31C B1C C21C C26C 95.2(5) . . . . ?
C11C B1C C21C C26C -141.0(4) . . . . ?
C41C B1C C21C C22C 159.3(4) . . . . ?
C31C B1C C21C C22C -79.5(5) . . . . ?
C11C B1C C21C C22C 44.3(5) . . . . ?
C26C C21C C22C C23C 0.9(6) . . . . ?
B1C C21C C22C C23C 175.9(5) . . . . ?
C21C C22C C23C C24C 0.9(8) . . . . ?
C21C C22C C23C C27C -178.6(7) . . . . ?
C22C C23C C24C C25C -1.7(11) . . . . ?
C27C C23C C24C C25C 177.8(8) . . . . ?
C23C C24C C25C C26C 0.7(10) . . . . ?
C23C C24C C25C C28C -178.9(7) . . . . ?
C22C C21C C26C C25C -1.8(7) . . . . ?
B1C C21C C26C C25C -176.6(5) . . . . ?
C24C C25C C26C C21C 1.0(9) . . . . ?
C28C C25C C26C C21C -179.3(6) . . . . ?
C22C C23C C27C F276 -25(2) . . . . ?
C24C C23C C27C F276 155.1(16) . . . . ?
C22C C23C C27C F272 -175.4(14) . . . . ?
C24C C23C C27C F272 5.0(19) . . . . ?
C22C C23C C27C F275 137.6(9) . . . . ?
C24C C23C C27C F275 -42.0(13) . . . . ?
C22C C23C C27C F273 50.2(11) . . . . ?
C24C C23C C27C F273 -129.4(9) . . . . ?
C22C C23C C27C F271 -44.3(11) . . . . ?
C24C C23C C27C F271 136.1(8) . . . . ?
C22C C23C C27C F274 -134.0(7) . . . . ?
C24C C23C C27C F274 46.4(10) . . . . ?
C24C C25C C28C F286 170.3(18) . . . . ?
C26C C25C C28C F286 -9(2) . . . . ?
C24C C25C C28C F282 85.1(19) . . . . ?
C26C C25C C28C F282 -94.6(19) . . . . ?
C24C C25C C28C F284 -39.4(16) . . . . ?
C26C C25C C28C F284 141.0(14) . . . . ?
C24C C25C C28C F281 -48.2(15) . . . . ?
C26C C25C C28C F281 132.1(11) . . . . ?
C24C C25C C28C F283 -142.4(13) . . . . ?
C26C C25C C28C F283 37.9(15) . . . . ?
C24C C25C C28C F285 57.9(12) . . . . ?
C26C C25C C28C F285 -121.8(10) . . . . ?
C41C B1C C31C C32C -142.5(4) . . . . ?
C21C B1C C31C C32C 96.0(5) . . . . ?
C11C B1C C31C C32C -23.6(6) . . . . ?
C41C B1C C31C C36C 45.8(5) . . . . ?
C21C B1C C31C C36C -75.7(5) . . . . ?
C11C B1C C31C C36C 164.8(4) . . . . ?
C36C C31C C32C C33C -0.6(6) . . . . ?
B1C C31C C32C C33C -172.5(5) . . . . ?
C31C C32C C33C C34C 0.6(8) . . . . ?
C31C C32C C33C C37C -178.8(8) . . . . ?
C32C C33C C34C C35C 0.0(9) . . . . ?
C37C C33C C34C C35C 179.3(9) . . . . ?
C33C C34C C35C C36C -0.5(9) . . . . ?
C33C C34C C35C C38C 177.6(6) . . . . ?
C34C C35C C36C C31C 0.5(8) . . . . ?
C38C C35C C36C C31C -177.6(5) . . . . ?
C32C C31C C36C C35C 0.1(7) . . . . ?
B1C C31C C36C C35C 172.4(4) . . . . ?
C34C C33C C37C F373 -77.9(17) . . . . ?
C32C C33C C37C F373 101.4(14) . . . . ?
C34C C33C C37C F375 -6.4(19) . . . . ?
C32C C33C C37C F375 172.9(12) . . . . ?
C34C C33C C37C F374 140.7(14) . . . . ?
C32C C33C C37C F374 -39.9(18) . . . . ?
C34C C33C C37C F371 140.9(10) . . . . ?
C32C C33C C37C F371 -39.7(14) . . . . ?
C34C C33C C37C F372 42.4(13) . . . . ?
C32C C33C C37C F372 -138.3(8) . . . . ?
C34C C33C C37C F376 -112.8(8) . . . . ?
C32C C33C C37C F376 66.6(10) . . . . ?
C34C C35C C38C F385 -99.5(11) . . . . ?
C36C C35C C38C F385 78.6(11) . . . . ?
C34C C35C C38C F384 26.1(14) . . . . ?
C36C C35C C38C F384 -155.8(13) . . . . ?
C34C C35C C38C F383 175.9(11) . . . . ?
C36C C35C C38C F383 -6.1(13) . . . . ?
C34C C35C C38C F381 42.8(15) . . . . ?
C36C C35C C38C F381 -139.2(13) . . . . ?
C34C C35C C38C F386 142.0(9) . . . . ?
C36C C35C C38C F386 -39.9(10) . . . . ?
C34C C35C C38C F382 -69.1(9) . . . . ?
C36C C35C C38C F382 108.9(8) . . . . ?
C21C B1C C41C C42C 144.7(4) . . . . ?
C31C B1C C41C C42C 28.8(6) . . . . ?
C11C B1C C41C C42C -96.9(5) . . . . ?
C21C B1C C41C C46C -42.7(5) . . . . ?
C31C B1C C41C C46C -158.7(4) . . . . ?
C11C B1C C41C C46C 75.6(5) . . . . ?
C46C C41C C42C C43C 0.4(6) . . . . ?
B1C C41C C42C C43C 173.4(4) . . . . ?
C41C C42C C43C C44C 0.5(6) . . . . ?
C41C C42C C43C C47C 179.2(4) . . . . ?
C42C C43C C44C C45C -1.1(6) . . . . ?
C47C C43C C44C C45C -179.8(4) . . . . ?
C43C C44C C45C C46C 0.8(6) . . . . ?
C43C C44C C45C C48C 179.4(4) . . . . ?
C44C C45C C46C C41C 0.2(6) . . . . ?
C48C C45C C46C C41C -178.4(4) . . . . ?
C42C C41C C46C C45C -0.7(6) . . . . ?
B1C C41C C46C C45C -173.9(4) . . . . ?
C44C C43C C47C F474 -136.2(9) . . . . ?
C42C C43C C47C F474 45.1(10) . . . . ?
C44C C43C C47C F472 71.2(11) . . . . ?
C42C C43C C47C F472 -107.5(11) . . . . ?
C44C C43C C47C F475 98.3(11) . . . . ?
C42C C43C C47C F475 -80.4(11) . . . . ?
C44C C43C C47C F476 -15.2(9) . . . . ?
C42C C43C C47C F476 166.2(8) . . . . ?
C44C C43C C47C F473 -51.6(8) . . . . ?
C42C C43C C47C F473 129.7(7) . . . . ?
C44C C43C C47C F471 -165.8(8) . . . . ?
C42C C43C C47C F471 15.5(9) . . . . ?
C46C C45C C48C F484 -41.5(12) . . . . ?
C44C C45C C48C F484 139.9(11) . . . . ?
C46C C45C C48C F485 81.2(10) . . . . ?
C44C C45C C48C F485 -97.4(10) . . . . ?
C46C C45C C48C F483 -131.2(8) . . . . ?
C44C C45C C48C F483 50.2(10) . . . . ?
C46C C45C C48C F482 99.9(10) . . . . ?
C44C C45C C48C F482 -78.7(10) . . . . ?
C46C C45C C48C F486 -168.0(10) . . . . ?
C44C C45C C48C F486 13.4(11) . . . . ?
C46C C45C C48C F481 -16.2(9) . . . . ?
C44C C45C C48C F481 165.2(8) . . . . ?
Cl1E Cl1D C1E Cl2D 90(4) . . . 5_656 ?
C1D Cl1D C1E Cl2D 120(3) . . . 5_656 ?
Cl1E Cl1D C1E Cl2D 157(3) 5_656 . . 5_656 ?
Cl1E Cl1D C1E C1D -64(5) . . . 5_656 ?
C1D Cl1D C1E C1D -34(4) . . . 5_656 ?
Cl1E Cl1D C1E C1D 3.4(17) 5_656 . . 5_656 ?
Cl1E Cl1D C1E C1D -30(3) . . . . ?
Cl1E Cl1D C1E C1D 38(3) 5_656 . . . ?
C1D Cl1D C1E Cl1E 30(3) . . . . ?
Cl1E Cl1D C1E Cl1E 67(5) 5_656 . . . ?
Cl1E Cl1D C1E Cl1E -67(5) . . . 5_656 ?
C1D Cl1D C1E Cl1E -38(3) . . . 5_656 ?
C1E C1D C1E Cl1D -126(6) 5_656 . . . ?
Cl1E C1D C1E Cl1D 35(4) . . . . ?
Cl2D C1D C1E Cl1D -135(4) . . . . ?
Cl1E C1D C1E Cl1D -137(4) 5_656 . . . ?
C1E C1D C1E Cl2D -164(6) 5_656 . . 5_656 ?
Cl1E C1D C1E Cl2D -3(3) . . . 5_656 ?
Cl2D C1D C1E Cl2D -173(3) . . . 5_656 ?
Cl1D C1D C1E Cl2D -38(3) . . . 5_656 ?
Cl1E C1D C1E Cl2D -176(3) 5_656 . . 5_656 ?
C1E C1D C1E C1D -0.004(11) 5_656 . . 5_656 ?
Cl1E C1D C1E C1D 161(6) . . . 5_656 ?
Cl2D C1D C1E C1D -9(3) . . . 5_656 ?
Cl1D C1D C1E C1D 126(6) . . . 5_656 ?
Cl1E C1D C1E C1D -12(4) 5_656 . . 5_656 ?
C1E C1D C1E Cl1E -161(6) 5_656 . . . ?
Cl2D C1D C1E Cl1E -170(3) . . . . ?
Cl1D C1D C1E Cl1E -35(4) . . . . ?
Cl1E C1D C1E Cl1E -172(2) 5_656 . . . ?
C1E C1D C1E Cl1E 12(4) 5_656 . . 5_656 ?
Cl1E C1D C1E Cl1E 172(2) . . . 5_656 ?
Cl2D C1D C1E Cl1E 2.6(18) . . . 5_656 ?
Cl1D C1D C1E Cl1E 137(4) . . . 5_656 ?
C1E C1D Cl1E Cl1D 141(6) 5_656 . . . ?
Cl2D C1D Cl1E Cl1D 116(10) . . . . ?
Cl1E C1D Cl1E Cl1D -5(3) 5_656 . . . ?
C1E C1D Cl1E Cl1D -15.0(14) . . . . ?
C1E C1D Cl1E Cl2D 158(6) 5_656 . . 5_656 ?
Cl2D C1D Cl1E Cl2D 133(9) . . . 5_656 ?
Cl1D C1D Cl1E Cl2D 16.8(10) . . . 5_656 ?
Cl1E C1D Cl1E Cl2D 11(4) 5_656 . . 5_656 ?
C1E C1D Cl1E Cl2D 1.8(16) . . . 5_656 ?
C1E C1D Cl1E C1D 147(9) 5_656 . . 5_656 ?
Cl2D C1D Cl1E C1D 122(12) . . . 5_656 ?
Cl1D C1D Cl1E C1D 5(3) . . . 5_656 ?
Cl1E C1D Cl1E C1D 0.000(8) 5_656 . . 5_656 ?
C1E C1D Cl1E C1D -10(3) . . . 5_656 ?
C1E C1D Cl1E C1E 156(6) 5_656 . . . ?
Cl2D C1D Cl1E C1E 131(10) . . . . ?
Cl1D C1D Cl1E C1E 15.0(14) . . . . ?
Cl1E C1D Cl1E C1E 10(3) 5_656 . . . ?
Cl2D C1D Cl1E C1E -25(7) . . . 5_656 ?
Cl1D C1D Cl1E C1E -141(6) . . . 5_656 ?
Cl1E C1D Cl1E C1E -147(9) 5_656 . . 5_656 ?
C1E C1D Cl1E C1E -156(6) . . . 5_656 ?
C1E C1D Cl1E Cl1D -106(26) 5_656 . . 5_656 ?
Cl2D C1D Cl1E Cl1D -131(31) . . . 5_656 ?
Cl1D C1D Cl1E Cl1D 113(26) . . . 5_656 ?
Cl1E C1D Cl1E Cl1D 107(28) 5_656 . . 5_656 ?
C1E C1D Cl1E Cl1D 98(26) . . . 5_656 ?
C1E Cl1D Cl1E C1D 52(6) . . . . ?
Cl1E Cl1D Cl1E C1D 3.3(19) 5_656 . . . ?
C1E Cl1D Cl1E Cl2D -81(5) . . . 5_656 ?
C1D Cl1D Cl1E Cl2D -133(3) . . . 5_656 ?
Cl1E Cl1D Cl1E Cl2D -130(3) 5_656 . . 5_656 ?
C1E Cl1D Cl1E C1D 46(5) . . . 5_656 ?
C1D Cl1D Cl1E C1D -6(4) . . . 5_656 ?
Cl1E Cl1D Cl1E C1D -2.8(16) 5_656 . . 5_656 ?
C1D Cl1D Cl1E C1E -52(6) . . . . ?
Cl1E Cl1D Cl1E C1E -49(5) 5_656 . . . ?
C1E Cl1D Cl1E C1E 63(6) . . . 5_656 ?
C1D Cl1D Cl1E C1E 10(2) . . . 5_656 ?
Cl1E Cl1D Cl1E C1E 13.7(12) 5_656 . . 5_656 ?
C1E Cl1D Cl1E Cl1D 49(5) . . . 5_656 ?
C1D Cl1D Cl1E Cl1D -3.3(19) . . . 5_656 ?
Cl1E Cl1D Cl1E Cl1D -0.002(1) 5_656 . . 5_656 ?
Cl1D C1E Cl1E C1D -125(6) . . . . ?
Cl2D C1E Cl1E C1D 176(4) 5_656 . . . ?
C1D C1E Cl1E C1D -14(4) 5_656 . . . ?
Cl1E C1E Cl1E C1D -7(2) 5_656 . . . ?
Cl2D C1E Cl1E Cl1D -59(4) 5_656 . . . ?
C1D C1E Cl1E Cl1D 111(6) 5_656 . . . ?
C1D C1E Cl1E Cl1D 125(6) . . . . ?
Cl1E C1E Cl1E Cl1D 118(5) 5_656 . . . ?
Cl1D C1E Cl1E Cl2D 59(4) . . . 5_656 ?
C1D C1E Cl1E Cl2D 170(5) 5_656 . . 5_656 ?
C1D C1E Cl1E Cl2D -176(4) . . . 5_656 ?
Cl1E C1E Cl1E Cl2D 177(4) 5_656 . . 5_656 ?
Cl1D C1E Cl1E C1D -111(6) . . . 5_656 ?
Cl2D C1E Cl1E C1D -170(5) 5_656 . . 5_656 ?
C1D C1E Cl1E C1D 14(4) . . . 5_656 ?
Cl1E C1E Cl1E C1D 7(2) 5_656 . . 5_656 ?
Cl1D C1E Cl1E C1E -118(5) . . . 5_656 ?
Cl2D C1E Cl1E C1E -177(4) 5_656 . . 5_656 ?
C1D C1E Cl1E C1E -7(2) 5_656 . . 5_656 ?
C1D C1E Cl1E C1E 7(2) . . . 5_656 ?
Cl1E C1E Cl1E C1E -0.002(3) 5_656 . . 5_656 ?
Cl1D C1E Cl1E Cl1D -129(5) . . . 5_656 ?
Cl2D C1E Cl1E Cl1D 172(3) 5_656 . . 5_656 ?
C1D C1E Cl1E Cl1D -18(3) 5_656 . . 5_656 ?
C1D C1E Cl1E Cl1D -3.7(19) . . . 5_656 ?
Cl1E C1E Cl1E Cl1D -10.3(9) 5_656 . . 5_656 ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 1.405
_refine_diff_density_min -0.800
_refine_diff_density_rms 0.086
_iucr_refine_instructions_details
;
TITL Chinmin1_C2byc in C2/c
CELL 0.71073 28.8655 12.9022 29.8343 90.000 104.722 90.000
ZERR 8.00 0.0012 0.0005 0.0012 0.000 0.001 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H B N F Cl Ir
UNIT 395 280 8 32 192 14 8
OMIT -2 0 2
OMIT 4 0 0
OMIT 2 0 0
OMIT 0 0 2
OMIT 1 1 0
OMIT 0 2 0
OMIT -1 1 1
OMIT 3 1 0
OMIT 0 2 2
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
SADI 0.01 F181 F182 F182 F183 F183 F181
SADI 0.01 C18C F184 C18C F185 C18C F186
SADI 0.01 C18C F187 C18C F188 C18C F189
SADI 0.01 C27C C22C C27C C24C
SADI 0.01 F271 F272 F272 F273 F273 F271
SADI 0.01 F274 F275 F275 F276 F276 F274
SADI 0.01 F371 F372 F372 F373 F373 F371
SADI 0.01 F374 F375 F375 F376 F376 F374
SADI 0.01 C23C C27C C25C C28C
CONF
SIZE 0.364 0.262 0.176
DFIX 1.65 0.01 C1D CL1D C1D CL2D
FLAT C21C > C28C
FLAT C31C > C38C
DELU 0.005 C18C F184 F185 F186 F187 F188 F189
DELU 0.001 C18C F181 F182 F183
DELU 0.01 F271 > F276
DELU 0.005 F371 > F376
DELU 0.005 F281 F282 F283
DELU 0.005 F284 F285 F286
DELU 0.01 F381 > F386
DELU 0.01 C21C > C28C
DELU 0.01 F481 > F486
DELU 0.01 F471 > F476
DELU 0.01 C1D CL1D CL2D
SIMU 0.0051 F371 > F376
SIMU 0.001 C18C F181 F182 F183
SIMU 0.005 C18C F184 F185 F186 F187 F188 F189
SIMU 0.01 F271 > F276
SIMU 0.005 F281 F282 F283
SIMU 0.005 F284 F285 F286
SIMU 0.01 F381 > F386
SIMU 0.01 C21C > C28C
SIMU 0.01 F481 > F486
SIMU 0.01 F471 > F476
TEMP -118.100
WGHT 0.100000 0.500000
FVAR 0.02988
PART -1
MOLE 3
C1D 1 0.492032 0.014541 0.518759 10.25000 0.08075
CL1D 6 0.543327 0.027445 0.503873 10.25000 0.12699
CL2D 6 0.449315 -0.070981 0.499721 10.25000 0.11059
PART 0
MOLE 1
IR1 7 0.747758 0.125787 0.696814 11.00000 0.02353 0.02255 =
0.02582 -0.00100 0.00623 0.00005
N1 4 0.833001 0.128053 0.781492 11.00000 0.04115 0.03286 =
0.03410 -0.01105 -0.00400 0.00087
N2 4 0.814213 0.171195 0.739773 11.00000 0.03209 0.02782 =
0.03384 -0.00893 0.00467 0.00007
C3 1 0.846000 0.241729 0.733740 11.00000 0.03333 0.03698 =
0.05078 -0.01596 0.01356 -0.01093
AFIX 43
H3 2 0.842637 0.284857 0.707297 11.00000 -1.20000
AFIX 0
C4 1 0.884898 0.241646 0.772604 11.00000 0.03307 0.04735 =
0.06892 -0.03276 -0.00010 -0.00413
AFIX 43
H4 2 0.912366 0.284867 0.777374 11.00000 -1.20000
AFIX 0
C5 1 0.876655 0.169958 0.801931 11.00000 0.03324 0.03910 =
0.05172 -0.01833 -0.01020 0.00299
AFIX 43
H5 2 0.897095 0.151781 0.831171 11.00000 -1.20000
AFIX 0
C1A 1 0.809413 0.041536 0.797059 11.00000 0.05414 0.03579 =
0.02894 0.00106 -0.00402 0.00774
AFIX 23
H1A1 2 0.807900 -0.017648 0.775616 11.00000 -1.20000
H1A2 2 0.828032 0.019611 0.828240 11.00000 -1.20000
AFIX 0
N1' 4 0.761909 0.069978 0.798788 11.00000 0.06873 0.02956 =
0.02711 -0.00141 0.01131 0.00141
N2' 4 0.729279 0.103694 0.759461 11.00000 0.04274 0.03185 =
0.03687 -0.00439 0.01482 -0.00249
C3' 1 0.687663 0.113723 0.770728 11.00000 0.05136 0.04080 =
0.06172 -0.00831 0.03467 -0.00076
AFIX 43
H3' 2 0.658789 0.138051 0.750466 11.00000 -1.20000
AFIX 0
C4' 1 0.692650 0.083464 0.816347 11.00000 0.10176 0.04879 =
0.06277 -0.00607 0.06177 -0.00686
AFIX 43
H4' 2 0.668203 0.081537 0.832470 11.00000 -1.20000
AFIX 0
C5' 1 0.739347 0.057169 0.833384 11.00000 0.08554 0.04751 =
0.03737 -0.00647 0.02449 -0.00520
AFIX 43
H5' 2 0.753747 0.033966 0.863974 11.00000 -1.20000
AFIX 0
C1B 1 0.773376 0.069514 0.639273 11.00000 0.02405 0.03727 =
0.02462 -0.00749 0.00355 -0.00547
C2B 1 0.730430 0.125052 0.621667 11.00000 0.02739 0.03075 =
0.02709 0.00037 0.00111 0.00021
C3B 1 0.692847 0.075221 0.638188 11.00000 0.02670 0.03302 =
0.02562 0.00116 0.00010 -0.00136
C4B 1 0.713604 -0.013520 0.664500 11.00000 0.03105 0.02388 =
0.02725 -0.00006 0.00437 -0.00615
C5B 1 0.763772 -0.016496 0.667214 11.00000 0.02938 0.03105 =
0.02247 -0.01034 0.00096 0.00286
C6B 1 0.821733 0.092464 0.631632 11.00000 0.03082 0.06051 =
0.03937 -0.01075 0.01662 -0.00966
AFIX 137
H6B1 2 0.827644 0.046342 0.607579 11.00000 -1.50000
H6B2 2 0.846407 0.081352 0.660564 11.00000 -1.50000
H6B3 2 0.822744 0.164692 0.621760 11.00000 -1.50000
AFIX 0
C7B 1 0.723587 0.217320 0.590396 11.00000 0.04607 0.04470 =
0.04257 0.01230 0.00785 -0.00401
AFIX 137
H7B1 2 0.753765 0.255778 0.595599 11.00000 -1.50000
H7B2 2 0.698796 0.262322 0.597032 11.00000 -1.50000
H7B3 2 0.713711 0.194373 0.558049 11.00000 -1.50000
AFIX 0
C8B 1 0.640795 0.106341 0.625513 11.00000 0.03050 0.06189 =
0.05655 0.01757 0.00376 0.00551
AFIX 137
H8B1 2 0.625901 0.085362 0.593524 11.00000 -1.50000
H8B2 2 0.638287 0.181690 0.628312 11.00000 -1.50000
H8B3 2 0.624363 0.072200 0.646464 11.00000 -1.50000
AFIX 0
C9B 1 0.686621 -0.089020 0.686696 11.00000 0.04094 0.03158 =
0.04045 0.00107 0.01106 -0.00947
AFIX 137
H9B1 2 0.671695 -0.141888 0.664022 11.00000 -1.50000
H9B2 2 0.661759 -0.052113 0.697405 11.00000 -1.50000
H9B3 2 0.708805 -0.122318 0.713144 11.00000 -1.50000
AFIX 0
C10B 1 0.798416 -0.099192 0.688429 11.00000 0.06008 0.03919 =
0.03185 -0.00653 0.00487 0.02325
AFIX 137
H10A 2 0.786426 -0.136421 0.711822 11.00000 -1.50000
H10B 2 0.829489 -0.067812 0.703095 11.00000 -1.50000
H10C 2 0.802134 -0.147768 0.664331 11.00000 -1.50000
AFIX 0
CL1 6 0.724350 0.302408 0.700377 11.00000 0.05386 0.02856 =
0.04753 -0.00108 0.01227 0.01155
MOLE 2
B1C 3 0.589651 0.703347 0.406127 11.00000 0.03153 0.02334 =
0.02671 -0.00035 0.00628 -0.00020
C11C 1 0.644052 0.665319 0.431884 11.00000 0.04296 0.02335 =
0.01994 -0.00471 0.00345 0.00295
C12C 1 0.686111 0.705908 0.422988 11.00000 0.03618 0.02920 =
0.02151 0.00152 0.00430 0.00113
AFIX 43
H12C 2 0.683620 0.764838 0.403427 11.00000 -1.20000
AFIX 0
C13C 1 0.730536 0.663904 0.441390 11.00000 0.03585 0.03257 =
0.02881 -0.00650 -0.00078 -0.00078
C14C 1 0.736329 0.576028 0.469344 11.00000 0.03385 0.04882 =
0.02599 0.00413 -0.00036 0.00716
AFIX 43
H14C 2 0.767080 0.546594 0.481786 11.00000 -1.20000
AFIX 0
C15C 1 0.695243 0.532583 0.478467 11.00000 0.04159 0.04047 =
0.02879 0.00557 0.00938 0.01272
C16C 1 0.651348 0.577250 0.460823 11.00000 0.04006 0.02937 =
0.02904 -0.00078 0.00807 0.00204
AFIX 43
H16C 2 0.624312 0.547235 0.468507 11.00000 -1.20000
AFIX 0
C17C 1 0.699515 0.436237 0.507355 11.00000 0.04969 0.05894 =
0.04297 0.01363 0.01079 0.01966
C18C 1 0.774524 0.710870 0.432650 11.00000 0.03712 0.05901 =
0.04729 -0.01574 0.00371 -0.01142
PART 1
F181 5 0.765953 0.723326 0.382717 10.33330 0.03687 0.05485 =
0.04638 -0.01895 0.00548 -0.00982
F182 5 0.814523 0.658254 0.445463 10.33330 0.03653 0.06489 =
0.05313 -0.01167 0.00213 -0.01076
F183 5 0.781880 0.812614 0.446514 10.33330 0.03846 0.06190 =
0.04616 -0.02093 0.00301 -0.01620
PART 2
F184 5 0.770519 0.753952 0.391767 10.33330 0.04587 0.07467 =
0.06116 0.00506 0.01125 -0.02991
F185 5 0.804223 0.632894 0.424893 10.33330 0.04241 0.05975 =
0.05046 -0.03503 0.01608 -0.01887
F186 5 0.800748 0.767742 0.465263 10.33330 0.04823 0.06360 =
0.06248 -0.03547 0.01811 -0.01802
PART 3
F187 5 0.783225 0.689655 0.394291 10.33330 0.03413 0.07885 =
0.05347 -0.02305 0.00964 -0.02232
F188 5 0.811505 0.707660 0.469932 10.33330 0.03312 0.03987 =
0.04991 -0.00992 -0.00147 -0.01346
F189 5 0.767883 0.816146 0.427288 10.33330 0.03524 0.05376 =
0.05542 -0.00166 -0.00640 -0.02618
PART 0
F171 5 0.661527 0.373728 0.494208 11.00000 0.10121 0.04772 =
0.08762 0.02573 0.01210 -0.00381
F172 5 0.734736 0.375568 0.503564 11.00000 0.07208 0.06487 =
0.13097 0.04131 0.03661 0.03765
F173 5 0.700909 0.454818 0.550235 11.00000 0.20124 0.06099 =
0.03279 0.01228 0.01652 -0.00797
C21C 1 0.554658 0.685353 0.440865 11.00000 0.04433 0.03141 =
0.03703 0.01189 0.01709 0.01411
C22C 1 0.571451 0.714270 0.487937 11.00000 0.07349 0.06194 =
0.04385 0.00889 0.02727 0.02621
AFIX 43
H22C 2 0.603220 0.739267 0.499396 11.00000 -1.20000
AFIX 0
C23C 1 0.541349 0.705946 0.517204 11.00000 0.11252 0.10188 =
0.05394 0.02289 0.05320 0.04722
C24C 1 0.494718 0.668613 0.502706 11.00000 0.09644 0.10131 =
0.08583 0.04250 0.07210 0.04344
AFIX 43
H24C 2 0.475145 0.662017 0.523784 11.00000 -1.20000
AFIX 0
C25C 1 0.477566 0.641058 0.455992 11.00000 0.06321 0.08361 =
0.09557 0.04790 0.05304 0.03179
C26C 1 0.507263 0.650314 0.425587 11.00000 0.04339 0.04806 =
0.05946 0.02697 0.02476 0.01392
AFIX 43
H26C 2 0.494983 0.632425 0.393897 11.00000 -1.20000
AFIX 0
C27C 1 0.559763 0.739835 0.567651 11.00000 0.15321 0.15642 =
0.06001 0.01809 0.04959 0.05377
C28C 1 0.426397 0.600816 0.436277 11.00000 0.05961 0.12318 =
0.13991 0.06677 0.06218 0.01376
PART 1
F271 5 0.611687 0.698066 0.587807 10.50000 0.06665 0.11867 =
0.03514 0.00315 0.00817 0.02728
F272 5 0.543262 0.735893 0.598560 10.50000 0.09078 0.18586 =
0.04543 -0.00649 0.03270 0.01833
F273 5 0.582334 0.849176 0.571843 10.50000 0.16954 0.09569 =
0.06040 -0.02277 0.03842 -0.01244
PART 2
F274 5 0.540421 0.636832 0.591736 10.50000 0.16826 0.17340 =
0.04251 -0.00250 0.03940 0.02423
F275 5 0.523285 0.792018 0.577376 10.50000 0.17123 0.14856 =
0.06962 -0.03378 0.04004 0.04376
F276 5 0.591876 0.738026 0.579794 10.50000 0.11439 0.18816 =
0.03811 -0.01529 0.01395 0.01256
PART 1
F281 5 0.408374 0.521100 0.460084 10.50000 0.05317 0.05451 =
0.13594 0.04320 0.06381 0.00224
F282 5 0.392198 0.659797 0.422817 10.50000 0.05622 0.10915 =
0.20110 0.09374 0.00647 0.00794
F283 5 0.426827 0.519902 0.402365 10.50000 0.11308 0.15568 =
0.22013 -0.01747 0.10953 -0.06006
PART 2
F284 5 0.422199 0.545085 0.469222 10.50000 0.04420 0.07712 =
0.24997 0.07549 0.06497 -0.01534
F285 5 0.400103 0.695921 0.449540 10.50000 0.05445 0.09632 =
0.17980 0.06315 0.04855 0.02602
F286 5 0.413684 0.593112 0.395312 10.50000 0.03893 0.25374 =
0.10294 0.05833 0.02088 -0.03368
PART 0
C31C 1 0.583437 0.827086 0.393844 11.00000 0.03457 0.02521 =
0.02670 -0.00148 0.00745 0.00123
C32C 1 0.614575 0.904619 0.416830 11.00000 0.04525 0.02644 =
0.05007 0.00131 -0.00840 0.00669
AFIX 43
H32C 2 0.643335 0.885182 0.438700 11.00000 -1.20000
AFIX 0
C33C 1 0.604328 1.010300 0.408344 11.00000 0.05394 0.02566 =
0.07734 0.00078 -0.02658 -0.00590
C34C 1 0.562567 1.041141 0.377019 11.00000 0.05504 0.02505 =
0.07096 0.00663 -0.00866 0.01085
AFIX 43
H34C 2 0.555640 1.112628 0.371297 11.00000 -1.20000
AFIX 0
C35C 1 0.531177 0.966471 0.354248 11.00000 0.03614 0.02621 =
0.04134 0.00629 0.00376 0.00166
C36C 1 0.541645 0.862590 0.362488 11.00000 0.03695 0.02448 =
0.02875 0.00125 0.00929 0.00039
AFIX 43
H36C 2 0.519448 0.812816 0.346114 11.00000 -1.20000
AFIX 0
C37C 1 0.639601 1.088375 0.433380 11.00000 0.10733 0.03540 =
0.16173 0.01231 -0.06449 -0.00877
C38C 1 0.484962 0.999868 0.321685 11.00000 0.04431 0.03783 =
0.05667 0.01048 -0.00090 -0.00072
PART 1
F371 5 0.657015 1.053745 0.478042 10.50000 0.08331 0.05091 =
0.11475 -0.02908 -0.04957 0.00276
F372 5 0.609225 1.174268 0.447716 10.50000 0.10733 0.03453 =
0.17208 -0.02686 -0.06633 0.00600
F373 5 0.663342 1.125328 0.415563 10.50000 0.09039 0.07320 =
0.17850 -0.00361 -0.00708 -0.03393
PART 2
F374 5 0.661203 1.074562 0.476181 10.50000 0.07852 0.04676 =
0.10239 -0.02165 -0.03497 -0.01374
F375 5 0.632228 1.182281 0.421909 10.50000 0.09288 0.02736 =
0.16548 0.00351 -0.04328 -0.01688
F376 5 0.685736 1.073689 0.414183 10.50000 0.05670 0.09360 =
0.15317 -0.03497 0.03519 -0.03747
PART 1
F381 5 0.486463 1.077484 0.293763 10.50000 0.06202 0.07592 =
0.05703 0.04045 0.00277 0.00704
F382 5 0.454626 1.044926 0.347923 10.50000 0.05223 0.09392 =
0.08854 -0.01560 0.01397 0.02464
F383 5 0.456418 0.929644 0.297878 10.50000 0.03362 0.04504 =
0.16406 -0.01878 -0.04139 0.01572
PART 2
F384 5 0.489177 1.090716 0.305449 10.50000 0.07489 0.03109 =
0.10214 0.02305 -0.04300 0.00915
F385 5 0.450609 0.996085 0.338389 10.50000 0.03520 0.13343 =
0.12661 0.04159 0.02663 0.00802
F386 5 0.476041 0.935151 0.285629 10.50000 0.05825 0.06661 =
0.11288 -0.01567 -0.05385 0.03329
PART 0
C41C 1 0.574844 0.631344 0.359856 11.00000 0.01964 0.02705 =
0.03146 0.00358 0.00398 0.00204
C42C 1 0.578921 0.664339 0.316488 11.00000 0.01847 0.02169 =
0.03198 0.00353 0.00166 0.00034
AFIX 43
H42C 2 0.587603 0.734262 0.312832 11.00000 -1.20000
AFIX 0
C43C 1 0.570606 0.597532 0.277975 11.00000 0.02048 0.03169 =
0.02993 -0.00021 0.00207 0.00110
C44C 1 0.557580 0.495891 0.281411 11.00000 0.01838 0.03005 =
0.04165 -0.00827 0.00101 0.00080
AFIX 43
H44C 2 0.551428 0.451242 0.255241 11.00000 -1.20000
AFIX 0
C45C 1 0.553642 0.460052 0.324691 11.00000 0.01467 0.02513 =
0.04339 0.00092 0.00288 -0.00122
C46C 1 0.562171 0.526565 0.362502 11.00000 0.02282 0.02760 =
0.03674 0.00597 0.00585 0.00204
AFIX 43
H46C 2 0.559331 0.500216 0.391418 11.00000 -1.20000
AFIX 0
C47C 1 0.574825 0.637346 0.232245 11.00000 0.02751 0.03710 =
0.03416 -0.00291 0.00155 -0.00220
C48C 1 0.539218 0.351351 0.329822 11.00000 0.03765 0.02744 =
0.05752 -0.00151 0.00555 0.00209
PART 1
F471 5 0.598554 0.731625 0.235036 10.50000 0.10088 0.04676 =
0.03231 -0.00577 0.02981 -0.03108
F472 5 0.535146 0.648853 0.201505 10.50000 0.03554 0.13426 =
0.04825 0.02907 -0.00904 -0.02533
F473 5 0.602442 0.577479 0.213549 10.50000 0.06282 0.08492 =
0.03809 0.01468 0.02884 0.03915
PART 2
F474 5 0.610745 0.691595 0.234066 10.50000 0.06414 0.13163 =
0.04928 0.03050 -0.00178 -0.04237
F475 5 0.537224 0.686857 0.210506 10.50000 0.05465 0.12862 =
0.06245 0.06239 0.01999 0.04796
F476 5 0.576328 0.562008 0.203107 10.50000 0.18027 0.05398 =
0.05856 -0.00665 0.05195 0.00965
PART 1
F481 5 0.548588 0.321933 0.376710 10.50000 0.08969 0.02967 =
0.05957 0.01245 0.02672 -0.00535
F482 5 0.492956 0.335488 0.314428 10.50000 0.04210 0.04868 =
0.09593 0.03021 -0.05076 -0.02668
F483 5 0.563810 0.283375 0.313213 10.50000 0.08282 0.01276 =
0.15072 -0.00237 0.08529 0.00562
PART 2
F484 5 0.561329 0.308134 0.366527 10.50000 0.09281 0.03648 =
0.13592 0.02564 -0.04828 -0.01098
F485 5 0.495117 0.340750 0.327562 10.50000 0.05269 0.05453 =
0.13718 0.00185 0.06299 -0.01886
F486 5 0.541474 0.294374 0.293506 10.50000 0.21366 0.04089 =
0.14974 -0.04513 0.12145 -0.04485
PART 0
C1E 1 0.533158 0.032477 0.479293 10.12500 0.02689
CL1E 6 0.520462 0.058899 0.537386 10.25000 0.15572
HKLF 4
REM Chinmin1_C2byc in C2/c
REM R1 = 0.0310 for 8380 Fo > 4sig(Fo) and 0.0374 for all 9435 data
REM 962 parameters refined using 341 restraints
END
WGHT 0.0375 66.0990
REM Highest difference peak 1.405, deepest hole -0.800, 1-sigma level 0.086
Q1 1 0.7490 0.4651 0.5492 11.00000 0.05 1.41
Q2 1 0.7572 0.8728 0.4114 11.00000 0.05 0.77
Q3 1 0.7318 0.0765 0.7142 11.00000 0.05 0.75
Q4 1 0.5087 0.3140 0.2828 11.00000 0.05 0.71
Q5 1 0.7668 0.8466 0.4357 11.00000 0.05 0.65
Q6 1 0.5574 -0.0228 0.5191 11.00000 0.05 0.65
Q7 1 0.7008 0.3648 0.4929 11.00000 0.05 0.60
Q8 1 0.5629 0.7409 0.2230 11.00000 0.05 0.58
Q9 1 0.5400 0.0680 0.5217 11.00000 0.05 0.57
Q10 1 0.5794 0.2853 0.3407 11.00000 0.05 0.56
Q11 1 0.8180 0.6202 0.4328 11.00000 0.05 0.56
Q12 1 0.6757 0.5060 0.5564 11.00000 0.05 0.56
Q13 1 0.6209 0.6255 0.2248 11.00000 0.05 0.54
Q14 1 0.7986 0.6325 0.4038 11.00000 0.05 0.53
Q15 1 0.8088 0.7269 0.4813 11.00000 0.05 0.53
Q16 1 0.6732 0.4218 0.5242 11.00000 0.05 0.52
Q17 1 0.5178 0.3346 0.3611 11.00000 0.05 0.50
Q18 1 0.5447 0.5777 0.1926 11.00000 0.05 0.50
Q19 1 0.4334 0.6280 0.4608 11.00000 0.05 0.48
Q20 1 0.7560 -0.0303 0.6563 11.00000 0.05 0.47
;
#===END
data_carol5_p1bar
_audit_update_record
;
2012-07-24 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'2(C32 H12 B F23.97), 2(C23 H28 Cl N5 Rh), C H2 Cl2'
_chemical_formula_sum
'C55.50 H41 B Cl2 F24 N5 Rh'
_chemical_formula_weight 1418.55
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Rh' 'Rh' -1.1178 0.9187
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Triclinic'
_symmetry_space_group_name_H-M 'P-1'
_symmetry_space_group_name_Hall '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 12.4931(16)
_cell_length_b 16.3598(8)
_cell_length_c 16.8978(10)
_cell_angle_alpha 117.365(2)
_cell_angle_beta 96.805(3)
_cell_angle_gamma 101.470(3)
_cell_volume 2917.2(4)
_cell_formula_units_Z 2
_cell_measurement_temperature 152(2)
_cell_measurement_reflns_used 9931
_cell_measurement_theta_min 2.459
_cell_measurement_theta_max 30.049
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'Yellow orange'
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.12
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.615
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1418
_exptl_absorpt_coefficient_mu 0.504
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8513
_exptl_absorpt_correction_T_max 0.9718
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 152(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 33968
_diffrn_reflns_av_R_equivalents 0.0842
_diffrn_reflns_av_sigmaI/netI 0.0525
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 3.12
_diffrn_reflns_theta_max 25.00
_reflns_number_total 10077
_reflns_number_gt 8671
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
Atomic displacement parameters revealed higher anisotropies for the CF3 groups,
one of them is modelled as orientationally disodered over three equally
occupied sites. Difference Fourier at this stage also revealed a solvent
molecule that was modelled over two disordered positions.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+1.9149P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 10077
_refine_ls_number_parameters 865
_refine_ls_number_restraints 174
_refine_ls_R_factor_all 0.0441
_refine_ls_R_factor_gt 0.0346
_refine_ls_wR_factor_ref 0.0822
_refine_ls_wR_factor_gt 0.0783
_refine_ls_goodness_of_fit_ref 1.042
_refine_ls_restrained_S_all 1.042
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh -0.125948(14) 0.837072(12) 0.622087(12) 0.01819(7) Uani 1 1 d . . .
N1 N -0.05809(16) 1.05971(13) 0.74884(13) 0.0244(4) Uani 1 1 d . . .
N2 N -0.14199(16) 0.97588(13) 0.70863(13) 0.0244(4) Uani 1 1 d . . .
C3 C -0.2351(2) 1.00106(19) 0.72737(18) 0.0312(6) Uani 1 1 d . . .
H3 H -0.3079 0.9571 0.7073 0.037 Uiso 1 1 calc R . .
C4 C -0.2111(2) 1.10006(19) 0.78006(19) 0.0375(6) Uani 1 1 d . . .
H4 H -0.2624 1.1358 0.8028 0.045 Uiso 1 1 calc R . .
C5 C -0.0979(2) 1.13530(18) 0.79230(17) 0.0320(6) Uani 1 1 d . . .
H5 H -0.0552 1.2011 0.8254 0.038 Uiso 1 1 calc R . .
C1A C 0.0575(2) 1.05996(17) 0.74510(16) 0.0264(5) Uani 1 1 d . . .
H1A1 H 0.0851 1.0315 0.7811 0.032 Uiso 1 1 calc R . .
H2A1 H 0.1053 1.1271 0.7735 0.032 Uiso 1 1 calc R . .
N1' N 0.11210(16) 0.94430(13) 0.51800(13) 0.0225(4) Uani 1 1 d . . .
N2' N 0.02956(16) 0.87502(13) 0.51276(13) 0.0226(4) Uani 1 1 d . . .
N3' N 0.00299(15) 0.91222(13) 0.59237(12) 0.0203(4) Uani 1 1 d . . .
C4' C 0.06839(19) 1.00432(15) 0.64816(16) 0.0215(5) Uani 1 1 d . . .
C5' C 0.1387(2) 1.02515(16) 0.60001(17) 0.0260(5) Uani 1 1 d . . .
H5' H 0.1943 1.0839 0.6200 0.031 Uiso 1 1 calc R . .
C6' C 0.1682(2) 0.92173(17) 0.44165(17) 0.0264(5) Uani 1 1 d . . .
H16' H 0.1976 0.9808 0.4386 0.032 Uiso 1 1 calc R . .
H26' H 0.1127 0.8744 0.3831 0.032 Uiso 1 1 calc R . .
C7' C 0.2635(2) 0.88165(17) 0.45351(16) 0.0251(5) Uani 1 1 d . . .
C8' C 0.2491(2) 0.78423(18) 0.40719(18) 0.0328(6) Uani 1 1 d . . .
H8' H 0.1782 0.7418 0.3673 0.039 Uiso 1 1 calc R . .
C9' C 0.3372(2) 0.7472(2) 0.4182(2) 0.0405(7) Uani 1 1 d . . .
H9' H 0.3264 0.6798 0.3858 0.049 Uiso 1 1 calc R . .
C10' C 0.4389(2) 0.8073(2) 0.4753(2) 0.0415(7) Uani 1 1 d . . .
H10' H 0.4996 0.7820 0.4813 0.050 Uiso 1 1 calc R . .
C11' C 0.4538(2) 0.9052(2) 0.5246(2) 0.0446(7) Uani 1 1 d . . .
H11' H 0.5240 0.9470 0.5661 0.053 Uiso 1 1 calc R . .
C12' C 0.3665(2) 0.94225(19) 0.51361(18) 0.0354(6) Uani 1 1 d . . .
H12' H 0.3770 1.0096 0.5474 0.043 Uiso 1 1 calc R . .
C1B C -0.0373(2) 0.73781(17) 0.62490(17) 0.0257(5) Uani 1 1 d . . .
C2B C -0.1436(2) 0.68694(16) 0.56043(17) 0.0262(5) Uani 1 1 d . . .
C3B C -0.2297(2) 0.70767(17) 0.61038(18) 0.0286(6) Uani 1 1 d . . .
C4B C -0.1762(2) 0.77315(18) 0.70370(18) 0.0283(5) Uani 1 1 d . . .
C5B C -0.0559(2) 0.79381(17) 0.71370(17) 0.0266(5) Uani 1 1 d . . .
C6B C 0.0747(2) 0.7343(2) 0.6037(2) 0.0437(7) Uani 1 1 d . . .
H6B1 H 0.0964 0.6827 0.6098 0.065 Uiso 1 1 calc R . .
H6B2 H 0.1309 0.7959 0.6467 0.065 Uiso 1 1 calc R . .
H6B3 H 0.0705 0.7221 0.5408 0.065 Uiso 1 1 calc R . .
C7B C -0.1626(3) 0.6184(2) 0.45977(19) 0.0470(8) Uani 1 1 d . . .
H7B1 H -0.0984 0.6378 0.4377 0.070 Uiso 1 1 calc R . .
H7B2 H -0.2315 0.6194 0.4262 0.070 Uiso 1 1 calc R . .
H7B3 H -0.1702 0.5534 0.4497 0.070 Uiso 1 1 calc R . .
C8B C -0.3535(2) 0.6645(2) 0.5698(2) 0.0495(8) Uani 1 1 d . . .
H8B1 H -0.3768 0.6011 0.5646 0.074 Uiso 1 1 calc R . .
H8B2 H -0.3713 0.6579 0.5087 0.074 Uiso 1 1 calc R . .
H8B3 H -0.3936 0.7063 0.6094 0.074 Uiso 1 1 calc R . .
C9B C -0.2338(3) 0.8146(2) 0.7795(2) 0.0507(8) Uani 1 1 d . . .
H9B1 H -0.3061 0.8192 0.7550 0.076 Uiso 1 1 calc R . .
H9B2 H -0.1863 0.8788 0.8267 0.076 Uiso 1 1 calc R . .
H9B3 H -0.2466 0.7730 0.8067 0.076 Uiso 1 1 calc R . .
C10B C 0.0326(3) 0.8532(2) 0.8017(2) 0.0463(8) Uani 1 1 d . . .
H10B H 0.0450 0.8133 0.8289 0.069 Uiso 1 1 calc R . .
H10C H 0.0079 0.9067 0.8443 0.069 Uiso 1 1 calc R . .
H10D H 0.1029 0.8785 0.7896 0.069 Uiso 1 1 calc R . .
Cl1A Cl -0.25709(5) 0.82822(4) 0.50027(4) 0.02530(13) Uani 1 1 d . . .
B1C B 0.2470(2) 0.67635(18) 0.89586(18) 0.0198(5) Uani 1 1 d . . .
C11C C 0.30132(18) 0.76830(16) 0.88349(15) 0.0200(5) Uani 1 1 d . . .
C12C C 0.30781(19) 0.86199(16) 0.94991(16) 0.0226(5) Uani 1 1 d . . .
H12C H 0.2906 0.8726 1.0065 0.027 Uiso 1 1 calc R . .
C13C C 0.33847(19) 0.93994(16) 0.93603(17) 0.0249(5) Uani 1 1 d . . .
C14C C 0.3663(2) 0.92795(18) 0.85531(18) 0.0293(6) Uani 1 1 d . . .
H14C H 0.3885 0.9813 0.8460 0.035 Uiso 1 1 calc R . .
C15C C 0.3608(2) 0.83619(17) 0.78835(17) 0.0262(5) Uani 1 1 d . . .
C16C C 0.32755(19) 0.75816(17) 0.80193(16) 0.0227(5) Uani 1 1 d . . .
H16C H 0.3225 0.6958 0.7541 0.027 Uiso 1 1 calc R . .
C17C C 0.3345(2) 1.03623(18) 1.0064(2) 0.0368(6) Uani 1 1 d . . .
C18C C 0.3913(2) 0.8226(2) 0.7011(2) 0.0369(6) Uani 1 1 d . . .
F1C F 0.36572(16) 1.05330(12) 1.09257(12) 0.0563(5) Uani 1 1 d . . .
F2C F 0.4024(2) 1.10857(12) 1.00495(16) 0.0786(7) Uani 1 1 d . . .
F3C F 0.23199(16) 1.04565(13) 0.99833(14) 0.0703(6) Uani 1 1 d . . .
F4C F 0.49982(15) 0.85991(19) 0.71276(14) 0.0750(7) Uani 1 1 d . . .
F5C F 0.34020(15) 0.86727(15) 0.66573(13) 0.0585(5) Uani 1 1 d . . .
F6C F 0.3605(2) 0.73232(15) 0.63481(13) 0.0816(7) Uani 1 1 d . . .
C21C C 0.11103(18) 0.65675(15) 0.86319(15) 0.0203(5) Uani 1 1 d . . .
C22C C 0.04848(19) 0.70416(16) 0.92364(16) 0.0216(5) Uani 1 1 d . . .
H22C H 0.0852 0.7470 0.9865 0.026 Uiso 1 1 calc R . .
C23C C -0.06543(19) 0.69069(16) 0.89480(16) 0.0236(5) Uani 1 1 d . . .
C24C C -0.12278(19) 0.62879(17) 0.80394(17) 0.0242(5) Uani 1 1 d . . .
H24C H -0.2011 0.6187 0.7844 0.029 Uiso 1 1 calc R . .
C25C C -0.06237(19) 0.58204(16) 0.74242(16) 0.0232(5) Uani 1 1 d . . .
C26C C 0.05199(19) 0.59635(16) 0.77175(16) 0.0218(5) Uani 1 1 d . . .
H26C H 0.0913 0.5638 0.7279 0.026 Uiso 1 1 calc R . .
C27C C -0.1251(2) 0.7440(2) 0.96536(18) 0.0332(6) Uani 1 1 d . . .
C28C C -0.1189(2) 0.51174(17) 0.64410(18) 0.0291(6) Uani 1 1 d . . .
F7C F -0.12247(16) 0.72041(15) 1.03129(12) 0.0556(5) Uani 1 1 d . . .
F8C F -0.07698(15) 0.83914(12) 1.00959(13) 0.0582(5) Uani 1 1 d . . .
F9C F -0.23251(13) 0.72981(14) 0.93082(11) 0.0492(4) Uani 1 1 d . . .
F10C F -0.22476(13) 0.51106(13) 0.62053(12) 0.0540(5) Uani 1 1 d . . .
F11C F -0.06544(14) 0.52827(11) 0.58625(10) 0.0420(4) Uani 1 1 d . . .
F12C F -0.12069(14) 0.42167(10) 0.62268(11) 0.0432(4) Uani 1 1 d . . .
C31C C 0.28422(18) 0.57965(15) 0.83510(15) 0.0192(5) Uani 1 1 d . . .
C32C C 0.38661(19) 0.58032(16) 0.80964(16) 0.0228(5) Uani 1 1 d . . .
H32C H 0.4367 0.6399 0.8243 0.027 Uiso 1 1 calc R . .
C33C C 0.41760(19) 0.49685(17) 0.76367(16) 0.0256(5) Uani 1 1 d . A .
C34C C 0.3493(2) 0.40838(17) 0.74437(16) 0.0266(5) Uani 1 1 d . . .
H34C H 0.3707 0.3512 0.7135 0.032 Uiso 1 1 calc R . .
C35C C 0.24935(19) 0.40687(16) 0.77180(15) 0.0233(5) Uani 1 1 d . . .
C36C C 0.21702(19) 0.48991(16) 0.81475(15) 0.0212(5) Uani 1 1 d . . .
H36C H 0.1467 0.4858 0.8310 0.025 Uiso 1 1 calc R . .
C37C C 0.5249(2) 0.50055(19) 0.7336(2) 0.0402(7) Uani 1 1 d DU . .
C38C C 0.1731(2) 0.31513(17) 0.75534(18) 0.0327(6) Uani 1 1 d . . .
F13C F 0.5631(15) 0.5742(10) 0.7223(12) 0.056(4) Uani 0.33 1 d PDU A 1
F14C F 0.6110(8) 0.5129(12) 0.8022(9) 0.064(3) Uani 0.33 1 d PDU A 1
F15C F 0.5242(7) 0.4219(6) 0.6604(7) 0.0409(18) Uani 0.33 1 d PDU A 1
F131 F 0.5865(13) 0.5896(10) 0.7588(11) 0.045(4) Uani 0.33 1 d PDU A 2
F132 F 0.5956(10) 0.4651(11) 0.7663(11) 0.062(3) Uani 0.33 1 d PDU A 2
F133 F 0.5095(7) 0.4530(9) 0.6432(5) 0.052(2) Uiso 0.33 1 d PDU A 2
F13' F 0.6058(10) 0.5746(11) 0.7923(10) 0.082(5) Uani 0.33 1 d PDU A 3
F14' F 0.5520(11) 0.4194(8) 0.7035(13) 0.066(3) Uani 0.33 1 d PDU A 3
F15' F 0.5068(6) 0.5099(11) 0.6542(7) 0.0653(18) Uani 0.33 1 d PDU A 3
F16C F 0.22208(18) 0.24507(12) 0.73274(18) 0.0790(7) Uani 1 1 d . . .
F17C F 0.08134(18) 0.28209(14) 0.68939(14) 0.0761(7) Uani 1 1 d . . .
F18C F 0.13572(15) 0.32317(11) 0.82815(11) 0.0499(4) Uani 1 1 d . . .
C41C C 0.28249(18) 0.69655(15) 1.00098(15) 0.0196(5) Uani 1 1 d . . .
C42C C 0.38674(19) 0.75505(16) 1.06131(16) 0.0220(5) Uani 1 1 d . . .
H42C H 0.4371 0.7922 1.0442 0.026 Uiso 1 1 calc R . .
C43C C 0.4196(2) 0.76088(16) 1.14607(16) 0.0244(5) Uani 1 1 d . . .
C44C C 0.3492(2) 0.70728(17) 1.17361(16) 0.0263(5) Uani 1 1 d . . .
H44C H 0.3714 0.7111 1.2312 0.032 Uiso 1 1 calc R . .
C45C C 0.2456(2) 0.64816(16) 1.11469(16) 0.0241(5) Uani 1 1 d . . .
C46C C 0.21299(19) 0.64378(16) 1.03116(16) 0.0215(5) Uani 1 1 d . . .
H46C H 0.1407 0.6034 0.9928 0.026 Uiso 1 1 calc R . .
C47C C 0.5292(2) 0.8298(2) 1.20937(19) 0.0397(7) Uani 1 1 d . . .
C48C C 0.1646(2) 0.5886(2) 1.13991(19) 0.0362(6) Uani 1 1 d . . .
F19C F 0.61140(15) 0.83342(18) 1.16750(14) 0.0793(7) Uani 1 1 d . . .
F20C F 0.5238(2) 0.92039(13) 1.25158(16) 0.0842(7) Uani 1 1 d . . .
F21C F 0.56588(15) 0.81301(14) 1.27586(13) 0.0621(5) Uani 1 1 d . . .
F22C F 0.21125(15) 0.57986(13) 1.20893(12) 0.0540(5) Uani 1 1 d . . .
F23C F 0.08278(17) 0.62774(18) 1.16776(18) 0.0807(7) Uani 1 1 d . . .
F24C F 0.11454(19) 0.50126(13) 1.07078(13) 0.0719(6) Uani 1 1 d . . .
C1D C 0.4665(8) 0.5299(7) 0.0122(6) 0.069(2) Uani 0.50 1 d P . .
H1D1 H 0.4414 0.5484 -0.0335 0.083 Uiso 0.50 1 calc PR . .
H1D2 H 0.4924 0.5853 0.0755 0.083 Uiso 0.50 1 calc PR . .
Cl1D Cl 0.6051(4) 0.5558(5) -0.0022(3) 0.149(2) Uani 0.50 1 d P . .
Cl2D Cl 0.5756(4) 0.5966(3) 0.0265(3) 0.1067(14) Uani 0.50 1 d P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.01897(10) 0.01697(10) 0.02223(11) 0.01174(8) 0.00694(7) 0.00623(7)
N1 0.0316(11) 0.0185(10) 0.0225(10) 0.0088(8) 0.0099(9) 0.0074(8)
N2 0.0276(11) 0.0218(10) 0.0288(11) 0.0146(9) 0.0108(9) 0.0098(8)
C3 0.0312(14) 0.0334(14) 0.0389(15) 0.0208(12) 0.0173(12) 0.0169(11)
C4 0.0488(17) 0.0371(15) 0.0409(16) 0.0210(13) 0.0260(13) 0.0284(13)
C5 0.0510(17) 0.0218(13) 0.0273(13) 0.0111(11) 0.0177(12) 0.0167(12)
C1A 0.0293(13) 0.0207(12) 0.0244(13) 0.0084(10) 0.0066(10) 0.0043(10)
N1' 0.0260(10) 0.0184(10) 0.0263(11) 0.0122(8) 0.0115(8) 0.0072(8)
N2' 0.0240(10) 0.0207(10) 0.0249(11) 0.0123(8) 0.0092(8) 0.0057(8)
N3' 0.0222(10) 0.0194(10) 0.0208(10) 0.0106(8) 0.0068(8) 0.0066(8)
C4' 0.0222(12) 0.0163(11) 0.0244(12) 0.0089(10) 0.0061(10) 0.0052(9)
C5' 0.0291(13) 0.0155(11) 0.0295(13) 0.0089(10) 0.0091(11) 0.0031(9)
C6' 0.0350(14) 0.0258(13) 0.0272(13) 0.0171(11) 0.0168(11) 0.0115(10)
C7' 0.0300(13) 0.0279(13) 0.0256(13) 0.0172(11) 0.0148(11) 0.0098(10)
C8' 0.0294(14) 0.0274(14) 0.0388(15) 0.0135(12) 0.0110(12) 0.0086(11)
C9' 0.0425(17) 0.0366(15) 0.0493(17) 0.0213(14) 0.0201(14) 0.0206(13)
C10' 0.0352(16) 0.061(2) 0.0496(18) 0.0383(16) 0.0206(14) 0.0237(14)
C11' 0.0313(15) 0.060(2) 0.0439(17) 0.0322(16) 0.0051(13) 0.0023(14)
C12' 0.0374(15) 0.0308(14) 0.0331(15) 0.0149(12) 0.0089(12) 0.0018(12)
C1B 0.0272(13) 0.0251(12) 0.0377(14) 0.0229(11) 0.0115(11) 0.0131(10)
C2B 0.0362(14) 0.0164(12) 0.0289(13) 0.0134(10) 0.0055(11) 0.0096(10)
C3B 0.0266(13) 0.0258(13) 0.0435(15) 0.0258(12) 0.0069(11) 0.0067(10)
C4B 0.0375(14) 0.0296(13) 0.0360(14) 0.0260(12) 0.0183(12) 0.0162(11)
C5B 0.0344(14) 0.0228(12) 0.0274(13) 0.0173(11) 0.0032(11) 0.0084(10)
C6B 0.0359(15) 0.0501(18) 0.070(2) 0.0420(17) 0.0258(15) 0.0259(13)
C7B 0.078(2) 0.0286(15) 0.0310(15) 0.0111(12) 0.0055(15) 0.0218(14)
C8B 0.0311(15) 0.0434(17) 0.080(2) 0.0418(18) 0.0039(15) 0.0003(13)
C9B 0.072(2) 0.062(2) 0.057(2) 0.0455(18) 0.0454(18) 0.0414(18)
C10B 0.0548(19) 0.0379(16) 0.0401(17) 0.0237(14) -0.0103(14) 0.0029(14)
Cl1A 0.0230(3) 0.0255(3) 0.0312(3) 0.0193(3) 0.0009(2) 0.0049(2)
B1C 0.0221(13) 0.0186(13) 0.0222(13) 0.0115(11) 0.0080(11) 0.0074(10)
C11C 0.0173(11) 0.0216(12) 0.0253(12) 0.0136(10) 0.0074(9) 0.0079(9)
C12C 0.0235(12) 0.0242(12) 0.0246(12) 0.0139(10) 0.0103(10) 0.0087(9)
C13C 0.0224(12) 0.0205(12) 0.0324(13) 0.0131(11) 0.0076(10) 0.0070(9)
C14C 0.0289(13) 0.0274(13) 0.0417(15) 0.0246(12) 0.0116(11) 0.0080(10)
C15C 0.0247(12) 0.0312(13) 0.0302(13) 0.0200(11) 0.0101(10) 0.0094(10)
C16C 0.0232(12) 0.0236(12) 0.0249(12) 0.0134(10) 0.0096(10) 0.0087(9)
C17C 0.0390(16) 0.0251(14) 0.0463(17) 0.0168(13) 0.0128(13) 0.0102(12)
C18C 0.0398(16) 0.0418(16) 0.0407(16) 0.0284(14) 0.0180(13) 0.0105(13)
F1C 0.0738(13) 0.0395(10) 0.0399(10) 0.0046(8) 0.0092(9) 0.0255(9)
F2C 0.1145(18) 0.0215(9) 0.0941(16) 0.0220(10) 0.0544(14) 0.0079(10)
F3C 0.0524(11) 0.0500(11) 0.0784(14) 0.0027(10) 0.0013(10) 0.0362(9)
F4C 0.0349(10) 0.150(2) 0.0613(12) 0.0692(14) 0.0247(9) 0.0193(11)
F5C 0.0598(11) 0.0920(15) 0.0565(11) 0.0587(11) 0.0228(9) 0.0275(10)
F6C 0.153(2) 0.0551(12) 0.0446(11) 0.0254(10) 0.0570(13) 0.0240(13)
C21C 0.0243(12) 0.0188(11) 0.0261(12) 0.0159(10) 0.0099(10) 0.0088(9)
C22C 0.0266(12) 0.0216(12) 0.0228(12) 0.0145(10) 0.0089(10) 0.0089(9)
C23C 0.0276(13) 0.0240(12) 0.0306(13) 0.0190(11) 0.0138(11) 0.0124(10)
C24C 0.0199(11) 0.0261(12) 0.0351(14) 0.0214(11) 0.0084(10) 0.0073(10)
C25C 0.0262(12) 0.0197(12) 0.0279(13) 0.0154(10) 0.0062(10) 0.0063(9)
C26C 0.0260(12) 0.0203(12) 0.0243(12) 0.0134(10) 0.0092(10) 0.0093(9)
C27C 0.0324(14) 0.0431(16) 0.0371(15) 0.0244(13) 0.0175(12) 0.0208(12)
C28C 0.0295(13) 0.0237(13) 0.0334(14) 0.0144(11) 0.0047(11) 0.0075(10)
F7C 0.0676(12) 0.0901(14) 0.0464(10) 0.0479(10) 0.0371(9) 0.0488(11)
F8C 0.0581(11) 0.0407(10) 0.0698(12) 0.0134(9) 0.0345(10) 0.0264(9)
F9C 0.0333(9) 0.0795(13) 0.0461(10) 0.0313(9) 0.0204(8) 0.0324(9)
F10C 0.0321(9) 0.0572(11) 0.0459(10) 0.0079(9) -0.0083(8) 0.0140(8)
F11C 0.0576(10) 0.0379(9) 0.0273(8) 0.0176(7) 0.0061(7) 0.0056(7)
F12C 0.0609(11) 0.0202(8) 0.0400(9) 0.0118(7) 0.0050(8) 0.0065(7)
C31C 0.0212(11) 0.0198(11) 0.0183(11) 0.0106(9) 0.0039(9) 0.0068(9)
C32C 0.0206(12) 0.0200(12) 0.0260(12) 0.0108(10) 0.0037(10) 0.0045(9)
C33C 0.0217(12) 0.0265(13) 0.0265(13) 0.0104(11) 0.0063(10) 0.0092(10)
C34C 0.0313(13) 0.0215(12) 0.0252(13) 0.0083(10) 0.0066(11) 0.0127(10)
C35C 0.0285(13) 0.0186(12) 0.0205(12) 0.0088(10) 0.0040(10) 0.0055(10)
C36C 0.0219(12) 0.0229(12) 0.0206(12) 0.0116(10) 0.0072(9) 0.0069(9)
C37C 0.0315(15) 0.0334(16) 0.0478(18) 0.0108(14) 0.0166(13) 0.0133(12)
C38C 0.0407(15) 0.0211(13) 0.0314(14) 0.0097(11) 0.0109(12) 0.0064(11)
F13C 0.049(10) 0.059(7) 0.093(12) 0.054(8) 0.047(8) 0.025(6)
F14C 0.023(3) 0.080(9) 0.091(7) 0.039(6) 0.017(4) 0.024(6)
F15C 0.036(4) 0.037(3) 0.059(5) 0.020(4) 0.031(4) 0.027(3)
F131 0.019(7) 0.043(4) 0.061(11) 0.017(6) 0.014(7) 0.005(3)
F132 0.041(6) 0.074(8) 0.103(10) 0.054(6) 0.033(6) 0.047(7)
F13' 0.020(4) 0.078(8) 0.079(8) -0.008(6) 0.010(5) -0.001(6)
F14' 0.057(7) 0.062(5) 0.109(9) 0.050(6) 0.048(7) 0.046(5)
F15' 0.049(4) 0.107(6) 0.081(6) 0.068(5) 0.045(4) 0.032(4)
F16C 0.0884(15) 0.0252(9) 0.137(2) 0.0376(11) 0.0679(15) 0.0268(9)
F17C 0.0730(14) 0.0609(12) 0.0593(12) 0.0337(10) -0.0251(11) -0.0381(11)
F18C 0.0702(12) 0.0337(9) 0.0440(10) 0.0210(8) 0.0242(9) 0.0007(8)
C41C 0.0233(12) 0.0174(11) 0.0218(12) 0.0103(9) 0.0088(10) 0.0104(9)
C42C 0.0259(12) 0.0177(11) 0.0252(12) 0.0116(10) 0.0093(10) 0.0076(9)
C43C 0.0285(13) 0.0195(12) 0.0244(12) 0.0101(10) 0.0045(10) 0.0087(10)
C44C 0.0375(14) 0.0252(13) 0.0215(12) 0.0134(10) 0.0085(11) 0.0144(11)
C45C 0.0326(13) 0.0197(12) 0.0253(13) 0.0131(10) 0.0105(11) 0.0112(10)
C46C 0.0223(12) 0.0194(11) 0.0252(12) 0.0120(10) 0.0077(10) 0.0074(9)
C47C 0.0411(16) 0.0388(16) 0.0360(16) 0.0219(14) -0.0016(13) 0.0029(12)
C48C 0.0428(16) 0.0390(16) 0.0383(16) 0.0277(14) 0.0130(13) 0.0116(13)
F19C 0.0357(10) 0.1191(19) 0.0555(12) 0.0405(13) -0.0033(9) -0.0185(11)
F20C 0.0891(16) 0.0289(10) 0.0827(15) 0.0061(10) -0.0325(12) -0.0018(10)
F21C 0.0526(11) 0.0714(13) 0.0565(11) 0.0441(11) -0.0187(9) -0.0068(9)
F22C 0.0626(11) 0.0628(11) 0.0515(10) 0.0477(10) 0.0072(9) 0.0025(9)
F23C 0.0648(13) 0.1095(18) 0.140(2) 0.1008(17) 0.0691(14) 0.0474(13)
F24C 0.0985(16) 0.0457(11) 0.0474(11) 0.0252(9) 0.0077(10) -0.0276(10)
C1D 0.074(5) 0.083(6) 0.063(5) 0.035(5) 0.016(4) 0.054(5)
Cl1D 0.079(2) 0.231(7) 0.117(3) 0.076(4) 0.021(2) 0.032(3)
Cl2D 0.147(4) 0.0803(19) 0.084(2) 0.0321(16) 0.005(2) 0.050(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N3' 2.0809(18) . ?
Rh1 N2 2.1291(19) . ?
Rh1 C2B 2.132(2) . ?
Rh1 C5B 2.144(2) . ?
Rh1 C1B 2.154(2) . ?
Rh1 C4B 2.159(2) . ?
Rh1 C3B 2.159(2) . ?
Rh1 Cl1A 2.4031(6) . ?
N1 C5 1.346(3) . ?
N1 N2 1.358(3) . ?
N1 C1A 1.453(3) . ?
N2 C3 1.334(3) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.504(3) . ?
C1A H1A1 0.9900 . ?
C1A H2A1 0.9900 . ?
N1' N2' 1.333(3) . ?
N1' C5' 1.346(3) . ?
N1' C6' 1.473(3) . ?
N2' N3' 1.313(3) . ?
N3' C4' 1.360(3) . ?
C4' C5' 1.362(3) . ?
C5' H5' 0.9500 . ?
C6' C7' 1.505(3) . ?
C6' H16' 0.9900 . ?
C6' H26' 0.9900 . ?
C7' C8' 1.375(3) . ?
C7' C12' 1.388(4) . ?
C8' C9' 1.391(4) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.361(4) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.383(4) . ?
C10' H10' 0.9500 . ?
C11' C12' 1.382(4) . ?
C11' H11' 0.9500 . ?
C12' H12' 0.9500 . ?
C1B C2B 1.424(3) . ?
C1B C5B 1.431(3) . ?
C1B C6B 1.491(3) . ?
C2B C3B 1.442(4) . ?
C2B C7B 1.501(4) . ?
C3B C4B 1.412(4) . ?
C3B C8B 1.494(4) . ?
C4B C5B 1.445(4) . ?
C4B C9B 1.494(4) . ?
C5B C10B 1.494(4) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
C10B H10D 0.9800 . ?
B1C C41C 1.636(3) . ?
B1C C11C 1.638(3) . ?
B1C C31C 1.639(3) . ?
B1C C21C 1.641(3) . ?
C11C C16C 1.397(3) . ?
C11C C12C 1.401(3) . ?
C12C C13C 1.389(3) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.383(4) . ?
C13C C17C 1.490(4) . ?
C14C C15C 1.385(4) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.391(3) . ?
C15C C18C 1.494(4) . ?
C16C H16C 0.9500 . ?
C17C F3C 1.319(3) . ?
C17C F2C 1.324(3) . ?
C17C F1C 1.340(3) . ?
C18C F6C 1.318(3) . ?
C18C F4C 1.321(3) . ?
C18C F5C 1.340(3) . ?
C21C C26C 1.394(3) . ?
C21C C22C 1.399(3) . ?
C22C C23C 1.387(3) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.385(3) . ?
C23C C27C 1.500(3) . ?
C24C C25C 1.386(3) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.391(3) . ?
C25C C28C 1.491(3) . ?
C26C H26C 0.9500 . ?
C27C F9C 1.327(3) . ?
C27C F7C 1.336(3) . ?
C27C F8C 1.339(3) . ?
C28C F10C 1.332(3) . ?
C28C F12C 1.341(3) . ?
C28C F11C 1.342(3) . ?
C31C C32C 1.397(3) . ?
C31C C36C 1.398(3) . ?
C32C C33C 1.387(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.392(3) . ?
C33C C37C 1.489(4) . ?
C34C C35C 1.383(3) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.384(3) . ?
C35C C38C 1.491(3) . ?
C36C H36C 0.9500 . ?
C37C F13' 1.282(10) . ?
C37C F15C 1.310(7) . ?
C37C F13C 1.312(12) . ?
C37C F14' 1.317(9) . ?
C37C F133 1.325(8) . ?
C37C F131 1.342(13) . ?
C37C F132 1.343(9) . ?
C37C F14C 1.395(10) . ?
C37C F15' 1.418(7) . ?
C38C F17C 1.321(3) . ?
C38C F18C 1.327(3) . ?
C38C F16C 1.329(3) . ?
C41C C42C 1.394(3) . ?
C41C C46C 1.404(3) . ?
C42C C43C 1.396(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.387(3) . ?
C43C C47C 1.491(4) . ?
C44C C45C 1.383(3) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.386(3) . ?
C45C C48C 1.499(3) . ?
C46C H46C 0.9500 . ?
C47C F19C 1.321(3) . ?
C47C F21C 1.327(3) . ?
C47C F20C 1.337(3) . ?
C48C F24C 1.317(3) . ?
C48C F22C 1.322(3) . ?
C48C F23C 1.331(3) . ?
C1D C1D 1.365(13) 2_665 ?
C1D Cl1D 1.430(11) 2_665 ?
C1D Cl1D 1.771(11) . ?
C1D Cl2D 1.798(11) 2_665 ?
C1D H1D1 0.9900 . ?
C1D H1D2 0.9900 . ?
Cl1D Cl2D 0.811(5) . ?
Cl1D C1D 1.430(11) 2_665 ?
Cl2D C1D 1.798(11) 2_665 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3' Rh1 N2 84.00(7) . . ?
N3' Rh1 C2B 113.98(8) . . ?
N2 Rh1 C2B 161.47(9) . . ?
N3' Rh1 C5B 109.74(8) . . ?
N2 Rh1 C5B 105.20(8) . . ?
C2B Rh1 C5B 65.63(9) . . ?
N3' Rh1 C1B 94.24(8) . . ?
N2 Rh1 C1B 140.79(9) . . ?
C2B Rh1 C1B 38.80(9) . . ?
C5B Rh1 C1B 38.90(9) . . ?
N3' Rh1 C4B 148.32(9) . . ?
N2 Rh1 C4B 97.31(8) . . ?
C2B Rh1 C4B 65.18(9) . . ?
C5B Rh1 C4B 39.24(9) . . ?
C1B Rh1 C4B 64.93(9) . . ?
N3' Rh1 C3B 153.23(9) . . ?
N2 Rh1 C3B 122.75(9) . . ?
C2B Rh1 C3B 39.28(10) . . ?
C5B Rh1 C3B 65.16(9) . . ?
C1B Rh1 C3B 64.90(9) . . ?
C4B Rh1 C3B 38.17(10) . . ?
N3' Rh1 Cl1A 88.99(5) . . ?
N2 Rh1 Cl1A 87.71(6) . . ?
C2B Rh1 Cl1A 96.66(7) . . ?
C5B Rh1 Cl1A 157.98(7) . . ?
C1B Rh1 Cl1A 131.48(7) . . ?
C4B Rh1 Cl1A 122.67(7) . . ?
C3B Rh1 Cl1A 92.88(7) . . ?
C5 N1 N2 110.9(2) . . ?
C5 N1 C1A 128.2(2) . . ?
N2 N1 C1A 120.87(18) . . ?
C3 N2 N1 105.41(19) . . ?
C3 N2 Rh1 128.67(17) . . ?
N1 N2 Rh1 125.59(14) . . ?
N2 C3 C4 110.8(2) . . ?
N2 C3 H3 124.6 . . ?
C4 C3 H3 124.6 . . ?
C5 C4 C3 105.4(2) . . ?
C5 C4 H4 127.3 . . ?
C3 C4 H4 127.3 . . ?
N1 C5 C4 107.4(2) . . ?
N1 C5 H5 126.3 . . ?
C4 C5 H5 126.3 . . ?
N1 C1A C4' 111.90(19) . . ?
N1 C1A H1A1 109.2 . . ?
C4' C1A H1A1 109.2 . . ?
N1 C1A H2A1 109.2 . . ?
C4' C1A H2A1 109.2 . . ?
H1A1 C1A H2A1 107.9 . . ?
N2' N1' C5' 111.91(18) . . ?
N2' N1' C6' 118.77(18) . . ?
C5' N1' C6' 129.0(2) . . ?
N3' N2' N1' 105.57(17) . . ?
N2' N3' C4' 110.54(18) . . ?
N2' N3' Rh1 122.60(14) . . ?
C4' N3' Rh1 126.84(15) . . ?
N3' C4' C5' 107.02(19) . . ?
N3' C4' C1A 120.11(19) . . ?
C5' C4' C1A 132.8(2) . . ?
N1' C5' C4' 104.97(19) . . ?
N1' C5' H5' 127.5 . . ?
C4' C5' H5' 127.5 . . ?
N1' C6' C7' 111.37(19) . . ?
N1' C6' H16' 109.4 . . ?
C7' C6' H16' 109.4 . . ?
N1' C6' H26' 109.4 . . ?
C7' C6' H26' 109.4 . . ?
H16' C6' H26' 108.0 . . ?
C8' C7' C12' 118.9(2) . . ?
C8' C7' C6' 120.6(2) . . ?
C12' C7' C6' 120.5(2) . . ?
C7' C8' C9' 120.5(3) . . ?
C7' C8' H8' 119.7 . . ?
C9' C8' H8' 119.7 . . ?
C10' C9' C8' 120.2(3) . . ?
C10' C9' H9' 119.9 . . ?
C8' C9' H9' 119.9 . . ?
C9' C10' C11' 120.0(3) . . ?
C9' C10' H10' 120.0 . . ?
C11' C10' H10' 120.0 . . ?
C12' C11' C10' 120.0(3) . . ?
C12' C11' H11' 120.0 . . ?
C10' C11' H11' 120.0 . . ?
C11' C12' C7' 120.4(3) . . ?
C11' C12' H12' 119.8 . . ?
C7' C12' H12' 119.8 . . ?
C2B C1B C5B 108.5(2) . . ?
C2B C1B C6B 125.9(2) . . ?
C5B C1B C6B 125.6(2) . . ?
C2B C1B Rh1 69.75(13) . . ?
C5B C1B Rh1 70.16(13) . . ?
C6B C1B Rh1 125.47(17) . . ?
C1B C2B C3B 107.7(2) . . ?
C1B C2B C7B 126.0(2) . . ?
C3B C2B C7B 126.2(2) . . ?
C1B C2B Rh1 71.45(13) . . ?
C3B C2B Rh1 71.40(13) . . ?
C7B C2B Rh1 126.03(17) . . ?
C4B C3B C2B 108.1(2) . . ?
C4B C3B C8B 126.5(3) . . ?
C2B C3B C8B 125.3(3) . . ?
C4B C3B Rh1 70.89(13) . . ?
C2B C3B Rh1 69.32(13) . . ?
C8B C3B Rh1 126.69(18) . . ?
C3B C4B C5B 108.4(2) . . ?
C3B C4B C9B 126.0(3) . . ?
C5B C4B C9B 125.5(3) . . ?
C3B C4B Rh1 70.95(13) . . ?
C5B C4B Rh1 69.83(13) . . ?
C9B C4B Rh1 124.86(18) . . ?
C1B C5B C4B 107.2(2) . . ?
C1B C5B C10B 126.0(2) . . ?
C4B C5B C10B 126.5(2) . . ?
C1B C5B Rh1 70.94(13) . . ?
C4B C5B Rh1 70.93(13) . . ?
C10B C5B Rh1 128.75(17) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C5B C10B H10D 109.5 . . ?
H10B C10B H10D 109.5 . . ?
H10C C10B H10D 109.5 . . ?
C41C B1C C11C 113.74(19) . . ?
C41C B1C C31C 103.55(17) . . ?
C11C B1C C31C 114.75(18) . . ?
C41C B1C C21C 111.11(18) . . ?
C11C B1C C21C 103.22(17) . . ?
C31C B1C C21C 110.68(18) . . ?
C16C C11C C12C 115.6(2) . . ?
C16C C11C B1C 122.8(2) . . ?
C12C C11C B1C 120.88(19) . . ?
C13C C12C C11C 122.4(2) . . ?
C13C C12C H12C 118.8 . . ?
C11C C12C H12C 118.8 . . ?
C14C C13C C12C 120.7(2) . . ?
C14C C13C C17C 119.7(2) . . ?
C12C C13C C17C 119.5(2) . . ?
C13C C14C C15C 118.3(2) . . ?
C13C C14C H14C 120.9 . . ?
C15C C14C H14C 120.9 . . ?
C14C C15C C16C 120.7(2) . . ?
C14C C15C C18C 118.7(2) . . ?
C16C C15C C18C 120.6(2) . . ?
C15C C16C C11C 122.3(2) . . ?
C15C C16C H16C 118.8 . . ?
C11C C16C H16C 118.8 . . ?
F3C C17C F2C 107.9(2) . . ?
F3C C17C F1C 104.9(2) . . ?
F2C C17C F1C 104.6(2) . . ?
F3C C17C C13C 112.1(2) . . ?
F2C C17C C13C 113.6(2) . . ?
F1C C17C C13C 113.0(2) . . ?
F6C C18C F4C 108.8(3) . . ?
F6C C18C F5C 104.3(2) . . ?
F4C C18C F5C 104.5(2) . . ?
F6C C18C C15C 113.9(2) . . ?
F4C C18C C15C 112.9(2) . . ?
F5C C18C C15C 111.7(2) . . ?
C26C C21C C22C 115.7(2) . . ?
C26C C21C B1C 121.8(2) . . ?
C22C C21C B1C 122.4(2) . . ?
C23C C22C C21C 122.2(2) . . ?
C23C C22C H22C 118.9 . . ?
C21C C22C H22C 118.9 . . ?
C24C C23C C22C 121.0(2) . . ?
C24C C23C C27C 121.0(2) . . ?
C22C C23C C27C 118.0(2) . . ?
C23C C24C C25C 117.9(2) . . ?
C23C C24C H24C 121.0 . . ?
C25C C24C H24C 121.0 . . ?
C24C C25C C26C 120.7(2) . . ?
C24C C25C C28C 121.1(2) . . ?
C26C C25C C28C 118.1(2) . . ?
C25C C26C C21C 122.4(2) . . ?
C25C C26C H26C 118.8 . . ?
C21C C26C H26C 118.8 . . ?
F9C C27C F7C 106.7(2) . . ?
F9C C27C F8C 106.5(2) . . ?
F7C C27C F8C 104.9(2) . . ?
F9C C27C C23C 113.7(2) . . ?
F7C C27C C23C 112.4(2) . . ?
F8C C27C C23C 112.1(2) . . ?
F10C C28C F12C 107.2(2) . . ?
F10C C28C F11C 106.3(2) . . ?
F12C C28C F11C 104.6(2) . . ?
F10C C28C C25C 113.5(2) . . ?
F12C C28C C25C 112.0(2) . . ?
F11C C28C C25C 112.7(2) . . ?
C32C C31C C36C 115.7(2) . . ?
C32C C31C B1C 124.36(19) . . ?
C36C C31C B1C 119.57(19) . . ?
C33C C32C C31C 122.2(2) . . ?
C33C C32C H32C 118.9 . . ?
C31C C32C H32C 118.9 . . ?
C32C C33C C34C 121.0(2) . . ?
C32C C33C C37C 120.2(2) . . ?
C34C C33C C37C 118.8(2) . . ?
C35C C34C C33C 117.5(2) . . ?
C35C C34C H34C 121.2 . . ?
C33C C34C H34C 121.2 . . ?
C34C C35C C36C 121.2(2) . . ?
C34C C35C C38C 120.6(2) . . ?
C36C C35C C38C 118.2(2) . . ?
C35C C36C C31C 122.3(2) . . ?
C35C C36C H36C 118.8 . . ?
C31C C36C H36C 118.8 . . ?
F13' C37C F15C 131.3(7) . . ?
F13' C37C F13C 56.9(9) . . ?
F15C C37C F13C 108.7(8) . . ?
F13' C37C F14' 113.6(8) . . ?
F15C C37C F14' 35.0(5) . . ?
F13C C37C F14' 129.2(10) . . ?
F13' C37C F133 127.7(8) . . ?
F15C C37C F133 32.3(4) . . ?
F13C C37C F133 81.9(8) . . ?
F14' C37C F133 66.9(6) . . ?
F13' C37C F131 32.9(7) . . ?
F15C C37C F131 125.2(8) . . ?
F13C C37C F131 24.4(8) . . ?
F14' C37C F131 130.8(9) . . ?
F133 C37C F131 104.1(8) . . ?
F13' C37C F132 75.6(8) . . ?
F15C C37C F132 76.6(6) . . ?
F13C C37C F132 121.0(9) . . ?
F14' C37C F132 43.1(5) . . ?
F133 C37C F132 105.8(7) . . ?
F131 C37C F132 104.4(8) . . ?
F13' C37C F14C 48.8(7) . . ?
F15C C37C F14C 104.9(6) . . ?
F13C C37C F14C 102.9(8) . . ?
F14' C37C F14C 72.6(7) . . ?
F133 C37C F14C 129.8(6) . . ?
F131 C37C F14C 80.9(8) . . ?
F132 C37C F14C 29.7(5) . . ?
F13' C37C F15' 105.5(8) . . ?
F15C C37C F15' 68.9(5) . . ?
F13C C37C F15' 49.7(6) . . ?
F14' C37C F15' 102.7(7) . . ?
F133 C37C F15' 36.9(4) . . ?
F131 C37C F15' 74.0(7) . . ?
F132 C37C F15' 134.1(6) . . ?
F14C C37C F15' 141.5(6) . . ?
F13' C37C C33C 113.1(6) . . ?
F15C C37C C33C 114.6(4) . . ?
F13C C37C C33C 115.1(9) . . ?
F14' C37C C33C 113.7(5) . . ?
F133 C37C C33C 113.1(4) . . ?
F131 C37C C33C 114.0(8) . . ?
F132 C37C C33C 114.4(5) . . ?
F14C C37C C33C 109.6(5) . . ?
F15' C37C C33C 107.2(3) . . ?
F17C C38C F18C 104.9(2) . . ?
F17C C38C F16C 106.7(2) . . ?
F18C C38C F16C 105.4(2) . . ?
F17C C38C C35C 112.9(2) . . ?
F18C C38C C35C 113.2(2) . . ?
F16C C38C C35C 113.0(2) . . ?
C42C C41C C46C 115.5(2) . . ?
C42C C41C B1C 123.84(19) . . ?
C46C C41C B1C 120.1(2) . . ?
C41C C42C C43C 122.2(2) . . ?
C41C C42C H42C 118.9 . . ?
C43C C42C H42C 118.9 . . ?
C44C C43C C42C 120.9(2) . . ?
C44C C43C C47C 120.0(2) . . ?
C42C C43C C47C 119.0(2) . . ?
C45C C44C C43C 118.0(2) . . ?
C45C C44C H44C 121.0 . . ?
C43C C44C H44C 121.0 . . ?
C44C C45C C46C 120.8(2) . . ?
C44C C45C C48C 121.1(2) . . ?
C46C C45C C48C 118.1(2) . . ?
C45C C46C C41C 122.7(2) . . ?
C45C C46C H46C 118.7 . . ?
C41C C46C H46C 118.7 . . ?
F19C C47C F21C 106.9(2) . . ?
F19C C47C F20C 103.7(2) . . ?
F21C C47C F20C 105.7(2) . . ?
F19C C47C C43C 113.7(2) . . ?
F21C C47C C43C 114.0(2) . . ?
F20C C47C C43C 112.0(2) . . ?
F24C C48C F22C 107.3(2) . . ?
F24C C48C F23C 106.2(3) . . ?
F22C C48C F23C 104.7(2) . . ?
F24C C48C C45C 112.9(2) . . ?
F22C C48C C45C 113.5(2) . . ?
F23C C48C C45C 111.7(2) . . ?
C1D C1D Cl1D 78.6(9) 2_665 2_665 ?
C1D C1D Cl1D 52.3(7) 2_665 . ?
Cl1D C1D Cl1D 130.9(5) 2_665 . ?
C1D C1D Cl2D 53.8(7) 2_665 2_665 ?
Cl1D C1D Cl2D 26.1(3) 2_665 2_665 ?
Cl1D C1D Cl2D 105.6(4) . 2_665 ?
C1D C1D H1D1 115.5 2_665 . ?
Cl1D C1D H1D1 115.5 2_665 . ?
Cl1D C1D H1D1 89.1 . . ?
Cl2D C1D H1D1 115.6 2_665 . ?
C1D C1D H1D2 115.5 2_665 . ?
Cl1D C1D H1D2 115.5 2_665 . ?
Cl1D C1D H1D2 89.1 . . ?
Cl2D C1D H1D2 129.6 2_665 . ?
H1D1 C1D H1D2 112.5 . . ?
Cl2D Cl1D C1D 103.2(7) . 2_665 ?
Cl2D Cl1D C1D 56.2(6) . . ?
C1D Cl1D C1D 49.1(5) 2_665 . ?
Cl1D Cl2D C1D 50.8(6) . 2_665 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 C3 0.5(3) . . . . ?
C1A N1 N2 C3 178.0(2) . . . . ?
C5 N1 N2 Rh1 174.36(16) . . . . ?
C1A N1 N2 Rh1 -8.2(3) . . . . ?
N3' Rh1 N2 C3 145.1(2) . . . . ?
C2B Rh1 N2 C3 -48.4(4) . . . . ?
C5B Rh1 N2 C3 -106.0(2) . . . . ?
C1B Rh1 N2 C3 -125.5(2) . . . . ?
C4B Rh1 N2 C3 -66.8(2) . . . . ?
C3B Rh1 N2 C3 -36.1(2) . . . . ?
Cl1A Rh1 N2 C3 55.9(2) . . . . ?
N3' Rh1 N2 N1 -27.27(18) . . . . ?
C2B Rh1 N2 N1 139.3(3) . . . . ?
C5B Rh1 N2 N1 81.60(19) . . . . ?
C1B Rh1 N2 N1 62.1(2) . . . . ?
C4B Rh1 N2 N1 120.86(18) . . . . ?
C3B Rh1 N2 N1 151.55(17) . . . . ?
Cl1A Rh1 N2 N1 -116.49(17) . . . . ?
N1 N2 C3 C4 -0.7(3) . . . . ?
Rh1 N2 C3 C4 -174.28(17) . . . . ?
N2 C3 C4 C5 0.6(3) . . . . ?
N2 N1 C5 C4 -0.2(3) . . . . ?
C1A N1 C5 C4 -177.4(2) . . . . ?
C3 C4 C5 N1 -0.3(3) . . . . ?
C5 N1 C1A C4' -128.7(2) . . . . ?
N2 N1 C1A C4' 54.4(3) . . . . ?
C5' N1' N2' N3' 0.1(3) . . . . ?
C6' N1' N2' N3' 174.24(19) . . . . ?
N1' N2' N3' C4' -0.3(2) . . . . ?
N1' N2' N3' Rh1 177.97(14) . . . . ?
N2 Rh1 N3' N2' -149.78(17) . . . . ?
C2B Rh1 N3' N2' 34.87(19) . . . . ?
C5B Rh1 N3' N2' 106.19(17) . . . . ?
C1B Rh1 N3' N2' 69.56(18) . . . . ?
C4B Rh1 N3' N2' 116.0(2) . . . . ?
C3B Rh1 N3' N2' 32.4(3) . . . . ?
Cl1A Rh1 N3' N2' -61.97(16) . . . . ?
N2 Rh1 N3' C4' 28.21(19) . . . . ?
C2B Rh1 N3' C4' -147.14(18) . . . . ?
C5B Rh1 N3' C4' -75.8(2) . . . . ?
C1B Rh1 N3' C4' -112.45(19) . . . . ?
C4B Rh1 N3' C4' -66.0(3) . . . . ?
C3B Rh1 N3' C4' -149.6(2) . . . . ?
Cl1A Rh1 N3' C4' 116.02(18) . . . . ?
N2' N3' C4' C5' 0.4(3) . . . . ?
Rh1 N3' C4' C5' -177.82(16) . . . . ?
N2' N3' C4' C1A -176.6(2) . . . . ?
Rh1 N3' C4' C1A 5.2(3) . . . . ?
N1 C1A C4' N3' -53.2(3) . . . . ?
N1 C1A C4' C5' 130.7(3) . . . . ?
N2' N1' C5' C4' 0.1(3) . . . . ?
C6' N1' C5' C4' -173.3(2) . . . . ?
N3' C4' C5' N1' -0.3(3) . . . . ?
C1A C4' C5' N1' 176.2(2) . . . . ?
N2' N1' C6' C7' -86.6(3) . . . . ?
C5' N1' C6' C7' 86.4(3) . . . . ?
N1' C6' C7' C8' 99.4(3) . . . . ?
N1' C6' C7' C12' -78.6(3) . . . . ?
C12' C7' C8' C9' -2.0(4) . . . . ?
C6' C7' C8' C9' -180.0(2) . . . . ?
C7' C8' C9' C10' 0.2(4) . . . . ?
C8' C9' C10' C11' 1.9(4) . . . . ?
C9' C10' C11' C12' -2.1(4) . . . . ?
C10' C11' C12' C7' 0.3(4) . . . . ?
C8' C7' C12' C11' 1.7(4) . . . . ?
C6' C7' C12' C11' 179.8(2) . . . . ?
N3' Rh1 C1B C2B -123.93(14) . . . . ?
N2 Rh1 C1B C2B 150.36(14) . . . . ?
C5B Rh1 C1B C2B 119.5(2) . . . . ?
C4B Rh1 C1B C2B 80.92(15) . . . . ?
C3B Rh1 C1B C2B 38.59(14) . . . . ?
Cl1A Rh1 C1B C2B -31.53(17) . . . . ?
N3' Rh1 C1B C5B 116.57(14) . . . . ?
N2 Rh1 C1B C5B 30.86(19) . . . . ?
C2B Rh1 C1B C5B -119.5(2) . . . . ?
C4B Rh1 C1B C5B -38.58(14) . . . . ?
C3B Rh1 C1B C5B -80.90(15) . . . . ?
Cl1A Rh1 C1B C5B -151.03(11) . . . . ?
N3' Rh1 C1B C6B -3.6(2) . . . . ?
N2 Rh1 C1B C6B -89.3(3) . . . . ?
C2B Rh1 C1B C6B 120.4(3) . . . . ?
C5B Rh1 C1B C6B -120.1(3) . . . . ?
C4B Rh1 C1B C6B -158.7(3) . . . . ?
C3B Rh1 C1B C6B 159.0(3) . . . . ?
Cl1A Rh1 C1B C6B 88.8(2) . . . . ?
C5B C1B C2B C3B -2.9(3) . . . . ?
C6B C1B C2B C3B 177.6(2) . . . . ?
Rh1 C1B C2B C3B -62.59(15) . . . . ?
C5B C1B C2B C7B -178.8(2) . . . . ?
C6B C1B C2B C7B 1.8(4) . . . . ?
Rh1 C1B C2B C7B 121.5(2) . . . . ?
C5B C1B C2B Rh1 59.68(16) . . . . ?
C6B C1B C2B Rh1 -119.8(2) . . . . ?
N3' Rh1 C2B C1B 64.91(15) . . . . ?
N2 Rh1 C2B C1B -100.4(3) . . . . ?
C5B Rh1 C2B C1B -36.88(14) . . . . ?
C4B Rh1 C2B C1B -80.22(15) . . . . ?
C3B Rh1 C2B C1B -116.8(2) . . . . ?
Cl1A Rh1 C2B C1B 156.77(13) . . . . ?
N3' Rh1 C2B C3B -178.26(13) . . . . ?
N2 Rh1 C2B C3B 16.4(3) . . . . ?
C5B Rh1 C2B C3B 79.96(15) . . . . ?
C1B Rh1 C2B C3B 116.8(2) . . . . ?
C4B Rh1 C2B C3B 36.61(14) . . . . ?
Cl1A Rh1 C2B C3B -86.40(13) . . . . ?
N3' Rh1 C2B C7B -56.6(3) . . . . ?
N2 Rh1 C2B C7B 138.1(3) . . . . ?
C5B Rh1 C2B C7B -158.4(3) . . . . ?
C1B Rh1 C2B C7B -121.5(3) . . . . ?
C4B Rh1 C2B C7B 158.3(3) . . . . ?
C3B Rh1 C2B C7B 121.7(3) . . . . ?
Cl1A Rh1 C2B C7B 35.3(2) . . . . ?
C1B C2B C3B C4B 2.1(3) . . . . ?
C7B C2B C3B C4B 177.9(2) . . . . ?
Rh1 C2B C3B C4B -60.55(16) . . . . ?
C1B C2B C3B C8B -176.4(2) . . . . ?
C7B C2B C3B C8B -0.5(4) . . . . ?
Rh1 C2B C3B C8B 121.0(2) . . . . ?
C1B C2B C3B Rh1 62.63(15) . . . . ?
C7B C2B C3B Rh1 -121.5(2) . . . . ?
N3' Rh1 C3B C4B 122.4(2) . . . . ?
N2 Rh1 C3B C4B -55.02(16) . . . . ?
C2B Rh1 C3B C4B 118.8(2) . . . . ?
C5B Rh1 C3B C4B 37.61(14) . . . . ?
C1B Rh1 C3B C4B 80.71(15) . . . . ?
Cl1A Rh1 C3B C4B -144.15(13) . . . . ?
N3' Rh1 C3B C2B 3.5(3) . . . . ?
N2 Rh1 C3B C2B -173.87(13) . . . . ?
C5B Rh1 C3B C2B -81.23(15) . . . . ?
C1B Rh1 C3B C2B -38.13(14) . . . . ?
C4B Rh1 C3B C2B -118.8(2) . . . . ?
Cl1A Rh1 C3B C2B 97.00(13) . . . . ?
N3' Rh1 C3B C8B -115.8(3) . . . . ?
N2 Rh1 C3B C8B 66.8(3) . . . . ?
C2B Rh1 C3B C8B -119.3(3) . . . . ?
C5B Rh1 C3B C8B 159.4(3) . . . . ?
C1B Rh1 C3B C8B -157.5(3) . . . . ?
C4B Rh1 C3B C8B 121.8(3) . . . . ?
Cl1A Rh1 C3B C8B -22.3(3) . . . . ?
C2B C3B C4B C5B -0.5(3) . . . . ?
C8B C3B C4B C5B 178.0(2) . . . . ?
Rh1 C3B C4B C5B -60.02(16) . . . . ?
C2B C3B C4B C9B 179.3(2) . . . . ?
C8B C3B C4B C9B -2.3(4) . . . . ?
Rh1 C3B C4B C9B 119.8(2) . . . . ?
C2B C3B C4B Rh1 59.57(16) . . . . ?
C8B C3B C4B Rh1 -122.0(2) . . . . ?
N3' Rh1 C4B C3B -133.59(17) . . . . ?
N2 Rh1 C4B C3B 135.99(14) . . . . ?
C2B Rh1 C4B C3B -37.66(14) . . . . ?
C5B Rh1 C4B C3B -118.9(2) . . . . ?
C1B Rh1 C4B C3B -80.64(15) . . . . ?
Cl1A Rh1 C4B C3B 44.01(16) . . . . ?
N3' Rh1 C4B C5B -14.7(2) . . . . ?
N2 Rh1 C4B C5B -105.12(14) . . . . ?
C2B Rh1 C4B C5B 81.23(15) . . . . ?
C1B Rh1 C4B C5B 38.25(14) . . . . ?
C3B Rh1 C4B C5B 118.9(2) . . . . ?
Cl1A Rh1 C4B C5B 162.90(11) . . . . ?
N3' Rh1 C4B C9B 105.2(3) . . . . ?
N2 Rh1 C4B C9B 14.8(3) . . . . ?
C2B Rh1 C4B C9B -158.8(3) . . . . ?
C5B Rh1 C4B C9B 119.9(3) . . . . ?
C1B Rh1 C4B C9B 158.2(3) . . . . ?
C3B Rh1 C4B C9B -121.2(3) . . . . ?
Cl1A Rh1 C4B C9B -77.2(3) . . . . ?
C2B C1B C5B C4B 2.6(3) . . . . ?
C6B C1B C5B C4B -177.9(2) . . . . ?
Rh1 C1B C5B C4B 62.05(15) . . . . ?
C2B C1B C5B C10B 176.0(2) . . . . ?
C6B C1B C5B C10B -4.5(4) . . . . ?
Rh1 C1B C5B C10B -124.6(2) . . . . ?
C2B C1B C5B Rh1 -59.43(16) . . . . ?
C6B C1B C5B Rh1 120.0(2) . . . . ?
C3B C4B C5B C1B -1.3(3) . . . . ?
C9B C4B C5B C1B 178.9(2) . . . . ?
Rh1 C4B C5B C1B -62.05(15) . . . . ?
C3B C4B C5B C10B -174.7(2) . . . . ?
C9B C4B C5B C10B 5.5(4) . . . . ?
Rh1 C4B C5B C10B 124.6(2) . . . . ?
C3B C4B C5B Rh1 60.73(16) . . . . ?
C9B C4B C5B Rh1 -119.1(2) . . . . ?
N3' Rh1 C5B C1B -71.37(14) . . . . ?
N2 Rh1 C5B C1B -160.36(13) . . . . ?
C2B Rh1 C5B C1B 36.79(14) . . . . ?
C4B Rh1 C5B C1B 116.8(2) . . . . ?
C3B Rh1 C5B C1B 80.17(15) . . . . ?
Cl1A Rh1 C5B C1B 75.5(2) . . . . ?
N3' Rh1 C5B C4B 171.86(13) . . . . ?
N2 Rh1 C5B C4B 82.86(14) . . . . ?
C2B Rh1 C5B C4B -79.99(15) . . . . ?
C1B Rh1 C5B C4B -116.8(2) . . . . ?
C3B Rh1 C5B C4B -36.60(14) . . . . ?
Cl1A Rh1 C5B C4B -41.3(3) . . . . ?
N3' Rh1 C5B C10B 49.9(3) . . . . ?
N2 Rh1 C5B C10B -39.1(3) . . . . ?
C2B Rh1 C5B C10B 158.1(3) . . . . ?
C1B Rh1 C5B C10B 121.3(3) . . . . ?
C4B Rh1 C5B C10B -121.9(3) . . . . ?
C3B Rh1 C5B C10B -158.5(3) . . . . ?
Cl1A Rh1 C5B C10B -163.24(19) . . . . ?
C41C B1C C11C C16C 149.7(2) . . . . ?
C31C B1C C11C C16C 30.7(3) . . . . ?
C21C B1C C11C C16C -89.8(2) . . . . ?
C41C B1C C11C C12C -40.4(3) . . . . ?
C31C B1C C11C C12C -159.4(2) . . . . ?
C21C B1C C11C C12C 80.1(2) . . . . ?
C16C C11C C12C C13C -0.1(3) . . . . ?
B1C C11C C12C C13C -170.8(2) . . . . ?
C11C C12C C13C C14C -1.2(4) . . . . ?
C11C C12C C13C C17C 175.0(2) . . . . ?
C12C C13C C14C C15C 1.1(4) . . . . ?
C17C C13C C14C C15C -175.1(2) . . . . ?
C13C C14C C15C C16C 0.4(4) . . . . ?
C13C C14C C15C C18C -179.6(2) . . . . ?
C14C C15C C16C C11C -1.8(4) . . . . ?
C18C C15C C16C C11C 178.2(2) . . . . ?
C12C C11C C16C C15C 1.6(3) . . . . ?
B1C C11C C16C C15C 172.1(2) . . . . ?
C14C C13C C17C F3C 94.9(3) . . . . ?
C12C C13C C17C F3C -81.4(3) . . . . ?
C14C C13C C17C F2C -27.8(4) . . . . ?
C12C C13C C17C F2C 155.9(2) . . . . ?
C14C C13C C17C F1C -146.8(2) . . . . ?
C12C C13C C17C F1C 36.9(3) . . . . ?
C14C C15C C18C F6C -166.0(2) . . . . ?
C16C C15C C18C F6C 14.0(4) . . . . ?
C14C C15C C18C F4C 69.3(3) . . . . ?
C16C C15C C18C F4C -110.7(3) . . . . ?
C14C C15C C18C F5C -48.1(3) . . . . ?
C16C C15C C18C F5C 131.9(2) . . . . ?
C41C B1C C21C C26C -149.1(2) . . . . ?
C11C B1C C21C C26C 88.7(2) . . . . ?
C31C B1C C21C C26C -34.6(3) . . . . ?
C41C B1C C21C C22C 35.3(3) . . . . ?
C11C B1C C21C C22C -87.0(2) . . . . ?
C31C B1C C21C C22C 149.8(2) . . . . ?
C26C C21C C22C C23C 1.1(3) . . . . ?
B1C C21C C22C C23C 176.9(2) . . . . ?
C21C C22C C23C C24C 0.2(3) . . . . ?
C21C C22C C23C C27C 179.2(2) . . . . ?
C22C C23C C24C C25C -1.1(3) . . . . ?
C27C C23C C24C C25C 179.9(2) . . . . ?
C23C C24C C25C C26C 0.8(3) . . . . ?
C23C C24C C25C C28C 177.9(2) . . . . ?
C24C C25C C26C C21C 0.6(3) . . . . ?
C28C C25C C26C C21C -176.6(2) . . . . ?
C22C C21C C26C C25C -1.5(3) . . . . ?
B1C C21C C26C C25C -177.4(2) . . . . ?
C24C C23C C27C F9C -3.6(3) . . . . ?
C22C C23C C27C F9C 177.3(2) . . . . ?
C24C C23C C27C F7C 117.7(3) . . . . ?
C22C C23C C27C F7C -61.3(3) . . . . ?
C24C C23C C27C F8C -124.4(2) . . . . ?
C22C C23C C27C F8C 56.5(3) . . . . ?
C24C C25C C28C F10C 9.9(3) . . . . ?
C26C C25C C28C F10C -172.9(2) . . . . ?
C24C C25C C28C F12C -111.6(2) . . . . ?
C26C C25C C28C F12C 65.6(3) . . . . ?
C24C C25C C28C F11C 130.8(2) . . . . ?
C26C C25C C28C F11C -52.0(3) . . . . ?
C41C B1C C31C C32C -95.2(2) . . . . ?
C11C B1C C31C C32C 29.3(3) . . . . ?
C21C B1C C31C C32C 145.6(2) . . . . ?
C41C B1C C31C C36C 77.3(2) . . . . ?
C11C B1C C31C C36C -158.2(2) . . . . ?
C21C B1C C31C C36C -41.9(3) . . . . ?
C36C C31C C32C C33C 2.6(3) . . . . ?
B1C C31C C32C C33C 175.4(2) . . . . ?
C31C C32C C33C C34C -2.9(4) . . . . ?
C31C C32C C33C C37C 176.8(2) . . . . ?
C32C C33C C34C C35C 0.7(4) . . . . ?
C37C C33C C34C C35C -179.0(2) . . . . ?
C33C C34C C35C C36C 1.6(4) . . . . ?
C33C C34C C35C C38C -178.7(2) . . . . ?
C34C C35C C36C C31C -1.9(4) . . . . ?
C38C C35C C36C C31C 178.4(2) . . . . ?
C32C C31C C36C C35C -0.3(3) . . . . ?
B1C C31C C36C C35C -173.4(2) . . . . ?
C32C C33C C37C F13' 38.9(11) . . . . ?
C34C C33C C37C F13' -141.4(11) . . . . ?
C32C C33C C37C F15C -151.1(7) . . . . ?
C34C C33C C37C F15C 28.6(8) . . . . ?
C32C C33C C37C F13C -24.0(9) . . . . ?
C34C C33C C37C F13C 155.7(9) . . . . ?
C32C C33C C37C F14' 170.4(9) . . . . ?
C34C C33C C37C F14' -9.9(10) . . . . ?
C32C C33C C37C F133 -115.8(7) . . . . ?
C34C C33C C37C F133 63.9(8) . . . . ?
C32C C33C C37C F131 2.8(8) . . . . ?
C34C C33C C37C F131 -177.5(8) . . . . ?
C32C C33C C37C F132 123.0(9) . . . . ?
C34C C33C C37C F132 -57.3(9) . . . . ?
C32C C33C C37C F14C 91.3(8) . . . . ?
C34C C33C C37C F14C -89.0(8) . . . . ?
C32C C33C C37C F15' -76.9(7) . . . . ?
C34C C33C C37C F15' 102.8(7) . . . . ?
C34C C35C C38C F17C -107.1(3) . . . . ?
C36C C35C C38C F17C 72.6(3) . . . . ?
C34C C35C C38C F18C 133.9(2) . . . . ?
C36C C35C C38C F18C -46.4(3) . . . . ?
C34C C35C C38C F16C 14.1(4) . . . . ?
C36C C35C C38C F16C -166.1(2) . . . . ?
C11C B1C C41C C42C -33.9(3) . . . . ?
C31C B1C C41C C42C 91.3(2) . . . . ?
C21C B1C C41C C42C -149.9(2) . . . . ?
C11C B1C C41C C46C 155.1(2) . . . . ?
C31C B1C C41C C46C -79.7(2) . . . . ?
C21C B1C C41C C46C 39.1(3) . . . . ?
C46C C41C C42C C43C -0.2(3) . . . . ?
B1C C41C C42C C43C -171.5(2) . . . . ?
C41C C42C C43C C44C 0.6(3) . . . . ?
C41C C42C C43C C47C -176.1(2) . . . . ?
C42C C43C C44C C45C -0.1(3) . . . . ?
C47C C43C C44C C45C 176.5(2) . . . . ?
C43C C44C C45C C46C -0.8(3) . . . . ?
C43C C44C C45C C48C -179.5(2) . . . . ?
C44C C45C C46C C41C 1.3(3) . . . . ?
C48C C45C C46C C41C -180.0(2) . . . . ?
C42C C41C C46C C45C -0.8(3) . . . . ?
B1C C41C C46C C45C 170.9(2) . . . . ?
C44C C43C C47C F19C 142.6(3) . . . . ?
C42C C43C C47C F19C -40.7(3) . . . . ?
C44C C43C C47C F21C 19.8(4) . . . . ?
C42C C43C C47C F21C -163.6(2) . . . . ?
C44C C43C C47C F20C -100.2(3) . . . . ?
C42C C43C C47C F20C 76.5(3) . . . . ?
C44C C45C C48C F24C -138.4(3) . . . . ?
C46C C45C C48C F24C 42.9(3) . . . . ?
C44C C45C C48C F22C -16.0(3) . . . . ?
C46C C45C C48C F22C 165.2(2) . . . . ?
C44C C45C C48C F23C 102.0(3) . . . . ?
C46C C45C C48C F23C -76.7(3) . . . . ?
C1D C1D Cl1D Cl2D -160.8(11) 2_665 . . . ?
Cl1D C1D Cl1D Cl2D -160.8(11) 2_665 . . . ?
Cl2D C1D Cl1D Cl2D -168.1(7) 2_665 . . . ?
Cl1D C1D Cl1D C1D 0.0 2_665 . . 2_665 ?
Cl2D C1D Cl1D C1D -7.4(4) 2_665 . . 2_665 ?
C1D Cl1D Cl2D C1D 14.8(8) . . . 2_665 ?
_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max 0.610
_refine_diff_density_min -0.816
_refine_diff_density_rms 0.119
_iucr_refine_instructions_details
;
TITL Carol5_P1bar in P-1
CELL 0.71073 12.4931 16.3598 16.8978 117.365 96.805 101.470
ZERR 2.00 0.0016 0.0008 0.0010 0.002 0.003 0.003
LATT 1
SFAC C H B N F Cl Rh
UNIT 111 82 2 10 48 4 2
OMIT -1 1 1
OMIT 1 0 1
OMIT 0 1 1
OMIT 1 0 0
OMIT 0 -2 1
OMIT 0 0 2
OMIT -1 1 0
OMIT 1 1 0
OMIT -1 -1 1
OMIT 1 -1 1
OMIT -1 0 1
OMIT 0 -1 1
OMIT 0 0 1
OMIT 1 -2 1
OMIT 0 -1 2
OMIT -1 2 0
OMIT -1 0 2
OMIT -1 1 2
OMIT 0 -2 2
OMIT 1 1 1
OMIT -2 1 0
OMIT -1 -1 2
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.330 0.119 0.057
CONF
SADI 0.02 C37C F13C C37C F14C C37C F15C
SADI 0.02 C37C F131 C37C F132 C37C F133
SADI 0.02 C37C F13' C37C F14' C37C F15'
FREE C1D F23C
FREE Cl2D C1D
DELU 0.02 C37C F13C F14C F15C F131 F132 F133 F13' F14' F15'
SIMU 0.02 C37C F13C F14C F15C F131 F132 F133 F13' F14' F15'
TEMP -120.760
WGHT 0.039700 1.914900
FVAR 0.13092
MOLE 1
RH1 7 -0.125948 0.837072 0.622087 11.00000 0.01897 0.01697 =
0.02223 0.01174 0.00694 0.00623
N1 4 -0.058093 1.059709 0.748836 11.00000 0.03156 0.01848 =
0.02252 0.00877 0.00987 0.00736
N2 4 -0.141991 0.975880 0.708635 11.00000 0.02760 0.02185 =
0.02882 0.01456 0.01076 0.00977
C3 1 -0.235054 1.001060 0.727375 11.00000 0.03123 0.03336 =
0.03890 0.02079 0.01732 0.01687
AFIX 43
H3 2 -0.307898 0.957132 0.707349 11.00000 -1.20000
AFIX 0
C4 1 -0.211060 1.100063 0.780057 11.00000 0.04881 0.03709 =
0.04094 0.02104 0.02602 0.02836
AFIX 43
H4 2 -0.262382 1.135845 0.802827 11.00000 -1.20000
AFIX 0
C5 1 -0.097870 1.135297 0.792300 11.00000 0.05101 0.02175 =
0.02725 0.01106 0.01766 0.01667
AFIX 43
H5 2 -0.055178 1.201052 0.825407 11.00000 -1.20000
AFIX 0
C1A 1 0.057544 1.059956 0.745100 11.00000 0.02927 0.02075 =
0.02443 0.00843 0.00655 0.00428
AFIX 23
H1A1 2 0.085068 1.031479 0.781103 11.00000 -1.20000
H2A1 2 0.105325 1.127104 0.773489 11.00000 -1.20000
AFIX 0
N1' 4 0.112100 0.944296 0.517998 11.00000 0.02605 0.01845 =
0.02631 0.01223 0.01151 0.00723
N2' 4 0.029560 0.875016 0.512765 11.00000 0.02401 0.02066 =
0.02492 0.01228 0.00922 0.00568
N3' 4 0.002993 0.912222 0.592373 11.00000 0.02216 0.01939 =
0.02080 0.01063 0.00678 0.00660
C4' 1 0.068385 1.004320 0.648164 11.00000 0.02220 0.01629 =
0.02441 0.00886 0.00605 0.00522
C5' 1 0.138672 1.025152 0.600009 11.00000 0.02905 0.01545 =
0.02955 0.00885 0.00913 0.00312
AFIX 43
H5' 2 0.194326 1.083938 0.619955 11.00000 -1.20000
AFIX 0
C6' 1 0.168195 0.921733 0.441654 11.00000 0.03497 0.02584 =
0.02723 0.01706 0.01685 0.01149
AFIX 23
H16' 2 0.197578 0.980807 0.438632 11.00000 -1.20000
H26' 2 0.112696 0.874351 0.383051 11.00000 -1.20000
AFIX 0
C7' 1 0.263547 0.881648 0.453510 11.00000 0.03003 0.02790 =
0.02555 0.01723 0.01482 0.00984
C8' 1 0.249051 0.784233 0.407188 11.00000 0.02938 0.02742 =
0.03880 0.01345 0.01100 0.00855
AFIX 43
H8' 2 0.178244 0.741846 0.367330 11.00000 -1.20000
AFIX 0
C9' 1 0.337231 0.747243 0.418217 11.00000 0.04254 0.03661 =
0.04932 0.02129 0.02008 0.02057
AFIX 43
H9' 2 0.326441 0.679832 0.385771 11.00000 -1.20000
AFIX 0
C10' 1 0.438916 0.807311 0.475339 11.00000 0.03518 0.06101 =
0.04962 0.03827 0.02061 0.02366
AFIX 43
H10' 2 0.499629 0.781992 0.481340 11.00000 -1.20000
AFIX 0
C11' 1 0.453819 0.905203 0.524632 11.00000 0.03134 0.06001 =
0.04387 0.03216 0.00514 0.00234
AFIX 43
H11' 2 0.524021 0.946973 0.566051 11.00000 -1.20000
AFIX 0
C12' 1 0.366514 0.942250 0.513609 11.00000 0.03735 0.03083 =
0.03306 0.01485 0.00887 0.00178
AFIX 43
H12' 2 0.377036 1.009562 0.547352 11.00000 -1.20000
AFIX 0
C1B 1 -0.037282 0.737809 0.624903 11.00000 0.02723 0.02508 =
0.03766 0.02292 0.01147 0.01306
C2B 1 -0.143591 0.686945 0.560426 11.00000 0.03619 0.01645 =
0.02891 0.01340 0.00550 0.00959
C3B 1 -0.229662 0.707667 0.610377 11.00000 0.02656 0.02577 =
0.04348 0.02577 0.00687 0.00668
C4B 1 -0.176215 0.773154 0.703703 11.00000 0.03748 0.02958 =
0.03599 0.02604 0.01830 0.01619
C5B 1 -0.055897 0.793811 0.713704 11.00000 0.03444 0.02283 =
0.02741 0.01730 0.00319 0.00838
C6B 1 0.074750 0.734333 0.603717 11.00000 0.03593 0.05014 =
0.07044 0.04201 0.02582 0.02585
AFIX 137
H6B1 2 0.096443 0.682735 0.609779 11.00000 -1.50000
H6B2 2 0.130932 0.795924 0.646667 11.00000 -1.50000
H6B3 2 0.070526 0.722053 0.540775 11.00000 -1.50000
AFIX 0
C7B 1 -0.162556 0.618440 0.459771 11.00000 0.07767 0.02857 =
0.03099 0.01106 0.00545 0.02185
AFIX 137
H7B1 2 -0.098435 0.637804 0.437664 11.00000 -1.50000
H7B2 2 -0.231454 0.619406 0.426229 11.00000 -1.50000
H7B3 2 -0.170167 0.553370 0.449681 11.00000 -1.50000
AFIX 0
C8B 1 -0.353496 0.664531 0.569760 11.00000 0.03114 0.04339 =
0.08009 0.04176 0.00394 0.00025
AFIX 137
H8B1 2 -0.376847 0.601081 0.564590 11.00000 -1.50000
H8B2 2 -0.371291 0.657948 0.508673 11.00000 -1.50000
H8B3 2 -0.393591 0.706265 0.609368 11.00000 -1.50000
AFIX 0
C9B 1 -0.233764 0.814605 0.779524 11.00000 0.07234 0.06205 =
0.05708 0.04547 0.04544 0.04140
AFIX 137
H9B1 2 -0.306081 0.819156 0.754957 11.00000 -1.50000
H9B2 2 -0.186337 0.878818 0.826654 11.00000 -1.50000
H9B3 2 -0.246628 0.773031 0.806699 11.00000 -1.50000
AFIX 0
C10B 1 0.032585 0.853171 0.801711 11.00000 0.05477 0.03787 =
0.04013 0.02365 -0.01028 0.00293
AFIX 137
H10B 2 0.044964 0.813285 0.828929 11.00000 -1.50000
H10C 2 0.007946 0.906702 0.844341 11.00000 -1.50000
H10D 2 0.102879 0.878460 0.789589 11.00000 -1.50000
AFIX 0
CL1A 6 -0.257092 0.828219 0.500269 11.00000 0.02302 0.02548 =
0.03123 0.01925 0.00089 0.00490
MOLE 2
B1C 3 0.247027 0.676352 0.895860 11.00000 0.02206 0.01855 =
0.02219 0.01149 0.00805 0.00741
C11C 1 0.301321 0.768304 0.883489 11.00000 0.01732 0.02163 =
0.02533 0.01360 0.00744 0.00788
C12C 1 0.307811 0.861991 0.949906 11.00000 0.02353 0.02418 =
0.02458 0.01387 0.01027 0.00865
AFIX 43
H12C 2 0.290605 0.872603 1.006522 11.00000 -1.20000
AFIX 0
C13C 1 0.338473 0.939936 0.936030 11.00000 0.02238 0.02048 =
0.03237 0.01308 0.00757 0.00698
C14C 1 0.366262 0.927954 0.855314 11.00000 0.02888 0.02744 =
0.04174 0.02463 0.01164 0.00797
AFIX 43
H14C 2 0.388523 0.981284 0.846047 11.00000 -1.20000
AFIX 0
C15C 1 0.360795 0.836189 0.788346 11.00000 0.02467 0.03121 =
0.03022 0.01998 0.01009 0.00936
C16C 1 0.327552 0.758159 0.801925 11.00000 0.02325 0.02364 =
0.02491 0.01337 0.00956 0.00865
AFIX 43
H16C 2 0.322510 0.695802 0.754076 11.00000 -1.20000
AFIX 0
C17C 1 0.334550 1.036233 1.006444 11.00000 0.03903 0.02512 =
0.04635 0.01681 0.01276 0.01020
C18C 1 0.391321 0.822619 0.701144 11.00000 0.03978 0.04183 =
0.04074 0.02843 0.01799 0.01047
F1C 5 0.365722 1.053304 1.092574 11.00000 0.07375 0.03945 =
0.03994 0.00460 0.00923 0.02551
F2C 5 0.402369 1.108566 1.004946 11.00000 0.11449 0.02152 =
0.09408 0.02204 0.05436 0.00793
F3C 5 0.231993 1.045651 0.998333 11.00000 0.05241 0.04996 =
0.07836 0.00267 0.00131 0.03624
F4C 5 0.499824 0.859909 0.712764 11.00000 0.03487 0.14992 =
0.06135 0.06920 0.02465 0.01931
F5C 5 0.340205 0.867270 0.665731 11.00000 0.05985 0.09196 =
0.05646 0.05872 0.02284 0.02750
F6C 5 0.360516 0.732321 0.634814 11.00000 0.15254 0.05514 =
0.04464 0.02542 0.05697 0.02396
C21C 1 0.111034 0.656752 0.863193 11.00000 0.02429 0.01882 =
0.02610 0.01594 0.00993 0.00882
C22C 1 0.048476 0.704165 0.923644 11.00000 0.02664 0.02160 =
0.02285 0.01450 0.00895 0.00893
AFIX 43
H22C 2 0.085240 0.746994 0.986510 11.00000 -1.20000
AFIX 0
C23C 1 -0.065431 0.690693 0.894804 11.00000 0.02756 0.02399 =
0.03065 0.01904 0.01382 0.01243
C24C 1 -0.122782 0.628790 0.803936 11.00000 0.01987 0.02615 =
0.03514 0.02142 0.00843 0.00729
AFIX 43
H24C 2 -0.201092 0.618693 0.784394 11.00000 -1.20000
AFIX 0
C25C 1 -0.062374 0.582043 0.742415 11.00000 0.02623 0.01970 =
0.02787 0.01544 0.00618 0.00627
C26C 1 0.051986 0.596346 0.771754 11.00000 0.02595 0.02031 =
0.02430 0.01339 0.00920 0.00931
AFIX 43
H26C 2 0.091323 0.563762 0.727881 11.00000 -1.20000
AFIX 0
C27C 1 -0.125060 0.744048 0.965357 11.00000 0.03244 0.04314 =
0.03711 0.02438 0.01753 0.02078
C28C 1 -0.118877 0.511738 0.644100 11.00000 0.02948 0.02374 =
0.03340 0.01440 0.00472 0.00748
F7C 5 -0.122469 0.720406 1.031288 11.00000 0.06760 0.09007 =
0.04643 0.04792 0.03709 0.04881
F8C 5 -0.076983 0.839141 1.009592 11.00000 0.05806 0.04073 =
0.06978 0.01343 0.03448 0.02638
F9C 5 -0.232513 0.729807 0.930821 11.00000 0.03329 0.07946 =
0.04614 0.03131 0.02038 0.03245
F10C 5 -0.224760 0.511057 0.620530 11.00000 0.03206 0.05725 =
0.04594 0.00788 -0.00829 0.01403
F11C 5 -0.065441 0.528269 0.586245 11.00000 0.05756 0.03788 =
0.02730 0.01758 0.00615 0.00563
F12C 5 -0.120692 0.421670 0.622676 11.00000 0.06089 0.02020 =
0.04001 0.01176 0.00497 0.00654
C31C 1 0.284223 0.579647 0.835100 11.00000 0.02117 0.01980 =
0.01830 0.01055 0.00390 0.00675
C32C 1 0.386613 0.580324 0.809636 11.00000 0.02056 0.01996 =
0.02597 0.01084 0.00372 0.00445
AFIX 43
H32C 2 0.436703 0.639929 0.824279 11.00000 -1.20000
AFIX 0
C33C 1 0.417595 0.496852 0.763672 11.00000 0.02167 0.02646 =
0.02649 0.01042 0.00628 0.00921
C34C 1 0.349342 0.408384 0.744366 11.00000 0.03135 0.02151 =
0.02518 0.00831 0.00665 0.01274
AFIX 43
H34C 2 0.370670 0.351171 0.713485 11.00000 -1.20000
AFIX 0
C35C 1 0.249351 0.406873 0.771804 11.00000 0.02855 0.01859 =
0.02053 0.00877 0.00405 0.00554
C36C 1 0.217018 0.489913 0.814750 11.00000 0.02191 0.02295 =
0.02058 0.01156 0.00720 0.00693
AFIX 43
H36C 2 0.146674 0.485788 0.830970 11.00000 -1.20000
AFIX 0
C37C 1 0.524907 0.500554 0.733639 11.00000 0.03153 0.03338 =
0.04783 0.01082 0.01659 0.01326
C38C 1 0.173062 0.315133 0.755342 11.00000 0.04074 0.02112 =
0.03138 0.00969 0.01092 0.00639
PART 1
F13C 5 0.563128 0.574170 0.722268 10.33333 0.04855 0.05936 =
0.09313 0.05388 0.04739 0.02538
F14C 5 0.611019 0.512883 0.802238 10.33333 0.02349 0.08009 =
0.09054 0.03935 0.01725 0.02449
F15C 5 0.524178 0.421922 0.660388 10.33333 0.03597 0.03726 =
0.05884 0.02029 0.03098 0.02723
PART 2
F131 5 0.586518 0.589602 0.758832 10.33333 0.01929 0.04288 =
0.06082 0.01663 0.01430 0.00519
F132 5 0.595576 0.465052 0.766285 10.33333 0.04077 0.07385 =
0.10291 0.05357 0.03329 0.04675
F133 5 0.509506 0.452961 0.643180 10.33333 0.05153
PART 3
F13' 5 0.605845 0.574628 0.792319 10.33333 0.02043 0.07840 =
0.07950 -0.00823 0.00998 -0.00084
F14' 5 0.551987 0.419395 0.703466 10.33333 0.05690 0.06185 =
0.10949 0.04983 0.04763 0.04592
F15' 5 0.506809 0.509945 0.654170 10.33333 0.04892 0.10650 =
0.08073 0.06814 0.04493 0.03193
PART 0
F16C 5 0.222080 0.245068 0.732736 11.00000 0.08841 0.02522 =
0.13702 0.03763 0.06792 0.02679
F17C 5 0.081342 0.282094 0.689387 11.00000 0.07296 0.06088 =
0.05934 0.03369 -0.02509 -0.03813
F18C 5 0.135724 0.323172 0.828152 11.00000 0.07020 0.03366 =
0.04399 0.02102 0.02424 0.00072
C41C 1 0.282485 0.696553 1.000977 11.00000 0.02333 0.01739 =
0.02180 0.01026 0.00876 0.01036
C42C 1 0.386739 0.755054 1.061311 11.00000 0.02586 0.01772 =
0.02524 0.01158 0.00932 0.00761
AFIX 43
H42C 2 0.437121 0.792194 1.044153 11.00000 -1.20000
AFIX 0
C43C 1 0.419561 0.760879 1.146068 11.00000 0.02850 0.01953 =
0.02440 0.01012 0.00453 0.00871
C44C 1 0.349173 0.707284 1.173612 11.00000 0.03751 0.02519 =
0.02145 0.01340 0.00851 0.01436
AFIX 43
H44C 2 0.371438 0.711080 1.231229 11.00000 -1.20000
AFIX 0
C45C 1 0.245620 0.648163 1.114686 11.00000 0.03259 0.01973 =
0.02529 0.01310 0.01047 0.01124
C46C 1 0.212986 0.643777 1.031162 11.00000 0.02228 0.01938 =
0.02519 0.01199 0.00772 0.00735
AFIX 43
H46C 2 0.140682 0.603434 0.992809 11.00000 -1.20000
AFIX 0
C47C 1 0.529215 0.829830 1.209368 11.00000 0.04112 0.03880 =
0.03604 0.02191 -0.00157 0.00294
C48C 1 0.164577 0.588647 1.139908 11.00000 0.04282 0.03904 =
0.03830 0.02773 0.01303 0.01157
F19C 5 0.611400 0.833418 1.167503 11.00000 0.03571 0.11909 =
0.05546 0.04050 -0.00326 -0.01855
F20C 5 0.523771 0.920394 1.251584 11.00000 0.08911 0.02892 =
0.08269 0.00607 -0.03246 -0.00182
F21C 5 0.565879 0.813011 1.275864 11.00000 0.05260 0.07138 =
0.05645 0.04407 -0.01868 -0.00677
F22C 5 0.211255 0.579859 1.208927 11.00000 0.06262 0.06280 =
0.05148 0.04774 0.00724 0.00249
F23C 5 0.082775 0.627744 1.167759 11.00000 0.06481 0.10951 =
0.14033 0.10080 0.06912 0.04738
F24C 5 0.114536 0.501258 1.070778 11.00000 0.09852 0.04571 =
0.04735 0.02515 0.00774 -0.02757
MOLE 3
C1D 1 0.466539 0.529923 0.012163 10.50000 0.07364 0.08276 =
0.06329 0.03464 0.01622 0.05367
AFIX 23
H1D1 2 0.441384 0.548352 -0.033533 10.50000 -1.20000
H1D2 2 0.492435 0.585283 0.075472 10.50000 -1.20000
AFIX 0
CL1D 6 0.605051 0.555822 -0.002209 10.50000 0.07909 0.23094 =
0.11723 0.07567 0.02120 0.03219
CL2D 6 0.575606 0.596618 0.026481 10.50000 0.14700 0.08035 =
0.08378 0.03206 0.00469 0.05042
HKLF 4
REM Carol5_P1bar in P-1
REM R1 = 0.0346 for 8671 Fo > 4sig(Fo) and 0.0441 for all 10077 data
REM 865 parameters refined using 174 restraints
END
WGHT 0.0397 1.9147
REM Highest difference peak 0.610, deepest hole -0.816, 1-sigma level 0.119
Q1 1 0.4583 0.7510 0.6795 11.00000 0.05 0.61
Q2 1 0.3220 0.7950 0.6311 11.00000 0.05 0.57
Q3 1 0.1968 0.4957 1.0914 11.00000 0.05 0.52
Q4 1 0.1616 0.2338 0.6790 11.00000 0.05 0.48
Q5 1 0.5020 0.5755 0.0279 11.00000 0.05 0.41
Q6 1 -0.2775 0.8484 0.5368 11.00000 0.05 0.37
Q7 1 -0.3007 0.8090 0.4804 11.00000 0.05 0.37
Q8 1 0.0657 0.5653 1.1036 11.00000 0.05 0.36
Q9 1 0.3833 0.8577 1.0629 11.00000 0.05 0.36
Q10 1 0.5812 0.4080 0.7416 11.00000 0.05 0.36
Q11 1 0.3149 1.0914 0.9631 11.00000 0.05 0.35
Q12 1 0.1206 0.8102 0.7721 11.00000 0.05 0.35
Q13 1 0.0630 0.7807 0.7870 11.00000 0.05 0.35
Q14 1 0.4923 0.7220 0.9892 11.00000 0.05 0.35
Q15 1 0.5123 0.8931 1.2908 11.00000 0.05 0.34
Q16 1 0.2373 0.9213 0.7592 11.00000 0.05 0.34
Q17 1 0.2435 0.5247 1.1597 11.00000 0.05 0.34
Q18 1 0.1612 0.8467 0.7124 11.00000 0.05 0.34
Q19 1 0.6195 0.4181 0.8048 11.00000 0.05 0.33
Q20 1 -0.1229 0.5146 0.3598 11.00000 0.05 0.33
;
#===END
data_carol9_c2byc
_audit_update_record
;
2012-07-24 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C54.88 H39.75 B Cl2.75 F24 N5 Rh'
_chemical_formula_weight 1436.37
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Rh' 'Rh' -1.1178 0.9187
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'C 2/c'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 29.9749(17)
_cell_length_b 13.0963(8)
_cell_length_c 36.371(2)
_cell_angle_alpha 90.00
_cell_angle_beta 111.572(2)
_cell_angle_gamma 90.00
_cell_volume 13277.7(13)
_cell_formula_units_Z 8
_cell_measurement_temperature 151(2)
_cell_measurement_reflns_used 9870
_cell_measurement_theta_min 2.313
_cell_measurement_theta_max 26.627
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'Yellow'
_exptl_crystal_size_max 0.34
_exptl_crystal_size_mid 0.23
_exptl_crystal_size_min 0.15
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.437
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5734
_exptl_absorpt_coefficient_mu 0.473
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8565
_exptl_absorpt_correction_T_max 0.9311
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 151(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 40705
_diffrn_reflns_av_R_equivalents 0.0717
_diffrn_reflns_av_sigmaI/netI 0.0718
_diffrn_reflns_limit_h_min -35
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_k_min -5
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -43
_diffrn_reflns_limit_l_max 42
_diffrn_reflns_theta_min 2.57
_diffrn_reflns_theta_max 25.00
_reflns_number_total 11579
_reflns_number_gt 8562
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1023P)^2^+205.5653P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 11579
_refine_ls_number_parameters 922
_refine_ls_number_restraints 336
_refine_ls_R_factor_all 0.1136
_refine_ls_R_factor_gt 0.0883
_refine_ls_wR_factor_ref 0.2599
_refine_ls_wR_factor_gt 0.2429
_refine_ls_goodness_of_fit_ref 1.102
_refine_ls_restrained_S_all 1.098
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.83606(2) 0.41403(4) 0.810823(17) 0.0296(2) Uani 1 1 d . . .
N1 N 0.7791(2) 0.6147(5) 0.80141(19) 0.0323(14) Uani 1 1 d . . .
N2 N 0.7881(2) 0.5210(5) 0.8188(2) 0.0381(16) Uani 1 1 d . . .
C3 C 0.7554(3) 0.5088(8) 0.8354(3) 0.054(2) Uani 1 1 d . . .
H3 H 0.7529 0.4500 0.8498 0.065 Uiso 1 1 calc R . .
C4 C 0.7256(4) 0.5930(9) 0.8286(3) 0.062(3) Uani 1 1 d . . .
H4 H 0.6999 0.6035 0.8375 0.074 Uiso 1 1 calc R . .
C5 C 0.7414(3) 0.6584(8) 0.8062(3) 0.050(2) Uani 1 1 d . . .
H5 H 0.7278 0.7228 0.7960 0.060 Uiso 1 1 calc R . .
C1A C 0.8082(3) 0.6513(6) 0.7803(2) 0.0314(16) Uani 1 1 d . . .
H1A1 H 0.8418 0.6582 0.7988 0.038 Uiso 1 1 calc R . .
H1A2 H 0.7968 0.7197 0.7692 0.038 Uiso 1 1 calc R . .
N1' N 0.8002(2) 0.5041(5) 0.69351(18) 0.0304(14) Uani 1 1 d . . .
N2' N 0.8127(2) 0.4320(5) 0.72175(19) 0.0318(14) Uani 1 1 d . . .
N3' N 0.8166(2) 0.4800(4) 0.75493(18) 0.0296(14) Uani 1 1 d . . .
C4' C 0.8063(3) 0.5806(6) 0.7476(2) 0.0322(16) Uani 1 1 d . . .
C5' C 0.7954(3) 0.5973(6) 0.7084(2) 0.0337(17) Uani 1 1 d . . .
H5' H 0.7865 0.6600 0.6945 0.040 Uiso 1 1 calc R . .
C6' C 0.7935(3) 0.4778(6) 0.6539(2) 0.0377(18) Uani 1 1 d . . .
C7' C 0.8215(4) 0.4024(9) 0.6474(3) 0.070(3) Uani 1 1 d . . .
H7' H 0.8437 0.3650 0.6687 0.084 Uiso 1 1 calc R . .
C8' C 0.8164(6) 0.3825(13) 0.6083(4) 0.106(5) Uani 1 1 d . . .
H8' H 0.8354 0.3313 0.6027 0.127 Uiso 1 1 calc R . .
C9' C 0.7831(6) 0.4382(13) 0.5775(4) 0.095(5) Uani 1 1 d . . .
H9' H 0.7790 0.4231 0.5509 0.114 Uiso 1 1 calc R . .
C10' C 0.7571(4) 0.5120(9) 0.5850(3) 0.063(3) Uani 1 1 d . . .
H10' H 0.7355 0.5504 0.5637 0.075 Uiso 1 1 calc R . .
C11' C 0.7614(3) 0.5333(7) 0.6235(3) 0.047(2) Uani 1 1 d . . .
H11' H 0.7425 0.5854 0.6288 0.056 Uiso 1 1 calc R . .
C1B C 0.9100(3) 0.3880(6) 0.8176(2) 0.0364(18) Uani 1 1 d . . .
C2B C 0.9077(2) 0.4641(6) 0.8453(2) 0.0318(17) Uani 1 1 d . . .
C3B C 0.8866(3) 0.4163(7) 0.8713(2) 0.0377(18) Uani 1 1 d . . .
C4B C 0.8748(3) 0.3141(7) 0.8585(3) 0.051(2) Uani 1 1 d . . .
C5B C 0.8895(3) 0.2962(6) 0.8256(3) 0.045(2) Uani 1 1 d . . .
C6B C 0.9297(3) 0.4029(8) 0.7858(3) 0.054(2) Uani 1 1 d . . .
H6B1 H 0.9634 0.3821 0.7956 0.081 Uiso 1 1 calc R . .
H6B2 H 0.9271 0.4750 0.7782 0.081 Uiso 1 1 calc R . .
H6B3 H 0.9114 0.3612 0.7628 0.081 Uiso 1 1 calc R . .
C7B C 0.8863(4) 0.1956(7) 0.8044(4) 0.077(4) Uani 1 1 d . . .
H7A1 H 0.9182 0.1763 0.8051 0.116 Uiso 1 1 calc R . .
H7A2 H 0.8643 0.2026 0.7768 0.116 Uiso 1 1 calc R . .
H7A3 H 0.8743 0.1428 0.8175 0.116 Uiso 1 1 calc R . .
C8B C 0.8538(4) 0.2368(9) 0.8772(4) 0.078(4) Uani 1 1 d . . .
H8A1 H 0.8252 0.2069 0.8571 0.117 Uiso 1 1 calc R . .
H8A2 H 0.8448 0.2695 0.8977 0.117 Uiso 1 1 calc R . .
H8A3 H 0.8774 0.1830 0.8891 0.117 Uiso 1 1 calc R . .
C9B C 0.8795(4) 0.4672(9) 0.9048(3) 0.059(3) Uani 1 1 d . . .
H9A1 H 0.9080 0.4571 0.9289 0.088 Uiso 1 1 calc R . .
H9A2 H 0.8514 0.4380 0.9086 0.088 Uiso 1 1 calc R . .
H9A3 H 0.8745 0.5404 0.8993 0.088 Uiso 1 1 calc R . .
C10B C 0.9284(3) 0.5686(6) 0.8499(3) 0.042(2) Uani 1 1 d . . .
H10A H 0.9100 0.6142 0.8604 0.063 Uiso 1 1 calc R . .
H10B H 0.9268 0.5938 0.8241 0.063 Uiso 1 1 calc R . .
H10C H 0.9619 0.5667 0.8681 0.063 Uiso 1 1 calc R . .
Cl1 Cl 0.76879(8) 0.30300(17) 0.78594(7) 0.0504(6) Uani 1 1 d . . .
B1C B 1.0177(3) 0.9108(6) 0.8765(2) 0.0245(16) Uani 1 1 d . . .
C11C C 1.0293(2) 1.0311(5) 0.8705(2) 0.0251(15) Uani 1 1 d . . .
C12C C 1.0180(3) 1.1106(5) 0.8910(2) 0.0283(16) Uani 1 1 d . . .
H12C H 1.0049 1.0945 0.9104 0.034 Uiso 1 1 calc R . .
C13C C 1.0253(3) 1.2121(6) 0.8841(2) 0.0344(18) Uani 1 1 d . . .
C14C C 1.0424(3) 1.2389(6) 0.8549(2) 0.0363(18) Uani 1 1 d . . .
H14C H 1.0476 1.3084 0.8501 0.044 Uiso 1 1 calc R . .
C15C C 1.0514(3) 1.1616(6) 0.8332(2) 0.0347(18) Uani 1 1 d . . .
C16C C 1.0459(3) 1.0599(5) 0.8409(2) 0.0289(16) Uani 1 1 d . . .
H16C H 1.0537 1.0086 0.8258 0.035 Uiso 1 1 calc R . .
C17C C 1.0161(3) 1.2919(6) 0.9094(3) 0.046(2) Uani 1 1 d . . .
C18C C 1.0693(4) 1.1876(7) 0.8008(3) 0.051(2) Uani 1 1 d . . .
F1C F 1.0551(3) 1.1247(6) 0.77044(19) 0.087(2) Uani 1 1 d . . .
F2C F 1.1167(2) 1.1882(6) 0.8132(2) 0.083(2) Uani 1 1 d . . .
F3C F 1.0560(3) 1.2804(5) 0.7862(3) 0.113(3) Uani 1 1 d . . .
F4C F 1.0118(2) 1.3859(4) 0.89385(19) 0.0682(17) Uani 1 1 d . . .
F5C F 1.0504(2) 1.2948(5) 0.94539(18) 0.083(2) Uani 1 1 d . . .
F6C F 0.9752(2) 1.2773(4) 0.91554(16) 0.0562(14) Uani 1 1 d . . .
C21C C 1.0561(2) 0.8339(5) 0.8675(2) 0.0246(15) Uani 1 1 d . . .
C22C C 1.1050(3) 0.8569(6) 0.8812(2) 0.0294(16) Uani 1 1 d . . .
H22C H 1.1156 0.9202 0.8942 0.035 Uiso 1 1 calc R . .
C23C C 1.1388(3) 0.7910(6) 0.8766(2) 0.0346(18) Uani 1 1 d . . .
C24C C 1.1242(3) 0.6973(6) 0.8577(2) 0.0386(19) Uani 1 1 d . . .
H24C H 1.1472 0.6514 0.8546 0.046 Uiso 1 1 calc R . .
C25C C 1.0767(3) 0.6724(6) 0.8437(2) 0.0335(17) Uani 1 1 d . . .
C26C C 1.0432(2) 0.7390(5) 0.8487(2) 0.0280(16) Uani 1 1 d . . .
H26C H 1.0104 0.7194 0.8390 0.034 Uiso 1 1 calc R . .
C27C C 1.1910(3) 0.8182(8) 0.8924(3) 0.058(3) Uani 1 1 d . . .
C28C C 1.0603(3) 0.5740(7) 0.8227(3) 0.049(2) Uani 1 1 d . . .
F7C F 1.1981(2) 0.9174(5) 0.8931(3) 0.087(2) Uani 1 1 d . . .
F8C F 1.2140(2) 0.7818(8) 0.9273(2) 0.120(4) Uani 1 1 d . . .
F9C F 1.2138(2) 0.7813(5) 0.8698(2) 0.082(2) Uani 1 1 d . . .
F10C F 1.0866(2) 0.5432(5) 0.8029(2) 0.087(2) Uani 1 1 d . . .
F11C F 1.0582(4) 0.5001(5) 0.8458(3) 0.119(3) Uani 1 1 d . . .
F12C F 1.0161(3) 0.5801(6) 0.7953(3) 0.108(3) Uani 1 1 d . . .
C31C C 0.9629(2) 0.8950(5) 0.8455(2) 0.0226(14) Uani 1 1 d . . .
C32C C 0.9527(3) 0.8813(5) 0.8048(2) 0.0281(16) Uani 1 1 d . . .
H32C H 0.9786 0.8727 0.7960 0.034 Uiso 1 1 calc R . .
C33C C 0.9066(3) 0.8800(6) 0.7774(2) 0.0297(16) Uani 1 1 d . A .
C34C C 0.8671(3) 0.8935(5) 0.7887(2) 0.0314(16) Uani 1 1 d . . .
H34C H 0.8353 0.8934 0.7697 0.038 Uiso 1 1 calc R . .
C35C C 0.8762(3) 0.9069(6) 0.8287(2) 0.0312(16) Uani 1 1 d . B .
C36C C 0.9232(2) 0.9075(5) 0.8563(2) 0.0276(15) Uani 1 1 d . . .
H36C H 0.9282 0.9168 0.8834 0.033 Uiso 1 1 calc R . .
C37C C 0.8967(3) 0.8586(6) 0.7344(2) 0.0511(19) Uani 1 1 d DU . .
C38C C 0.8346(3) 0.9218(6) 0.8409(2) 0.0506(19) Uani 1 1 d DU . .
F13B F 0.9354(6) 0.8457(18) 0.7264(9) 0.055(4) Uani 0.51(4) 1 d PDU A 1
F14B F 0.8735(8) 0.9411(15) 0.7133(6) 0.075(4) Uani 0.51(4) 1 d PDU A 1
F15B F 0.8669(8) 0.7817(17) 0.7194(6) 0.076(4) Uani 0.51(4) 1 d PDU A 1
F13C F 0.9343(6) 0.875(2) 0.7246(10) 0.052(4) Uani 0.49(4) 1 d PDU A 2
F14C F 0.8590(6) 0.903(2) 0.7082(5) 0.079(4) Uani 0.49(4) 1 d PDU A 2
F15C F 0.8881(11) 0.7568(10) 0.7292(6) 0.073(4) Uani 0.49(4) 1 d PDU A 2
F16A F 0.7948(6) 0.9483(19) 0.8129(5) 0.075(4) Uani 0.35 1 d PDU B 1
F17A F 0.8267(6) 0.8288(12) 0.8539(6) 0.065(4) Uani 0.35 1 d PDU B 1
F18A F 0.8444(11) 0.9837(15) 0.8712(5) 0.045(4) Uani 0.35 1 d PDU B 1
F16B F 0.7934(9) 0.881(3) 0.8163(9) 0.050(5) Uani 0.15 1 d PDU B 2
F17B F 0.8425(11) 0.877(3) 0.8766(7) 0.058(5) Uani 0.15 1 d PDU B 2
F18B F 0.8242(13) 1.0195(13) 0.8455(12) 0.059(5) Uani 0.15 1 d PDU B 2
F16C F 0.8061(3) 1.0027(9) 0.8192(4) 0.053(2) Uani 0.50 1 d PDU B 3
F17C F 0.8042(4) 0.8458(9) 0.8333(4) 0.049(3) Uani 0.50 1 d PDU B 3
F18C F 0.8453(8) 0.9514(11) 0.8781(3) 0.050(4) Uani 0.50 1 d PDU B 3
C41C C 1.0243(2) 0.8811(5) 0.9222(2) 0.0256(15) Uani 1 1 d . . .
C42C C 1.0046(3) 0.7883(5) 0.9286(2) 0.0299(16) Uani 1 1 d . . .
H42C H 0.9865 0.7477 0.9065 0.036 Uiso 1 1 calc R . .
C43C C 1.0111(3) 0.7542(6) 0.9668(2) 0.0368(18) Uani 1 1 d . . .
C44C C 1.0367(3) 0.8132(6) 0.9996(2) 0.041(2) Uani 1 1 d . . .
H44C H 1.0410 0.7912 1.0256 0.049 Uiso 1 1 calc R . .
C45C C 1.0554(3) 0.9032(6) 0.9935(2) 0.0364(18) Uani 1 1 d . . .
C46C C 1.0506(3) 0.9359(5) 0.9556(2) 0.0300(16) Uani 1 1 d . . .
H46C H 1.0658 0.9974 0.9527 0.036 Uiso 1 1 calc R . .
C47C C 0.9894(4) 0.6550(7) 0.9715(3) 0.050(2) Uani 1 1 d . . .
C48C C 1.0827(3) 0.9675(7) 1.0289(2) 0.046(2) Uani 1 1 d . . .
F19C F 1.0785(4) 1.0663(4) 1.0215(2) 0.116(3) Uani 1 1 d . . .
F20C F 1.1289(2) 0.9467(6) 1.0424(2) 0.089(2) Uani 1 1 d . . .
F21C F 1.0695(2) 0.9532(5) 1.05904(16) 0.0740(18) Uani 1 1 d . . .
F22C F 1.0110(3) 0.6146(4) 1.00760(16) 0.080(2) Uani 1 1 d . . .
F23C F 0.9425(3) 0.6642(6) 0.9663(3) 0.101(3) Uani 1 1 d . . .
F24C F 0.9908(3) 0.5843(4) 0.94564(16) 0.0737(19) Uani 1 1 d . . .
C1M C 0.1324(8) 0.6693(15) 0.9680(6) 0.081(7) Uiso 0.50 1 d PDU . .
H1M1 H 0.1037 0.7138 0.9584 0.097 Uiso 0.50 1 calc PR C 1
H1M2 H 0.1521 0.6845 0.9520 0.097 Uiso 0.50 1 calc PR C 1
Cl1M Cl 0.1650(7) 0.6981(17) 1.0166(4) 0.096(5) Uiso 0.25 1 d PDU D 1
Cl2M Cl 0.1143(13) 0.5442(13) 0.9606(11) 0.161(16) Uiso 0.25 1 d PDU D 1
Cl1N Cl 0.1820(8) 0.671(2) 1.0107(6) 0.082(8) Uiso 0.13 1 d PDU D 2
Cl2N Cl 0.1028(10) 0.5586(15) 0.9484(9) 0.066(7) Uiso 0.13 1 d PDU D 2
Cl1O Cl 0.1688(13) 0.737(3) 1.0082(9) 0.108(12) Uiso 0.13 1 d PDU D 3
Cl2O Cl 0.1070(11) 0.5540(14) 0.9721(10) 0.074(8) Uiso 0.13 1 d PDU D 3
C1P C 0.803(2) 0.938(3) 0.0452(15) 0.20(5) Uiso 0.25 1 d PDU . .
H1P1 H 0.7849 0.8846 0.0267 0.242 Uiso 0.25 1 calc PR E 1
H1P2 H 0.7806 0.9739 0.0547 0.242 Uiso 0.25 1 calc PR E 1
Cl1P Cl 0.8404(8) 0.8818(17) 0.0819(7) 0.065(5) Uiso 0.13 1 d PDU F 1
Cl2P Cl 0.8191(16) 1.018(3) 0.0199(11) 0.111(15) Uiso 0.13 1 d PDU F 1
Cl1R Cl 0.8476(8) 0.8642(18) 0.0577(7) 0.071(6) Uiso 0.13 1 d PDU F 2
Cl2R Cl 0.8051(12) 1.0368(18) 0.0209(8) 0.071(8) Uiso 0.13 1 d PDU F 2
C1Q C 0.828(2) 0.733(5) -0.0367(10) 0.043(16) Uiso 0.13 1 d PDU F .
H1Q1 H 0.8452 0.7932 -0.0419 0.052 Uiso 0.13 1 calc PR . .
H1Q2 H 0.8538 0.6810 -0.0262 0.052 Uiso 0.13 1 calc PR . .
Cl1Q Cl 0.8022(9) 0.692(2) -0.0799(7) 0.079(7) Uiso 0.13 1 d PDU . .
Cl2Q Cl 0.8221(12) 0.768(3) 0.0024(9) 0.104(9) Uiso 0.13 1 d PDU . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0287(3) 0.0222(3) 0.0351(3) 0.0017(2) 0.0085(2) -0.0049(2)
N1 0.033(3) 0.027(3) 0.038(4) -0.002(3) 0.014(3) 0.003(3)
N2 0.037(4) 0.034(4) 0.044(4) 0.007(3) 0.015(3) 0.004(3)
C3 0.044(5) 0.059(6) 0.071(7) 0.006(5) 0.037(5) -0.002(5)
C4 0.044(5) 0.069(7) 0.084(8) -0.003(6) 0.035(5) 0.005(5)
C5 0.041(5) 0.052(5) 0.056(6) -0.005(4) 0.016(4) 0.007(4)
C1A 0.030(4) 0.026(4) 0.036(4) 0.000(3) 0.009(3) -0.003(3)
N1' 0.024(3) 0.034(3) 0.035(3) 0.003(3) 0.013(3) -0.002(3)
N2' 0.025(3) 0.028(3) 0.041(4) 0.002(3) 0.011(3) -0.002(3)
N3' 0.023(3) 0.025(3) 0.038(4) -0.001(3) 0.009(3) -0.003(2)
C4' 0.026(4) 0.026(4) 0.045(5) 0.002(3) 0.013(3) -0.001(3)
C5' 0.033(4) 0.023(4) 0.047(5) 0.004(3) 0.017(4) 0.001(3)
C6' 0.033(4) 0.043(5) 0.040(5) -0.003(4) 0.017(4) -0.004(4)
C7' 0.077(8) 0.078(8) 0.058(6) -0.012(6) 0.027(6) 0.017(6)
C8' 0.125(13) 0.119(12) 0.083(10) -0.030(9) 0.050(9) 0.037(10)
C9' 0.108(11) 0.127(13) 0.045(7) -0.025(8) 0.022(7) -0.006(10)
C10' 0.065(7) 0.082(8) 0.040(5) -0.003(5) 0.017(5) -0.008(6)
C11' 0.037(5) 0.057(6) 0.047(5) -0.003(4) 0.017(4) -0.008(4)
C1B 0.027(4) 0.035(4) 0.040(5) -0.001(3) 0.005(3) 0.005(3)
C2B 0.020(4) 0.037(4) 0.034(4) -0.001(3) 0.005(3) -0.001(3)
C3B 0.026(4) 0.045(5) 0.037(4) 0.009(4) 0.005(3) -0.006(4)
C4B 0.052(5) 0.035(5) 0.051(5) 0.019(4) 0.000(4) -0.008(4)
C5B 0.041(5) 0.025(4) 0.060(6) -0.002(4) 0.008(4) 0.004(3)
C6B 0.036(5) 0.078(7) 0.050(5) -0.017(5) 0.019(4) -0.006(5)
C7B 0.076(8) 0.032(5) 0.105(9) -0.014(5) 0.011(7) 0.012(5)
C8B 0.081(8) 0.057(7) 0.078(8) 0.039(6) 0.008(6) -0.021(6)
C9B 0.056(6) 0.088(8) 0.033(5) -0.001(5) 0.018(4) -0.011(5)
C10B 0.035(4) 0.033(4) 0.053(5) -0.003(4) 0.010(4) -0.006(3)
Cl1 0.0480(12) 0.0430(12) 0.0530(13) -0.0019(10) 0.0100(10) -0.0249(10)
B1C 0.026(4) 0.024(4) 0.026(4) -0.001(3) 0.012(3) -0.003(3)
C11C 0.023(3) 0.025(4) 0.027(4) 0.002(3) 0.009(3) -0.004(3)
C12C 0.027(4) 0.029(4) 0.030(4) 0.004(3) 0.012(3) 0.001(3)
C13C 0.035(4) 0.026(4) 0.035(4) 0.005(3) 0.005(3) 0.003(3)
C14C 0.030(4) 0.027(4) 0.047(5) 0.012(3) 0.008(4) -0.003(3)
C15C 0.029(4) 0.032(4) 0.044(5) 0.013(3) 0.016(4) -0.004(3)
C16C 0.032(4) 0.021(4) 0.036(4) 0.003(3) 0.015(3) -0.001(3)
C17C 0.053(6) 0.034(5) 0.045(5) 0.003(4) 0.010(4) 0.008(4)
C18C 0.063(6) 0.042(5) 0.063(6) 0.009(5) 0.040(5) -0.005(4)
F1C 0.128(6) 0.094(5) 0.065(4) 0.000(4) 0.065(4) -0.037(4)
F2C 0.056(4) 0.111(6) 0.106(5) 0.009(4) 0.058(4) -0.013(4)
F3C 0.178(8) 0.074(5) 0.153(7) 0.072(5) 0.139(7) 0.050(5)
F4C 0.101(5) 0.026(3) 0.094(4) 0.004(3) 0.055(4) 0.007(3)
F5C 0.077(4) 0.083(5) 0.060(4) -0.027(3) -0.008(3) 0.032(4)
F6C 0.068(4) 0.046(3) 0.066(3) 0.003(3) 0.038(3) 0.014(3)
C21C 0.022(3) 0.028(4) 0.027(4) 0.009(3) 0.012(3) 0.001(3)
C22C 0.025(4) 0.029(4) 0.036(4) 0.005(3) 0.012(3) -0.002(3)
C23C 0.022(4) 0.041(4) 0.045(5) 0.011(4) 0.017(3) 0.000(3)
C24C 0.035(4) 0.041(5) 0.050(5) 0.012(4) 0.027(4) 0.008(4)
C25C 0.035(4) 0.031(4) 0.042(4) 0.006(3) 0.023(4) 0.001(3)
C26C 0.022(4) 0.028(4) 0.040(4) 0.009(3) 0.018(3) 0.002(3)
C27C 0.034(5) 0.061(7) 0.080(7) 0.011(5) 0.023(5) -0.006(5)
C28C 0.051(5) 0.033(5) 0.075(6) -0.008(4) 0.036(5) 0.008(4)
F7C 0.039(3) 0.066(4) 0.163(7) -0.028(4) 0.044(4) -0.020(3)
F8C 0.035(3) 0.213(10) 0.087(5) 0.057(6) -0.009(3) -0.024(5)
F9C 0.040(3) 0.083(4) 0.142(6) -0.014(4) 0.055(4) -0.002(3)
F10C 0.082(5) 0.071(4) 0.133(6) -0.048(4) 0.070(5) -0.013(3)
F11C 0.224(10) 0.037(4) 0.133(7) -0.010(4) 0.110(7) -0.039(5)
F12C 0.072(5) 0.072(5) 0.154(7) -0.062(5) 0.012(5) 0.001(4)
C31C 0.021(3) 0.021(3) 0.028(4) 0.000(3) 0.011(3) -0.003(3)
C32C 0.028(4) 0.029(4) 0.031(4) 0.001(3) 0.015(3) 0.000(3)
C33C 0.036(4) 0.029(4) 0.026(4) -0.001(3) 0.014(3) -0.003(3)
C34C 0.023(4) 0.030(4) 0.037(4) -0.004(3) 0.006(3) -0.001(3)
C35C 0.026(4) 0.031(4) 0.040(4) -0.007(3) 0.016(3) 0.003(3)
C36C 0.029(4) 0.024(3) 0.031(4) -0.002(3) 0.013(3) -0.005(3)
C37C 0.040(4) 0.082(5) 0.031(4) -0.006(4) 0.013(3) -0.011(4)
C38C 0.029(3) 0.068(5) 0.060(4) -0.029(4) 0.023(3) -0.015(3)
F13B 0.051(6) 0.085(11) 0.036(7) -0.016(9) 0.024(5) -0.009(6)
F14B 0.064(9) 0.113(8) 0.032(7) 0.014(7) -0.002(7) 0.010(7)
F15B 0.066(8) 0.124(8) 0.034(8) -0.032(7) 0.012(7) -0.049(7)
F13C 0.056(6) 0.077(10) 0.033(6) 0.001(8) 0.027(5) -0.009(6)
F14C 0.049(7) 0.138(10) 0.030(6) -0.015(8) -0.008(6) 0.003(7)
F15C 0.090(11) 0.094(7) 0.031(8) -0.030(6) 0.016(8) -0.043(7)
F16A 0.033(6) 0.107(9) 0.076(7) -0.036(8) 0.009(5) -0.015(8)
F17A 0.038(8) 0.077(7) 0.094(9) -0.038(6) 0.042(7) -0.038(6)
F18A 0.024(6) 0.065(8) 0.055(7) -0.030(7) 0.027(6) -0.012(8)
F16B 0.023(8) 0.068(9) 0.068(9) -0.031(9) 0.028(7) -0.019(8)
F17B 0.033(8) 0.084(9) 0.064(7) -0.028(8) 0.026(7) -0.022(9)
F18B 0.034(9) 0.072(7) 0.072(9) -0.038(8) 0.019(8) -0.016(8)
F16C 0.017(5) 0.067(6) 0.076(6) -0.023(5) 0.019(4) -0.007(4)
F17C 0.019(5) 0.074(6) 0.063(7) -0.036(5) 0.027(5) -0.028(5)
F18C 0.030(5) 0.075(8) 0.056(5) -0.042(5) 0.028(5) -0.019(7)
C41C 0.025(4) 0.026(4) 0.026(4) 0.003(3) 0.010(3) 0.000(3)
C42C 0.039(4) 0.027(4) 0.023(4) -0.002(3) 0.010(3) -0.007(3)
C43C 0.056(5) 0.029(4) 0.028(4) -0.001(3) 0.019(4) -0.013(4)
C44C 0.064(6) 0.031(4) 0.024(4) 0.001(3) 0.012(4) -0.010(4)
C45C 0.048(5) 0.028(4) 0.024(4) -0.001(3) 0.003(3) -0.001(4)
C46C 0.029(4) 0.024(4) 0.032(4) 0.005(3) 0.005(3) -0.006(3)
C47C 0.073(7) 0.040(5) 0.035(5) 0.004(4) 0.019(5) -0.020(5)
C48C 0.059(6) 0.036(5) 0.033(5) 0.003(4) 0.006(4) -0.007(4)
F19C 0.209(9) 0.030(3) 0.061(4) -0.006(3) -0.008(5) -0.025(4)
F20C 0.058(4) 0.132(7) 0.070(4) -0.044(4) 0.014(3) -0.027(4)
F21C 0.098(5) 0.082(4) 0.040(3) -0.023(3) 0.024(3) -0.025(4)
F22C 0.150(6) 0.039(3) 0.040(3) 0.007(2) 0.023(4) -0.035(3)
F23C 0.095(5) 0.074(5) 0.149(7) 0.011(5) 0.061(5) -0.043(4)
F24C 0.144(6) 0.035(3) 0.053(3) -0.010(3) 0.048(4) -0.036(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N3' 2.085(6) . ?
Rh1 N2 2.103(7) . ?
Rh1 C4B 2.143(8) . ?
Rh1 C5B 2.145(8) . ?
Rh1 C2B 2.154(7) . ?
Rh1 C3B 2.164(8) . ?
Rh1 C1B 2.165(8) . ?
Rh1 Cl1 2.378(2) . ?
N1 C5 1.334(11) . ?
N1 N2 1.361(9) . ?
N1 C1A 1.440(10) . ?
N2 C3 1.336(11) . ?
C3 C4 1.383(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.381(14) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.492(11) . ?
C1A H1A1 0.9900 . ?
C1A H1A2 0.9900 . ?
N1' N2' 1.343(8) . ?
N1' C5' 1.365(10) . ?
N1' C6' 1.420(10) . ?
N2' N3' 1.326(9) . ?
N3' C4' 1.358(9) . ?
C4' C5' 1.356(11) . ?
C5' H5' 0.9500 . ?
C6' C7' 1.374(13) . ?
C6' C11' 1.376(12) . ?
C7' C8' 1.395(17) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.40(2) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.329(18) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.389(13) . ?
C10' H10' 0.9500 . ?
C11' H11' 0.9500 . ?
C1B C5B 1.428(12) . ?
C1B C2B 1.439(11) . ?
C1B C6B 1.490(12) . ?
C2B C3B 1.457(11) . ?
C2B C10B 1.485(11) . ?
C3B C4B 1.418(12) . ?
C3B C9B 1.473(13) . ?
C4B C5B 1.439(14) . ?
C4B C8B 1.483(13) . ?
C5B C7B 1.511(12) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7A1 0.9800 . ?
C7B H7A2 0.9800 . ?
C7B H7A3 0.9800 . ?
C8B H8A1 0.9800 . ?
C8B H8A2 0.9800 . ?
C8B H8A3 0.9800 . ?
C9B H9A1 0.9800 . ?
C9B H9A2 0.9800 . ?
C9B H9A3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C31C 1.630(10) . ?
B1C C11C 1.645(10) . ?
B1C C41C 1.646(10) . ?
B1C C21C 1.651(10) . ?
C11C C16C 1.392(10) . ?
C11C C12C 1.392(10) . ?
C12C C13C 1.384(10) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.384(11) . ?
C13C C17C 1.484(12) . ?
C14C C15C 1.372(12) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.384(10) . ?
C15C C18C 1.500(12) . ?
C16C H16C 0.9500 . ?
C17C F5C 1.335(10) . ?
C17C F6C 1.339(11) . ?
C17C F4C 1.341(10) . ?
C18C F1C 1.316(12) . ?
C18C F2C 1.324(12) . ?
C18C F3C 1.328(11) . ?
C21C C22C 1.395(10) . ?
C21C C26C 1.404(10) . ?
C22C C23C 1.387(11) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.395(12) . ?
C23C C27C 1.499(12) . ?
C24C C25C 1.365(11) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.391(10) . ?
C25C C28C 1.487(12) . ?
C26C H26C 0.9500 . ?
C27C F8C 1.293(12) . ?
C27C F7C 1.315(12) . ?
C27C F9C 1.338(12) . ?
C28C F11C 1.299(11) . ?
C28C F10C 1.311(10) . ?
C28C F12C 1.338(12) . ?
C31C C36C 1.393(10) . ?
C31C C32C 1.409(10) . ?
C32C C33C 1.375(10) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.402(11) . ?
C33C C37C 1.504(11) . ?
C34C C35C 1.389(11) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.395(10) . ?
C35C C38C 1.484(11) . ?
C36C H36C 0.9500 . ?
C37C F13B 1.308(13) . ?
C37C F14C 1.318(12) . ?
C37C F13C 1.319(13) . ?
C37C F15B 1.323(11) . ?
C37C F15C 1.358(12) . ?
C37C F14B 1.359(11) . ?
C38C F16A 1.299(15) . ?
C38C F17C 1.308(11) . ?
C38C F18A 1.311(17) . ?
C38C F18C 1.328(13) . ?
C38C F18B 1.342(15) . ?
C38C F16B 1.343(15) . ?
C38C F17A 1.357(15) . ?
C38C F17B 1.360(15) . ?
C38C F16C 1.408(11) . ?
C41C C46C 1.381(10) . ?
C41C C42C 1.408(10) . ?
C42C C43C 1.401(10) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.393(11) . ?
C43C C47C 1.492(11) . ?
C44C C45C 1.358(11) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.400(11) . ?
C45C C48C 1.504(11) . ?
C46C H46C 0.9500 . ?
C47C F24C 1.333(11) . ?
C47C F22C 1.341(10) . ?
C47C F23C 1.352(13) . ?
C48C F21C 1.309(11) . ?
C48C F20C 1.317(11) . ?
C48C F19C 1.318(10) . ?
C1M Cl1N 1.712(16) . ?
C1M Cl2N 1.712(16) . ?
C1M Cl2M 1.715(16) . ?
C1M Cl1O 1.717(16) . ?
C1M Cl1M 1.721(15) . ?
C1M Cl2O 1.723(16) . ?
C1M H1M1 0.9900 . ?
C1M H1M2 0.9900 . ?
C1P Cl1R 1.57(3) . ?
C1P Cl2P 1.57(3) . ?
C1P Cl1P 1.57(3) . ?
C1P Cl2R 1.57(3) . ?
C1P H1P1 0.9900 . ?
C1P H1P2 0.9900 . ?
Cl1R Cl2Q 2.26(4) . ?
C1Q Cl1Q 1.57(3) . ?
C1Q Cl2Q 1.57(3) . ?
C1Q H1Q1 0.9900 . ?
C1Q H1Q2 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3' Rh1 N2 84.2(2) . . ?
N3' Rh1 C4B 156.4(3) . . ?
N2 Rh1 C4B 119.3(4) . . ?
N3' Rh1 C5B 117.2(3) . . ?
N2 Rh1 C5B 158.5(3) . . ?
C4B Rh1 C5B 39.2(4) . . ?
N3' Rh1 C2B 107.7(3) . . ?
N2 Rh1 C2B 107.6(3) . . ?
C4B Rh1 C2B 65.6(3) . . ?
C5B Rh1 C2B 65.2(3) . . ?
N3' Rh1 C3B 145.6(3) . . ?
N2 Rh1 C3B 96.3(3) . . ?
C4B Rh1 C3B 38.4(3) . . ?
C5B Rh1 C3B 64.9(3) . . ?
C2B Rh1 C3B 39.4(3) . . ?
N3' Rh1 C1B 94.8(3) . . ?
N2 Rh1 C1B 144.3(3) . . ?
C4B Rh1 C1B 65.4(4) . . ?
C5B Rh1 C1B 38.7(3) . . ?
C2B Rh1 C1B 38.9(3) . . ?
C3B Rh1 C1B 65.3(3) . . ?
N3' Rh1 Cl1 89.34(17) . . ?
N2 Rh1 Cl1 86.2(2) . . ?
C4B Rh1 Cl1 93.8(2) . . ?
C5B Rh1 Cl1 96.1(2) . . ?
C2B Rh1 Cl1 158.8(2) . . ?
C3B Rh1 Cl1 125.0(2) . . ?
C1B Rh1 Cl1 129.5(2) . . ?
C5 N1 N2 111.0(7) . . ?
C5 N1 C1A 129.4(7) . . ?
N2 N1 C1A 119.5(6) . . ?
C3 N2 N1 105.4(7) . . ?
C3 N2 Rh1 129.4(6) . . ?
N1 N2 Rh1 124.4(5) . . ?
N2 C3 C4 110.9(9) . . ?
N2 C3 H3 124.5 . . ?
C4 C3 H3 124.5 . . ?
C5 C4 C3 105.1(8) . . ?
C5 C4 H4 127.4 . . ?
C3 C4 H4 127.4 . . ?
N1 C5 C4 107.5(8) . . ?
N1 C5 H5 126.2 . . ?
C4 C5 H5 126.2 . . ?
N1 C1A C4' 111.5(6) . . ?
N1 C1A H1A1 109.3 . . ?
C4' C1A H1A1 109.3 . . ?
N1 C1A H1A2 109.3 . . ?
C4' C1A H1A2 109.3 . . ?
H1A1 C1A H1A2 108.0 . . ?
N2' N1' C5' 111.4(6) . . ?
N2' N1' C6' 120.0(6) . . ?
C5' N1' C6' 128.6(7) . . ?
N3' N2' N1' 105.6(6) . . ?
N2' N3' C4' 110.0(6) . . ?
N2' N3' Rh1 126.2(5) . . ?
C4' N3' Rh1 123.8(5) . . ?
C5' C4' N3' 108.2(7) . . ?
C5' C4' C1A 131.4(7) . . ?
N3' C4' C1A 120.4(7) . . ?
C4' C5' N1' 104.7(7) . . ?
C4' C5' H5' 127.6 . . ?
N1' C5' H5' 127.6 . . ?
C7' C6' C11' 122.1(9) . . ?
C7' C6' N1' 118.8(8) . . ?
C11' C6' N1' 118.9(8) . . ?
C6' C7' C8' 117.7(11) . . ?
C6' C7' H7' 121.1 . . ?
C8' C7' H7' 121.2 . . ?
C7' C8' C9' 119.8(12) . . ?
C7' C8' H8' 120.1 . . ?
C9' C8' H8' 120.1 . . ?
C10' C9' C8' 120.9(11) . . ?
C10' C9' H9' 119.6 . . ?
C8' C9' H9' 119.6 . . ?
C9' C10' C11' 120.6(11) . . ?
C9' C10' H10' 119.7 . . ?
C11' C10' H10' 119.7 . . ?
C6' C11' C10' 118.9(9) . . ?
C6' C11' H11' 120.6 . . ?
C10' C11' H11' 120.6 . . ?
C5B C1B C2B 107.8(7) . . ?
C5B C1B C6B 126.3(8) . . ?
C2B C1B C6B 126.0(8) . . ?
C5B C1B Rh1 69.9(5) . . ?
C2B C1B Rh1 70.1(4) . . ?
C6B C1B Rh1 124.9(6) . . ?
C1B C2B C3B 107.5(7) . . ?
C1B C2B C10B 126.2(7) . . ?
C3B C2B C10B 126.0(7) . . ?
C1B C2B Rh1 71.0(4) . . ?
C3B C2B Rh1 70.7(4) . . ?
C10B C2B Rh1 129.1(6) . . ?
C4B C3B C2B 108.0(8) . . ?
C4B C3B C9B 127.2(8) . . ?
C2B C3B C9B 124.8(8) . . ?
C4B C3B Rh1 70.0(5) . . ?
C2B C3B Rh1 69.9(4) . . ?
C9B C3B Rh1 126.0(6) . . ?
C3B C4B C5B 108.1(7) . . ?
C3B C4B C8B 126.2(10) . . ?
C5B C4B C8B 125.6(9) . . ?
C3B C4B Rh1 71.6(5) . . ?
C5B C4B Rh1 70.5(5) . . ?
C8B C4B Rh1 126.3(7) . . ?
C1B C5B C4B 108.6(7) . . ?
C1B C5B C7B 125.5(9) . . ?
C4B C5B C7B 125.8(9) . . ?
C1B C5B Rh1 71.4(4) . . ?
C4B C5B Rh1 70.3(5) . . ?
C7B C5B Rh1 126.7(7) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C5B C7B H7A1 109.5 . . ?
C5B C7B H7A2 109.5 . . ?
H7A1 C7B H7A2 109.5 . . ?
C5B C7B H7A3 109.5 . . ?
H7A1 C7B H7A3 109.5 . . ?
H7A2 C7B H7A3 109.5 . . ?
C4B C8B H8A1 109.5 . . ?
C4B C8B H8A2 109.5 . . ?
H8A1 C8B H8A2 109.5 . . ?
C4B C8B H8A3 109.5 . . ?
H8A1 C8B H8A3 109.5 . . ?
H8A2 C8B H8A3 109.5 . . ?
C3B C9B H9A1 109.5 . . ?
C3B C9B H9A2 109.5 . . ?
H9A1 C9B H9A2 109.5 . . ?
C3B C9B H9A3 109.5 . . ?
H9A1 C9B H9A3 109.5 . . ?
H9A2 C9B H9A3 109.5 . . ?
C2B C10B H10A 109.5 . . ?
C2B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C2B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C31C B1C C11C 103.7(5) . . ?
C31C B1C C41C 112.6(6) . . ?
C11C B1C C41C 114.1(6) . . ?
C31C B1C C21C 112.6(6) . . ?
C11C B1C C21C 111.1(6) . . ?
C41C B1C C21C 102.9(5) . . ?
C16C C11C C12C 115.9(6) . . ?
C16C C11C B1C 121.1(6) . . ?
C12C C11C B1C 122.7(6) . . ?
C13C C12C C11C 122.5(7) . . ?
C13C C12C H12C 118.8 . . ?
C11C C12C H12C 118.8 . . ?
C14C C13C C12C 120.6(7) . . ?
C14C C13C C17C 120.1(7) . . ?
C12C C13C C17C 119.2(7) . . ?
C15C C14C C13C 117.5(7) . . ?
C15C C14C H14C 121.2 . . ?
C13C C14C H14C 121.2 . . ?
C14C C15C C16C 121.9(7) . . ?
C14C C15C C18C 119.3(7) . . ?
C16C C15C C18C 118.8(8) . . ?
C15C C16C C11C 121.5(7) . . ?
C15C C16C H16C 119.3 . . ?
C11C C16C H16C 119.3 . . ?
F5C C17C F6C 105.3(8) . . ?
F5C C17C F4C 107.9(8) . . ?
F6C C17C F4C 104.4(7) . . ?
F5C C17C C13C 112.1(7) . . ?
F6C C17C C13C 113.1(7) . . ?
F4C C17C C13C 113.4(8) . . ?
F1C C18C F2C 105.3(8) . . ?
F1C C18C F3C 106.3(9) . . ?
F2C C18C F3C 105.0(8) . . ?
F1C C18C C15C 114.7(7) . . ?
F2C C18C C15C 112.5(8) . . ?
F3C C18C C15C 112.2(8) . . ?
C22C C21C C26C 115.6(6) . . ?
C22C C21C B1C 121.0(6) . . ?
C26C C21C B1C 123.3(6) . . ?
C23C C22C C21C 122.6(7) . . ?
C23C C22C H22C 118.7 . . ?
C21C C22C H22C 118.7 . . ?
C22C C23C C24C 119.8(7) . . ?
C22C C23C C27C 120.7(8) . . ?
C24C C23C C27C 119.4(8) . . ?
C25C C24C C23C 119.2(7) . . ?
C25C C24C H24C 120.4 . . ?
C23C C24C H24C 120.4 . . ?
C24C C25C C26C 120.4(7) . . ?
C24C C25C C28C 120.1(7) . . ?
C26C C25C C28C 119.5(7) . . ?
C25C C26C C21C 122.3(7) . . ?
C25C C26C H26C 118.8 . . ?
C21C C26C H26C 118.8 . . ?
F8C C27C F7C 108.8(10) . . ?
F8C C27C F9C 105.2(9) . . ?
F7C C27C F9C 104.7(8) . . ?
F8C C27C C23C 113.3(8) . . ?
F7C C27C C23C 112.4(8) . . ?
F9C C27C C23C 112.0(9) . . ?
F11C C28C F10C 108.1(8) . . ?
F11C C28C F12C 104.8(9) . . ?
F10C C28C F12C 104.0(9) . . ?
F11C C28C C25C 113.5(8) . . ?
F10C C28C C25C 113.4(8) . . ?
F12C C28C C25C 112.4(7) . . ?
C36C C31C C32C 115.7(6) . . ?
C36C C31C B1C 122.6(6) . . ?
C32C C31C B1C 121.1(6) . . ?
C33C C32C C31C 122.4(7) . . ?
C33C C32C H32C 118.8 . . ?
C31C C32C H32C 118.8 . . ?
C32C C33C C34C 121.1(7) . . ?
C32C C33C C37C 121.3(7) . . ?
C34C C33C C37C 117.5(7) . . ?
C35C C34C C33C 117.5(7) . . ?
C35C C34C H34C 121.3 . . ?
C33C C34C H34C 121.3 . . ?
C34C C35C C36C 120.8(7) . . ?
C34C C35C C38C 117.8(6) . . ?
C36C C35C C38C 121.4(7) . . ?
C31C C36C C35C 122.5(7) . . ?
C31C C36C H36C 118.8 . . ?
C35C C36C H36C 118.8 . . ?
F13B C37C F14C 119(2) . . ?
F13B C37C F13C 17.0(16) . . ?
F14C C37C F13C 108.7(12) . . ?
F13B C37C F15B 109.2(12) . . ?
F14C C37C F15B 76.8(10) . . ?
F13C C37C F15B 121.7(19) . . ?
F13B C37C F15C 88.9(14) . . ?
F14C C37C F15C 105.6(9) . . ?
F13C C37C F15C 105.0(11) . . ?
F15B C37C F15C 29.6(9) . . ?
F13B C37C F14B 106.6(11) . . ?
F14C C37C F14B 27.6(9) . . ?
F13C C37C F14B 91.5(15) . . ?
F15B C37C F14B 104.2(9) . . ?
F15C C37C F14B 132.1(10) . . ?
F13B C37C C33C 113.7(15) . . ?
F14C C37C C33C 117.3(12) . . ?
F13C C37C C33C 112.7(16) . . ?
F15B C37C C33C 114.7(10) . . ?
F15C C37C C33C 106.5(10) . . ?
F14B C37C C33C 107.7(11) . . ?
F16A C38C F17C 70.7(10) . . ?
F16A C38C F18A 110.6(13) . . ?
F17C C38C F18A 125.0(16) . . ?
F16A C38C F18C 121.9(15) . . ?
F17C C38C F18C 109.1(10) . . ?
F18A C38C F18C 21.3(12) . . ?
F16A C38C F18B 69.8(15) . . ?
F17C C38C F18B 125.2(17) . . ?
F18A C38C F18B 45.3(16) . . ?
F18C C38C F18B 64.9(17) . . ?
F16A C38C F16B 39.6(15) . . ?
F17C C38C F16B 32.4(15) . . ?
F18A C38C F16B 133(2) . . ?
F18C C38C F16B 128(2) . . ?
F18B C38C F16B 105.5(14) . . ?
F16A C38C F17A 106.5(11) . . ?
F17C C38C F17A 36.4(7) . . ?
F18A C38C F17A 106.1(12) . . ?
F18C C38C F17A 85.2(11) . . ?
F18B C38C F17A 137.2(18) . . ?
F16B C38C F17A 68.8(15) . . ?
F16A C38C F17B 130.4(17) . . ?
F17C C38C F17B 74.9(15) . . ?
F18A C38C F17B 63.8(17) . . ?
F18C C38C F17B 42.5(16) . . ?
F18B C38C F17B 104.9(13) . . ?
F16B C38C F17B 105.0(13) . . ?
F17A C38C F17B 43.6(15) . . ?
F16A C38C F16C 33.4(9) . . ?
F17C C38C F16C 102.8(8) . . ?
F18A C38C F16C 84.8(11) . . ?
F18C C38C F16C 102.9(9) . . ?
F18B C38C F16C 39.8(16) . . ?
F16B C38C F16C 73.0(16) . . ?
F17A C38C F16C 136.3(10) . . ?
F17B C38C F16C 135.6(17) . . ?
F16A C38C C35C 115.6(11) . . ?
F17C C38C C35C 115.7(8) . . ?
F18A C38C C35C 112.2(16) . . ?
F18C C38C C35C 115.4(12) . . ?
F18B C38C C35C 114.9(16) . . ?
F16B C38C C35C 114.5(17) . . ?
F17A C38C C35C 105.1(9) . . ?
F17B C38C C35C 111.1(16) . . ?
F16C C38C C35C 109.5(7) . . ?
C46C C41C C42C 116.2(6) . . ?
C46C C41C B1C 125.6(6) . . ?
C42C C41C B1C 118.0(6) . . ?
C43C C42C C41C 121.7(7) . . ?
C43C C42C H42C 119.2 . . ?
C41C C42C H42C 119.2 . . ?
C44C C43C C42C 120.4(7) . . ?
C44C C43C C47C 120.6(7) . . ?
C42C C43C C47C 119.0(7) . . ?
C45C C44C C43C 118.1(7) . . ?
C45C C44C H44C 121.0 . . ?
C43C C44C H44C 121.0 . . ?
C44C C45C C46C 121.8(7) . . ?
C44C C45C C48C 118.2(7) . . ?
C46C C45C C48C 119.9(7) . . ?
C41C C46C C45C 121.7(7) . . ?
C41C C46C H46C 119.1 . . ?
C45C C46C H46C 119.1 . . ?
F24C C47C F22C 106.7(8) . . ?
F24C C47C F23C 105.3(8) . . ?
F22C C47C F23C 106.1(8) . . ?
F24C C47C C43C 113.2(7) . . ?
F22C C47C C43C 112.5(7) . . ?
F23C C47C C43C 112.5(8) . . ?
F21C C48C F20C 104.9(7) . . ?
F21C C48C F19C 105.9(9) . . ?
F20C C48C F19C 106.8(9) . . ?
F21C C48C C45C 113.5(8) . . ?
F20C C48C C45C 111.8(8) . . ?
F19C C48C C45C 113.2(7) . . ?
Cl1N C1M Cl2N 122(2) . . ?
Cl1N C1M Cl2M 106(2) . . ?
Cl2N C1M Cl2M 16.4(17) . . ?
Cl1N C1M Cl1O 31.7(17) . . ?
Cl2N C1M Cl1O 150(2) . . ?
Cl2M C1M Cl1O 134(3) . . ?
Cl1N C1M Cl1M 24.0(11) . . ?
Cl2N C1M Cl1M 129(2) . . ?
Cl2M C1M Cl1M 113(2) . . ?
Cl1O C1M Cl1M 21.0(14) . . ?
Cl1N C1M Cl2O 102(2) . . ?
Cl2N C1M Cl2O 27.8(15) . . ?
Cl2M C1M Cl2O 18.6(17) . . ?
Cl1O C1M Cl2O 123(2) . . ?
Cl1M C1M Cl2O 101.8(18) . . ?
Cl1N C1M H1M1 131.4 . . ?
Cl2N C1M H1M1 95.8 . . ?
Cl2M C1M H1M1 108.9 . . ?
Cl1O C1M H1M1 101.1 . . ?
Cl1M C1M H1M1 108.9 . . ?
Cl2O C1M H1M1 101.0 . . ?
Cl1N C1M H1M2 91.3 . . ?
Cl2N C1M H1M2 104.9 . . ?
Cl2M C1M H1M2 108.9 . . ?
Cl1O C1M H1M2 93.8 . . ?
Cl1M C1M H1M2 108.9 . . ?
Cl2O C1M H1M2 127.4 . . ?
H1M1 C1M H1M2 107.7 . . ?
Cl1R C1P Cl2P 100(3) . . ?
Cl1R C1P Cl1P 37.4(13) . . ?
Cl2P C1P Cl1P 123(4) . . ?
Cl1R C1P Cl2R 118(4) . . ?
Cl2P C1P Cl2R 18.4(19) . . ?
Cl1P C1P Cl2R 135(5) . . ?
Cl1R C1P H1P1 87.7 . . ?
Cl2P C1P H1P1 106.7 . . ?
Cl1P C1P H1P1 106.7 . . ?
Cl2R C1P H1P1 109.1 . . ?
Cl1R C1P H1P2 143.9 . . ?
Cl2P C1P H1P2 106.7 . . ?
Cl1P C1P H1P2 106.7 . . ?
Cl2R C1P H1P2 88.8 . . ?
H1P1 C1P H1P2 106.6 . . ?
C1P Cl1R Cl2Q 97(3) . . ?
Cl1Q C1Q Cl2Q 146(5) . . ?
Cl1Q C1Q H1Q1 100.5 . . ?
Cl2Q C1Q H1Q1 100.5 . . ?
Cl1Q C1Q H1Q2 100.5 . . ?
Cl2Q C1Q H1Q2 100.5 . . ?
H1Q1 C1Q H1Q2 104.3 . . ?
C1Q Cl2Q Cl1R 149(3) . . ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max 1.543
_refine_diff_density_min -1.492
_refine_diff_density_rms 0.135
_iucr_refine_instructions_details
;
TITL Carol9_C2byc in C2/c
CELL 0.71073 29.9749 13.0963 36.3708 90.000 111.572 90.000
ZERR 8.00 0.0017 0.0008 0.0021 0.000 0.002 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H B N F Rh Cl
UNIT 439 318 8 40 192 8 22
OMIT 2 0 2
OMIT 0 0 2
OMIT -2 0 2
OMIT 0 0 4
OMIT 1 1 1
OMIT 2 0 0
OMIT 1 1 2
OMIT -1 1 1
OMIT -1 1 3
OMIT -2 0 4
OMIT -6 0 4
OMIT -1 1 2
OMIT 1 1 0
OMIT 0 2 3
OMIT 6 0 0
OMIT -2 2 2
OMIT -4 0 4
OMIT 3 1 0
OMIT -2 2 1
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.338 0.229 0.153
SADI F13B F14B F14B F15B F15B F13B F13C F14C F14C F15C F15C F13C
SADI C37C F13B C37C F14B C37C F15B C37C F13C C37C F14C C37C F15C
SADI C38C F16B C38C F17B C38C F18B C38C F16C C38C F17C C38C F18C
SADI C38C F16A C38C F17A C38C F18A
SADI F16A F17A F17A F18A F18A F16A
SADI F16B F17B F17B F18B F18B F16B F16C F17C F17C F18C F18C F16C
SADI 0.01 C1M CL1N C1M CL2N C1M CL1M C1M CL2M C1M CL1O C1M CL2O
SADI 0.01 C1Q CL1Q C1Q CL2Q C1P CL1P C1P CL2P C1P CL1R C1P CL2R
DELU 0.01 C37C F13B F14B F15B F13C F14C F15C
DELU 0.01 C38C F16A F17A F18A F16B F17B F18B F16C F17C F18C
DELU C1M CL1M CL2M CL1N CL2N CL1O CL2O
DELU C1Q CL1Q CL2Q
DELU C1P CL1P CL2P CL1R CL2R
SIMU 0.01 C37C F13B F14B F15B F13C F14C F15C
SIMU 0.01 C38C F16A F17A F18A F16B F17B F18B F16C F17C F18C
TEMP -121.740
WGHT 0.102300 205.565308
FVAR 0.03140 0.51340
MOLE 1
RH1 6 0.836059 0.414025 0.810823 11.00000 0.02870 0.02219 =
0.03507 0.00175 0.00852 -0.00493
N1 4 0.779101 0.614709 0.801407 11.00000 0.03271 0.02691 =
0.03842 -0.00240 0.01449 0.00297
N2 4 0.788124 0.521044 0.818828 11.00000 0.03656 0.03388 =
0.04398 0.00719 0.01486 0.00441
C3 1 0.755397 0.508750 0.835368 11.00000 0.04440 0.05943 =
0.07096 0.00569 0.03686 -0.00240
AFIX 43
H3 2 0.752910 0.450029 0.849830 11.00000 -1.20000
AFIX 0
C4 1 0.725621 0.592961 0.828615 11.00000 0.04360 0.06882 =
0.08355 -0.00279 0.03504 0.00536
AFIX 43
H4 2 0.699870 0.603518 0.837494 11.00000 -1.20000
AFIX 0
C5 1 0.741382 0.658407 0.806183 11.00000 0.04111 0.05203 =
0.05565 -0.00497 0.01589 0.00736
AFIX 43
H5 2 0.727839 0.722802 0.796006 11.00000 -1.20000
AFIX 0
C1A 1 0.808195 0.651296 0.780272 11.00000 0.02960 0.02563 =
0.03624 0.00030 0.00879 -0.00318
AFIX 23
H1A1 2 0.841835 0.658178 0.798836 11.00000 -1.20000
H1A2 2 0.796760 0.719674 0.769198 11.00000 -1.20000
AFIX 0
N1' 4 0.800235 0.504115 0.693506 11.00000 0.02417 0.03355 =
0.03511 0.00321 0.01286 -0.00184
N2' 4 0.812679 0.432003 0.721753 11.00000 0.02528 0.02827 =
0.04125 0.00179 0.01145 -0.00242
N3' 4 0.816635 0.479955 0.754933 11.00000 0.02341 0.02467 =
0.03834 -0.00073 0.00856 -0.00279
C4' 1 0.806292 0.580601 0.747576 11.00000 0.02590 0.02552 =
0.04547 0.00208 0.01343 -0.00113
C5' 1 0.795427 0.597284 0.708444 11.00000 0.03269 0.02314 =
0.04697 0.00368 0.01670 0.00146
AFIX 43
H5' 2 0.786455 0.659953 0.694512 11.00000 -1.20000
AFIX 0
C6' 1 0.793473 0.477814 0.653934 11.00000 0.03326 0.04292 =
0.04014 -0.00270 0.01717 -0.00437
C7' 1 0.821547 0.402352 0.647377 11.00000 0.07674 0.07812 =
0.05815 -0.01222 0.02719 0.01719
AFIX 43
H7' 2 0.843693 0.365005 0.668693 11.00000 -1.20000
AFIX 0
C8' 1 0.816395 0.382503 0.608342 11.00000 0.12529 0.11917 =
0.08252 -0.02981 0.05037 0.03658
AFIX 43
H8' 2 0.835413 0.331350 0.602679 11.00000 -1.20000
AFIX 0
C9' 1 0.783087 0.438230 0.577501 11.00000 0.10767 0.12723 =
0.04540 -0.02489 0.02197 -0.00621
AFIX 43
H9' 2 0.779002 0.423096 0.550911 11.00000 -1.20000
AFIX 0
C10' 1 0.757138 0.511974 0.584963 11.00000 0.06502 0.08150 =
0.04022 -0.00258 0.01723 -0.00849
AFIX 43
H10' 2 0.735478 0.550416 0.563735 11.00000 -1.20000
AFIX 0
C11' 1 0.761404 0.533343 0.623525 11.00000 0.03684 0.05691 =
0.04736 -0.00270 0.01662 -0.00816
AFIX 43
H11' 2 0.742510 0.585390 0.628815 11.00000 -1.20000
AFIX 0
C1B 1 0.909987 0.387960 0.817562 11.00000 0.02742 0.03543 =
0.04022 -0.00140 0.00527 0.00473
C2B 1 0.907715 0.464148 0.845348 11.00000 0.02005 0.03736 =
0.03404 -0.00126 0.00516 -0.00135
C3B 1 0.886623 0.416261 0.871298 11.00000 0.02616 0.04486 =
0.03661 0.00876 0.00525 -0.00630
C4B 1 0.874834 0.314083 0.858537 11.00000 0.05168 0.03549 =
0.05077 0.01947 0.00037 -0.00770
C5B 1 0.889492 0.296214 0.825583 11.00000 0.04119 0.02465 =
0.06047 -0.00172 0.00836 0.00353
C6B 1 0.929655 0.402864 0.785820 11.00000 0.03639 0.07760 =
0.05041 -0.01707 0.01875 -0.00631
AFIX 137
H6B1 2 0.963431 0.382142 0.795585 11.00000 -1.50000
H6B2 2 0.927067 0.475025 0.778184 11.00000 -1.50000
H6B3 2 0.911405 0.361230 0.762807 11.00000 -1.50000
AFIX 0
C7B 1 0.886265 0.195645 0.804392 11.00000 0.07630 0.03210 =
0.10450 -0.01370 0.01121 0.01186
AFIX 137
H7A1 2 0.918151 0.176263 0.805106 11.00000 -1.50000
H7A2 2 0.864298 0.202603 0.776848 11.00000 -1.50000
H7A3 2 0.874251 0.142846 0.817478 11.00000 -1.50000
AFIX 0
C8B 1 0.853756 0.236842 0.877201 11.00000 0.08131 0.05662 =
0.07776 0.03880 0.00756 -0.02112
AFIX 137
H8A1 2 0.825199 0.206943 0.857098 11.00000 -1.50000
H8A2 2 0.844767 0.269523 0.897717 11.00000 -1.50000
H8A3 2 0.877370 0.183010 0.889123 11.00000 -1.50000
AFIX 0
C9B 1 0.879535 0.467210 0.904838 11.00000 0.05600 0.08843 =
0.03315 -0.00142 0.01835 -0.01098
AFIX 137
H9A1 2 0.907998 0.457068 0.928851 11.00000 -1.50000
H9A2 2 0.851431 0.438029 0.908636 11.00000 -1.50000
H9A3 2 0.874461 0.540438 0.899345 11.00000 -1.50000
AFIX 0
C10B 1 0.928367 0.568561 0.849865 11.00000 0.03462 0.03348 =
0.05306 -0.00266 0.00968 -0.00585
AFIX 137
H10A 2 0.910023 0.614157 0.860393 11.00000 -1.50000
H10B 2 0.926825 0.593773 0.824056 11.00000 -1.50000
H10C 2 0.961883 0.566658 0.868127 11.00000 -1.50000
AFIX 0
CL1 7 0.768792 0.303000 0.785942 11.00000 0.04800 0.04297 =
0.05304 -0.00193 0.01003 -0.02493
MOLE 2
B1C 3 1.017727 0.910806 0.876517 11.00000 0.02602 0.02367 =
0.02587 -0.00148 0.01194 -0.00253
C11C 1 1.029260 1.031075 0.870455 11.00000 0.02333 0.02468 =
0.02705 0.00245 0.00911 -0.00375
C12C 1 1.018044 1.110567 0.890972 11.00000 0.02665 0.02922 =
0.03002 0.00394 0.01158 0.00099
AFIX 43
H12C 2 1.004933 1.094546 0.910409 11.00000 -1.20000
AFIX 0
C13C 1 1.025277 1.212059 0.884117 11.00000 0.03510 0.02639 =
0.03504 0.00472 0.00492 0.00315
C14C 1 1.042368 1.238946 0.854908 11.00000 0.02999 0.02665 =
0.04724 0.01207 0.00813 -0.00270
AFIX 43
H14C 2 1.047628 1.308370 0.850092 11.00000 -1.20000
AFIX 0
C15C 1 1.051435 1.161648 0.833166 11.00000 0.02944 0.03229 =
0.04449 0.01307 0.01620 -0.00405
C16C 1 1.045923 1.059918 0.840947 11.00000 0.03181 0.02125 =
0.03625 0.00270 0.01548 -0.00053
AFIX 43
H16C 2 1.053687 1.008639 0.825809 11.00000 -1.20000
AFIX 0
C17C 1 1.016097 1.291900 0.909406 11.00000 0.05272 0.03428 =
0.04501 0.00271 0.00966 0.00759
C18C 1 1.069304 1.187579 0.800808 11.00000 0.06332 0.04190 =
0.06287 0.00947 0.03958 -0.00520
F1C 5 1.055123 1.124719 0.770442 11.00000 0.12761 0.09362 =
0.06511 0.00028 0.06504 -0.03695
F2C 5 1.116726 1.188201 0.813168 11.00000 0.05637 0.11094 =
0.10555 0.00939 0.05832 -0.01252
F3C 5 1.055956 1.280436 0.786240 11.00000 0.17819 0.07419 =
0.15282 0.07191 0.13854 0.05011
F4C 5 1.011753 1.385920 0.893853 11.00000 0.10122 0.02621 =
0.09385 0.00426 0.05544 0.00676
F5C 5 1.050408 1.294788 0.945391 11.00000 0.07695 0.08282 =
0.06012 -0.02744 -0.00819 0.03159
F6C 5 0.975185 1.277285 0.915544 11.00000 0.06798 0.04627 =
0.06579 0.00260 0.03805 0.01441
C21C 1 1.056139 0.833933 0.867464 11.00000 0.02199 0.02774 =
0.02677 0.00860 0.01198 0.00090
C22C 1 1.105001 0.856901 0.881196 11.00000 0.02474 0.02865 =
0.03598 0.00488 0.01238 -0.00177
AFIX 43
H22C 2 1.115561 0.920217 0.894244 11.00000 -1.20000
AFIX 0
C23C 1 1.138757 0.791001 0.876559 11.00000 0.02212 0.04078 =
0.04466 0.01107 0.01667 0.00009
C24C 1 1.124245 0.697322 0.857695 11.00000 0.03513 0.04066 =
0.05013 0.01241 0.02749 0.00837
AFIX 43
H24C 2 1.147170 0.651444 0.854609 11.00000 -1.20000
AFIX 0
C25C 1 1.076701 0.672365 0.843721 11.00000 0.03486 0.03146 =
0.04154 0.00557 0.02263 0.00074
C26C 1 1.043175 0.738957 0.848674 11.00000 0.02210 0.02758 =
0.03986 0.00888 0.01791 0.00188
AFIX 43
H26C 2 1.010352 0.719448 0.838996 11.00000 -1.20000
AFIX 0
C27C 1 1.191004 0.818228 0.892408 11.00000 0.03449 0.06121 =
0.07953 0.01144 0.02328 -0.00565
C28C 1 1.060333 0.573967 0.822688 11.00000 0.05085 0.03292 =
0.07462 -0.00788 0.03619 0.00845
F7C 5 1.198081 0.917435 0.893115 11.00000 0.03931 0.06628 =
0.16302 -0.02817 0.04447 -0.01963
F8C 5 1.214043 0.781765 0.927302 11.00000 0.03486 0.21272 =
0.08655 0.05667 -0.00878 -0.02368
F9C 5 1.213769 0.781345 0.869761 11.00000 0.03951 0.08302 =
0.14153 -0.01428 0.05480 -0.00176
F10C 5 1.086646 0.543235 0.802904 11.00000 0.08153 0.07072 =
0.13321 -0.04835 0.06955 -0.01322
F11C 5 1.058157 0.500130 0.845799 11.00000 0.22417 0.03667 =
0.13263 -0.00994 0.11020 -0.03920
F12C 5 1.016059 0.580121 0.795253 11.00000 0.07246 0.07239 =
0.15425 -0.06160 0.01222 0.00062
C31C 1 0.962860 0.895033 0.845493 11.00000 0.02076 0.02145 =
0.02751 -0.00022 0.01106 -0.00317
C32C 1 0.952704 0.881331 0.804794 11.00000 0.02792 0.02907 =
0.03108 0.00137 0.01543 -0.00026
AFIX 43
H32C 2 0.978634 0.872696 0.795988 11.00000 -1.20000
AFIX 0
C33C 1 0.906636 0.880005 0.777362 11.00000 0.03617 0.02941 =
0.02555 -0.00075 0.01380 -0.00294
C34C 1 0.867097 0.893453 0.788703 11.00000 0.02298 0.03031 =
0.03674 -0.00366 0.00613 -0.00137
AFIX 43
H34C 2 0.835252 0.893355 0.769749 11.00000 -1.20000
AFIX 0
C35C 1 0.876242 0.906922 0.828692 11.00000 0.02573 0.03128 =
0.03982 -0.00693 0.01577 0.00334
C36C 1 0.923164 0.907532 0.856274 11.00000 0.02860 0.02430 =
0.03143 -0.00241 0.01280 -0.00514
AFIX 43
H36C 2 0.928220 0.916819 0.883419 11.00000 -1.20000
AFIX 0
C37C 1 0.896654 0.858566 0.734441 11.00000 0.04005 0.08212 =
0.03082 -0.00555 0.01273 -0.01058
C38C 1 0.834592 0.921760 0.840928 11.00000 0.02929 0.06833 =
0.05964 -0.02941 0.02290 -0.01497
PART 1
F13B 5 0.935385 0.845668 0.726406 21.00000 0.05089 0.08538 =
0.03637 -0.01552 0.02449 -0.00867
F14B 5 0.873545 0.941108 0.713337 21.00000 0.06427 0.11277 =
0.03165 0.01433 -0.00182 0.00953
F15B 5 0.866870 0.781744 0.719388 21.00000 0.06620 0.12428 =
0.03376 -0.03199 0.01246 -0.04934
PART 2
F13C 5 0.934262 0.874985 0.724639 -21.00000 0.05611 0.07692 =
0.03275 0.00070 0.02671 -0.00894
F14C 5 0.859010 0.903418 0.708206 -21.00000 0.04877 0.13844 =
0.03046 -0.01485 -0.00822 0.00320
F15C 5 0.888051 0.756783 0.729208 -21.00000 0.08972 0.09442 =
0.03082 -0.03005 0.01602 -0.04271
PART 1
F16A 5 0.794783 0.948252 0.812930 10.35000 0.03309 0.10659 =
0.07616 -0.03649 0.00944 -0.01504
F17A 5 0.826714 0.828809 0.853890 10.35000 0.03839 0.07680 =
0.09373 -0.03821 0.04196 -0.03797
F18A 5 0.844438 0.983688 0.871218 10.35000 0.02381 0.06514 =
0.05530 -0.02972 0.02674 -0.01204
PART 2
F16B 5 0.793438 0.880644 0.816273 10.15000 0.02258 0.06783 =
0.06809 -0.03117 0.02799 -0.01915
F17B 5 0.842460 0.877256 0.876569 10.15000 0.03327 0.08409 =
0.06400 -0.02832 0.02576 -0.02193
F18B 5 0.824190 1.019489 0.845508 10.15000 0.03434 0.07193 =
0.07180 -0.03755 0.01942 -0.01574
PART 3
F16C 5 0.806062 1.002652 0.819159 10.50000 0.01666 0.06651 =
0.07610 -0.02283 0.01869 -0.00737
F17C 5 0.804203 0.845803 0.833286 10.50000 0.01933 0.07441 =
0.06257 -0.03581 0.02736 -0.02751
F18C 5 0.845310 0.951380 0.878130 10.50000 0.03045 0.07513 =
0.05553 -0.04244 0.02812 -0.01870
PART 0
C41C 1 1.024277 0.881087 0.922192 11.00000 0.02514 0.02575 =
0.02634 0.00259 0.01003 -0.00022
C42C 1 1.004626 0.788256 0.928628 11.00000 0.03881 0.02685 =
0.02328 -0.00184 0.01040 -0.00690
AFIX 43
H42C 2 0.986474 0.747673 0.906539 11.00000 -1.20000
AFIX 0
C43C 1 1.011145 0.754181 0.966760 11.00000 0.05563 0.02920 =
0.02820 -0.00142 0.01867 -0.01332
C44C 1 1.036704 0.813242 0.999635 11.00000 0.06386 0.03092 =
0.02394 0.00071 0.01189 -0.00960
AFIX 43
H44C 2 1.040958 0.791174 1.025591 11.00000 -1.20000
AFIX 0
C45C 1 1.055356 0.903249 0.993502 11.00000 0.04848 0.02762 =
0.02443 -0.00075 0.00328 -0.00055
C46C 1 1.050570 0.935890 0.955580 11.00000 0.02878 0.02433 =
0.03174 0.00497 0.00505 -0.00557
AFIX 43
H46C 2 1.065815 0.997372 0.952741 11.00000 -1.20000
AFIX 0
C47C 1 0.989378 0.655045 0.971537 11.00000 0.07342 0.04000 =
0.03495 0.00434 0.01944 -0.01963
C48C 1 1.082738 0.967506 1.028899 11.00000 0.05880 0.03626 =
0.03321 0.00256 0.00619 -0.00661
F19C 5 1.078497 1.066320 1.021518 11.00000 0.20857 0.03043 =
0.06108 -0.00636 -0.00838 -0.02527
F20C 5 1.128941 0.946653 1.042433 11.00000 0.05841 0.13201 =
0.06971 -0.04445 0.01391 -0.02676
F21C 5 1.069542 0.953216 1.059042 11.00000 0.09823 0.08201 =
0.04039 -0.02272 0.02382 -0.02480
F22C 5 1.011043 0.614574 1.007605 11.00000 0.14992 0.03909 =
0.04034 0.00748 0.02282 -0.03454
F23C 5 0.942508 0.664217 0.966306 11.00000 0.09532 0.07448 =
0.14860 0.01099 0.06130 -0.04346
F24C 5 0.990795 0.584280 0.945635 11.00000 0.14378 0.03504 =
0.05259 -0.00991 0.04817 -0.03592
MOLE 3
C1M 1 0.132405 0.669260 0.967952 10.50000 0.08106
AFIX 23
H1M1 2 0.103716 0.713757 0.958401 10.50000 -1.20000
H1M2 2 0.152133 0.684528 0.951974 10.50000 -1.20000
PART 1
AFIX 0
CL1M 7 0.165027 0.698079 1.016635 10.25000 0.09609
CL2M 7 0.114336 0.544195 0.960584 10.25000 0.16142
PART 2
CL1N 7 0.182047 0.671444 1.010693 10.12500 0.08232
CL2N 7 0.102794 0.558572 0.948394 10.12500 0.06627
PART 3
CL1O 7 0.168845 0.737031 1.008209 10.12500 0.10803
CL2O 7 0.106989 0.553953 0.972090 10.12500 0.07361
PART 0
MOLE 5
C1P 1 0.803422 0.938301 0.045155 10.25000 0.20197
AFIX 23
H1P1 2 0.784929 0.884598 0.026664 10.25000 -1.20000
H1P2 2 0.780579 0.973882 0.054673 10.25000 -1.20000
PART 1
AFIX 0
CL1P 7 0.840434 0.881771 0.081909 10.12500 0.06546
CL2P 7 0.819071 1.017670 0.019931 10.12500 0.11119
PART 2
CL1R 7 0.847592 0.864218 0.057684 10.12500 0.07100
CL2R 7 0.805076 1.036841 0.020915 10.12500 0.07135
PART 0
MOLE 6
C1Q 1 0.828323 0.733159 -0.036743 10.12500 0.04309
AFIX 23
H1Q1 2 0.845196 0.793187 -0.041949 10.12500 -1.20000
H1Q2 2 0.853756 0.680977 -0.026226 10.12500 -1.20000
AFIX 0
CL1Q 7 0.802215 0.692352 -0.079874 10.12500 0.07910
CL2Q 7 0.822130 0.768005 0.002364 10.12500 0.10351
HKLF 4
REM Carol9_C2byc in C2/c
REM R1 = 0.0883 for 8562 Fo > 4sig(Fo) and 0.1136 for all 11579 data
REM 922 parameters refined using 336 restraints
END
WGHT 0.1083 148.4169
REM Highest difference peak 1.543, deepest hole -1.492, 1-sigma level 0.135
Q1 1 0.8751 0.7173 0.8455 11.00000 0.05 1.54
Q2 1 0.8173 0.7166 -0.0010 11.00000 0.05 1.08
Q3 1 0.8077 0.6763 -0.0545 11.00000 0.05 1.07
Q4 1 0.8396 0.8129 0.0227 11.00000 0.05 1.01
Q5 1 0.1228 0.5987 0.9500 11.00000 0.05 0.92
Q6 1 0.8304 0.7877 -0.0145 11.00000 0.05 0.88
Q7 1 0.8394 0.3478 0.8069 11.00000 0.05 0.85
Q8 1 0.1327 0.5340 0.9877 11.00000 0.05 0.85
Q9 1 0.8201 0.7381 -0.0753 11.00000 0.05 0.84
Q10 1 1.1149 1.0363 1.0158 11.00000 0.05 0.84
Q11 1 0.8333 0.8930 0.0536 11.00000 0.05 0.70
Q12 1 0.1830 0.6770 0.9932 11.00000 0.05 0.67
Q13 1 0.1744 0.6296 1.0135 11.00000 0.05 0.66
Q14 1 0.8426 0.8157 0.8754 11.00000 0.05 0.65
Q15 1 0.1470 0.7226 0.9892 11.00000 0.05 0.64
Q16 1 0.1774 0.5677 1.0126 11.00000 0.05 0.62
Q17 1 0.9291 0.7803 0.7307 11.00000 0.05 0.59
Q18 1 1.0997 0.5023 0.8392 11.00000 0.05 0.58
Q19 1 0.1721 0.7414 1.0277 11.00000 0.05 0.57
Q20 1 1.0232 0.5442 0.8244 11.00000 0.05 0.54
;
#===END
data_carol12_p21byn
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum
'C46 H46 B Cl N5 Rh'
_chemical_formula_weight 818.05
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Rh' 'Rh' -1.1178 0.9187
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'P2(1)/n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 12.0994(3)
_cell_length_b 24.4422(7)
_cell_length_c 13.3308(4)
_cell_angle_alpha 90.00
_cell_angle_beta 93.5650(10)
_cell_angle_gamma 90.00
_cell_volume 3934.77(19)
_cell_formula_units_Z 4
_cell_measurement_temperature 155(2)
_cell_measurement_reflns_used 9972
_cell_measurement_theta_min 2.263
_cell_measurement_theta_max 30.474
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'Red orange'
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.16
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.381
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1696
_exptl_absorpt_coefficient_mu 0.542
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.8600
_exptl_absorpt_correction_T_max 0.9207
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 155(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 25137
_diffrn_reflns_av_R_equivalents 0.1478
_diffrn_reflns_av_sigmaI/netI 0.7772
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -29
_diffrn_reflns_limit_k_max 29
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.93
_diffrn_reflns_theta_max 25.00
_reflns_number_total 6909
_reflns_number_gt 5495
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0208P)^2^+2.9167P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 6909
_refine_ls_number_parameters 492
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.1904
_refine_ls_R_factor_gt 0.0269
_refine_ls_wR_factor_ref 0.0683
_refine_ls_wR_factor_gt 0.0634
_refine_ls_goodness_of_fit_ref 1.061
_refine_ls_restrained_S_all 1.061
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.727053(14) 0.423038(6) 0.752579(10) 0.01759(6) Uani 1 1 d . . .
N1 N 0.72645(17) 0.35782(7) 0.55263(12) 0.0244(4) Uani 1 1 d . . .
N2 N 0.66829(16) 0.38860(7) 0.61531(11) 0.0220(4) Uani 1 1 d . . .
C3 C 0.5650(2) 0.39129(9) 0.57205(15) 0.0256(5) Uani 1 1 d . . .
H3 H 0.5054 0.4107 0.5986 0.031 Uiso 1 1 calc R . .
C4 C 0.5581(2) 0.36154(9) 0.48270(15) 0.0301(5) Uani 1 1 d . . .
H4 H 0.4946 0.3567 0.4381 0.036 Uiso 1 1 calc R . .
C5 C 0.6610(2) 0.34098(9) 0.47258(15) 0.0286(5) Uani 1 1 d . . .
H5 H 0.6831 0.3187 0.4189 0.034 Uiso 1 1 calc R . .
C1A C 0.84153(19) 0.34352(8) 0.57866(16) 0.0255(5) Uani 1 1 d . . .
H1A1 H 0.8735 0.3264 0.5198 0.031 Uiso 1 1 calc R . .
H2A1 H 0.8445 0.3163 0.6338 0.031 Uiso 1 1 calc R . .
N1' N 1.03577(15) 0.45297(7) 0.64493(11) 0.0214(4) Uani 1 1 d . . .
N2' N 0.95307(16) 0.46431(7) 0.70411(12) 0.0243(4) Uani 1 1 d . . .
N3' N 0.87723(16) 0.42704(7) 0.68329(12) 0.0221(4) Uani 1 1 d . . .
C4' C 0.91008(18) 0.39238(8) 0.61087(14) 0.0211(4) Uani 1 1 d . . .
C5' C 1.01172(19) 0.40853(8) 0.58600(14) 0.0225(5) Uani 1 1 d . . .
H5' H 1.0565 0.3924 0.5380 0.027 Uiso 1 1 calc R . .
C6' C 1.13627(19) 0.48376(8) 0.65473(15) 0.0227(5) Uani 1 1 d . . .
C7' C 1.1713(2) 0.50482(9) 0.74830(15) 0.0278(5) Uani 1 1 d . . .
H7' H 1.1277 0.4998 0.8044 0.033 Uiso 1 1 calc R . .
C8' C 1.2695(2) 0.53287(9) 0.75859(16) 0.0300(5) Uani 1 1 d . . .
H8' H 1.2932 0.5480 0.8220 0.036 Uiso 1 1 calc R . .
C9' C 1.3345(2) 0.53936(10) 0.67733(16) 0.0331(6) Uani 1 1 d . . .
H9' H 1.4032 0.5581 0.6852 0.040 Uiso 1 1 calc R . .
C10' C 1.2983(2) 0.51819(10) 0.58425(16) 0.0342(6) Uani 1 1 d . . .
H10' H 1.3428 0.5225 0.5286 0.041 Uiso 1 1 calc R . .
C11' C 1.1985(2) 0.49106(9) 0.57179(15) 0.0276(5) Uani 1 1 d . . .
H11' H 1.1729 0.4776 0.5077 0.033 Uiso 1 1 calc R . .
C1B C 0.6100(2) 0.42312(11) 0.86597(17) 0.0387(7) Uani 1 1 d . . .
C2B C 0.6352(2) 0.36795(10) 0.84306(15) 0.0334(6) Uani 1 1 d . . .
C3B C 0.7522(2) 0.35956(9) 0.86359(14) 0.0260(5) Uani 1 1 d . . .
C4B C 0.7958(2) 0.41023(9) 0.90414(15) 0.0309(6) Uani 1 1 d . . .
C5B C 0.7107(2) 0.44875(10) 0.90424(15) 0.0368(6) Uani 1 1 d . . .
C6B C 0.4986(3) 0.44955(19) 0.8570(2) 0.0787(13) Uani 1 1 d . . .
H6B1 H 0.4492 0.4284 0.8107 0.118 Uiso 1 1 calc R . .
H6B2 H 0.5056 0.4869 0.8313 0.118 Uiso 1 1 calc R . .
H6B3 H 0.4677 0.4508 0.9233 0.118 Uiso 1 1 calc R . .
C7B C 0.5553(3) 0.32654(14) 0.8028(2) 0.0690(11) Uani 1 1 d . . .
H7B1 H 0.5280 0.3052 0.8585 0.103 Uiso 1 1 calc R . .
H7B2 H 0.5919 0.3021 0.7570 0.103 Uiso 1 1 calc R . .
H7B3 H 0.4929 0.3449 0.7664 0.103 Uiso 1 1 calc R . .
C8B C 0.8121(3) 0.30673(11) 0.8555(2) 0.0510(8) Uani 1 1 d . . .
H8B1 H 0.8892 0.3139 0.8410 0.077 Uiso 1 1 calc R . .
H8B2 H 0.7763 0.2848 0.8012 0.077 Uiso 1 1 calc R . .
H8B3 H 0.8102 0.2867 0.9191 0.077 Uiso 1 1 calc R . .
C9B C 0.9146(3) 0.41889(15) 0.9395(2) 0.0602(10) Uani 1 1 d . . .
H9B1 H 0.9337 0.4576 0.9326 0.090 Uiso 1 1 calc R . .
H9B2 H 0.9623 0.3967 0.8989 0.090 Uiso 1 1 calc R . .
H9B3 H 0.9255 0.4081 1.0102 0.090 Uiso 1 1 calc R . .
C10B C 0.7224(4) 0.50697(12) 0.94121(19) 0.0719(12) Uani 1 1 d . . .
H10B H 0.7977 0.5200 0.9318 0.108 Uiso 1 1 calc R . .
H10C H 0.7082 0.5084 1.0127 0.108 Uiso 1 1 calc R . .
H10D H 0.6690 0.5303 0.9031 0.108 Uiso 1 1 calc R . .
Cl1 Cl 0.67785(5) 0.51049(2) 0.68373(4) 0.03074(14) Uani 1 1 d . . .
B1 B 0.2334(2) 0.24984(9) 0.67545(16) 0.0215(5) Uani 1 1 d . . .
C11C C 0.12633(18) 0.20934(8) 0.68428(13) 0.0198(4) Uani 1 1 d . . .
C12C C 0.03994(19) 0.22039(8) 0.74636(14) 0.0247(5) Uani 1 1 d . . .
H12C H 0.0446 0.2523 0.7871 0.030 Uiso 1 1 calc R . .
C13C C -0.0522(2) 0.18687(9) 0.75116(15) 0.0292(5) Uani 1 1 d . . .
H13C H -0.1091 0.1964 0.7940 0.035 Uiso 1 1 calc R . .
C14C C -0.0620(2) 0.13970(9) 0.69393(16) 0.0293(5) Uani 1 1 d . . .
H14C H -0.1238 0.1161 0.6983 0.035 Uiso 1 1 calc R . .
C15C C 0.0209(2) 0.12782(9) 0.62999(16) 0.0283(5) Uani 1 1 d . . .
H15C H 0.0152 0.0961 0.5888 0.034 Uiso 1 1 calc R . .
C16C C 0.11193(19) 0.16183(8) 0.62566(14) 0.0242(5) Uani 1 1 d . . .
H16C H 0.1672 0.1526 0.5810 0.029 Uiso 1 1 calc R . .
C21C C 0.21086(19) 0.29065(8) 0.57776(14) 0.0210(5) Uani 1 1 d . . .
C22C C 0.1293(2) 0.28028(8) 0.50007(14) 0.0228(5) Uani 1 1 d . . .
H22C H 0.0804 0.2503 0.5069 0.027 Uiso 1 1 calc R . .
C23C C 0.1174(2) 0.31229(9) 0.41362(15) 0.0274(5) Uani 1 1 d . . .
H23C H 0.0617 0.3035 0.3628 0.033 Uiso 1 1 calc R . .
C24C C 0.1861(2) 0.35679(9) 0.40122(15) 0.0290(5) Uani 1 1 d . . .
H24C H 0.1787 0.3784 0.3419 0.035 Uiso 1 1 calc R . .
C25C C 0.2661(2) 0.36936(9) 0.47724(16) 0.0279(5) Uani 1 1 d . . .
H25C H 0.3138 0.3999 0.4706 0.033 Uiso 1 1 calc R . .
C26C C 0.27598(19) 0.33677(9) 0.56345(15) 0.0267(5) Uani 1 1 d . . .
H26C H 0.3300 0.3465 0.6151 0.032 Uiso 1 1 calc R . .
C31C C 0.34727(18) 0.21378(8) 0.66153(14) 0.0217(4) Uani 1 1 d . . .
C32C C 0.4348(2) 0.23151(9) 0.60615(15) 0.0278(5) Uani 1 1 d . . .
H32C H 0.4269 0.2651 0.5706 0.033 Uiso 1 1 calc R . .
C33C C 0.5328(2) 0.20253(10) 0.60044(17) 0.0333(5) Uani 1 1 d . . .
H33C H 0.5899 0.2166 0.5620 0.040 Uiso 1 1 calc R . .
C34C C 0.5475(2) 0.15331(10) 0.65038(16) 0.0329(6) Uani 1 1 d . . .
H34C H 0.6145 0.1333 0.6468 0.039 Uiso 1 1 calc R . .
C35C C 0.4631(2) 0.13360(9) 0.70561(16) 0.0305(5) Uani 1 1 d . . .
H35C H 0.4719 0.0998 0.7404 0.037 Uiso 1 1 calc R . .
C36C C 0.36545(19) 0.16320(9) 0.71026(15) 0.0252(5) Uani 1 1 d . . .
H36C H 0.3083 0.1486 0.7481 0.030 Uiso 1 1 calc R . .
C41C C 0.25025(18) 0.28689(8) 0.77960(14) 0.0197(4) Uani 1 1 d . . .
C42C C 0.31444(19) 0.26848(8) 0.86442(14) 0.0222(5) Uani 1 1 d . . .
H42C H 0.3528 0.2347 0.8605 0.027 Uiso 1 1 calc R . .
C43C C 0.3240(2) 0.29800(9) 0.95416(15) 0.0266(5) Uani 1 1 d . . .
H43C H 0.3674 0.2839 1.0102 0.032 Uiso 1 1 calc R . .
C44C C 0.2706(2) 0.34739(9) 0.96174(15) 0.0275(5) Uani 1 1 d . . .
H44C H 0.2775 0.3678 1.0225 0.033 Uiso 1 1 calc R . .
C45C C 0.2069(2) 0.36702(9) 0.87982(17) 0.0336(6) Uani 1 1 d . . .
H45C H 0.1696 0.4011 0.8839 0.040 Uiso 1 1 calc R . .
C46C C 0.1977(2) 0.33658(9) 0.79089(16) 0.0293(5) Uani 1 1 d . . .
H46C H 0.1532 0.3507 0.7356 0.035 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.01830(11) 0.01784(9) 0.01703(9) 0.00039(5) 0.00434(6) 0.00013(6)
N1 0.0233(12) 0.0254(9) 0.0249(9) -0.0064(7) 0.0040(7) -0.0040(8)
N2 0.0220(12) 0.0226(8) 0.0222(8) -0.0023(6) 0.0093(7) 0.0008(8)
C3 0.0164(13) 0.0319(11) 0.0289(11) -0.0017(8) 0.0043(9) -0.0021(10)
C4 0.0251(14) 0.0369(12) 0.0280(11) -0.0042(9) -0.0014(9) -0.0081(11)
C5 0.0287(16) 0.0308(11) 0.0266(11) -0.0091(8) 0.0039(9) -0.0095(10)
C1A 0.0224(14) 0.0219(10) 0.0325(11) -0.0064(8) 0.0043(9) -0.0015(9)
N1' 0.0193(11) 0.0221(8) 0.0235(8) -0.0024(6) 0.0060(7) -0.0017(8)
N2' 0.0214(11) 0.0249(9) 0.0273(9) -0.0045(7) 0.0069(7) -0.0046(8)
N3' 0.0201(11) 0.0221(8) 0.0245(9) -0.0037(6) 0.0050(7) -0.0026(8)
C4' 0.0207(13) 0.0202(10) 0.0226(9) -0.0034(7) 0.0020(8) 0.0012(9)
C5' 0.0220(13) 0.0219(10) 0.0238(10) -0.0039(8) 0.0037(8) 0.0000(9)
C6' 0.0222(14) 0.0179(9) 0.0281(10) 0.0003(8) 0.0023(9) -0.0013(9)
C7' 0.0322(15) 0.0263(11) 0.0250(10) -0.0004(8) 0.0040(9) -0.0013(10)
C8' 0.0305(15) 0.0296(11) 0.0295(11) -0.0006(8) -0.0026(10) -0.0050(10)
C9' 0.0274(16) 0.0324(12) 0.0393(12) 0.0067(9) -0.0008(10) -0.0118(11)
C10' 0.0331(17) 0.0371(13) 0.0335(12) 0.0038(9) 0.0102(10) -0.0098(12)
C11' 0.0300(15) 0.0265(11) 0.0264(10) -0.0020(8) 0.0038(9) -0.0045(10)
C1B 0.0357(17) 0.0551(16) 0.0273(12) 0.0209(10) 0.0184(10) 0.0219(13)
C2B 0.0289(15) 0.0452(14) 0.0263(11) 0.0172(9) 0.0030(9) -0.0088(11)
C3B 0.0295(14) 0.0261(10) 0.0229(10) 0.0087(8) 0.0066(9) 0.0035(10)
C4B 0.0371(16) 0.0371(12) 0.0181(10) 0.0064(8) -0.0013(9) -0.0033(11)
C5B 0.062(2) 0.0351(12) 0.0142(10) 0.0011(8) 0.0066(10) 0.0106(13)
C6B 0.052(2) 0.128(3) 0.0592(19) 0.050(2) 0.0350(16) 0.050(2)
C7B 0.066(2) 0.076(2) 0.0625(19) 0.0399(16) -0.0189(17) -0.0461(19)
C8B 0.071(2) 0.0368(14) 0.0469(15) 0.0147(11) 0.0145(14) 0.0249(15)
C9B 0.048(2) 0.085(2) 0.0450(16) 0.0235(15) -0.0206(14) -0.0213(17)
C10B 0.146(4) 0.0411(16) 0.0288(14) -0.0105(11) 0.0072(16) 0.0206(19)
Cl1 0.0452(4) 0.0204(2) 0.0274(3) 0.00436(18) 0.0086(2) 0.0047(2)
B1 0.0232(15) 0.0212(11) 0.0198(10) 0.0001(8) -0.0008(9) -0.0021(10)
C11C 0.0201(12) 0.0215(9) 0.0175(9) 0.0049(7) -0.0028(8) 0.0003(9)
C12C 0.0251(13) 0.0244(10) 0.0244(10) 0.0014(8) 0.0002(9) -0.0010(9)
C13C 0.0231(13) 0.0362(12) 0.0284(11) 0.0089(9) 0.0019(9) -0.0022(10)
C14C 0.0242(14) 0.0295(11) 0.0331(11) 0.0126(9) -0.0063(10) -0.0091(10)
C15C 0.0295(14) 0.0242(10) 0.0301(11) 0.0013(8) -0.0081(10) -0.0049(10)
C16C 0.0245(13) 0.0260(10) 0.0219(10) 0.0017(8) -0.0011(8) 0.0003(9)
C21C 0.0205(13) 0.0219(10) 0.0208(9) 0.0000(7) 0.0037(8) 0.0017(9)
C22C 0.0245(14) 0.0207(10) 0.0233(10) -0.0019(7) 0.0033(9) -0.0005(9)
C23C 0.0326(15) 0.0276(11) 0.0218(10) -0.0009(8) -0.0002(9) 0.0062(10)
C24C 0.0350(16) 0.0294(11) 0.0235(10) 0.0072(8) 0.0093(9) 0.0084(11)
C25C 0.0228(15) 0.0246(10) 0.0375(12) 0.0071(9) 0.0114(9) 0.0005(10)
C26C 0.0219(13) 0.0282(11) 0.0299(11) 0.0019(8) 0.0008(9) -0.0003(10)
C31C 0.0194(12) 0.0257(10) 0.0196(9) -0.0051(7) -0.0014(8) -0.0024(9)
C32C 0.0258(14) 0.0298(11) 0.0278(10) -0.0013(8) 0.0024(9) -0.0017(10)
C33C 0.0228(14) 0.0422(13) 0.0353(12) -0.0069(10) 0.0056(10) -0.0020(11)
C34C 0.0243(14) 0.0389(13) 0.0350(12) -0.0129(10) -0.0025(10) 0.0079(11)
C35C 0.0309(15) 0.0285(11) 0.0309(11) -0.0057(9) -0.0066(10) 0.0038(10)
C36C 0.0229(13) 0.0269(10) 0.0255(10) -0.0038(8) 0.0004(9) -0.0006(10)
C41C 0.0159(13) 0.0226(10) 0.0208(9) 0.0006(7) 0.0029(8) -0.0056(9)
C42C 0.0213(14) 0.0217(10) 0.0241(10) 0.0011(8) 0.0043(8) -0.0015(9)
C43C 0.0267(14) 0.0321(11) 0.0209(10) 0.0011(8) -0.0002(9) -0.0053(10)
C44C 0.0252(14) 0.0311(11) 0.0265(11) -0.0082(8) 0.0042(9) -0.0062(10)
C45C 0.0363(17) 0.0275(11) 0.0368(12) -0.0061(9) 0.0000(11) 0.0049(11)
C46C 0.0291(14) 0.0309(11) 0.0272(11) -0.0016(9) -0.0040(9) 0.0049(10)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N3' 2.0912(19) . ?
Rh1 N2 2.0977(16) . ?
Rh1 C1B 2.135(2) . ?
Rh1 C5B 2.138(2) . ?
Rh1 C3B 2.1527(19) . ?
Rh1 C4B 2.1594(19) . ?
Rh1 C2B 2.161(2) . ?
Rh1 Cl1 2.3869(5) . ?
N1 C5 1.353(3) . ?
N1 N2 1.354(3) . ?
N1 C1A 1.456(3) . ?
N2 C3 1.345(3) . ?
C3 C4 1.394(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.357(4) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A C4' 1.501(3) . ?
C1A H1A1 0.9900 . ?
C1A H2A1 0.9900 . ?
N1' N2' 1.341(3) . ?
N1' C5' 1.361(3) . ?
N1' C6' 1.429(3) . ?
N2' N3' 1.310(2) . ?
N3' C4' 1.362(3) . ?
C4' C5' 1.352(3) . ?
C5' H5' 0.9500 . ?
C6' C11' 1.388(3) . ?
C6' C7' 1.391(3) . ?
C7' C8' 1.371(3) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.387(4) . ?
C8' H8' 0.9500 . ?
C9' C10' 1.390(3) . ?
C9' H9' 0.9500 . ?
C10' C11' 1.378(3) . ?
C10' H10' 0.9500 . ?
C11' H11' 0.9500 . ?
C1B C2B 1.420(4) . ?
C1B C5B 1.435(4) . ?
C1B C6B 1.493(4) . ?
C2B C3B 1.440(3) . ?
C2B C7B 1.477(4) . ?
C3B C4B 1.438(3) . ?
C3B C8B 1.488(3) . ?
C4B C5B 1.395(4) . ?
C4B C9B 1.500(4) . ?
C5B C10B 1.510(4) . ?
C6B H6B1 0.9800 . ?
C6B H6B2 0.9800 . ?
C6B H6B3 0.9800 . ?
C7B H7B1 0.9800 . ?
C7B H7B2 0.9800 . ?
C7B H7B3 0.9800 . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
C10B H10D 0.9800 . ?
B1 C11C 1.640(3) . ?
B1 C21C 1.650(3) . ?
B1 C31C 1.656(3) . ?
B1 C41C 1.660(3) . ?
C11C C12C 1.399(3) . ?
C11C C16C 1.404(3) . ?
C12C C13C 1.389(3) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.384(3) . ?
C13C H13C 0.9500 . ?
C14C C15C 1.387(4) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.384(3) . ?
C15C H15C 0.9500 . ?
C16C H16C 0.9500 . ?
C21C C26C 1.395(3) . ?
C21C C22C 1.409(3) . ?
C22C C23C 1.393(3) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.385(3) . ?
C23C H23C 0.9500 . ?
C24C C25C 1.392(3) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.397(3) . ?
C25C H25C 0.9500 . ?
C26C H26C 0.9500 . ?
C31C C32C 1.397(3) . ?
C31C C36C 1.407(3) . ?
C32C C33C 1.387(3) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.381(3) . ?
C33C H33C 0.9500 . ?
C34C C35C 1.382(4) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.390(3) . ?
C35C H35C 0.9500 . ?
C36C H36C 0.9500 . ?
C41C C46C 1.383(3) . ?
C41C C42C 1.405(3) . ?
C42C C43C 1.396(3) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.375(3) . ?
C43C H43C 0.9500 . ?
C44C C45C 1.383(3) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.398(3) . ?
C45C H45C 0.9500 . ?
C46C H46C 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3' Rh1 N2 83.69(7) . . ?
N3' Rh1 C1B 161.03(9) . . ?
N2 Rh1 C1B 114.47(10) . . ?
N3' Rh1 C5B 122.54(9) . . ?
N2 Rh1 C5B 153.70(10) . . ?
C1B Rh1 C5B 39.25(11) . . ?
N3' Rh1 C3B 104.34(8) . . ?
N2 Rh1 C3B 109.65(7) . . ?
C1B Rh1 C3B 65.52(9) . . ?
C5B Rh1 C3B 65.12(8) . . ?
N3' Rh1 C4B 97.21(8) . . ?
N2 Rh1 C4B 147.98(8) . . ?
C1B Rh1 C4B 64.62(10) . . ?
C5B Rh1 C4B 37.89(10) . . ?
C3B Rh1 C4B 38.96(8) . . ?
N3' Rh1 C2B 140.07(8) . . ?
N2 Rh1 C2B 94.51(8) . . ?
C1B Rh1 C2B 38.60(10) . . ?
C5B Rh1 C2B 64.81(10) . . ?
C3B Rh1 C2B 39.01(9) . . ?
C4B Rh1 C2B 64.46(9) . . ?
N3' Rh1 Cl1 89.49(5) . . ?
N2 Rh1 Cl1 87.76(5) . . ?
C1B Rh1 Cl1 96.37(6) . . ?
C5B Rh1 Cl1 93.72(6) . . ?
C3B Rh1 Cl1 158.59(6) . . ?
C4B Rh1 Cl1 124.19(6) . . ?
C2B Rh1 Cl1 130.39(7) . . ?
C5 N1 N2 110.79(19) . . ?
C5 N1 C1A 128.23(18) . . ?
N2 N1 C1A 120.82(16) . . ?
C3 N2 N1 105.50(16) . . ?
C3 N2 Rh1 127.59(15) . . ?
N1 N2 Rh1 126.90(14) . . ?
N2 C3 C4 110.2(2) . . ?
N2 C3 H3 124.9 . . ?
C4 C3 H3 124.9 . . ?
C5 C4 C3 105.77(19) . . ?
C5 C4 H4 127.1 . . ?
C3 C4 H4 127.1 . . ?
N1 C5 C4 107.71(19) . . ?
N1 C5 H5 126.1 . . ?
C4 C5 H5 126.1 . . ?
N1 C1A C4' 112.34(17) . . ?
N1 C1A H1A1 109.1 . . ?
C4' C1A H1A1 109.1 . . ?
N1 C1A H2A1 109.1 . . ?
C4' C1A H2A1 109.1 . . ?
H1A1 C1A H2A1 107.9 . . ?
N2' N1' C5' 111.34(18) . . ?
N2' N1' C6' 119.94(16) . . ?
C5' N1' C6' 128.54(19) . . ?
N3' N2' N1' 105.66(16) . . ?
N2' N3' C4' 110.56(18) . . ?
N2' N3' Rh1 123.72(13) . . ?
C4' N3' Rh1 125.71(14) . . ?
C5' C4' N3' 107.57(17) . . ?
C5' C4' C1A 131.0(2) . . ?
N3' C4' C1A 121.1(2) . . ?
C4' C5' N1' 104.86(19) . . ?
C4' C5' H5' 127.6 . . ?
N1' C5' H5' 127.6 . . ?
C11' C6' C7' 121.1(2) . . ?
C11' C6' N1' 119.73(17) . . ?
C7' C6' N1' 119.14(19) . . ?
C8' C7' C6' 119.2(2) . . ?
C8' C7' H7' 120.4 . . ?
C6' C7' H7' 120.4 . . ?
C7' C8' C9' 120.6(2) . . ?
C7' C8' H8' 119.7 . . ?
C9' C8' H8' 119.7 . . ?
C8' C9' C10' 119.5(2) . . ?
C8' C9' H9' 120.3 . . ?
C10' C9' H9' 120.3 . . ?
C11' C10' C9' 120.8(2) . . ?
C11' C10' H10' 119.6 . . ?
C9' C10' H10' 119.6 . . ?
C10' C11' C6' 118.73(19) . . ?
C10' C11' H11' 120.6 . . ?
C6' C11' H11' 120.6 . . ?
C2B C1B C5B 107.6(2) . . ?
C2B C1B C6B 126.8(3) . . ?
C5B C1B C6B 125.6(3) . . ?
C2B C1B Rh1 71.70(14) . . ?
C5B C1B Rh1 70.50(14) . . ?
C6B C1B Rh1 125.41(16) . . ?
C1B C2B C3B 108.4(2) . . ?
C1B C2B C7B 125.8(3) . . ?
C3B C2B C7B 125.8(3) . . ?
C1B C2B Rh1 69.70(14) . . ?
C3B C2B Rh1 70.19(12) . . ?
C7B C2B Rh1 124.90(17) . . ?
C4B C3B C2B 106.4(2) . . ?
C4B C3B C8B 127.3(2) . . ?
C2B C3B C8B 126.0(2) . . ?
C4B C3B Rh1 70.77(11) . . ?
C2B C3B Rh1 70.80(12) . . ?
C8B C3B Rh1 128.66(16) . . ?
C5B C4B C3B 109.2(2) . . ?
C5B C4B C9B 126.7(3) . . ?
C3B C4B C9B 124.2(3) . . ?
C5B C4B Rh1 70.23(11) . . ?
C3B C4B Rh1 70.27(11) . . ?
C9B C4B Rh1 125.43(18) . . ?
C4B C5B C1B 108.4(2) . . ?
C4B C5B C10B 125.6(3) . . ?
C1B C5B C10B 126.0(3) . . ?
C4B C5B Rh1 71.88(12) . . ?
C1B C5B Rh1 70.24(12) . . ?
C10B C5B Rh1 124.99(17) . . ?
C1B C6B H6B1 109.5 . . ?
C1B C6B H6B2 109.5 . . ?
H6B1 C6B H6B2 109.5 . . ?
C1B C6B H6B3 109.5 . . ?
H6B1 C6B H6B3 109.5 . . ?
H6B2 C6B H6B3 109.5 . . ?
C2B C7B H7B1 109.5 . . ?
C2B C7B H7B2 109.5 . . ?
H7B1 C7B H7B2 109.5 . . ?
C2B C7B H7B3 109.5 . . ?
H7B1 C7B H7B3 109.5 . . ?
H7B2 C7B H7B3 109.5 . . ?
C3B C8B H8B1 109.5 . . ?
C3B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C3B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C4B C9B H9B1 109.5 . . ?
C4B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C4B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C5B C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C5B C10B H10D 109.5 . . ?
H10B C10B H10D 109.5 . . ?
H10C C10B H10D 109.5 . . ?
C11C B1 C21C 109.21(16) . . ?
C11C B1 C31C 110.68(16) . . ?
C21C B1 C31C 109.35(18) . . ?
C11C B1 C41C 109.01(17) . . ?
C21C B1 C41C 109.64(16) . . ?
C31C B1 C41C 108.93(16) . . ?
C12C C11C C16C 114.7(2) . . ?
C12C C11C B1 123.25(18) . . ?
C16C C11C B1 122.0(2) . . ?
C13C C12C C11C 123.0(2) . . ?
C13C C12C H12C 118.5 . . ?
C11C C12C H12C 118.5 . . ?
C14C C13C C12C 120.5(2) . . ?
C14C C13C H13C 119.8 . . ?
C12C C13C H13C 119.8 . . ?
C13C C14C C15C 118.3(2) . . ?
C13C C14C H14C 120.9 . . ?
C15C C14C H14C 120.9 . . ?
C16C C15C C14C 120.5(2) . . ?
C16C C15C H15C 119.7 . . ?
C14C C15C H15C 119.7 . . ?
C15C C16C C11C 123.0(2) . . ?
C15C C16C H16C 118.5 . . ?
C11C C16C H16C 118.5 . . ?
C26C C21C C22C 114.89(18) . . ?
C26C C21C B1 121.97(17) . . ?
C22C C21C B1 123.05(19) . . ?
C23C C22C C21C 122.6(2) . . ?
C23C C22C H22C 118.7 . . ?
C21C C22C H22C 118.7 . . ?
C24C C23C C22C 120.52(19) . . ?
C24C C23C H23C 119.7 . . ?
C22C C23C H23C 119.7 . . ?
C23C C24C C25C 118.82(19) . . ?
C23C C24C H24C 120.6 . . ?
C25C C24C H24C 120.6 . . ?
C24C C25C C26C 119.5(2) . . ?
C24C C25C H25C 120.2 . . ?
C26C C25C H25C 120.2 . . ?
C21C C26C C25C 123.58(19) . . ?
C21C C26C H26C 118.2 . . ?
C25C C26C H26C 118.2 . . ?
C32C C31C C36C 114.5(2) . . ?
C32C C31C B1 123.89(19) . . ?
C36C C31C B1 121.5(2) . . ?
C33C C32C C31C 123.3(2) . . ?
C33C C32C H32C 118.4 . . ?
C31C C32C H32C 118.4 . . ?
C34C C33C C32C 120.3(2) . . ?
C34C C33C H33C 119.9 . . ?
C32C C33C H33C 119.9 . . ?
C33C C34C C35C 118.9(2) . . ?
C33C C34C H34C 120.6 . . ?
C35C C34C H34C 120.6 . . ?
C34C C35C C36C 120.0(2) . . ?
C34C C35C H35C 120.0 . . ?
C36C C35C H35C 120.0 . . ?
C35C C36C C31C 123.1(2) . . ?
C35C C36C H36C 118.5 . . ?
C31C C36C H36C 118.5 . . ?
C46C C41C C42C 115.35(18) . . ?
C46C C41C B1 122.46(17) . . ?
C42C C41C B1 122.10(19) . . ?
C43C C42C C41C 122.4(2) . . ?
C43C C42C H42C 118.8 . . ?
C41C C42C H42C 118.8 . . ?
C44C C43C C42C 120.17(19) . . ?
C44C C43C H43C 119.9 . . ?
C42C C43C H43C 119.9 . . ?
C43C C44C C45C 119.17(19) . . ?
C43C C44C H44C 120.4 . . ?
C45C C44C H44C 120.4 . . ?
C44C C45C C46C 119.8(2) . . ?
C44C C45C H45C 120.1 . . ?
C46C C45C H45C 120.1 . . ?
C41C C46C C45C 123.12(19) . . ?
C41C C46C H46C 118.4 . . ?
C45C C46C H46C 118.4 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 1.058
_refine_diff_density_min -0.758
_refine_diff_density_rms 0.082
_iucr_refine_instructions_details
;
TITL Carol12_P21byn in P2(1)/n
CELL 0.71073 12.0994 24.4422 13.3308 90.000 93.565 90.000
ZERR 4.00 0.0003 0.0007 0.0004 0.000 0.001 0.000
LATT 1
SYMM 0.5-X, 0.5+Y, 0.5-Z
SFAC C H B N Cl Rh
UNIT 184 184 4 20 4 4
OMIT 0 2 1
OMIT 1 0 1
OMIT -1 0 1
OMIT 0 2 0
OMIT 0 1 1
OMIT -1 1 1
OMIT 1 1 1
OMIT 1 2 0
OMIT 2 2 0
OMIT -1 2 1
OMIT 1 1 0
OMIT 1 2 1
OMIT -3 50
L.S. 15
ACTA
BOND $H
FMAP 2
PLAN 20
SIZE 0.287 0.171 0.155
TEMP -118.140
WGHT 0.020800 2.916700
FVAR 0.16408
MOLE 1
RH1 6 0.727053 0.423038 0.752579 11.00000 0.01830 0.01784 =
0.01703 0.00039 0.00434 0.00013
N1 4 0.726450 0.357818 0.552632 11.00000 0.02330 0.02544 =
0.02486 -0.00637 0.00397 -0.00402
N2 4 0.668288 0.388602 0.615314 11.00000 0.02204 0.02263 =
0.02217 -0.00226 0.00934 0.00076
C3 1 0.565025 0.391293 0.572047 11.00000 0.01645 0.03195 =
0.02886 -0.00174 0.00431 -0.00214
AFIX 43
H3 2 0.505363 0.410684 0.598571 11.00000 -1.20000
AFIX 0
C4 1 0.558131 0.361543 0.482701 11.00000 0.02509 0.03687 =
0.02799 -0.00420 -0.00138 -0.00814
AFIX 43
H4 2 0.494555 0.356667 0.438105 11.00000 -1.20000
AFIX 0
C5 1 0.661024 0.340976 0.472578 11.00000 0.02867 0.03083 =
0.02662 -0.00906 0.00394 -0.00948
AFIX 43
H5 2 0.683135 0.318745 0.418909 11.00000 -1.20000
AFIX 0
C1A 1 0.841526 0.343515 0.578655 11.00000 0.02240 0.02194 =
0.03245 -0.00643 0.00434 -0.00155
AFIX 23
H1A1 2 0.873503 0.326350 0.519751 11.00000 -1.20000
H2A1 2 0.844474 0.316326 0.633803 11.00000 -1.20000
AFIX 0
N1' 4 1.035771 0.452967 0.644934 11.00000 0.01929 0.02205 =
0.02353 -0.00244 0.00600 -0.00170
N2' 4 0.953068 0.464310 0.704111 11.00000 0.02139 0.02485 =
0.02733 -0.00445 0.00688 -0.00455
N3' 4 0.877230 0.427044 0.683286 11.00000 0.02009 0.02213 =
0.02447 -0.00370 0.00499 -0.00256
C4' 1 0.910075 0.392376 0.610870 11.00000 0.02071 0.02016 =
0.02259 -0.00339 0.00203 0.00119
C5' 1 1.011723 0.408530 0.586002 11.00000 0.02201 0.02192 =
0.02376 -0.00391 0.00367 0.00004
AFIX 43
H5' 2 1.056512 0.392405 0.537951 11.00000 -1.20000
AFIX 0
C6' 1 1.136273 0.483761 0.654735 11.00000 0.02224 0.01789 =
0.02813 0.00029 0.00233 -0.00133
C7' 1 1.171301 0.504824 0.748303 11.00000 0.03222 0.02634 =
0.02500 -0.00035 0.00400 -0.00132
AFIX 43
H7' 2 1.127688 0.499834 0.804441 11.00000 -1.20000
AFIX 0
C8' 1 1.269495 0.532872 0.758589 11.00000 0.03049 0.02956 =
0.02954 -0.00061 -0.00263 -0.00502
AFIX 43
H8' 2 1.293223 0.547994 0.821957 11.00000 -1.20000
AFIX 0
C9' 1 1.334472 0.539360 0.677326 11.00000 0.02735 0.03242 =
0.03928 0.00667 -0.00078 -0.01180
AFIX 43
H9' 2 1.403214 0.558133 0.685214 11.00000 -1.20000
AFIX 0
C10' 1 1.298271 0.518191 0.584249 11.00000 0.03308 0.03706 =
0.03349 0.00381 0.01025 -0.00983
AFIX 43
H10' 2 1.342817 0.522476 0.528554 11.00000 -1.20000
AFIX 0
C11' 1 1.198532 0.491059 0.571793 11.00000 0.03002 0.02652 =
0.02643 -0.00196 0.00382 -0.00449
AFIX 43
H11' 2 1.172887 0.477609 0.507651 11.00000 -1.20000
AFIX 0
C1B 1 0.610011 0.423119 0.865971 11.00000 0.03566 0.05513 =
0.02726 0.02094 0.01836 0.02186
C2B 1 0.635200 0.367952 0.843056 11.00000 0.02895 0.04517 =
0.02629 0.01723 0.00301 -0.00879
C3B 1 0.752235 0.359559 0.863593 11.00000 0.02947 0.02611 =
0.02292 0.00871 0.00663 0.00347
C4B 1 0.795785 0.410225 0.904139 11.00000 0.03711 0.03710 =
0.01813 0.00644 -0.00128 -0.00333
C5B 1 0.710706 0.448750 0.904240 11.00000 0.06165 0.03514 =
0.01419 0.00114 0.00661 0.01057
C6B 1 0.498556 0.449549 0.857028 11.00000 0.05249 0.12840 =
0.05921 0.05039 0.03502 0.05025
AFIX 137
H6B1 2 0.449232 0.428371 0.810653 11.00000 -1.50000
H6B2 2 0.505554 0.486867 0.831302 11.00000 -1.50000
H6B3 2 0.467741 0.450753 0.923261 11.00000 -1.50000
AFIX 0
C7B 1 0.555277 0.326544 0.802841 11.00000 0.06592 0.07557 =
0.06253 0.03985 -0.01886 -0.04608
AFIX 137
H7B1 2 0.528001 0.305228 0.858454 11.00000 -1.50000
H7B2 2 0.591876 0.302071 0.757035 11.00000 -1.50000
H7B3 2 0.492934 0.344863 0.766357 11.00000 -1.50000
AFIX 0
C8B 1 0.812078 0.306729 0.855524 11.00000 0.07069 0.03684 =
0.04689 0.01474 0.01450 0.02488
AFIX 137
H8B1 2 0.889161 0.313864 0.840973 11.00000 -1.50000
H8B2 2 0.776279 0.284805 0.801188 11.00000 -1.50000
H8B3 2 0.810216 0.286714 0.919096 11.00000 -1.50000
AFIX 0
C9B 1 0.914640 0.418888 0.939545 11.00000 0.04782 0.08478 =
0.04505 0.02350 -0.02062 -0.02129
AFIX 137
H9B1 2 0.933711 0.457615 0.932613 11.00000 -1.50000
H9B2 2 0.962308 0.396655 0.898900 11.00000 -1.50000
H9B3 2 0.925530 0.408054 1.010248 11.00000 -1.50000
AFIX 0
C10B 1 0.722405 0.506966 0.941208 11.00000 0.14593 0.04114 =
0.02884 -0.01055 0.00720 0.02062
AFIX 137
H10B 2 0.797671 0.519984 0.931817 11.00000 -1.50000
H10C 2 0.708175 0.508426 1.012730 11.00000 -1.50000
H10D 2 0.668964 0.530282 0.903075 11.00000 -1.50000
AFIX 0
CL1 5 0.677848 0.510487 0.683733 11.00000 0.04523 0.02038 =
0.02740 0.00436 0.00859 0.00472
MOLE 2
B1 3 0.233400 0.249836 0.675447 11.00000 0.02322 0.02123 =
0.01975 0.00009 -0.00076 -0.00207
C11C 1 0.126327 0.209336 0.684280 11.00000 0.02007 0.02146 =
0.01751 0.00488 -0.00280 0.00027
C12C 1 0.039942 0.220387 0.746359 11.00000 0.02506 0.02440 =
0.02444 0.00144 0.00019 -0.00099
AFIX 43
H12C 2 0.044577 0.252292 0.787104 11.00000 -1.20000
AFIX 0
C13C 1 -0.052244 0.186874 0.751161 11.00000 0.02311 0.03624 =
0.02840 0.00891 0.00191 -0.00221
AFIX 43
H13C 2 -0.109055 0.196406 0.794048 11.00000 -1.20000
AFIX 0
C14C 1 -0.061953 0.139701 0.693935 11.00000 0.02423 0.02947 =
0.03312 0.01255 -0.00631 -0.00914
AFIX 43
H14C 2 -0.123789 0.116062 0.698335 11.00000 -1.20000
AFIX 0
C15C 1 0.020919 0.127821 0.629990 11.00000 0.02955 0.02417 =
0.03008 0.00126 -0.00806 -0.00487
AFIX 43
H15C 2 0.015171 0.096093 0.588836 11.00000 -1.20000
AFIX 0
C16C 1 0.111932 0.161831 0.625665 11.00000 0.02446 0.02605 =
0.02193 0.00166 -0.00111 0.00029
AFIX 43
H16C 2 0.167222 0.152619 0.580987 11.00000 -1.20000
AFIX 0
C21C 1 0.210857 0.290654 0.577756 11.00000 0.02050 0.02187 =
0.02083 0.00004 0.00372 0.00167
C22C 1 0.129284 0.280278 0.500068 11.00000 0.02451 0.02070 =
0.02331 -0.00187 0.00328 -0.00048
AFIX 43
H22C 2 0.080450 0.250257 0.506897 11.00000 -1.20000
AFIX 0
C23C 1 0.117377 0.312291 0.413616 11.00000 0.03258 0.02757 =
0.02185 -0.00093 -0.00019 0.00621
AFIX 43
H23C 2 0.061699 0.303532 0.362760 11.00000 -1.20000
AFIX 0
C24C 1 0.186079 0.356794 0.401221 11.00000 0.03498 0.02943 =
0.02353 0.00719 0.00935 0.00844
AFIX 43
H24C 2 0.178688 0.378359 0.341895 11.00000 -1.20000
AFIX 0
C25C 1 0.266145 0.369357 0.477239 11.00000 0.02277 0.02460 =
0.03750 0.00713 0.01142 0.00045
AFIX 43
H25C 2 0.313762 0.399871 0.470554 11.00000 -1.20000
AFIX 0
C26C 1 0.275979 0.336768 0.563447 11.00000 0.02187 0.02817 =
0.02987 0.00189 0.00076 -0.00026
AFIX 43
H26C 2 0.329956 0.346546 0.615138 11.00000 -1.20000
AFIX 0
C31C 1 0.347271 0.213776 0.661530 11.00000 0.01940 0.02566 =
0.01963 -0.00515 -0.00142 -0.00244
C32C 1 0.434834 0.231514 0.606151 11.00000 0.02584 0.02984 =
0.02776 -0.00127 0.00238 -0.00167
AFIX 43
H32C 2 0.426870 0.265118 0.570627 11.00000 -1.20000
AFIX 0
C33C 1 0.532757 0.202534 0.600444 11.00000 0.02278 0.04218 =
0.03529 -0.00686 0.00557 -0.00201
AFIX 43
H33C 2 0.589920 0.216589 0.562039 11.00000 -1.20000
AFIX 0
C34C 1 0.547514 0.153313 0.650378 11.00000 0.02433 0.03886 =
0.03500 -0.01292 -0.00249 0.00795
AFIX 43
H34C 2 0.614524 0.133348 0.646825 11.00000 -1.20000
AFIX 0
C35C 1 0.463120 0.133599 0.705606 11.00000 0.03094 0.02851 =
0.03091 -0.00573 -0.00656 0.00377
AFIX 43
H35C 2 0.471853 0.099805 0.740400 11.00000 -1.20000
AFIX 0
C36C 1 0.365452 0.163203 0.710263 11.00000 0.02288 0.02691 =
0.02553 -0.00383 0.00044 -0.00063
AFIX 43
H36C 2 0.308335 0.148616 0.748100 11.00000 -1.20000
AFIX 0
C41C 1 0.250250 0.286889 0.779596 11.00000 0.01594 0.02260 =
0.02084 0.00057 0.00287 -0.00557
C42C 1 0.314439 0.268481 0.864421 11.00000 0.02127 0.02165 =
0.02411 0.00107 0.00425 -0.00147
AFIX 43
H42C 2 0.352765 0.234699 0.860532 11.00000 -1.20000
AFIX 0
C43C 1 0.323957 0.297999 0.954158 11.00000 0.02669 0.03208 =
0.02094 0.00110 -0.00020 -0.00530
AFIX 43
H43C 2 0.367378 0.283942 1.010154 11.00000 -1.20000
AFIX 0
C44C 1 0.270633 0.347389 0.961738 11.00000 0.02519 0.03111 =
0.02646 -0.00815 0.00415 -0.00618
AFIX 43
H44C 2 0.277482 0.367763 1.022495 11.00000 -1.20000
AFIX 0
C45C 1 0.206931 0.367017 0.879816 11.00000 0.03634 0.02750 =
0.03681 -0.00612 0.00002 0.00487
AFIX 43
H45C 2 0.169585 0.401056 0.883942 11.00000 -1.20000
AFIX 0
C46C 1 0.197693 0.336579 0.790894 11.00000 0.02913 0.03095 =
0.02721 -0.00163 -0.00398 0.00489
AFIX 43
H46C 2 0.153213 0.350687 0.735603 11.00000 -1.20000
HKLF 4
REM Carol12_P21byn in P2(1)/n
REM R1 = 0.0269 for 5495 Fo > 4sig(Fo) and 0.1904 for all 6909 data
REM 492 parameters refined using 0 restraints
END
WGHT 0.0208 2.9114
REM Highest difference peak 1.058, deepest hole -0.758, 1-sigma level 0.082
Q1 1 0.7380 0.4033 0.6375 11.00000 0.05 1.06
Q2 1 0.8020 0.4233 0.7905 11.00000 0.05 0.56
Q3 1 0.7731 0.3907 0.7431 11.00000 0.05 0.54
Q4 1 0.7611 0.4403 0.6942 11.00000 0.05 0.49
Q5 1 0.8413 0.4157 0.9019 11.00000 0.05 0.45
Q6 1 0.8209 0.4149 0.8626 11.00000 0.05 0.44
Q7 1 0.6434 0.4945 0.9340 11.00000 0.05 0.44
Q8 1 0.6586 0.4243 0.7320 11.00000 0.05 0.42
Q9 1 0.3016 0.2309 0.6721 11.00000 0.05 0.40
Q10 1 0.4615 0.4055 0.8250 11.00000 0.05 0.35
Q11 1 0.7831 0.4465 0.7681 11.00000 0.05 0.35
Q12 1 0.7657 0.5077 0.7131 11.00000 0.05 0.34
Q13 1 0.9030 0.4288 1.0105 11.00000 0.05 0.33
Q14 1 0.6990 0.3778 0.5868 11.00000 0.05 0.31
Q15 1 0.3394 0.1900 0.6797 11.00000 0.05 0.31
Q16 1 0.9395 0.4095 0.5667 11.00000 0.05 0.31
Q17 1 0.6815 0.4548 0.7729 11.00000 0.05 0.30
Q18 1 -0.0016 0.1229 0.6789 11.00000 0.05 0.29
Q19 1 0.6940 0.3634 0.8409 11.00000 0.05 0.28
Q20 1 0.6178 0.3002 0.7820 11.00000 0.05 0.28
;
#===END
data_chinmin2_c2byc
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
'(C17 H23 Cl N4 Rh), (C32 H12 B F24), 0.125(C Cl2)'
_chemical_formula_sum
'C49.12 H35 B Cl1.25 F24 N4 Rh'
_chemical_formula_weight 1295.34
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'B' 'B' 0.0013 0.0007
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'F' 'F' 0.0171 0.0103
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cl' 'Cl' 0.1484 0.1585
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Rh' 'Rh' -1.1178 0.9187
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting 'Monoclinic'
_symmetry_space_group_name_H-M 'C 2/c '
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 28.8126(10)
_cell_length_b 12.8881(4)
_cell_length_c 29.9049(11)
_cell_angle_alpha 90.00
_cell_angle_beta 104.623(2)
_cell_angle_gamma 90.00
_cell_volume 10745.2(6)
_cell_formula_units_Z 8
_cell_measurement_temperature 152(2)
_cell_measurement_reflns_used 7504
_cell_measurement_theta_min 2.353
_cell_measurement_theta_max 24.620
_exptl_crystal_description 'Blocks'
_exptl_crystal_colour 'yellow'
_exptl_crystal_size_max 0.18
_exptl_crystal_size_mid 0.15
_exptl_crystal_size_min 0.05
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.601
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5160
_exptl_absorpt_coefficient_mu 0.502
_exptl_absorpt_correction_type Multi-scan
_exptl_absorpt_correction_T_min 0.9133
_exptl_absorpt_correction_T_max 0.9739
_exptl_absorpt_process_details 'SADABS (Bruker, 2001)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 152(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker kappa APEXII CCD Diffractometer'
_diffrn_measurement_method '\f scans, and \w scans with \k offsets'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 39871
_diffrn_reflns_av_R_equivalents 0.0530
_diffrn_reflns_av_sigmaI/netI 0.0477
_diffrn_reflns_limit_h_min -34
_diffrn_reflns_limit_h_max 34
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -35
_diffrn_reflns_limit_l_max 35
_diffrn_reflns_theta_min 1.81
_diffrn_reflns_theta_max 25.00
_reflns_number_total 9456
_reflns_number_gt 7065
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2007)'
_computing_cell_refinement 'APEX2 (Bruker, 2007)'
_computing_data_reduction 'APEX2 (Bruker, 2007)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'SHELXTL-Plus (Sheldrick, 2008)'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 9456
_refine_ls_number_parameters 759
_refine_ls_number_restraints 124
_refine_ls_R_factor_all 0.1026
_refine_ls_R_factor_gt 0.0748
_refine_ls_wR_factor_ref 0.2218
_refine_ls_wR_factor_gt 0.2038
_refine_ls_goodness_of_fit_ref 1.461
_refine_ls_restrained_S_all 1.500
_refine_ls_shift/su_max 0.005
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.248339(16) 0.87384(4) 0.197951(15) 0.02261(18) Uani 1 1 d . . .
N1 N 0.2620(2) 0.9302(4) 0.30007(18) 0.0381(14) Uani 1 1 d . . .
N2 N 0.2301(2) 0.8968(4) 0.26125(19) 0.0357(13) Uani 1 1 d . . .
C3 C 0.1888(3) 0.8868(6) 0.2728(3) 0.0464(19) Uani 1 1 d . . .
H3 H 0.1599 0.8629 0.2526 0.056 Uiso 1 1 calc R . .
C4 C 0.1936(4) 0.9160(7) 0.3185(3) 0.061(3) Uani 1 1 d . . .
H4 H 0.1692 0.9171 0.3348 0.073 Uiso 1 1 calc R . .
C5 C 0.2399(4) 0.9425(6) 0.3346(3) 0.060(3) Uani 1 1 d . . .
H5 H 0.2546 0.9658 0.3650 0.072 Uiso 1 1 calc R . .
C1A C 0.3101(3) 0.9591(5) 0.2981(2) 0.0412(18) Uani 1 1 d . . .
H2A H 0.3083 1.0182 0.2766 0.049 Uiso 1 1 calc R . .
H1A H 0.3286 0.9816 0.3291 0.049 Uiso 1 1 calc R . .
N1' N 0.3343(2) 0.8738(4) 0.28277(19) 0.0375(14) Uani 1 1 d . . .
N2' N 0.31668(19) 0.8319(4) 0.24033(17) 0.0298(12) Uani 1 1 d . . .
C3' C 0.3482(2) 0.7627(6) 0.2352(3) 0.0392(17) Uani 1 1 d . . .
H3' H 0.3449 0.7203 0.2086 0.047 Uiso 1 1 calc R . .
C4' C 0.3869(3) 0.7591(6) 0.2734(3) 0.046(2) Uani 1 1 d . . .
H4' H 0.4143 0.7156 0.2780 0.055 Uiso 1 1 calc R . .
C5' C 0.3773(3) 0.8313(6) 0.3033(3) 0.047(2) Uani 1 1 d . . .
H5' H 0.3971 0.8485 0.3328 0.056 Uiso 1 1 calc R . .
C1B C 0.2298(2) 0.8744(5) 0.1232(2) 0.0303(14) Uani 1 1 d . . .
C2B C 0.2729(2) 0.9320(5) 0.1406(2) 0.0290(14) Uani 1 1 d . . .
C3B C 0.2628(2) 1.0167(5) 0.16790(19) 0.0262(14) Uani 1 1 d . . .
C4B C 0.2130(2) 1.0129(5) 0.1666(2) 0.0281(14) Uani 1 1 d . . .
C5B C 0.1925(2) 0.9234(5) 0.1401(2) 0.0311(15) Uani 1 1 d . . .
C6B C 0.2230(3) 0.7831(6) 0.0917(2) 0.0458(19) Uani 1 1 d . . .
H6A1 H 0.2106 0.8064 0.0597 0.069 Uiso 1 1 calc R . .
H6A2 H 0.2001 0.7349 0.0998 0.069 Uiso 1 1 calc R . .
H6A3 H 0.2538 0.7479 0.0949 0.069 Uiso 1 1 calc R . .
C7B C 0.3209(2) 0.9095(6) 0.1320(2) 0.0416(18) Uani 1 1 d . . .
H7A1 H 0.3215 0.8378 0.1213 0.062 Uiso 1 1 calc R . .
H7A2 H 0.3459 0.9188 0.1608 0.062 Uiso 1 1 calc R . .
H7A3 H 0.3267 0.9570 0.1084 0.062 Uiso 1 1 calc R . .
C8B C 0.2978(3) 1.1000(6) 0.1893(2) 0.0421(18) Uani 1 1 d . . .
H8A1 H 0.3016 1.1487 0.1653 0.063 Uiso 1 1 calc R . .
H8A2 H 0.3289 1.0684 0.2039 0.063 Uiso 1 1 calc R . .
H8A3 H 0.2858 1.1373 0.2127 0.063 Uiso 1 1 calc R . .
C9B C 0.1866(3) 1.0888(6) 0.1884(2) 0.0406(17) Uani 1 1 d . . .
H9A1 H 0.2080 1.1153 0.2169 0.061 Uiso 1 1 calc R . .
H9A2 H 0.1589 1.0546 0.1955 0.061 Uiso 1 1 calc R . .
H9A3 H 0.1755 1.1465 0.1670 0.061 Uiso 1 1 calc R . .
C10B C 0.1411(2) 0.8889(7) 0.1292(3) 0.055(2) Uani 1 1 d . . .
H10A H 0.1247 0.9110 0.0979 0.082 Uiso 1 1 calc R . .
H10B H 0.1253 0.9201 0.1514 0.082 Uiso 1 1 calc R . .
H10C H 0.1398 0.8131 0.1313 0.082 Uiso 1 1 calc R . .
Cl1 Cl 0.22567(7) 0.69656(13) 0.19988(6) 0.0435(5) Uani 1 1 d . . .
B1C B 0.4102(3) 0.2030(6) 0.0940(2) 0.0270(15) Uani 1 1 d . . .
C11C C 0.4246(2) 0.1305(5) 0.1404(2) 0.0255(13) Uani 1 1 d . . .
C12C C 0.4207(2) 0.1638(5) 0.1837(2) 0.0244(13) Uani 1 1 d . . .
H12C H 0.4119 0.2338 0.1872 0.029 Uiso 1 1 calc R . .
C13C C 0.4291(2) 0.0977(5) 0.2221(2) 0.0264(14) Uani 1 1 d . A .
C14C C 0.4417(2) -0.0043(5) 0.2184(2) 0.0312(15) Uani 1 1 d . . .
H14C H 0.4473 -0.0494 0.2443 0.037 Uiso 1 1 calc R . .
C15C C 0.4459(2) -0.0395(5) 0.1758(2) 0.0310(15) Uani 1 1 d . B .
C16C C 0.4376(2) 0.0253(5) 0.1380(2) 0.0296(14) Uani 1 1 d . . .
H16C H 0.4408 -0.0015 0.1093 0.036 Uiso 1 1 calc R . .
C17C C 0.42526(17) 0.1379(4) 0.2674(2) 0.0324(15) Uani 1 1 d D . .
C18C C 0.46002(18) -0.1493(5) 0.17010(19) 0.0429(18) Uani 1 1 d DU . .
F171 F 0.4090(4) 0.0645(6) 0.2918(3) 0.048(2) Uiso 0.50 1 d PD A 1
F172 F 0.4666(2) 0.1725(7) 0.2935(3) 0.0339(18) Uiso 0.50 1 d PD A 1
F173 F 0.3939(3) 0.2174(7) 0.2634(3) 0.0326(18) Uiso 0.50 1 d PD A 1
F174 F 0.4398(6) 0.0635(11) 0.3010(5) 0.049(4) Uiso 0.25 1 d PD A 2
F175 F 0.4560(5) 0.2192(12) 0.2813(6) 0.051(5) Uiso 0.25 1 d PD A 2
F176 F 0.3815(5) 0.1683(13) 0.2693(5) 0.043(4) Uiso 0.25 1 d PD A 2
F177 F 0.3892(5) 0.0910(12) 0.2840(5) 0.030(4) Uiso 0.25 1 d PD A 3
F178 F 0.4651(4) 0.1302(12) 0.3040(5) 0.034(4) Uiso 0.25 1 d PD A 3
F179 F 0.4125(6) 0.2428(9) 0.2674(5) 0.040(4) Uiso 0.25 1 d PD A 3
F181 F 0.4365(4) -0.1913(9) 0.1306(3) 0.062(3) Uiso 0.45 1 d PDU B 1
F182 F 0.5066(2) -0.1557(7) 0.1718(3) 0.027(2) Uiso 0.45 1 d PDU B 1
F183 F 0.4527(4) -0.2097(9) 0.2039(4) 0.063(3) Uiso 0.45 1 d PDU B 1
F184 F 0.4525(4) -0.1768(8) 0.1229(3) 0.027(2) Uiso 0.35 1 d PDU B 2
F185 F 0.5070(3) -0.1713(9) 0.1881(4) 0.036(3) Uiso 0.35 1 d PDU B 2
F186 F 0.4342(4) -0.2214(8) 0.1860(4) 0.031(2) Uiso 0.35 1 d PDU B 2
F187 F 0.4225(6) -0.2147(13) 0.1572(7) 0.035(4) Uiso 0.20 1 d PDU B 3
F188 F 0.4904(7) -0.176(2) 0.1445(7) 0.088(9) Uiso 0.20 1 d PDU B 3
F189 F 0.4829(7) -0.1871(15) 0.2136(5) 0.042(5) Uiso 0.20 1 d PDU B 3
C21C C 0.4462(3) 0.1837(5) 0.0601(2) 0.0358(16) Uani 1 1 d . . .
C22C C 0.4307(4) 0.2135(7) 0.0134(3) 0.059(2) Uani 1 1 d . C .
H22C H 0.3990 0.2390 0.0016 0.070 Uiso 1 1 calc R . .
C23C C 0.4616(5) 0.2057(10) -0.0154(3) 0.093(4) Uani 1 1 d D . .
C24C C 0.5081(5) 0.1659(11) 0.0011(4) 0.098(4) Uani 1 1 d . C .
H24C H 0.5286 0.1573 -0.0191 0.118 Uiso 1 1 calc R . .
C25C C 0.5229(3) 0.1405(9) 0.0454(4) 0.082(4) Uani 1 1 d D . .
C26C C 0.4928(3) 0.1480(6) 0.0755(3) 0.048(2) Uani 1 1 d . C .
H26C H 0.5046 0.1283 0.1069 0.058 Uiso 1 1 calc R . .
C27C C 0.4346(5) 0.2499(11) -0.0649(7) 0.101(7) Uiso 0.60 1 d PDU C 1
F271 F 0.3927(4) 0.2021(9) -0.0852(4) 0.091(3) Uiso 0.60 1 d PDU C 1
F272 F 0.4219(5) 0.3505(10) -0.0683(5) 0.142(5) Uiso 0.60 1 d PD C 1
F273 F 0.4598(5) 0.2405(10) -0.0965(5) 0.126(4) Uiso 0.60 1 d PD C 1
C27" C 0.4519(5) 0.2191(11) -0.0696(7) 0.159(18) Uiso 0.40 1 d PD C 2
F274 F 0.4073(6) 0.2485(13) -0.0798(6) 0.095(5) Uiso 0.40 1 d PD C 2
F275 F 0.4806(5) 0.2942(12) -0.0740(6) 0.099(5) Uiso 0.40 1 d PD C 2
F276 F 0.4591(5) 0.1352(11) -0.0910(6) 0.088(4) Uiso 0.40 1 d PD C 2
C28C C 0.5733(4) 0.0863(7) 0.0689(3) 0.064(4) Uiso 0.65 1 d PDU C 2
F284 F 0.5719(7) 0.0046(13) 0.0990(5) 0.091(5) Uiso 0.35 1 d PD D 1
F285 F 0.5804(6) 0.0442(10) 0.0281(5) 0.045(4) Uiso 0.35 1 d PD E 1
F286 F 0.6117(7) 0.1496(16) 0.0887(6) 0.113(9) Uiso 0.35 1 d PD F 1
F281 F 0.5844(7) 0.0506(14) 0.1133(5) 0.072(5) Uiso 0.30 1 d PDU C 2
F282 F 0.5921(4) 0.0119(9) 0.0462(4) 0.022(3) Uiso 0.30 1 d PDU C 2
F283 F 0.6059(5) 0.1663(11) 0.0712(6) 0.048(4) Uiso 0.30 1 d PDU C 2
C28' C 0.5792(6) 0.1236(15) 0.0580(6) 0.111(14) Uiso 0.35 1 d PDU C 3
F287 F 0.586(2) 0.044(2) 0.0366(10) 0.25(3) Uiso 0.35 1 d PDU C 3
F288 F 0.6013(5) 0.2003(12) 0.0480(5) 0.064(4) Uiso 0.35 1 d PDU C 3
F289 F 0.5886(7) 0.1087(15) 0.1007(6) 0.080(5) Uiso 0.35 1 d PDU C 3
C31C C 0.3557(2) 0.1635(5) 0.06833(19) 0.0273(14) Uani 1 1 d . . .
C32C C 0.3492(2) 0.0767(5) 0.0393(2) 0.0308(14) Uani 1 1 d . . .
H32C H 0.3765 0.0477 0.0317 0.037 Uiso 1 1 calc R . .
C33C C 0.3050(2) 0.0308(5) 0.0212(2) 0.0340(15) Uani 1 1 d . G .
C34C C 0.2638(3) 0.0747(6) 0.0301(2) 0.0374(17) Uani 1 1 d . . .
H34C H 0.2331 0.0455 0.0172 0.045 Uiso 1 1 calc R . .
C35C C 0.2690(2) 0.1612(5) 0.0578(2) 0.0321(15) Uani 1 1 d . H .
C36C C 0.3139(2) 0.2042(5) 0.0771(2) 0.0297(14) Uani 1 1 d . . .
H36C H 0.3163 0.2627 0.0969 0.036 Uiso 1 1 calc R . .
C37C C 0.3021(2) -0.0681(6) -0.0072(2) 0.055(2) Uani 1 1 d DU . .
C38C C 0.2254(2) 0.2092(5) 0.06674(18) 0.0440(18) Uani 1 1 d DU . .
F371 F 0.2926(3) -0.0478(6) -0.0511(2) 0.063(2) Uiso 0.70 1 d PDU G 1
F372 F 0.2682(2) -0.1309(5) -0.0003(2) 0.0515(17) Uiso 0.70 1 d PDU G 1
F373 F 0.3420(2) -0.1233(6) 0.0034(3) 0.0542(19) Uiso 0.70 1 d PDU G 1
F374 F 0.3123(5) -0.0436(10) -0.0486(4) 0.031(3) Uiso 0.30 1 d PDU G 2
F375 F 0.3340(5) -0.1413(14) 0.0139(6) 0.071(6) Uiso 0.30 1 d PDU G 2
F376 F 0.2571(5) -0.1099(15) -0.0175(6) 0.079(6) Uiso 0.30 1 d PDU G 2
F381 F 0.2310(3) 0.2306(8) 0.1131(2) 0.0255(19) Uiso 0.40 1 d PDU H 1
F382 F 0.2093(5) 0.2965(9) 0.0456(4) 0.064(3) Uiso 0.40 1 d PDU H 1
F383 F 0.1865(4) 0.1445(9) 0.0588(5) 0.071(4) Uiso 0.40 1 d PDU H 1
F384 F 0.2147(5) 0.1866(10) 0.1056(4) 0.058(3) Uiso 0.40 1 d PDU H 2
F385 F 0.1857(4) 0.1962(10) 0.0317(4) 0.055(3) Uiso 0.40 1 d PDU H 2
F386 F 0.2299(4) 0.3176(7) 0.0674(4) 0.038(2) Uiso 0.40 1 d PDU H 2
F387 F 0.1997(6) 0.1377(13) 0.0842(7) 0.035(4) Uiso 0.20 1 d PDU H 3
F388 F 0.1944(5) 0.2409(15) 0.0274(5) 0.022(4) Uiso 0.20 1 d PDU H 3
F389 F 0.2299(10) 0.2901(15) 0.0959(7) 0.084(8) Uiso 0.20 1 d PDU H 3
C41C C 0.4156(2) 0.3270(5) 0.1064(2) 0.0286(14) Uani 1 1 d . . .
C42C C 0.3848(3) 0.4032(5) 0.0838(3) 0.0432(18) Uani 1 1 d . I .
H42C H 0.3560 0.3833 0.0621 0.052 Uiso 1 1 calc R . .
C43C C 0.3947(3) 0.5092(6) 0.0919(3) 0.063(3) Uani 1 1 d . . .
C44C C 0.4360(3) 0.5405(6) 0.1231(3) 0.055(2) Uani 1 1 d . I .
H44C H 0.4426 0.6121 0.1290 0.066 Uiso 1 1 calc R . .
C45C C 0.4681(3) 0.4656(5) 0.1459(2) 0.0370(16) Uani 1 1 d . . .
C46C C 0.4579(2) 0.3621(5) 0.1375(2) 0.0294(14) Uani 1 1 d . I .
H46C H 0.4804 0.3122 0.1534 0.035 Uiso 1 1 calc R . .
C48C C 0.5136(3) 0.5000(4) 0.1774(2) 0.0487(19) Uani 1 1 d DU I .
C47C C 0.3511(6) 0.5856(13) 0.0725(4) 0.059(5) Uiso 0.50 1 d PDU I 1
F471 F 0.3350(4) 0.5722(9) 0.0290(4) 0.068(3) Uiso 0.50 1 d PDU I 1
F472 F 0.3646(4) 0.6797(8) 0.0780(3) 0.070(3) Uiso 0.50 1 d PDU I 1
F473 F 0.3141(5) 0.5763(11) 0.0883(4) 0.110(5) Uiso 0.50 1 d PDU I 1
C47' C 0.3673(6) 0.5916(14) 0.0596(5) 0.068(5) Uiso 0.50 1 d PDU I 2
F474 F 0.3458(4) 0.5578(10) 0.0176(4) 0.074(4) Uiso 0.50 1 d PDU I 2
F475 F 0.3337(7) 0.6195(15) 0.0806(7) 0.163(8) Uiso 0.50 1 d PDU I 2
F476 F 0.3902(5) 0.6782(11) 0.0539(5) 0.101(4) Uiso 0.50 1 d PDU I 2
F481 F 0.5431(3) 0.5444(7) 0.1524(3) 0.060(3) Uiso 0.50 1 d PDU I 1
F482 F 0.5092(4) 0.5740(7) 0.2078(3) 0.052(3) Uiso 0.50 1 d PDU I 1
F483 F 0.5414(3) 0.4248(7) 0.2011(3) 0.056(2) Uiso 0.50 1 d PDU I 1
F484 F 0.5519(4) 0.4928(9) 0.1619(4) 0.101(4) Uiso 0.50 1 d PDU I 2
F485 F 0.5127(4) 0.5958(7) 0.1935(3) 0.053(3) Uiso 0.50 1 d PDU I 2
F486 F 0.5231(4) 0.4406(7) 0.2162(3) 0.068(3) Uiso 0.50 1 d PDU I 2
C1D C -0.0071(14) 0.980(5) 0.023(2) 0.051(16) Uiso 0.13 1 d PD . .
Cl1D Cl 0.0458(13) 0.961(4) 0.0033(19) 0.13(2) Uiso 0.13 1 d PD . .
Cl2D Cl 0.0464(14) 0.933(5) 0.010(2) 0.14(2) Uiso 0.13 1 d PD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0230(3) 0.0197(3) 0.0257(3) 0.0006(2) 0.00705(18) 0.0001(2)
N1 0.067(4) 0.020(3) 0.030(3) 0.000(2) 0.018(3) 0.000(3)
N2 0.043(3) 0.032(3) 0.037(3) 0.000(2) 0.019(3) 0.002(3)
C3 0.056(5) 0.042(5) 0.051(4) 0.007(4) 0.031(4) 0.004(4)
C4 0.101(8) 0.039(5) 0.063(5) 0.012(4) 0.058(6) 0.007(5)
C5 0.115(8) 0.040(5) 0.036(4) 0.005(4) 0.041(5) 0.000(5)
C1A 0.063(5) 0.027(4) 0.028(3) -0.002(3) 0.000(3) -0.004(4)
N1' 0.040(3) 0.028(3) 0.036(3) 0.004(3) -0.006(2) -0.001(3)
N2' 0.034(3) 0.023(3) 0.032(3) 0.007(2) 0.006(2) 0.004(2)
C3' 0.036(4) 0.030(4) 0.054(4) 0.015(3) 0.016(3) 0.004(3)
C4' 0.032(4) 0.035(4) 0.069(5) 0.026(4) 0.008(4) 0.002(3)
C5' 0.039(4) 0.039(4) 0.053(4) 0.018(4) -0.007(3) -0.010(4)
C1B 0.030(3) 0.033(4) 0.026(3) -0.002(3) 0.003(2) 0.004(3)
C2B 0.026(3) 0.036(4) 0.026(3) 0.006(3) 0.007(2) 0.006(3)
C3B 0.031(3) 0.023(3) 0.021(3) 0.010(2) 0.001(2) -0.002(3)
C4B 0.028(3) 0.028(4) 0.026(3) 0.001(3) 0.002(2) 0.006(3)
C5B 0.027(3) 0.031(4) 0.032(3) -0.002(3) 0.001(3) 0.002(3)
C6B 0.054(5) 0.043(5) 0.036(4) -0.012(3) 0.004(3) 0.007(4)
C7B 0.028(4) 0.061(5) 0.040(4) 0.010(4) 0.016(3) 0.007(3)
C8B 0.051(4) 0.040(4) 0.033(4) 0.007(3) 0.006(3) -0.015(4)
C9B 0.047(4) 0.035(4) 0.041(4) -0.004(3) 0.013(3) 0.008(3)
C10B 0.021(4) 0.078(6) 0.061(5) -0.018(4) 0.001(3) -0.006(4)
Cl1 0.0588(11) 0.0245(9) 0.0472(10) 0.0000(7) 0.0134(8) -0.0132(8)
B1C 0.028(4) 0.024(4) 0.028(3) -0.007(3) 0.006(3) -0.002(3)
C11C 0.023(3) 0.018(3) 0.035(3) -0.003(3) 0.005(2) -0.002(3)
C12C 0.018(3) 0.020(3) 0.032(3) -0.004(3) 0.001(2) 0.002(2)
C13C 0.017(3) 0.026(4) 0.033(3) -0.003(3) 0.000(2) -0.006(3)
C14C 0.016(3) 0.031(4) 0.043(4) 0.002(3) 0.002(3) 0.002(3)
C15C 0.016(3) 0.021(3) 0.055(4) 0.002(3) 0.007(3) -0.004(3)
C16C 0.021(3) 0.022(3) 0.044(4) -0.003(3) 0.005(3) -0.002(3)
C17C 0.030(3) 0.032(4) 0.033(3) 0.003(3) 0.003(3) -0.004(3)
C18C 0.035(4) 0.026(4) 0.067(5) 0.002(3) 0.011(4) 0.004(3)
C21C 0.046(4) 0.031(4) 0.034(3) -0.011(3) 0.017(3) -0.016(3)
C22C 0.078(6) 0.058(6) 0.050(5) -0.015(4) 0.034(4) -0.029(5)
C23C 0.124(10) 0.127(11) 0.045(5) -0.024(6) 0.052(6) -0.057(9)
C24C 0.089(9) 0.138(11) 0.089(8) -0.052(8) 0.064(7) -0.051(8)
C25C 0.057(6) 0.109(9) 0.094(8) -0.066(7) 0.047(6) -0.040(6)
C26C 0.052(5) 0.041(5) 0.060(5) -0.028(4) 0.029(4) -0.013(4)
C31C 0.036(4) 0.024(3) 0.022(3) 0.003(2) 0.006(3) -0.005(3)
C32C 0.037(4) 0.029(4) 0.024(3) -0.002(3) 0.006(3) -0.005(3)
C33C 0.042(4) 0.031(4) 0.030(3) -0.002(3) 0.009(3) -0.006(3)
C34C 0.038(4) 0.042(4) 0.027(3) -0.001(3) -0.001(3) -0.011(3)
C35C 0.032(4) 0.030(4) 0.030(3) 0.001(3) -0.002(3) 0.003(3)
C36C 0.037(4) 0.027(4) 0.022(3) 0.000(3) 0.002(3) 0.002(3)
C37C 0.046(5) 0.082(7) 0.034(4) -0.018(4) 0.007(3) -0.032(5)
C38C 0.036(4) 0.046(5) 0.045(4) 0.002(3) 0.000(3) -0.007(3)
C41C 0.036(4) 0.022(3) 0.028(3) -0.001(3) 0.009(3) 0.002(3)
C42C 0.049(4) 0.025(4) 0.046(4) -0.006(3) -0.005(3) -0.005(3)
C43C 0.059(5) 0.029(4) 0.077(6) -0.002(4) -0.024(4) 0.004(4)
C44C 0.056(5) 0.019(4) 0.076(6) -0.007(4) -0.009(4) -0.004(4)
C45C 0.041(4) 0.026(4) 0.040(4) -0.006(3) 0.004(3) -0.004(3)
C46C 0.037(4) 0.023(4) 0.027(3) -0.001(3) 0.005(3) 0.004(3)
C48C 0.055(5) 0.030(4) 0.059(5) -0.008(4) 0.010(4) -0.005(4)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 N2 2.109(5) . ?
Rh1 N2' 2.125(5) . ?
Rh1 C3B 2.136(6) . ?
Rh1 C5B 2.140(6) . ?
Rh1 C2B 2.149(6) . ?
Rh1 C4B 2.156(6) . ?
Rh1 C1B 2.162(6) . ?
Rh1 Cl1 2.3811(17) . ?
N1 C5 1.352(9) . ?
N1 N2 1.356(8) . ?
N1 C1A 1.450(10) . ?
N2 C3 1.327(9) . ?
C3 C4 1.390(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.345(13) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
C1A N1' 1.437(9) . ?
C1A H2A 0.9900 . ?
C1A H1A 0.9900 . ?
N1' C5' 1.352(9) . ?
N1' N2' 1.355(7) . ?
N2' C3' 1.309(9) . ?
C3' C4' 1.381(10) . ?
C3' H3' 0.9500 . ?
C4' C5' 1.365(12) . ?
C4' H4' 0.9500 . ?
C5' H5' 0.9500 . ?
C1B C2B 1.427(9) . ?
C1B C5B 1.443(9) . ?
C1B C6B 1.490(9) . ?
C2B C3B 1.437(9) . ?
C2B C7B 1.498(9) . ?
C3B C4B 1.426(9) . ?
C3B C8B 1.502(9) . ?
C4B C5B 1.438(9) . ?
C4B C9B 1.486(9) . ?
C5B C10B 1.502(9) . ?
C6B H6A1 0.9800 . ?
C6B H6A2 0.9800 . ?
C6B H6A3 0.9800 . ?
C7B H7A1 0.9800 . ?
C7B H7A2 0.9800 . ?
C7B H7A3 0.9800 . ?
C8B H8A1 0.9800 . ?
C8B H8A2 0.9800 . ?
C8B H8A3 0.9800 . ?
C9B H9A1 0.9800 . ?
C9B H9A2 0.9800 . ?
C9B H9A3 0.9800 . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
B1C C11C 1.637(9) . ?
B1C C41C 1.638(9) . ?
B1C C21C 1.644(9) . ?
B1C C31C 1.644(9) . ?
C11C C12C 1.393(8) . ?
C11C C16C 1.414(9) . ?
C12C C13C 1.401(9) . ?
C12C H12C 0.9500 . ?
C13C C14C 1.376(9) . ?
C13C C17C 1.482(9) . ?
C14C C15C 1.385(9) . ?
C14C H14C 0.9500 . ?
C15C C16C 1.379(9) . ?
C15C C18C 1.493(9) . ?
C16C H16C 0.9500 . ?
C17C F172 1.325(7) . ?
C17C F176 1.336(12) . ?
C17C F171 1.348(7) . ?
C17C F173 1.351(7) . ?
C17C F175 1.366(12) . ?
C17C F178 1.375(11) . ?
C17C F174 1.376(12) . ?
C17C F177 1.397(11) . ?
C17C F179 1.400(11) . ?
C18C F181 1.321(9) . ?
C18C F182 1.334(8) . ?
C18C F183 1.335(9) . ?
C18C F188 1.346(15) . ?
C18C F187 1.348(14) . ?
C18C F186 1.351(9) . ?
C18C F185 1.354(9) . ?
C18C F189 1.391(14) . ?
C18C F184 1.417(9) . ?
C21C C26C 1.384(11) . ?
C21C C22C 1.406(11) . ?
C22C C23C 1.393(13) . ?
C22C H22C 0.9500 . ?
C23C C24C 1.402(18) . ?
C23C C27" 1.58(2) . ?
C23C C27C 1.60(2) . ?
C24C C25C 1.328(17) . ?
C24C H24C 0.9500 . ?
C25C C26C 1.402(11) . ?
C25C C28' 1.584(18) . ?
C25C C28C 1.603(16) . ?
C26C H26C 0.9500 . ?
C27C F273 1.333(12) . ?
C27C F272 1.343(12) . ?
C27C F271 1.353(12) . ?
C27" F274 1.300(13) . ?
C27" F276 1.300(13) . ?
C27" F275 1.301(13) . ?
C28C F282 1.364(11) . ?
C28C F281 1.364(12) . ?
C28C F283 1.386(12) . ?
C28' F287 1.253(16) . ?
C28' F288 1.252(16) . ?
C28' F289 1.252(16) . ?
C31C C36C 1.398(9) . ?
C31C C32C 1.399(9) . ?
C32C C33C 1.383(9) . ?
C32C H32C 0.9500 . ?
C33C C34C 1.399(10) . ?
C33C C37C 1.523(10) . ?
C34C C35C 1.374(10) . ?
C34C H34C 0.9500 . ?
C35C C36C 1.394(9) . ?
C35C C38C 1.483(10) . ?
C36C H36C 0.9500 . ?
C37C F371 1.299(7) . ?
C37C F373 1.321(8) . ?
C37C F372 1.324(7) . ?
C37C F375 1.357(13) . ?
C37C F376 1.365(13) . ?
C37C F374 1.380(11) . ?
C38C F384 1.308(9) . ?
C38C F382 1.316(9) . ?
C38C F389 1.345(14) . ?
C38C F388 1.349(13) . ?
C38C F385 1.353(9) . ?
C38C F387 1.366(13) . ?
C38C F383 1.368(9) . ?
C38C F381 1.382(8) . ?
C38C F386 1.402(9) . ?
C41C C42C 1.381(10) . ?
C41C C46C 1.408(9) . ?
C42C C43C 1.405(11) . ?
C42C H42C 0.9500 . ?
C43C C44C 1.375(11) . ?
C43C C47' 1.52(2) . ?
C43C C47C 1.59(2) . ?
C44C C45C 1.390(10) . ?
C44C H44C 0.9500 . ?
C45C C46C 1.375(9) . ?
C45C C48C 1.477(10) . ?
C46C H46C 0.9500 . ?
C48C F484 1.303(9) . ?
C48C F485 1.328(9) . ?
C48C F483 1.338(8) . ?
C48C F482 1.347(8) . ?
C48C F486 1.360(9) . ?
C48C F481 1.391(9) . ?
C47C F472 1.271(13) . ?
C47C F473 1.276(13) . ?
C47C F471 1.277(13) . ?
C47' F474 1.325(14) . ?
C47' F476 1.328(14) . ?
C47' F475 1.330(14) . ?
C1D Cl1D 1.41(7) 5_575 ?
C1D C1D 1.60(11) 5_575 ?
C1D Cl2D 1.71(8) 5_575 ?
C1D Cl2D 1.780(11) . ?
C1D Cl1D 1.777(11) . ?
Cl1D C1D 1.41(7) 5_575 ?
Cl2D C1D 1.71(8) 5_575 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Rh1 N2' 84.5(2) . . ?
N2 Rh1 C3B 112.1(2) . . ?
N2' Rh1 C3B 102.8(2) . . ?
N2 Rh1 C5B 112.1(2) . . ?
N2' Rh1 C5B 162.2(2) . . ?
C3B Rh1 C5B 65.7(2) . . ?
N2 Rh1 C2B 151.0(2) . . ?
N2' Rh1 C2B 97.1(2) . . ?
C3B Rh1 C2B 39.2(2) . . ?
C5B Rh1 C2B 65.3(2) . . ?
N2 Rh1 C4B 94.4(2) . . ?
N2' Rh1 C4B 137.4(2) . . ?
C3B Rh1 C4B 38.8(2) . . ?
C5B Rh1 C4B 39.1(2) . . ?
C2B Rh1 C4B 65.0(2) . . ?
N2 Rh1 C1B 151.0(2) . . ?
N2' Rh1 C1B 124.6(2) . . ?
C3B Rh1 C1B 65.5(2) . . ?
C5B Rh1 C1B 39.2(2) . . ?
C2B Rh1 C1B 38.7(2) . . ?
C4B Rh1 C1B 65.2(2) . . ?
N2 Rh1 Cl1 88.90(16) . . ?
N2' Rh1 Cl1 87.72(15) . . ?
C3B Rh1 Cl1 157.14(17) . . ?
C5B Rh1 Cl1 98.69(19) . . ?
C2B Rh1 Cl1 120.12(19) . . ?
C4B Rh1 Cl1 134.90(18) . . ?
C1B Rh1 Cl1 91.75(18) . . ?
C5 N1 N2 110.1(7) . . ?
C5 N1 C1A 129.8(7) . . ?
N2 N1 C1A 119.6(5) . . ?
C3 N2 N1 105.4(6) . . ?
C3 N2 Rh1 131.6(5) . . ?
N1 N2 Rh1 123.0(4) . . ?
N2 C3 C4 111.0(8) . . ?
N2 C3 H3 124.5 . . ?
C4 C3 H3 124.5 . . ?
C5 C4 C3 105.3(7) . . ?
C5 C4 H4 127.4 . . ?
C3 C4 H4 127.4 . . ?
C4 C5 N1 108.2(8) . . ?
C4 C5 H5 125.9 . . ?
N1 C5 H5 125.9 . . ?
N1' C1A N1 111.3(6) . . ?
N1' C1A H2A 109.4 . . ?
N1 C1A H2A 109.4 . . ?
N1' C1A H1A 109.4 . . ?
N1 C1A H1A 109.4 . . ?
H2A C1A H1A 108.0 . . ?
C5' N1' N2' 110.3(6) . . ?
C5' N1' C1A 129.0(6) . . ?
N2' N1' C1A 120.3(5) . . ?
C3' N2' N1' 105.9(5) . . ?
C3' N2' Rh1 132.0(5) . . ?
N1' N2' Rh1 122.0(4) . . ?
N2' C3' C4' 111.5(7) . . ?
N2' C3' H3' 124.3 . . ?
C4' C3' H3' 124.3 . . ?
C5' C4' C3' 105.3(7) . . ?
C5' C4' H4' 127.4 . . ?
C3' C4' H4' 127.4 . . ?
N1' C5' C4' 107.1(7) . . ?
N1' C5' H5' 126.5 . . ?
C4' C5' H5' 126.5 . . ?
C2B C1B C5B 107.5(5) . . ?
C2B C1B C6B 127.2(6) . . ?
C5B C1B C6B 125.2(6) . . ?
C2B C1B Rh1 70.2(3) . . ?
C5B C1B Rh1 69.6(3) . . ?
C6B C1B Rh1 127.6(5) . . ?
C1B C2B C3B 108.6(5) . . ?
C1B C2B C7B 126.4(6) . . ?
C3B C2B C7B 125.0(6) . . ?
C1B C2B Rh1 71.2(4) . . ?
C3B C2B Rh1 69.9(3) . . ?
C7B C2B Rh1 124.9(4) . . ?
C4B C3B C2B 107.8(5) . . ?
C4B C3B C8B 126.9(6) . . ?
C2B C3B C8B 125.0(6) . . ?
C4B C3B Rh1 71.4(3) . . ?
C2B C3B Rh1 70.9(3) . . ?
C8B C3B Rh1 128.2(4) . . ?
C3B C4B C5B 108.2(5) . . ?
C3B C4B C9B 126.0(6) . . ?
C5B C4B C9B 125.8(6) . . ?
C3B C4B Rh1 69.8(3) . . ?
C5B C4B Rh1 69.8(4) . . ?
C9B C4B Rh1 126.4(5) . . ?
C4B C5B C1B 107.8(5) . . ?
C4B C5B C10B 127.0(6) . . ?
C1B C5B C10B 125.1(6) . . ?
C4B C5B Rh1 71.1(3) . . ?
C1B C5B Rh1 71.2(3) . . ?
C10B C5B Rh1 125.9(5) . . ?
C1B C6B H6A1 109.5 . . ?
C1B C6B H6A2 109.5 . . ?
H6A1 C6B H6A2 109.5 . . ?
C1B C6B H6A3 109.5 . . ?
H6A1 C6B H6A3 109.5 . . ?
H6A2 C6B H6A3 109.5 . . ?
C2B C7B H7A1 109.5 . . ?
C2B C7B H7A2 109.5 . . ?
H7A1 C7B H7A2 109.5 . . ?
C2B C7B H7A3 109.5 . . ?
H7A1 C7B H7A3 109.5 . . ?
H7A2 C7B H7A3 109.5 . . ?
C3B C8B H8A1 109.5 . . ?
C3B C8B H8A2 109.5 . . ?
H8A1 C8B H8A2 109.5 . . ?
C3B C8B H8A3 109.5 . . ?
H8A1 C8B H8A3 109.5 . . ?
H8A2 C8B H8A3 109.5 . . ?
C4B C9B H9A1 109.5 . . ?
C4B C9B H9A2 109.5 . . ?
H9A1 C9B H9A2 109.5 . . ?
C4B C9B H9A3 109.5 . . ?
H9A1 C9B H9A3 109.5 . . ?
H9A2 C9B H9A3 109.5 . . ?
C5B C10B H10A 109.5 . . ?
C5B C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C5B C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
C11C B1C C41C 112.1(5) . . ?
C11C B1C C21C 111.9(5) . . ?
C41C B1C C21C 104.4(5) . . ?
C11C B1C C31C 103.1(5) . . ?
C41C B1C C31C 115.7(5) . . ?
C21C B1C C31C 109.9(5) . . ?
C12C C11C C16C 115.4(6) . . ?
C12C C11C B1C 123.2(5) . . ?
C16C C11C B1C 121.1(5) . . ?
C11C C12C C13C 122.3(6) . . ?
C11C C12C H12C 118.8 . . ?
C13C C12C H12C 118.8 . . ?
C14C C13C C12C 120.7(6) . . ?
C14C C13C C17C 119.3(6) . . ?
C12C C13C C17C 120.0(5) . . ?
C13C C14C C15C 118.2(6) . . ?
C13C C14C H14C 120.9 . . ?
C15C C14C H14C 120.9 . . ?
C16C C15C C14C 121.3(6) . . ?
C16C C15C C18C 118.4(6) . . ?
C14C C15C C18C 120.4(6) . . ?
C15C C16C C11C 122.1(6) . . ?
C15C C16C H16C 119.0 . . ?
C11C C16C H16C 119.0 . . ?
F172 C17C F176 126.4(9) . . ?
F172 C17C F171 107.6(5) . . ?
F176 C17C F171 73.9(7) . . ?
F172 C17C F173 106.1(5) . . ?
F176 C17C F173 33.3(6) . . ?
F171 C17C F173 105.4(5) . . ?
F172 C17C F175 31.4(6) . . ?
F176 C17C F175 107.9(7) . . ?
F171 C17C F175 131.4(9) . . ?
F173 C17C F175 79.2(7) . . ?
F172 C17C F178 27.2(5) . . ?
F176 C17C F178 126.5(10) . . ?
F171 C17C F178 81.6(6) . . ?
F173 C17C F178 122.0(8) . . ?
F175 C17C F178 57.8(8) . . ?
F172 C17C F174 75.0(7) . . ?
F176 C17C F174 106.9(7) . . ?
F171 C17C F174 36.9(6) . . ?
F173 C17C F174 131.9(9) . . ?
F175 C17C F174 104.9(7) . . ?
F178 C17C F174 47.8(7) . . ?
F172 C17C F177 125.1(8) . . ?
F176 C17C F177 46.9(7) . . ?
F171 C17C F177 27.6(5) . . ?
F173 C17C F177 79.6(6) . . ?
F175 C17C F177 134.9(11) . . ?
F178 C17C F177 103.4(7) . . ?
F174 C17C F177 63.7(7) . . ?
F172 C17C F179 82.6(7) . . ?
F176 C17C F179 57.8(8) . . ?
F171 C17C F179 123.4(8) . . ?
F173 C17C F179 25.7(6) . . ?
F175 C17C F179 53.8(8) . . ?
F178 C17C F179 103.6(7) . . ?
F174 C17C F179 134.8(11) . . ?
F177 C17C F179 101.5(7) . . ?
F172 C17C C13C 113.1(5) . . ?
F176 C17C C13C 115.6(8) . . ?
F171 C17C C13C 111.4(6) . . ?
F173 C17C C13C 112.7(5) . . ?
F175 C17C C13C 110.7(9) . . ?
F178 C17C C13C 117.6(8) . . ?
F174 C17C C13C 110.2(8) . . ?
F177 C17C C13C 114.1(7) . . ?
F179 C17C C13C 114.7(8) . . ?
F181 C18C F182 107.0(6) . . ?
F181 C18C F183 107.2(6) . . ?
F182 C18C F183 106.6(6) . . ?
F181 C18C F188 69.3(9) . . ?
F182 C18C F188 38.0(8) . . ?
F183 C18C F188 121.9(14) . . ?
F181 C18C F187 45.1(7) . . ?
F182 C18C F187 134.4(10) . . ?
F183 C18C F187 65.4(8) . . ?
F188 C18C F187 105.4(10) . . ?
F181 C18C F186 80.2(6) . . ?
F182 C18C F186 125.7(7) . . ?
F183 C18C F186 28.9(5) . . ?
F188 C18C F186 121.2(14) . . ?
F187 C18C F186 36.6(7) . . ?
F181 C18C F185 120.4(8) . . ?
F182 C18C F185 22.6(5) . . ?
F183 C18C F185 84.8(6) . . ?
F188 C18C F185 56.2(9) . . ?
F187 C18C F185 129.2(11) . . ?
F186 C18C F185 107.5(6) . . ?
F181 C18C F189 135.2(11) . . ?
F182 C18C F189 73.0(8) . . ?
F183 C18C F189 38.2(7) . . ?
F188 C18C F189 102.6(9) . . ?
F187 C18C F189 101.9(9) . . ?
F186 C18C F189 66.6(8) . . ?
F185 C18C F189 50.5(8) . . ?
F181 C18C F184 24.8(5) . . ?
F182 C18C F184 85.5(6) . . ?
F183 C18C F184 126.5(8) . . ?
F188 C18C F184 47.7(9) . . ?
F187 C18C F184 69.5(8) . . ?
F186 C18C F184 102.7(6) . . ?
F185 C18C F184 103.3(6) . . ?
F189 C18C F184 139.6(11) . . ?
F181 C18C C15C 113.4(7) . . ?
F182 C18C C15C 110.8(6) . . ?
F183 C18C C15C 111.5(7) . . ?
F188 C18C C15C 123.0(14) . . ?
F187 C18C C15C 113.8(9) . . ?
F186 C18C C15C 114.9(6) . . ?
F185 C18C C15C 115.2(7) . . ?
F189 C18C C15C 107.6(10) . . ?
F184 C18C C15C 111.9(6) . . ?
C26C C21C C22C 117.4(7) . . ?
C26C C21C B1C 123.7(6) . . ?
C22C C21C B1C 118.6(7) . . ?
C23C C22C C21C 120.0(10) . . ?
C23C C22C H22C 120.0 . . ?
C21C C22C H22C 120.0 . . ?
C22C C23C C24C 121.0(10) . . ?
C22C C23C C27" 130.6(12) . . ?
C24C C23C C27" 107.8(10) . . ?
C22C C23C C27C 108.0(11) . . ?
C24C C23C C27C 131.0(9) . . ?
C27" C23C C27C 24.7(7) . . ?
C25C C24C C23C 118.5(9) . . ?
C25C C24C H24C 120.7 . . ?
C23C C24C H24C 120.7 . . ?
C24C C25C C26C 122.0(11) . . ?
C24C C25C C28' 108.8(10) . . ?
C26C C25C C28' 128.3(12) . . ?
C24C C25C C28C 124.8(9) . . ?
C26C C25C C28C 112.8(10) . . ?
C28' C25C C28C 22.7(7) . . ?
C21C C26C C25C 121.0(9) . . ?
C21C C26C H26C 119.5 . . ?
C25C C26C H26C 119.5 . . ?
F273 C27C F272 102.7(12) . . ?
F273 C27C F271 102.9(12) . . ?
F272 C27C F271 102.2(12) . . ?
F273 C27C C23C 113.5(13) . . ?
F272 C27C C23C 118.4(14) . . ?
F271 C27C C23C 115.2(12) . . ?
F274 C27" F276 113.5(11) . . ?
F274 C27" F275 112.1(11) . . ?
F276 C27" F275 112.7(11) . . ?
F274 C27" C23C 100.4(14) . . ?
F276 C27" C23C 113.8(16) . . ?
F275 C27" C23C 103.4(15) . . ?
F282 C28C F281 102.8(9) . . ?
F282 C28C F283 101.4(9) . . ?
F281 C28C F283 102.2(9) . . ?
F282 C28C C25C 121.2(9) . . ?
F281 C28C C25C 122.6(12) . . ?
F283 C28C C25C 103.0(10) . . ?
F287 C28' F288 112.2(14) . . ?
F287 C28' F289 112.0(14) . . ?
F288 C28' F289 111.8(13) . . ?
F287 C28' C25C 106(4) . . ?
F288 C28' C25C 112.7(15) . . ?
F289 C28' C25C 102.0(14) . . ?
C36C C31C C32C 115.4(6) . . ?
C36C C31C B1C 124.2(5) . . ?
C32C C31C B1C 120.1(6) . . ?
C33C C32C C31C 123.4(6) . . ?
C33C C32C H32C 118.3 . . ?
C31C C32C H32C 118.3 . . ?
C32C C33C C34C 119.6(6) . . ?
C32C C33C C37C 119.5(6) . . ?
C34C C33C C37C 120.9(6) . . ?
C35C C34C C33C 118.3(6) . . ?
C35C C34C H34C 120.9 . . ?
C33C C34C H34C 120.9 . . ?
C34C C35C C36C 121.4(6) . . ?
C34C C35C C38C 118.7(6) . . ?
C36C C35C C38C 119.9(6) . . ?
C35C C36C C31C 121.8(6) . . ?
C35C C36C H36C 119.1 . . ?
C31C C36C H36C 119.1 . . ?
F371 C37C F373 107.4(6) . . ?
F371 C37C F372 107.8(6) . . ?
F373 C37C F372 105.4(6) . . ?
F371 C37C F375 123.7(10) . . ?
F373 C37C F375 21.1(7) . . ?
F372 C37C F375 86.7(8) . . ?
F371 C37C F376 84.6(8) . . ?
F373 C37C F376 124.2(10) . . ?
F372 C37C F376 25.6(7) . . ?
F375 C37C F376 108.9(8) . . ?
F371 C37C F374 23.7(5) . . ?
F373 C37C F374 88.2(7) . . ?
F372 C37C F374 127.8(8) . . ?
F375 C37C F374 107.6(8) . . ?
F376 C37C F374 107.1(8) . . ?
F371 C37C C33C 111.3(7) . . ?
F373 C37C C33C 113.2(6) . . ?
F372 C37C C33C 111.3(6) . . ?
F375 C37C C33C 112.8(10) . . ?
F376 C37C C33C 111.8(11) . . ?
F374 C37C C33C 108.4(8) . . ?
F384 C38C F382 119.0(9) . . ?
F384 C38C F389 66.5(9) . . ?
F382 C38C F389 67.3(9) . . ?
F384 C38C F388 126.1(10) . . ?
F382 C38C F388 41.2(7) . . ?
F389 C38C F388 105.4(9) . . ?
F384 C38C F385 108.5(7) . . ?
F382 C38C F385 66.9(6) . . ?
F389 C38C F385 121.6(13) . . ?
F388 C38C F385 28.0(7) . . ?
F384 C38C F387 40.4(7) . . ?
F382 C38C F387 127.0(11) . . ?
F389 C38C F387 104.4(9) . . ?
F388 C38C F387 103.4(8) . . ?
F385 C38C F387 77.1(8) . . ?
F384 C38C F383 69.6(6) . . ?
F382 C38C F383 105.4(7) . . ?
F389 C38C F383 121.7(14) . . ?
F388 C38C F383 72.5(8) . . ?
F385 C38C F383 45.1(6) . . ?
F387 C38C F383 32.3(7) . . ?
F384 C38C F381 31.5(5) . . ?
F382 C38C F381 104.4(7) . . ?
F389 C38C F381 39.3(9) . . ?
F388 C38C F381 134.3(10) . . ?
F385 C38C F381 131.6(8) . . ?
F387 C38C F381 71.9(8) . . ?
F383 C38C F381 100.3(6) . . ?
F384 C38C F386 104.6(7) . . ?
F382 C38C F386 34.4(5) . . ?
F389 C38C F386 39.3(9) . . ?
F388 C38C F386 75.5(8) . . ?
F385 C38C F386 101.1(6) . . ?
F387 C38C F386 136.5(10) . . ?
F383 C38C F386 132.8(9) . . ?
F381 C38C F386 78.5(5) . . ?
F384 C38C C35C 117.8(7) . . ?
F382 C38C C35C 118.8(7) . . ?
F389 C38C C35C 119.6(13) . . ?
F388 C38C C35C 111.9(9) . . ?
F385 C38C C35C 113.4(7) . . ?
F387 C38C C35C 110.6(9) . . ?
F383 C38C C35C 114.0(8) . . ?
F381 C38C C35C 112.0(6) . . ?
F386 C38C C35C 109.8(6) . . ?
C42C C41C C46C 115.9(6) . . ?
C42C C41C B1C 124.7(6) . . ?
C46C C41C B1C 118.7(5) . . ?
C41C C42C C43C 122.0(7) . . ?
C41C C42C H42C 119.0 . . ?
C43C C42C H42C 119.0 . . ?
C44C C43C C42C 120.4(7) . . ?
C44C C43C C47' 116.7(8) . . ?
C42C C43C C47' 121.4(7) . . ?
C44C C43C C47C 122.5(7) . . ?
C42C C43C C47C 115.7(7) . . ?
C47' C43C C47C 25.3(6) . . ?
C43C C44C C45C 119.0(7) . . ?
C43C C44C H44C 120.5 . . ?
C45C C44C H44C 120.5 . . ?
C46C C45C C44C 119.9(6) . . ?
C46C C45C C48C 121.5(6) . . ?
C44C C45C C48C 118.6(6) . . ?
C45C C46C C41C 122.8(6) . . ?
C45C C46C H46C 118.6 . . ?
C41C C46C H46C 118.6 . . ?
F484 C48C F485 107.0(7) . . ?
F484 C48C F483 71.9(6) . . ?
F485 C48C F483 123.1(8) . . ?
F484 C48C F482 121.6(9) . . ?
F485 C48C F482 23.4(5) . . ?
F483 C48C F482 107.5(6) . . ?
F484 C48C F486 105.0(7) . . ?
F485 C48C F486 103.4(6) . . ?
F483 C48C F486 34.6(5) . . ?
F482 C48C F486 81.6(6) . . ?
F484 C48C F481 31.8(6) . . ?
F485 C48C F481 83.3(6) . . ?
F483 C48C F481 102.6(6) . . ?
F482 C48C F481 104.3(6) . . ?
F486 C48C F481 132.4(8) . . ?
F484 C48C C45C 116.5(8) . . ?
F485 C48C C45C 114.4(7) . . ?
F483 C48C C45C 115.8(6) . . ?
F482 C48C C45C 115.1(7) . . ?
F486 C48C C45C 109.3(7) . . ?
F481 C48C C45C 110.1(7) . . ?
F472 C47C F473 107.5(13) . . ?
F472 C47C F471 106.3(12) . . ?
F473 C47C F471 104.0(12) . . ?
F472 C47C C43C 110.8(12) . . ?
F473 C47C C43C 117.7(14) . . ?
F471 C47C C43C 109.8(13) . . ?
F474 C47' F476 106.5(12) . . ?
F474 C47' F475 108.3(12) . . ?
F476 C47' F475 106.1(12) . . ?
F474 C47' C43C 114.7(13) . . ?
F476 C47' C43C 118.3(14) . . ?
F475 C47' C43C 102.2(16) . . ?
Cl1D C1D C1D 72(4) 5_575 5_575 ?
Cl1D C1D Cl2D 10(3) 5_575 5_575 ?
C1D C1D Cl2D 65(4) 5_575 5_575 ?
Cl1D C1D Cl2D 132(5) 5_575 . ?
C1D C1D Cl2D 61(3) 5_575 . ?
Cl2D C1D Cl2D 125(3) 5_575 . ?
Cl1D C1D Cl1D 121(4) 5_575 . ?
C1D C1D Cl1D 49(2) 5_575 . ?
Cl2D C1D Cl1D 113(4) 5_575 . ?
Cl2D C1D Cl1D 13(3) . . ?
C1D Cl1D C1D 59(4) 5_575 . ?
C1D Cl2D C1D 55(3) 5_575 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 N2 C3 -1.3(8) . . . . ?
C1A N1 N2 C3 -173.8(6) . . . . ?
C5 N1 N2 Rh1 177.1(5) . . . . ?
C1A N1 N2 Rh1 4.6(8) . . . . ?
N2' Rh1 N2 C3 -149.4(7) . . . . ?
C3B Rh1 N2 C3 109.1(6) . . . . ?
C5B Rh1 N2 C3 37.4(7) . . . . ?
C2B Rh1 N2 C3 116.0(7) . . . . ?
C4B Rh1 N2 C3 73.4(7) . . . . ?
C1B Rh1 N2 C3 30.1(9) . . . . ?
Cl1 Rh1 N2 C3 -61.6(6) . . . . ?
N2' Rh1 N2 N1 32.6(5) . . . . ?
C3B Rh1 N2 N1 -68.9(5) . . . . ?
C5B Rh1 N2 N1 -140.6(5) . . . . ?
C2B Rh1 N2 N1 -62.0(7) . . . . ?
C4B Rh1 N2 N1 -104.6(5) . . . . ?
C1B Rh1 N2 N1 -147.9(5) . . . . ?
Cl1 Rh1 N2 N1 120.4(5) . . . . ?
N1 N2 C3 C4 1.5(8) . . . . ?
Rh1 N2 C3 C4 -176.7(5) . . . . ?
N2 C3 C4 C5 -1.2(10) . . . . ?
C3 C4 C5 N1 0.3(9) . . . . ?
N2 N1 C5 C4 0.6(9) . . . . ?
C1A N1 C5 C4 172.1(7) . . . . ?
C5 N1 C1A N1' 130.0(7) . . . . ?
N2 N1 C1A N1' -59.1(8) . . . . ?
N1 C1A N1' C5' -125.9(7) . . . . ?
N1 C1A N1' N2' 61.5(8) . . . . ?
C5' N1' N2' C3' 1.3(7) . . . . ?
C1A N1' N2' C3' 175.1(6) . . . . ?
C5' N1' N2' Rh1 177.5(4) . . . . ?
C1A N1' N2' Rh1 -8.6(8) . . . . ?
N2 Rh1 N2' C3' 144.5(6) . . . . ?
C3B Rh1 N2' C3' -104.1(6) . . . . ?
C5B Rh1 N2' C3' -56.4(10) . . . . ?
C2B Rh1 N2' C3' -64.7(6) . . . . ?
C4B Rh1 N2' C3' -125.0(6) . . . . ?
C1B Rh1 N2' C3' -35.2(7) . . . . ?
Cl1 Rh1 N2' C3' 55.4(6) . . . . ?
N2 Rh1 N2' N1' -30.7(5) . . . . ?
C3B Rh1 N2' N1' 80.7(5) . . . . ?
C5B Rh1 N2' N1' 128.5(7) . . . . ?
C2B Rh1 N2' N1' 120.1(5) . . . . ?
C4B Rh1 N2' N1' 59.8(6) . . . . ?
C1B Rh1 N2' N1' 149.7(5) . . . . ?
Cl1 Rh1 N2' N1' -119.8(5) . . . . ?
N1' N2' C3' C4' -0.9(8) . . . . ?
Rh1 N2' C3' C4' -176.6(5) . . . . ?
N2' C3' C4' C5' 0.2(8) . . . . ?
N2' N1' C5' C4' -1.1(8) . . . . ?
C1A N1' C5' C4' -174.3(7) . . . . ?
C3' C4' C5' N1' 0.6(8) . . . . ?
N2 Rh1 C1B C2B 129.2(5) . . . . ?
N2' Rh1 C1B C2B -51.5(4) . . . . ?
C3B Rh1 C1B C2B 37.4(4) . . . . ?
C5B Rh1 C1B C2B 118.4(5) . . . . ?
C4B Rh1 C1B C2B 80.3(4) . . . . ?
Cl1 Rh1 C1B C2B -139.9(4) . . . . ?
N2 Rh1 C1B C5B 10.8(7) . . . . ?
N2' Rh1 C1B C5B -169.9(3) . . . . ?
C3B Rh1 C1B C5B -81.0(4) . . . . ?
C2B Rh1 C1B C5B -118.4(5) . . . . ?
C4B Rh1 C1B C5B -38.1(4) . . . . ?
Cl1 Rh1 C1B C5B 101.7(4) . . . . ?
N2 Rh1 C1B C6B -108.6(7) . . . . ?
N2' Rh1 C1B C6B 70.7(7) . . . . ?
C3B Rh1 C1B C6B 159.6(7) . . . . ?
C5B Rh1 C1B C6B -119.4(8) . . . . ?
C2B Rh1 C1B C6B 122.2(8) . . . . ?
C4B Rh1 C1B C6B -157.5(7) . . . . ?
Cl1 Rh1 C1B C6B -17.7(6) . . . . ?
C5B C1B C2B C3B -0.3(7) . . . . ?
C6B C1B C2B C3B 177.2(6) . . . . ?
Rh1 C1B C2B C3B -60.1(4) . . . . ?
C5B C1B C2B C7B 179.8(6) . . . . ?
C6B C1B C2B C7B -2.7(11) . . . . ?
Rh1 C1B C2B C7B 120.0(6) . . . . ?
C5B C1B C2B Rh1 59.8(4) . . . . ?
C6B C1B C2B Rh1 -122.7(7) . . . . ?
N2 Rh1 C2B C1B -129.2(5) . . . . ?
N2' Rh1 C2B C1B 139.5(4) . . . . ?
C3B Rh1 C2B C1B -119.0(5) . . . . ?
C5B Rh1 C2B C1B -37.7(4) . . . . ?
C4B Rh1 C2B C1B -81.0(4) . . . . ?
Cl1 Rh1 C2B C1B 48.0(4) . . . . ?
N2 Rh1 C2B C3B -10.2(6) . . . . ?
N2' Rh1 C2B C3B -101.5(3) . . . . ?
C5B Rh1 C2B C3B 81.2(4) . . . . ?
C4B Rh1 C2B C3B 38.0(3) . . . . ?
C1B Rh1 C2B C3B 119.0(5) . . . . ?
Cl1 Rh1 C2B C3B 167.0(3) . . . . ?
N2 Rh1 C2B C7B 109.0(7) . . . . ?
N2' Rh1 C2B C7B 17.7(6) . . . . ?
C3B Rh1 C2B C7B 119.3(7) . . . . ?
C5B Rh1 C2B C7B -159.5(7) . . . . ?
C4B Rh1 C2B C7B 157.2(7) . . . . ?
C1B Rh1 C2B C7B -121.8(8) . . . . ?
Cl1 Rh1 C2B C7B -73.7(6) . . . . ?
C1B C2B C3B C4B -1.3(7) . . . . ?
C7B C2B C3B C4B 178.5(6) . . . . ?
Rh1 C2B C3B C4B -62.3(4) . . . . ?
C1B C2B C3B C8B -175.3(6) . . . . ?
C7B C2B C3B C8B 4.6(9) . . . . ?
Rh1 C2B C3B C8B 123.8(6) . . . . ?
C1B C2B C3B Rh1 60.9(4) . . . . ?
C7B C2B C3B Rh1 -119.2(6) . . . . ?
N2 Rh1 C3B C4B -68.1(4) . . . . ?
N2' Rh1 C3B C4B -157.3(3) . . . . ?
C5B Rh1 C3B C4B 37.1(3) . . . . ?
C2B Rh1 C3B C4B 117.2(5) . . . . ?
C1B Rh1 C3B C4B 80.3(4) . . . . ?
Cl1 Rh1 C3B C4B 87.1(5) . . . . ?
N2 Rh1 C3B C2B 174.7(3) . . . . ?
N2' Rh1 C3B C2B 85.5(4) . . . . ?
C5B Rh1 C3B C2B -80.1(4) . . . . ?
C4B Rh1 C3B C2B -117.2(5) . . . . ?
C1B Rh1 C3B C2B -36.9(3) . . . . ?
Cl1 Rh1 C3B C2B -30.1(6) . . . . ?
N2 Rh1 C3B C8B 54.6(7) . . . . ?
N2' Rh1 C3B C8B -34.6(6) . . . . ?
C5B Rh1 C3B C8B 159.8(7) . . . . ?
C2B Rh1 C3B C8B -120.1(8) . . . . ?
C4B Rh1 C3B C8B 122.7(8) . . . . ?
C1B Rh1 C3B C8B -157.0(7) . . . . ?
Cl1 Rh1 C3B C8B -150.1(5) . . . . ?
C2B C3B C4B C5B 2.5(7) . . . . ?
C8B C3B C4B C5B 176.3(6) . . . . ?
Rh1 C3B C4B C5B -59.5(4) . . . . ?
C2B C3B C4B C9B -177.1(6) . . . . ?
C8B C3B C4B C9B -3.3(10) . . . . ?
Rh1 C3B C4B C9B 121.0(6) . . . . ?
C2B C3B C4B Rh1 62.0(4) . . . . ?
C8B C3B C4B Rh1 -124.3(6) . . . . ?
N2 Rh1 C4B C3B 120.4(4) . . . . ?
N2' Rh1 C4B C3B 33.8(5) . . . . ?
C5B Rh1 C4B C3B -119.4(5) . . . . ?
C2B Rh1 C4B C3B -38.3(3) . . . . ?
C1B Rh1 C4B C3B -81.1(4) . . . . ?
Cl1 Rh1 C4B C3B -146.8(3) . . . . ?
N2 Rh1 C4B C5B -120.3(4) . . . . ?
N2' Rh1 C4B C5B 153.1(4) . . . . ?
C3B Rh1 C4B C5B 119.4(5) . . . . ?
C2B Rh1 C4B C5B 81.0(4) . . . . ?
C1B Rh1 C4B C5B 38.2(4) . . . . ?
Cl1 Rh1 C4B C5B -27.4(5) . . . . ?
N2 Rh1 C4B C9B 0.0(6) . . . . ?
N2' Rh1 C4B C9B -86.6(7) . . . . ?
C3B Rh1 C4B C9B -120.4(7) . . . . ?
C5B Rh1 C4B C9B 120.2(7) . . . . ?
C2B Rh1 C4B C9B -158.8(7) . . . . ?
C1B Rh1 C4B C9B 158.4(7) . . . . ?
Cl1 Rh1 C4B C9B 92.8(6) . . . . ?
C3B C4B C5B C1B -2.7(7) . . . . ?
C9B C4B C5B C1B 176.9(6) . . . . ?
Rh1 C4B C5B C1B -62.1(4) . . . . ?
C3B C4B C5B C10B -179.4(7) . . . . ?
C9B C4B C5B C10B 0.2(11) . . . . ?
Rh1 C4B C5B C10B 121.2(7) . . . . ?
C3B C4B C5B Rh1 59.5(4) . . . . ?
C9B C4B C5B Rh1 -121.0(6) . . . . ?
C2B C1B C5B C4B 1.8(7) . . . . ?
C6B C1B C5B C4B -175.7(6) . . . . ?
Rh1 C1B C5B C4B 62.0(4) . . . . ?
C2B C1B C5B C10B 178.6(7) . . . . ?
C6B C1B C5B C10B 1.1(11) . . . . ?
Rh1 C1B C5B C10B -121.2(7) . . . . ?
C2B C1B C5B Rh1 -60.2(4) . . . . ?
C6B C1B C5B Rh1 122.3(7) . . . . ?
N2 Rh1 C5B C4B 68.4(4) . . . . ?
N2' Rh1 C5B C4B -89.1(8) . . . . ?
C3B Rh1 C5B C4B -36.8(4) . . . . ?
C2B Rh1 C5B C4B -80.0(4) . . . . ?
C1B Rh1 C5B C4B -117.2(5) . . . . ?
Cl1 Rh1 C5B C4B 160.7(3) . . . . ?
N2 Rh1 C5B C1B -174.4(4) . . . . ?
N2' Rh1 C5B C1B 28.1(9) . . . . ?
C3B Rh1 C5B C1B 80.4(4) . . . . ?
C2B Rh1 C5B C1B 37.2(4) . . . . ?
C4B Rh1 C5B C1B 117.2(5) . . . . ?
Cl1 Rh1 C5B C1B -82.0(4) . . . . ?
N2 Rh1 C5B C10B -54.2(7) . . . . ?
N2' Rh1 C5B C10B 148.3(7) . . . . ?
C3B Rh1 C5B C10B -159.3(7) . . . . ?
C2B Rh1 C5B C10B 157.4(7) . . . . ?
C4B Rh1 C5B C10B -122.5(8) . . . . ?
C1B Rh1 C5B C10B 120.2(8) . . . . ?
Cl1 Rh1 C5B C10B 38.2(6) . . . . ?
C41C B1C C11C C12C 27.0(8) . . . . ?
C21C B1C C11C C12C 143.8(6) . . . . ?
C31C B1C C11C C12C -98.1(6) . . . . ?
C41C B1C C11C C16C -159.0(5) . . . . ?
C21C B1C C11C C16C -42.2(8) . . . . ?
C31C B1C C11C C16C 75.9(7) . . . . ?
C16C C11C C12C C13C 0.0(8) . . . . ?
B1C C11C C12C C13C 174.3(5) . . . . ?
C11C C12C C13C C14C -0.2(9) . . . . ?
C11C C12C C13C C17C 179.0(5) . . . . ?
C12C C13C C14C C15C 0.3(9) . . . . ?
C17C C13C C14C C15C -178.9(5) . . . . ?
C13C C14C C15C C16C -0.3(9) . . . . ?
C13C C14C C15C C18C 179.3(5) . . . . ?
C14C C15C C16C C11C 0.1(9) . . . . ?
C18C C15C C16C C11C -179.5(5) . . . . ?
C12C C11C C16C C15C 0.0(8) . . . . ?
B1C C11C C16C C15C -174.4(6) . . . . ?
C14C C13C C17C F172 87.3(7) . . . . ?
C12C C13C C17C F172 -91.9(7) . . . . ?
C14C C13C C17C F176 -115.8(9) . . . . ?
C12C C13C C17C F176 65.0(10) . . . . ?
C14C C13C C17C F171 -34.0(8) . . . . ?
C12C C13C C17C F171 146.8(7) . . . . ?
C14C C13C C17C F173 -152.3(6) . . . . ?
C12C C13C C17C F173 28.5(8) . . . . ?
C14C C13C C17C F175 121.1(9) . . . . ?
C12C C13C C17C F175 -58.1(10) . . . . ?
C14C C13C C17C F178 57.5(10) . . . . ?
C12C C13C C17C F178 -121.7(9) . . . . ?
C14C C13C C17C F174 5.5(10) . . . . ?
C12C C13C C17C F174 -173.7(9) . . . . ?
C14C C13C C17C F177 -63.8(9) . . . . ?
C12C C13C C17C F177 117.0(9) . . . . ?
C14C C13C C17C F179 179.7(8) . . . . ?
C12C C13C C17C F179 0.5(10) . . . . ?
C16C C15C C18C F181 -39.9(8) . . . . ?
C14C C15C C18C F181 140.5(7) . . . . ?
C16C C15C C18C F182 80.5(7) . . . . ?
C14C C15C C18C F182 -99.1(7) . . . . ?
C16C C15C C18C F183 -161.0(7) . . . . ?
C14C C15C C18C F183 19.4(9) . . . . ?
C16C C15C C18C F188 39.9(13) . . . . ?
C14C C15C C18C F188 -139.7(12) . . . . ?
C16C C15C C18C F187 -89.4(10) . . . . ?
C14C C15C C18C F187 91.0(10) . . . . ?
C16C C15C C18C F186 -129.7(7) . . . . ?
C14C C15C C18C F186 50.7(8) . . . . ?
C16C C15C C18C F185 104.6(8) . . . . ?
C14C C15C C18C F185 -75.0(8) . . . . ?
C16C C15C C18C F189 158.5(10) . . . . ?
C14C C15C C18C F189 -21.1(10) . . . . ?
C16C C15C C18C F184 -13.1(8) . . . . ?
C14C C15C C18C F184 167.3(6) . . . . ?
C11C B1C C21C C26C -25.6(9) . . . . ?
C41C B1C C21C C26C 95.8(7) . . . . ?
C31C B1C C21C C26C -139.5(7) . . . . ?
C11C B1C C21C C22C 160.3(6) . . . . ?
C41C B1C C21C C22C -78.3(7) . . . . ?
C31C B1C C21C C22C 46.3(8) . . . . ?
C26C C21C C22C C23C 0.6(12) . . . . ?
B1C C21C C22C C23C 175.1(8) . . . . ?
C21C C22C C23C C24C 1.6(15) . . . . ?
C21C C22C C23C C27" 170.9(11) . . . . ?
C21C C22C C23C C27C -177.4(8) . . . . ?
C22C C23C C24C C25C -3.3(18) . . . . ?
C27" C23C C24C C25C -174.8(11) . . . . ?
C27C C23C C24C C25C 175.4(11) . . . . ?
C23C C24C C25C C26C 2.9(17) . . . . ?
C23C C24C C25C C28' -166.8(12) . . . . ?
C23C C24C C25C C28C 175.1(10) . . . . ?
C22C C21C C26C C25C -1.0(11) . . . . ?
B1C C21C C26C C25C -175.2(7) . . . . ?
C24C C25C C26C C21C -0.8(14) . . . . ?
C28' C25C C26C C21C 166.7(12) . . . . ?
C28C C25C C26C C21C -173.9(7) . . . . ?
C22C C23C C27C F273 -176.1(9) . . . . ?
C24C C23C C27C F273 5.1(17) . . . . ?
C27" C23C C27C F273 -17.7(13) . . . . ?
C22C C23C C27C F272 63.5(12) . . . . ?
C24C C23C C27C F272 -115.4(14) . . . . ?
C27" C23C C27C F272 -138.1(18) . . . . ?
C22C C23C C27C F271 -57.9(12) . . . . ?
C24C C23C C27C F271 123.3(13) . . . . ?
C27" C23C C27C F271 100.6(17) . . . . ?
C22C C23C C27" F274 5.1(16) . . . . ?
C24C C23C C27" F274 175.6(11) . . . . ?
C27C C23C C27" F274 -22.3(13) . . . . ?
C22C C23C C27" F276 -116.4(14) . . . . ?
C24C C23C C27" F276 54.0(13) . . . . ?
C27C C23C C27" F276 -143.8(19) . . . . ?
C22C C23C C27" F275 121.0(13) . . . . ?
C24C C23C C27" F275 -68.6(12) . . . . ?
C27C C23C C27" F275 93.6(16) . . . . ?
C24C C25C C28C F282 -38.0(15) . . . . ?
C26C C25C C28C F282 134.8(9) . . . . ?
C28' C25C C28C F282 -88(2) . . . . ?
C24C C25C C28C F281 -172.0(12) . . . . ?
C26C C25C C28C F281 0.9(13) . . . . ?
C28' C25C C28C F281 138(2) . . . . ?
C24C C25C C28C F283 74.1(13) . . . . ?
C26C C25C C28C F283 -113.0(9) . . . . ?
C28' C25C C28C F283 24(2) . . . . ?
C24C C25C C28' F287 -67.9(13) . . . . ?
C26C C25C C28' F287 123.3(14) . . . . ?
C28C C25C C28' F287 71(2) . . . . ?
C24C C25C C28' F288 54.9(16) . . . . ?
C26C C25C C28' F288 -113.9(15) . . . . ?
C28C C25C C28' F288 -167(3) . . . . ?
C24C C25C C28' F289 174.9(12) . . . . ?
C26C C25C C28' F289 6.1(18) . . . . ?
C28C C25C C28' F289 -46.4(17) . . . . ?
C11C B1C C31C C36C 88.0(7) . . . . ?
C41C B1C C31C C36C -34.6(8) . . . . ?
C21C B1C C31C C36C -152.5(6) . . . . ?
C11C B1C C31C C32C -84.6(6) . . . . ?
C41C B1C C31C C32C 152.7(6) . . . . ?
C21C B1C C31C C32C 34.9(8) . . . . ?
C36C C31C C32C C33C -1.8(9) . . . . ?
B1C C31C C32C C33C 171.4(6) . . . . ?
C31C C32C C33C C34C 3.1(10) . . . . ?
C31C C32C C33C C37C -175.7(6) . . . . ?
C32C C33C C34C C35C -1.8(10) . . . . ?
C37C C33C C34C C35C 177.0(6) . . . . ?
C33C C34C C35C C36C -0.6(10) . . . . ?
C33C C34C C35C C38C 179.0(6) . . . . ?
C34C C35C C36C C31C 1.8(10) . . . . ?
C38C C35C C36C C31C -177.8(5) . . . . ?
C32C C31C C36C C35C -0.6(9) . . . . ?
B1C C31C C36C C35C -173.6(6) . . . . ?
C32C C33C C37C F371 -94.8(7) . . . . ?
C34C C33C C37C F371 86.4(7) . . . . ?
C32C C33C C37C F373 26.3(8) . . . . ?
C34C C33C C37C F373 -152.5(6) . . . . ?
C32C C33C C37C F372 144.9(6) . . . . ?
C34C C33C C37C F372 -33.9(8) . . . . ?
C32C C33C C37C F375 49.3(10) . . . . ?
C34C C33C C37C F375 -129.5(9) . . . . ?
C32C C33C C37C F376 172.5(8) . . . . ?
C34C C33C C37C F376 -6.3(10) . . . . ?
C32C C33C C37C F374 -69.8(8) . . . . ?
C34C C33C C37C F374 111.5(8) . . . . ?
C34C C35C C38C F384 98.7(9) . . . . ?
C36C C35C C38C F384 -81.7(9) . . . . ?
C34C C35C C38C F382 -105.1(9) . . . . ?
C36C C35C C38C F382 74.5(9) . . . . ?
C34C C35C C38C F389 176.1(12) . . . . ?
C36C C35C C38C F389 -4.3(13) . . . . ?
C34C C35C C38C F388 -60.0(11) . . . . ?
C36C C35C C38C F388 119.7(10) . . . . ?
C34C C35C C38C F385 -29.6(9) . . . . ?
C36C C35C C38C F385 150.0(8) . . . . ?
C34C C35C C38C F387 54.8(11) . . . . ?
C36C C35C C38C F387 -125.6(10) . . . . ?
C34C C35C C38C F383 20.0(9) . . . . ?
C36C C35C C38C F383 -160.4(8) . . . . ?
C34C C35C C38C F381 133.0(7) . . . . ?
C36C C35C C38C F381 -47.4(8) . . . . ?
C34C C35C C38C F386 -141.8(7) . . . . ?
C36C C35C C38C F386 37.8(8) . . . . ?
C11C B1C C41C C42C -142.1(7) . . . . ?
C21C B1C C41C C42C 96.6(8) . . . . ?
C31C B1C C41C C42C -24.3(9) . . . . ?
C11C B1C C41C C46C 47.6(8) . . . . ?
C21C B1C C41C C46C -73.7(7) . . . . ?
C31C B1C C41C C46C 165.4(5) . . . . ?
C46C C41C C42C C43C -1.1(11) . . . . ?
B1C C41C C42C C43C -171.6(8) . . . . ?
C41C C42C C43C C44C 0.1(15) . . . . ?
C41C C42C C43C C47' 165.5(9) . . . . ?
C41C C42C C43C C47C -166.4(8) . . . . ?
C42C C43C C44C C45C 0.9(15) . . . . ?
C47' C43C C44C C45C -165.1(9) . . . . ?
C47C C43C C44C C45C 166.5(9) . . . . ?
C43C C44C C45C C46C -0.9(13) . . . . ?
C43C C44C C45C C48C 176.8(8) . . . . ?
C44C C45C C46C C41C -0.1(11) . . . . ?
C48C C45C C46C C41C -177.8(6) . . . . ?
C42C C41C C46C C45C 1.1(10) . . . . ?
B1C C41C C46C C45C 172.2(6) . . . . ?
C46C C45C C48C F484 74.4(9) . . . . ?
C44C C45C C48C F484 -103.3(9) . . . . ?
C46C C45C C48C F485 -159.7(7) . . . . ?
C44C C45C C48C F485 22.6(10) . . . . ?
C46C C45C C48C F483 -7.4(10) . . . . ?
C44C C45C C48C F483 174.9(7) . . . . ?
C46C C45C C48C F482 -133.9(7) . . . . ?
C44C C45C C48C F482 48.4(10) . . . . ?
C46C C45C C48C F486 -44.3(9) . . . . ?
C44C C45C C48C F486 138.0(8) . . . . ?
C46C C45C C48C F481 108.5(8) . . . . ?
C44C C45C C48C F481 -69.2(9) . . . . ?
C44C C43C C47C F472 19.5(14) . . . . ?
C42C C43C C47C F472 -174.3(9) . . . . ?
C47' C43C C47C F472 -64.7(14) . . . . ?
C44C C43C C47C F473 -104.7(12) . . . . ?
C42C C43C C47C F473 61.5(12) . . . . ?
C47' C43C C47C F473 171.1(18) . . . . ?
C44C C43C C47C F471 136.7(10) . . . . ?
C42C C43C C47C F471 -57.1(11) . . . . ?
C47' C43C C47C F471 52.5(14) . . . . ?
C44C C43C C47' F474 145.4(10) . . . . ?
C42C C43C C47' F474 -20.4(15) . . . . ?
C47C C43C C47' F474 -104.5(17) . . . . ?
C44C C43C C47' F476 18.4(15) . . . . ?
C42C C43C C47' F476 -147.5(10) . . . . ?
C47C C43C C47' F476 128.5(18) . . . . ?
C44C C43C C47' F475 -97.6(11) . . . . ?
C42C C43C C47' F475 96.5(12) . . . . ?
C47C C43C C47' F475 12.4(13) . . . . ?
Cl1D C1D Cl1D C1D -0.002(10) 5_575 . . 5_575 ?
Cl2D C1D Cl1D C1D -8(5) 5_575 . . 5_575 ?
Cl2D C1D Cl1D C1D 149(18) . . . 5_575 ?
Cl1D C1D Cl2D C1D 10(6) 5_575 . . 5_575 ?
Cl2D C1D Cl2D C1D -0.001(11) 5_575 . . 5_575 ?
Cl1D C1D Cl2D C1D -26(15) . . . 5_575 ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 1.472
_refine_diff_density_min -0.942
_refine_diff_density_rms 0.129
_iucr_refine_instructions_details
;
TITL Chinmin2_C2byc in C2/c
CELL 0.71073 28.8126 12.8881 29.9049 90.000 104.623 90.000
ZERR 8.00 0.0010 0.0004 0.0011 0.000 0.002 0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC C H B N F Cl Rh
UNIT 393 280 8 32 192 10 8
OMIT -2 0 2
OMIT 2 0 0
OMIT 0 0 2
OMIT 1 1 0
OMIT -3 50
L.S. 20
ACTA
BOND $H
FMAP 2
PLAN 20
SADI 0.01 F474 F475 F475 F476 F476 F474
SADI 0.01 C47' F474 C47' F475 C47' F476
SADI 0.01 F471 F472 F472 F473 F473 F471
SADI 0.01 C47C F471 C47C F472 C47C F473
SADI 0.01 F484 F485 F485 F486 F486 F484
SADI 0.01 F481 F482 F482 F483 F483 F481
SADI 0.01 C48C F484 C48C F485 C48C F486
SADI 0.01 C48C F481 C48C F482 C48C F483
SADI 0.01 F387 F388 F388 F389 F389 F387
SADI 0.01 F384 F385 F385 F386 F386 F384
SADI 0.01 F381 F382 F382 F383 F383 F381
SADI 0.01 C38C F387 C38C F388 C38C F389
SADI 0.01 C38C F384 C38C F385 C38C F386
SADI 0.01 C38C F381 C38C F382 C38C F383
SADI 0.01 F374 F375 F375 F376 F376 F374
SADI 0.01 F371 F372 F372 F373 F373 F371
SADI 0.01 C37C F374 C37C F375 C37C F376
SADI 0.01 C37C F371 C37C F372 C37C F373
SADI 0.01 F274 F275 F275 F276 F276 F274
SADI 0.01 F271 F272 F272 F273 F273 F271
SADI 0.01 C27" F274 C27" F275 C27" F276
SADI 0.01 C27C F271 C27C F272 C27C F273
SADI 0.01 F371 F372 F372 F373 F373 F371
SADI 0.01 F374 F375 F375 F376 F376 F374
SADI 0.01 C17C F171 C17C F172 C17C F173
SADI 0.01 C17C F174 C17C F175 C17C F176
SADI 0.01 C17C F177 C17C F178 C17C F179
SADI 0.01 C18C F187 C18C F188 C18C F189
SADI 0.01 C18C F184 C18C F185 C18C F186
SADI 0.01 C18C F181 C18C F182 C18C F183
SADI 0.01 F171 F172 F172 F173 F173 F171
SADI 0.01 F174 F175 F175 F176 F176 F174
SADI 0.01 F177 F178 F178 F179 F179 F177
SADI 0.01 F187 F188 F188 F189 F189 F187
SADI 0.01 F184 F185 F185 F186 F186 F184
SADI 0.01 F181 F182 F182 F183 F183 F181
SADI 0.01 C25C C28C C25C C28'
SADI 0.01 C28C F284 C28C F285 C28C F286
SADI 0.01 C28C F281 C28C F282 C28C F283
SADI 0.01 C28' F287 C28' F288 C28' F289
SADI 0.01 F284 F285 F285 F286 F286 F284
SADI 0.01 F287 F288 F288 F289 F289 F287
SADI 0.01 F281 F282 F282 F283 F283 F281
SADI 0.01 C23C C27C C23C C27"
CONF
SIZE 0.184 0.154 0.053
DFIX 1.78 0.01 C1D CL1D C1D CL2D
DELU 0.01 C47C C47' F471 > F476
DELU 0.01 C48C F481 > F486
DELU 0.01 C38C F381 > F389
DELU 0.01 C37C F371 > F376
DELU 0.01 C28C C28' F281 > F289
DELU 0.01 C27C C27" F271 > 276
DELU 0.01 C18C F181 > F189
TEMP -120.910
WGHT 0.100000 15.000000
FVAR 0.03362
MOLE 1
RH1 7 0.248339 0.873841 0.197951 11.00000 0.02298 0.01970 =
0.02565 0.00062 0.00705 0.00006
N1 4 0.261986 0.930163 0.300065 11.00000 0.06732 0.02034 =
0.02990 0.00040 0.01826 0.00045
N2 4 0.230114 0.896789 0.261247 11.00000 0.04292 0.03183 =
0.03683 -0.00003 0.01864 0.00190
C3 1 0.188817 0.886802 0.272819 11.00000 0.05576 0.04212 =
0.05053 0.00675 0.03066 0.00415
AFIX 43
H3 2 0.159861 0.862864 0.252585 11.00000 -1.20000
AFIX 0
C4 1 0.193558 0.916022 0.318483 11.00000 0.10067 0.03944 =
0.06312 0.01176 0.05752 0.00691
AFIX 43
H4 2 0.169243 0.917094 0.334819 11.00000 -1.20000
AFIX 0
C5 1 0.239927 0.942455 0.334600 11.00000 0.11541 0.04046 =
0.03616 0.00473 0.04123 -0.00038
AFIX 43
H5 2 0.254645 0.965751 0.365014 11.00000 -1.20000
AFIX 0
C1A 1 0.310061 0.959054 0.298068 11.00000 0.06272 0.02717 =
0.02754 -0.00194 0.00012 -0.00399
AFIX 23
H2A 2 0.308308 1.018236 0.276600 11.00000 -1.20000
H1A 2 0.328599 0.981574 0.329092 11.00000 -1.20000
AFIX 0
N1' 4 0.334320 0.873815 0.282767 11.00000 0.04028 0.02791 =
0.03617 0.00383 -0.00557 -0.00126
N2' 4 0.316677 0.831931 0.240325 11.00000 0.03369 0.02282 =
0.03174 0.00695 0.00586 0.00353
C3' 1 0.348205 0.762735 0.235236 11.00000 0.03593 0.03024 =
0.05398 0.01491 0.01621 0.00370
AFIX 43
H3' 2 0.344881 0.720349 0.208623 11.00000 -1.20000
AFIX 0
C4' 1 0.386903 0.759113 0.273422 11.00000 0.03164 0.03516 =
0.06939 0.02647 0.00802 0.00240
AFIX 43
H4' 2 0.414327 0.715643 0.277959 11.00000 -1.20000
AFIX 0
C5' 1 0.377328 0.831343 0.303256 11.00000 0.03914 0.03887 =
0.05273 0.01820 -0.00697 -0.00951
AFIX 43
H5' 2 0.397147 0.848523 0.332834 11.00000 -1.20000
AFIX 0
C1B 1 0.229773 0.874398 0.123227 11.00000 0.02964 0.03331 =
0.02589 -0.00170 0.00300 0.00362
C2B 1 0.272869 0.932030 0.140570 11.00000 0.02568 0.03592 =
0.02569 0.00623 0.00721 0.00552
C3B 1 0.262760 1.016729 0.167895 11.00000 0.03136 0.02301 =
0.02132 0.01036 0.00140 -0.00181
C4B 1 0.212968 1.012940 0.166569 11.00000 0.02815 0.02788 =
0.02562 0.00064 0.00212 0.00595
C5B 1 0.192496 0.923414 0.140146 11.00000 0.02728 0.03101 =
0.03173 -0.00225 0.00132 0.00160
C6B 1 0.222973 0.783090 0.091692 11.00000 0.05404 0.04305 =
0.03616 -0.01206 0.00359 0.00712
AFIX 137
H6A1 2 0.210598 0.806384 0.059699 11.00000 -1.50000
H6A2 2 0.200062 0.734916 0.099781 11.00000 -1.50000
H6A3 2 0.253786 0.747905 0.094851 11.00000 -1.50000
AFIX 0
C7B 1 0.320893 0.909450 0.132027 11.00000 0.02772 0.06135 =
0.03990 0.01046 0.01615 0.00679
AFIX 137
H7A1 2 0.321516 0.837750 0.121283 11.00000 -1.50000
H7A2 2 0.345919 0.918811 0.160771 11.00000 -1.50000
H7A3 2 0.326669 0.957016 0.108438 11.00000 -1.50000
AFIX 0
C8B 1 0.297819 1.100004 0.189303 11.00000 0.05129 0.03997 =
0.03284 0.00696 0.00630 -0.01539
AFIX 137
H8A1 2 0.301649 1.148680 0.165313 11.00000 -1.50000
H8A2 2 0.328884 1.068403 0.203909 11.00000 -1.50000
H8A3 2 0.285800 1.137267 0.212656 11.00000 -1.50000
AFIX 0
C9B 1 0.186589 1.088802 0.188374 11.00000 0.04662 0.03505 =
0.04138 -0.00436 0.01319 0.00826
AFIX 137
H9A1 2 0.207968 1.115305 0.216946 11.00000 -1.50000
H9A2 2 0.158947 1.054581 0.195518 11.00000 -1.50000
H9A3 2 0.175461 1.146540 0.167037 11.00000 -1.50000
AFIX 0
C10B 1 0.141076 0.888904 0.129226 11.00000 0.02110 0.07754 =
0.06125 -0.01762 0.00142 -0.00610
AFIX 137
H10A 2 0.124664 0.910975 0.097860 11.00000 -1.50000
H10B 2 0.125252 0.920092 0.151370 11.00000 -1.50000
H10C 2 0.139756 0.813126 0.131322 11.00000 -1.50000
AFIX 0
CL1 6 0.225669 0.696556 0.199884 11.00000 0.05879 0.02451 =
0.04717 -0.00003 0.01344 -0.01319
MOLE 2
B1C 3 0.410193 0.203016 0.094042 11.00000 0.02839 0.02446 =
0.02776 -0.00678 0.00611 -0.00175
C11C 1 0.424553 0.130469 0.140439 11.00000 0.02270 0.01783 =
0.03475 -0.00280 0.00521 -0.00233
C12C 1 0.420654 0.163803 0.183661 11.00000 0.01766 0.02039 =
0.03244 -0.00365 0.00146 0.00190
AFIX 43
H12C 2 0.411927 0.233831 0.187208 11.00000 -1.20000
AFIX 0
C13C 1 0.429144 0.097726 0.222084 11.00000 0.01711 0.02573 =
0.03297 -0.00273 -0.00025 -0.00554
C14C 1 0.441699 -0.004299 0.218382 11.00000 0.01611 0.03128 =
0.04346 0.00240 0.00233 0.00205
AFIX 43
H14C 2 0.447318 -0.049407 0.244321 11.00000 -1.20000
AFIX 0
C15C 1 0.445931 -0.039512 0.175831 11.00000 0.01595 0.02084 =
0.05529 0.00152 0.00710 -0.00443
C16C 1 0.437639 0.025330 0.137950 11.00000 0.02102 0.02220 =
0.04399 -0.00256 0.00534 -0.00159
AFIX 43
H16C 2 0.440821 -0.001509 0.109287 11.00000 -1.20000
AFIX 0
C17C 1 0.425258 0.137911 0.267422 11.00000 0.02964 0.03229 =
0.03276 0.00311 0.00337 -0.00419
C18C 1 0.460020 -0.149271 0.170098 11.00000 0.03461 0.02558 =
0.06723 0.00211 0.01071 0.00372
PART 1
F171 5 0.408996 0.064460 0.291759 10.50000 0.04761
F172 5 0.466580 0.172537 0.293502 10.50000 0.03392
F173 5 0.393935 0.217449 0.263359 10.50000 0.03255
PART 2
F174 5 0.439845 0.063539 0.301040 10.25000 0.04866
F175 5 0.455951 0.219165 0.281308 10.25000 0.05140
F176 5 0.381467 0.168346 0.269322 10.25000 0.04253
PART 3
F177 5 0.389193 0.091023 0.284015 10.25000 0.03021
F178 5 0.465089 0.130217 0.304031 10.25000 0.03385
F179 5 0.412523 0.242782 0.267414 10.25000 0.04031
PART 1
F181 5 0.436498 -0.191276 0.130558 10.45000 0.06151
F182 5 0.506634 -0.155699 0.171779 10.45000 0.02716
F183 5 0.452709 -0.209734 0.203915 10.45000 0.06320
PART 2
F184 5 0.452519 -0.176772 0.122924 10.35000 0.02745
F185 5 0.506991 -0.171291 0.188144 10.35000 0.03619
F186 5 0.434155 -0.221368 0.186035 10.35000 0.03077
PART 3
F187 5 0.422510 -0.214656 0.157205 10.20000 0.03511
F188 5 0.490422 -0.176298 0.144543 10.20000 0.08811
F189 5 0.482926 -0.187066 0.213641 10.20000 0.04235
PART 0
C21C 1 0.446200 0.183733 0.060077 11.00000 0.04558 0.03142 =
0.03439 -0.01077 0.01736 -0.01644
C22C 1 0.430652 0.213540 0.013449 11.00000 0.07845 0.05754 =
0.04969 -0.01451 0.03408 -0.02907
AFIX 43
H22C 2 0.398992 0.239044 0.001603 11.00000 -1.20000
AFIX 0
C23C 1 0.461647 0.205687 -0.015369 11.00000 0.12430 0.12683 =
0.04473 -0.02363 0.05174 -0.05652
C24C 1 0.508137 0.165921 0.001071 11.00000 0.08885 0.13788 =
0.08948 -0.05169 0.06410 -0.05072
AFIX 43
H24C 2 0.528602 0.157326 -0.019080 11.00000 -1.20000
AFIX 0
C25C 1 0.522917 0.140545 0.045433 11.00000 0.05687 0.10948 =
0.09407 -0.06612 0.04739 -0.03972
C26C 1 0.492806 0.148030 0.075501 11.00000 0.05155 0.04080 =
0.05990 -0.02840 0.02935 -0.01273
AFIX 43
H26C 2 0.504566 0.128298 0.106939 11.00000 -1.20000
PART 1
AFIX 0
C27C 1 0.434560 0.249940 -0.064911 10.60000 0.10142
F271 5 0.392733 0.202135 -0.085238 10.60000 0.09069
F272 5 0.421917 0.350516 -0.068308 10.60000 0.14225
F273 5 0.459764 0.240547 -0.096453 10.60000 0.12581
PART 2
C27" 1 0.451926 0.219137 -0.069613 10.40000 0.15892
F274 5 0.407339 0.248511 -0.079787 10.40000 0.09527
F275 5 0.480616 0.294231 -0.073991 10.40000 0.09870
F276 5 0.459143 0.135169 -0.090959 10.40000 0.08841
C28C 1 0.573258 0.086294 0.068898 10.65000 0.06413
PART 1
F284 5 0.571870 0.004646 0.098986 10.35000 0.09053
F285 5 0.580358 0.044201 0.028123 10.35000 0.04477
F286 5 0.611717 0.149601 0.088688 10.35000 0.11265
PART 2
F281 5 0.584425 0.050578 0.113255 10.30000 0.07207
F282 5 0.592102 0.011917 0.046180 10.30000 0.02209
F283 5 0.605919 0.166329 0.071248 10.30000 0.04770
PART 3
C28' 1 0.579169 0.123577 0.057988 10.35000 0.11102
F287 5 0.585649 0.043565 0.036561 10.35000 0.24555
F288 5 0.601250 0.200325 0.048006 10.35000 0.06377
F289 5 0.588599 0.108721 0.100722 10.35000 0.08017
PART 0
C31C 1 0.355723 0.163508 0.068332 11.00000 0.03605 0.02350 =
0.02162 0.00305 0.00612 -0.00545
C32C 1 0.349169 0.076670 0.039332 11.00000 0.03749 0.02915 =
0.02448 -0.00200 0.00555 -0.00465
AFIX 43
H32C 2 0.376480 0.047700 0.031657 11.00000 -1.20000
AFIX 0
C33C 1 0.305011 0.030785 0.021249 11.00000 0.04182 0.03103 =
0.02951 -0.00215 0.00948 -0.00633
C34C 1 0.263807 0.074682 0.030073 11.00000 0.03813 0.04201 =
0.02684 -0.00073 -0.00146 -0.01144
AFIX 43
H34C 2 0.233054 0.045468 0.017236 11.00000 -1.20000
AFIX 0
C35C 1 0.268960 0.161152 0.057789 11.00000 0.03178 0.02973 =
0.02951 0.00143 -0.00180 0.00265
C36C 1 0.313944 0.204161 0.077146 11.00000 0.03747 0.02735 =
0.02163 0.00044 0.00247 0.00245
AFIX 43
H36C 2 0.316265 0.262732 0.096876 11.00000 -1.20000
AFIX 0
C37C 1 0.302077 -0.068124 -0.007210 11.00000 0.04647 0.08179 =
0.03445 -0.01751 0.00714 -0.03227
C38C 1 0.225404 0.209240 0.066742 11.00000 0.03640 0.04584 =
0.04453 0.00194 0.00033 -0.00671
PART 1
F371 5 0.292572 -0.047786 -0.051134 10.70000 0.06311
F372 5 0.268165 -0.130937 -0.000323 10.70000 0.05154
F373 5 0.341995 -0.123271 0.003351 10.70000 0.05424
PART 2
F374 5 0.312296 -0.043553 -0.048624 10.30000 0.03131
F375 5 0.333997 -0.141329 0.013853 10.30000 0.07085
F376 5 0.257074 -0.109873 -0.017527 10.30000 0.07871
PART 1
F381 5 0.231000 0.230633 0.113075 10.40000 0.02553
F382 5 0.209338 0.296527 0.045598 10.40000 0.06361
F383 5 0.186540 0.144482 0.058818 10.40000 0.07094
PART 2
F384 5 0.214717 0.186626 0.105617 10.40000 0.05826
F385 5 0.185684 0.196150 0.031698 10.40000 0.05537
F386 5 0.229932 0.317556 0.067360 10.40000 0.03792
PART 3
F387 5 0.199661 0.137671 0.084155 10.20000 0.03501
F388 5 0.194352 0.240888 0.027385 10.20000 0.02212
F389 5 0.229912 0.290119 0.095939 10.20000 0.08390
PART 0
C41C 1 0.415627 0.326968 0.106423 11.00000 0.03621 0.02196 =
0.02812 -0.00125 0.00912 0.00205
C42C 1 0.384799 0.403175 0.083779 11.00000 0.04883 0.02521 =
0.04639 -0.00590 -0.00523 -0.00489
AFIX 43
H42C 2 0.356048 0.383263 0.062051 11.00000 -1.20000
AFIX 0
C43C 1 0.394684 0.509218 0.091914 11.00000 0.05921 0.02901 =
0.07723 -0.00202 -0.02406 0.00446
C44C 1 0.436046 0.540470 0.123098 11.00000 0.05616 0.01949 =
0.07632 -0.00668 -0.00920 -0.00426
AFIX 43
H44C 2 0.442582 0.612120 0.128995 11.00000 -1.20000
AFIX 0
C45C 1 0.468135 0.465609 0.145852 11.00000 0.04117 0.02638 =
0.04015 -0.00640 0.00406 -0.00417
C46C 1 0.457912 0.362138 0.137491 11.00000 0.03723 0.02258 =
0.02661 -0.00069 0.00481 0.00352
AFIX 43
H46C 2 0.480357 0.312221 0.153370 11.00000 -1.20000
AFIX 0
C48C 1 0.513639 0.499990 0.177406 11.00000 0.05535 0.02957 =
0.05872 -0.00842 0.00964 -0.00518
PART 1
C47C 1 0.351070 0.585632 0.072488 10.50000 0.05910
F471 5 0.335015 0.572160 0.029002 10.50000 0.06843
F472 5 0.364603 0.679668 0.077970 10.50000 0.07004
F473 5 0.314066 0.576268 0.088289 10.50000 0.11025
PART 2
C47' 1 0.367311 0.591633 0.059556 10.50000 0.06823
F474 5 0.345830 0.557849 0.017577 10.50000 0.07402
F475 5 0.333698 0.619482 0.080575 10.50000 0.16285
F476 5 0.390220 0.678176 0.053924 10.50000 0.10119
PART 1
F481 5 0.543146 0.544441 0.152353 10.50000 0.06032
F482 5 0.509189 0.574018 0.207841 10.50000 0.05199
F483 5 0.541352 0.424844 0.201059 10.50000 0.05640
PART 2
F484 5 0.551934 0.492777 0.161949 10.50000 0.10054
F485 5 0.512653 0.595815 0.193500 10.50000 0.05270
F486 5 0.523061 0.440560 0.216234 10.50000 0.06836
PART 0
MOLE 3
C1D 1 -0.007131 0.979651 0.022672 10.12500 0.05130
CL1D 6 0.045786 0.961464 0.003331 10.12500 0.13155
CL2D 6 0.046425 0.933476 0.010142 10.12500 0.14264
HKLF 4
REM Chinmin2_C2byc in C2/c
REM R1 = 0.0748 for 7065 Fo > 4sig(Fo) and 0.1026 for all 9456 data
REM 759 parameters refined using 124 restraints
END
WGHT 0.1033 144.3870
REM Highest difference peak 1.472, deepest hole -0.942, 1-sigma level 0.129
Q1 1 0.2547 -0.0400 -0.0497 11.00000 0.05 1.47
Q2 1 0.5493 0.4395 0.1799 11.00000 0.05 1.44
Q3 1 0.3781 0.6826 0.0672 11.00000 0.05 1.25
Q4 1 0.4029 0.6609 0.0370 11.00000 0.05 1.19
Q5 1 0.4732 -0.1971 0.2251 11.00000 0.05 1.17
Q6 1 0.0220 0.9474 0.0277 11.00000 0.05 1.15
Q7 1 0.5789 0.0609 0.0851 11.00000 0.05 1.12
Q8 1 0.1895 0.1144 0.0717 11.00000 0.05 1.11
Q9 1 0.3066 0.5494 0.0716 11.00000 0.05 1.11
Q10 1 0.3550 0.6758 0.0973 11.00000 0.05 1.08
Q11 1 0.5635 0.1285 0.0465 11.00000 0.05 0.98
Q12 1 0.1923 0.2041 0.0148 11.00000 0.05 0.94
Q13 1 0.3313 0.6187 0.1032 11.00000 0.05 0.84
Q14 1 0.4587 0.2026 -0.0577 11.00000 0.05 0.84
Q15 1 -0.0256 1.0136 0.0142 11.00000 0.05 0.81
Q16 1 0.5499 0.5192 0.1434 11.00000 0.05 0.80
Q17 1 0.5103 0.4388 0.2327 11.00000 0.05 0.79
Q18 1 0.5758 0.0817 0.0063 11.00000 0.05 0.79
Q19 1 0.5270 0.5993 0.1679 11.00000 0.05 0.77
Q20 1 0.4421 -0.1755 0.1077 11.00000 0.05 0.76
;
#===END