data_0082abc14 #==================================================================== # [{Ir(IBioxMe4)2(H)2}2Cl][BArF4] #-------------------------------------------------------------------- # Collected and solved by Adrian Chaplin #-------------------------------------------------------------------- # Start Validation Reply Form _vrf_PLAT041_0082abc14 ; PROBLEM: Calc. and Reported SumFormula Strings Differ Please Check RESPONSE: The hydride ligands were not located. ; _vrf_PLAT301_0082abc14 ; PROBLEM: Main Residue Disorder ............ Percentage = 13 Note RESPONSE: The structure contains a significant degree of disorder. See _publ_section_exptl_refinement. ; _vrf_PLAT606_0082abc14 ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! Info RESPONSE: Problematic solvent disorder in the solution was treated using the SQUEEZE algorithm. See _platon_squeeze for details. ; # End Validation Reply Form #-------------------------------------------------------------------- _publ_contact_author_name 'Adrian B. Chaplin' _publ_contact_author_email a.b.chaplin@warwick.ac.uk _publ_section_exptl_refinement ; Solved with SHELXT-2014 by direct methods. Refined full-matrix least squares on F2 using SHELXL-2014. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions and refined using the riding model. The hydride ligands were not located. Disorder present in some of the NHC ligands was treated by modelling the appropriate parts over two sites and restraining their geometry. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms or entire CF3 group over two sites and restraining their geometry. Problematic solvent disorder was treated using the SQUEEZE algorithm see _platon_squeeze for details. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; #==================================================================== _audit_creation_date 2015-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C44 H64 Cl Ir2 N8 O8, C32 H12 B F24' _chemical_formula_sum 'C76 H80 B Cl F24 Ir2 N8 O8' _chemical_formula_weight 2120.14 _chemical_absolute_configuration . _chemical_melting_point 'not measured' 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.50552(17) _cell_length_b 22.2205(3) _cell_length_c 30.8469(5) _cell_angle_alpha 90 _cell_angle_beta 98.4554(13) _cell_angle_gamma 90 _cell_volume 9156.5(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 29932 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 31.0960 _cell_measurement_theta_min 3.4060 _shelx_estimated_absorpt_T_max . _shelx_estimated_absorpt_T_min . _exptl_absorpt_coefficient_mu 3.034 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details . _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 4192 _exptl_crystal_recrystallization_method 'Crystals grown from C6H4F2-heptane at 253 K' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_special_details . _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_unetI/netI 0.0461 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 133044 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 27.102 _diffrn_reflns_theta_max 27.102 _diffrn_reflns_theta_min 3.168 _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2833 _diffrn_detector_type Ruby _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -10.00 98.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 22.1076 77.0000 60.0000 108 #__ type_ start__ end____ width___ exp.time_ 2 omega -10.00 98.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 22.1076 77.0000 -180.0000 108 #__ type_ start__ end____ width___ exp.time_ 3 omega -10.00 98.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 22.1076 77.0000 30.0000 108 #__ type_ start__ end____ width___ exp.time_ 4 omega -56.00 53.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - -23.0451 77.0000 -150.0000 109 #__ type_ start__ end____ width___ exp.time_ 5 omega -25.00 63.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 22.1076 -99.0000 -60.0000 88 #__ type_ start__ end____ width___ exp.time_ 6 omega 35.00 111.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 22.1076 178.0000 60.0000 76 #__ type_ start__ end____ width___ exp.time_ 7 omega -52.00 -27.00 1.0000 45.0000 omega____ theta____ kappa____ phi______ frames - 22.1076 -38.0000 60.0000 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction: Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0407434000 _diffrn_orient_matrix_UB_12 0.0203811000 _diffrn_orient_matrix_UB_13 0.0013012000 _diffrn_orient_matrix_UB_21 0.0004198000 _diffrn_orient_matrix_UB_22 -0.0031531000 _diffrn_orient_matrix_UB_23 -0.0228546000 _diffrn_orient_matrix_UB_31 -0.0340332000 _diffrn_orient_matrix_UB_32 0.0243678000 _diffrn_orient_matrix_UB_33 -0.0040539000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 15277 _reflns_number_total 20182 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.555 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.114 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1201 _refine_ls_number_reflns 20182 _refine_ls_number_restraints 708 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0392 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+11.1141P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.1008 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C23A-C30A \\sim C23A-C130 \\sim C29A-C23A \\sim C23A-C129 with sigma of 0.01 O28-C127 \\sim O28-C27 \\sim O25A-C124 \\sim O25A-C24A with sigma of 0.01 C127-C26 \\sim C27-C26 \\sim C23A-C124 \\sim C24A-C23A with sigma of 0.01 C30A-C29A \\sim C130-C129 with sigma of 0.01 C223-F13 \\sim C223-F14 \\sim C223-F15 \\sim C223-F13A \\sim C223-F14A \\sim C223-F15A with sigma of 0.01 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F13A-F14A \\sim F14A-F15A \\sim F15A-F13A with sigma of 0.01 C219-F13 \\sim C219-F14 \\sim C219-F15 \\sim C219-F13A \\sim C219-F14A \\sim C219-F15A with sigma of 0.01 C316-F10A \\sim C316-F11A \\sim C316-F12A \\sim C216-F10 \\sim C216-F11 \\sim C216-F12 with sigma of 0.01 F10A-F11A \\sim F11A-F12A \\sim F12A-F10A \\sim F10-F11 \\sim F11-F12 \\sim F12-F10 with sigma of 0.01 C213-F10A \\sim C213-F11A \\sim C213-F12A \\sim C213-F10 \\sim C213-F11 \\sim C213-F12 with sigma of 0.01 C213-C316 \\sim C213-C216 with sigma of 0.01 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C307-F1A \\sim C307-F2A \\sim C307-F3A with sigma of 0.01 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A with sigma of 0.01 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim C203-F3A with sigma of 0.01 C203-C207 \\sim C203-C307 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints C27 \\sim C127 \\sim C124 \\sim C24A \\sim C30A \\sim C130 \\sim C29A \\sim C129 \\sim C307 \\sim C207 \\sim C316 \\sim C216 \\sim F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F10A \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim F15A \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24: within 1.7A with sigma of 0.007 and sigma for terminal atoms of 0.02 Uanis(C27) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C124) \\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C30A) \\sim Ueq, Uanis(C130) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C307) \\sim Ueq, Uanis(C207) \\sim Ueq, Uanis(C316) \\sim Ueq, Uanis(C216) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F15A) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02 Uanis(C124) = Uanis(C24A) Uanis(C27) = Uanis(C127) Uanis(C30A) = Uanis(C130) Uanis(C29A) = Uanis(C129) Uanis(C316) = Uanis(C216) Uanis(C307) = Uanis(C207) 4. Others Sof(C124)=Sof(H12E)=Sof(H12F)=Sof(C129)=Sof(H12I)=Sof(H12J)=Sof(H12K)= Sof(C130)=Sof(H13A)=Sof(H13B)=Sof(H13C)=1-FVAR(1) Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)= Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=FVAR(1) Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(C316)=1-FVAR(2) Sof(F10)=Sof(F11)=Sof(F12)=Sof(C216)=FVAR(2) Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(C307)=1-FVAR(3) Sof(F1)=Sof(F2)=Sof(F3)=Sof(C207)=FVAR(3) Fixed Sof: C27(0.5) H27A(0.5) H27B(0.5) C127(0.5) H12G(0.5) H12H(0.5) F13(0.5) F13A(0.5) F14(0.5) F14A(0.5) F15(0.5) F15A(0.5) 5.a Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C9A(H9AA,H9AB), C12(H12A,H12B), C12A(H12C,H12D), C24(H24A,H24B), C24A(H24C,H24D), C27(H27A,H27B), C27A(H27C,H27D), C124(H12E,H12F), C127(H12G, H12H) 5.b Aromatic/amide H refined with riding coordinates: C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230) 5.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15(H15A,H15B,H15C), C15A(H15D, H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C29(H29A,H29B,H29C), C29A(H29D,H29E,H29F), C30(H30A,H30B, H30C), C30A(H30D,H30E,H30F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F), C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F), C129(H12I,H12J,H12K), C130(H13A, H13B,H13C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.19375(2) 0.39539(2) 0.47287(2) 0.02424(5) Uani 1 1 d . . . . . Ir1A Ir 0.18896(2) 0.17419(2) 0.46758(2) 0.02711(6) Uani 1 1 d . . . . . Cl2 Cl 0.18694(10) 0.28579(6) 0.46433(5) 0.0464(3) Uani 1 1 d . . . . . O10 O 0.5956(2) 0.39341(19) 0.50101(12) 0.0481(10) Uani 1 1 d . . . . . O10A O 0.5801(2) 0.19642(19) 0.45576(13) 0.0489(10) Uani 1 1 d . . . . . O13 O 0.5101(2) 0.40013(16) 0.60049(11) 0.0387(8) Uani 1 1 d . . . . . O13A O 0.4522(3) 0.17782(19) 0.35238(12) 0.0508(10) Uani 1 1 d . . . . . O25 O -0.1319(2) 0.43080(16) 0.35252(10) 0.0379(8) Uani 1 1 d . . . . . O25A O -0.0816(3) 0.15149(19) 0.57885(12) 0.0509(10) Uani 1 1 d D . . . . O28 O -0.2063(2) 0.40246(17) 0.45261(11) 0.0405(9) Uani 1 1 d D . . . . O28A O -0.2046(3) 0.18358(19) 0.47627(13) 0.0523(10) Uani 1 1 d . . . . . N4 N 0.4252(3) 0.39120(19) 0.48700(13) 0.0323(9) Uani 1 1 d . . . . . N4A N 0.4152(3) 0.18598(17) 0.46323(13) 0.0298(9) Uani 1 1 d . . . . . N7 N 0.3725(3) 0.39603(16) 0.54763(12) 0.0260(8) Uani 1 1 d . . . . . N7A N 0.3372(3) 0.17020(17) 0.40003(13) 0.0309(9) Uani 1 1 d . . . . . N19 N 0.0094(3) 0.41409(16) 0.40144(12) 0.0246(8) Uani 1 1 d . . . . . N19A N 0.0380(3) 0.16053(18) 0.53340(13) 0.0321(9) Uani 1 1 d . . . . . N22 N -0.0359(3) 0.39894(17) 0.46280(12) 0.0278(8) Uani 1 1 d . . . . . N22A N -0.0378(3) 0.18087(18) 0.47074(13) 0.0329(9) Uani 1 1 d . . . . . C3 C 0.3381(3) 0.3933(2) 0.50438(14) 0.0266(10) Uani 1 1 d . . . . . C3A C 0.3200(3) 0.1758(2) 0.44226(15) 0.0266(10) Uani 1 1 d . . . . . C5 C 0.5087(3) 0.3935(2) 0.51847(16) 0.0332(11) Uani 1 1 d . . . . . C5A C 0.4858(3) 0.1875(2) 0.43494(17) 0.0360(12) Uani 1 1 d . . . . . C6 C 0.4760(3) 0.3961(2) 0.55682(15) 0.0293(10) Uani 1 1 d . . . . . C6A C 0.4364(3) 0.1784(2) 0.39486(17) 0.0373(12) Uani 1 1 d . . . . . C8 C 0.4541(4) 0.3934(3) 0.44275(16) 0.0389(12) Uani 1 1 d . . . . . C8A C 0.4652(3) 0.1896(2) 0.50906(16) 0.0328(11) Uani 1 1 d . . . . . C9 C 0.5669(4) 0.3764(4) 0.4550(2) 0.071(2) Uani 1 1 d . . . . . H9A H 0.5765 0.3327 0.4511 0.085 Uiso 1 1 calc R . . . . H9B H 0.6080 0.3984 0.4361 0.085 Uiso 1 1 calc R . . . . C9A C 0.5697(4) 0.2113(3) 0.50064(19) 0.0468(14) Uani 1 1 d . . . . . H9AA H 0.5760 0.2553 0.5053 0.056 Uiso 1 1 calc R . . . . H9AB H 0.6227 0.1911 0.5211 0.056 Uiso 1 1 calc R . . . . C11 C 0.3291(3) 0.4002(2) 0.58878(15) 0.0298(10) Uani 1 1 d . . . . . C11A C 0.2761(4) 0.1648(2) 0.35612(16) 0.0368(12) Uani 1 1 d . . . . . C12 C 0.4247(4) 0.3887(4) 0.62139(19) 0.0644(19) Uani 1 1 d . . . . . H12A H 0.4259 0.4153 0.6472 0.077 Uiso 1 1 calc R . . . . H12B H 0.4258 0.3464 0.6316 0.077 Uiso 1 1 calc R . . . . C12A C 0.3626(4) 0.1496(3) 0.32982(18) 0.0488(14) Uani 1 1 d . . . . . H12C H 0.3719 0.1054 0.3285 0.059 Uiso 1 1 calc R . . . . H12D H 0.3472 0.1652 0.2995 0.059 Uiso 1 1 calc R . . . . C14 C 0.4025(4) 0.3460(3) 0.41255(19) 0.0478(14) Uani 1 1 d . . . . . H14A H 0.4141 0.3063 0.4262 0.072 Uiso 1 1 calc GR . . . . H14B H 0.4293 0.3467 0.3847 0.072 Uiso 1 1 calc GR . . . . H14C H 0.3304 0.3542 0.4071 0.072 Uiso 1 1 calc GR . . . . C14A C 0.4168(4) 0.2358(2) 0.53565(18) 0.0417(13) Uani 1 1 d . . . . . H14D H 0.4116 0.2744 0.5201 0.063 Uiso 1 1 calc GR . . . . H14E H 0.4579 0.2408 0.5644 0.063 Uiso 1 1 calc GR . . . . H14F H 0.3498 0.2220 0.5396 0.063 Uiso 1 1 calc GR . . . . C15 C 0.4346(6) 0.4552(3) 0.4236(2) 0.0667(19) Uani 1 1 d . . . . . H15A H 0.3624 0.4629 0.4186 0.100 Uiso 1 1 calc GR . . . . H15B H 0.4608 0.4578 0.3956 0.100 Uiso 1 1 calc GR . . . . H15C H 0.4679 0.4853 0.4439 0.100 Uiso 1 1 calc GR . . . . C15A C 0.4690(4) 0.1279(2) 0.52950(19) 0.0479(14) Uani 1 1 d . . . . . H15D H 0.4007 0.1139 0.5310 0.072 Uiso 1 1 calc GR . . . . H15E H 0.5068 0.1297 0.5591 0.072 Uiso 1 1 calc GR . . . . H15F H 0.5019 0.0998 0.5116 0.072 Uiso 1 1 calc GR . . . . C16 C 0.2551(4) 0.3509(3) 0.59176(18) 0.0502(15) Uani 1 1 d . . . . . H16A H 0.1972 0.3565 0.5689 0.075 Uiso 1 1 calc GR . . . . H16B H 0.2330 0.3520 0.6206 0.075 Uiso 1 1 calc GR . . . . H16C H 0.2865 0.3120 0.5877 0.075 Uiso 1 1 calc GR . . . . C16A C 0.2302(4) 0.2256(3) 0.34262(19) 0.0479(14) Uani 1 1 d . . . . . H16D H 0.1836 0.2371 0.3627 0.072 Uiso 1 1 calc GR . . . . H16E H 0.1939 0.2230 0.3127 0.072 Uiso 1 1 calc GR . . . . H16F H 0.2833 0.2558 0.3437 0.072 Uiso 1 1 calc GR . . . . C17 C 0.2876(5) 0.4626(3) 0.5933(2) 0.0572(16) Uani 1 1 d . . . . . H17A H 0.3407 0.4924 0.5922 0.086 Uiso 1 1 calc GR . . . . H17B H 0.2624 0.4659 0.6215 0.086 Uiso 1 1 calc GR . . . . H17C H 0.2328 0.4700 0.5694 0.086 Uiso 1 1 calc GR . . . . C17A C 0.2006(4) 0.1149(3) 0.35370(19) 0.0477(14) Uani 1 1 d . . . . . H17D H 0.2345 0.0771 0.3631 0.072 Uiso 1 1 calc GR . . . . H17E H 0.1669 0.1108 0.3235 0.072 Uiso 1 1 calc GR . . . . H17F H 0.1510 0.1243 0.3729 0.072 Uiso 1 1 calc GR . . . . C18 C 0.0487(3) 0.40237(19) 0.44367(14) 0.0243(9) Uani 1 1 d . . . . . C18A C 0.0572(3) 0.1708(2) 0.49206(16) 0.0296(10) Uani 1 1 d . . . . . C20 C -0.0940(3) 0.4179(2) 0.39475(15) 0.0317(11) Uani 1 1 d . . . . . C20A C -0.0628(4) 0.1626(2) 0.53719(18) 0.0376(12) Uani 1 1 d . . . . . C21 C -0.1222(3) 0.4078(2) 0.43353(16) 0.0307(10) Uani 1 1 d . . . . . C21A C -0.1105(3) 0.1758(2) 0.49777(18) 0.0378(12) Uani 1 1 d . . . . . C23 C 0.0471(3) 0.4241(2) 0.35917(14) 0.0292(10) Uani 1 1 d . . . . . C23A C 0.0950(4) 0.1421(2) 0.57593(17) 0.0469(14) Uani 1 1 d D . . . . C24 C -0.0520(4) 0.4133(3) 0.32862(17) 0.0396(12) Uani 1 1 d . . . . . H24A H -0.0543 0.4377 0.3016 0.048 Uiso 1 1 calc R . . . . H24B H -0.0586 0.3703 0.3202 0.048 Uiso 1 1 calc R . . . . C24A C 0.0152(5) 0.1539(5) 0.6057(2) 0.0472(19) Uani 0.685(8) 1 d D U P A 1 H24C H 0.0196 0.1230 0.6290 0.057 Uiso 0.685(8) 1 calc R . P A 1 H24D H 0.0258 0.1939 0.6197 0.057 Uiso 0.685(8) 1 calc R . P A 1 C26 C -0.0605(3) 0.3863(2) 0.50736(15) 0.0292(10) Uani 1 1 d D . . . . C26A C -0.0864(4) 0.1848(2) 0.42470(17) 0.0374(12) Uani 1 1 d . . . . . C27 C -0.1740(5) 0.3729(5) 0.4939(3) 0.0367(18) Uani 0.5 1 d D U P B 1 H27A H -0.1851 0.3290 0.4909 0.044 Uiso 0.5 1 calc R . P B 1 H27B H -0.2124 0.3882 0.5166 0.044 Uiso 0.5 1 calc R . P B 1 C27A C -0.1915(4) 0.2048(3) 0.4331(2) 0.0525(16) Uani 1 1 d . . . . . H27C H -0.1971 0.2492 0.4317 0.063 Uiso 1 1 calc R . . . . H27D H -0.2436 0.1874 0.4107 0.063 Uiso 1 1 calc R . . . . C29 C 0.1250(4) 0.3783(3) 0.35112(18) 0.0489(14) Uani 1 1 d . . . . . H29A H 0.1875 0.3863 0.3707 0.073 Uiso 1 1 calc GR . . . . H29B H 0.1369 0.3809 0.3206 0.073 Uiso 1 1 calc GR . . . . H29C H 0.1011 0.3378 0.3568 0.073 Uiso 1 1 calc GR . . . . C29A C 0.1942(6) 0.1735(5) 0.5888(3) 0.066(3) Uani 0.685(8) 1 d D U P A 1 H29D H 0.2369 0.1666 0.5662 0.099 Uiso 0.685(8) 1 calc GR . P A 1 H29E H 0.2271 0.1575 0.6168 0.099 Uiso 0.685(8) 1 calc GR . P A 1 H29F H 0.1829 0.2168 0.5916 0.099 Uiso 0.685(8) 1 calc GR . P A 1 C30 C 0.0832(4) 0.4884(2) 0.35672(17) 0.0450(13) Uani 1 1 d . . . . . H30A H 0.0281 0.5161 0.3596 0.067 Uiso 1 1 calc GR . . . . H30B H 0.1063 0.4950 0.3285 0.067 Uiso 1 1 calc GR . . . . H30C H 0.1385 0.4957 0.3805 0.067 Uiso 1 1 calc GR . . . . C30A C 0.1129(7) 0.0732(3) 0.5717(3) 0.054(2) Uani 0.685(8) 1 d D U P A 1 H30D H 0.0484 0.0526 0.5648 0.081 Uiso 0.685(8) 1 calc GR . P A 1 H30E H 0.1485 0.0578 0.5995 0.081 Uiso 0.685(8) 1 calc GR . P A 1 H30F H 0.1532 0.0660 0.5483 0.081 Uiso 0.685(8) 1 calc GR . P A 1 C31 C -0.0215(5) 0.3258(2) 0.5232(2) 0.0515(15) Uani 1 1 d . . . . . H31A H -0.0508 0.2947 0.5027 0.077 Uiso 1 1 calc GR . . . . H31B H -0.0398 0.3179 0.5522 0.077 Uiso 1 1 calc GR . . . . H31C H 0.0515 0.3252 0.5250 0.077 Uiso 1 1 calc GR . . . . C31A C -0.0384(4) 0.2310(3) 0.39830(19) 0.0529(16) Uani 1 1 d . . . . . H31D H -0.0336 0.2696 0.4138 0.079 Uiso 1 1 calc GR . . . . H31E H -0.0793 0.2359 0.3695 0.079 Uiso 1 1 calc GR . . . . H31F H 0.0288 0.2174 0.3944 0.079 Uiso 1 1 calc GR . . . . C32 C -0.0222(5) 0.4349(3) 0.53950(19) 0.0554(16) Uani 1 1 d . . . . . H32A H 0.0511 0.4353 0.5435 0.083 Uiso 1 1 calc GR . . . . H32B H -0.0451 0.4270 0.5677 0.083 Uiso 1 1 calc GR . . . . H32C H -0.0477 0.4740 0.5282 0.083 Uiso 1 1 calc GR . . . . C32A C -0.0909(5) 0.1219(3) 0.4050(2) 0.0626(18) Uani 1 1 d . . . . . H32D H -0.0229 0.1077 0.4033 0.094 Uiso 1 1 calc GR . . . . H32E H -0.1296 0.1229 0.3755 0.094 Uiso 1 1 calc GR . . . . H32F H -0.1232 0.0944 0.4235 0.094 Uiso 1 1 calc GR . . . . C124 C 0.0093(7) 0.1269(10) 0.6023(5) 0.0472(19) Uani 0.315(8) 1 d D U P A 2 H12E H 0.0031 0.0828 0.6052 0.057 Uiso 0.315(8) 1 calc R . P A 2 H12F H 0.0232 0.1447 0.6320 0.057 Uiso 0.315(8) 1 calc R . P A 2 C127 C -0.1739(6) 0.4019(5) 0.4994(2) 0.0367(18) Uani 0.5 1 d D U P B 2 H12G H -0.2121 0.3714 0.5135 0.044 Uiso 0.5 1 calc R . P B 2 H12H H -0.1854 0.4417 0.5121 0.044 Uiso 0.5 1 calc R . P B 2 C129 C 0.1373(16) 0.2039(6) 0.5931(7) 0.066(3) Uani 0.315(8) 1 d D U P A 2 H12I H 0.1774 0.2211 0.5722 0.099 Uiso 0.315(8) 1 calc GR . P A 2 H12J H 0.1793 0.1985 0.6215 0.099 Uiso 0.315(8) 1 calc GR . P A 2 H12K H 0.0818 0.2311 0.5964 0.099 Uiso 0.315(8) 1 calc GR . P A 2 C130 C 0.1780(12) 0.0959(7) 0.5806(7) 0.054(2) Uani 0.315(8) 1 d D U P A 2 H13A H 0.1541 0.0591 0.5649 0.081 Uiso 0.315(8) 1 calc GR . P A 2 H13B H 0.1984 0.0867 0.6117 0.081 Uiso 0.315(8) 1 calc GR . P A 2 H13C H 0.2354 0.1119 0.5682 0.081 Uiso 0.315(8) 1 calc GR . P A 2 F1 F 0.3536(5) 0.2513(4) 0.2384(3) 0.100(3) Uani 0.604(7) 1 d D U P C 1 F1A F 0.3726(9) 0.2898(6) 0.1722(3) 0.093(4) Uani 0.396(7) 1 d D U P C 2 F2 F 0.3272(4) 0.3289(3) 0.1995(3) 0.097(3) Uani 0.604(7) 1 d D U P C 1 F2A F 0.4143(8) 0.2168(3) 0.2145(4) 0.097(4) Uani 0.396(7) 1 d D U P C 2 F3 F 0.4015(6) 0.2553(4) 0.1758(3) 0.102(3) Uani 0.604(7) 1 d D U P C 1 F3A F 0.3270(6) 0.2867(6) 0.2351(5) 0.096(4) Uani 0.396(7) 1 d D U P C 2 F4 F 0.5973(3) 0.29302(18) 0.36464(11) 0.0667(11) Uani 1 1 d . U . . . F5 F 0.7451(2) 0.31546(17) 0.35255(10) 0.0589(9) Uani 1 1 d . U . . . F6 F 0.6426(3) 0.38513(18) 0.36212(11) 0.0675(10) Uani 1 1 d . U . . . F7 F 0.7870(3) 0.15049(15) 0.10068(13) 0.0809(13) Uani 1 1 d . U . . . F8 F 0.7707(3) 0.22921(15) 0.06119(10) 0.0562(9) Uani 1 1 d . U . . . F9 F 0.6509(3) 0.20213(17) 0.09324(13) 0.0705(11) Uani 1 1 d . U . . . F10 F 1.0191(8) 0.2753(4) 0.2676(3) 0.100(3) Uani 0.656(13) 1 d D U P D 1 F10A F 1.0229(12) 0.1878(5) 0.2328(5) 0.089(4) Uani 0.344(13) 1 d D U P D 2 F11 F 1.0831(4) 0.2458(5) 0.2124(3) 0.116(3) Uani 0.656(13) 1 d D U P D 1 F11A F 0.9710(12) 0.2501(9) 0.2769(3) 0.098(5) Uani 0.344(13) 1 d D U P D 2 F12 F 0.9943(6) 0.1856(3) 0.2450(3) 0.094(3) Uani 0.656(13) 1 d D U P D 1 F12A F 1.0736(8) 0.2785(8) 0.2351(6) 0.096(4) Uani 0.344(13) 1 d D U P D 2 F13 F 1.0961(6) 0.5585(3) 0.2117(3) 0.079(3) Uani 0.5 1 d D U P E 1 F13A F 1.1029(5) 0.4493(3) 0.2101(4) 0.078(3) Uani 0.5 1 d D U P E 2 F14 F 1.1230(5) 0.4705(5) 0.2349(3) 0.102(4) Uani 0.5 1 d D U P E 1 F14A F 1.0572(7) 0.5191(5) 0.1668(2) 0.090(4) Uani 0.5 1 d D U P E 2 F15 F 1.0654(6) 0.4861(4) 0.1686(2) 0.077(3) Uani 0.5 1 d D U P E 1 F15A F 1.1196(5) 0.5384(4) 0.2322(3) 0.084(4) Uani 0.5 1 d D U P E 2 F16 F 0.8606(3) 0.59584(15) 0.32263(10) 0.0586(9) Uani 1 1 d . U . . . F17 F 0.7811(3) 0.63878(14) 0.26612(11) 0.0583(9) Uani 1 1 d . U . . . F18 F 0.7082(2) 0.57306(16) 0.30015(11) 0.0591(9) Uani 1 1 d . U . . . F19 F 0.8189(3) 0.48993(18) 0.04683(12) 0.0695(10) Uani 1 1 d . U . . . F20 F 0.6824(3) 0.51304(15) 0.00525(11) 0.0638(10) Uani 1 1 d . U . . . F21 F 0.7238(3) 0.42056(15) 0.01645(11) 0.0608(9) Uani 1 1 d . U . . . F22 F 0.4244(3) 0.5531(2) 0.14775(16) 0.1018(17) Uani 1 1 d . U . . . F23 F 0.4039(3) 0.56253(18) 0.07925(15) 0.0842(13) Uani 1 1 d . U . . . F24 F 0.3575(3) 0.48293(18) 0.10708(17) 0.0899(14) Uani 1 1 d . U . . . C201 C 0.6427(3) 0.3693(2) 0.22315(15) 0.0303(10) Uani 1 1 d . . . . . C202 C 0.5524(4) 0.3412(2) 0.20614(18) 0.0410(12) Uani 1 1 d . . . . . H202 H 0.5300 0.3432 0.1755 0.049 Uiso 1 1 calc R . . . . C203 C 0.4949(4) 0.3106(2) 0.23237(18) 0.0489(14) Uani 1 1 d D . . . . C204 C 0.5252(4) 0.3065(3) 0.27722(19) 0.0495(14) Uani 1 1 d . . . . . H204 H 0.4857 0.2853 0.2953 0.059 Uiso 1 1 calc R . . . . C205 C 0.6128(4) 0.3335(2) 0.29505(17) 0.0367(12) Uani 1 1 d . . . . . C206 C 0.6705(3) 0.3645(2) 0.26838(15) 0.0303(10) Uani 1 1 d . . . . . H206 H 0.7310 0.3831 0.2815 0.036 Uiso 1 1 calc R . . . . C207 C 0.3949(6) 0.2868(3) 0.2116(3) 0.0788(18) Uani 0.604(7) 1 d D U P C 1 C208 C 0.6496(4) 0.3315(3) 0.34351(19) 0.0475(14) Uani 1 1 d . . . . . C209 C 0.7787(3) 0.33551(19) 0.17934(15) 0.0270(10) Uani 1 1 d . . . . . C210 C 0.7458(4) 0.2978(2) 0.14424(15) 0.0289(10) Uani 1 1 d . . . . . H210 H 0.6893 0.3096 0.1240 0.035 Uiso 1 1 calc R . . . . C211 C 0.7923(4) 0.2433(2) 0.13750(16) 0.0346(11) Uani 1 1 d . . . . . C212 C 0.8742(4) 0.2243(2) 0.1662(2) 0.0464(14) Uani 1 1 d . . . . . H212 H 0.9063 0.1873 0.1617 0.056 Uiso 1 1 calc R . . . . C213 C 0.9086(4) 0.2609(2) 0.20191(18) 0.0492(15) Uani 1 1 d D . . . . C214 C 0.8615(4) 0.3144(2) 0.20787(17) 0.0376(12) Uani 1 1 d . . . . . H214 H 0.8865 0.3383 0.2326 0.045 Uiso 1 1 calc R . . . . C215 C 0.7506(5) 0.2059(2) 0.0986(2) 0.0459(14) Uani 1 1 d . . . . . C216 C 1.0021(6) 0.2416(3) 0.2317(3) 0.0782(18) Uani 0.656(13) 1 d D U P D 1 C217 C 0.7954(3) 0.44744(19) 0.21430(13) 0.0239(9) Uani 1 1 d . . . . . C218 C 0.8919(3) 0.4542(2) 0.20355(14) 0.0275(10) Uani 1 1 d . . . . . H218 H 0.9149 0.4260 0.1841 0.033 Uiso 1 1 calc R . . . . C219 C 0.9555(3) 0.50052(19) 0.22022(14) 0.0284(10) Uani 1 1 d D . . . . C220 C 0.9247(3) 0.5423(2) 0.24786(15) 0.0298(10) Uani 1 1 d . . . . . H220 H 0.9684 0.5736 0.2598 0.036 Uiso 1 1 calc R . . . . C221 C 0.8290(3) 0.5381(2) 0.25799(14) 0.0271(10) Uani 1 1 d . . . . . C222 C 0.7658(3) 0.4917(2) 0.24176(14) 0.0267(10) Uani 1 1 d . . . . . H222 H 0.7004 0.4899 0.2496 0.032 Uiso 1 1 calc R . . . . C223 C 1.0588(4) 0.50301(19) 0.20808(15) 0.0486(14) Uani 1 1 d D . . . . C224 C 0.7945(4) 0.5861(2) 0.28670(16) 0.0373(12) Uani 1 1 d . . . . . C225 C 0.6611(3) 0.42997(19) 0.14749(14) 0.0278(10) Uani 1 1 d . . . . . C226 C 0.7084(4) 0.4364(2) 0.11001(15) 0.0312(11) Uani 1 1 d . . . . . H226 H 0.7697 0.4159 0.1089 0.037 Uiso 1 1 calc R . . . . C227 C 0.6682(4) 0.4718(2) 0.07461(15) 0.0341(11) Uani 1 1 d . . . . . C228 C 0.5785(4) 0.5017(2) 0.07494(17) 0.0413(13) Uani 1 1 d . . . . . H228 H 0.5514 0.5263 0.0509 0.050 Uiso 1 1 calc R . . . . C229 C 0.5293(4) 0.4952(2) 0.11051(17) 0.0382(12) Uani 1 1 d . . . . . C230 C 0.5709(3) 0.4602(2) 0.14638(16) 0.0339(11) Uani 1 1 d . . . . . H230 H 0.5361 0.4570 0.1709 0.041 Uiso 1 1 calc R . . . . C231 C 0.7223(5) 0.4742(2) 0.03610(18) 0.0480(14) Uani 1 1 d . . . . . C232 C 0.4294(4) 0.5234(3) 0.1110(2) 0.0528(16) Uani 1 1 d . . . . . C307 C 0.4031(7) 0.2759(4) 0.2136(3) 0.0788(18) Uani 0.396(7) 1 d D U P C 2 C316 C 0.9943(8) 0.2439(5) 0.2369(4) 0.0782(18) Uani 0.344(13) 1 d D U P D 2 B200 B 0.7177(4) 0.3959(2) 0.19089(17) 0.0275(11) 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 0.01715(9) 0.03176(10) 0.02371(10) 0.00310(7) 0.00263(6) 0.00190(7) Ir1A 0.02023(9) 0.03069(10) 0.02910(10) 0.00000(8) -0.00076(7) 0.00211(7) Cl2 0.0399(7) 0.0312(6) 0.0671(10) 0.0003(6) 0.0052(6) 0.0051(5) O10 0.0165(17) 0.091(3) 0.037(2) -0.011(2) 0.0030(15) -0.0033(17) O10A 0.0204(18) 0.075(3) 0.050(2) -0.014(2) 0.0003(16) 0.0021(17) O13 0.0284(18) 0.059(2) 0.0269(18) -0.0083(16) -0.0037(14) 0.0049(15) O13A 0.032(2) 0.081(3) 0.040(2) -0.014(2) 0.0084(17) -0.0017(19) O25 0.0239(17) 0.060(2) 0.0276(18) 0.0121(16) -0.0031(14) 0.0062(15) O25A 0.038(2) 0.073(3) 0.044(2) 0.019(2) 0.0141(18) 0.0020(19) O28 0.0190(16) 0.066(3) 0.037(2) 0.0185(17) 0.0057(14) 0.0078(15) O28A 0.0236(19) 0.076(3) 0.056(3) 0.020(2) 0.0034(17) 0.0032(18) N4 0.0175(19) 0.053(3) 0.026(2) 0.0004(18) 0.0024(16) -0.0020(17) N4A 0.022(2) 0.036(2) 0.030(2) -0.0074(17) -0.0017(16) 0.0062(16) N7 0.0219(19) 0.032(2) 0.024(2) -0.0007(16) 0.0018(15) 0.0021(15) N7A 0.022(2) 0.038(2) 0.032(2) -0.0088(18) -0.0014(16) 0.0067(16) N19 0.0188(18) 0.031(2) 0.024(2) 0.0058(16) 0.0025(15) 0.0045(15) N19A 0.025(2) 0.038(2) 0.033(2) 0.0055(18) 0.0045(17) 0.0008(16) N22 0.0172(18) 0.036(2) 0.030(2) 0.0075(17) 0.0028(15) 0.0024(15) N22A 0.022(2) 0.041(2) 0.036(2) 0.0038(18) 0.0051(17) 0.0030(17) C3 0.019(2) 0.036(3) 0.024(2) 0.0008(19) 0.0031(17) -0.0006(18) C3A 0.020(2) 0.029(2) 0.029(2) -0.0011(19) -0.0022(18) 0.0053(17) C5 0.019(2) 0.050(3) 0.030(3) -0.003(2) 0.0007(19) -0.001(2) C5A 0.018(2) 0.046(3) 0.042(3) -0.008(2) 0.001(2) 0.005(2) C6 0.022(2) 0.035(3) 0.028(2) -0.002(2) -0.0030(18) -0.0002(18) C6A 0.023(3) 0.051(3) 0.038(3) -0.008(2) 0.006(2) 0.002(2) C8 0.025(3) 0.064(4) 0.030(3) 0.003(2) 0.010(2) -0.008(2) C8A 0.027(3) 0.032(3) 0.035(3) -0.005(2) -0.008(2) 0.004(2) C9 0.031(3) 0.140(7) 0.044(4) -0.006(4) 0.010(3) -0.003(4) C9A 0.026(3) 0.062(4) 0.050(4) -0.007(3) -0.004(2) -0.001(2) C11 0.032(3) 0.037(3) 0.021(2) -0.0014(19) 0.0031(19) 0.005(2) C11A 0.032(3) 0.050(3) 0.028(3) -0.009(2) 0.000(2) 0.004(2) C12 0.036(3) 0.125(6) 0.032(3) 0.001(3) 0.006(3) -0.001(3) C12A 0.041(3) 0.074(4) 0.031(3) -0.009(3) 0.005(2) 0.003(3) C14 0.049(3) 0.055(4) 0.044(3) -0.006(3) 0.020(3) 0.004(3) C14A 0.036(3) 0.045(3) 0.041(3) -0.010(2) -0.005(2) 0.006(2) C15 0.102(5) 0.058(4) 0.048(4) -0.003(3) 0.036(4) -0.023(4) C15A 0.049(3) 0.042(3) 0.046(3) 0.001(3) -0.019(3) 0.004(2) C16 0.064(4) 0.054(4) 0.037(3) -0.009(3) 0.023(3) -0.019(3) C16A 0.042(3) 0.059(4) 0.039(3) 0.000(3) -0.006(2) 0.009(3) C17 0.087(5) 0.044(3) 0.045(4) -0.005(3) 0.023(3) 0.021(3) C17A 0.042(3) 0.058(4) 0.041(3) -0.015(3) 0.000(2) -0.011(3) C18 0.017(2) 0.029(2) 0.027(2) 0.0038(18) 0.0036(17) 0.0022(17) C18A 0.024(2) 0.033(3) 0.030(3) 0.001(2) -0.0027(19) 0.0025(18) C20 0.022(2) 0.043(3) 0.028(3) 0.009(2) -0.0036(19) 0.005(2) C20A 0.026(3) 0.043(3) 0.045(3) 0.005(2) 0.008(2) 0.001(2) C21 0.017(2) 0.041(3) 0.034(3) 0.008(2) 0.0018(19) 0.0034(18) C21A 0.019(2) 0.048(3) 0.047(3) 0.006(2) 0.008(2) 0.004(2) C23 0.029(2) 0.037(3) 0.022(2) 0.004(2) 0.0033(18) 0.004(2) C23A 0.037(3) 0.067(4) 0.036(3) 0.022(3) 0.003(2) -0.003(3) C24 0.034(3) 0.052(3) 0.032(3) 0.006(2) 0.003(2) 0.005(2) C24A 0.050(3) 0.051(4) 0.041(3) 0.005(3) 0.008(2) 0.005(3) C26 0.019(2) 0.040(3) 0.029(3) 0.007(2) 0.0069(18) 0.0033(19) C26A 0.026(3) 0.051(3) 0.032(3) 0.001(2) -0.006(2) -0.001(2) C27 0.031(3) 0.043(4) 0.036(3) 0.005(3) 0.007(2) 0.005(3) C27A 0.029(3) 0.081(5) 0.047(4) 0.013(3) 0.004(2) 0.003(3) C29 0.047(3) 0.066(4) 0.033(3) 0.002(3) 0.006(2) 0.022(3) C29A 0.043(5) 0.109(7) 0.042(4) 0.017(5) -0.007(4) -0.020(4) C30 0.051(3) 0.052(3) 0.032(3) 0.007(2) 0.007(2) -0.008(3) C30A 0.041(4) 0.062(5) 0.061(5) 0.030(4) 0.014(4) 0.016(4) C31 0.071(4) 0.038(3) 0.051(4) 0.016(3) 0.027(3) 0.007(3) C31A 0.034(3) 0.084(5) 0.037(3) 0.012(3) -0.005(2) 0.000(3) C32 0.082(4) 0.045(3) 0.046(4) -0.004(3) 0.032(3) -0.002(3) C32A 0.048(4) 0.080(5) 0.054(4) -0.013(3) -0.009(3) 0.005(3) C124 0.050(3) 0.051(4) 0.041(3) 0.005(3) 0.008(2) 0.005(3) C127 0.031(3) 0.043(4) 0.036(3) 0.005(3) 0.007(2) 0.005(3) C129 0.043(5) 0.109(7) 0.042(4) 0.017(5) -0.007(4) -0.020(4) C130 0.041(4) 0.062(5) 0.061(5) 0.030(4) 0.014(4) 0.016(4) F1 0.067(5) 0.117(6) 0.106(5) 0.044(5) -0.023(4) -0.060(5) F1A 0.070(6) 0.102(8) 0.094(7) 0.021(6) -0.039(5) -0.045(6) F2 0.054(4) 0.106(5) 0.117(6) -0.001(5) -0.031(4) -0.022(4) F2A 0.072(6) 0.089(6) 0.119(7) -0.019(6) -0.018(6) -0.031(5) F3 0.077(5) 0.107(6) 0.112(6) -0.055(5) -0.016(4) -0.027(5) F3A 0.047(5) 0.113(8) 0.126(8) -0.021(7) 0.007(6) -0.020(6) F4 0.064(2) 0.095(3) 0.043(2) 0.0159(18) 0.0150(17) -0.030(2) F5 0.048(2) 0.092(3) 0.0345(18) 0.0181(17) -0.0024(15) -0.0058(18) F6 0.090(3) 0.078(3) 0.037(2) -0.0119(18) 0.0148(18) -0.009(2) F7 0.140(4) 0.0337(19) 0.062(3) -0.0178(17) -0.008(2) 0.014(2) F8 0.073(2) 0.061(2) 0.0345(18) -0.0113(15) 0.0075(16) 0.0012(17) F9 0.063(2) 0.078(3) 0.070(3) -0.039(2) 0.0101(19) -0.0293(19) F10 0.103(6) 0.073(5) 0.098(5) -0.028(4) -0.070(4) 0.038(4) F10A 0.086(7) 0.059(7) 0.110(8) -0.001(6) -0.021(7) 0.049(6) F11 0.073(4) 0.114(6) 0.145(7) 0.014(6) -0.035(4) 0.023(4) F11A 0.094(8) 0.099(9) 0.088(7) 0.015(7) -0.032(7) 0.031(7) F12 0.115(6) 0.060(4) 0.093(5) 0.017(4) -0.033(5) 0.036(4) F12A 0.058(6) 0.097(8) 0.118(8) 0.011(7) -0.037(6) 0.000(6) F13 0.060(5) 0.075(5) 0.113(8) -0.030(5) 0.044(5) -0.035(4) F13A 0.036(4) 0.057(5) 0.146(8) -0.008(5) 0.032(5) 0.007(3) F14 0.041(5) 0.145(9) 0.119(8) 0.023(7) 0.010(5) 0.012(6) F14A 0.082(6) 0.120(8) 0.080(6) 0.024(6) 0.049(5) -0.009(6) F15 0.061(5) 0.102(7) 0.078(6) -0.054(5) 0.047(4) -0.040(5) F15A 0.035(4) 0.118(8) 0.102(7) -0.055(6) 0.016(4) -0.030(5) F16 0.062(2) 0.072(2) 0.0375(19) -0.0273(16) -0.0052(16) 0.0115(17) F17 0.083(2) 0.0350(18) 0.057(2) -0.0045(16) 0.0131(18) 0.0144(17) F18 0.054(2) 0.063(2) 0.066(2) -0.0301(18) 0.0293(17) -0.0074(17) F19 0.067(2) 0.087(3) 0.054(2) 0.017(2) 0.0068(18) -0.018(2) F20 0.098(3) 0.054(2) 0.0373(19) 0.0205(16) 0.0002(18) 0.0048(19) F21 0.098(3) 0.0443(19) 0.043(2) -0.0033(16) 0.0200(18) -0.0024(18) F22 0.078(3) 0.123(4) 0.096(3) -0.042(3) -0.013(2) 0.059(3) F23 0.065(2) 0.067(3) 0.111(3) 0.028(2) -0.020(2) 0.025(2) F24 0.041(2) 0.062(2) 0.164(4) 0.007(3) 0.004(2) 0.0009(18) C201 0.028(2) 0.033(3) 0.029(3) -0.004(2) 0.0006(19) 0.0012(19) C202 0.039(3) 0.045(3) 0.035(3) -0.004(2) -0.005(2) -0.004(2) C203 0.035(3) 0.062(4) 0.047(4) 0.000(3) 0.000(3) -0.020(3) C204 0.042(3) 0.061(4) 0.047(4) 0.004(3) 0.011(3) -0.019(3) C205 0.031(3) 0.045(3) 0.034(3) 0.001(2) 0.006(2) -0.004(2) C206 0.026(2) 0.038(3) 0.026(3) -0.003(2) 0.0013(19) -0.0042(19) C207 0.065(3) 0.088(3) 0.081(3) 0.004(3) 0.001(3) -0.024(3) C208 0.048(4) 0.059(4) 0.038(3) 0.004(3) 0.014(3) -0.012(3) C209 0.030(2) 0.026(2) 0.023(2) 0.0030(18) 0.0005(19) 0.0009(18) C210 0.033(3) 0.031(3) 0.021(2) 0.0006(19) 0.0003(19) 0.0004(19) C211 0.041(3) 0.030(3) 0.032(3) -0.004(2) 0.004(2) -0.001(2) C212 0.053(3) 0.029(3) 0.057(4) -0.008(2) 0.004(3) 0.010(2) C213 0.051(3) 0.035(3) 0.055(4) 0.001(3) -0.014(3) 0.009(3) C214 0.044(3) 0.033(3) 0.031(3) 0.000(2) -0.010(2) 0.004(2) C215 0.060(4) 0.031(3) 0.047(4) -0.012(2) 0.007(3) -0.004(2) C216 0.078(3) 0.063(3) 0.085(3) -0.004(3) -0.016(3) 0.025(3) C217 0.029(2) 0.026(2) 0.016(2) 0.0023(17) -0.0016(17) 0.0013(17) C218 0.034(3) 0.027(2) 0.022(2) -0.0023(18) 0.0042(19) 0.0041(19) C219 0.028(2) 0.030(2) 0.027(2) 0.0027(19) 0.0040(19) 0.0015(19) C220 0.038(3) 0.026(2) 0.025(2) 0.0022(19) 0.0009(19) -0.0041(19) C221 0.033(2) 0.029(2) 0.019(2) 0.0028(18) 0.0027(18) 0.0046(19) C222 0.027(2) 0.030(2) 0.022(2) 0.0025(19) 0.0011(18) 0.0029(18) C223 0.037(3) 0.051(4) 0.060(4) 0.000(3) 0.014(3) -0.009(3) C224 0.042(3) 0.039(3) 0.031(3) -0.006(2) 0.004(2) 0.002(2) C225 0.034(3) 0.023(2) 0.023(2) -0.0076(18) -0.0067(19) -0.0022(18) C226 0.037(3) 0.023(2) 0.030(3) -0.0025(19) -0.008(2) -0.0004(19) C227 0.051(3) 0.023(2) 0.025(3) -0.0019(19) -0.006(2) -0.008(2) C228 0.056(3) 0.027(3) 0.033(3) 0.002(2) -0.018(2) 0.000(2) C229 0.038(3) 0.030(3) 0.040(3) -0.007(2) -0.016(2) 0.005(2) C230 0.033(3) 0.033(3) 0.033(3) -0.006(2) -0.004(2) 0.001(2) C231 0.071(4) 0.037(3) 0.033(3) 0.011(2) -0.004(3) -0.009(3) C232 0.047(3) 0.043(3) 0.061(4) -0.007(3) -0.016(3) 0.010(3) C307 0.065(3) 0.088(3) 0.081(3) 0.004(3) 0.001(3) -0.024(3) C316 0.078(3) 0.063(3) 0.085(3) -0.004(3) -0.016(3) 0.025(3) B200 0.032(3) 0.027(3) 0.022(3) -0.003(2) -0.001(2) 0.002(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 Ir1 Cl2 2.4499(13) . ? Ir1 C3 2.047(4) . ? Ir1 C18 2.038(4) . ? Ir1A Cl2 2.4817(13) . ? Ir1A C3A 2.038(4) . ? Ir1A C18A 2.034(5) . ? O10 C5 1.361(6) . ? O10 C9 1.466(7) . ? O10A C5A 1.354(6) . ? O10A C9A 1.450(7) . ? O13 C6 1.361(5) . ? O13 C12 1.424(6) . ? O13A C6A 1.358(6) . ? O13A C12A 1.448(6) . ? O25 C20 1.358(5) . ? O25 C24 1.447(6) . ? O25A C20A 1.368(6) . ? O25A C24A 1.441(7) . ? O25A C124 1.438(9) . ? O28 C21 1.360(5) . ? O28 C27 1.444(7) . ? O28 C127 1.446(7) . ? O28A C21A 1.355(6) . ? O28A C27A 1.447(7) . ? N4 C3 1.363(5) . ? N4 C5 1.377(6) . ? N4 C8 1.475(6) . ? N4A C3A 1.370(6) . ? N4A C5A 1.385(6) . ? N4A C8A 1.477(6) . ? N7 C3 1.348(6) . ? N7 C6 1.385(6) . ? N7 C11 1.478(6) . ? N7A C3A 1.362(6) . ? N7A C6A 1.384(6) . ? N7A C11A 1.484(6) . ? N19 C18 1.358(5) . ? N19 C20 1.384(6) . ? N19 C23 1.485(5) . ? N19A C18A 1.357(6) . ? N19A C20A 1.385(6) . ? N19A C23A 1.478(6) . ? N22 C18 1.362(5) . ? N22 C21 1.380(6) . ? N22 C26 1.488(6) . ? N22A C18A 1.372(6) . ? N22A C21A 1.383(6) . ? N22A C26A 1.477(6) . ? C5 C6 1.324(7) . ? C5A C6A 1.331(7) . ? C8 C9 1.560(8) . ? C8 C14 1.508(7) . ? C8 C15 1.503(8) . ? C8A C9A 1.549(7) . ? C8A C14A 1.521(7) . ? C8A C15A 1.508(7) . ? C11 C12 1.538(7) . ? C11 C16 1.494(7) . ? C11 C17 1.509(7) . ? C11A C12A 1.554(7) . ? C11A C16A 1.519(7) . ? C11A C17A 1.501(7) . ? C20 C21 1.326(6) . ? C20A C21A 1.322(7) . ? C23 C24 1.538(7) . ? C23 C29 1.511(7) . ? C23 C30 1.514(7) . ? C23A C24A 1.537(7) . ? C23A C29A 1.510(7) . ? C23A C30A 1.557(8) . ? C23A C124 1.546(9) . ? C23A C129 1.550(9) . ? C23A C130 1.511(9) . ? C26 C27 1.556(8) . ? C26 C31 1.499(7) . ? C26 C32 1.505(7) . ? C26 C127 1.554(8) . ? C26A C27A 1.546(7) . ? C26A C31A 1.515(8) . ? C26A C32A 1.522(8) . ? F1 C207 1.323(7) . ? F1A C307 1.318(7) . ? F2 C207 1.323(7) . ? F2A C307 1.321(7) . ? F3 C207 1.321(7) . ? F3A C307 1.324(7) . ? F4 C208 1.338(6) . ? F5 C208 1.328(7) . ? F6 C208 1.331(7) . ? F7 C215 1.323(6) . ? F8 C215 1.330(7) . ? F9 C215 1.335(7) . ? F10 C216 1.328(7) . ? F10A C316 1.317(7) . ? F11 C216 1.323(7) . ? F11A C316 1.325(7) . ? F12 C216 1.319(7) . ? F12A C316 1.326(7) . ? F13 C223 1.330(6) . ? F13A C223 1.332(6) . ? F14 C223 1.322(6) . ? F14A C223 1.320(6) . ? F15 C223 1.291(6) . ? F15A C223 1.292(6) . ? F16 C224 1.335(6) . ? F17 C224 1.332(6) . ? F18 C224 1.325(6) . ? F19 C231 1.345(7) . ? F20 C231 1.339(6) . ? F21 C231 1.338(6) . ? F22 C232 1.324(7) . ? F23 C232 1.317(7) . ? F24 C232 1.315(7) . ? C201 C202 1.402(7) . ? C201 C206 1.395(6) . ? C201 B200 1.631(7) . ? C202 C203 1.379(7) . ? C203 C204 1.387(8) . ? C203 C207 1.504(10) . ? C203 C307 1.504(11) . ? C204 C205 1.368(7) . ? C205 C206 1.396(6) . ? C205 C208 1.505(8) . ? C209 C210 1.390(6) . ? C209 C214 1.398(6) . ? C209 B200 1.641(7) . ? C210 C211 1.393(6) . ? C211 C212 1.377(7) . ? C211 C215 1.499(7) . ? C212 C213 1.393(7) . ? C213 C214 1.373(7) . ? C213 C216 1.511(9) . ? C213 C316 1.510(11) . ? C217 C218 1.400(6) . ? C217 C222 1.393(6) . ? C217 B200 1.646(7) . ? C218 C219 1.390(6) . ? C219 C220 1.367(6) . ? C219 C223 1.497(7) . ? C220 C221 1.377(6) . ? C221 C222 1.385(6) . ? C221 C224 1.502(6) . ? C225 C226 1.408(7) . ? C225 C230 1.386(6) . ? C225 B200 1.628(7) . ? C226 C227 1.390(6) . ? C227 C228 1.383(7) . ? C227 C231 1.484(8) . ? C228 C229 1.371(8) . ? C229 C230 1.402(7) . ? C229 C232 1.489(7) . ? 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 C3 Ir1 Cl2 92.66(13) . . ? C18 Ir1 Cl2 90.55(12) . . ? C18 Ir1 C3 176.35(18) . . ? C3A Ir1A Cl2 88.42(13) . . ? C18A Ir1A Cl2 92.72(13) . . ? C18A Ir1A C3A 178.62(19) . . ? Ir1 Cl2 Ir1A 171.47(7) . . ? C5 O10 C9 105.3(4) . . ? C5A O10A C9A 105.7(4) . . ? C6 O13 C12 104.9(4) . . ? C6A O13A C12A 103.3(4) . . ? C20 O25 C24 103.2(3) . . ? C20A O25A C24A 104.8(4) . . ? C20A O25A C124 106.2(6) . . ? C21 O28 C27 104.9(4) . . ? C21 O28 C127 106.5(4) . . ? C21A O28A C27A 105.1(4) . . ? C3 N4 C5 112.7(4) . . ? C3 N4 C8 136.4(4) . . ? C5 N4 C8 110.5(4) . . ? C3A N4A C5A 113.1(4) . . ? C3A N4A C8A 136.6(4) . . ? C5A N4A C8A 109.9(4) . . ? C3 N7 C6 113.1(4) . . ? C3 N7 C11 137.0(4) . . ? C6 N7 C11 109.9(4) . . ? C3A N7A C6A 113.7(4) . . ? C3A N7A C11A 136.9(4) . . ? C6A N7A C11A 108.9(4) . . ? C18 N19 C20 113.5(4) . . ? C18 N19 C23 137.3(4) . . ? C20 N19 C23 109.2(3) . . ? C18A N19A C20A 113.6(4) . . ? C18A N19A C23A 137.2(4) . . ? C20A N19A C23A 108.9(4) . . ? C18 N22 C21 113.0(4) . . ? C18 N22 C26 136.6(4) . . ? C21 N22 C26 110.4(3) . . ? C18A N22A C21A 113.2(4) . . ? C18A N22A C26A 136.3(4) . . ? C21A N22A C26A 109.3(4) . . ? N4 C3 Ir1 129.1(3) . . ? N7 C3 Ir1 129.3(3) . . ? N7 C3 N4 101.5(4) . . ? N4A C3A Ir1A 129.0(3) . . ? N7A C3A Ir1A 130.2(3) . . ? N7A C3A N4A 100.8(4) . . ? O10 C5 N4 112.7(4) . . ? C6 C5 O10 140.8(4) . . ? C6 C5 N4 106.5(4) . . ? O10A C5A N4A 113.1(4) . . ? C6A C5A O10A 140.4(5) . . ? C6A C5A N4A 106.5(4) . . ? O13 C6 N7 112.8(4) . . ? C5 C6 O13 141.1(4) . . ? C5 C6 N7 106.1(4) . . ? O13A C6A N7A 113.7(4) . . ? C5A C6A O13A 140.3(5) . . ? C5A C6A N7A 105.9(4) . . ? N4 C8 C9 98.6(4) . . ? N4 C8 C14 112.8(4) . . ? N4 C8 C15 109.9(4) . . ? C14 C8 C9 109.1(5) . . ? C15 C8 C9 115.2(5) . . ? C15 C8 C14 110.9(5) . . ? N4A C8A C9A 99.0(4) . . ? N4A C8A C14A 112.4(4) . . ? N4A C8A C15A 109.4(4) . . ? C14A C8A C9A 110.8(4) . . ? C15A C8A C9A 112.2(4) . . ? C15A C8A C14A 112.3(5) . . ? O10 C9 C8 106.3(5) . . ? O10A C9A C8A 107.9(4) . . ? N7 C11 C12 98.6(4) . . ? N7 C11 C16 111.1(4) . . ? N7 C11 C17 109.7(4) . . ? C16 C11 C12 110.0(5) . . ? C16 C11 C17 114.0(5) . . ? C17 C11 C12 112.3(5) . . ? N7A C11A C12A 97.7(4) . . ? N7A C11A C16A 109.2(4) . . ? N7A C11A C17A 112.8(4) . . ? C16A C11A C12A 111.0(5) . . ? C17A C11A C12A 111.8(4) . . ? C17A C11A C16A 113.3(5) . . ? O13 C12 C11 109.4(4) . . ? O13A C12A C11A 107.1(4) . . ? N19 C18 Ir1 130.8(3) . . ? N19 C18 N22 101.0(3) . . ? N22 C18 Ir1 128.1(3) . . ? N19A C18A Ir1A 130.8(3) . . ? N19A C18A N22A 100.5(4) . . ? N22A C18A Ir1A 128.6(4) . . ? O25 C20 N19 112.7(4) . . ? C21 C20 O25 141.5(4) . . ? C21 C20 N19 105.8(4) . . ? O25A C20A N19A 113.1(4) . . ? C21A C20A O25A 140.5(5) . . ? C21A C20A N19A 106.4(4) . . ? O28 C21 N22 112.6(4) . . ? C20 C21 O28 140.7(4) . . ? C20 C21 N22 106.7(4) . . ? O28A C21A N22A 113.1(5) . . ? C20A C21A O28A 140.6(5) . . ? C20A C21A N22A 106.3(4) . . ? N19 C23 C24 97.7(3) . . ? N19 C23 C29 112.3(4) . . ? N19 C23 C30 109.9(4) . . ? C29 C23 C24 111.0(4) . . ? C29 C23 C30 113.0(4) . . ? C30 C23 C24 112.0(4) . . ? N19A C23A C24A 99.4(4) . . ? N19A C23A C29A 115.5(5) . . ? N19A C23A C30A 105.4(5) . . ? N19A C23A C124 101.3(5) . . ? N19A C23A C129 100.1(8) . . ? N19A C23A C130 123.7(9) . . ? C24A C23A C30A 110.4(6) . . ? C29A C23A C24A 115.9(6) . . ? C29A C23A C30A 109.4(7) . . ? C124 C23A C129 106.3(12) . . ? C130 C23A C124 113.8(9) . . ? C130 C23A C129 109.8(9) . . ? O25 C24 C23 107.0(4) . . ? O25A C24A C23A 107.9(5) . . ? N22 C26 C27 97.8(4) . . ? N22 C26 C31 110.7(4) . . ? N22 C26 C32 111.8(4) . . ? N22 C26 C127 99.3(4) . . ? C31 C26 C27 101.5(5) . . ? C31 C26 C32 111.0(5) . . ? C31 C26 C127 122.8(6) . . ? C32 C26 C27 122.8(6) . . ? C32 C26 C127 100.3(5) . . ? N22A C26A C27A 98.3(4) . . ? N22A C26A C31A 113.1(4) . . ? N22A C26A C32A 108.5(4) . . ? C31A C26A C27A 111.8(5) . . ? C31A C26A C32A 113.8(5) . . ? C32A C26A C27A 110.3(5) . . ? O28 C27 C26 107.9(5) . . ? O28A C27A C26A 107.4(4) . . ? O25A C124 C23A 107.6(7) . . ? O28 C127 C26 107.8(5) . . ? C202 C201 B200 121.2(4) . . ? C206 C201 C202 115.6(4) . . ? C206 C201 B200 122.5(4) . . ? C203 C202 C201 122.2(5) . . ? C202 C203 C204 120.6(5) . . ? C202 C203 C207 118.1(5) . . ? C202 C203 C307 122.0(5) . . ? C204 C203 C207 121.0(5) . . ? C204 C203 C307 117.1(5) . . ? C205 C204 C203 118.8(5) . . ? C204 C205 C206 120.3(5) . . ? C204 C205 C208 121.7(5) . . ? C206 C205 C208 117.9(4) . . ? C201 C206 C205 122.4(4) . . ? F1 C207 C203 112.3(6) . . ? F2 C207 F1 105.1(6) . . ? F2 C207 C203 114.3(6) . . ? F3 C207 F1 106.9(7) . . ? F3 C207 F2 105.5(7) . . ? F3 C207 C203 112.1(6) . . ? F4 C208 C205 112.5(5) . . ? F5 C208 F4 106.9(5) . . ? F5 C208 F6 106.2(5) . . ? F5 C208 C205 112.7(4) . . ? F6 C208 F4 106.6(5) . . ? F6 C208 C205 111.6(5) . . ? C210 C209 C214 115.0(4) . . ? C210 C209 B200 123.3(4) . . ? C214 C209 B200 121.2(4) . . ? C209 C210 C211 122.8(4) . . ? C210 C211 C215 118.4(5) . . ? C212 C211 C210 120.5(4) . . ? C212 C211 C215 121.1(5) . . ? C211 C212 C213 118.2(5) . . ? C212 C213 C216 117.9(5) . . ? C212 C213 C316 123.4(6) . . ? C214 C213 C212 120.3(5) . . ? C214 C213 C216 121.7(5) . . ? C214 C213 C316 116.2(6) . . ? C213 C214 C209 123.3(5) . . ? F7 C215 F8 106.4(5) . . ? F7 C215 F9 108.0(5) . . ? F7 C215 C211 112.6(5) . . ? F8 C215 F9 104.3(5) . . ? F8 C215 C211 112.2(4) . . ? F9 C215 C211 112.8(5) . . ? F10 C216 C213 112.0(6) . . ? F11 C216 F10 106.5(6) . . ? F11 C216 C213 112.2(6) . . ? F12 C216 F10 106.6(6) . . ? F12 C216 F11 108.3(6) . . ? F12 C216 C213 111.0(6) . . ? C218 C217 B200 121.8(4) . . ? C222 C217 C218 115.4(4) . . ? C222 C217 B200 122.4(4) . . ? C219 C218 C217 122.5(4) . . ? C218 C219 C223 118.8(4) . . ? C220 C219 C218 120.4(4) . . ? C220 C219 C223 120.7(4) . . ? C219 C220 C221 118.5(4) . . ? C220 C221 C222 121.1(4) . . ? C220 C221 C224 117.9(4) . . ? C222 C221 C224 120.9(4) . . ? C221 C222 C217 122.0(4) . . ? F13 C223 C219 111.6(5) . . ? F13A C223 C219 112.5(4) . . ? F14 C223 F13 104.4(5) . . ? F14 C223 C219 111.9(5) . . ? F14A C223 F13A 103.4(5) . . ? F14A C223 C219 111.6(5) . . ? F15 C223 F13 105.7(5) . . ? F15 C223 F14 107.5(5) . . ? F15 C223 C219 115.0(5) . . ? F15A C223 F13A 106.1(5) . . ? F15A C223 F14A 108.0(5) . . ? F15A C223 C219 114.5(5) . . ? F16 C224 C221 112.2(4) . . ? F17 C224 F16 106.2(4) . . ? F17 C224 C221 112.0(4) . . ? F18 C224 F16 106.7(4) . . ? F18 C224 F17 106.1(4) . . ? F18 C224 C221 113.2(4) . . ? C226 C225 B200 120.5(4) . . ? C230 C225 C226 115.7(4) . . ? C230 C225 B200 123.4(4) . . ? C227 C226 C225 122.0(5) . . ? C226 C227 C231 117.8(5) . . ? C228 C227 C226 120.5(5) . . ? C228 C227 C231 121.6(5) . . ? C229 C228 C227 118.9(5) . . ? C228 C229 C230 120.3(5) . . ? C228 C229 C232 120.6(5) . . ? C230 C229 C232 119.0(5) . . ? C225 C230 C229 122.5(5) . . ? F19 C231 C227 112.7(5) . . ? F20 C231 F19 106.4(4) . . ? F20 C231 C227 113.4(5) . . ? F21 C231 F19 105.4(5) . . ? F21 C231 F20 106.5(4) . . ? F21 C231 C227 111.9(4) . . ? F22 C232 C229 112.3(5) . . ? F23 C232 F22 105.4(5) . . ? F23 C232 C229 114.2(6) . . ? F24 C232 F22 106.8(6) . . ? F24 C232 F23 105.9(5) . . ? F24 C232 C229 111.7(5) . . ? F1A C307 F2A 105.7(7) . . ? F1A C307 F3A 106.8(7) . . ? F1A C307 C203 112.1(7) . . ? F2A C307 F3A 105.3(7) . . ? F2A C307 C203 114.6(7) . . ? F3A C307 C203 111.7(7) . . ? F10A C316 F11A 107.5(7) . . ? F10A C316 F12A 107.2(7) . . ? F10A C316 C213 111.9(7) . . ? F11A C316 F12A 106.5(7) . . ? F11A C316 C213 112.2(7) . . ? F12A C316 C213 111.4(7) . . ? C201 B200 C209 102.3(4) . . ? C201 B200 C217 113.4(4) . . ? C209 B200 C217 110.9(4) . . ? C225 B200 C201 114.3(4) . . ? C225 B200 C209 113.1(4) . . ? C225 B200 C217 103.3(4) . . ? # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 26 6 ' ' 2 0.000 0.000 0.500 26 6 ' ' 3 0.354 0.564 0.264 281 69 ' ' 4 0.354 0.936 0.764 281 69 ' ' 5 0.646 1.064 0.236 281 69 ' ' 6 0.646 0.436 0.736 281 70 ' ' # Missing Reflections Below sin(th)/lambda=0.3 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 7.903 2 0 0 11.213 1 1 0 8.542 2 1 0 11.461 0 2 0 8.672 1 2 0 9.901 1 3 0 11.388 -2 1 1 11.417 -1 1 1 8.639 0 1 1 6.810 1 1 1 9.009 -1 2 1 9.965 0 2 1 8.948 1 2 1 10.214 0 3 1 10.797 -2 0 2 11.388 -1 0 2 8.766 0 0 2 7.393 1 0 2 9.440 -1 1 2 9.254 0 1 2 8.147 1 1 2 9.839 -1 2 2 10.386 0 2 2 9.654 1 2 2 10.817 0 3 2 11.227 -1 1 3 10.152 0 1 3 9.512 1 1 3 10.819 -1 2 3 11.057 0 2 3 10.573 1 2 3 11.590 -1 0 4 10.881 0 0 4 10.484 -1 1 4 11.151 0 1 4 10.784 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ; ) TITL 0082abc14 CELL 13.5055 22.2206 30.8469 90.00 98.46 90.00 SPGR P21/c # Solvent Accessible Volume = 1177.7 # Electrons Found in S.A.V. = 284.5 # Note: Atoms in Void as Cxxx and Qxxx all others C101 0.639 0.937 0.202 ! 6.64 eA-3 C102 0.705 0.329 0.756 ! 5.64 eA-3 C103 0.280 0.669 0.201 ! 5.42 eA-3 C104 0.240 0.815 0.703 ! 5.25 eA-3 C105 0.281 0.827 0.706 ! 4.81 eA-3 C106 0.690 0.553 0.701 ! 4.74 eA-3 C107 0.413 0.023 0.765 ! 4.66 eA-3 C108 0.578 0.946 0.236 ! 4.60 eA-3 C109 0.300 0.795 0.752 ! 4.58 eA-3 C110 0.671 0.905 0.215 ! 4.41 eA-3 C111 0.447 0.970 0.761 ! 4.41 eA-3 C112 0.393 0.045 0.774 ! 4.36 eA-3 C113 0.612 0.469 0.711 ! 4.29 eA-3 C114 0.347 0.933 0.757 ! 4.29 eA-3 C115 0.407 0.634 0.256 ! 4.28 eA-3 Q116 0.816 0.794 0.536 ! 4.25 eA-3 C117 0.465 0.493 0.259 ! 4.24 eA-3 C118 0.277 0.829 0.757 ! 4.19 eA-3 C119 0.356 0.006 0.804 ! 4.19 eA-3 C120 0.612 0.064 0.222 ! 4.17 eA-3 C121 0.411 0.868 0.759 ! 4.15 eA-3 C122 0.326 0.676 0.255 ! 4.12 eA-3 C123 0.608 0.177 0.233 ! 4.12 eA-3 C124 0.374 0.602 0.255 ! 4.11 eA-3 C125 0.348 0.531 0.302 ! 3.98 eA-3 C126 0.439 0.601 0.258 ! 3.87 eA-3 C127 0.392 0.907 0.764 ! 3.83 eA-3 C128 0.635 0.409 0.726 ! 3.81 eA-3 C129 0.655 0.522 0.712 ! 3.68 eA-3 C130 0.346 0.969 0.806 ! 3.64 eA-3 C131 0.598 0.500 0.706 ! 3.58 eA-3 C132 0.646 0.310 0.759 ! 3.57 eA-3 C133 0.354 0.918 0.782 ! 3.53 eA-3 C134 0.596 0.572 0.711 ! 3.41 eA-3 Q135 0.422 0.656 0.268 ! 3.41 eA-3 C136 0.766 0.288 0.793 ! 3.39 eA-3 C137 0.364 0.016 0.773 ! 3.37 eA-3 C138 0.481 0.945 0.751 ! 3.34 eA-3 C139 0.541 0.515 0.727 ! 3.28 eA-3 C140 0.440 0.929 0.762 ! 3.26 eA-3 C141 0.390 0.086 0.797 ! 3.13 eA-3 C142 0.324 0.560 0.297 ! 3.12 eA-3 C143 0.347 0.071 0.815 ! 3.06 eA-3 C144 0.276 0.809 0.726 ! 3.05 eA-3 C145 0.607 0.413 0.753 ! 3.05 eA-3 C146 0.402 0.055 0.796 ! 2.99 eA-3 C147 0.370 0.859 0.767 ! 2.97 eA-3 C148 0.375 0.834 0.751 ! 2.95 eA-3 C149 0.308 0.861 0.768 ! 2.91 eA-3 C150 0.703 0.149 0.290 ! 2.90 eA-3 C151 0.692 0.345 0.719 ! 2.82 eA-3 C152 0.637 0.392 0.702 ! 2.81 eA-3 C153 0.564 0.051 0.224 ! 2.80 eA-3 C154 0.754 0.307 0.760 ! 2.76 eA-3 C155 0.302 0.703 0.274 ! 2.75 eA-3 C156 0.651 0.208 0.226 ! 2.72 eA-3 C157 0.599 0.115 0.272 ! 2.71 eA-3 C158 0.439 0.013 0.789 ! 2.68 eA-3 C159 0.639 0.350 0.718 ! 2.68 eA-3 C160 0.503 0.517 0.240 ! 2.65 eA-3 C161 0.685 0.343 0.796 ! 2.64 eA-3 C162 0.421 0.039 0.741 ! 2.63 eA-3 C163 0.640 0.374 0.759 ! 2.62 eA-3 C164 0.735 0.443 0.656 ! 2.57 eA-3 C165 0.297 0.469 0.305 ! 2.54 eA-3 C166 0.578 0.515 0.753 ! 2.54 eA-3 C167 0.369 0.875 0.785 ! 2.53 eA-3 Q168 0.829 0.922 0.026 ! 2.44 eA-3 Q169 0.216 0.770 0.721 ! 2.42 eA-3 C170 0.549 0.572 0.765 ! 2.41 eA-3 C171 0.464 0.471 0.278 ! 2.41 eA-3 C172 0.614 0.044 0.242 ! 2.38 eA-3 Q173 0.158 0.689 0.205 ! 2.32 eA-3 Q174 0.433 0.131 0.281 ! 2.32 eA-3 C175 0.693 0.394 0.720 ! 2.31 eA-3 Q176 0.222 0.912 0.845 ! 2.31 eA-3 Q177 0.228 0.411 0.304 ! 2.29 eA-3 C178 0.719 0.219 0.272 ! 2.27 eA-3 C179 0.320 0.632 0.289 ! 2.26 eA-3 C180 0.319 0.867 0.790 ! 2.26 eA-3 C181 0.331 0.978 0.788 ! 2.26 eA-3 C182 0.224 0.378 0.282 ! 2.24 eA-3 C183 0.327 0.683 0.202 ! 2.23 eA-3 C184 0.295 0.408 0.312 ! 2.21 eA-3 C185 0.422 0.016 0.806 ! 2.20 eA-3 Q186 0.169 0.078 0.974 ! 2.20 eA-3 C187 0.407 0.076 0.773 ! 2.15 eA-3 C188 0.709 0.163 0.314 ! 2.13 eA-3 C189 0.467 0.579 0.283 ! 2.12 eA-3 C190 0.533 0.116 0.274 ! 2.12 eA-3 C191 0.362 0.813 0.783 ! 2.11 eA-3 Q192 0.192 0.592 0.164 ! 2.11 eA-3 Q193 0.721 0.273 0.706 ! 2.08 eA-3 Q194 0.051 0.928 0.530 ! 2.08 eA-3 C195 0.346 0.017 0.749 ! 2.08 eA-3 C196 0.420 0.543 0.235 ! 2.06 eA-3 Q197 0.238 0.742 0.703 ! 2.06 eA-3 C198 0.653 0.498 0.719 ! 2.06 eA-3 C199 0.369 0.015 0.729 ! 2.05 eA-3 ) ; _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_0068abc14 #==================================================================== # [Ir(IBioxMe4)2(Bipy)(H)2][BArF4] #-------------------------------------------------------------------- # Collected and solved by Adrian Chaplin #-------------------------------------------------------------------- # Start Validation Reply Form _vrf_PLAT301_0068abc14 ; PROBLEM: Main Residue Disorder ............ Percentage = 9 Note RESPONSE: The structure contains a significant degree of disorder. See _publ_section_exptl_refinement. ; # End Validation Reply Form #-------------------------------------------------------------------- _publ_contact_author_name 'Adrian B. Chaplin' _publ_contact_author_email a.b.chaplin@warwick.ac.uk _publ_section_exptl_refinement ; Solved with SHELXT-2014 by direct methods. Refined full-matrix least squares on F2 using SHELXL-2014. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms except H2 and H3 were placed in calculated positions and refined using the riding model. H2 and H3 were located on the Fourier difference map; their isotropic displacement parameters were fixed to ride on the parent atom. The Ir1-H2 and Ir1-H3 distances are restrained to equal length. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; #==================================================================== _audit_creation_date 2015-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C32 H42 Ir N6 O4, C32 H12 B F24' _chemical_formula_sum 'C64 H54 B F24 Ir N6 O4' _chemical_formula_weight 1630.14 _chemical_absolute_configuration . _chemical_melting_point 'not measured' 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3830(3) _cell_length_b 15.0025(4) _cell_length_c 18.0812(5) _cell_angle_alpha 106.251(2) _cell_angle_beta 108.604(2) _cell_angle_gamma 104.9131(19) _cell_volume 3282.23(15) _cell_formula_units_Z 2 _cell_measurement_reflns_used 20169 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 33.1190 _cell_measurement_theta_min 3.0590 _shelx_estimated_absorpt_T_max . _shelx_estimated_absorpt_T_min . _exptl_absorpt_coefficient_mu 2.155 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.66547 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details . _exptl_crystal_colour 'dark yellow' _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 1620 _exptl_crystal_recrystallization_method 'Crystals grown from C6H4F2-heptane at 293 K' _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_special_details . _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 50594 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 27.103 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 2.918 _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.2833 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 19.00 45.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 23.4718 -99.0000 30.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -5.00 25.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 23.4718 77.0000 -150.0000 30 #__ type_ start__ end____ width___ exp.time_ 3 omega 81.00 107.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 23.4718 -178.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 4 omega -51.00 35.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 23.4718 -38.0000 -30.0000 86 #__ type_ start__ end____ width___ exp.time_ 5 omega -22.00 65.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 23.4718 -99.0000 90.0000 87 #__ type_ start__ end____ width___ exp.time_ 6 omega 68.00 94.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - 23.4718 77.0000 -150.0000 26 #__ type_ start__ end____ width___ exp.time_ 7 omega -49.00 35.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 38.0000 -180.0000 84 #__ type_ start__ end____ width___ exp.time_ 8 omega -51.00 8.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 38.0000 -90.0000 59 #__ type_ start__ end____ width___ exp.time_ 9 omega -30.00 5.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 -57.0000 90.0000 35 #__ type_ start__ end____ width___ exp.time_ 10 omega -8.00 44.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 57.0000 -90.0000 52 #__ type_ start__ end____ width___ exp.time_ 11 omega -34.00 9.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 -77.0000 -90.0000 43 #__ type_ start__ end____ width___ exp.time_ 12 omega -99.00 -61.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 -57.0000 -150.0000 38 #__ type_ start__ end____ width___ exp.time_ 13 omega -103.00 9.00 1.0000 1.0000 omega____ theta____ kappa____ phi______ frames - -24.5655 -77.0000 60.0000 112 ; _diffrn_measurement_device_type 'Oxford Diffraction: Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0549169000 _diffrn_orient_matrix_UB_12 -0.0182478000 _diffrn_orient_matrix_UB_13 -0.0266601000 _diffrn_orient_matrix_UB_21 0.0107689000 _diffrn_orient_matrix_UB_22 -0.0136151000 _diffrn_orient_matrix_UB_23 -0.0363209000 _diffrn_orient_matrix_UB_31 -0.0059496000 _diffrn_orient_matrix_UB_32 -0.0481521000 _diffrn_orient_matrix_UB_33 0.0006737000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 13270 _reflns_number_total 14458 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.287 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.081 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 999 _refine_ls_number_reflns 14458 _refine_ls_number_restraints 442 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0273 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+2.3379P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.0666 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All Ir(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim C208-F6A with sigma of 0.01 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A with sigma of 0.01 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim C205-F6A with sigma of 0.01 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim C231-F21A with sigma of 0.01 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim F21A-F19A with sigma of 0.01 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim C227-F21A with sigma of 0.01 C223-F13A \\sim C223-F14A \\sim C223-F15A \\sim C223-F13 \\sim C223-F14 \\sim C223-F15 with sigma of 0.01 F13A-F14A \\sim F14A-F15A \\sim F15A-F13A \\sim F13-F14 \\sim F14-F15 \\sim F15-F13 with sigma of 0.01 C219-F13A \\sim C219-F14A \\sim C219-F15A \\sim C219-F13 \\sim C219-F14 \\sim C219-F15 with sigma of 0.01 Ir1-H2 \\sim Ir1-H3 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints F0AA \\sim F1 \\sim F1AA \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F13A \\sim F14 \\sim F14A \\sim F15 \\sim F15A \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F19A \\sim F20 \\sim F20A \\sim F21 \\sim F21A \\sim F22 \\sim F23 \\sim F24: within 1.7A with sigma of 0.007 and sigma for terminal atoms of 0.02 Uanis(F0AA) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1AA) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F13A) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F14A) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F15A) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02 4. Others Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1) Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1) Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(2) Sof(F13)=Sof(F14)=Sof(F15)=FVAR(2) Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3) Sof(F4)=Sof(F5)=Sof(F6)=FVAR(3) 5.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C13(H13A,H13B), C25(H25A,H25B), C28(H28A,H28B) 5.b Aromatic/amide H refined with riding coordinates: C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43), C44(H44), C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230) 5.c Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B, H18C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A, H33B,H33C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.24615(2) 0.63885(2) 0.92730(2) 0.01822(4) Uani 1 1 d D . . . . H2 H 0.211(2) 0.5831(19) 0.9673(17) 0.022 Uiso 1 1 d DR . . . . H3 H 0.1570(18) 0.5671(18) 0.8599(15) 0.022 Uiso 1 1 d DR . . . . C4 C 0.13629(19) 0.69955(18) 0.94140(16) 0.0208(5) Uani 1 1 d . . . . . C6 C -0.0287(2) 0.7027(2) 0.92091(19) 0.0264(6) Uani 1 1 d . . . . . C7 C 0.0388(2) 0.7751(2) 0.99638(18) 0.0263(6) Uani 1 1 d . . . . . C9 C -0.0472(2) 0.5663(2) 0.80923(18) 0.0292(6) Uani 1 1 d . . . . . C10 C -0.1449(2) 0.5960(2) 0.7918(2) 0.0344(7) Uani 1 1 d . . . . . H10A H -0.1467 0.6333 0.7545 0.041 Uiso 1 1 calc R . . . . H10B H -0.2111 0.5352 0.7637 0.041 Uiso 1 1 calc R . . . . C12 C 0.2162(2) 0.8474(2) 1.09435(17) 0.0262(6) Uani 1 1 d . . . . . C13 C 0.1477(2) 0.9060(2) 1.1154(2) 0.0405(8) Uani 1 1 d . . . . . H13A H 0.1615 0.9250 1.1760 0.049 Uiso 1 1 calc R . . . . H13B H 0.1660 0.9682 1.1049 0.049 Uiso 1 1 calc R . . . . C15 C -0.0640(2) 0.4762(2) 0.8334(2) 0.0395(7) Uani 1 1 d . . . . . H15A H 0.0023 0.4649 0.8513 0.059 Uiso 1 1 calc GR . . . . H15B H -0.1194 0.4166 0.7843 0.059 Uiso 1 1 calc GR . . . . H15C H -0.0858 0.4890 0.8802 0.059 Uiso 1 1 calc GR . . . . C16 C -0.0235(2) 0.5498(3) 0.73181(19) 0.0458(9) Uani 1 1 d . . . . . H16A H -0.0050 0.6127 0.7235 0.069 Uiso 1 1 calc GR . . . . H16B H -0.0862 0.4983 0.6816 0.069 Uiso 1 1 calc GR . . . . H16C H 0.0361 0.5276 0.7401 0.069 Uiso 1 1 calc GR . . . . C17 C 0.2403(3) 0.7917(2) 1.1517(2) 0.0379(7) Uani 1 1 d . . . . . H17A H 0.1752 0.7567 1.1552 0.057 Uiso 1 1 calc GR . . . . H17B H 0.2934 0.8397 1.2085 0.057 Uiso 1 1 calc GR . . . . H17C H 0.2680 0.7427 1.1283 0.057 Uiso 1 1 calc GR . . . . C18 C 0.3143(2) 0.9190(2) 1.0964(2) 0.0355(7) Uani 1 1 d . . . . . H18A H 0.3608 0.8836 1.0874 0.053 Uiso 1 1 calc GR . . . . H18B H 0.3522 0.9759 1.1517 0.053 Uiso 1 1 calc GR . . . . H18C H 0.2930 0.9436 1.0513 0.053 Uiso 1 1 calc GR . . . . C19 C 0.31395(19) 0.53595(18) 0.90136(16) 0.0210(5) Uani 1 1 d . . . . . C21 C 0.3710(3) 0.4066(2) 0.9050(2) 0.0363(7) Uani 1 1 d . . . . . C22 C 0.3726(2) 0.4211(2) 0.8368(2) 0.0335(7) Uani 1 1 d . . . . . C24 C 0.2971(2) 0.4359(2) 1.0018(2) 0.0313(6) Uani 1 1 d . . . . . C25 C 0.3670(3) 0.3739(3) 1.0161(2) 0.0436(8) Uani 1 1 d . . . . . H25A H 0.4361 0.4163 1.0655 0.052 Uiso 1 1 calc R . . . . H25B H 0.3313 0.3165 1.0272 0.052 Uiso 1 1 calc R . . . . C27 C 0.3307(2) 0.5131(2) 0.75505(19) 0.0326(6) Uani 1 1 d . . . . . C28 C 0.3430(4) 0.4154(3) 0.7087(3) 0.0609(11) Uani 1 1 d . . . . . H28A H 0.2722 0.3624 0.6691 0.073 Uiso 1 1 calc R . . . . H28B H 0.3841 0.4284 0.6755 0.073 Uiso 1 1 calc R . . . . C30 C 0.1803(3) 0.3689(2) 0.9504(2) 0.0405(7) Uani 1 1 d . . . . . H30A H 0.1393 0.4099 0.9377 0.061 Uiso 1 1 calc GR . . . . H30B H 0.1557 0.3342 0.9833 0.061 Uiso 1 1 calc GR . . . . H30C H 0.1707 0.3192 0.8972 0.061 Uiso 1 1 calc GR . . . . C31 C 0.3203(3) 0.5109(2) 1.08767(19) 0.0352(7) Uani 1 1 d . . . . . H31A H 0.3952 0.5561 1.1156 0.053 Uiso 1 1 calc GR . . . . H31B H 0.3051 0.4751 1.1228 0.053 Uiso 1 1 calc GR . . . . H31C H 0.2756 0.5501 1.0803 0.053 Uiso 1 1 calc GR . . . . C32 C 0.2208(2) 0.5070(3) 0.7042(2) 0.0408(8) Uani 1 1 d . . . . . H32A H 0.1675 0.4445 0.6953 0.061 Uiso 1 1 calc GR . . . . H32B H 0.2155 0.5081 0.6491 0.061 Uiso 1 1 calc GR . . . . H32C H 0.2086 0.5644 0.7353 0.061 Uiso 1 1 calc GR . . . . C33 C 0.4180(3) 0.6073(3) 0.7718(2) 0.0442(8) Uani 1 1 d . . . . . H33A H 0.4141 0.6656 0.8101 0.066 Uiso 1 1 calc GR . . . . H33B H 0.4097 0.6144 0.7180 0.066 Uiso 1 1 calc GR . . . . H33C H 0.4869 0.6031 0.7980 0.066 Uiso 1 1 calc GR . . . . C35 C 0.2461(2) 0.7495(2) 0.80259(18) 0.0285(6) Uani 1 1 d . . . . . H35 H 0.1742 0.7040 0.7710 0.034 Uiso 1 1 calc R . . . . C36 C 0.2852(3) 0.8183(2) 0.7724(2) 0.0368(7) Uani 1 1 d . . . . . H36 H 0.2416 0.8195 0.7209 0.044 Uiso 1 1 calc R . . . . C37 C 0.3893(3) 0.8857(2) 0.8185(2) 0.0410(8) Uani 1 1 d . . . . . H37 H 0.4190 0.9332 0.7987 0.049 Uiso 1 1 calc R . . . . C38 C 0.4490(2) 0.8827(2) 0.8935(2) 0.0354(7) Uani 1 1 d . . . . . H38 H 0.5202 0.9293 0.9266 0.042 Uiso 1 1 calc R . . . . C39 C 0.4054(2) 0.81164(19) 0.92112(17) 0.0248(5) Uani 1 1 d . . . . . C40 C 0.4620(2) 0.80789(19) 1.00265(17) 0.0239(5) Uani 1 1 d . . . . . C41 C 0.5691(2) 0.8676(2) 1.05505(19) 0.0321(6) Uani 1 1 d . . . . . H41 H 0.6101 0.9077 1.0356 0.039 Uiso 1 1 calc R . . . . C42 C 0.6151(2) 0.8682(2) 1.13464(19) 0.0340(7) Uani 1 1 d . . . . . H42 H 0.6877 0.9087 1.1708 0.041 Uiso 1 1 calc R . . . . C43 C 0.5535(2) 0.8090(2) 1.16055(18) 0.0312(6) Uani 1 1 d . . . . . H43 H 0.5820 0.8097 1.2160 0.037 Uiso 1 1 calc R . . . . C44 C 0.4495(2) 0.7485(2) 1.10486(17) 0.0247(5) Uani 1 1 d . . . . . H44 H 0.4089 0.7054 1.1226 0.030 Uiso 1 1 calc R . . . . N5 N 0.03014(16) 0.65899(15) 0.88686(14) 0.0220(4) Uani 1 1 d . . . . . N8 N 0.13853(16) 0.77427(16) 1.00727(14) 0.0214(4) Uani 1 1 d . . . . . N20 N 0.33684(19) 0.47622(17) 0.94545(16) 0.0282(5) Uani 1 1 d . . . . . N23 N 0.33894(18) 0.49931(16) 0.83484(15) 0.0253(5) Uani 1 1 d . . . . . N34 N 0.30415(17) 0.74317(16) 0.87445(14) 0.0224(4) Uani 1 1 d . . . . . N45 N 0.40240(16) 0.74686(16) 1.02717(14) 0.0217(4) Uani 1 1 d . . . . . O11 O -0.13498(15) 0.65827(15) 0.87297(14) 0.0326(5) Uani 1 1 d . . . . . O14 O 0.03796(16) 0.84356(16) 1.06280(14) 0.0380(5) Uani 1 1 d . . . . . O26 O 0.3825(2) 0.33848(19) 0.93970(19) 0.0547(7) Uani 1 1 d . . . . . O29 O 0.3964(2) 0.38360(17) 0.77038(16) 0.0454(6) Uani 1 1 d . . . . . B200 B 0.7587(2) 0.8324(2) 0.59013(18) 0.0199(5) Uani 1 1 d . . . . . C201 C 0.7790(2) 0.73023(18) 0.55229(16) 0.0209(5) Uani 1 1 d . . . . . C202 C 0.8772(2) 0.73433(19) 0.55229(16) 0.0230(5) Uani 1 1 d . . . . . H202 H 0.9273 0.7968 0.5625 0.028 Uiso 1 1 calc R . . . . C203 C 0.9045(2) 0.65076(19) 0.53796(17) 0.0242(5) Uani 1 1 d . . . . . C204 C 0.8323(2) 0.5573(2) 0.52029(18) 0.0279(6) Uani 1 1 d . . . . . H204 H 0.8503 0.4997 0.5105 0.034 Uiso 1 1 calc R . . . . C205 C 0.7336(2) 0.55068(19) 0.51744(18) 0.0287(6) Uani 1 1 d D . . . . C206 C 0.7073(2) 0.6347(2) 0.53326(17) 0.0264(6) Uani 1 1 d . . . . . H206 H 0.6387 0.6274 0.5311 0.032 Uiso 1 1 calc R . . . . C207 C 1.0120(2) 0.6591(2) 0.54168(19) 0.0297(6) Uani 1 1 d . . . . . C208 C 0.6554(3) 0.4512(2) 0.5008(2) 0.0457(8) Uani 1 1 d D . . . . C209 C 0.80739(19) 0.85642(18) 0.69159(16) 0.0206(5) Uani 1 1 d . . . . . C210 C 0.9169(2) 0.90319(19) 0.74210(17) 0.0222(5) Uani 1 1 d . . . . . H210 H 0.9619 0.9294 0.7182 0.027 Uiso 1 1 calc R . . . . C211 C 0.9625(2) 0.91284(19) 0.82574(17) 0.0241(5) Uani 1 1 d . . . . . C212 C 0.8996(2) 0.87576(19) 0.86334(17) 0.0257(5) Uani 1 1 d . . . . . H212 H 0.9301 0.8823 0.9205 0.031 Uiso 1 1 calc R . . . . C213 C 0.7909(2) 0.82887(19) 0.81463(18) 0.0250(5) Uani 1 1 d . . . . . C214 C 0.7461(2) 0.81863(18) 0.73101(17) 0.0231(5) Uani 1 1 d . . . . . H214 H 0.6714 0.7850 0.6993 0.028 Uiso 1 1 calc R . . . . C215 C 1.0803(2) 0.9597(3) 0.8741(2) 0.0380(7) Uani 1 1 d . . . . . C216 C 0.7189(3) 0.7877(2) 0.8517(2) 0.0343(7) Uani 1 1 d . . . . . C217 C 0.63444(19) 0.81958(18) 0.54931(16) 0.0212(5) Uani 1 1 d . . . . . C218 C 0.5907(2) 0.8758(2) 0.59347(18) 0.0264(6) Uani 1 1 d . . . . . H218 H 0.6313 0.9162 0.6524 0.032 Uiso 1 1 calc R . . . . C219 C 0.4902(2) 0.8745(2) 0.55409(18) 0.0302(6) Uani 1 1 d D . . . . C220 C 0.4281(2) 0.8168(2) 0.46789(19) 0.0299(6) Uani 1 1 d . . . . . H220 H 0.3592 0.8160 0.4407 0.036 Uiso 1 1 calc R . . . . C221 C 0.4696(2) 0.7608(2) 0.42304(17) 0.0256(6) Uani 1 1 d . . . . . C222 C 0.5703(2) 0.76199(19) 0.46293(17) 0.0233(5) Uani 1 1 d . . . . . H222 H 0.5964 0.7223 0.4304 0.028 Uiso 1 1 calc R . . . . C223 C 0.4457(2) 0.9346(3) 0.6042(2) 0.0487(9) Uani 1 1 d D . . . . C224 C 0.4084(2) 0.7006(2) 0.3297(2) 0.0364(7) Uani 1 1 d . . . . . C225 C 0.81746(19) 0.92487(18) 0.56902(17) 0.0213(5) Uani 1 1 d . . . . . C226 C 0.8590(2) 1.02500(19) 0.62558(17) 0.0254(5) Uani 1 1 d . . . . . H226 H 0.8613 1.0395 0.6809 0.030 Uiso 1 1 calc R . . . . C227 C 0.8969(2) 1.1040(2) 0.60390(18) 0.0310(6) Uani 1 1 d D . . . . C228 C 0.8933(2) 1.0856(2) 0.52345(19) 0.0307(6) Uani 1 1 d . . . . . H228 H 0.9190 1.1396 0.5083 0.037 Uiso 1 1 calc R . . . . C229 C 0.8513(2) 0.9871(2) 0.46542(17) 0.0246(5) Uani 1 1 d . . . . . C230 C 0.81497(19) 0.90807(19) 0.48815(17) 0.0223(5) Uani 1 1 d . . . . . H230 H 0.7878 0.8410 0.4477 0.027 Uiso 1 1 calc R . . . . C231 C 0.9392(3) 1.2104(2) 0.6661(2) 0.0511(10) Uani 1 1 d D . . . . C232 C 0.8397(2) 0.9674(2) 0.37680(18) 0.0316(6) Uani 1 1 d . . . . . F0AA F 1.05602(15) 0.61201(16) 0.58683(15) 0.0512(5) Uani 1 1 d . U . . . F1 F 1.01071(16) 0.61912(19) 0.46543(13) 0.0597(6) Uani 1 1 d . U . . . F1AA F 1.08163(14) 0.75378(14) 0.57691(15) 0.0493(5) Uani 1 1 d . U . . . F4 F 0.5608(3) 0.4274(3) 0.4362(3) 0.0757(14) Uani 0.721(7) 1 d D U P A 1 F4A F 0.7012(7) 0.4177(7) 0.5605(7) 0.072(4) Uani 0.279(7) 1 d D U P A 2 F5 F 0.6798(4) 0.3758(2) 0.4753(5) 0.095(2) Uani 0.721(7) 1 d D U P A 1 F5A F 0.5707(6) 0.4506(6) 0.5074(10) 0.083(4) Uani 0.279(7) 1 d D U P A 2 F6 F 0.6290(5) 0.4521(3) 0.5628(3) 0.102(2) Uani 0.721(7) 1 d D U P A 1 F6A F 0.6345(11) 0.3796(5) 0.4315(5) 0.089(5) Uani 0.279(7) 1 d D U P A 2 F7 F 1.11326(16) 0.98465(18) 0.95682(13) 0.0596(6) Uani 1 1 d . U . . . F8 F 1.12615(18) 0.8977(2) 0.85069(19) 0.1066(12) Uani 1 1 d . U . . . F9 F 1.12320(17) 1.0423(2) 0.86492(17) 0.0845(9) Uani 1 1 d . U . . . F10 F 0.6446(2) 0.82643(18) 0.84668(19) 0.0685(7) Uani 1 1 d . U . . . F11 F 0.76968(18) 0.80403(15) 0.93279(13) 0.0527(5) Uani 1 1 d . U . . . F12 F 0.66589(13) 0.68794(13) 0.81004(12) 0.0382(4) Uani 1 1 d . U . . . F13 F 0.4049(5) 0.9889(5) 0.5687(4) 0.0754(17) Uani 0.657(10) 1 d D U P B 1 F13A F 0.4269(13) 0.9044(9) 0.6586(7) 0.091(3) Uani 0.343(10) 1 d D U P B 2 F14 F 0.5090(4) 0.9907(6) 0.6831(3) 0.096(3) Uani 0.657(10) 1 d D U P B 1 F14A F 0.3638(8) 0.9459(10) 0.5574(5) 0.095(5) Uani 0.343(10) 1 d D U P B 2 F15 F 0.3619(5) 0.8734(4) 0.6089(5) 0.087(2) Uani 0.657(10) 1 d D U P B 1 F15A F 0.5193(6) 1.0303(4) 0.6492(8) 0.082(3) Uani 0.343(10) 1 d D U P B 2 F16 F 0.30795(16) 0.6894(2) 0.30096(14) 0.0796(8) Uani 1 1 d . U . . . F17 F 0.40967(18) 0.60797(15) 0.30585(12) 0.0581(6) Uani 1 1 d . U . . . F18 F 0.44849(19) 0.74149(18) 0.28428(13) 0.0637(7) Uani 1 1 d . U . . . F19 F 0.8884(9) 1.2628(5) 0.6349(5) 0.091(3) Uani 0.515(17) 1 d D U P C 1 F19A F 0.9872(13) 1.2200(5) 0.7445(3) 0.103(4) Uani 0.485(17) 1 d D U P C 2 F20 F 0.9318(11) 1.2208(5) 0.7369(4) 0.086(3) Uani 0.515(17) 1 d D U P C 1 F20A F 1.0095(10) 1.2715(5) 0.6542(7) 0.095(4) Uani 0.485(17) 1 d D U P C 2 F21 F 1.0382(5) 1.2603(5) 0.6848(8) 0.093(3) Uani 0.515(17) 1 d D U P C 1 F21A F 0.8650(6) 1.2451(7) 0.6645(10) 0.127(5) Uani 0.485(17) 1 d D U P C 2 F22 F 0.76272(19) 0.9921(2) 0.33384(14) 0.0723(7) Uani 1 1 d . U . . . F23 F 0.92625(16) 1.02040(17) 0.37314(13) 0.0559(6) Uani 1 1 d . U . . . F24 F 0.8155(2) 0.87276(16) 0.33068(14) 0.0740(8) Uani 1 1 d . U . . . 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 0.01530(5) 0.02061(5) 0.01621(5) 0.00546(4) 0.00610(4) 0.00566(4) C4 0.0205(12) 0.0226(12) 0.0173(12) 0.0071(10) 0.0062(10) 0.0083(10) C6 0.0197(13) 0.0286(14) 0.0353(15) 0.0137(12) 0.0142(11) 0.0116(11) C7 0.0239(13) 0.0286(14) 0.0310(15) 0.0106(12) 0.0148(11) 0.0143(11) C9 0.0157(12) 0.0302(14) 0.0275(14) 0.0023(12) 0.0036(11) 0.0040(11) C10 0.0206(14) 0.0378(16) 0.0346(16) 0.0083(13) 0.0064(12) 0.0088(12) C12 0.0273(14) 0.0258(13) 0.0188(13) 0.0013(11) 0.0076(11) 0.0108(11) C13 0.0361(17) 0.0421(18) 0.0310(16) -0.0009(14) 0.0079(13) 0.0210(14) C15 0.0257(15) 0.0253(14) 0.051(2) 0.0068(14) 0.0093(14) 0.0030(12) C16 0.0221(15) 0.070(2) 0.0229(15) 0.0020(15) 0.0018(12) 0.0114(15) C17 0.0416(18) 0.0474(18) 0.0268(15) 0.0154(14) 0.0131(13) 0.0209(15) C18 0.0317(15) 0.0225(14) 0.0366(17) 0.0022(12) 0.0074(13) 0.0057(11) C19 0.0173(12) 0.0242(12) 0.0219(12) 0.0100(10) 0.0092(10) 0.0063(10) C21 0.0451(18) 0.0342(16) 0.052(2) 0.0246(15) 0.0320(16) 0.0261(14) C22 0.0379(16) 0.0307(15) 0.0447(18) 0.0145(13) 0.0284(14) 0.0190(13) C24 0.0344(15) 0.0315(15) 0.0366(16) 0.0207(13) 0.0194(13) 0.0118(12) C25 0.057(2) 0.0406(18) 0.055(2) 0.0330(17) 0.0320(18) 0.0262(16) C27 0.0417(17) 0.0387(16) 0.0253(14) 0.0111(13) 0.0207(13) 0.0207(13) C28 0.090(3) 0.067(3) 0.047(2) 0.019(2) 0.041(2) 0.049(2) C30 0.0404(18) 0.0383(17) 0.0410(18) 0.0191(15) 0.0203(15) 0.0044(14) C31 0.0402(17) 0.0370(16) 0.0298(15) 0.0195(13) 0.0147(13) 0.0101(13) C32 0.0334(17) 0.0480(19) 0.0236(15) 0.0075(14) 0.0059(13) 0.0042(14) C33 0.0318(16) 0.068(2) 0.0365(18) 0.0260(17) 0.0204(14) 0.0109(15) C35 0.0254(14) 0.0327(14) 0.0242(14) 0.0105(12) 0.0074(11) 0.0110(11) C36 0.0450(18) 0.0402(17) 0.0291(16) 0.0190(14) 0.0139(14) 0.0183(14) C37 0.052(2) 0.0334(16) 0.0365(17) 0.0188(14) 0.0206(16) 0.0073(14) C38 0.0342(16) 0.0308(15) 0.0329(16) 0.0117(13) 0.0139(13) 0.0012(12) C39 0.0252(13) 0.0227(12) 0.0225(13) 0.0048(10) 0.0111(11) 0.0064(10) C40 0.0228(13) 0.0226(12) 0.0234(13) 0.0058(10) 0.0101(11) 0.0073(10) C41 0.0227(14) 0.0314(15) 0.0325(15) 0.0087(12) 0.0098(12) 0.0021(11) C42 0.0220(14) 0.0333(15) 0.0295(15) 0.0049(12) 0.0018(12) 0.0041(11) C43 0.0279(14) 0.0340(15) 0.0214(13) 0.0075(12) 0.0025(11) 0.0099(12) C44 0.0237(13) 0.0272(13) 0.0232(13) 0.0094(11) 0.0091(11) 0.0111(11) N5 0.0184(10) 0.0221(11) 0.0222(11) 0.0064(9) 0.0075(9) 0.0064(8) N8 0.0197(10) 0.0227(11) 0.0200(11) 0.0065(9) 0.0078(9) 0.0083(8) N20 0.0316(12) 0.0308(12) 0.0336(13) 0.0178(11) 0.0202(11) 0.0155(10) N23 0.0287(12) 0.0267(11) 0.0272(12) 0.0115(10) 0.0165(10) 0.0139(9) N34 0.0214(11) 0.0253(11) 0.0206(11) 0.0087(9) 0.0098(9) 0.0083(9) N45 0.0196(10) 0.0244(11) 0.0206(11) 0.0075(9) 0.0084(9) 0.0089(8) O11 0.0176(9) 0.0362(11) 0.0396(12) 0.0111(9) 0.0104(9) 0.0100(8) O14 0.0314(11) 0.0376(12) 0.0393(12) 0.0022(10) 0.0166(10) 0.0165(9) O26 0.0847(19) 0.0520(15) 0.0766(19) 0.0456(15) 0.0561(17) 0.0503(14) O29 0.0636(16) 0.0447(13) 0.0540(15) 0.0218(12) 0.0431(13) 0.0346(12) B200 0.0188(13) 0.0187(13) 0.0189(13) 0.0055(11) 0.0076(11) 0.0046(10) C201 0.0231(12) 0.0209(12) 0.0155(11) 0.0068(10) 0.0067(10) 0.0059(10) C202 0.0235(13) 0.0206(12) 0.0199(12) 0.0064(10) 0.0075(10) 0.0047(10) C203 0.0268(13) 0.0265(13) 0.0191(12) 0.0106(11) 0.0080(10) 0.0105(11) C204 0.0390(16) 0.0224(13) 0.0260(14) 0.0119(11) 0.0143(12) 0.0138(11) C205 0.0352(15) 0.0192(13) 0.0274(14) 0.0089(11) 0.0128(12) 0.0048(11) C206 0.0255(13) 0.0262(13) 0.0255(14) 0.0097(11) 0.0113(11) 0.0065(11) C207 0.0319(15) 0.0298(14) 0.0286(15) 0.0128(12) 0.0111(12) 0.0143(12) C208 0.052(2) 0.0258(16) 0.055(2) 0.0140(15) 0.0281(18) 0.0037(14) C209 0.0216(12) 0.0181(11) 0.0220(13) 0.0073(10) 0.0099(10) 0.0071(9) C210 0.0200(12) 0.0239(12) 0.0226(13) 0.0075(10) 0.0109(10) 0.0078(10) C211 0.0203(13) 0.0260(13) 0.0237(13) 0.0080(11) 0.0072(10) 0.0104(10) C212 0.0330(14) 0.0284(13) 0.0212(13) 0.0122(11) 0.0114(11) 0.0174(11) C213 0.0317(14) 0.0222(13) 0.0285(14) 0.0134(11) 0.0176(12) 0.0114(11) C214 0.0206(12) 0.0193(12) 0.0264(13) 0.0069(10) 0.0095(10) 0.0058(10) C215 0.0266(15) 0.0526(19) 0.0263(15) 0.0111(14) 0.0059(12) 0.0139(14) C216 0.0422(17) 0.0348(16) 0.0419(18) 0.0230(14) 0.0266(15) 0.0191(13) C217 0.0186(12) 0.0199(12) 0.0223(13) 0.0093(10) 0.0078(10) 0.0031(9) C218 0.0233(13) 0.0278(13) 0.0225(13) 0.0068(11) 0.0072(11) 0.0077(11) C219 0.0282(14) 0.0367(15) 0.0293(15) 0.0141(13) 0.0130(12) 0.0155(12) C220 0.0200(13) 0.0363(15) 0.0318(15) 0.0160(13) 0.0083(11) 0.0087(11) C221 0.0198(12) 0.0275(13) 0.0210(13) 0.0098(11) 0.0049(10) 0.0005(10) C222 0.0212(12) 0.0217(12) 0.0222(13) 0.0065(10) 0.0092(10) 0.0029(10) C223 0.042(2) 0.063(2) 0.041(2) 0.0124(18) 0.0140(16) 0.0339(18) C224 0.0250(15) 0.0444(18) 0.0281(15) 0.0125(14) 0.0051(12) 0.0053(13) C225 0.0160(12) 0.0229(12) 0.0230(13) 0.0084(10) 0.0074(10) 0.0061(10) C226 0.0286(14) 0.0231(13) 0.0227(13) 0.0066(11) 0.0124(11) 0.0078(11) C227 0.0365(16) 0.0215(13) 0.0291(15) 0.0063(11) 0.0146(13) 0.0054(11) C228 0.0314(15) 0.0265(14) 0.0304(15) 0.0135(12) 0.0117(12) 0.0044(11) C229 0.0195(12) 0.0305(14) 0.0217(13) 0.0109(11) 0.0080(10) 0.0065(10) C230 0.0179(12) 0.0234(12) 0.0218(13) 0.0065(10) 0.0070(10) 0.0064(10) C231 0.080(3) 0.0250(16) 0.042(2) 0.0089(15) 0.032(2) 0.0083(17) C232 0.0287(15) 0.0352(15) 0.0252(14) 0.0111(12) 0.0116(12) 0.0044(12) F0AA 0.0437(11) 0.0650(13) 0.0753(15) 0.0514(12) 0.0284(11) 0.0364(10) F1 0.0390(11) 0.0988(17) 0.0378(11) 0.0153(11) 0.0211(9) 0.0276(11) F1AA 0.0249(9) 0.0356(10) 0.0788(15) 0.0195(10) 0.0149(9) 0.0110(8) F4 0.056(2) 0.042(2) 0.094(3) 0.020(2) 0.021(2) -0.0127(16) F4A 0.056(5) 0.048(5) 0.095(7) 0.060(5) 0.006(5) -0.008(4) F5 0.074(3) 0.0232(17) 0.187(6) 0.029(3) 0.066(4) 0.0175(18) F5A 0.050(5) 0.038(4) 0.177(10) 0.041(6) 0.069(6) 0.018(4) F6 0.145(5) 0.060(2) 0.077(3) 0.026(2) 0.068(3) -0.022(3) F6A 0.130(9) 0.035(5) 0.045(5) -0.007(4) 0.039(6) -0.031(6) F7 0.0375(11) 0.0807(16) 0.0307(10) 0.0155(10) -0.0012(9) 0.0043(10) F8 0.0373(13) 0.129(2) 0.091(2) -0.0280(18) -0.0022(13) 0.0511(15) F9 0.0288(11) 0.116(2) 0.0827(18) 0.0689(17) -0.0023(11) -0.0120(12) F10 0.0838(16) 0.0836(16) 0.120(2) 0.0747(16) 0.0864(17) 0.0631(14) F11 0.0690(14) 0.0499(12) 0.0349(11) 0.0183(9) 0.0301(10) 0.0041(10) F12 0.0274(9) 0.0391(10) 0.0448(11) 0.0206(8) 0.0150(8) 0.0036(7) F13 0.104(4) 0.082(3) 0.091(4) 0.049(3) 0.061(3) 0.072(3) F13A 0.141(8) 0.114(7) 0.066(6) 0.041(5) 0.083(6) 0.065(6) F14 0.068(3) 0.142(5) 0.043(2) -0.019(3) 0.005(2) 0.071(3) F14A 0.055(5) 0.149(9) 0.061(5) 0.000(6) 0.006(4) 0.080(6) F15 0.087(4) 0.086(3) 0.108(5) 0.022(3) 0.077(4) 0.037(3) F15A 0.089(5) 0.064(5) 0.081(6) -0.007(4) 0.039(5) 0.046(4) F16 0.0248(10) 0.123(2) 0.0415(12) -0.0050(13) -0.0055(9) 0.0181(12) F17 0.0730(15) 0.0406(11) 0.0283(10) 0.0001(9) 0.0036(10) 0.0099(10) F18 0.0680(15) 0.0723(15) 0.0276(10) 0.0206(10) 0.0126(10) 0.0002(12) F19 0.157(7) 0.043(3) 0.072(4) 0.015(3) 0.039(4) 0.057(4) F19A 0.160(8) 0.037(3) 0.031(3) -0.001(2) -0.013(4) -0.004(4) F20 0.162(7) 0.026(2) 0.052(4) -0.002(3) 0.069(4) -0.001(4) F20A 0.148(7) 0.029(3) 0.066(5) 0.010(3) 0.049(5) -0.025(4) F21 0.078(4) 0.040(3) 0.099(6) -0.020(3) 0.035(4) -0.017(3) F21A 0.098(5) 0.075(5) 0.130(8) -0.045(5) 0.023(5) 0.043(4) F22 0.0610(14) 0.138(2) 0.0339(11) 0.0424(14) 0.0180(11) 0.0558(15) F23 0.0425(11) 0.0744(14) 0.0362(11) 0.0185(10) 0.0219(9) -0.0029(10) F24 0.135(2) 0.0421(12) 0.0377(12) 0.0087(10) 0.0490(14) 0.0135(13) _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 H2 1.36(2) . ? Ir1 H3 1.36(2) . ? Ir1 C4 2.064(3) . ? Ir1 C19 2.053(3) . ? Ir1 N34 2.175(2) . ? Ir1 N45 2.199(2) . ? C4 N5 1.378(3) . ? C4 N8 1.373(3) . ? C6 C7 1.329(4) . ? C6 N5 1.385(3) . ? C6 O11 1.356(3) . ? C7 N8 1.388(3) . ? C7 O14 1.350(3) . ? C9 C10 1.545(4) . ? C9 C15 1.518(4) . ? C9 C16 1.514(4) . ? C9 N5 1.502(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 O11 1.441(4) . ? C12 C13 1.544(4) . ? C12 C17 1.516(4) . ? C12 C18 1.520(4) . ? C12 N8 1.487(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 O14 1.434(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N20 1.390(3) . ? C19 N23 1.373(3) . ? C21 C22 1.319(4) . ? C21 N20 1.390(4) . ? C21 O26 1.357(4) . ? C22 N23 1.384(4) . ? C22 O29 1.363(4) . ? C24 C25 1.546(4) . ? C24 C30 1.520(4) . ? C24 C31 1.512(4) . ? C24 N20 1.506(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 O26 1.445(4) . ? C27 C28 1.556(5) . ? C27 C32 1.517(4) . ? C27 C33 1.507(4) . ? C27 N23 1.486(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 O29 1.415(5) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 H35 0.9500 . ? C35 C36 1.377(4) . ? C35 N34 1.346(3) . ? C36 H36 0.9500 . ? C36 C37 1.382(5) . ? C37 H37 0.9500 . ? C37 C38 1.375(5) . ? C38 H38 0.9500 . ? C38 C39 1.390(4) . ? C39 C40 1.464(4) . ? C39 N34 1.359(3) . ? C40 C41 1.399(4) . ? C40 N45 1.355(3) . ? C41 H41 0.9500 . ? C41 C42 1.375(4) . ? C42 H42 0.9500 . ? C42 C43 1.374(4) . ? C43 H43 0.9500 . ? C43 C44 1.379(4) . ? C44 H44 0.9500 . ? C44 N45 1.341(3) . ? B200 C201 1.634(4) . ? B200 C209 1.633(4) . ? B200 C217 1.637(4) . ? B200 C225 1.638(4) . ? C201 C202 1.398(4) . ? C201 C206 1.404(3) . ? C202 H202 0.9500 . ? C202 C203 1.389(4) . ? C203 C204 1.391(4) . ? C203 C207 1.496(4) . ? C204 H204 0.9500 . ? C204 C205 1.380(4) . ? C205 C206 1.389(4) . ? C205 C208 1.501(4) . ? C206 H206 0.9500 . ? C207 F0AA 1.339(3) . ? C207 F1 1.333(4) . ? C207 F1AA 1.334(3) . ? C208 F4 1.358(4) . ? C208 F4A 1.369(5) . ? C208 F5 1.277(4) . ? C208 F5A 1.259(5) . ? C208 F6 1.292(4) . ? C208 F6A 1.285(5) . ? C209 C210 1.400(3) . ? C209 C214 1.406(4) . ? C210 H210 0.9500 . ? C210 C211 1.391(4) . ? C211 C212 1.390(4) . ? C211 C215 1.493(4) . ? C212 H212 0.9500 . ? C212 C213 1.387(4) . ? C213 C214 1.387(4) . ? C213 C216 1.500(4) . ? C214 H214 0.9500 . ? C215 F7 1.320(4) . ? C215 F8 1.325(4) . ? C215 F9 1.315(4) . ? C216 F10 1.333(4) . ? C216 F11 1.329(4) . ? C216 F12 1.343(3) . ? C217 C218 1.401(4) . ? C217 C222 1.397(4) . ? C218 H218 0.9500 . ? C218 C219 1.385(4) . ? C219 C220 1.391(4) . ? C219 C223 1.501(4) . ? C220 H220 0.9500 . ? C220 C221 1.381(4) . ? C221 C222 1.390(4) . ? C221 C224 1.493(4) . ? C222 H222 0.9500 . ? C223 F13 1.313(4) . ? C223 F13A 1.264(5) . ? C223 F14 1.295(4) . ? C223 F14A 1.296(5) . ? C223 F15 1.356(5) . ? C223 F15A 1.364(6) . ? C224 F16 1.317(4) . ? C224 F17 1.341(4) . ? C224 F18 1.336(4) . ? C225 C226 1.396(4) . ? C225 C230 1.400(4) . ? C226 H226 0.9500 . ? C226 C227 1.386(4) . ? C227 C228 1.384(4) . ? C227 C231 1.497(4) . ? C228 H228 0.9500 . ? C228 C229 1.385(4) . ? C229 C230 1.393(4) . ? C229 C232 1.490(4) . ? C230 H230 0.9500 . ? C231 F19 1.323(5) . ? C231 F19A 1.310(5) . ? C231 F20 1.288(5) . ? C231 F20A 1.295(5) . ? C231 F21 1.305(5) . ? C231 F21A 1.298(5) . ? C232 F22 1.338(4) . ? C232 F23 1.326(3) . ? C232 F24 1.315(4) . ? 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 H2 Ir1 H3 81.1(16) . . ? C4 Ir1 H2 84.0(12) . . ? C4 Ir1 H3 80.2(12) . . ? C4 Ir1 N34 91.44(9) . . ? C4 Ir1 N45 107.05(9) . . ? C19 Ir1 H2 82.5(12) . . ? C19 Ir1 H3 84.6(12) . . ? C19 Ir1 C4 161.10(10) . . ? C19 Ir1 N34 102.95(9) . . ? C19 Ir1 N45 88.78(9) . . ? N34 Ir1 H2 173.4(12) . . ? N34 Ir1 H3 103.0(11) . . ? N34 Ir1 N45 74.49(8) . . ? N45 Ir1 H2 102.2(12) . . ? N45 Ir1 H3 172.2(12) . . ? N5 C4 Ir1 125.19(18) . . ? N8 C4 Ir1 133.09(18) . . ? N8 C4 N5 100.9(2) . . ? C7 C6 N5 107.2(2) . . ? C7 C6 O11 138.3(3) . . ? O11 C6 N5 114.4(2) . . ? C6 C7 N8 106.0(2) . . ? C6 C7 O14 139.5(2) . . ? O14 C7 N8 114.4(2) . . ? C15 C9 C10 111.5(2) . . ? C16 C9 C10 107.9(3) . . ? C16 C9 C15 113.3(3) . . ? N5 C9 C10 98.0(2) . . ? N5 C9 C15 109.1(2) . . ? N5 C9 C16 116.0(2) . . ? C9 C10 H10A 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? O11 C10 C9 106.9(2) . . ? O11 C10 H10A 110.3 . . ? O11 C10 H10B 110.3 . . ? C17 C12 C13 111.4(3) . . ? C17 C12 C18 113.9(3) . . ? C18 C12 C13 109.0(2) . . ? N8 C12 C13 98.6(2) . . ? N8 C12 C17 109.5(2) . . ? N8 C12 C18 113.4(2) . . ? C12 C13 H13A 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? O14 C13 C12 108.9(2) . . ? O14 C13 H13A 109.9 . . ? O14 C13 H13B 109.9 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C16 H16A 109.5 . . ? C9 C16 H16B 109.5 . . ? C9 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N20 C19 Ir1 126.92(19) . . ? N23 C19 Ir1 131.83(19) . . ? N23 C19 N20 101.0(2) . . ? C22 C21 N20 107.3(2) . . ? C22 C21 O26 137.8(3) . . ? O26 C21 N20 114.4(3) . . ? C21 C22 N23 106.7(2) . . ? C21 C22 O29 139.9(3) . . ? O29 C22 N23 113.4(3) . . ? C30 C24 C25 111.7(3) . . ? C31 C24 C25 108.0(3) . . ? C31 C24 C30 113.0(3) . . ? N20 C24 C25 97.4(2) . . ? N20 C24 C30 108.3(2) . . ? N20 C24 C31 117.3(2) . . ? C24 C25 H25A 110.3 . . ? C24 C25 H25B 110.3 . . ? H25A C25 H25B 108.6 . . ? O26 C25 C24 107.1(3) . . ? O26 C25 H25A 110.3 . . ? O26 C25 H25B 110.3 . . ? C32 C27 C28 108.1(3) . . ? C33 C27 C28 113.1(3) . . ? C33 C27 C32 113.1(3) . . ? N23 C27 C28 98.4(2) . . ? N23 C27 C32 111.6(2) . . ? N23 C27 C33 111.6(3) . . ? C27 C28 H28A 110.0 . . ? C27 C28 H28B 110.0 . . ? H28A C28 H28B 108.4 . . ? O29 C28 C27 108.5(3) . . ? O29 C28 H28A 110.0 . . ? O29 C28 H28B 110.0 . . ? C24 C30 H30A 109.5 . . ? C24 C30 H30B 109.5 . . ? C24 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C24 C31 H31A 109.5 . . ? C24 C31 H31B 109.5 . . ? C24 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C35 H35 118.2 . . ? N34 C35 H35 118.2 . . ? N34 C35 C36 123.5(3) . . ? C35 C36 H36 120.7 . . ? C35 C36 C37 118.6(3) . . ? C37 C36 H36 120.7 . . ? C36 C37 H37 120.6 . . ? C38 C37 C36 118.8(3) . . ? C38 C37 H37 120.6 . . ? C37 C38 H38 119.9 . . ? C37 C38 C39 120.1(3) . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 123.1(2) . . ? N34 C39 C38 121.1(3) . . ? N34 C39 C40 115.7(2) . . ? C41 C40 C39 122.8(2) . . ? N45 C40 C39 115.7(2) . . ? N45 C40 C41 121.4(3) . . ? C40 C41 H41 119.9 . . ? C42 C41 C40 120.1(3) . . ? C42 C41 H41 119.9 . . ? C41 C42 H42 120.8 . . ? C43 C42 C41 118.3(3) . . ? C43 C42 H42 120.8 . . ? C42 C43 H43 120.5 . . ? C42 C43 C44 119.0(3) . . ? C44 C43 H43 120.5 . . ? C43 C44 H44 118.1 . . ? N45 C44 C43 123.9(3) . . ? N45 C44 H44 118.1 . . ? C4 N5 C6 112.5(2) . . ? C4 N5 C9 138.6(2) . . ? C6 N5 C9 107.2(2) . . ? C4 N8 C7 113.2(2) . . ? C4 N8 C12 137.7(2) . . ? C7 N8 C12 108.4(2) . . ? C19 N20 C21 111.9(2) . . ? C19 N20 C24 136.3(2) . . ? C21 N20 C24 106.3(2) . . ? C19 N23 C22 113.1(2) . . ? C19 N23 C27 137.7(2) . . ? C22 N23 C27 108.8(2) . . ? C35 N34 Ir1 125.35(18) . . ? C35 N34 C39 117.7(2) . . ? C39 N34 Ir1 116.80(17) . . ? C40 N45 Ir1 115.54(17) . . ? C44 N45 Ir1 126.54(17) . . ? C44 N45 C40 117.2(2) . . ? C6 O11 C10 103.8(2) . . ? C7 O14 C13 104.4(2) . . ? C21 O26 C25 104.1(2) . . ? C22 O29 C28 104.0(2) . . ? C201 B200 C217 114.0(2) . . ? C201 B200 C225 113.5(2) . . ? C209 B200 C201 101.2(2) . . ? C209 B200 C217 114.1(2) . . ? C209 B200 C225 112.4(2) . . ? C217 B200 C225 102.2(2) . . ? C202 C201 B200 121.4(2) . . ? C202 C201 C206 115.6(2) . . ? C206 C201 B200 122.0(2) . . ? C201 C202 H202 118.7 . . ? C203 C202 C201 122.7(2) . . ? C203 C202 H202 118.7 . . ? C202 C203 C204 120.5(3) . . ? C202 C203 C207 121.0(2) . . ? C204 C203 C207 118.5(2) . . ? C203 C204 H204 121.0 . . ? C205 C204 C203 117.9(2) . . ? C205 C204 H204 121.0 . . ? C204 C205 C206 121.4(2) . . ? C204 C205 C208 118.9(2) . . ? C206 C205 C208 119.6(3) . . ? C201 C206 H206 119.1 . . ? C205 C206 C201 121.9(3) . . ? C205 C206 H206 119.1 . . ? F0AA C207 C203 112.8(2) . . ? F1 C207 C203 113.1(2) . . ? F1 C207 F0AA 105.3(2) . . ? F1 C207 F1AA 105.9(2) . . ? F1AA C207 C203 113.3(2) . . ? F1AA C207 F0AA 105.8(2) . . ? F4 C208 C205 110.8(3) . . ? F4A C208 C205 108.4(3) . . ? F5 C208 C205 115.3(3) . . ? F5 C208 F4 102.9(3) . . ? F5 C208 F6 111.4(4) . . ? F5A C208 C205 116.8(4) . . ? F5A C208 F4A 103.8(5) . . ? F5A C208 F6A 110.0(5) . . ? F6 C208 C205 113.2(3) . . ? F6 C208 F4 102.0(4) . . ? F6A C208 C205 114.5(4) . . ? F6A C208 F4A 101.5(5) . . ? C210 C209 B200 121.1(2) . . ? C210 C209 C214 115.3(2) . . ? C214 C209 B200 122.9(2) . . ? C209 C210 H210 118.6 . . ? C211 C210 C209 122.8(2) . . ? C211 C210 H210 118.6 . . ? C210 C211 C215 119.4(2) . . ? C212 C211 C210 120.6(2) . . ? C212 C211 C215 119.9(3) . . ? C211 C212 H212 121.1 . . ? C213 C212 C211 117.8(2) . . ? C213 C212 H212 121.1 . . ? C212 C213 C216 120.3(3) . . ? C214 C213 C212 121.3(2) . . ? C214 C213 C216 118.4(3) . . ? C209 C214 H214 118.9 . . ? C213 C214 C209 122.2(2) . . ? C213 C214 H214 118.9 . . ? F7 C215 C211 113.9(3) . . ? F7 C215 F8 104.4(3) . . ? F8 C215 C211 111.8(3) . . ? F9 C215 C211 113.0(3) . . ? F9 C215 F7 105.8(3) . . ? F9 C215 F8 107.2(3) . . ? F10 C216 C213 111.9(2) . . ? F10 C216 F12 105.5(3) . . ? F11 C216 C213 113.4(3) . . ? F11 C216 F10 107.2(3) . . ? F11 C216 F12 106.3(2) . . ? F12 C216 C213 112.0(2) . . ? C218 C217 B200 123.2(2) . . ? C222 C217 B200 120.3(2) . . ? C222 C217 C218 115.8(2) . . ? C217 C218 H218 118.9 . . ? C219 C218 C217 122.2(3) . . ? C219 C218 H218 118.9 . . ? C218 C219 C220 120.9(3) . . ? C218 C219 C223 120.4(3) . . ? C220 C219 C223 118.7(2) . . ? C219 C220 H220 121.0 . . ? C221 C220 C219 118.0(3) . . ? C221 C220 H220 121.0 . . ? C220 C221 C222 120.9(3) . . ? C220 C221 C224 120.4(3) . . ? C222 C221 C224 118.6(3) . . ? C217 C222 H222 118.9 . . ? C221 C222 C217 122.2(3) . . ? C221 C222 H222 118.9 . . ? F13 C223 C219 113.7(3) . . ? F13 C223 F15 102.9(3) . . ? F13A C223 C219 114.6(4) . . ? F13A C223 F14A 110.5(5) . . ? F13A C223 F15A 105.8(5) . . ? F14 C223 C219 116.0(3) . . ? F14 C223 F13 108.8(4) . . ? F14 C223 F15 103.3(4) . . ? F14A C223 C219 113.6(4) . . ? F14A C223 F15A 103.3(5) . . ? F15 C223 C219 110.9(3) . . ? F15A C223 C219 108.1(4) . . ? F16 C224 C221 113.7(3) . . ? F16 C224 F17 106.5(3) . . ? F16 C224 F18 106.1(3) . . ? F17 C224 C221 112.9(3) . . ? F18 C224 C221 112.4(2) . . ? F18 C224 F17 104.5(3) . . ? C226 C225 B200 122.2(2) . . ? C226 C225 C230 116.3(2) . . ? C230 C225 B200 120.9(2) . . ? C225 C226 H226 118.8 . . ? C227 C226 C225 122.3(3) . . ? C227 C226 H226 118.8 . . ? C226 C227 C231 120.6(3) . . ? C228 C227 C226 120.4(3) . . ? C228 C227 C231 119.0(2) . . ? C227 C228 H228 120.6 . . ? C227 C228 C229 118.8(2) . . ? C229 C228 H228 120.6 . . ? C228 C229 C230 120.5(3) . . ? C228 C229 C232 118.9(2) . . ? C230 C229 C232 120.5(2) . . ? C225 C230 H230 119.2 . . ? C229 C230 C225 121.7(2) . . ? C229 C230 H230 119.2 . . ? F19 C231 C227 111.6(4) . . ? F19A C231 C227 112.0(4) . . ? F20 C231 C227 114.8(4) . . ? F20 C231 F19 105.2(5) . . ? F20 C231 F21 107.0(5) . . ? F20A C231 C227 113.3(4) . . ? F20A C231 F19A 105.0(5) . . ? F20A C231 F21A 107.4(5) . . ? F21 C231 C227 113.4(4) . . ? F21 C231 F19 103.8(4) . . ? F21A C231 C227 112.5(4) . . ? F21A C231 F19A 106.1(5) . . ? F22 C232 C229 112.0(3) . . ? F23 C232 C229 113.1(2) . . ? F23 C232 F22 105.0(3) . . ? F24 C232 C229 114.1(2) . . ? F24 C232 F22 105.4(3) . . ? F24 C232 F23 106.6(3) . . ? 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 Ir1 C4 N5 C6 166.95(18) . . . . ? Ir1 C4 N5 C9 4.9(4) . . . . ? Ir1 C4 N8 C7 -165.8(2) . . . . ? Ir1 C4 N8 C12 3.1(5) . . . . ? Ir1 C19 N20 C21 172.9(2) . . . . ? Ir1 C19 N20 C24 23.7(4) . . . . ? Ir1 C19 N23 C22 -172.7(2) . . . . ? Ir1 C19 N23 C27 -0.2(5) . . . . ? C6 C7 N8 C4 -2.6(3) . . . . ? C6 C7 N8 C12 -174.7(2) . . . . ? C6 C7 O14 C13 -171.0(4) . . . . ? C7 C6 N5 C4 2.6(3) . . . . ? C7 C6 N5 C9 170.3(2) . . . . ? C7 C6 O11 C10 170.9(4) . . . . ? C9 C10 O11 C6 28.6(3) . . . . ? C10 C9 N5 C4 -175.6(3) . . . . ? C10 C9 N5 C6 21.8(3) . . . . ? C12 C13 O14 C7 -21.6(3) . . . . ? C13 C12 N8 C4 175.2(3) . . . . ? C13 C12 N8 C7 -15.6(3) . . . . ? C15 C9 C10 O11 83.6(3) . . . . ? C15 C9 N5 C4 68.3(4) . . . . ? C15 C9 N5 C6 -94.4(3) . . . . ? C16 C9 C10 O11 -151.4(2) . . . . ? C16 C9 N5 C4 -61.1(4) . . . . ? C16 C9 N5 C6 136.2(3) . . . . ? C17 C12 C13 O14 -92.2(3) . . . . ? C17 C12 N8 C4 -68.4(4) . . . . ? C17 C12 N8 C7 100.9(3) . . . . ? C18 C12 C13 O14 141.2(3) . . . . ? C18 C12 N8 C4 60.1(4) . . . . ? C18 C12 N8 C7 -130.7(2) . . . . ? C21 C22 N23 C19 -0.6(3) . . . . ? C21 C22 N23 C27 -175.3(3) . . . . ? C21 C22 O29 C28 160.1(5) . . . . ? C22 C21 N20 C19 1.2(4) . . . . ? C22 C21 N20 C24 159.6(3) . . . . ? C22 C21 O26 C25 -178.5(4) . . . . ? C24 C25 O26 C21 25.6(4) . . . . ? C25 C24 N20 C19 177.4(3) . . . . ? C25 C24 N20 C21 27.1(3) . . . . ? C27 C28 O29 C22 26.7(4) . . . . ? C28 C27 N23 C19 -161.6(3) . . . . ? C28 C27 N23 C22 11.1(3) . . . . ? C30 C24 C25 O26 81.0(3) . . . . ? C30 C24 N20 C19 61.6(4) . . . . ? C30 C24 N20 C21 -88.7(3) . . . . ? C31 C24 C25 O26 -154.2(3) . . . . ? C31 C24 N20 C19 -67.8(4) . . . . ? C31 C24 N20 C21 141.8(3) . . . . ? C32 C27 C28 O29 -139.3(3) . . . . ? C32 C27 N23 C19 -48.2(4) . . . . ? C32 C27 N23 C22 124.5(3) . . . . ? C33 C27 C28 O29 94.7(4) . . . . ? C33 C27 N23 C19 79.4(4) . . . . ? C33 C27 N23 C22 -107.9(3) . . . . ? C35 C36 C37 C38 -1.3(5) . . . . ? C36 C35 N34 Ir1 178.4(2) . . . . ? C36 C35 N34 C39 3.0(4) . . . . ? C36 C37 C38 C39 1.2(5) . . . . ? C37 C38 C39 C40 -176.2(3) . . . . ? C37 C38 C39 N34 0.9(5) . . . . ? C38 C39 C40 C41 -8.0(4) . . . . ? C38 C39 C40 N45 168.2(3) . . . . ? C38 C39 N34 Ir1 -178.8(2) . . . . ? C38 C39 N34 C35 -3.0(4) . . . . ? C39 C40 C41 C42 173.4(3) . . . . ? C39 C40 N45 Ir1 15.0(3) . . . . ? C39 C40 N45 C44 -174.2(2) . . . . ? C40 C39 N34 Ir1 -1.4(3) . . . . ? C40 C39 N34 C35 174.4(2) . . . . ? C40 C41 C42 C43 0.2(5) . . . . ? C41 C40 N45 Ir1 -168.8(2) . . . . ? C41 C40 N45 C44 2.1(4) . . . . ? C41 C42 C43 C44 2.5(4) . . . . ? C42 C43 C44 N45 -3.1(4) . . . . ? C43 C44 N45 Ir1 170.5(2) . . . . ? C43 C44 N45 C40 0.8(4) . . . . ? N5 C4 N8 C7 3.9(3) . . . . ? N5 C4 N8 C12 172.8(3) . . . . ? N5 C6 C7 N8 0.0(3) . . . . ? N5 C6 C7 O14 -177.8(3) . . . . ? N5 C6 O11 C10 -14.5(3) . . . . ? N5 C9 C10 O11 -30.7(3) . . . . ? N8 C4 N5 C6 -3.9(3) . . . . ? N8 C4 N5 C9 -166.0(3) . . . . ? N8 C7 O14 C13 11.4(3) . . . . ? N8 C12 C13 O14 22.7(3) . . . . ? N20 C19 N23 C22 1.3(3) . . . . ? N20 C19 N23 C27 173.7(3) . . . . ? N20 C21 C22 N23 -0.3(4) . . . . ? N20 C21 C22 O29 179.8(4) . . . . ? N20 C21 O26 C25 -7.4(4) . . . . ? N20 C24 C25 O26 -32.2(3) . . . . ? N23 C19 N20 C21 -1.4(3) . . . . ? N23 C19 N20 C24 -150.7(3) . . . . ? N23 C22 O29 C28 -19.8(4) . . . . ? N23 C27 C28 O29 -23.1(4) . . . . ? N34 C35 C36 C37 -0.9(5) . . . . ? N34 C39 C40 C41 174.7(3) . . . . ? N34 C39 C40 N45 -9.1(3) . . . . ? N45 C40 C41 C42 -2.6(4) . . . . ? O11 C6 C7 N8 174.8(3) . . . . ? O11 C6 C7 O14 -2.9(7) . . . . ? O11 C6 N5 C4 -173.7(2) . . . . ? O11 C6 N5 C9 -6.0(3) . . . . ? O14 C7 N8 C4 175.8(2) . . . . ? O14 C7 N8 C12 3.7(3) . . . . ? O26 C21 C22 N23 171.2(4) . . . . ? O26 C21 C22 O29 -8.7(8) . . . . ? O26 C21 N20 C19 -172.6(3) . . . . ? O26 C21 N20 C24 -14.2(4) . . . . ? O29 C22 N23 C19 179.3(2) . . . . ? O29 C22 N23 C27 4.6(3) . . . . ? B200 C201 C202 C203 165.8(2) . . . . ? B200 C201 C206 C205 -166.9(3) . . . . ? B200 C209 C210 C211 -171.1(2) . . . . ? B200 C209 C214 C213 171.6(2) . . . . ? B200 C217 C218 C219 170.4(2) . . . . ? B200 C217 C222 C221 -170.4(2) . . . . ? B200 C225 C226 C227 -171.9(2) . . . . ? B200 C225 C230 C229 170.9(2) . . . . ? C201 B200 C209 C210 79.8(3) . . . . ? C201 B200 C209 C214 -90.0(3) . . . . ? C201 B200 C217 C218 151.1(2) . . . . ? C201 B200 C217 C222 -38.9(3) . . . . ? C201 B200 C225 C226 -145.5(2) . . . . ? C201 B200 C225 C230 43.7(3) . . . . ? C201 C202 C203 C204 1.9(4) . . . . ? C201 C202 C203 C207 -177.7(2) . . . . ? C202 C201 C206 C205 1.4(4) . . . . ? C202 C203 C204 C205 0.1(4) . . . . ? C202 C203 C207 F0AA 133.7(3) . . . . ? C202 C203 C207 F1 -107.0(3) . . . . ? C202 C203 C207 F1AA 13.5(4) . . . . ? C203 C204 C205 C206 -1.2(4) . . . . ? C203 C204 C205 C208 -178.4(3) . . . . ? C204 C203 C207 F0AA -46.0(4) . . . . ? C204 C203 C207 F1 73.4(3) . . . . ? C204 C203 C207 F1AA -166.1(2) . . . . ? C204 C205 C206 C201 0.5(4) . . . . ? C204 C205 C208 F4 -128.4(4) . . . . ? C204 C205 C208 F4A 56.1(7) . . . . ? C204 C205 C208 F5 -12.1(5) . . . . ? C204 C205 C208 F5A 172.8(9) . . . . ? C204 C205 C208 F6 117.8(5) . . . . ? C204 C205 C208 F6A -56.5(8) . . . . ? C206 C201 C202 C203 -2.6(4) . . . . ? C206 C205 C208 F4 54.4(4) . . . . ? C206 C205 C208 F4A -121.2(7) . . . . ? C206 C205 C208 F5 170.7(4) . . . . ? C206 C205 C208 F5A -4.4(9) . . . . ? C206 C205 C208 F6 -59.4(5) . . . . ? C206 C205 C208 F6A 126.3(8) . . . . ? C207 C203 C204 C205 179.7(3) . . . . ? C208 C205 C206 C201 177.6(3) . . . . ? C209 B200 C201 C202 -82.8(3) . . . . ? C209 B200 C201 C206 84.9(3) . . . . ? C209 B200 C217 C218 35.5(3) . . . . ? C209 B200 C217 C222 -154.4(2) . . . . ? C209 B200 C225 C226 -31.4(3) . . . . ? C209 B200 C225 C230 157.8(2) . . . . ? C209 C210 C211 C212 -0.2(4) . . . . ? C209 C210 C211 C215 177.3(3) . . . . ? C210 C209 C214 C213 1.2(4) . . . . ? C210 C211 C212 C213 0.3(4) . . . . ? C210 C211 C215 F7 166.1(3) . . . . ? C210 C211 C215 F8 -75.8(4) . . . . ? C210 C211 C215 F9 45.3(4) . . . . ? C211 C212 C213 C214 0.3(4) . . . . ? C211 C212 C213 C216 -179.7(2) . . . . ? C212 C211 C215 F7 -16.4(4) . . . . ? C212 C211 C215 F8 101.7(4) . . . . ? C212 C211 C215 F9 -137.2(3) . . . . ? C212 C213 C214 C209 -1.2(4) . . . . ? C212 C213 C216 F10 123.3(3) . . . . ? C212 C213 C216 F11 1.9(4) . . . . ? C212 C213 C216 F12 -118.4(3) . . . . ? C214 C209 C210 C211 -0.6(4) . . . . ? C214 C213 C216 F10 -56.7(4) . . . . ? C214 C213 C216 F11 -178.2(2) . . . . ? C214 C213 C216 F12 61.5(3) . . . . ? C215 C211 C212 C213 -177.2(3) . . . . ? C216 C213 C214 C209 178.9(2) . . . . ? C217 B200 C201 C202 154.4(2) . . . . ? C217 B200 C201 C206 -38.0(3) . . . . ? C217 B200 C209 C210 -157.4(2) . . . . ? C217 B200 C209 C214 32.8(3) . . . . ? C217 B200 C225 C226 91.3(3) . . . . ? C217 B200 C225 C230 -79.5(3) . . . . ? C217 C218 C219 C220 -0.2(4) . . . . ? C217 C218 C219 C223 178.9(3) . . . . ? C218 C217 C222 C221 0.3(4) . . . . ? C218 C219 C220 C221 0.2(4) . . . . ? C218 C219 C223 F13 131.5(5) . . . . ? C218 C219 C223 F13A -67.2(9) . . . . ? C218 C219 C223 F14 4.2(6) . . . . ? C218 C219 C223 F14A 164.5(8) . . . . ? C218 C219 C223 F15 -113.2(5) . . . . ? C218 C219 C223 F15A 50.4(7) . . . . ? C219 C220 C221 C222 0.1(4) . . . . ? C219 C220 C221 C224 -177.6(3) . . . . ? C220 C219 C223 F13 -49.4(5) . . . . ? C220 C219 C223 F13A 111.9(9) . . . . ? C220 C219 C223 F14 -176.6(6) . . . . ? C220 C219 C223 F14A -16.4(9) . . . . ? C220 C219 C223 F15 66.0(5) . . . . ? C220 C219 C223 F15A -130.4(7) . . . . ? C220 C221 C222 C217 -0.3(4) . . . . ? C220 C221 C224 F16 -14.0(4) . . . . ? C220 C221 C224 F17 -135.6(3) . . . . ? C220 C221 C224 F18 106.6(3) . . . . ? C222 C217 C218 C219 0.0(4) . . . . ? C222 C221 C224 F16 168.3(3) . . . . ? C222 C221 C224 F17 46.7(4) . . . . ? C222 C221 C224 F18 -71.1(4) . . . . ? C223 C219 C220 C221 -178.9(3) . . . . ? C224 C221 C222 C217 177.3(2) . . . . ? C225 B200 C201 C202 37.9(3) . . . . ? C225 B200 C201 C206 -154.5(2) . . . . ? C225 B200 C209 C210 -41.6(3) . . . . ? C225 B200 C209 C214 148.6(2) . . . . ? C225 B200 C217 C218 -86.0(3) . . . . ? C225 B200 C217 C222 84.0(3) . . . . ? C225 C226 C227 C228 1.0(4) . . . . ? C225 C226 C227 C231 179.0(3) . . . . ? C226 C225 C230 C229 -0.4(4) . . . . ? C226 C227 C228 C229 -0.2(4) . . . . ? C226 C227 C231 F19 -123.1(7) . . . . ? C226 C227 C231 F19A 34.0(10) . . . . ? C226 C227 C231 F20 -3.5(8) . . . . ? C226 C227 C231 F20A 152.5(8) . . . . ? C226 C227 C231 F21 120.0(8) . . . . ? C226 C227 C231 F21A -85.4(11) . . . . ? C227 C228 C229 C230 -0.9(4) . . . . ? C227 C228 C229 C232 175.4(3) . . . . ? C228 C227 C231 F19 54.9(7) . . . . ? C228 C227 C231 F19A -147.9(9) . . . . ? C228 C227 C231 F20 174.6(8) . . . . ? C228 C227 C231 F20A -29.4(9) . . . . ? C228 C227 C231 F21 -61.9(8) . . . . ? C228 C227 C231 F21A 92.6(11) . . . . ? C228 C229 C230 C225 1.2(4) . . . . ? C228 C229 C232 F22 -70.8(3) . . . . ? C228 C229 C232 F23 47.6(4) . . . . ? C228 C229 C232 F24 169.7(3) . . . . ? C230 C225 C226 C227 -0.7(4) . . . . ? C230 C229 C232 F22 105.5(3) . . . . ? C230 C229 C232 F23 -136.1(3) . . . . ? C230 C229 C232 F24 -14.0(4) . . . . ? C231 C227 C228 C229 -178.2(3) . . . . ? C232 C229 C230 C225 -175.0(2) . . . . ? _shelx_SHELXL_version_number '2014/7' _olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)' _olex2_submission_special_instructions 'No special instructions were received' #===END data_0057abc14 #==================================================================== # [Ir(IBioxMe4)3(H)2][BArF4].C6H4F2 (Z' = 2) #-------------------------------------------------------------------- # Collected and solved by Adrian Chaplin #-------------------------------------------------------------------- # Start Validation Reply Form _vrf_PLAT041_0057abc14 ; PROBLEM: Calc. and Reported SumFormula Strings Differ Please Check RESPONSE: The hydride ligands were not located. ; _vrf_PLAT112_0057abc14 ; PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... b/2 Check RESPONSE: Checked. ; _vrf_PLAT301_0057abc14 ; PROBLEM: Main Residue Disorder ............ Percentage = 9 Note RESPONSE: The structure contains a significant degree of disorder. See _publ_section_exptl_refinement. ; # End Validation Reply Form #-------------------------------------------------------------------- _publ_contact_author_name 'Adrian B. Chaplin' _publ_contact_author_email a.b.chaplin@warwick.ac.uk _publ_section_exptl_refinement ; Solved with SHELXT-XX by direct methods. Refined full-matrix least squares on F2 using SHELXL-2014. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions and refined using the riding model. The hydride ligands were not located. Disorder present in some of the NHC ligands was treated by modelling the appropriate parts over two sites and restraining their geometry. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; #==================================================================== _audit_creation_date 2015-06-18 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C33 H48 Ir N6 O6, C6 H4 F2, C32 H12 B F24' _chemical_formula_sum 'C71 H66 B F26 Ir N6 O6' _chemical_formula_weight 1796.30 _chemical_absolute_configuration . _chemical_melting_point 'not measured' 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.2120(3) _cell_length_b 19.9992(2) _cell_length_c 20.9223(3) _cell_angle_alpha 99.7323(12) _cell_angle_beta 99.5664(14) _cell_angle_gamma 100.4143(12) _cell_volume 7233.26(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 37277 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 31.6950 _cell_measurement_theta_min 2.9800 _shelx_estimated_absorpt_T_max . _shelx_estimated_absorpt_T_min . _exptl_absorpt_coefficient_mu 1.970 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.79397 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details . _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 3592 _exptl_crystal_recrystallization_method 'Crystals grown from C6H4F2-heptane at 278 K' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_special_details . _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 87194 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 27.103 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 2.976 _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2833 _diffrn_detector_type Ruby _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 19.00 44.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 17.3155 -38.0000 150.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -59.00 -30.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 17.3155 -38.0000 150.0000 29 #__ type_ start__ end____ width___ exp.time_ 3 omega 14.00 93.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 17.3155 38.0000 60.0000 79 #__ type_ start__ end____ width___ exp.time_ 4 omega -52.00 44.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 17.3155 -38.0000 -120.0000 96 #__ type_ start__ end____ width___ exp.time_ 5 omega 35.00 81.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 17.3155 178.0000 -90.0000 46 #__ type_ start__ end____ width___ exp.time_ 6 omega -104.00 -59.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -18.2530 -178.0000 -30.0000 45 #__ type_ start__ end____ width___ exp.time_ 7 omega -108.00 -83.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -18.2530 -178.0000 0.0000 25 #__ type_ start__ end____ width___ exp.time_ 8 omega -37.00 5.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -18.2530 -57.0000 60.0000 42 #__ type_ start__ end____ width___ exp.time_ 9 omega -23.00 24.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -18.2530 -99.0000 -60.0000 47 #__ type_ start__ end____ width___ exp.time_ 10 omega -107.00 -78.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - -18.2530 -178.0000 120.0000 29 #__ type_ start__ end____ width___ exp.time_ 11 omega -9.00 38.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 17.3155 38.0000 -90.0000 47 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction: Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0185289000 _diffrn_orient_matrix_UB_12 -0.0009925000 _diffrn_orient_matrix_UB_13 -0.0272979000 _diffrn_orient_matrix_UB_21 -0.0357778000 _diffrn_orient_matrix_UB_22 -0.0059292000 _diffrn_orient_matrix_UB_23 -0.0219054000 _diffrn_orient_matrix_UB_31 0.0034788000 _diffrn_orient_matrix_UB_32 0.0363513000 _diffrn_orient_matrix_UB_33 0.0029905000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 26299 _reflns_number_total 31874 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.937 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.078 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 2191 _refine_ls_number_reflns 31874 _refine_ls_number_restraints 1092 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0304 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+4.7347P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.0762 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C408-F404 \\sim C408-F405 \\sim C408-F406 \\sim C408-F504 \\sim C408-F505 \\sim C408-F506 with sigma of 0.01 F404-F405 \\sim F405-F406 \\sim F406-F404 \\sim F504-F505 \\sim F505-F506 \\sim F506-F504 with sigma of 0.01 C405-F404 \\sim C405-F405 \\sim C405-F406 \\sim C405-F504 \\sim C405-F505 \\sim C405-F506 with sigma of 0.01 C424-F416 \\sim C424-F417 \\sim C424-F418 \\sim C424-F516 \\sim C424-F517 \\sim C424-F518 with sigma of 0.01 F416-F417 \\sim F417-F418 \\sim F418-F416 \\sim F516-F517 \\sim F517-F518 \\sim F518-F516 with sigma of 0.01 C421-F416 \\sim C421-F417 \\sim C421-F418 \\sim C421-F516 \\sim C421-F517 \\sim C421-F518 with sigma of 0.01 C432-F422 \\sim C432-F423 \\sim C432-F424 \\sim C432-F522 \\sim C432-F523 \\sim C432-F524 with sigma of 0.01 F422-F423 \\sim F423-F424 \\sim F424-F422 \\sim F522-F523 \\sim F523-F524 \\sim F524-F522 with sigma of 0.01 C429-F422 \\sim C429-F423 \\sim C429-F424 \\sim C429-F522 \\sim C429-F523 \\sim C429-F524 with sigma of 0.01 C207-F201 \\sim C207-F202 \\sim C207-F203 \\sim C207-F301 \\sim C207-F302 \\sim C207-F303 with sigma of 0.01 F201-F202 \\sim F202-F203 \\sim F203-F201 \\sim F301-F302 \\sim F302-F303 \\sim F303-F301 with sigma of 0.01 C203-F201 \\sim C203-F202 \\sim C203-F203 \\sim C203-F301 \\sim C203-F302 \\sim C203-F303 with sigma of 0.01 C224-F216 \\sim C224-F217 \\sim C224-F218 \\sim C224-F316 \\sim C224-F317 \\sim C224-F318 with sigma of 0.01 F216-F217 \\sim F217-F218 \\sim F218-F216 \\sim F316-F317 \\sim F317-F318 \\sim F318-F316 with sigma of 0.01 C221-F216 \\sim C221-F217 \\sim C221-F218 \\sim C221-F316 \\sim C221-F317 \\sim C221-F318 with sigma of 0.01 C15A-C16A \\sim C15B-C16B with sigma of 0.01 C10A-C16A \\sim C10A-C16B \\sim C15A-C10A \\sim C15B-C10A with sigma of 0.01 C11B-C10A \\sim C11A-C10A with sigma of 0.01 O12A-C11B \\sim O12A-C11A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints C30 \\sim C31 \\sim C25 \\sim C26 \\sim O27 \\sim C20 \\sim N21 \\sim C17 \\sim N18 \\sim C19 \\sim O24 \\sim C23 \\sim C28 \\sim C22 \\sim C29 \\sim C16A \\sim C16B \\sim C10A \\sim C15A \\sim C15B \\sim C11B \\sim C11A \\sim O12A \\sim F907 \\sim F908 \\sim F401 \\sim F402 \\sim F403 \\sim F404 \\sim F405 \\sim F406 \\sim F407 \\sim F408 \\sim F409 \\sim F410 \\sim F411 \\sim F412 \\sim F413 \\sim F414 \\sim F415 \\sim F416 \\sim F417 \\sim F418 \\sim F419 \\sim F420 \\sim F421 \\sim F422 \\sim F423 \\sim F424 \\sim F504 \\sim F505 \\sim F506 \\sim F516 \\sim F517 \\sim F518 \\sim F522 \\sim F523 \\sim F524 \\sim F201 \\sim F202 \\sim F203 \\sim F204 \\sim F205 \\sim F206 \\sim F207 \\sim F208 \\sim F209 \\sim F210 \\sim F211 \\sim F212 \\sim F213 \\sim F214 \\sim F215 \\sim F216 \\sim F217 \\sim F218 \\sim F219 \\sim F220 \\sim F221 \\sim F222 \\sim F223 \\sim F224 \\sim F301 \\sim F302 \\sim F303 \\sim F316 \\sim F317 \\sim F318 \\sim F915 \\sim F916: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.02 Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(N21) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N18) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(C11B) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(O12A) \\sim Ueq, Uanis(F907) \\sim Ueq, Uanis(F908) \\sim Ueq, Uanis(F401) \\sim Ueq, Uanis(F402) \\sim Ueq, Uanis(F403) \\sim Ueq, Uanis(F404) \\sim Ueq, Uanis(F405) \\sim Ueq, Uanis(F406) \\sim Ueq, Uanis(F407) \\sim Ueq, Uanis(F408) \\sim Ueq, Uanis(F409) \\sim Ueq, Uanis(F410) \\sim Ueq, Uanis(F411) \\sim Ueq, Uanis(F412) \\sim Ueq, Uanis(F413) \\sim Ueq, Uanis(F414) \\sim Ueq, Uanis(F415) \\sim Ueq, Uanis(F416) \\sim Ueq, Uanis(F417) \\sim Ueq, Uanis(F418) \\sim Ueq, Uanis(F419) \\sim Ueq, Uanis(F420) \\sim Ueq, Uanis(F421) \\sim Ueq, Uanis(F422) \\sim Ueq, Uanis(F423) \\sim Ueq, Uanis(F424) \\sim Ueq, Uanis(F504) \\sim Ueq, Uanis(F505) \\sim Ueq, Uanis(F506) \\sim Ueq, Uanis(F516) \\sim Ueq, Uanis(F517) \\sim Ueq, Uanis(F518) \\sim Ueq, Uanis(F522) \\sim Ueq, Uanis(F523) \\sim Ueq, Uanis(F524) \\sim Ueq, Uanis(F201) \\sim Ueq, Uanis(F202) \\sim Ueq, Uanis(F203) \\sim Ueq, Uanis(F204) \\sim Ueq, Uanis(F205) \\sim Ueq, Uanis(F206) \\sim Ueq, Uanis(F207) \\sim Ueq, Uanis(F208) \\sim Ueq, Uanis(F209) \\sim Ueq, Uanis(F210) \\sim Ueq, Uanis(F211) \\sim Ueq, Uanis(F212) \\sim Ueq, Uanis(F213) \\sim Ueq, Uanis(F214) \\sim Ueq, Uanis(F215) \\sim Ueq, Uanis(F216) \\sim Ueq, Uanis(F217) \\sim Ueq, Uanis(F218) \\sim Ueq, Uanis(F219) \\sim Ueq, Uanis(F220) \\sim Ueq, Uanis(F221) \\sim Ueq, Uanis(F222) \\sim Ueq, Uanis(F223) \\sim Ueq, Uanis(F224) \\sim Ueq, Uanis(F301) \\sim Ueq, Uanis(F302) \\sim Ueq, Uanis(F303) \\sim Ueq, Uanis(F316) \\sim Ueq, Uanis(F317) \\sim Ueq, Uanis(F318) \\sim Ueq, Uanis(F915) \\sim Ueq, Uanis(F916) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008 4. Others Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)= Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1) Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=Sof(H15C)= Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1) Sof(F522)=Sof(F523)=Sof(F524)=1-FVAR(2) Sof(F422)=Sof(F423)=Sof(F424)=FVAR(2) Sof(F504)=Sof(F505)=Sof(F506)=1-FVAR(3) Sof(F404)=Sof(F405)=Sof(F406)=FVAR(3) Sof(F516)=Sof(F517)=Sof(F518)=1-FVAR(4) Sof(F416)=Sof(F417)=Sof(F418)=FVAR(4) Fixed Sof: F201(0.5) F202(0.5) F203(0.5) F216(0.5) F217(0.5) F218(0.5) F301(0.5) F302(0.5) F303(0.5) F316(0.5) F317(0.5) F318(0.5) 5.a Secondary CH2 refined with riding coordinates: C8(H8A,H8B), C11(H11E,H11F), C23(H23C,H23D), C26(H26C,H26D), C38(H38C,H38D), C41(H41C,H41D), C8A(H8AA,H8AB), C11A(H11A,H11B), C11B(H11C,H11D), C23A(H23A, H23B), C26A(H26A,H26B), C38A(H38A,H38B), C41A(H41A,H41B) 5.b Aromatic/amide H refined with riding coordinates: C903(H903), C904(H904), C905(H905), C906(H906), C402(H402), C404(H404), C406(H406), C410(H410), C412(H412), C414(H414), C418(H418), C420(H420), C422(H422), C426(H426), C428(H428), C430(H430), C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230), C911(H911), C912(H912), C913(H913), C914(H914) 5.c Idealised Me refined as rotating group: C13(H13D,H13E,H13F), C14(H14D,H14E,H14F), C15(H15G,H15H,H15I), C16(H16G,H16H, H16I), C28(H28D,H28E,H28F), C29(H29D,H29E,H29F), C30(H30D,H30E,H30F), C31(H31D, H31E,H31F), C43(H43D,H43E,H43F), C44(H44D,H44E,H44F), C45(H45D,H45E,H45F), C46(H46D,H46E,H46F), C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C15A(H15A, H15B,H15C), C15B(H15D,H15E,H15F), C16A(H16A,H16B,H16C), C16B(H16D,H16E,H16F), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C31A(H31A, H31B,H31C), C43A(H43A,H43B,H43C), C44A(H44A,H44B,H44C), C45A(H45A,H45B,H45C), C46A(H46A,H46B,H46C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.20439(2) 0.41694(2) 0.26680(2) 0.01696(3) Uani 1 1 d . . . . . O9 O 0.30439(10) 0.56745(9) 0.09804(9) 0.0251(4) Uani 1 1 d . . . . . O12 O 0.11540(11) 0.56782(10) 0.08606(10) 0.0285(4) Uani 1 1 d . . . . . O24 O 0.27814(16) 0.39119(15) 0.52080(12) 0.0608(7) Uani 1 1 d . U . . . O27 O 0.29782(16) 0.24525(14) 0.41987(14) 0.0617(7) Uani 1 1 d . U . . . O39 O -0.05570(12) 0.21412(10) 0.21372(11) 0.0352(5) Uani 1 1 d . . . . . O42 O 0.02153(13) 0.20105(10) 0.07613(10) 0.0376(5) Uani 1 1 d . . . . . N3 N 0.26147(12) 0.49988(10) 0.16850(10) 0.0179(4) Uani 1 1 d . . . . . N6 N 0.14451(11) 0.50062(10) 0.16179(10) 0.0173(4) Uani 1 1 d . . . . . N18 N 0.23733(14) 0.40389(13) 0.41454(12) 0.0344(6) Uani 1 1 d . U . . . N21 N 0.25312(14) 0.31425(13) 0.35268(13) 0.0346(6) Uani 1 1 d . U . . . N33 N 0.05152(12) 0.30176(10) 0.23830(10) 0.0190(4) Uani 1 1 d . . . . . N36 N 0.10126(13) 0.29233(10) 0.15335(11) 0.0216(5) Uani 1 1 d . . . . . C2 C 0.20097(14) 0.47463(12) 0.19500(12) 0.0172(5) Uani 1 1 d . . . . . C4 C 0.24378(15) 0.53967(12) 0.12241(13) 0.0204(5) Uani 1 1 d . . . . . C5 C 0.17000(15) 0.54018(12) 0.11805(13) 0.0199(5) Uani 1 1 d . . . . . C7 C 0.34621(15) 0.51143(14) 0.18617(14) 0.0242(6) Uani 1 1 d . . . . . C8 C 0.36299(15) 0.53133(15) 0.12122(14) 0.0275(6) Uani 1 1 d . . . . . H8A H 0.4132 0.5613 0.1290 0.033 Uiso 1 1 calc R . . . . H8B H 0.3612 0.4901 0.0886 0.033 Uiso 1 1 calc R . . . . C10 C 0.06539(15) 0.50940(13) 0.16596(14) 0.0234(6) Uani 1 1 d . . . . . C11 C 0.04448(16) 0.53060(15) 0.09909(15) 0.0298(6) Uani 1 1 d . . . . . H11E H 0.0222 0.4898 0.0643 0.036 Uiso 1 1 calc R . . . . H11F H 0.0080 0.5603 0.1012 0.036 Uiso 1 1 calc R . . . . C13 C 0.37591(18) 0.57348(16) 0.24430(15) 0.0374(7) Uani 1 1 d . . . . . H13D H 0.3584 0.6132 0.2329 0.056 Uiso 1 1 calc GR . . . . H13E H 0.4306 0.5835 0.2540 0.056 Uiso 1 1 calc GR . . . . H13F H 0.3574 0.5626 0.2825 0.056 Uiso 1 1 calc GR . . . . C14 C 0.37658(16) 0.44840(16) 0.19947(17) 0.0350(7) Uani 1 1 d . . . . . H14D H 0.3611 0.4353 0.2381 0.052 Uiso 1 1 calc GR . . . . H14E H 0.4312 0.4593 0.2067 0.052 Uiso 1 1 calc GR . . . . H14F H 0.3566 0.4106 0.1621 0.052 Uiso 1 1 calc GR . . . . C15 C 0.07088(18) 0.56874(16) 0.22375(16) 0.0383(8) Uani 1 1 d . . . . . H15G H 0.0912 0.5563 0.2644 0.057 Uiso 1 1 calc GR . . . . H15H H 0.0211 0.5777 0.2251 0.057 Uiso 1 1 calc GR . . . . H15I H 0.1039 0.6097 0.2183 0.057 Uiso 1 1 calc GR . . . . C16 C 0.01178(16) 0.44388(15) 0.17051(16) 0.0326(7) Uani 1 1 d . . . . . H16G H 0.0099 0.4077 0.1333 0.049 Uiso 1 1 calc GR . . . . H16H H -0.0383 0.4527 0.1703 0.049 Uiso 1 1 calc GR . . . . H16I H 0.0298 0.4296 0.2108 0.049 Uiso 1 1 calc GR . . . . C17 C 0.23085(16) 0.37553(15) 0.34869(14) 0.0274(6) Uani 1 1 d . U . . . C19 C 0.2646(2) 0.3606(2) 0.45522(16) 0.0442(7) Uani 1 1 d . U . . . C20 C 0.2737(2) 0.3051(2) 0.41697(18) 0.0462(8) Uani 1 1 d . U . . . C22 C 0.2466(2) 0.47402(18) 0.45606(16) 0.0434(8) Uani 1 1 d . U . . . C23 C 0.2459(2) 0.4506(2) 0.52340(17) 0.0539(9) Uani 1 1 d . U . . . H23C H 0.2755 0.4875 0.5596 0.065 Uiso 1 1 calc R . . . . H23D H 0.1941 0.4396 0.5303 0.065 Uiso 1 1 calc R . . . . C25 C 0.26980(19) 0.25644(17) 0.30685(18) 0.0416(7) Uani 1 1 d . U . . . C26 C 0.3218(2) 0.2292(2) 0.3576(2) 0.0609(9) Uani 1 1 d . U . . . H26C H 0.3165 0.1795 0.3439 0.073 Uiso 1 1 calc R . . . . H26D H 0.3747 0.2517 0.3618 0.073 Uiso 1 1 calc R . . . . C28 C 0.3254(2) 0.5171(2) 0.45631(19) 0.0729(14) Uani 1 1 d . U . . . H28D H 0.3640 0.4930 0.4711 0.109 Uiso 1 1 calc GR . . . . H28E H 0.3336 0.5614 0.4857 0.109 Uiso 1 1 calc GR . . . . H28F H 0.3280 0.5239 0.4123 0.109 Uiso 1 1 calc GR . . . . C29 C 0.1842(3) 0.51163(19) 0.43840(19) 0.0660(12) Uani 1 1 d . U . . . H29D H 0.1850 0.5226 0.3955 0.099 Uiso 1 1 calc GR . . . . H29E H 0.1919 0.5538 0.4708 0.099 Uiso 1 1 calc GR . . . . H29F H 0.1358 0.4826 0.4376 0.099 Uiso 1 1 calc GR . . . . C30 C 0.3119(2) 0.2846(2) 0.2573(2) 0.0549(10) Uani 1 1 d . U . . . H30D H 0.2803 0.3076 0.2311 0.082 Uiso 1 1 calc GR . . . . H30E H 0.3243 0.2470 0.2290 0.082 Uiso 1 1 calc GR . . . . H30F H 0.3580 0.3171 0.2804 0.082 Uiso 1 1 calc GR . . . . C31 C 0.1986(2) 0.20244(17) 0.2746(2) 0.0507(9) Uani 1 1 d . U . . . H31D H 0.1749 0.1855 0.3081 0.076 Uiso 1 1 calc GR . . . . H31E H 0.2115 0.1647 0.2470 0.076 Uiso 1 1 calc GR . . . . H31F H 0.1640 0.2227 0.2480 0.076 Uiso 1 1 calc GR . . . . C32 C 0.11372(14) 0.33243(12) 0.21599(13) 0.0184(5) Uani 1 1 d . . . . . C34 C 0.00526(16) 0.24552(14) 0.19221(14) 0.0264(6) Uani 1 1 d . . . . . C35 C 0.03587(17) 0.24001(13) 0.13870(14) 0.0277(6) Uani 1 1 d . . . . . C37 C 0.01893(15) 0.30846(13) 0.29990(13) 0.0224(5) Uani 1 1 d . . . . . C38 C -0.06223(16) 0.26600(15) 0.26858(15) 0.0310(6) Uani 1 1 d . . . . . H38C H -0.0844 0.2439 0.3008 0.037 Uiso 1 1 calc R . . . . H38D H -0.0945 0.2960 0.2530 0.037 Uiso 1 1 calc R . . . . C40 C 0.13061(17) 0.29319(13) 0.09045(14) 0.0281(6) Uani 1 1 d . . . . . C41 C 0.09328(18) 0.21752(14) 0.05502(15) 0.0325(7) Uani 1 1 d . . . . . H41C H 0.0847 0.2132 0.0074 0.039 Uiso 1 1 calc R . . . . H41D H 0.1258 0.1864 0.0674 0.039 Uiso 1 1 calc R . . . . C43 C 0.05784(17) 0.27268(17) 0.34970(16) 0.0357(7) Uani 1 1 d . . . . . H43D H 0.0558 0.2255 0.3290 0.054 Uiso 1 1 calc GR . . . . H43E H 0.0323 0.2731 0.3863 0.054 Uiso 1 1 calc GR . . . . H43F H 0.1101 0.2967 0.3653 0.054 Uiso 1 1 calc GR . . . . C44 C 0.01682(19) 0.38211(15) 0.32969(16) 0.0365(7) Uani 1 1 d . . . . . H44D H 0.0677 0.4099 0.3418 0.055 Uiso 1 1 calc GR . . . . H44E H -0.0052 0.3825 0.3684 0.055 Uiso 1 1 calc GR . . . . H44F H -0.0135 0.4007 0.2979 0.055 Uiso 1 1 calc GR . . . . C45 C 0.21621(18) 0.30750(17) 0.10087(17) 0.0444(9) Uani 1 1 d . . . . . H45D H 0.2372 0.3523 0.1292 0.067 Uiso 1 1 calc GR . . . . H45E H 0.2312 0.3068 0.0590 0.067 Uiso 1 1 calc GR . . . . H45F H 0.2347 0.2725 0.1211 0.067 Uiso 1 1 calc GR . . . . C46 C 0.0974(2) 0.34305(15) 0.05283(15) 0.0424(8) Uani 1 1 d . . . . . H46D H 0.0429 0.3328 0.0478 0.064 Uiso 1 1 calc GR . . . . H46E H 0.1104 0.3380 0.0099 0.064 Uiso 1 1 calc GR . . . . H46F H 0.1178 0.3899 0.0770 0.064 Uiso 1 1 calc GR . . . . Ir1A Ir 0.20623(2) 0.92285(2) 0.27479(2) 0.01583(3) Uani 1 1 d . . . . . O9A O 0.31175(10) 1.06996(10) 0.10400(10) 0.0268(4) Uani 1 1 d . . . . . O12A O 0.12122(11) 1.06366(10) 0.08488(10) 0.0292(4) Uani 1 1 d D U . . . O24A O 0.24831(13) 0.95810(11) 0.53751(10) 0.0380(5) Uani 1 1 d . . . . . O27A O 0.29112(12) 0.80263(10) 0.48304(10) 0.0341(5) Uani 1 1 d . . . . . O39A O -0.05242(11) 0.71774(10) 0.22127(10) 0.0324(5) Uani 1 1 d . . . . . O42A O 0.04013(11) 0.69217(9) 0.09475(10) 0.0309(5) Uani 1 1 d . . . . . N3A N 0.26826(11) 1.00182(10) 0.17415(10) 0.0169(4) Uani 1 1 d . . . . . N6A N 0.14971(12) 0.99810(10) 0.16177(10) 0.0180(4) Uani 1 1 d . . . . . N18A N 0.22453(13) 0.94019(11) 0.42401(11) 0.0232(5) Uani 1 1 d . . . . . N21A N 0.25123(12) 0.84370(11) 0.38981(11) 0.0214(5) Uani 1 1 d . . . . . N33A N 0.05436(12) 0.80608(10) 0.24669(10) 0.0192(4) Uani 1 1 d . . . . . N36A N 0.11176(12) 0.79104(10) 0.16703(11) 0.0193(4) Uani 1 1 d . . . . . C2A C 0.20608(14) 0.97460(12) 0.19765(12) 0.0169(5) Uani 1 1 d . . . . . C4A C 0.25063(15) 1.04099(13) 0.12710(13) 0.0208(5) Uani 1 1 d . . . . . C5A C 0.17615(15) 1.03893(12) 0.11970(13) 0.0200(5) Uani 1 1 d . . . . . C7A C 0.35318(15) 1.01185(14) 0.19072(13) 0.0229(6) Uani 1 1 d . . . . . C8A C 0.36966(15) 1.03281(15) 0.12584(14) 0.0271(6) Uani 1 1 d . . . . . H8AA H 0.4201 1.0624 0.1337 0.033 Uiso 1 1 calc R . . . . H8AB H 0.3671 0.9919 0.0925 0.033 Uiso 1 1 calc R . . . . C10A C 0.06625(15) 0.99367(13) 0.15561(13) 0.0224(5) Uani 1 1 d D U . . . C11A C 0.0582(3) 1.0539(3) 0.1189(3) 0.0253(10) Uani 0.594(8) 1 d D U P A 1 H11A H 0.0100 1.0425 0.0874 0.030 Uiso 0.594(8) 1 calc R . P A 1 H11B H 0.0598 1.0961 0.1503 0.030 Uiso 0.594(8) 1 calc R . P A 1 C11B C 0.0498(4) 1.0237(5) 0.0925(4) 0.0294(13) Uani 0.406(8) 1 d D U P A 2 H11C H 0.0287 0.9863 0.0541 0.035 Uiso 0.406(8) 1 calc R . P A 2 H11D H 0.0133 1.0531 0.0968 0.035 Uiso 0.406(8) 1 calc R . P A 2 C13A C 0.38549(17) 1.07199(16) 0.24964(15) 0.0363(7) Uani 1 1 d . . . . . H13A H 0.3677 1.1124 0.2405 0.054 Uiso 1 1 calc GR . . . . H13B H 0.4402 1.0816 0.2573 0.054 Uiso 1 1 calc GR . . . . H13C H 0.3690 1.0599 0.2882 0.054 Uiso 1 1 calc GR . . . . C14A C 0.38307(17) 0.94745(16) 0.20094(17) 0.0345(7) Uani 1 1 d . . . . . H14A H 0.3729 0.9358 0.2417 0.052 Uiso 1 1 calc GR . . . . H14B H 0.4370 0.9564 0.2027 0.052 Uiso 1 1 calc GR . . . . H14C H 0.3581 0.9095 0.1648 0.052 Uiso 1 1 calc GR . . . . C15A C 0.0454(4) 1.0064(4) 0.2223(3) 0.0372(15) Uani 0.594(8) 1 d D U P A 1 H15A H 0.0557 0.9701 0.2448 0.056 Uiso 0.594(8) 1 calc GR . P A 1 H15B H -0.0078 1.0071 0.2169 0.056 Uiso 0.594(8) 1 calc GR . P A 1 H15C H 0.0750 1.0503 0.2479 0.056 Uiso 0.594(8) 1 calc GR . P A 1 C15B C 0.0529(5) 1.0405(5) 0.2163(4) 0.034(2) Uani 0.406(8) 1 d D U P A 2 H15D H 0.0695 1.0235 0.2553 0.051 Uiso 0.406(8) 1 calc GR . P A 2 H15E H -0.0005 1.0406 0.2114 0.051 Uiso 0.406(8) 1 calc GR . P A 2 H15F H 0.0812 1.0870 0.2204 0.051 Uiso 0.406(8) 1 calc GR . P A 2 C16A C 0.0232(4) 0.9250(3) 0.1115(4) 0.0388(16) Uani 0.594(8) 1 d D U P A 1 H16A H 0.0368 0.9213 0.0689 0.058 Uiso 0.594(8) 1 calc GR . P A 1 H16B H -0.0307 0.9227 0.1066 0.058 Uiso 0.594(8) 1 calc GR . P A 1 H16C H 0.0360 0.8876 0.1312 0.058 Uiso 0.594(8) 1 calc GR . P A 1 C16B C 0.0179(5) 0.9209(3) 0.1446(5) 0.032(2) Uani 0.406(8) 1 d D U P A 2 H16D H 0.0300 0.8916 0.1083 0.047 Uiso 0.406(8) 1 calc GR . P A 2 H16E H -0.0351 0.9225 0.1346 0.047 Uiso 0.406(8) 1 calc GR . P A 2 H16F H 0.0281 0.9026 0.1839 0.047 Uiso 0.406(8) 1 calc GR . P A 2 C17A C 0.22757(14) 0.89760(13) 0.36609(12) 0.0200(5) Uani 1 1 d . . . . . C19A C 0.24631(17) 0.91396(15) 0.48007(13) 0.0280(6) Uani 1 1 d . . . . . C20A C 0.26357(16) 0.85347(14) 0.45850(13) 0.0263(6) Uani 1 1 d . . . . . C22A C 0.22753(18) 1.01574(14) 0.44696(14) 0.0306(7) Uani 1 1 d . . . . . C23A C 0.2124(2) 1.01247(16) 0.51646(15) 0.0395(8) Uani 1 1 d . . . . . H23A H 0.2344 1.0567 0.5467 0.047 Uiso 1 1 calc R . . . . H23B H 0.1580 1.0013 0.5153 0.047 Uiso 1 1 calc R . . . . C25A C 0.27774(16) 0.78084(14) 0.36308(14) 0.0252(6) Uani 1 1 d . . . . . C26A C 0.2930(2) 0.75102(17) 0.42641(16) 0.0413(8) Uani 1 1 d . . . . . H26A H 0.2544 0.7095 0.4230 0.050 Uiso 1 1 calc R . . . . H26B H 0.3424 0.7386 0.4315 0.050 Uiso 1 1 calc R . . . . C28A C 0.30799(19) 1.05657(15) 0.45100(16) 0.0416(8) Uani 1 1 d . . . . . H28A H 0.3439 1.0383 0.4784 0.062 Uiso 1 1 calc GR . . . . H28B H 0.3117 1.1046 0.4698 0.062 Uiso 1 1 calc GR . . . . H28C H 0.3190 1.0525 0.4074 0.062 Uiso 1 1 calc GR . . . . C29A C 0.1682(2) 1.04327(15) 0.40521(16) 0.0416(8) Uani 1 1 d . . . . . H29A H 0.1738 1.0345 0.3599 0.062 Uiso 1 1 calc GR . . . . H29B H 0.1751 1.0924 0.4211 0.062 Uiso 1 1 calc GR . . . . H29C H 0.1182 1.0204 0.4081 0.062 Uiso 1 1 calc GR . . . . C30A C 0.35028(19) 0.80144(18) 0.33836(19) 0.0460(9) Uani 1 1 d . . . . . H30A H 0.3392 0.8207 0.2997 0.069 Uiso 1 1 calc GR . . . . H30B H 0.3712 0.7612 0.3274 0.069 Uiso 1 1 calc GR . . . . H30C H 0.3865 0.8355 0.3723 0.069 Uiso 1 1 calc GR . . . . C31A C 0.21690(18) 0.72923(15) 0.31073(16) 0.0367(7) Uani 1 1 d . . . . . H31A H 0.1737 0.7143 0.3296 0.055 Uiso 1 1 calc GR . . . . H31B H 0.2370 0.6898 0.2948 0.055 Uiso 1 1 calc GR . . . . H31C H 0.2015 0.7509 0.2746 0.055 Uiso 1 1 calc GR . . . . C32A C 0.11897(14) 0.83517(12) 0.22697(12) 0.0181(5) Uani 1 1 d . . . . . C34A C 0.01112(16) 0.74754(13) 0.20205(14) 0.0252(6) Uani 1 1 d . . . . . C35A C 0.04713(15) 0.73826(13) 0.15228(14) 0.0232(6) Uani 1 1 d . . . . . C37A C 0.01633(15) 0.81729(13) 0.30452(13) 0.0220(5) Uani 1 1 d . . . . . C38A C -0.06362(16) 0.77269(15) 0.27095(15) 0.0309(6) Uani 1 1 d . . . . . H38A H -0.0885 0.7533 0.3033 0.037 Uiso 1 1 calc R . . . . H38B H -0.0951 0.8007 0.2505 0.037 Uiso 1 1 calc R . . . . C40A C 0.15832(15) 0.77688(13) 0.11545(13) 0.0234(6) Uani 1 1 d . . . . . C41A C 0.09605(17) 0.72457(14) 0.06197(14) 0.0298(6) Uani 1 1 d . . . . . H41A H 0.0724 0.7484 0.0302 0.036 Uiso 1 1 calc R . . . . H41B H 0.1183 0.6898 0.0385 0.036 Uiso 1 1 calc R . . . . C43A C 0.05246(17) 0.78600(17) 0.35958(15) 0.0354(7) Uani 1 1 d . . . . . H43A H 0.0502 0.7377 0.3430 0.053 Uiso 1 1 calc GR . . . . H43B H 0.0254 0.7905 0.3952 0.053 Uiso 1 1 calc GR . . . . H43C H 0.1047 0.8099 0.3755 0.053 Uiso 1 1 calc GR . . . . C44A C 0.01326(19) 0.89174(15) 0.32801(17) 0.0389(8) Uani 1 1 d . . . . . H44A H 0.0640 0.9199 0.3396 0.058 Uiso 1 1 calc GR . . . . H44B H -0.0099 0.8956 0.3661 0.058 Uiso 1 1 calc GR . . . . H44C H -0.0163 0.9073 0.2933 0.058 Uiso 1 1 calc GR . . . . C45A C 0.22169(17) 0.74221(16) 0.14222(15) 0.0355(7) Uani 1 1 d . . . . . H45A H 0.2560 0.7738 0.1793 0.053 Uiso 1 1 calc GR . . . . H45B H 0.2492 0.7301 0.1081 0.053 Uiso 1 1 calc GR . . . . H45C H 0.1998 0.7010 0.1560 0.053 Uiso 1 1 calc GR . . . . C46A C 0.18862(19) 0.83841(14) 0.08721(15) 0.0340(7) Uani 1 1 d . . . . . H46A H 0.1480 0.8611 0.0743 0.051 Uiso 1 1 calc GR . . . . H46B H 0.2090 0.8228 0.0492 0.051 Uiso 1 1 calc GR . . . . H46C H 0.2281 0.8704 0.1201 0.051 Uiso 1 1 calc GR . . . . F907 F 0.79932(12) 0.87363(10) 0.02140(12) 0.0547(6) Uani 1 1 d . U . . . F908 F 0.86786(11) 0.80479(11) 0.10389(10) 0.0500(5) Uani 1 1 d . U . . . C901 C 0.75780(18) 0.81634(14) 0.03415(16) 0.0326(7) Uani 1 1 d . . . . . C902 C 0.79291(17) 0.78090(15) 0.07634(15) 0.0311(6) Uani 1 1 d . . . . . C903 C 0.7533(2) 0.72248(16) 0.09071(16) 0.0388(8) Uani 1 1 d . . . . . H903 H 0.7772 0.6988 0.1197 0.047 Uiso 1 1 calc R . . . . C904 C 0.6772(2) 0.69928(16) 0.06141(17) 0.0437(8) Uani 1 1 d . . . . . H904 H 0.6495 0.6594 0.0707 0.052 Uiso 1 1 calc R . . . . C905 C 0.6417(2) 0.73419(18) 0.01885(18) 0.0432(8) Uani 1 1 d . . . . . H905 H 0.5903 0.7178 -0.0006 0.052 Uiso 1 1 calc R . . . . C906 C 0.68190(19) 0.79375(16) 0.00469(16) 0.0372(7) Uani 1 1 d . . . . . H906 H 0.6582 0.8178 -0.0240 0.045 Uiso 1 1 calc R . . . . F401 F 0.53467(10) 0.19119(10) 0.84950(12) 0.0515(5) Uani 1 1 d . U . . . F402 F 0.56599(12) 0.27038(15) 0.79940(17) 0.0925(10) Uani 1 1 d . U . . . F403 F 0.54139(16) 0.29614(15) 0.89308(16) 0.1112(13) Uani 1 1 d . U . . . F404 F 0.27243(19) 0.06597(16) 0.7776(3) 0.0534(15) Uani 0.633(10) 1 d D U P B 1 F405 F 0.2171(3) 0.0981(3) 0.69509(16) 0.0689(18) Uani 0.633(10) 1 d D U P B 1 F406 F 0.1900(2) 0.1278(2) 0.7886(3) 0.0429(13) Uani 0.633(10) 1 d D U P B 1 F407 F 0.46190(10) 0.56281(9) 1.00900(8) 0.0394(4) Uani 1 1 d . U . . . F408 F 0.44269(10) 0.63000(8) 0.94199(10) 0.0387(4) Uani 1 1 d . U . . . F409 F 0.51365(9) 0.55752(9) 0.92405(9) 0.0395(4) Uani 1 1 d . U . . . F410 F 0.18349(11) 0.47214(11) 0.97929(9) 0.0504(5) Uani 1 1 d . U . . . F411 F 0.13186(12) 0.49130(13) 0.88797(13) 0.0665(7) Uani 1 1 d . U . . . F412 F 0.13360(11) 0.38801(9) 0.89806(10) 0.0487(5) Uani 1 1 d . U . . . F413 F 0.50475(18) 0.59776(11) 0.61183(14) 0.0926(10) Uani 1 1 d . U . . . F414 F 0.48702(12) 0.61807(9) 0.70977(10) 0.0476(5) Uani 1 1 d . U . . . F415 F 0.39403(14) 0.59986(10) 0.63003(14) 0.0744(8) Uani 1 1 d . U . . . F416 F 0.4922(3) 0.35642(18) 0.50757(14) 0.0892(13) Uani 0.851(5) 1 d D U P C 1 F417 F 0.56288(15) 0.34100(19) 0.59078(18) 0.0820(12) Uani 0.851(5) 1 d D U P C 1 F418 F 0.4545(2) 0.27542(12) 0.55417(19) 0.0746(12) Uani 0.851(5) 1 d D U P C 1 F419 F 0.06934(17) 0.46774(16) 0.58498(15) 0.0980(11) Uani 1 1 d . U . . . F420 F -0.00579(10) 0.39853(10) 0.62254(12) 0.0590(6) Uani 1 1 d . U . . . F421 F 0.07813(11) 0.47746(9) 0.68800(11) 0.0550(6) Uani 1 1 d . U . . . F422 F 0.0905(5) 0.2141(3) 0.4778(3) 0.0543(17) Uani 0.609(15) 1 d D U P D 1 F423 F 0.1094(6) 0.16069(18) 0.5555(3) 0.0578(18) Uani 0.609(15) 1 d D U P D 1 F424 F 0.2010(2) 0.2007(4) 0.5136(4) 0.0582(18) Uani 0.609(15) 1 d D U P D 1 F504 F 0.1796(3) 0.1270(4) 0.7610(5) 0.044(2) Uani 0.367(10) 1 d D U P B 2 F505 F 0.2633(4) 0.0872(5) 0.8159(5) 0.066(3) Uani 0.367(10) 1 d D U P B 2 F506 F 0.2503(5) 0.0717(3) 0.7127(5) 0.064(3) Uani 0.367(10) 1 d D U P B 2 F516 F 0.5122(10) 0.2908(7) 0.5948(6) 0.062(4) Uani 0.149(5) 1 d D U P C 2 F517 F 0.4395(6) 0.3062(8) 0.5126(6) 0.076(5) Uani 0.149(5) 1 d D U P C 2 F518 F 0.5491(7) 0.3682(5) 0.5447(8) 0.060(4) Uani 0.149(5) 1 d D U P C 2 F522 F 0.1918(5) 0.1788(5) 0.5349(5) 0.053(3) Uani 0.391(15) 1 d D U P D 2 F523 F 0.1247(8) 0.2240(4) 0.4703(2) 0.053(2) Uani 0.391(15) 1 d D U P D 2 F524 F 0.0753(5) 0.1714(4) 0.5362(6) 0.055(3) Uani 0.391(15) 1 d D U P D 2 C401 C 0.34184(14) 0.30339(12) 0.75766(12) 0.0152(5) Uani 1 1 d . . . . . C402 C 0.41685(15) 0.30299(12) 0.78624(12) 0.0195(5) Uani 1 1 d . . . . . H402 H 0.4545 0.3428 0.7914 0.023 Uiso 1 1 calc R . . . . C403 C 0.43728(15) 0.24537(13) 0.80724(13) 0.0224(5) Uani 1 1 d . . . . . C404 C 0.38318(15) 0.18485(13) 0.80036(13) 0.0234(6) Uani 1 1 d . . . . . H404 H 0.3967 0.1459 0.8138 0.028 Uiso 1 1 calc R . . . . C405 C 0.30867(15) 0.18421(12) 0.77300(13) 0.0214(5) Uani 1 1 d D . . . . C406 C 0.28813(15) 0.24230(12) 0.75280(12) 0.0186(5) Uani 1 1 d . . . . . H406 H 0.2371 0.2404 0.7356 0.022 Uiso 1 1 calc R . . . . C407 C 0.51892(18) 0.25009(15) 0.83782(18) 0.0366(7) Uani 1 1 d . . . . . C408 C 0.24904(16) 0.11931(13) 0.76190(15) 0.0322(7) Uani 1 1 d D . . . . C409 C 0.31839(14) 0.42523(11) 0.80481(11) 0.0142(5) Uani 1 1 d . . . . . C410 C 0.38260(14) 0.47260(12) 0.84392(12) 0.0165(5) Uani 1 1 d . . . . . H410 H 0.4280 0.4779 0.8287 0.020 Uiso 1 1 calc R . . . . C411 C 0.38077(14) 0.51214(12) 0.90505(12) 0.0164(5) Uani 1 1 d . . . . . C412 C 0.31369(14) 0.50582(12) 0.92957(12) 0.0187(5) Uani 1 1 d . . . . . H412 H 0.3120 0.5325 0.9700 0.022 Uiso 1 1 calc R . . . . C413 C 0.24998(14) 0.45886(12) 0.89213(12) 0.0180(5) Uani 1 1 d . . . . . C414 C 0.25232(14) 0.41918(12) 0.83113(12) 0.0161(5) Uani 1 1 d . . . . . H414 H 0.2085 0.3876 0.8072 0.019 Uiso 1 1 calc R . . . . C415 C 0.44946(15) 0.56464(13) 0.94446(13) 0.0214(5) Uani 1 1 d . . . . . C416 C 0.17574(16) 0.45207(14) 0.91486(14) 0.0254(6) Uani 1 1 d . . . . . C417 C 0.38225(14) 0.40682(12) 0.69452(12) 0.0162(5) Uani 1 1 d . . . . . C418 C 0.39807(14) 0.47721(12) 0.69173(12) 0.0193(5) Uani 1 1 d . . . . . H418 H 0.3778 0.5080 0.7186 0.023 Uiso 1 1 calc R . . . . C419 C 0.44306(16) 0.50257(13) 0.65005(13) 0.0245(6) Uani 1 1 d . . . . . C420 C 0.47420(16) 0.45896(14) 0.60873(13) 0.0269(6) Uani 1 1 d . . . . . H420 H 0.5045 0.4761 0.5809 0.032 Uiso 1 1 calc R . . . . C421 C 0.45862(15) 0.38890(13) 0.61028(13) 0.0237(6) Uani 1 1 d D . . . . C422 C 0.41460(14) 0.36371(13) 0.65239(12) 0.0190(5) Uani 1 1 d . . . . . H422 H 0.4061 0.3165 0.6528 0.023 Uiso 1 1 calc R . . . . C423 C 0.45731(19) 0.57880(15) 0.64961(16) 0.0348(7) Uani 1 1 d . . . . . C424 C 0.49079(17) 0.33974(15) 0.56566(14) 0.0368(7) Uani 1 1 d D . . . . C425 C 0.23948(14) 0.35582(12) 0.68201(12) 0.0158(5) Uani 1 1 d . . . . . C426 C 0.18706(14) 0.39928(12) 0.68008(12) 0.0171(5) Uani 1 1 d . . . . . H426 H 0.1970 0.4399 0.7122 0.020 Uiso 1 1 calc R . . . . C427 C 0.12065(15) 0.38357(13) 0.63161(13) 0.0209(5) Uani 1 1 d . . . . . C428 C 0.10358(15) 0.32412(13) 0.58228(13) 0.0210(5) Uani 1 1 d . . . . . H428 H 0.0589 0.3134 0.5502 0.025 Uiso 1 1 calc R . . . . C429 C 0.15562(14) 0.28111(12) 0.58242(12) 0.0196(5) Uani 1 1 d D . . . . C430 C 0.22178(14) 0.29679(12) 0.63073(12) 0.0179(5) Uani 1 1 d . . . . . H430 H 0.2556 0.2671 0.6291 0.022 Uiso 1 1 calc R . . . . C431 C 0.06623(16) 0.43176(15) 0.63135(15) 0.0295(6) Uani 1 1 d . . . . . C432 C 0.13870(14) 0.21463(13) 0.53207(13) 0.0263(6) Uani 1 1 d D . . . . B400 B 0.32021(16) 0.37374(13) 0.73557(13) 0.0144(5) Uani 1 1 d . . . . . F201 F 0.7432(3) 0.4185(3) 0.1878(3) 0.0660(18) Uani 0.5 1 d D U P E 1 F202 F 0.8256(2) 0.3786(3) 0.2444(3) 0.0513(18) Uani 0.5 1 d D U P E 1 F203 F 0.7504(3) 0.4294(2) 0.2907(3) 0.0682(19) Uani 0.5 1 d D U P E 1 F204 F 0.46926(10) 0.30580(9) 0.15005(10) 0.0412(5) Uani 1 1 d . U . . . F205 F 0.44013(11) 0.21242(12) 0.18366(14) 0.0689(7) Uani 1 1 d . U . . . F206 F 0.47650(13) 0.21004(13) 0.09235(12) 0.0758(8) Uani 1 1 d . U . . . F207 F 0.82176(12) 0.02367(12) 0.02015(10) 0.0588(6) Uani 1 1 d . U . . . F208 F 0.87582(13) 0.01119(16) 0.11205(15) 0.0866(9) Uani 1 1 d . U . . . F209 F 0.87121(13) 0.11131(11) 0.09590(14) 0.0784(9) Uani 1 1 d . U . . . F210 F 0.54554(11) -0.06116(10) -0.00643(8) 0.0432(5) Uani 1 1 d . U . . . F211 F 0.56116(10) -0.12610(8) 0.06274(10) 0.0436(5) Uani 1 1 d . U . . . F212 F 0.49311(9) -0.05091(9) 0.07789(10) 0.0437(5) Uani 1 1 d . U . . . F213 F 0.88198(12) 0.28053(9) 0.53378(8) 0.0420(5) Uani 1 1 d . U . . . F214 F 0.93132(12) 0.33232(9) 0.46528(10) 0.0510(5) Uani 1 1 d . U . . . F215 F 0.81271(11) 0.32443(9) 0.46784(9) 0.0473(5) Uani 1 1 d . U . . . F216 F 0.9175(3) 0.0161(2) 0.3257(2) 0.0526(16) Uani 0.5 1 d D U P F 1 F217 F 0.9528(4) 0.0482(3) 0.4318(3) 0.064(2) Uani 0.5 1 d D U P F 1 F218 F 1.0074(3) 0.1026(3) 0.3679(3) 0.0375(15) Uani 0.5 1 d D U P F 1 F219 F 0.52209(14) 0.14984(11) 0.49592(10) 0.0598(6) Uani 1 1 d . U . . . F220 F 0.44583(11) 0.15852(12) 0.41092(12) 0.0620(6) Uani 1 1 d . U . . . F221 F 0.55304(12) 0.22920(9) 0.44420(10) 0.0494(5) Uani 1 1 d . U . . . F222 F 0.53107(13) -0.08973(9) 0.40782(10) 0.0517(5) Uani 1 1 d . U . . . F223 F 0.51416(11) -0.11382(8) 0.30208(9) 0.0421(5) Uani 1 1 d . U . . . F224 F 0.62595(11) -0.09678(9) 0.36071(11) 0.0459(5) Uani 1 1 d . U . . . F301 F 0.7822(3) 0.4096(3) 0.3043(2) 0.0645(17) Uani 0.5 1 d D U P E 2 F302 F 0.7307(3) 0.4359(2) 0.2174(3) 0.0525(16) Uani 0.5 1 d D U P E 2 F303 F 0.8166(2) 0.3771(3) 0.2148(3) 0.0461(16) Uani 0.5 1 d D U P E 2 F316 F 0.9720(3) 0.0729(3) 0.4424(2) 0.0429(15) Uani 0.5 1 d D U P F 2 F317 F 0.9957(3) 0.0870(3) 0.3490(3) 0.053(2) Uani 0.5 1 d D U P F 2 F318 F 0.9042(3) 0.00497(19) 0.3563(3) 0.0602(18) Uani 0.5 1 d D U P F 2 C201 C 0.66685(14) 0.19912(12) 0.24222(11) 0.0149(5) Uani 1 1 d . . . . . C202 C 0.71898(14) 0.26138(12) 0.24778(12) 0.0175(5) Uani 1 1 d . . . . . H202 H 0.7699 0.2648 0.2666 0.021 Uiso 1 1 calc R . . . . C203 C 0.69738(14) 0.31849(12) 0.22617(13) 0.0203(5) Uani 1 1 d D . . . . C204 C 0.62289(15) 0.31538(12) 0.19633(13) 0.0218(5) Uani 1 1 d . . . . . H204 H 0.6085 0.3535 0.1819 0.026 Uiso 1 1 calc R . . . . C205 C 0.57023(15) 0.25367(13) 0.18863(13) 0.0204(5) Uani 1 1 d . . . . . C206 C 0.59172(14) 0.19714(12) 0.21112(12) 0.0179(5) Uani 1 1 d . . . . . H206 H 0.5550 0.1565 0.2054 0.021 Uiso 1 1 calc R . . . . C207 C 0.75529(16) 0.38514(13) 0.23854(14) 0.0307(7) Uani 1 1 d D . . . . C208 C 0.48979(16) 0.24609(14) 0.15400(16) 0.0296(6) Uani 1 1 d . . . . . C209 C 0.69139(13) 0.07745(11) 0.19687(11) 0.0140(5) Uani 1 1 d . . . . . C210 C 0.75718(14) 0.08220(12) 0.17006(12) 0.0164(5) Uani 1 1 d . . . . . H210 H 0.8017 0.1130 0.1938 0.020 Uiso 1 1 calc R . . . . C211 C 0.75800(15) 0.04194(12) 0.10855(13) 0.0189(5) Uani 1 1 d . . . . . C212 C 0.69331(14) -0.00401(12) 0.07153(12) 0.0195(5) Uani 1 1 d . . . . . H212 H 0.6940 -0.0308 0.0308 0.023 Uiso 1 1 calc R . . . . C213 C 0.62680(14) -0.00919(12) 0.09677(12) 0.0180(5) Uani 1 1 d . . . . . C214 C 0.62632(14) 0.03067(11) 0.15817(12) 0.0161(5) Uani 1 1 d . . . . . H214 H 0.5812 0.0260 0.1739 0.019 Uiso 1 1 calc R . . . . C215 C 0.83070(16) 0.04789(14) 0.08403(14) 0.0280(6) Uani 1 1 d . . . . . C216 C 0.55723(15) -0.06079(13) 0.05823(13) 0.0223(5) Uani 1 1 d . . . . . C217 C 0.76920(14) 0.14844(12) 0.31997(12) 0.0150(5) Uani 1 1 d . . . . . C218 C 0.78571(14) 0.20791(12) 0.37112(12) 0.0169(5) Uani 1 1 d . . . . . H218 H 0.7523 0.2380 0.3712 0.020 Uiso 1 1 calc R . . . . C219 C 0.84977(15) 0.22314(12) 0.42120(12) 0.0197(5) Uani 1 1 d . . . . . C220 C 0.90011(15) 0.17878(13) 0.42451(13) 0.0217(5) Uani 1 1 d . . . . . H220 H 0.9431 0.1889 0.4583 0.026 Uiso 1 1 calc R . . . . C221 C 0.88430(14) 0.11903(12) 0.37600(13) 0.0216(5) Uani 1 1 d D . . . . C222 C 0.82054(14) 0.10428(12) 0.32464(12) 0.0172(5) Uani 1 1 d . . . . . H222 H 0.8118 0.0639 0.2925 0.021 Uiso 1 1 calc R . . . . C223 C 0.86820(16) 0.28971(14) 0.47147(13) 0.0250(6) Uani 1 1 d . . . . . C224 C 0.93859(16) 0.07124(13) 0.37772(14) 0.0328(7) Uani 1 1 d D . . . . C225 C 0.62779(13) 0.09675(12) 0.30678(12) 0.0150(5) Uani 1 1 d . . . . . C226 C 0.59477(14) 0.13979(12) 0.34843(12) 0.0174(5) Uani 1 1 d . . . . . H226 H 0.6011 0.1865 0.3465 0.021 Uiso 1 1 calc R . . . . C227 C 0.55311(14) 0.11497(13) 0.39235(12) 0.0211(5) Uani 1 1 d . . . . . C228 C 0.54101(15) 0.04532(14) 0.39627(13) 0.0235(6) Uani 1 1 d . . . . . H228 H 0.5128 0.0285 0.4256 0.028 Uiso 1 1 calc R . . . . C229 C 0.57242(15) 0.00175(13) 0.35508(13) 0.0220(5) Uani 1 1 d . . . . . C230 C 0.61505(14) 0.02701(12) 0.31158(12) 0.0183(5) Uani 1 1 d . . . . . H230 H 0.6357 -0.0035 0.2849 0.022 Uiso 1 1 calc R . . . . C231 C 0.51910(17) 0.16341(15) 0.43575(14) 0.0295(6) Uani 1 1 d . . . . . C232 C 0.56090(18) -0.07412(14) 0.35682(15) 0.0301(6) Uani 1 1 d . . . . . B200 B 0.68937(15) 0.12980(12) 0.26554(13) 0.0132(5) Uani 1 1 d . . . . . F915 F 0.79576(12) 0.37555(9) 0.02064(11) 0.0516(5) Uani 1 1 d . U . . . F916 F 0.87269(11) 0.31136(11) 0.10254(11) 0.0548(5) Uani 1 1 d . U . . . C909 C 0.75851(18) 0.31721(14) 0.03506(15) 0.0316(7) Uani 1 1 d . . . . . C910 C 0.79790(18) 0.28398(15) 0.07709(15) 0.0322(7) Uani 1 1 d . . . . . C911 C 0.7627(2) 0.22466(16) 0.09271(16) 0.0393(8) Uani 1 1 d . . . . . H911 H 0.7893 0.2027 0.1217 0.047 Uiso 1 1 calc R . . . . C912 C 0.6869(2) 0.19791(18) 0.06482(17) 0.0464(9) Uani 1 1 d . . . . . H912 H 0.6623 0.1573 0.0749 0.056 Uiso 1 1 calc R . . . . C913 C 0.6472(2) 0.23021(19) 0.02239(18) 0.0462(9) Uani 1 1 d . . . . . H913 H 0.5961 0.2113 0.0038 0.055 Uiso 1 1 calc R . . . . C914 C 0.68333(19) 0.29122(17) 0.00715(16) 0.0386(8) Uani 1 1 d . . . . . H914 H 0.6569 0.3137 -0.0214 0.046 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 0.01384(5) 0.02116(5) 0.01563(5) 0.00643(4) 0.00352(4) 0.00016(4) O9 0.0199(10) 0.0334(10) 0.0273(10) 0.0165(8) 0.0105(8) 0.0042(8) O12 0.0205(10) 0.0338(10) 0.0401(12) 0.0231(9) 0.0105(9) 0.0099(8) O24 0.0614(15) 0.0873(16) 0.0296(12) 0.0229(12) 0.0040(11) -0.0003(13) O27 0.0604(15) 0.0767(15) 0.0634(15) 0.0463(13) 0.0061(13) 0.0304(13) O39 0.0269(11) 0.0364(11) 0.0362(12) 0.0029(9) 0.0131(10) -0.0108(9) O42 0.0410(13) 0.0314(10) 0.0300(11) -0.0057(9) 0.0116(10) -0.0119(9) N3 0.0131(10) 0.0224(10) 0.0175(10) 0.0057(8) 0.0024(9) 0.0009(8) N6 0.0127(10) 0.0191(10) 0.0206(11) 0.0074(8) 0.0039(9) 0.0006(8) N18 0.0297(12) 0.0477(13) 0.0230(11) 0.0128(10) 0.0049(10) -0.0037(10) N21 0.0261(12) 0.0475(13) 0.0362(13) 0.0249(10) 0.0056(10) 0.0086(10) N33 0.0166(11) 0.0212(10) 0.0197(11) 0.0069(8) 0.0041(9) 0.0029(9) N36 0.0232(12) 0.0200(10) 0.0218(11) 0.0046(9) 0.0084(10) 0.0016(9) C2 0.0165(13) 0.0156(11) 0.0170(12) 0.0016(9) 0.0029(10) -0.0006(10) C4 0.0207(14) 0.0218(12) 0.0194(13) 0.0071(10) 0.0064(11) 0.0018(10) C5 0.0197(13) 0.0204(12) 0.0209(13) 0.0082(10) 0.0046(11) 0.0036(10) C7 0.0121(13) 0.0363(15) 0.0237(14) 0.0116(11) 0.0027(11) 0.0000(11) C8 0.0168(14) 0.0415(16) 0.0284(15) 0.0164(12) 0.0070(12) 0.0066(12) C10 0.0137(13) 0.0283(13) 0.0317(15) 0.0115(11) 0.0074(12) 0.0059(11) C11 0.0192(14) 0.0356(15) 0.0395(17) 0.0200(13) 0.0060(13) 0.0066(12) C13 0.0302(17) 0.0424(17) 0.0295(16) 0.0071(13) 0.0014(14) -0.0132(14) C14 0.0181(15) 0.0510(18) 0.0421(18) 0.0255(15) 0.0057(14) 0.0091(14) C15 0.0369(18) 0.0408(17) 0.0449(19) 0.0086(14) 0.0219(16) 0.0160(15) C16 0.0174(14) 0.0372(16) 0.0483(19) 0.0219(14) 0.0086(14) 0.0052(12) C17 0.0186(12) 0.0398(13) 0.0243(13) 0.0160(11) 0.0037(11) -0.0011(11) C19 0.0373(15) 0.0677(17) 0.0277(14) 0.0280(13) 0.0020(12) -0.0015(14) C20 0.0400(16) 0.0632(17) 0.0423(15) 0.0340(14) 0.0024(13) 0.0127(14) C22 0.0431(16) 0.0509(16) 0.0274(14) 0.0061(13) 0.0064(13) -0.0101(14) C23 0.0550(18) 0.0684(19) 0.0279(15) 0.0052(14) 0.0123(14) -0.0126(16) C25 0.0332(15) 0.0489(15) 0.0521(17) 0.0216(13) 0.0110(14) 0.0197(13) C26 0.0529(18) 0.0731(19) 0.069(2) 0.0317(17) 0.0104(16) 0.0308(16) C28 0.068(3) 0.090(3) 0.035(2) 0.0052(19) 0.009(2) -0.041(2) C29 0.095(3) 0.050(2) 0.040(2) -0.0158(17) 0.014(2) 0.004(2) C30 0.049(2) 0.063(2) 0.066(3) 0.0227(19) 0.029(2) 0.0218(18) C31 0.043(2) 0.0437(18) 0.074(3) 0.0184(17) 0.0181(19) 0.0201(16) C32 0.0183(13) 0.0190(11) 0.0214(13) 0.0086(10) 0.0078(11) 0.0051(10) C34 0.0227(15) 0.0255(13) 0.0291(15) 0.0068(11) 0.0068(12) -0.0024(11) C35 0.0281(16) 0.0234(13) 0.0270(15) 0.0003(11) 0.0062(13) -0.0026(12) C37 0.0173(13) 0.0294(13) 0.0236(14) 0.0106(11) 0.0104(11) 0.0027(11) C38 0.0188(14) 0.0407(16) 0.0340(16) 0.0097(13) 0.0102(13) 0.0013(12) C40 0.0354(17) 0.0246(13) 0.0229(14) -0.0001(11) 0.0144(13) -0.0001(12) C41 0.0415(18) 0.0235(13) 0.0288(15) -0.0011(11) 0.0140(14) -0.0028(13) C43 0.0257(16) 0.0538(19) 0.0344(17) 0.0254(15) 0.0106(14) 0.0065(14) C44 0.0380(18) 0.0350(16) 0.0401(18) 0.0046(13) 0.0266(16) 0.0029(14) C45 0.0349(19) 0.0514(19) 0.0395(19) -0.0083(15) 0.0196(16) -0.0045(15) C46 0.071(3) 0.0287(15) 0.0219(15) 0.0054(12) 0.0057(16) 0.0009(16) Ir1A 0.01523(5) 0.01761(5) 0.01461(5) 0.00336(4) 0.00438(4) 0.00215(4) O9A 0.0183(10) 0.0362(10) 0.0326(11) 0.0180(9) 0.0116(9) 0.0067(8) O12A 0.0209(10) 0.0390(10) 0.0371(11) 0.0221(9) 0.0104(9) 0.0129(8) O24A 0.0509(14) 0.0446(12) 0.0170(10) 0.0004(9) 0.0072(10) 0.0118(11) O27A 0.0418(13) 0.0422(11) 0.0229(10) 0.0137(9) 0.0042(10) 0.0169(10) O39A 0.0221(11) 0.0335(10) 0.0368(12) 0.0036(9) 0.0087(9) -0.0058(9) O42A 0.0291(11) 0.0262(10) 0.0307(11) -0.0048(8) 0.0061(9) -0.0012(8) N3A 0.0123(10) 0.0195(10) 0.0196(11) 0.0047(8) 0.0047(9) 0.0026(8) N6A 0.0155(11) 0.0205(10) 0.0203(11) 0.0074(8) 0.0058(9) 0.0045(9) N18A 0.0247(12) 0.0241(11) 0.0183(11) 0.0022(9) 0.0030(10) 0.0016(9) N21A 0.0182(11) 0.0266(11) 0.0197(11) 0.0060(9) 0.0045(9) 0.0039(9) N33A 0.0188(11) 0.0187(10) 0.0205(11) 0.0038(8) 0.0062(9) 0.0028(9) N36A 0.0177(11) 0.0210(10) 0.0201(11) 0.0037(8) 0.0056(9) 0.0051(9) C2A 0.0157(12) 0.0167(11) 0.0174(12) 0.0024(9) 0.0042(10) 0.0015(10) C4A 0.0199(14) 0.0230(12) 0.0223(13) 0.0089(10) 0.0079(11) 0.0045(11) C5A 0.0204(13) 0.0205(12) 0.0225(13) 0.0093(10) 0.0072(11) 0.0058(10) C7A 0.0128(13) 0.0314(14) 0.0246(14) 0.0084(11) 0.0035(11) 0.0031(11) C8A 0.0175(14) 0.0376(15) 0.0311(15) 0.0143(12) 0.0091(12) 0.0080(12) C10A 0.0156(12) 0.0265(12) 0.0285(13) 0.0109(10) 0.0054(10) 0.0070(10) C11A 0.0195(17) 0.0314(19) 0.031(2) 0.0129(16) 0.0101(16) 0.0098(16) C11B 0.024(2) 0.034(2) 0.034(2) 0.0156(19) 0.006(2) 0.0075(19) C13A 0.0234(16) 0.0446(17) 0.0330(17) 0.0062(14) 0.0035(14) -0.0093(13) C14A 0.0222(15) 0.0443(17) 0.0463(19) 0.0223(15) 0.0120(14) 0.0139(14) C15A 0.028(3) 0.056(4) 0.040(3) 0.023(3) 0.020(2) 0.018(3) C15B 0.025(4) 0.042(4) 0.034(4) 0.000(4) 0.008(3) 0.009(4) C16A 0.023(3) 0.032(3) 0.055(4) 0.010(3) -0.008(3) 0.006(2) C16B 0.027(4) 0.031(4) 0.038(4) 0.013(3) 0.002(4) 0.008(3) C17A 0.0168(13) 0.0249(12) 0.0167(12) 0.0036(10) 0.0038(10) 0.0003(10) C19A 0.0307(16) 0.0368(15) 0.0157(13) 0.0041(11) 0.0066(12) 0.0047(13) C20A 0.0247(15) 0.0365(15) 0.0189(13) 0.0103(11) 0.0042(12) 0.0051(12) C22A 0.0357(17) 0.0241(13) 0.0260(15) -0.0031(11) 0.0030(13) 0.0018(12) C23A 0.047(2) 0.0411(17) 0.0276(16) -0.0038(13) 0.0098(15) 0.0113(15) C25A 0.0215(14) 0.0320(14) 0.0253(14) 0.0069(11) 0.0061(12) 0.0117(12) C26A 0.055(2) 0.0456(18) 0.0303(17) 0.0128(14) 0.0084(16) 0.0236(17) C28A 0.047(2) 0.0330(16) 0.0339(18) -0.0025(13) 0.0033(16) -0.0070(15) C29A 0.051(2) 0.0309(15) 0.0389(18) -0.0022(13) 0.0019(16) 0.0141(15) C30A 0.0370(19) 0.057(2) 0.058(2) 0.0203(17) 0.0259(18) 0.0208(17) C31A 0.0387(18) 0.0296(15) 0.0404(18) 0.0018(13) 0.0013(15) 0.0148(14) C32A 0.0198(13) 0.0187(11) 0.0198(13) 0.0078(10) 0.0071(11) 0.0079(10) C34A 0.0201(14) 0.0221(12) 0.0308(15) 0.0050(11) 0.0050(12) -0.0015(11) C35A 0.0213(14) 0.0196(12) 0.0264(14) 0.0026(10) 0.0034(12) 0.0016(11) C37A 0.0179(13) 0.0257(13) 0.0259(14) 0.0099(11) 0.0093(11) 0.0047(11) C38A 0.0208(15) 0.0397(16) 0.0334(16) 0.0100(13) 0.0084(13) 0.0044(13) C40A 0.0227(14) 0.0266(13) 0.0198(13) -0.0010(10) 0.0069(11) 0.0057(11) C41A 0.0310(16) 0.0296(14) 0.0261(15) 0.0009(12) 0.0071(13) 0.0036(12) C43A 0.0251(16) 0.0542(19) 0.0316(16) 0.0238(14) 0.0071(13) 0.0053(14) C44A 0.0424(19) 0.0337(16) 0.047(2) 0.0057(14) 0.0253(17) 0.0119(14) C45A 0.0338(17) 0.0450(17) 0.0282(16) 0.0004(13) 0.0062(14) 0.0168(14) C46A 0.0450(19) 0.0291(14) 0.0281(16) 0.0000(12) 0.0196(15) 0.0030(14) F907 0.0571(13) 0.0362(10) 0.0790(16) 0.0264(10) 0.0260(12) 0.0058(9) F908 0.0287(10) 0.0711(13) 0.0462(12) 0.0095(10) 0.0029(9) 0.0070(9) C901 0.0388(18) 0.0248(14) 0.0382(17) 0.0072(12) 0.0162(15) 0.0085(13) C902 0.0289(16) 0.0378(16) 0.0272(15) 0.0032(12) 0.0063(13) 0.0109(13) C903 0.052(2) 0.0389(17) 0.0314(17) 0.0153(14) 0.0113(16) 0.0131(16) C904 0.056(2) 0.0314(16) 0.043(2) 0.0092(14) 0.0204(18) -0.0026(16) C905 0.0338(19) 0.0474(19) 0.043(2) 0.0012(16) 0.0059(16) 0.0036(16) C906 0.0375(18) 0.0420(17) 0.0365(18) 0.0108(14) 0.0049(15) 0.0199(15) F401 0.0289(10) 0.0444(10) 0.0866(16) 0.0326(11) -0.0021(10) 0.0163(9) F402 0.0249(12) 0.122(2) 0.153(3) 0.098(2) 0.0131(15) 0.0116(13) F403 0.0740(18) 0.1017(19) 0.112(2) -0.0536(17) -0.0687(17) 0.0524(16) F404 0.0370(18) 0.0168(15) 0.110(4) 0.021(2) 0.011(2) 0.0106(13) F405 0.081(3) 0.049(3) 0.047(2) 0.0031(17) -0.007(2) -0.038(2) F406 0.030(2) 0.0313(18) 0.067(3) 0.0055(19) 0.0201(19) -0.0011(15) F407 0.0373(10) 0.0506(10) 0.0186(8) 0.0036(7) -0.0043(8) -0.0077(8) F408 0.0324(10) 0.0204(8) 0.0545(12) 0.0043(7) -0.0058(9) -0.0007(7) F409 0.0165(8) 0.0480(10) 0.0435(11) -0.0127(8) 0.0066(8) 0.0003(7) F410 0.0370(11) 0.0732(13) 0.0295(10) -0.0105(9) 0.0205(9) -0.0108(10) F411 0.0362(12) 0.0949(17) 0.0953(19) 0.0496(14) 0.0324(12) 0.0374(12) F412 0.0345(11) 0.0428(10) 0.0572(13) -0.0157(9) 0.0286(10) -0.0149(8) F413 0.155(3) 0.0411(12) 0.103(2) 0.0260(12) 0.097(2) 0.0013(14) F414 0.0625(13) 0.0264(9) 0.0445(11) 0.0051(8) 0.0011(10) -0.0034(9) F415 0.0737(16) 0.0348(10) 0.101(2) 0.0277(12) -0.0287(14) 0.0078(11) F416 0.158(4) 0.101(2) 0.0441(17) 0.0241(16) 0.063(2) 0.071(2) F417 0.0450(17) 0.101(2) 0.093(2) -0.0265(19) 0.0106(16) 0.0429(17) F418 0.084(2) 0.0426(14) 0.093(2) -0.0238(15) 0.065(2) -0.0033(14) F419 0.125(2) 0.131(2) 0.113(2) 0.0970(19) 0.0735(19) 0.106(2) F420 0.0197(10) 0.0500(11) 0.0936(17) -0.0158(11) -0.0001(10) 0.0117(9) F421 0.0397(11) 0.0429(10) 0.0689(14) -0.0196(10) -0.0110(10) 0.0239(9) F422 0.064(3) 0.046(2) 0.034(2) -0.0098(17) -0.027(2) 0.016(2) F423 0.103(4) 0.0208(16) 0.042(2) 0.0041(14) 0.018(3) -0.005(2) F424 0.036(2) 0.061(3) 0.058(3) -0.036(2) 0.014(2) 0.0014(19) F504 0.025(3) 0.024(3) 0.084(6) 0.016(3) 0.005(3) 0.008(2) F505 0.061(4) 0.046(4) 0.089(5) 0.047(4) -0.005(4) -0.007(3) F506 0.060(4) 0.031(3) 0.087(5) -0.021(3) 0.035(4) -0.011(3) F516 0.078(7) 0.057(6) 0.066(7) 0.012(5) 0.031(6) 0.043(5) F517 0.073(7) 0.075(7) 0.071(7) -0.021(6) 0.017(6) 0.026(6) F518 0.056(6) 0.061(6) 0.066(7) -0.007(5) 0.049(5) 0.005(5) F522 0.055(4) 0.044(4) 0.049(4) -0.018(3) -0.021(3) 0.032(3) F523 0.089(6) 0.045(3) 0.015(2) 0.004(2) 0.001(3) 0.001(4) F524 0.055(4) 0.038(3) 0.062(5) -0.015(3) 0.028(4) -0.011(3) C401 0.0169(12) 0.0160(11) 0.0139(11) 0.0029(9) 0.0043(10) 0.0058(10) C402 0.0186(13) 0.0175(11) 0.0209(13) 0.0033(10) 0.0013(11) 0.0030(10) C403 0.0195(14) 0.0239(12) 0.0224(13) 0.0037(10) -0.0003(11) 0.0064(11) C404 0.0258(15) 0.0176(12) 0.0280(14) 0.0070(10) 0.0016(12) 0.0086(11) C405 0.0226(14) 0.0155(11) 0.0264(14) 0.0046(10) 0.0047(12) 0.0047(10) C406 0.0179(13) 0.0179(11) 0.0199(13) 0.0024(9) 0.0041(11) 0.0051(10) C407 0.0278(17) 0.0267(14) 0.051(2) 0.0093(14) -0.0084(15) 0.0080(13) C408 0.0265(16) 0.0196(13) 0.053(2) 0.0111(13) 0.0081(15) 0.0069(12) C409 0.0163(12) 0.0136(10) 0.0140(11) 0.0055(9) 0.0033(10) 0.0040(9) C410 0.0136(12) 0.0181(11) 0.0192(12) 0.0047(9) 0.0051(10) 0.0044(10) C411 0.0154(12) 0.0158(11) 0.0169(12) 0.0033(9) 0.0015(10) 0.0025(10) C412 0.0212(13) 0.0207(12) 0.0146(12) 0.0023(9) 0.0052(10) 0.0052(10) C413 0.0161(13) 0.0218(12) 0.0180(12) 0.0061(10) 0.0060(10) 0.0051(10) C414 0.0157(12) 0.0161(11) 0.0172(12) 0.0051(9) 0.0043(10) 0.0026(10) C415 0.0210(14) 0.0232(12) 0.0203(13) 0.0031(10) 0.0062(11) 0.0048(11) C416 0.0216(14) 0.0289(14) 0.0249(14) 0.0010(11) 0.0106(12) 0.0022(12) C417 0.0130(12) 0.0218(12) 0.0130(11) 0.0029(9) 0.0002(10) 0.0041(10) C418 0.0178(13) 0.0220(12) 0.0170(12) 0.0026(10) 0.0026(10) 0.0034(10) C419 0.0253(15) 0.0254(13) 0.0210(13) 0.0076(11) 0.0026(12) 0.0005(11) C420 0.0227(15) 0.0381(15) 0.0203(13) 0.0090(11) 0.0084(12) 0.0010(12) C421 0.0196(14) 0.0324(14) 0.0185(13) 0.0018(11) 0.0050(11) 0.0060(11) C422 0.0172(13) 0.0228(12) 0.0167(12) 0.0027(10) 0.0038(10) 0.0046(10) C423 0.0424(19) 0.0292(15) 0.0328(17) 0.0125(13) 0.0118(15) -0.0021(14) C424 0.0376(19) 0.0450(18) 0.0305(17) 0.0012(14) 0.0192(15) 0.0109(15) C425 0.0139(12) 0.0176(11) 0.0167(12) 0.0059(9) 0.0049(10) 0.0013(10) C426 0.0178(13) 0.0155(11) 0.0177(12) 0.0042(9) 0.0030(10) 0.0028(10) C427 0.0170(13) 0.0239(12) 0.0240(14) 0.0095(10) 0.0034(11) 0.0061(11) C428 0.0171(13) 0.0262(13) 0.0186(13) 0.0066(10) 0.0005(11) 0.0025(11) C429 0.0184(13) 0.0229(12) 0.0164(12) 0.0041(10) 0.0027(10) 0.0018(10) C430 0.0184(13) 0.0196(11) 0.0176(12) 0.0054(9) 0.0052(10) 0.0058(10) C431 0.0220(15) 0.0329(15) 0.0351(16) 0.0081(13) 0.0040(13) 0.0110(12) C432 0.0260(15) 0.0286(14) 0.0206(14) 0.0007(11) 0.0022(12) 0.0027(12) B400 0.0142(13) 0.0146(12) 0.0136(13) 0.0019(10) 0.0025(11) 0.0027(10) F201 0.063(3) 0.043(3) 0.089(4) 0.048(3) -0.006(3) -0.007(2) F202 0.019(2) 0.028(2) 0.104(5) 0.021(3) -0.001(3) 0.0017(17) F203 0.063(4) 0.031(2) 0.092(4) -0.022(3) 0.028(3) -0.013(2) F204 0.0267(9) 0.0349(9) 0.0630(13) 0.0171(9) -0.0043(9) 0.0149(8) F205 0.0214(10) 0.0798(15) 0.121(2) 0.0646(15) 0.0123(12) 0.0114(10) F206 0.0485(13) 0.0921(16) 0.0615(15) -0.0339(13) -0.0317(12) 0.0356(12) F207 0.0412(12) 0.0879(15) 0.0362(11) -0.0142(10) 0.0258(10) -0.0057(11) F208 0.0426(13) 0.151(2) 0.107(2) 0.0719(19) 0.0422(14) 0.0588(15) F209 0.0559(14) 0.0520(12) 0.110(2) -0.0349(12) 0.0625(15) -0.0261(11) F210 0.0406(11) 0.0556(11) 0.0197(9) 0.0026(8) -0.0028(8) -0.0124(9) F211 0.0378(11) 0.0225(8) 0.0608(13) 0.0067(8) -0.0069(9) -0.0014(7) F212 0.0169(8) 0.0525(11) 0.0484(11) -0.0180(9) 0.0046(8) 0.0020(8) F213 0.0580(13) 0.0436(10) 0.0170(8) -0.0011(7) -0.0016(8) 0.0070(9) F214 0.0567(13) 0.0349(10) 0.0471(12) -0.0094(8) 0.0213(10) -0.0205(9) F215 0.0525(12) 0.0376(10) 0.0406(11) -0.0155(8) -0.0125(9) 0.0230(9) F216 0.041(3) 0.030(2) 0.076(4) -0.008(2) -0.017(3) 0.021(2) F217 0.066(4) 0.072(4) 0.084(4) 0.055(3) 0.032(3) 0.043(3) F218 0.023(2) 0.032(2) 0.055(4) -0.004(2) 0.009(2) 0.0092(17) F219 0.0941(18) 0.0749(14) 0.0323(11) 0.0192(10) 0.0395(12) 0.0426(13) F220 0.0303(11) 0.0835(15) 0.0668(15) -0.0141(12) 0.0067(10) 0.0283(11) F221 0.0632(13) 0.0368(10) 0.0541(13) -0.0021(9) 0.0366(11) 0.0140(9) F222 0.0754(15) 0.0399(10) 0.0476(12) 0.0247(9) 0.0313(11) 0.0007(10) F223 0.0473(12) 0.0264(8) 0.0431(11) 0.0075(8) -0.0029(9) -0.0057(8) F224 0.0404(11) 0.0304(9) 0.0717(14) 0.0261(9) 0.0063(10) 0.0097(8) F301 0.076(4) 0.047(3) 0.043(3) 0.003(2) -0.008(3) -0.034(3) F302 0.039(2) 0.0165(18) 0.101(4) 0.022(2) -0.002(3) 0.0085(17) F303 0.032(3) 0.031(2) 0.074(4) 0.006(3) 0.024(3) -0.004(2) F316 0.044(3) 0.035(3) 0.048(3) 0.0132(19) -0.015(2) 0.020(2) F317 0.051(4) 0.067(4) 0.057(4) 0.014(3) 0.026(3) 0.038(3) F318 0.046(3) 0.021(2) 0.097(4) -0.002(2) -0.029(3) 0.0159(19) C201 0.0167(12) 0.0162(11) 0.0128(11) 0.0020(9) 0.0051(10) 0.0048(10) C202 0.0145(12) 0.0177(11) 0.0203(12) 0.0031(9) 0.0032(10) 0.0047(10) C203 0.0177(13) 0.0174(11) 0.0261(14) 0.0067(10) 0.0044(11) 0.0028(10) C204 0.0228(14) 0.0185(12) 0.0267(14) 0.0079(10) 0.0042(12) 0.0089(11) C205 0.0171(13) 0.0227(12) 0.0215(13) 0.0043(10) 0.0023(11) 0.0063(10) C206 0.0152(12) 0.0160(11) 0.0208(13) 0.0021(9) 0.0034(10) 0.0011(10) C207 0.0249(16) 0.0200(13) 0.0468(19) 0.0113(12) 0.0024(14) 0.0043(12) C208 0.0190(14) 0.0275(14) 0.0402(17) 0.0090(12) -0.0024(13) 0.0054(12) C209 0.0154(12) 0.0147(10) 0.0143(11) 0.0058(9) 0.0036(10) 0.0064(9) C210 0.0160(12) 0.0150(11) 0.0181(12) 0.0038(9) 0.0044(10) 0.0018(9) C211 0.0190(13) 0.0202(12) 0.0203(13) 0.0051(10) 0.0092(11) 0.0056(10) C212 0.0206(13) 0.0212(12) 0.0161(12) -0.0004(10) 0.0049(11) 0.0056(10) C213 0.0173(13) 0.0183(11) 0.0184(12) 0.0035(9) 0.0024(10) 0.0055(10) C214 0.0164(12) 0.0161(11) 0.0179(12) 0.0043(9) 0.0055(10) 0.0058(10) C215 0.0224(15) 0.0322(14) 0.0288(15) -0.0026(12) 0.0138(13) 0.0045(12) C216 0.0206(14) 0.0231(12) 0.0219(13) 0.0003(10) 0.0043(11) 0.0053(11) C217 0.0136(12) 0.0170(11) 0.0161(12) 0.0062(9) 0.0060(10) 0.0022(9) C218 0.0176(13) 0.0181(11) 0.0158(12) 0.0041(9) 0.0047(10) 0.0045(10) C219 0.0215(13) 0.0195(12) 0.0170(12) 0.0031(10) 0.0039(11) 0.0022(10) C220 0.0172(13) 0.0263(13) 0.0206(13) 0.0082(10) -0.0012(11) 0.0037(11) C221 0.0147(13) 0.0203(12) 0.0304(15) 0.0091(11) 0.0027(11) 0.0037(10) C222 0.0158(13) 0.0177(11) 0.0186(12) 0.0047(9) 0.0046(10) 0.0027(10) C223 0.0229(14) 0.0286(14) 0.0177(13) -0.0001(11) -0.0022(11) 0.0015(12) C224 0.0255(16) 0.0270(14) 0.0434(19) 0.0063(13) -0.0036(14) 0.0103(13) C225 0.0105(11) 0.0201(11) 0.0132(11) 0.0045(9) 0.0005(9) 0.0014(9) C226 0.0158(12) 0.0220(12) 0.0148(12) 0.0036(9) 0.0036(10) 0.0049(10) C227 0.0161(13) 0.0314(13) 0.0163(12) 0.0044(10) 0.0032(11) 0.0068(11) C228 0.0192(14) 0.0335(14) 0.0197(13) 0.0113(11) 0.0072(11) 0.0019(11) C229 0.0193(14) 0.0255(13) 0.0195(13) 0.0077(10) 0.0016(11) -0.0002(11) C230 0.0165(13) 0.0214(12) 0.0170(12) 0.0035(10) 0.0040(10) 0.0038(10) C231 0.0287(16) 0.0402(16) 0.0244(15) 0.0073(12) 0.0128(13) 0.0127(13) C232 0.0345(17) 0.0274(14) 0.0286(15) 0.0126(12) 0.0082(14) -0.0003(13) B200 0.0135(13) 0.0114(11) 0.0143(13) 0.0025(10) 0.0022(11) 0.0021(10) F915 0.0640(14) 0.0345(10) 0.0649(14) 0.0209(9) 0.0255(12) 0.0113(10) F916 0.0355(11) 0.0622(13) 0.0582(14) 0.0070(10) -0.0032(10) 0.0055(10) C909 0.0412(18) 0.0258(14) 0.0325(16) 0.0081(12) 0.0150(14) 0.0105(13) C910 0.0314(17) 0.0370(16) 0.0272(15) 0.0037(12) 0.0042(13) 0.0086(13) C911 0.056(2) 0.0374(17) 0.0285(16) 0.0128(13) 0.0094(16) 0.0133(16) C912 0.060(2) 0.0407(18) 0.0375(19) 0.0087(15) 0.0231(19) -0.0037(17) C913 0.0293(18) 0.061(2) 0.039(2) -0.0046(17) 0.0087(16) -0.0006(16) C914 0.0366(19) 0.0530(19) 0.0292(17) 0.0081(14) 0.0045(15) 0.0195(16) _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 C2 2.043(2) . ? Ir1 C17 2.050(3) . ? Ir1 C32 2.124(3) . ? O9 C4 1.360(3) . ? O9 C8 1.456(3) . ? O12 C5 1.358(3) . ? O12 C11 1.461(3) . ? O24 C19 1.367(4) . ? O24 C23 1.414(5) . ? O27 C20 1.354(4) . ? O27 C26 1.445(5) . ? O39 C34 1.356(3) . ? O39 C38 1.448(3) . ? O42 C35 1.363(3) . ? O42 C41 1.448(3) . ? N3 C2 1.369(3) . ? N3 C4 1.384(3) . ? N3 C7 1.492(3) . ? N6 C2 1.374(3) . ? N6 C5 1.390(3) . ? N6 C10 1.498(3) . ? N18 C17 1.375(4) . ? N18 C19 1.409(4) . ? N18 C22 1.484(4) . ? N21 C17 1.370(4) . ? N21 C20 1.387(4) . ? N21 C25 1.482(4) . ? N33 C32 1.378(3) . ? N33 C34 1.388(3) . ? N33 C37 1.502(3) . ? N36 C32 1.376(3) . ? N36 C35 1.388(3) . ? N36 C40 1.502(3) . ? C4 C5 1.334(4) . ? C7 C8 1.541(4) . ? C7 C13 1.530(4) . ? C7 C14 1.514(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.538(4) . ? C10 C15 1.521(4) . ? C10 C16 1.513(4) . ? C11 H11E 0.9700 . ? C11 H11F 0.9700 . ? C13 H13D 0.9600 . ? C13 H13E 0.9600 . ? C13 H13F 0.9600 . ? C14 H14D 0.9600 . ? C14 H14E 0.9600 . ? C14 H14F 0.9600 . ? C15 H15G 0.9600 . ? C15 H15H 0.9600 . ? C15 H15I 0.9600 . ? C16 H16G 0.9600 . ? C16 H16H 0.9600 . ? C16 H16I 0.9600 . ? C19 C20 1.307(5) . ? C22 C23 1.559(5) . ? C22 C28 1.534(5) . ? C22 C29 1.503(6) . ? C23 H23C 0.9700 . ? C23 H23D 0.9700 . ? C25 C26 1.539(5) . ? C25 C30 1.512(5) . ? C25 C31 1.503(5) . ? C26 H26C 0.9700 . ? C26 H26D 0.9700 . ? C28 H28D 0.9600 . ? C28 H28E 0.9600 . ? C28 H28F 0.9600 . ? C29 H29D 0.9600 . ? C29 H29E 0.9600 . ? C29 H29F 0.9600 . ? C30 H30D 0.9600 . ? C30 H30E 0.9600 . ? C30 H30F 0.9600 . ? C31 H31D 0.9600 . ? C31 H31E 0.9600 . ? C31 H31F 0.9600 . ? C34 C35 1.328(4) . ? C37 C38 1.540(4) . ? C37 C43 1.513(4) . ? C37 C44 1.509(4) . ? C38 H38C 0.9700 . ? C38 H38D 0.9700 . ? C40 C41 1.544(4) . ? C40 C45 1.505(4) . ? C40 C46 1.518(4) . ? C41 H41C 0.9700 . ? C41 H41D 0.9700 . ? C43 H43D 0.9600 . ? C43 H43E 0.9600 . ? C43 H43F 0.9600 . ? C44 H44D 0.9600 . ? C44 H44E 0.9600 . ? C44 H44F 0.9600 . ? C45 H45D 0.9600 . ? C45 H45E 0.9600 . ? C45 H45F 0.9600 . ? C46 H46D 0.9600 . ? C46 H46E 0.9600 . ? C46 H46F 0.9600 . ? Ir1A C2A 2.059(2) . ? Ir1A C17A 2.051(3) . ? Ir1A C32A 2.115(3) . ? O9A C4A 1.360(3) . ? O9A C8A 1.453(3) . ? O12A C5A 1.355(3) . ? O12A C11A 1.450(4) . ? O12A C11B 1.447(6) . ? O24A C19A 1.356(3) . ? O24A C23A 1.459(4) . ? O27A C20A 1.351(3) . ? O27A C26A 1.443(4) . ? O39A C34A 1.357(3) . ? O39A C38A 1.447(3) . ? O42A C35A 1.359(3) . ? O42A C41A 1.439(3) . ? N3A C2A 1.369(3) . ? N3A C4A 1.390(3) . ? N3A C7A 1.496(3) . ? N6A C2A 1.370(3) . ? N6A C5A 1.384(3) . ? N6A C10A 1.489(3) . ? N18A C17A 1.374(3) . ? N18A C19A 1.392(3) . ? N18A C22A 1.494(3) . ? N21A C17A 1.368(3) . ? N21A C20A 1.391(3) . ? N21A C25A 1.483(3) . ? N33A C32A 1.374(3) . ? N33A C34A 1.384(3) . ? N33A C37A 1.496(3) . ? N36A C32A 1.377(3) . ? N36A C35A 1.384(3) . ? N36A C40A 1.501(3) . ? C4A C5A 1.332(4) . ? C7A C8A 1.546(4) . ? C7A C13A 1.521(4) . ? C7A C14A 1.520(4) . ? C8A H8AA 0.9700 . ? C8A H8AB 0.9700 . ? C10A C11A 1.550(5) . ? C10A C11B 1.548(6) . ? C10A C15A 1.499(5) . ? C10A C15B 1.527(6) . ? C10A C16A 1.514(5) . ? C10A C16B 1.517(6) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C13A H13A 0.9600 . ? C13A H13B 0.9600 . ? C13A H13C 0.9600 . ? C14A H14A 0.9600 . ? C14A H14B 0.9600 . ? C14A H14C 0.9600 . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C19A C20A 1.329(4) . ? C22A C23A 1.534(4) . ? C22A C28A 1.525(4) . ? C22A C29A 1.515(4) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C25A C26A 1.547(4) . ? C25A C30A 1.512(4) . ? C25A C31A 1.514(4) . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? C31A H31A 0.9600 . ? C31A H31B 0.9600 . ? C31A H31C 0.9600 . ? C34A C35A 1.325(4) . ? C37A C38A 1.545(4) . ? C37A C43A 1.514(4) . ? C37A C44A 1.501(4) . ? C38A H38A 0.9700 . ? C38A H38B 0.9700 . ? C40A C41A 1.545(4) . ? C40A C45A 1.527(4) . ? C40A C46A 1.509(4) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C43A H43A 0.9600 . ? C43A H43B 0.9600 . ? C43A H43C 0.9600 . ? C44A H44A 0.9600 . ? C44A H44B 0.9600 . ? C44A H44C 0.9600 . ? C45A H45A 0.9600 . ? C45A H45B 0.9600 . ? C45A H45C 0.9600 . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? F907 C901 1.346(3) . ? F908 C902 1.354(3) . ? C901 C902 1.370(4) . ? C901 C906 1.375(4) . ? C902 C903 1.365(4) . ? C903 H903 0.9300 . ? C903 C904 1.379(5) . ? C904 H904 0.9300 . ? C904 C905 1.371(5) . ? C905 H905 0.9300 . ? C905 C906 1.386(5) . ? C906 H906 0.9300 . ? F401 C407 1.314(3) . ? F402 C407 1.326(4) . ? F403 C407 1.303(4) . ? F404 C408 1.290(3) . ? F405 C408 1.383(4) . ? F406 C408 1.315(4) . ? F407 C415 1.339(3) . ? F408 C415 1.344(3) . ? F409 C415 1.332(3) . ? F410 C416 1.316(3) . ? F411 C416 1.341(3) . ? F412 C416 1.325(3) . ? F413 C423 1.314(4) . ? F414 C423 1.334(4) . ? F415 C423 1.323(4) . ? F416 C424 1.317(3) . ? F417 C424 1.325(4) . ? F418 C424 1.298(3) . ? F419 C431 1.305(4) . ? F420 C431 1.326(3) . ? F421 C431 1.328(3) . ? F422 C432 1.311(4) . ? F423 C432 1.321(4) . ? F424 C432 1.319(4) . ? F504 C408 1.298(5) . ? F505 C408 1.401(5) . ? F506 C408 1.285(4) . ? F516 C424 1.320(6) . ? F517 C424 1.316(6) . ? F518 C424 1.289(6) . ? F522 C432 1.302(5) . ? F523 C432 1.326(5) . ? F524 C432 1.336(5) . ? C401 C402 1.399(3) . ? C401 C406 1.397(3) . ? C401 B400 1.646(3) . ? C402 H402 0.9300 . ? C402 C403 1.390(3) . ? C403 C404 1.385(4) . ? C403 C407 1.497(4) . ? C404 H404 0.9300 . ? C404 C405 1.379(4) . ? C405 C406 1.393(3) . ? C405 C408 1.491(4) . ? C406 H406 0.9300 . ? C409 C410 1.398(3) . ? C409 C414 1.398(3) . ? C409 B400 1.638(3) . ? C410 H410 0.9300 . ? C410 C411 1.394(3) . ? C411 C412 1.395(3) . ? C411 C415 1.496(4) . ? C412 H412 0.9300 . ? C412 C413 1.377(4) . ? C413 C414 1.396(3) . ? C413 C416 1.497(3) . ? C414 H414 0.9300 . ? C417 C418 1.398(3) . ? C417 C422 1.402(3) . ? C417 B400 1.642(4) . ? C418 H418 0.9300 . ? C418 C419 1.388(4) . ? C419 C420 1.384(4) . ? C419 C423 1.501(4) . ? C420 H420 0.9300 . ? C420 C421 1.385(4) . ? C421 C422 1.383(3) . ? C421 C424 1.504(4) . ? C422 H422 0.9300 . ? C425 C426 1.403(3) . ? C425 C430 1.403(3) . ? C425 B400 1.635(4) . ? C426 H426 0.9300 . ? C426 C427 1.392(4) . ? C427 C428 1.386(4) . ? C427 C431 1.502(3) . ? C428 H428 0.9300 . ? C428 C429 1.390(3) . ? C429 C430 1.387(3) . ? C429 C432 1.498(3) . ? C430 H430 0.9300 . ? F201 C207 1.355(4) . ? F202 C207 1.299(4) . ? F203 C207 1.309(4) . ? F204 C208 1.326(3) . ? F205 C208 1.328(4) . ? F206 C208 1.327(4) . ? F207 C215 1.314(3) . ? F208 C215 1.327(4) . ? F209 C215 1.307(3) . ? F210 C216 1.333(3) . ? F211 C216 1.339(3) . ? F212 C216 1.337(3) . ? F213 C223 1.336(3) . ? F214 C223 1.341(3) . ? F215 C223 1.325(3) . ? F216 C224 1.361(4) . ? F217 C224 1.297(5) . ? F218 C224 1.360(5) . ? F219 C231 1.327(3) . ? F220 C231 1.329(3) . ? F221 C231 1.317(3) . ? F222 C232 1.332(3) . ? F223 C232 1.338(3) . ? F224 C232 1.338(3) . ? F301 C207 1.354(4) . ? F302 C207 1.296(4) . ? F303 C207 1.319(4) . ? F316 C224 1.380(4) . ? F317 C224 1.302(5) . ? F318 C224 1.325(4) . ? C201 C202 1.397(3) . ? C201 C206 1.405(3) . ? C201 B200 1.642(3) . ? C202 H202 0.9300 . ? C202 C203 1.393(3) . ? C203 C204 1.382(4) . ? C203 C207 1.497(4) . ? C204 H204 0.9300 . ? C204 C205 1.387(4) . ? C205 C206 1.390(3) . ? C205 C208 1.491(4) . ? C206 H206 0.9300 . ? C209 C210 1.400(3) . ? C209 C214 1.400(3) . ? C209 B200 1.639(3) . ? C210 H210 0.9300 . ? C210 C211 1.402(3) . ? C211 C212 1.377(4) . ? C211 C215 1.490(3) . ? C212 H212 0.9300 . ? C212 C213 1.394(3) . ? C213 C214 1.395(3) . ? C213 C216 1.492(4) . ? C214 H214 0.9300 . ? C217 C218 1.409(3) . ? C217 C222 1.400(3) . ? C217 B200 1.631(4) . ? C218 H218 0.9300 . ? C218 C219 1.382(4) . ? C219 C220 1.388(3) . ? C219 C223 1.496(3) . ? C220 H220 0.9300 . ? C220 C221 1.382(3) . ? C221 C222 1.394(4) . ? C221 C224 1.495(4) . ? C222 H222 0.9300 . ? C225 C226 1.403(3) . ? C225 C230 1.396(3) . ? C225 B200 1.639(3) . ? C226 H226 0.9300 . ? C226 C227 1.384(3) . ? C227 C228 1.389(4) . ? C227 C231 1.501(3) . ? C228 H228 0.9300 . ? C228 C229 1.385(4) . ? C229 C230 1.391(3) . ? C229 C232 1.501(4) . ? C230 H230 0.9300 . ? F915 C909 1.347(3) . ? F916 C910 1.352(4) . ? C909 C910 1.375(4) . ? C909 C914 1.364(4) . ? C910 C911 1.361(4) . ? C911 H911 0.9300 . ? C911 C912 1.375(5) . ? C912 H912 0.9300 . ? C912 C913 1.370(5) . ? C913 H913 0.9300 . ? C913 C914 1.391(5) . ? C914 H914 0.9300 . ? 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 C2 Ir1 C17 166.70(10) . . ? C2 Ir1 C32 97.55(9) . . ? C17 Ir1 C32 95.55(10) . . ? C4 O9 C8 103.43(19) . . ? C5 O12 C11 103.92(19) . . ? C19 O24 C23 105.6(3) . . ? C20 O27 C26 103.2(3) . . ? C34 O39 C38 103.4(2) . . ? C35 O42 C41 103.5(2) . . ? C2 N3 C4 113.5(2) . . ? C2 N3 C7 136.9(2) . . ? C4 N3 C7 107.6(2) . . ? C2 N6 C5 112.9(2) . . ? C2 N6 C10 138.5(2) . . ? C5 N6 C10 107.6(2) . . ? C17 N18 C19 111.1(3) . . ? C17 N18 C22 137.3(3) . . ? C19 N18 C22 108.4(3) . . ? C17 N21 C20 113.9(3) . . ? C17 N21 C25 137.2(3) . . ? C20 N21 C25 108.4(3) . . ? C32 N33 C34 112.9(2) . . ? C32 N33 C37 139.1(2) . . ? C34 N33 C37 107.9(2) . . ? C32 N36 C35 113.2(2) . . ? C32 N36 C40 139.0(2) . . ? C35 N36 C40 107.0(2) . . ? N3 C2 Ir1 125.63(18) . . ? N3 C2 N6 100.9(2) . . ? N6 C2 Ir1 133.48(18) . . ? O9 C4 N3 113.8(2) . . ? C5 C4 O9 139.8(2) . . ? C5 C4 N3 106.3(2) . . ? O12 C5 N6 113.7(2) . . ? C4 C5 O12 139.8(2) . . ? C4 C5 N6 106.4(2) . . ? N3 C7 C8 97.4(2) . . ? N3 C7 C13 108.7(2) . . ? N3 C7 C14 115.1(2) . . ? C13 C7 C8 110.8(2) . . ? C14 C7 C8 112.1(2) . . ? C14 C7 C13 111.9(3) . . ? O9 C8 C7 106.6(2) . . ? O9 C8 H8A 110.4 . . ? O9 C8 H8B 110.4 . . ? C7 C8 H8A 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? N6 C10 C11 98.2(2) . . ? N6 C10 C15 108.2(2) . . ? N6 C10 C16 114.2(2) . . ? C15 C10 C11 111.5(2) . . ? C16 C10 C11 112.0(2) . . ? C16 C10 C15 112.0(2) . . ? O12 C11 C10 106.4(2) . . ? O12 C11 H11E 110.4 . . ? O12 C11 H11F 110.4 . . ? C10 C11 H11E 110.4 . . ? C10 C11 H11F 110.4 . . ? H11E C11 H11F 108.6 . . ? C7 C13 H13D 109.5 . . ? C7 C13 H13E 109.5 . . ? C7 C13 H13F 109.5 . . ? H13D C13 H13E 109.5 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? C7 C14 H14D 109.5 . . ? C7 C14 H14E 109.5 . . ? C7 C14 H14F 109.5 . . ? H14D C14 H14E 109.5 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C10 C15 H15G 109.5 . . ? C10 C15 H15H 109.5 . . ? C10 C15 H15I 109.5 . . ? H15G C15 H15H 109.5 . . ? H15G C15 H15I 109.5 . . ? H15H C15 H15I 109.5 . . ? C10 C16 H16G 109.5 . . ? C10 C16 H16H 109.5 . . ? C10 C16 H16I 109.5 . . ? H16G C16 H16H 109.5 . . ? H16G C16 H16I 109.5 . . ? H16H C16 H16I 109.5 . . ? N18 C17 Ir1 129.7(2) . . ? N21 C17 Ir1 129.0(2) . . ? N21 C17 N18 101.2(2) . . ? O24 C19 N18 111.6(3) . . ? C20 C19 O24 140.1(3) . . ? C20 C19 N18 108.1(3) . . ? O27 C20 N21 113.0(3) . . ? C19 C20 O27 141.3(3) . . ? C19 C20 N21 105.7(3) . . ? N18 C22 C23 96.9(3) . . ? N18 C22 C28 108.7(3) . . ? N18 C22 C29 115.5(3) . . ? C28 C22 C23 110.3(3) . . ? C29 C22 C23 112.5(3) . . ? C29 C22 C28 111.9(3) . . ? O24 C23 C22 107.4(3) . . ? O24 C23 H23C 110.2 . . ? O24 C23 H23D 110.2 . . ? C22 C23 H23C 110.2 . . ? C22 C23 H23D 110.2 . . ? H23C C23 H23D 108.5 . . ? N21 C25 C26 98.7(3) . . ? N21 C25 C30 110.1(3) . . ? N21 C25 C31 111.4(3) . . ? C30 C25 C26 112.0(3) . . ? C31 C25 C26 111.1(3) . . ? C31 C25 C30 112.9(3) . . ? O27 C26 C25 106.5(3) . . ? O27 C26 H26C 110.4 . . ? O27 C26 H26D 110.4 . . ? C25 C26 H26C 110.4 . . ? C25 C26 H26D 110.4 . . ? H26C C26 H26D 108.6 . . ? C22 C28 H28D 109.5 . . ? C22 C28 H28E 109.5 . . ? C22 C28 H28F 109.5 . . ? H28D C28 H28E 109.5 . . ? H28D C28 H28F 109.5 . . ? H28E C28 H28F 109.5 . . ? C22 C29 H29D 109.5 . . ? C22 C29 H29E 109.5 . . ? C22 C29 H29F 109.5 . . ? H29D C29 H29E 109.5 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? C25 C30 H30D 109.5 . . ? C25 C30 H30E 109.5 . . ? C25 C30 H30F 109.5 . . ? H30D C30 H30E 109.5 . . ? H30D C30 H30F 109.5 . . ? H30E C30 H30F 109.5 . . ? C25 C31 H31D 109.5 . . ? C25 C31 H31E 109.5 . . ? C25 C31 H31F 109.5 . . ? H31D C31 H31E 109.5 . . ? H31D C31 H31F 109.5 . . ? H31E C31 H31F 109.5 . . ? N33 C32 Ir1 128.76(18) . . ? N36 C32 Ir1 130.46(18) . . ? N36 C32 N33 100.8(2) . . ? O39 C34 N33 113.6(2) . . ? C35 C34 O39 139.6(3) . . ? C35 C34 N33 106.8(2) . . ? O42 C35 N36 113.9(2) . . ? C34 C35 O42 139.7(3) . . ? C34 C35 N36 106.4(2) . . ? N33 C37 C38 97.8(2) . . ? N33 C37 C43 111.0(2) . . ? N33 C37 C44 113.9(2) . . ? C43 C37 C38 110.1(2) . . ? C44 C37 C38 110.5(2) . . ? C44 C37 C43 112.6(3) . . ? O39 C38 C37 106.9(2) . . ? O39 C38 H38C 110.3 . . ? O39 C38 H38D 110.3 . . ? C37 C38 H38C 110.3 . . ? C37 C38 H38D 110.3 . . ? H38C C38 H38D 108.6 . . ? N36 C40 C41 97.9(2) . . ? N36 C40 C45 113.6(3) . . ? N36 C40 C46 110.5(2) . . ? C45 C40 C41 112.4(2) . . ? C45 C40 C46 111.9(3) . . ? C46 C40 C41 109.9(3) . . ? O42 C41 C40 106.2(2) . . ? O42 C41 H41C 110.5 . . ? O42 C41 H41D 110.5 . . ? C40 C41 H41C 110.5 . . ? C40 C41 H41D 110.5 . . ? H41C C41 H41D 108.7 . . ? C37 C43 H43D 109.5 . . ? C37 C43 H43E 109.5 . . ? C37 C43 H43F 109.5 . . ? H43D C43 H43E 109.5 . . ? H43D C43 H43F 109.5 . . ? H43E C43 H43F 109.5 . . ? C37 C44 H44D 109.5 . . ? C37 C44 H44E 109.5 . . ? C37 C44 H44F 109.5 . . ? H44D C44 H44E 109.5 . . ? H44D C44 H44F 109.5 . . ? H44E C44 H44F 109.5 . . ? C40 C45 H45D 109.5 . . ? C40 C45 H45E 109.5 . . ? C40 C45 H45F 109.5 . . ? H45D C45 H45E 109.5 . . ? H45D C45 H45F 109.5 . . ? H45E C45 H45F 109.5 . . ? C40 C46 H46D 109.5 . . ? C40 C46 H46E 109.5 . . ? C40 C46 H46F 109.5 . . ? H46D C46 H46E 109.5 . . ? H46D C46 H46F 109.5 . . ? H46E C46 H46F 109.5 . . ? C2A Ir1A C32A 98.31(9) . . ? C17A Ir1A C2A 163.39(10) . . ? C17A Ir1A C32A 98.16(10) . . ? C4A O9A C8A 103.35(19) . . ? C5A O12A C11A 104.7(2) . . ? C5A O12A C11B 105.4(3) . . ? C19A O24A C23A 104.1(2) . . ? C20A O27A C26A 106.1(2) . . ? C34A O39A C38A 103.3(2) . . ? C35A O42A C41A 104.7(2) . . ? C2A N3A C4A 112.7(2) . . ? C2A N3A C7A 138.9(2) . . ? C4A N3A C7A 107.6(2) . . ? C2A N6A C5A 113.1(2) . . ? C2A N6A C10A 138.0(2) . . ? C5A N6A C10A 108.9(2) . . ? C17A N18A C19A 113.3(2) . . ? C17A N18A C22A 136.4(2) . . ? C19A N18A C22A 107.1(2) . . ? C17A N21A C20A 113.3(2) . . ? C17A N21A C25A 136.9(2) . . ? C20A N21A C25A 109.2(2) . . ? C32A N33A C34A 113.3(2) . . ? C32A N33A C37A 138.8(2) . . ? C34A N33A C37A 107.9(2) . . ? C32A N36A C35A 112.8(2) . . ? C32A N36A C40A 138.7(2) . . ? C35A N36A C40A 107.9(2) . . ? N3A C2A Ir1A 126.60(18) . . ? N3A C2A N6A 101.3(2) . . ? N6A C2A Ir1A 131.73(18) . . ? O9A C4A N3A 113.9(2) . . ? C5A C4A O9A 139.5(2) . . ? C5A C4A N3A 106.6(2) . . ? O12A C5A N6A 113.7(2) . . ? C4A C5A O12A 140.0(2) . . ? C4A C5A N6A 106.3(2) . . ? N3A C7A C8A 97.5(2) . . ? N3A C7A C13A 109.5(2) . . ? N3A C7A C14A 115.5(2) . . ? C13A C7A C8A 111.0(2) . . ? C14A C7A C8A 110.9(2) . . ? C14A C7A C13A 111.7(3) . . ? O9A C8A C7A 106.6(2) . . ? O9A C8A H8AA 110.4 . . ? O9A C8A H8AB 110.4 . . ? C7A C8A H8AA 110.4 . . ? C7A C8A H8AB 110.4 . . ? H8AA C8A H8AB 108.6 . . ? N6A C10A C11A 99.0(2) . . ? N6A C10A C11B 99.7(3) . . ? N6A C10A C15A 111.3(3) . . ? N6A C10A C15B 108.8(4) . . ? N6A C10A C16A 109.4(3) . . ? N6A C10A C16B 115.5(4) . . ? C15A C10A C11A 112.3(3) . . ? C15A C10A C16A 113.6(4) . . ? C15B C10A C11B 111.7(5) . . ? C16A C10A C11A 110.2(4) . . ? C16B C10A C11B 109.8(5) . . ? C16B C10A C15B 111.0(5) . . ? O12A C11A C10A 107.2(3) . . ? O12A C11A H11A 110.3 . . ? O12A C11A H11B 110.3 . . ? C10A C11A H11A 110.3 . . ? C10A C11A H11B 110.3 . . ? H11A C11A H11B 108.5 . . ? O12A C11B C10A 107.5(4) . . ? O12A C11B H11C 110.2 . . ? O12A C11B H11D 110.2 . . ? C10A C11B H11C 110.2 . . ? C10A C11B H11D 110.2 . . ? H11C C11B H11D 108.5 . . ? C7A C13A H13A 109.5 . . ? C7A C13A H13B 109.5 . . ? C7A C13A H13C 109.5 . . ? H13A C13A H13B 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? C7A C14A H14A 109.5 . . ? C7A C14A H14B 109.5 . . ? C7A C14A H14C 109.5 . . ? H14A C14A H14B 109.5 . . ? H14A C14A H14C 109.5 . . ? H14B C14A H14C 109.5 . . ? C10A C15A H15A 109.5 . . ? C10A C15A H15B 109.5 . . ? C10A C15A H15C 109.5 . . ? H15A C15A H15B 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C10A C15B H15D 109.5 . . ? C10A C15B H15E 109.5 . . ? C10A C15B H15F 109.5 . . ? H15D C15B H15E 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? C10A C16A H16A 109.5 . . ? C10A C16A H16B 109.5 . . ? C10A C16A H16C 109.5 . . ? H16A C16A H16B 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C10A C16B H16D 109.5 . . ? C10A C16B H16E 109.5 . . ? C10A C16B H16F 109.5 . . ? H16D C16B H16E 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? N18A C17A Ir1A 123.76(18) . . ? N21A C17A Ir1A 135.36(18) . . ? N21A C17A N18A 100.8(2) . . ? O24A C19A N18A 113.3(2) . . ? C20A C19A O24A 140.3(3) . . ? C20A C19A N18A 106.2(2) . . ? O27A C20A N21A 114.1(2) . . ? C19A C20A O27A 139.4(3) . . ? C19A C20A N21A 106.5(2) . . ? N18A C22A C23A 97.6(2) . . ? N18A C22A C28A 109.0(2) . . ? N18A C22A C29A 113.8(2) . . ? C28A C22A C23A 110.7(3) . . ? C29A C22A C23A 113.3(3) . . ? C29A C22A C28A 111.7(3) . . ? O24A C23A C22A 106.1(2) . . ? O24A C23A H23A 110.5 . . ? O24A C23A H23B 110.5 . . ? C22A C23A H23A 110.5 . . ? C22A C23A H23B 110.5 . . ? H23A C23A H23B 108.7 . . ? N21A C25A C26A 100.1(2) . . ? N21A C25A C30A 110.0(2) . . ? N21A C25A C31A 112.7(2) . . ? C30A C25A C26A 111.4(3) . . ? C30A C25A C31A 112.1(3) . . ? C31A C25A C26A 109.8(3) . . ? O27A C26A C25A 109.1(2) . . ? O27A C26A H26A 109.9 . . ? O27A C26A H26B 109.9 . . ? C25A C26A H26A 109.9 . . ? C25A C26A H26B 109.9 . . ? H26A C26A H26B 108.3 . . ? C22A C28A H28A 109.5 . . ? C22A C28A H28B 109.5 . . ? C22A C28A H28C 109.5 . . ? H28A C28A H28B 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C22A C29A H29A 109.5 . . ? C22A C29A H29B 109.5 . . ? C22A C29A H29C 109.5 . . ? H29A C29A H29B 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C25A C30A H30A 109.5 . . ? C25A C30A H30B 109.5 . . ? C25A C30A H30C 109.5 . . ? H30A C30A H30B 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C25A C31A H31A 109.5 . . ? C25A C31A H31B 109.5 . . ? C25A C31A H31C 109.5 . . ? H31A C31A H31B 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? N33A C32A Ir1A 130.16(17) . . ? N33A C32A N36A 100.6(2) . . ? N36A C32A Ir1A 129.21(18) . . ? O39A C34A N33A 113.9(2) . . ? C35A C34A O39A 139.7(3) . . ? C35A C34A N33A 106.3(2) . . ? O42A C35A N36A 114.1(2) . . ? C34A C35A O42A 138.8(3) . . ? C34A C35A N36A 107.0(2) . . ? N33A C37A C38A 98.1(2) . . ? N33A C37A C43A 110.1(2) . . ? N33A C37A C44A 113.6(2) . . ? C43A C37A C38A 110.3(2) . . ? C44A C37A C38A 111.4(2) . . ? C44A C37A C43A 112.4(3) . . ? O39A C38A C37A 106.7(2) . . ? O39A C38A H38A 110.4 . . ? O39A C38A H38B 110.4 . . ? C37A C38A H38A 110.4 . . ? C37A C38A H38B 110.4 . . ? H38A C38A H38B 108.6 . . ? N36A C40A C41A 98.8(2) . . ? N36A C40A C45A 109.5(2) . . ? N36A C40A C46A 115.5(2) . . ? C45A C40A C41A 111.0(2) . . ? C46A C40A C41A 109.4(2) . . ? C46A C40A C45A 111.9(2) . . ? O42A C41A C40A 107.8(2) . . ? O42A C41A H41A 110.2 . . ? O42A C41A H41B 110.2 . . ? C40A C41A H41A 110.2 . . ? C40A C41A H41B 110.2 . . ? H41A C41A H41B 108.5 . . ? C37A C43A H43A 109.5 . . ? C37A C43A H43B 109.5 . . ? C37A C43A H43C 109.5 . . ? H43A C43A H43B 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C37A C44A H44A 109.5 . . ? C37A C44A H44B 109.5 . . ? C37A C44A H44C 109.5 . . ? H44A C44A H44B 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C40A C45A H45A 109.5 . . ? C40A C45A H45B 109.5 . . ? C40A C45A H45C 109.5 . . ? H45A C45A H45B 109.5 . . ? H45A C45A H45C 109.5 . . ? H45B C45A H45C 109.5 . . ? C40A C46A H46A 109.5 . . ? C40A C46A H46B 109.5 . . ? C40A C46A H46C 109.5 . . ? H46A C46A H46B 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? F907 C901 C902 118.7(3) . . ? F907 C901 C906 120.3(3) . . ? C902 C901 C906 121.0(3) . . ? F908 C902 C901 119.0(3) . . ? F908 C902 C903 120.2(3) . . ? C903 C902 C901 120.9(3) . . ? C902 C903 H903 120.7 . . ? C902 C903 C904 118.7(3) . . ? C904 C903 H903 120.7 . . ? C903 C904 H904 119.6 . . ? C905 C904 C903 120.9(3) . . ? C905 C904 H904 119.6 . . ? C904 C905 H905 119.8 . . ? C904 C905 C906 120.3(3) . . ? C906 C905 H905 119.8 . . ? C901 C906 C905 118.3(3) . . ? C901 C906 H906 120.9 . . ? C905 C906 H906 120.9 . . ? C402 C401 B400 120.6(2) . . ? C406 C401 C402 115.5(2) . . ? C406 C401 B400 123.8(2) . . ? C401 C402 H402 118.7 . . ? C403 C402 C401 122.5(2) . . ? C403 C402 H402 118.7 . . ? C402 C403 C407 118.7(2) . . ? C404 C403 C402 120.7(2) . . ? C404 C403 C407 120.6(2) . . ? C403 C404 H404 121.1 . . ? C405 C404 C403 117.8(2) . . ? C405 C404 H404 121.1 . . ? C404 C405 C406 121.4(2) . . ? C404 C405 C408 119.8(2) . . ? C406 C405 C408 118.8(2) . . ? C401 C406 H406 119.0 . . ? C405 C406 C401 122.0(2) . . ? C405 C406 H406 119.0 . . ? F401 C407 F402 104.6(3) . . ? F401 C407 C403 114.5(3) . . ? F402 C407 C403 112.2(3) . . ? F403 C407 F401 107.9(3) . . ? F403 C407 F402 104.8(3) . . ? F403 C407 C403 112.1(3) . . ? F404 C408 F405 104.0(3) . . ? F404 C408 F406 109.4(3) . . ? F404 C408 C405 116.0(3) . . ? F405 C408 C405 109.5(3) . . ? F406 C408 F405 103.0(3) . . ? F406 C408 C405 113.7(3) . . ? F504 C408 F505 102.6(4) . . ? F504 C408 C405 116.4(4) . . ? F505 C408 C405 108.4(3) . . ? F506 C408 F504 109.8(4) . . ? F506 C408 F505 102.4(4) . . ? F506 C408 C405 115.4(3) . . ? C410 C409 C414 115.9(2) . . ? C410 C409 B400 123.3(2) . . ? C414 C409 B400 120.5(2) . . ? C409 C410 H410 118.9 . . ? C411 C410 C409 122.2(2) . . ? C411 C410 H410 118.9 . . ? C410 C411 C412 120.7(2) . . ? C410 C411 C415 120.9(2) . . ? C412 C411 C415 118.3(2) . . ? C411 C412 H412 120.9 . . ? C413 C412 C411 118.1(2) . . ? C413 C412 H412 120.9 . . ? C412 C413 C414 120.9(2) . . ? C412 C413 C416 120.2(2) . . ? C414 C413 C416 118.8(2) . . ? C409 C414 H414 118.9 . . ? C413 C414 C409 122.2(2) . . ? C413 C414 H414 118.9 . . ? F407 C415 F408 105.1(2) . . ? F407 C415 C411 112.8(2) . . ? F408 C415 C411 112.2(2) . . ? F409 C415 F407 106.6(2) . . ? F409 C415 F408 106.0(2) . . ? F409 C415 C411 113.5(2) . . ? F410 C416 F411 105.3(2) . . ? F410 C416 F412 107.1(2) . . ? F410 C416 C413 113.6(2) . . ? F411 C416 C413 111.6(2) . . ? F412 C416 F411 105.1(2) . . ? F412 C416 C413 113.4(2) . . ? C418 C417 C422 115.6(2) . . ? C418 C417 B400 122.9(2) . . ? C422 C417 B400 120.9(2) . . ? C417 C418 H418 119.0 . . ? C419 C418 C417 122.0(2) . . ? C419 C418 H418 119.0 . . ? C418 C419 C423 119.0(2) . . ? C420 C419 C418 121.3(2) . . ? C420 C419 C423 119.7(2) . . ? C419 C420 H420 121.2 . . ? C419 C420 C421 117.6(2) . . ? C421 C420 H420 121.2 . . ? C420 C421 C424 119.2(2) . . ? C422 C421 C420 121.1(2) . . ? C422 C421 C424 119.7(2) . . ? C417 C422 H422 118.9 . . ? C421 C422 C417 122.3(2) . . ? C421 C422 H422 118.9 . . ? F413 C423 F414 105.7(3) . . ? F413 C423 F415 107.0(3) . . ? F413 C423 C419 113.7(3) . . ? F414 C423 C419 112.4(2) . . ? F415 C423 F414 104.5(3) . . ? F415 C423 C419 112.7(3) . . ? F416 C424 F417 104.5(3) . . ? F416 C424 C421 112.7(3) . . ? F417 C424 C421 111.5(2) . . ? F418 C424 F416 106.7(3) . . ? F418 C424 F417 106.7(3) . . ? F418 C424 C421 114.1(2) . . ? F516 C424 C421 112.0(5) . . ? F517 C424 F516 105.0(6) . . ? F517 C424 C421 111.6(5) . . ? F518 C424 F516 106.1(6) . . ? F518 C424 F517 106.3(6) . . ? F518 C424 C421 115.2(5) . . ? C426 C425 C430 115.6(2) . . ? C426 C425 B400 124.0(2) . . ? C430 C425 B400 120.2(2) . . ? C425 C426 H426 119.0 . . ? C427 C426 C425 122.1(2) . . ? C427 C426 H426 119.0 . . ? C426 C427 C431 120.2(2) . . ? C428 C427 C426 121.2(2) . . ? C428 C427 C431 118.5(2) . . ? C427 C428 H428 121.2 . . ? C427 C428 C429 117.6(2) . . ? C429 C428 H428 121.2 . . ? C428 C429 C432 120.0(2) . . ? C430 C429 C428 121.1(2) . . ? C430 C429 C432 118.8(2) . . ? C425 C430 H430 118.8 . . ? C429 C430 C425 122.3(2) . . ? C429 C430 H430 118.8 . . ? F419 C431 F420 106.5(3) . . ? F419 C431 F421 106.4(3) . . ? F419 C431 C427 112.8(2) . . ? F420 C431 F421 104.5(2) . . ? F420 C431 C427 112.7(2) . . ? F421 C431 C427 113.3(2) . . ? F422 C432 F423 106.1(3) . . ? F422 C432 F424 106.6(3) . . ? F422 C432 C429 114.1(3) . . ? F423 C432 C429 112.1(3) . . ? F424 C432 F423 105.8(3) . . ? F424 C432 C429 111.6(3) . . ? F522 C432 F523 105.8(4) . . ? F522 C432 F524 105.8(4) . . ? F522 C432 C429 115.6(4) . . ? F523 C432 F524 103.6(4) . . ? F523 C432 C429 112.9(4) . . ? F524 C432 C429 112.2(3) . . ? C409 B400 C401 105.10(19) . . ? C409 B400 C417 114.04(19) . . ? C417 B400 C401 110.11(19) . . ? C425 B400 C401 111.67(19) . . ? C425 B400 C409 112.89(19) . . ? C425 B400 C417 103.20(19) . . ? C202 C201 C206 115.4(2) . . ? C202 C201 B200 124.4(2) . . ? C206 C201 B200 120.1(2) . . ? C201 C202 H202 118.9 . . ? C203 C202 C201 122.3(2) . . ? C203 C202 H202 118.9 . . ? C202 C203 C207 119.1(2) . . ? C204 C203 C202 121.1(2) . . ? C204 C203 C207 119.7(2) . . ? C203 C204 H204 121.0 . . ? C203 C204 C205 117.9(2) . . ? C205 C204 H204 121.0 . . ? C204 C205 C206 120.9(2) . . ? C204 C205 C208 120.4(2) . . ? C206 C205 C208 118.7(2) . . ? C201 C206 H206 118.8 . . ? C205 C206 C201 122.4(2) . . ? C205 C206 H206 118.8 . . ? F201 C207 C203 110.6(3) . . ? F202 C207 F201 105.4(4) . . ? F202 C207 F203 108.1(4) . . ? F202 C207 C203 115.1(3) . . ? F203 C207 F201 104.4(3) . . ? F203 C207 C203 112.4(3) . . ? F301 C207 C203 110.8(3) . . ? F302 C207 F301 104.6(3) . . ? F302 C207 F303 108.6(4) . . ? F302 C207 C203 115.4(3) . . ? F303 C207 F301 104.1(4) . . ? F303 C207 C203 112.5(3) . . ? F204 C208 F205 105.7(2) . . ? F204 C208 F206 106.3(3) . . ? F204 C208 C205 114.2(2) . . ? F205 C208 C205 112.2(3) . . ? F206 C208 F205 105.9(3) . . ? F206 C208 C205 111.8(2) . . ? C210 C209 B200 121.3(2) . . ? C214 C209 C210 115.9(2) . . ? C214 C209 B200 122.5(2) . . ? C209 C210 H210 119.0 . . ? C209 C210 C211 122.0(2) . . ? C211 C210 H210 119.0 . . ? C210 C211 C215 119.1(2) . . ? C212 C211 C210 121.0(2) . . ? C212 C211 C215 119.8(2) . . ? C211 C212 H212 120.9 . . ? C211 C212 C213 118.2(2) . . ? C213 C212 H212 120.9 . . ? C212 C213 C214 120.7(2) . . ? C212 C213 C216 118.5(2) . . ? C214 C213 C216 120.8(2) . . ? C209 C214 H214 118.9 . . ? C213 C214 C209 122.3(2) . . ? C213 C214 H214 118.9 . . ? F207 C215 F208 104.3(2) . . ? F207 C215 C211 114.0(2) . . ? F208 C215 C211 111.5(2) . . ? F209 C215 F207 106.5(3) . . ? F209 C215 F208 105.7(3) . . ? F209 C215 C211 114.1(2) . . ? F210 C216 F211 105.0(2) . . ? F210 C216 F212 106.5(2) . . ? F210 C216 C213 113.0(2) . . ? F211 C216 C213 112.5(2) . . ? F212 C216 F211 105.6(2) . . ? F212 C216 C213 113.6(2) . . ? C218 C217 B200 120.2(2) . . ? C222 C217 C218 115.5(2) . . ? C222 C217 B200 123.9(2) . . ? C217 C218 H218 118.8 . . ? C219 C218 C217 122.4(2) . . ? C219 C218 H218 118.8 . . ? C218 C219 C220 121.0(2) . . ? C218 C219 C223 120.4(2) . . ? C220 C219 C223 118.5(2) . . ? C219 C220 H220 121.0 . . ? C221 C220 C219 117.9(2) . . ? C221 C220 H220 121.0 . . ? C220 C221 C222 121.1(2) . . ? C220 C221 C224 118.9(2) . . ? C222 C221 C224 120.0(2) . . ? C217 C222 H222 119.0 . . ? C221 C222 C217 122.0(2) . . ? C221 C222 H222 119.0 . . ? F213 C223 F214 105.3(2) . . ? F213 C223 C219 113.1(2) . . ? F214 C223 C219 111.6(2) . . ? F215 C223 F213 105.7(2) . . ? F215 C223 F214 107.4(2) . . ? F215 C223 C219 113.2(2) . . ? F216 C224 C221 112.5(3) . . ? F217 C224 F216 108.4(4) . . ? F217 C224 F218 106.0(4) . . ? F217 C224 C221 116.4(4) . . ? F218 C224 F216 101.4(4) . . ? F218 C224 C221 110.9(3) . . ? F316 C224 C221 110.1(3) . . ? F317 C224 F316 104.6(4) . . ? F317 C224 F318 110.7(4) . . ? F317 C224 C221 115.0(4) . . ? F318 C224 F316 102.3(3) . . ? F318 C224 C221 113.0(3) . . ? C226 C225 B200 120.9(2) . . ? C230 C225 C226 115.9(2) . . ? C230 C225 B200 122.4(2) . . ? C225 C226 H226 118.9 . . ? C227 C226 C225 122.2(2) . . ? C227 C226 H226 118.9 . . ? C226 C227 C228 121.0(2) . . ? C226 C227 C231 119.9(2) . . ? C228 C227 C231 119.1(2) . . ? C227 C228 H228 121.1 . . ? C229 C228 C227 117.8(2) . . ? C229 C228 H228 121.1 . . ? C228 C229 C230 121.1(2) . . ? C228 C229 C232 120.2(2) . . ? C230 C229 C232 118.7(2) . . ? C225 C230 H230 119.0 . . ? C229 C230 C225 122.1(2) . . ? C229 C230 H230 119.0 . . ? F219 C231 F220 105.9(3) . . ? F219 C231 C227 112.6(2) . . ? F220 C231 C227 111.5(2) . . ? F221 C231 F219 106.2(2) . . ? F221 C231 F220 106.8(2) . . ? F221 C231 C227 113.4(2) . . ? F222 C232 F223 106.5(2) . . ? F222 C232 F224 106.6(2) . . ? F222 C232 C229 113.0(2) . . ? F223 C232 C229 112.1(2) . . ? F224 C232 F223 105.6(2) . . ? F224 C232 C229 112.5(2) . . ? C209 B200 C201 105.01(18) . . ? C209 B200 C225 113.67(18) . . ? C217 B200 C201 112.21(19) . . ? C217 B200 C209 113.56(19) . . ? C217 B200 C225 102.29(19) . . ? C225 B200 C201 110.31(18) . . ? F915 C909 C910 118.9(3) . . ? F915 C909 C914 120.1(3) . . ? C914 C909 C910 121.0(3) . . ? F916 C910 C909 118.6(3) . . ? F916 C910 C911 120.5(3) . . ? C911 C910 C909 120.9(3) . . ? C910 C911 H911 120.7 . . ? C910 C911 C912 118.6(3) . . ? C912 C911 H911 120.7 . . ? C911 C912 H912 119.5 . . ? C913 C912 C911 121.0(3) . . ? C913 C912 H912 119.5 . . ? C912 C913 H913 120.0 . . ? C912 C913 C914 120.1(3) . . ? C914 C913 H913 120.0 . . ? C909 C914 C913 118.3(3) . . ? C909 C914 H914 120.8 . . ? C913 C914 H914 120.8 . . ? 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 O9 C4 C5 O12 1.5(6) . . . . ? O9 C4 C5 N6 -176.8(3) . . . . ? O24 C19 C20 O27 4.2(9) . . . . ? O24 C19 C20 N21 -173.1(4) . . . . ? O39 C34 C35 O42 2.2(7) . . . . ? O39 C34 C35 N36 -179.9(3) . . . . ? N3 C4 C5 O12 178.3(3) . . . . ? N3 C4 C5 N6 0.1(3) . . . . ? N3 C7 C8 O9 33.0(3) . . . . ? N6 C10 C11 O12 -31.2(2) . . . . ? N18 C19 C20 O27 178.1(4) . . . . ? N18 C19 C20 N21 0.8(4) . . . . ? N18 C22 C23 O24 31.3(3) . . . . ? N21 C25 C26 O27 28.7(4) . . . . ? N33 C34 C35 O42 -176.9(4) . . . . ? N33 C34 C35 N36 1.0(3) . . . . ? N33 C37 C38 O39 30.4(3) . . . . ? N36 C40 C41 O42 33.2(3) . . . . ? C2 N3 C4 O9 177.3(2) . . . . ? C2 N3 C4 C5 -0.5(3) . . . . ? C2 N3 C7 C8 172.2(3) . . . . ? C2 N3 C7 C13 -72.9(4) . . . . ? C2 N3 C7 C14 53.5(4) . . . . ? C2 N6 C5 O12 -178.4(2) . . . . ? C2 N6 C5 C4 0.4(3) . . . . ? C2 N6 C10 C11 -169.6(3) . . . . ? C2 N6 C10 C15 74.5(4) . . . . ? C2 N6 C10 C16 -50.9(4) . . . . ? C4 O9 C8 C7 -28.5(3) . . . . ? C4 N3 C2 Ir1 -177.61(17) . . . . ? C4 N3 C2 N6 0.7(3) . . . . ? C4 N3 C7 C8 -25.9(2) . . . . ? C4 N3 C7 C13 89.1(2) . . . . ? C4 N3 C7 C14 -144.5(2) . . . . ? C5 O12 C11 C10 28.3(3) . . . . ? C5 N6 C2 Ir1 177.45(18) . . . . ? C5 N6 C2 N3 -0.7(3) . . . . ? C5 N6 C10 C11 23.2(2) . . . . ? C5 N6 C10 C15 -92.7(3) . . . . ? C5 N6 C10 C16 141.9(2) . . . . ? C7 N3 C2 Ir1 -16.4(4) . . . . ? C7 N3 C2 N6 161.9(3) . . . . ? C7 N3 C4 O9 10.6(3) . . . . ? C7 N3 C4 C5 -167.2(2) . . . . ? C8 O9 C4 N3 11.5(3) . . . . ? C8 O9 C4 C5 -171.8(3) . . . . ? C10 N6 C2 Ir1 10.7(4) . . . . ? C10 N6 C2 N3 -167.4(3) . . . . ? C10 N6 C5 O12 -7.5(3) . . . . ? C10 N6 C5 C4 171.2(2) . . . . ? C11 O12 C5 N6 -13.3(3) . . . . ? C11 O12 C5 C4 168.6(3) . . . . ? C13 C7 C8 O9 -80.3(3) . . . . ? C14 C7 C8 O9 153.9(2) . . . . ? C15 C10 C11 O12 82.1(3) . . . . ? C16 C10 C11 O12 -151.5(2) . . . . ? C17 N18 C19 O24 174.2(3) . . . . ? C17 N18 C19 C20 -1.6(4) . . . . ? C17 N18 C22 C23 178.6(3) . . . . ? C17 N18 C22 C28 -67.1(5) . . . . ? C17 N18 C22 C29 59.6(5) . . . . ? C17 N21 C20 O27 -178.0(3) . . . . ? C17 N21 C20 C19 0.2(4) . . . . ? C17 N21 C25 C26 156.7(3) . . . . ? C17 N21 C25 C30 39.4(5) . . . . ? C17 N21 C25 C31 -86.6(4) . . . . ? C19 O24 C23 C22 -26.9(4) . . . . ? C19 N18 C17 Ir1 -173.6(2) . . . . ? C19 N18 C17 N21 1.5(3) . . . . ? C19 N18 C22 C23 -24.6(3) . . . . ? C19 N18 C22 C28 89.7(3) . . . . ? C19 N18 C22 C29 -143.6(3) . . . . ? C20 O27 C26 C25 -32.1(4) . . . . ? C20 N21 C17 Ir1 174.1(2) . . . . ? C20 N21 C17 N18 -1.1(3) . . . . ? C20 N21 C25 C26 -15.2(3) . . . . ? C20 N21 C25 C30 -132.5(3) . . . . ? C20 N21 C25 C31 101.6(3) . . . . ? C22 N18 C17 Ir1 -17.2(5) . . . . ? C22 N18 C17 N21 157.9(3) . . . . ? C22 N18 C19 O24 10.9(4) . . . . ? C22 N18 C19 C20 -164.9(3) . . . . ? C23 O24 C19 N18 10.5(4) . . . . ? C23 O24 C19 C20 -175.7(5) . . . . ? C25 N21 C17 Ir1 2.6(5) . . . . ? C25 N21 C17 N18 -172.6(3) . . . . ? C25 N21 C20 O27 -4.1(4) . . . . ? C25 N21 C20 C19 174.1(3) . . . . ? C26 O27 C20 N21 22.8(4) . . . . ? C26 O27 C20 C19 -154.4(5) . . . . ? C28 C22 C23 O24 -81.7(4) . . . . ? C29 C22 C23 O24 152.6(3) . . . . ? C30 C25 C26 O27 144.5(3) . . . . ? C31 C25 C26 O27 -88.3(4) . . . . ? C32 N33 C34 O39 179.2(2) . . . . ? C32 N33 C34 C35 -1.5(3) . . . . ? C32 N33 C37 C38 164.2(3) . . . . ? C32 N33 C37 C43 -80.7(4) . . . . ? C32 N33 C37 C44 47.6(4) . . . . ? C32 N36 C35 O42 178.2(2) . . . . ? C32 N36 C35 C34 -0.3(3) . . . . ? C32 N36 C40 C41 167.7(3) . . . . ? C32 N36 C40 C45 49.1(4) . . . . ? C32 N36 C40 C46 -77.6(4) . . . . ? C34 O39 C38 C37 -30.9(3) . . . . ? C34 N33 C32 Ir1 -177.42(19) . . . . ? C34 N33 C32 N36 1.2(3) . . . . ? C34 N33 C37 C38 -19.3(3) . . . . ? C34 N33 C37 C43 95.8(3) . . . . ? C34 N33 C37 C44 -135.9(3) . . . . ? C35 O42 C41 C40 -31.0(3) . . . . ? C35 N36 C32 Ir1 178.06(19) . . . . ? C35 N36 C32 N33 -0.6(3) . . . . ? C35 N36 C40 C41 -23.5(3) . . . . ? C35 N36 C40 C45 -142.2(3) . . . . ? C35 N36 C40 C46 91.2(3) . . . . ? C37 N33 C32 Ir1 -1.0(4) . . . . ? C37 N33 C32 N36 177.6(3) . . . . ? C37 N33 C34 O39 1.6(3) . . . . ? C37 N33 C34 C35 -179.0(2) . . . . ? C38 O39 C34 N33 18.5(3) . . . . ? C38 O39 C34 C35 -160.6(4) . . . . ? C40 N36 C32 Ir1 -13.6(5) . . . . ? C40 N36 C32 N33 167.7(3) . . . . ? C40 N36 C35 O42 6.2(3) . . . . ? C40 N36 C35 C34 -172.3(2) . . . . ? C41 O42 C35 N36 15.9(3) . . . . ? C41 O42 C35 C34 -166.3(4) . . . . ? C43 C37 C38 O39 -85.4(3) . . . . ? C44 C37 C38 O39 149.6(2) . . . . ? C45 C40 C41 O42 152.7(3) . . . . ? C46 C40 C41 O42 -82.0(3) . . . . ? O9A C4A C5A O12A 1.1(6) . . . . ? O9A C4A C5A N6A -179.0(3) . . . . ? O24A C19A C20A O27A 2.0(7) . . . . ? O24A C19A C20A N21A -174.8(4) . . . . ? O39A C34A C35A O42A -2.6(7) . . . . ? O39A C34A C35A N36A -179.6(3) . . . . ? N3A C4A C5A O12A 179.5(3) . . . . ? N3A C4A C5A N6A -0.6(3) . . . . ? N3A C7A C8A O9A 32.5(2) . . . . ? N6A C10A C11A O12A 23.9(4) . . . . ? N6A C10A C11B O12A -20.8(6) . . . . ? N18A C19A C20A O27A 176.1(3) . . . . ? N18A C19A C20A N21A -0.6(3) . . . . ? N18A C22A C23A O24A 33.9(3) . . . . ? N21A C25A C26A O27A -12.1(3) . . . . ? N33A C34A C35A O42A 177.0(3) . . . . ? N33A C34A C35A N36A 0.0(3) . . . . ? N33A C37A C38A O39A 30.1(3) . . . . ? N36A C40A C41A O42A -25.2(3) . . . . ? C2A N3A C4A O9A 178.6(2) . . . . ? C2A N3A C4A C5A -0.3(3) . . . . ? C2A N3A C7A C8A 168.4(3) . . . . ? C2A N3A C7A C13A -76.2(4) . . . . ? C2A N3A C7A C14A 50.9(4) . . . . ? C2A N6A C5A O12A -178.7(2) . . . . ? C2A N6A C5A C4A 1.3(3) . . . . ? C2A N6A C10A C11A 163.7(3) . . . . ? C2A N6A C10A C11B -169.0(4) . . . . ? C2A N6A C10A C15A 45.4(5) . . . . ? C2A N6A C10A C15B 74.0(6) . . . . ? C2A N6A C10A C16A -81.0(5) . . . . ? C2A N6A C10A C16B -51.5(6) . . . . ? C4A O9A C8A C7A -29.9(3) . . . . ? C4A N3A C2A Ir1A -172.56(17) . . . . ? C4A N3A C2A N6A 1.0(3) . . . . ? C4A N3A C7A C8A -23.6(2) . . . . ? C4A N3A C7A C13A 91.9(3) . . . . ? C4A N3A C7A C14A -141.0(2) . . . . ? C5A O12A C11A C10A -25.0(4) . . . . ? C5A O12A C11B C10A 21.8(6) . . . . ? C5A N6A C2A Ir1A 171.69(18) . . . . ? C5A N6A C2A N3A -1.4(3) . . . . ? C5A N6A C10A C11A -14.6(3) . . . . ? C5A N6A C10A C11B 12.7(4) . . . . ? C5A N6A C10A C15A -133.0(4) . . . . ? C5A N6A C10A C15B -104.3(5) . . . . ? C5A N6A C10A C16A 100.6(4) . . . . ? C5A N6A C10A C16B 130.1(5) . . . . ? C7A N3A C2A Ir1A -4.9(4) . . . . ? C7A N3A C2A N6A 168.6(3) . . . . ? C7A N3A C4A O9A 7.1(3) . . . . ? C7A N3A C4A C5A -171.8(2) . . . . ? C8A O9A C4A N3A 14.6(3) . . . . ? C8A O9A C4A C5A -167.0(3) . . . . ? C10A N6A C2A Ir1A -6.6(4) . . . . ? C10A N6A C2A N3A -179.7(3) . . . . ? C10A N6A C5A O12A 0.1(3) . . . . ? C10A N6A C5A C4A -179.9(2) . . . . ? C11A O12A C5A N6A 15.9(4) . . . . ? C11A O12A C5A C4A -164.2(4) . . . . ? C11B O12A C5A N6A -14.0(5) . . . . ? C11B O12A C5A C4A 166.0(5) . . . . ? C13A C7A C8A O9A -81.7(3) . . . . ? C14A C7A C8A O9A 153.6(2) . . . . ? C15A C10A C11A O12A 141.5(5) . . . . ? C15B C10A C11B O12A 94.0(7) . . . . ? C16A C10A C11A O12A -90.8(5) . . . . ? C16B C10A C11B O12A -142.4(6) . . . . ? C17A N18A C19A O24A 175.8(2) . . . . ? C17A N18A C19A C20A -0.2(3) . . . . ? C17A N18A C22A C23A 175.0(3) . . . . ? C17A N18A C22A C28A -69.9(4) . . . . ? C17A N18A C22A C29A 55.4(4) . . . . ? C17A N21A C20A O27A -176.4(2) . . . . ? C17A N21A C20A C19A 1.2(3) . . . . ? C17A N21A C25A C26A 179.3(3) . . . . ? C17A N21A C25A C30A 62.0(4) . . . . ? C17A N21A C25A C31A -64.0(4) . . . . ? C19A O24A C23A C22A -28.3(3) . . . . ? C19A N18A C17A Ir1A -175.82(19) . . . . ? C19A N18A C17A N21A 0.9(3) . . . . ? C19A N18A C22A C23A -27.7(3) . . . . ? C19A N18A C22A C28A 87.3(3) . . . . ? C19A N18A C22A C29A -147.3(3) . . . . ? C20A O27A C26A C25A 10.5(3) . . . . ? C20A N21A C17A Ir1A 174.8(2) . . . . ? C20A N21A C17A N18A -1.3(3) . . . . ? C20A N21A C25A C26A 9.5(3) . . . . ? C20A N21A C25A C30A -107.8(3) . . . . ? C20A N21A C25A C31A 126.2(3) . . . . ? C22A N18A C17A Ir1A -19.5(4) . . . . ? C22A N18A C17A N21A 157.2(3) . . . . ? C22A N18A C19A O24A 12.6(3) . . . . ? C22A N18A C19A C20A -163.3(2) . . . . ? C23A O24A C19A N18A 10.1(3) . . . . ? C23A O24A C19A C20A -176.0(4) . . . . ? C25A N21A C17A Ir1A 5.3(5) . . . . ? C25A N21A C17A N18A -170.8(3) . . . . ? C25A N21A C20A O27A -4.0(3) . . . . ? C25A N21A C20A C19A 173.7(2) . . . . ? C26A O27A C20A N21A -4.2(3) . . . . ? C26A O27A C20A C19A 179.2(4) . . . . ? C28A C22A C23A O24A -79.8(3) . . . . ? C29A C22A C23A O24A 153.9(2) . . . . ? C30A C25A C26A O27A 104.2(3) . . . . ? C31A C25A C26A O27A -130.9(3) . . . . ? C32A N33A C34A O39A 179.2(2) . . . . ? C32A N33A C34A C35A -0.5(3) . . . . ? C32A N33A C37A C38A 163.7(3) . . . . ? C32A N33A C37A C43A -81.1(4) . . . . ? C32A N33A C37A C44A 46.0(4) . . . . ? C32A N36A C35A O42A -177.4(2) . . . . ? C32A N36A C35A C34A 0.4(3) . . . . ? C32A N36A C40A C41A -172.3(3) . . . . ? C32A N36A C40A C45A 71.7(4) . . . . ? C32A N36A C40A C46A -55.7(4) . . . . ? C34A O39A C38A C37A -30.7(3) . . . . ? C34A N33A C32A Ir1A -178.95(19) . . . . ? C34A N33A C32A N36A 0.7(3) . . . . ? C34A N33A C37A C38A -18.8(3) . . . . ? C34A N33A C37A C43A 96.4(3) . . . . ? C34A N33A C37A C44A -136.5(3) . . . . ? C35A O42A C41A C40A 23.9(3) . . . . ? C35A N36A C32A Ir1A 178.98(18) . . . . ? C35A N36A C32A N33A -0.7(3) . . . . ? C35A N36A C40A C41A 17.7(3) . . . . ? C35A N36A C40A C45A -98.4(3) . . . . ? C35A N36A C40A C46A 134.2(3) . . . . ? C37A N33A C32A Ir1A -1.6(4) . . . . ? C37A N33A C32A N36A 178.1(3) . . . . ? C37A N33A C34A O39A 1.0(3) . . . . ? C37A N33A C34A C35A -178.7(2) . . . . ? C38A O39A C34A N33A 18.9(3) . . . . ? C38A O39A C34A C35A -161.5(4) . . . . ? C40A N36A C32A Ir1A 9.2(4) . . . . ? C40A N36A C32A N33A -170.4(3) . . . . ? C40A N36A C35A O42A -4.5(3) . . . . ? C40A N36A C35A C34A 173.3(2) . . . . ? C41A O42A C35A N36A -12.4(3) . . . . ? C41A O42A C35A C34A 170.8(4) . . . . ? C43A C37A C38A O39A -84.9(3) . . . . ? C44A C37A C38A O39A 149.5(2) . . . . ? C45A C40A C41A O42A 89.7(3) . . . . ? C46A C40A C41A O42A -146.3(2) . . . . ? F907 C901 C902 F908 0.3(4) . . . . ? F907 C901 C902 C903 -179.9(3) . . . . ? F907 C901 C906 C905 179.4(3) . . . . ? F908 C902 C903 C904 -179.5(3) . . . . ? C901 C902 C903 C904 0.6(5) . . . . ? C902 C901 C906 C905 0.1(4) . . . . ? C902 C903 C904 C905 -0.2(5) . . . . ? C903 C904 C905 C906 -0.2(5) . . . . ? C904 C905 C906 C901 0.2(5) . . . . ? C906 C901 C902 F908 179.6(3) . . . . ? C906 C901 C902 C903 -0.5(4) . . . . ? C401 C402 C403 C404 0.2(4) . . . . ? C401 C402 C403 C407 -179.5(3) . . . . ? C402 C401 C406 C405 -2.2(3) . . . . ? C402 C401 B400 C409 -76.8(3) . . . . ? C402 C401 B400 C417 46.4(3) . . . . ? C402 C401 B400 C425 160.5(2) . . . . ? C402 C403 C404 C405 -0.9(4) . . . . ? C402 C403 C407 F401 -172.9(3) . . . . ? C402 C403 C407 F402 -53.8(4) . . . . ? C402 C403 C407 F403 63.8(4) . . . . ? C403 C404 C405 C406 0.1(4) . . . . ? C403 C404 C405 C408 177.3(2) . . . . ? C404 C403 C407 F401 7.5(4) . . . . ? C404 C403 C407 F402 126.6(3) . . . . ? C404 C403 C407 F403 -115.8(3) . . . . ? C404 C405 C406 C401 1.6(4) . . . . ? C404 C405 C408 F404 -1.8(5) . . . . ? C404 C405 C408 F405 -119.1(4) . . . . ? C404 C405 C408 F406 126.3(4) . . . . ? C404 C405 C408 F504 154.3(6) . . . . ? C404 C405 C408 F505 39.3(6) . . . . ? C404 C405 C408 F506 -74.8(7) . . . . ? C406 C401 C402 C403 1.3(4) . . . . ? C406 C401 B400 C409 99.9(3) . . . . ? C406 C401 B400 C417 -136.9(2) . . . . ? C406 C401 B400 C425 -22.9(3) . . . . ? C406 C405 C408 F404 175.6(4) . . . . ? C406 C405 C408 F405 58.3(5) . . . . ? C406 C405 C408 F406 -56.3(5) . . . . ? C406 C405 C408 F504 -28.4(6) . . . . ? C406 C405 C408 F505 -143.3(6) . . . . ? C406 C405 C408 F506 102.5(7) . . . . ? C407 C403 C404 C405 178.7(3) . . . . ? C408 C405 C406 C401 -175.8(2) . . . . ? C409 C410 C411 C412 -0.2(4) . . . . ? C409 C410 C411 C415 -177.3(2) . . . . ? C410 C409 C414 C413 1.2(3) . . . . ? C410 C409 B400 C401 88.7(3) . . . . ? C410 C409 B400 C417 -32.0(3) . . . . ? C410 C409 B400 C425 -149.4(2) . . . . ? C410 C411 C412 C413 0.9(4) . . . . ? C410 C411 C415 F407 -136.6(2) . . . . ? C410 C411 C415 F408 105.0(3) . . . . ? C410 C411 C415 F409 -15.2(3) . . . . ? C411 C412 C413 C414 -0.5(4) . . . . ? C411 C412 C413 C416 -177.6(2) . . . . ? C412 C411 C415 F407 46.2(3) . . . . ? C412 C411 C415 F408 -72.2(3) . . . . ? C412 C411 C415 F409 167.6(2) . . . . ? C412 C413 C414 C409 -0.5(4) . . . . ? C412 C413 C416 F410 -24.3(4) . . . . ? C412 C413 C416 F411 94.6(3) . . . . ? C412 C413 C416 F412 -146.8(3) . . . . ? C414 C409 C410 C411 -0.8(3) . . . . ? C414 C409 B400 C401 -85.4(3) . . . . ? C414 C409 B400 C417 153.9(2) . . . . ? C414 C409 B400 C425 36.6(3) . . . . ? C414 C413 C416 F410 158.7(2) . . . . ? C414 C413 C416 F411 -82.4(3) . . . . ? C414 C413 C416 F412 36.1(3) . . . . ? C415 C411 C412 C413 178.1(2) . . . . ? C416 C413 C414 C409 176.5(2) . . . . ? C417 C418 C419 C420 0.4(4) . . . . ? C417 C418 C419 C423 179.8(3) . . . . ? C418 C417 C422 C421 -0.7(4) . . . . ? C418 C417 B400 C401 -154.2(2) . . . . ? C418 C417 B400 C409 -36.4(3) . . . . ? C418 C417 B400 C425 86.4(3) . . . . ? C418 C419 C420 C421 0.2(4) . . . . ? C418 C419 C423 F413 175.6(3) . . . . ? C418 C419 C423 F414 55.5(4) . . . . ? C418 C419 C423 F415 -62.4(4) . . . . ? C419 C420 C421 C422 -1.0(4) . . . . ? C419 C420 C421 C424 179.4(3) . . . . ? C420 C419 C423 F413 -5.0(4) . . . . ? C420 C419 C423 F414 -125.1(3) . . . . ? C420 C419 C423 F415 117.0(3) . . . . ? C420 C421 C422 C417 1.3(4) . . . . ? C420 C421 C424 F416 -36.5(4) . . . . ? C420 C421 C424 F417 80.7(4) . . . . ? C420 C421 C424 F418 -158.4(3) . . . . ? C420 C421 C424 F516 142.3(9) . . . . ? C420 C421 C424 F517 -100.3(10) . . . . ? C420 C421 C424 F518 21.0(10) . . . . ? C422 C417 C418 C419 -0.2(4) . . . . ? C422 C417 B400 C401 34.9(3) . . . . ? C422 C417 B400 C409 152.7(2) . . . . ? C422 C417 B400 C425 -84.4(3) . . . . ? C422 C421 C424 F416 144.0(3) . . . . ? C422 C421 C424 F417 -98.9(4) . . . . ? C422 C421 C424 F418 22.0(4) . . . . ? C422 C421 C424 F516 -37.2(10) . . . . ? C422 C421 C424 F517 80.2(10) . . . . ? C422 C421 C424 F518 -158.5(10) . . . . ? C423 C419 C420 C421 -179.2(3) . . . . ? C424 C421 C422 C417 -179.2(2) . . . . ? C425 C426 C427 C428 -0.7(4) . . . . ? C425 C426 C427 C431 -179.8(2) . . . . ? C426 C425 C430 C429 -2.0(4) . . . . ? C426 C425 B400 C401 144.5(2) . . . . ? C426 C425 B400 C409 26.3(3) . . . . ? C426 C425 B400 C417 -97.3(3) . . . . ? C426 C427 C428 C429 -0.8(4) . . . . ? C426 C427 C431 F419 105.3(3) . . . . ? C426 C427 C431 F420 -134.0(3) . . . . ? C426 C427 C431 F421 -15.6(4) . . . . ? C427 C428 C429 C430 0.8(4) . . . . ? C427 C428 C429 C432 177.4(2) . . . . ? C428 C427 C431 F419 -73.9(4) . . . . ? C428 C427 C431 F420 46.8(4) . . . . ? C428 C427 C431 F421 165.2(3) . . . . ? C428 C429 C430 C425 0.7(4) . . . . ? C428 C429 C432 F422 23.9(6) . . . . ? C428 C429 C432 F423 -96.8(6) . . . . ? C428 C429 C432 F424 144.7(5) . . . . ? C428 C429 C432 F522 178.1(7) . . . . ? C428 C429 C432 F523 56.1(7) . . . . ? C428 C429 C432 F524 -60.5(8) . . . . ? C430 C425 C426 C427 2.0(4) . . . . ? C430 C425 B400 C401 -40.9(3) . . . . ? C430 C425 B400 C409 -159.1(2) . . . . ? C430 C425 B400 C417 77.3(3) . . . . ? C430 C429 C432 F422 -159.4(5) . . . . ? C430 C429 C432 F423 79.9(6) . . . . ? C430 C429 C432 F424 -38.6(6) . . . . ? C430 C429 C432 F522 -5.2(8) . . . . ? C430 C429 C432 F523 -127.2(7) . . . . ? C430 C429 C432 F524 116.2(8) . . . . ? C431 C427 C428 C429 178.4(2) . . . . ? C432 C429 C430 C425 -176.0(2) . . . . ? B400 C401 C402 C403 178.2(2) . . . . ? B400 C401 C406 C405 -179.0(2) . . . . ? B400 C409 C410 C411 -175.1(2) . . . . ? B400 C409 C414 C413 175.7(2) . . . . ? B400 C417 C418 C419 -171.5(2) . . . . ? B400 C417 C422 C421 170.8(2) . . . . ? B400 C425 C426 C427 176.8(2) . . . . ? B400 C425 C430 C429 -177.1(2) . . . . ? C201 C202 C203 C204 -1.7(4) . . . . ? C201 C202 C203 C207 175.3(2) . . . . ? C202 C201 C206 C205 -1.3(3) . . . . ? C202 C201 B200 C209 -102.0(2) . . . . ? C202 C201 B200 C217 21.8(3) . . . . ? C202 C201 B200 C225 135.1(2) . . . . ? C202 C203 C204 C205 0.1(4) . . . . ? C202 C203 C207 F201 145.3(4) . . . . ? C202 C203 C207 F202 26.0(5) . . . . ? C202 C203 C207 F203 -98.4(4) . . . . ? C202 C203 C207 F301 -60.8(4) . . . . ? C202 C203 C207 F302 -179.5(3) . . . . ? C202 C203 C207 F303 55.2(4) . . . . ? C203 C204 C205 C206 0.9(4) . . . . ? C203 C204 C205 C208 -177.2(2) . . . . ? C204 C203 C207 F201 -37.6(4) . . . . ? C204 C203 C207 F202 -156.9(4) . . . . ? C204 C203 C207 F203 78.7(4) . . . . ? C204 C203 C207 F301 116.3(4) . . . . ? C204 C203 C207 F302 -2.4(4) . . . . ? C204 C203 C207 F303 -127.6(4) . . . . ? C204 C205 C206 C201 -0.2(4) . . . . ? C204 C205 C208 F204 -18.9(4) . . . . ? C204 C205 C208 F205 -139.2(3) . . . . ? C204 C205 C208 F206 101.9(3) . . . . ? C206 C201 C202 C203 2.3(3) . . . . ? C206 C201 B200 C209 74.3(3) . . . . ? C206 C201 B200 C217 -161.9(2) . . . . ? C206 C201 B200 C225 -48.5(3) . . . . ? C206 C205 C208 F204 163.0(2) . . . . ? C206 C205 C208 F205 42.7(3) . . . . ? C206 C205 C208 F206 -76.2(3) . . . . ? C207 C203 C204 C205 -177.0(2) . . . . ? C208 C205 C206 C201 177.8(2) . . . . ? C209 C210 C211 C212 0.4(4) . . . . ? C209 C210 C211 C215 -177.9(2) . . . . ? C210 C209 C214 C213 0.3(3) . . . . ? C210 C209 B200 C201 86.1(3) . . . . ? C210 C209 B200 C217 -36.8(3) . . . . ? C210 C209 B200 C225 -153.2(2) . . . . ? C210 C211 C212 C213 0.3(4) . . . . ? C210 C211 C215 F207 -162.4(2) . . . . ? C210 C211 C215 F208 79.8(3) . . . . ? C210 C211 C215 F209 -39.8(4) . . . . ? C211 C212 C213 C214 -0.7(4) . . . . ? C211 C212 C213 C216 -177.7(2) . . . . ? C212 C211 C215 F207 19.2(4) . . . . ? C212 C211 C215 F208 -98.5(3) . . . . ? C212 C211 C215 F209 141.8(3) . . . . ? C212 C213 C214 C209 0.3(4) . . . . ? C212 C213 C216 F210 -43.8(3) . . . . ? C212 C213 C216 F211 74.9(3) . . . . ? C212 C213 C216 F212 -165.3(2) . . . . ? C214 C209 C210 C211 -0.7(3) . . . . ? C214 C209 B200 C201 -87.2(3) . . . . ? C214 C209 B200 C217 149.9(2) . . . . ? C214 C209 B200 C225 33.5(3) . . . . ? C214 C213 C216 F210 139.2(2) . . . . ? C214 C213 C216 F211 -102.1(3) . . . . ? C214 C213 C216 F212 17.7(3) . . . . ? C215 C211 C212 C213 178.6(2) . . . . ? C216 C213 C214 C209 177.3(2) . . . . ? C217 C218 C219 C220 -2.1(4) . . . . ? C217 C218 C219 C223 175.2(2) . . . . ? C218 C217 C222 C221 -1.0(4) . . . . ? C218 C217 B200 C201 40.9(3) . . . . ? C218 C217 B200 C209 159.7(2) . . . . ? C218 C217 B200 C225 -77.4(2) . . . . ? C218 C219 C220 C221 0.2(4) . . . . ? C218 C219 C223 F213 129.4(3) . . . . ? C218 C219 C223 F214 -112.0(3) . . . . ? C218 C219 C223 F215 9.3(4) . . . . ? C219 C220 C221 C222 1.1(4) . . . . ? C219 C220 C221 C224 178.7(2) . . . . ? C220 C219 C223 F213 -53.3(3) . . . . ? C220 C219 C223 F214 65.3(3) . . . . ? C220 C219 C223 F215 -173.4(2) . . . . ? C220 C221 C222 C217 -0.7(4) . . . . ? C220 C221 C224 F216 -177.5(3) . . . . ? C220 C221 C224 F217 56.5(5) . . . . ? C220 C221 C224 F218 -64.8(4) . . . . ? C220 C221 C224 F316 32.3(4) . . . . ? C220 C221 C224 F317 -85.5(4) . . . . ? C220 C221 C224 F318 146.1(4) . . . . ? C222 C217 C218 C219 2.4(4) . . . . ? C222 C217 B200 C201 -147.1(2) . . . . ? C222 C217 B200 C209 -28.2(3) . . . . ? C222 C217 B200 C225 94.7(2) . . . . ? C222 C221 C224 F216 0.1(4) . . . . ? C222 C221 C224 F217 -125.9(4) . . . . ? C222 C221 C224 F218 112.8(4) . . . . ? C222 C221 C224 F316 -150.0(3) . . . . ? C222 C221 C224 F317 92.1(4) . . . . ? C222 C221 C224 F318 -36.3(4) . . . . ? C223 C219 C220 C221 -177.0(2) . . . . ? C224 C221 C222 C217 -178.3(2) . . . . ? C225 C226 C227 C228 -1.1(4) . . . . ? C225 C226 C227 C231 180.0(2) . . . . ? C226 C225 C230 C229 -0.2(4) . . . . ? C226 C225 B200 C201 -35.1(3) . . . . ? C226 C225 B200 C209 -152.7(2) . . . . ? C226 C225 B200 C217 84.4(2) . . . . ? C226 C227 C228 C229 0.4(4) . . . . ? C226 C227 C231 F219 -142.4(3) . . . . ? C226 C227 C231 F220 98.7(3) . . . . ? C226 C227 C231 F221 -21.9(4) . . . . ? C227 C228 C229 C230 0.4(4) . . . . ? C227 C228 C229 C232 -179.7(3) . . . . ? C228 C227 C231 F219 38.6(4) . . . . ? C228 C227 C231 F220 -80.2(3) . . . . ? C228 C227 C231 F221 159.2(3) . . . . ? C228 C229 C230 C225 -0.5(4) . . . . ? C228 C229 C232 F222 -11.0(4) . . . . ? C228 C229 C232 F223 109.4(3) . . . . ? C228 C229 C232 F224 -131.8(3) . . . . ? C230 C225 C226 C227 1.0(4) . . . . ? C230 C225 B200 C201 156.0(2) . . . . ? C230 C225 B200 C209 38.3(3) . . . . ? C230 C225 B200 C217 -84.5(3) . . . . ? C230 C229 C232 F222 168.9(3) . . . . ? C230 C229 C232 F223 -70.7(3) . . . . ? C230 C229 C232 F224 48.1(4) . . . . ? C231 C227 C228 C229 179.3(2) . . . . ? C232 C229 C230 C225 179.5(2) . . . . ? B200 C201 C202 C203 178.8(2) . . . . ? B200 C201 C206 C205 -178.0(2) . . . . ? B200 C209 C210 C211 -174.4(2) . . . . ? B200 C209 C214 C213 174.0(2) . . . . ? B200 C217 C218 C219 175.1(2) . . . . ? B200 C217 C222 C221 -173.4(2) . . . . ? B200 C225 C226 C227 -168.6(2) . . . . ? B200 C225 C230 C229 169.3(2) . . . . ? F915 C909 C910 F916 0.2(4) . . . . ? F915 C909 C910 C911 -179.6(3) . . . . ? F915 C909 C914 C913 178.9(3) . . . . ? F916 C910 C911 C912 -178.8(3) . . . . ? C909 C910 C911 C912 0.9(5) . . . . ? C910 C909 C914 C913 0.2(4) . . . . ? C910 C911 C912 C913 -0.3(5) . . . . ? C911 C912 C913 C914 -0.3(5) . . . . ? C912 C913 C914 C909 0.4(5) . . . . ? C914 C909 C910 F916 178.9(3) . . . . ? C914 C909 C910 C911 -0.9(4) . . . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_0070abc14 #==================================================================== # [Ir(IBioxMe4)2(C2H4)2][BArF4] #-------------------------------------------------------------------- # Collected and solved by Adrian Chaplin #-------------------------------------------------------------------- # Start Validation Reply Form _vrf_PLAT301_0070abc14 ; PROBLEM: Main Residue Disorder ............ Percentage = 3 Note RESPONSE: The structure contains a significant degree of disorder. See _publ_section_exptl_refinement. ; # End Validation Reply Form #-------------------------------------------------------------------- _publ_contact_author_name 'Adrian B. Chaplin' _publ_contact_author_email a.b.chaplin@warwick.ac.uk _publ_section_exptl_refinement ; Solved with SHELXT-2014 by direct methods. Refined full-matrix least squares on F2 using SHELXL-2014. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions and refined using the riding model. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; #==================================================================== _audit_creation_date 2015-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C26 H40 Ir N4 O4, C32 H12 B F24' _chemical_formula_sum 'C58 H52 B F24 Ir N4 O4' _chemical_formula_weight 1528.04 _chemical_absolute_configuration . _chemical_melting_point 'not measured' 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_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 17.9906(2) _cell_length_b 18.4566(3) _cell_length_c 19.5861(2) _cell_angle_alpha 90 _cell_angle_beta 112.3623(14) _cell_angle_gamma 90 _cell_volume 6014.37(14) _cell_formula_units_Z 4 _cell_measurement_reflns_used 26864 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 34.1750 _cell_measurement_theta_min 3.2980 _shelx_estimated_absorpt_T_max . _shelx_estimated_absorpt_T_min . _exptl_absorpt_coefficient_mu 2.344 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70722 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details . _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method . _exptl_crystal_description block _exptl_crystal_F_000 3032 _exptl_crystal_recrystallization_method 'Crystals grown from C6H4F2-heptane at 293 K' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_special_details . _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 62393 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 27.103 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 3.055 _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.2833 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 39.00 87.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 178.0000 120.0000 48 #__ type_ start__ end____ width___ exp.time_ 2 omega 39.00 88.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 178.0000 30.0000 49 #__ type_ start__ end____ width___ exp.time_ 3 omega -38.00 5.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -57.0000 -180.0000 43 #__ type_ start__ end____ width___ exp.time_ 4 omega -61.00 9.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -77.0000 150.0000 70 #__ type_ start__ end____ width___ exp.time_ 5 omega -86.00 -60.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -38.0000 0.0000 26 #__ type_ start__ end____ width___ exp.time_ 6 omega -101.00 -45.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -77.0000 90.0000 56 #__ type_ start__ end____ width___ exp.time_ 7 omega -95.00 -55.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -57.0000 -180.0000 40 #__ type_ start__ end____ width___ exp.time_ 8 omega -114.00 -64.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -178.0000 -30.0000 50 #__ type_ start__ end____ width___ exp.time_ 9 omega -51.00 51.00 1.0000 4.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 38.0000 -180.0000 102 ; _diffrn_measurement_device_type 'Oxford Diffraction: Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0211573000 _diffrn_orient_matrix_UB_12 -0.0054645000 _diffrn_orient_matrix_UB_13 -0.0384087000 _diffrn_orient_matrix_UB_21 0.0250815000 _diffrn_orient_matrix_UB_22 0.0257748000 _diffrn_orient_matrix_UB_23 -0.0076131000 _diffrn_orient_matrix_UB_31 0.0272073000 _diffrn_orient_matrix_UB_32 -0.0279884000 _diffrn_orient_matrix_UB_33 0.0004992000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11596 _reflns_number_total 13246 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.092 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.083 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 865 _refine_ls_number_reflns 13246 _refine_ls_number_restraints 246 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0306 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+9.1737P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.0719 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim C208-F6A with sigma of 0.01 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A with sigma of 0.01 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim C205-F6A with sigma of 0.01 C223-F13 \\sim C223-F14 \\sim C223-F15 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints F1 \\sim F2 \\sim F3 \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq: with sigma of 0.007 and sigma for terminal atoms of 0.02 4. Others Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1) Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C12(H12A,H12B), C15(H15A, H15B), C27(H27A,H27B), C30(H30A,H30B) 5.b Aromatic/amide H refined with riding coordinates: C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230) 5.c Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B, H20C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A, H35B,H35C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 1.00236(2) 0.00476(2) 0.23980(2) 0.01991(4) Uani 1 1 d . . . . . O13 O 0.88207(14) -0.02675(13) 0.44946(12) 0.0358(5) Uani 1 1 d . . . . . O16 O 0.97773(16) -0.18427(12) 0.44423(13) 0.0400(6) Uani 1 1 d . . . . . O28 O 0.99702(13) 0.20097(13) 0.03146(14) 0.0395(6) Uani 1 1 d . . . . . O31 O 1.12629(13) 0.06581(13) 0.03519(13) 0.0380(6) Uani 1 1 d . . . . . N7 N 0.92853(14) -0.01440(13) 0.35635(13) 0.0237(5) Uani 1 1 d . . . . . N10 N 0.98744(15) -0.11253(13) 0.35231(13) 0.0249(5) Uani 1 1 d . . . . . N22 N 0.99216(14) 0.11965(13) 0.11842(14) 0.0254(5) Uani 1 1 d . . . . . N25 N 1.07270(14) 0.03537(13) 0.12065(13) 0.0245(5) Uani 1 1 d . . . . . C2 C 0.88308(19) -0.02913(19) 0.16667(18) 0.0343(7) Uani 1 1 d . . . . . H2A H 0.8491 -0.0521 0.1902 0.041 Uiso 1 1 calc R . . . . H2B H 0.8532 0.0045 0.1261 0.041 Uiso 1 1 calc R . . . . C3 C 0.9400(2) -0.07302(18) 0.15546(18) 0.0352(7) Uani 1 1 d . . . . . H3A H 0.9461 -0.0675 0.1076 0.042 Uiso 1 1 calc R . . . . H3B H 0.9419 -0.1241 0.1716 0.042 Uiso 1 1 calc R . . . . C4 C 1.10722(19) 0.0220(2) 0.34362(19) 0.0371(8) Uani 1 1 d . . . . . H4A H 1.0955 0.0309 0.3884 0.044 Uiso 1 1 calc R . . . . H4B H 1.1538 -0.0104 0.3525 0.044 Uiso 1 1 calc R . . . . C5 C 1.10153(19) 0.08060(18) 0.29919(17) 0.0337(7) Uani 1 1 d . . . . . H5A H 1.1443 0.0858 0.2793 0.040 Uiso 1 1 calc R . . . . H5B H 1.0859 0.1271 0.3152 0.040 Uiso 1 1 calc R . . . . C6 C 0.97013(16) -0.04618(16) 0.31869(16) 0.0231(6) Uani 1 1 d . . . . . C8 C 0.92205(18) -0.05812(17) 0.41099(16) 0.0270(6) Uani 1 1 d . . . . . C9 C 0.95851(19) -0.12020(17) 0.40835(17) 0.0292(7) Uani 1 1 d . . . . . C11 C 0.88628(18) 0.05517(17) 0.35483(17) 0.0276(6) Uani 1 1 d . . . . . C12 C 0.8773(3) 0.0489(2) 0.4302(2) 0.0461(9) Uani 1 1 d . . . . . H12A H 0.9207 0.0763 0.4684 0.055 Uiso 1 1 calc R . . . . H12B H 0.8250 0.0692 0.4266 0.055 Uiso 1 1 calc R . . . . C14 C 1.02801(19) -0.18188(16) 0.34735(17) 0.0301(7) Uani 1 1 d . . . . . C15 C 1.0446(2) -0.2109(2) 0.4260(2) 0.0448(9) Uani 1 1 d . . . . . H15A H 1.0461 -0.2645 0.4267 0.054 Uiso 1 1 calc R . . . . H15B H 1.0964 -0.1923 0.4616 0.054 Uiso 1 1 calc R . . . . C17 C 0.8041(2) 0.0544(2) 0.2919(2) 0.0479(10) Uani 1 1 d . . . . . H17A H 0.8109 0.0565 0.2446 0.072 Uiso 1 1 calc GR . . . . H17B H 0.7729 0.0964 0.2963 0.072 Uiso 1 1 calc GR . . . . H17C H 0.7756 0.0098 0.2942 0.072 Uiso 1 1 calc GR . . . . C18 C 0.9352(2) 0.1207(2) 0.3536(3) 0.0523(11) Uani 1 1 d . . . . . H18A H 0.9876 0.1181 0.3947 0.078 Uiso 1 1 calc GR . . . . H18B H 0.9069 0.1645 0.3585 0.078 Uiso 1 1 calc GR . . . . H18C H 0.9431 0.1223 0.3068 0.078 Uiso 1 1 calc GR . . . . C19 C 0.9704(2) -0.2326(2) 0.2913(2) 0.0465(9) Uani 1 1 d . . . . . H19A H 0.9233 -0.2409 0.3038 0.070 Uiso 1 1 calc GR . . . . H19B H 0.9973 -0.2789 0.2917 0.070 Uiso 1 1 calc GR . . . . H19C H 0.9533 -0.2110 0.2420 0.070 Uiso 1 1 calc GR . . . . C20 C 1.1063(2) -0.1711(2) 0.3366(2) 0.0485(10) Uani 1 1 d . . . . . H20A H 1.0956 -0.1465 0.2894 0.073 Uiso 1 1 calc GR . . . . H20B H 1.1311 -0.2183 0.3363 0.073 Uiso 1 1 calc GR . . . . H20C H 1.1427 -0.1414 0.3770 0.073 Uiso 1 1 calc GR . . . . C21 C 1.02283(16) 0.05666(15) 0.15516(15) 0.0224(6) Uani 1 1 d . . . . . C23 C 1.02395(18) 0.13758(18) 0.06621(17) 0.0303(7) Uani 1 1 d . . . . . C24 C 1.07444(17) 0.08445(18) 0.06745(17) 0.0287(7) Uani 1 1 d . . . . . C26 C 0.93877(18) 0.18017(16) 0.12241(18) 0.0289(7) Uani 1 1 d . . . . . C27 C 0.9283(2) 0.2188(2) 0.0494(2) 0.0538(11) Uani 1 1 d . . . . . H27A H 0.8781 0.2025 0.0095 0.065 Uiso 1 1 calc R . . . . H27B H 0.9251 0.2719 0.0552 0.065 Uiso 1 1 calc R . . . . C29 C 1.13827(18) -0.01851(18) 0.13141(18) 0.0305(7) Uani 1 1 d . . . . . C30 C 1.1449(2) -0.00940(19) 0.0558(2) 0.0377(8) Uani 1 1 d . . . . . H30A H 1.1999 -0.0213 0.0593 0.045 Uiso 1 1 calc R . . . . H30B H 1.1064 -0.0417 0.0187 0.045 Uiso 1 1 calc R . . . . C32 C 0.8576(2) 0.1553(2) 0.1199(2) 0.0466(9) Uani 1 1 d . . . . . H32A H 0.8317 0.1252 0.0760 0.070 Uiso 1 1 calc GR . . . . H32B H 0.8239 0.1977 0.1176 0.070 Uiso 1 1 calc GR . . . . H32C H 0.8648 0.1271 0.1643 0.070 Uiso 1 1 calc GR . . . . C33 C 0.9811(2) 0.2275(2) 0.1884(2) 0.0538(11) Uani 1 1 d . . . . . H33A H 0.9829 0.2028 0.2333 0.081 Uiso 1 1 calc GR . . . . H33B H 0.9519 0.2733 0.1830 0.081 Uiso 1 1 calc GR . . . . H33C H 1.0360 0.2372 0.1919 0.081 Uiso 1 1 calc GR . . . . C34 C 1.1170(2) -0.09544(19) 0.1433(2) 0.0426(8) Uani 1 1 d . . . . . H34A H 1.1065 -0.0980 0.1888 0.064 Uiso 1 1 calc GR . . . . H34B H 1.1618 -0.1276 0.1474 0.064 Uiso 1 1 calc GR . . . . H34C H 1.0688 -0.1105 0.1014 0.064 Uiso 1 1 calc GR . . . . C35 C 1.2150(2) 0.0070(2) 0.1935(2) 0.0401(8) Uani 1 1 d . . . . . H35A H 1.2250 0.0579 0.1855 0.060 Uiso 1 1 calc GR . . . . H35B H 1.2604 -0.0227 0.1939 0.060 Uiso 1 1 calc GR . . . . H35C H 1.2090 0.0021 0.2409 0.060 Uiso 1 1 calc GR . . . . F1 F 1.11353(13) 0.26736(12) 0.39838(12) 0.0495(6) Uani 1 1 d . U . . . F2 F 1.20117(12) 0.22797(10) 0.35834(11) 0.0428(5) Uani 1 1 d . U . . . F3 F 1.22822(13) 0.31906(12) 0.43162(11) 0.0509(6) Uani 1 1 d . U . . . F4 F 1.1865(2) 0.30757(17) 0.12376(18) 0.0801(12) Uani 0.895(4) 1 d D U P A 1 F4A F 1.1327(14) 0.4288(8) 0.0830(9) 0.065(5) Uani 0.105(4) 1 d D U P A 2 F5 F 1.09135(15) 0.3764(2) 0.06252(12) 0.0682(11) Uani 0.895(4) 1 d D U P A 1 F5A F 1.2301(5) 0.3625(14) 0.1451(7) 0.066(5) Uani 0.105(4) 1 d D U P A 2 F6 F 1.2048(2) 0.4205(2) 0.12602(18) 0.0818(13) Uani 0.895(4) 1 d D U P A 1 F6A F 1.1181(13) 0.3156(9) 0.0832(9) 0.078(6) Uani 0.105(4) 1 d D U P A 2 F7 F 0.74720(15) 0.24416(11) 0.23776(13) 0.0569(6) Uani 1 1 d . U . . . F8 F 0.83438(13) 0.29206(11) 0.33423(12) 0.0465(5) Uani 1 1 d . U . . . F9 F 0.71859(13) 0.33968(12) 0.28500(14) 0.0523(6) Uani 1 1 d . U . . . F10 F 0.68710(13) 0.35565(12) -0.00552(11) 0.0501(6) Uani 1 1 d . U . . . F11 F 0.80563(15) 0.35289(17) -0.00628(12) 0.0776(9) Uani 1 1 d . U . . . F12 F 0.74661(12) 0.45423(12) -0.01134(10) 0.0467(5) Uani 1 1 d . U . . . F13 F 1.16835(13) 0.57505(17) 0.57530(12) 0.0686(8) Uani 1 1 d D U . . . F14 F 1.18075(16) 0.65825(14) 0.50799(19) 0.0923(11) Uani 1 1 d D U . . . F15 F 1.21787(11) 0.55026(15) 0.49630(12) 0.0596(7) Uani 1 1 d D U . . . F16 F 0.85891(16) 0.68339(13) 0.42358(17) 0.0707(8) Uani 1 1 d . U . . . F17 F 0.87204(14) 0.59664(14) 0.49740(12) 0.0546(6) Uani 1 1 d . U . . . F18 F 0.79830(12) 0.58364(17) 0.38531(14) 0.0738(9) Uani 1 1 d . U . . . F19 F 1.17896(14) 0.63306(13) 0.16052(18) 0.0695(8) Uani 1 1 d . U . . . F20 F 1.16877(16) 0.72256(18) 0.22259(15) 0.0854(10) Uani 1 1 d . U . . . F21 F 1.12447(13) 0.72961(13) 0.10630(14) 0.0592(7) Uani 1 1 d . U . . . F22 F 0.83789(15) 0.76250(15) 0.03926(19) 0.0889(11) Uani 1 1 d . U . . . F23 F 0.78720(16) 0.71717(18) 0.11297(14) 0.0852(10) Uani 1 1 d . U . . . F24 F 0.78190(14) 0.66149(15) 0.01900(13) 0.0667(7) Uani 1 1 d . U . . . C201 C 1.04952(15) 0.43981(14) 0.25087(14) 0.0187(5) Uani 1 1 d . . . . . C202 C 1.08309(16) 0.39176(15) 0.30952(15) 0.0196(5) Uani 1 1 d . . . . . H202 H 1.0683 0.3956 0.3510 0.024 Uiso 1 1 calc R . . . . C203 C 1.13760(16) 0.33840(15) 0.30930(15) 0.0214(6) Uani 1 1 d . . . . . C204 C 1.16145(16) 0.33113(16) 0.25036(16) 0.0248(6) Uani 1 1 d . . . . . H204 H 1.1995 0.2954 0.2506 0.030 Uiso 1 1 calc R . . . . C205 C 1.12824(16) 0.37749(15) 0.19107(16) 0.0242(6) Uani 1 1 d D . . . . C206 C 1.07312(16) 0.43024(15) 0.19127(15) 0.0222(6) Uani 1 1 d . . . . . H206 H 1.0507 0.4608 0.1494 0.027 Uiso 1 1 calc R . . . . C207 C 1.17000(18) 0.28815(17) 0.37397(17) 0.0299(7) Uani 1 1 d . . . . . C208 C 1.15225(18) 0.37103(17) 0.12607(18) 0.0346(7) Uani 1 1 d D . . . . C209 C 0.89690(15) 0.44740(15) 0.21195(15) 0.0193(5) Uani 1 1 d . . . . . C210 C 0.86833(16) 0.40232(15) 0.25393(15) 0.0209(5) Uani 1 1 d . . . . . H210 H 0.8927 0.4047 0.3063 0.025 Uiso 1 1 calc R . . . . C211 C 0.80521(17) 0.35393(15) 0.22134(17) 0.0241(6) Uani 1 1 d . . . . . C212 C 0.76707(17) 0.34947(16) 0.14550(17) 0.0270(6) Uani 1 1 d . . . . . H212 H 0.7235 0.3171 0.1234 0.032 Uiso 1 1 calc R . . . . C213 C 0.79414(17) 0.39345(16) 0.10276(16) 0.0259(6) Uani 1 1 d . . . . . C214 C 0.85791(16) 0.44071(15) 0.13525(15) 0.0228(6) Uani 1 1 d . . . . . H214 H 0.8758 0.4696 0.1043 0.027 Uiso 1 1 calc R . . . . C215 C 0.77659(19) 0.30757(17) 0.26886(19) 0.0323(7) Uani 1 1 d . . . . . C216 C 0.7577(2) 0.3891(2) 0.01980(18) 0.0376(8) Uani 1 1 d . . . . . C217 C 0.99114(16) 0.52863(14) 0.32980(15) 0.0183(5) Uani 1 1 d . . . . . C218 C 1.06765(16) 0.54254(15) 0.38327(15) 0.0214(6) Uani 1 1 d . . . . . H218 H 1.1136 0.5293 0.3733 0.026 Uiso 1 1 calc R . . . . C219 C 1.07870(16) 0.57512(16) 0.45038(16) 0.0247(6) Uani 1 1 d . . . . . C220 C 1.01398(17) 0.59660(16) 0.46692(16) 0.0245(6) Uani 1 1 d . . . . . H220 H 1.0215 0.6184 0.5130 0.029 Uiso 1 1 calc R . . . . C221 C 0.93761(16) 0.58530(15) 0.41403(15) 0.0217(6) Uani 1 1 d . . . . . C222 C 0.92659(16) 0.55185(15) 0.34756(15) 0.0208(5) Uani 1 1 d . . . . . H222 H 0.8734 0.5444 0.3128 0.025 Uiso 1 1 calc R . . . . C223 C 1.16178(19) 0.59012(17) 0.50622(18) 0.0384(8) Uani 1 1 d D . . . . C224 C 0.86715(19) 0.61199(18) 0.42978(17) 0.0308(7) Uani 1 1 d . . . . . C225 C 0.97733(16) 0.56789(15) 0.19873(14) 0.0190(5) Uani 1 1 d . . . . . C226 C 1.04848(16) 0.59781(15) 0.19878(15) 0.0218(6) Uani 1 1 d . . . . . H226 H 1.0980 0.5755 0.2280 0.026 Uiso 1 1 calc R . . . . C227 C 1.05006(18) 0.65878(16) 0.15786(16) 0.0243(6) Uani 1 1 d . . . . . C228 C 0.97942(18) 0.69398(16) 0.11547(16) 0.0265(6) Uani 1 1 d . . . . . H228 H 0.9800 0.7352 0.0866 0.032 Uiso 1 1 calc R . . . . C229 C 0.90827(18) 0.66724(16) 0.11660(15) 0.0250(6) Uani 1 1 d . . . . . C230 C 0.90716(17) 0.60587(15) 0.15731(15) 0.0219(6) Uani 1 1 d . . . . . H230 H 0.8571 0.5891 0.1571 0.026 Uiso 1 1 calc R . . . . C231 C 1.12946(19) 0.68575(17) 0.16104(18) 0.0317(7) Uani 1 1 d . . . . . C232 C 0.8300(2) 0.70367(19) 0.07338(18) 0.0347(7) Uani 1 1 d . . . . . B200 B 0.97810(18) 0.49636(17) 0.24815(17) 0.0183(6) 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 0.01724(6) 0.02054(6) 0.01992(6) 0.00121(4) 0.00478(4) -0.00324(4) O13 0.0420(13) 0.0400(14) 0.0318(12) -0.0005(10) 0.0211(11) 0.0011(11) O16 0.0592(16) 0.0289(13) 0.0373(13) 0.0102(10) 0.0244(12) 0.0025(11) O28 0.0308(12) 0.0411(14) 0.0478(14) 0.0250(11) 0.0163(11) 0.0065(10) O31 0.0315(12) 0.0503(15) 0.0393(13) 0.0141(11) 0.0216(11) 0.0041(10) N7 0.0211(12) 0.0253(13) 0.0228(12) 0.0019(9) 0.0064(10) 0.0003(9) N10 0.0296(13) 0.0224(13) 0.0232(12) 0.0014(9) 0.0107(10) -0.0018(10) N22 0.0187(12) 0.0286(14) 0.0290(13) 0.0071(10) 0.0092(10) -0.0003(10) N25 0.0212(12) 0.0257(13) 0.0269(13) 0.0064(10) 0.0094(10) 0.0007(10) C2 0.0266(16) 0.0395(19) 0.0280(16) -0.0008(13) 0.0006(13) -0.0109(14) C3 0.0408(19) 0.0333(18) 0.0298(17) -0.0068(13) 0.0115(15) -0.0155(14) C4 0.0223(15) 0.045(2) 0.0319(17) -0.0009(14) -0.0036(13) -0.0116(14) C5 0.0262(16) 0.0364(19) 0.0316(17) -0.0061(13) 0.0033(13) -0.0123(13) C6 0.0175(13) 0.0256(15) 0.0233(14) -0.0011(11) 0.0046(11) -0.0043(11) C8 0.0280(15) 0.0307(17) 0.0230(15) -0.0004(12) 0.0106(12) -0.0036(12) C9 0.0350(17) 0.0281(16) 0.0246(15) 0.0026(12) 0.0115(13) -0.0045(13) C11 0.0238(15) 0.0274(16) 0.0308(16) -0.0010(12) 0.0095(13) 0.0039(12) C12 0.055(2) 0.045(2) 0.045(2) 0.0017(17) 0.0259(19) 0.0101(18) C14 0.0365(17) 0.0218(16) 0.0323(17) 0.0025(12) 0.0132(14) 0.0038(12) C15 0.058(2) 0.032(2) 0.043(2) 0.0093(15) 0.0181(18) 0.0075(17) C17 0.037(2) 0.053(2) 0.042(2) -0.0016(17) 0.0023(16) 0.0172(17) C18 0.042(2) 0.033(2) 0.089(3) -0.0080(19) 0.032(2) -0.0008(16) C19 0.059(2) 0.033(2) 0.045(2) -0.0062(15) 0.0163(19) -0.0010(17) C20 0.040(2) 0.041(2) 0.067(3) 0.0150(18) 0.024(2) 0.0120(16) C21 0.0179(13) 0.0238(15) 0.0235(14) 0.0020(11) 0.0057(11) -0.0047(11) C23 0.0225(15) 0.0363(18) 0.0308(16) 0.0129(13) 0.0086(13) -0.0038(12) C24 0.0199(14) 0.0374(18) 0.0282(16) 0.0101(13) 0.0086(12) -0.0006(12) C26 0.0233(15) 0.0245(16) 0.0378(17) 0.0068(12) 0.0103(13) 0.0010(12) C27 0.047(2) 0.052(3) 0.069(3) 0.027(2) 0.030(2) 0.0166(19) C29 0.0250(15) 0.0351(18) 0.0329(17) 0.0044(13) 0.0126(13) 0.0053(13) C30 0.0345(18) 0.043(2) 0.0412(19) 0.0025(15) 0.0209(15) 0.0033(15) C32 0.0264(17) 0.038(2) 0.073(3) 0.0016(18) 0.0162(18) -0.0006(14) C33 0.047(2) 0.038(2) 0.061(3) -0.0062(18) 0.004(2) 0.0052(17) C34 0.047(2) 0.0324(19) 0.057(2) 0.0076(16) 0.0285(19) 0.0072(15) C35 0.0265(16) 0.045(2) 0.043(2) 0.0058(15) 0.0075(15) 0.0102(14) F1 0.0474(12) 0.0506(13) 0.0591(14) 0.0318(11) 0.0302(11) 0.0207(10) F2 0.0508(12) 0.0291(11) 0.0485(12) 0.0087(9) 0.0190(10) 0.0203(9) F3 0.0505(13) 0.0485(13) 0.0325(11) 0.0012(9) -0.0080(10) 0.0089(10) F4 0.125(3) 0.075(2) 0.068(2) 0.0094(16) 0.067(2) 0.053(2) F4A 0.079(10) 0.094(11) 0.051(9) 0.001(8) 0.058(8) 0.014(9) F5 0.0476(16) 0.133(3) 0.0247(13) -0.0083(15) 0.0147(12) 0.0178(17) F5A 0.066(9) 0.088(11) 0.070(9) -0.002(9) 0.055(8) 0.003(9) F6 0.097(3) 0.106(3) 0.076(2) -0.0338(19) 0.070(2) -0.056(2) F6A 0.095(11) 0.093(11) 0.054(10) -0.022(9) 0.037(9) 0.002(10) F7 0.0819(17) 0.0322(12) 0.0659(15) -0.0122(10) 0.0386(14) -0.0282(11) F8 0.0506(13) 0.0431(12) 0.0470(12) 0.0144(9) 0.0201(10) -0.0061(10) F9 0.0487(13) 0.0463(13) 0.0821(17) 0.0062(11) 0.0475(13) 0.0031(10) F10 0.0446(12) 0.0477(13) 0.0367(11) -0.0150(9) -0.0084(9) -0.0092(10) F11 0.0588(15) 0.126(2) 0.0348(12) -0.0327(14) 0.0023(11) 0.0417(16) F12 0.0410(11) 0.0641(15) 0.0232(10) 0.0056(9) -0.0010(8) -0.0071(10) F13 0.0359(12) 0.125(2) 0.0300(12) -0.0193(13) -0.0041(10) 0.0042(13) F14 0.0494(15) 0.0528(17) 0.129(3) -0.0075(16) -0.0171(16) -0.0268(13) F15 0.0185(9) 0.101(2) 0.0496(13) -0.0305(13) 0.0022(9) 0.0061(11) F16 0.0758(17) 0.0447(14) 0.117(2) 0.0207(14) 0.0651(17) 0.0312(12) F17 0.0544(14) 0.0812(17) 0.0393(12) 0.0079(11) 0.0303(11) 0.0218(12) F18 0.0226(10) 0.129(2) 0.0691(16) -0.0534(16) 0.0165(11) -0.0026(13) F19 0.0447(13) 0.0439(14) 0.139(3) 0.0294(15) 0.0565(16) 0.0094(10) F20 0.0652(17) 0.134(3) 0.0654(17) -0.0391(17) 0.0347(14) -0.0648(18) F21 0.0419(12) 0.0670(16) 0.0736(16) 0.0412(13) 0.0275(12) 0.0021(11) F22 0.0482(15) 0.0666(18) 0.134(3) 0.0663(18) 0.0145(16) 0.0212(13) F23 0.0748(18) 0.137(3) 0.0501(15) 0.0189(15) 0.0303(14) 0.0779(18) F24 0.0403(13) 0.0866(19) 0.0508(14) -0.0008(13) -0.0077(11) 0.0219(12) C201 0.0160(12) 0.0196(14) 0.0185(13) -0.0019(10) 0.0044(10) -0.0027(10) C202 0.0175(13) 0.0210(14) 0.0199(13) -0.0011(10) 0.0068(11) -0.0020(10) C203 0.0154(13) 0.0207(14) 0.0240(14) -0.0005(11) 0.0030(11) -0.0007(10) C204 0.0182(13) 0.0236(15) 0.0308(16) -0.0066(11) 0.0075(12) -0.0005(11) C205 0.0188(13) 0.0277(16) 0.0273(15) -0.0067(11) 0.0103(12) -0.0043(11) C206 0.0195(13) 0.0247(15) 0.0216(14) 0.0001(11) 0.0069(11) -0.0013(11) C207 0.0281(16) 0.0272(17) 0.0319(17) 0.0028(12) 0.0085(13) 0.0078(12) C208 0.0332(17) 0.042(2) 0.0337(18) -0.0063(14) 0.0188(15) 0.0013(14) C209 0.0165(12) 0.0200(14) 0.0203(13) 0.0004(10) 0.0056(11) 0.0051(10) C210 0.0192(13) 0.0200(14) 0.0218(14) -0.0014(10) 0.0061(11) 0.0011(10) C211 0.0223(14) 0.0176(14) 0.0337(16) -0.0015(11) 0.0121(12) 0.0016(11) C212 0.0194(14) 0.0213(15) 0.0354(17) -0.0094(12) 0.0048(12) -0.0015(11) C213 0.0231(14) 0.0267(16) 0.0231(14) -0.0070(11) 0.0033(12) 0.0057(11) C214 0.0209(14) 0.0245(15) 0.0215(14) -0.0007(11) 0.0065(11) 0.0032(11) C215 0.0327(17) 0.0209(16) 0.047(2) -0.0037(13) 0.0188(15) -0.0056(12) C216 0.0291(17) 0.045(2) 0.0292(17) -0.0128(15) 0.0008(14) 0.0058(14) C217 0.0205(13) 0.0151(13) 0.0197(13) 0.0011(10) 0.0080(11) -0.0005(10) C218 0.0171(13) 0.0213(15) 0.0257(14) -0.0011(11) 0.0079(11) 0.0004(10) C219 0.0187(14) 0.0234(15) 0.0263(15) -0.0040(11) 0.0021(12) -0.0007(11) C220 0.0266(15) 0.0246(15) 0.0204(14) -0.0044(11) 0.0067(12) 0.0013(11) C221 0.0220(14) 0.0217(14) 0.0216(14) 0.0005(10) 0.0086(11) 0.0023(11) C222 0.0181(13) 0.0228(14) 0.0187(13) 0.0011(10) 0.0040(11) -0.0001(10) C223 0.0270(16) 0.041(2) 0.0398(19) -0.0169(15) 0.0042(14) -0.0016(14) C224 0.0295(16) 0.0384(19) 0.0260(16) -0.0045(13) 0.0123(13) 0.0067(13) C225 0.0214(13) 0.0204(14) 0.0149(13) 0.0002(10) 0.0063(11) 0.0021(10) C226 0.0206(13) 0.0220(14) 0.0208(14) 0.0029(10) 0.0058(11) 0.0030(11) C227 0.0288(15) 0.0224(15) 0.0239(14) 0.0007(11) 0.0125(12) -0.0004(11) C228 0.0348(16) 0.0212(15) 0.0238(15) 0.0037(11) 0.0114(13) 0.0030(12) C229 0.0280(15) 0.0248(15) 0.0196(14) 0.0023(11) 0.0061(12) 0.0077(12) C230 0.0217(14) 0.0225(15) 0.0217(14) 0.0001(11) 0.0086(11) 0.0035(11) C231 0.0345(17) 0.0272(17) 0.0368(18) 0.0083(13) 0.0172(15) -0.0010(13) C232 0.0326(17) 0.0361(19) 0.0314(17) 0.0088(14) 0.0078(14) 0.0124(14) B200 0.0148(13) 0.0218(16) 0.0174(14) 0.0015(11) 0.0051(11) 0.0012(11) _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 C2 2.170(3) . ? Ir1 C3 2.154(3) . ? Ir1 C4 2.208(3) . ? Ir1 C5 2.217(3) . ? Ir1 C6 2.071(3) . ? Ir1 C21 2.065(3) . ? O13 C8 1.354(4) . ? O13 C12 1.441(5) . ? O16 C9 1.352(4) . ? O16 C15 1.463(4) . ? O28 C23 1.348(4) . ? O28 C27 1.447(4) . ? O31 C24 1.355(4) . ? O31 C30 1.449(4) . ? N7 C6 1.367(4) . ? N7 C8 1.380(4) . ? N7 C11 1.487(4) . ? N10 C6 1.369(4) . ? N10 C9 1.389(4) . ? N10 C14 1.495(4) . ? N22 C21 1.368(4) . ? N22 C23 1.388(4) . ? N22 C26 1.495(4) . ? N25 C21 1.370(4) . ? N25 C24 1.390(4) . ? N25 C29 1.495(4) . ? C2 C3 1.387(5) . ? C4 C5 1.367(5) . ? C8 C9 1.331(4) . ? C11 C12 1.549(5) . ? C11 C17 1.523(4) . ? C11 C18 1.502(5) . ? C14 C15 1.549(5) . ? C14 C19 1.514(5) . ? C14 C20 1.514(5) . ? C23 C24 1.330(4) . ? C26 C27 1.543(5) . ? C26 C32 1.512(4) . ? C26 C33 1.504(5) . ? C29 C30 1.540(5) . ? C29 C34 1.512(5) . ? C29 C35 1.526(5) . ? F1 C207 1.333(4) . ? F2 C207 1.331(3) . ? F3 C207 1.341(4) . ? F4 C208 1.332(4) . ? F4A C208 1.321(6) . ? F5 C208 1.312(4) . ? F5A C208 1.314(6) . ? F6 C208 1.315(4) . ? F6A C208 1.317(6) . ? F7 C215 1.332(4) . ? F8 C215 1.338(4) . ? F9 C215 1.338(4) . ? F10 C216 1.327(4) . ? F11 C216 1.336(4) . ? F12 C216 1.329(4) . ? F13 C223 1.342(4) . ? F14 C223 1.300(4) . ? F15 C223 1.322(3) . ? F16 C224 1.326(4) . ? F17 C224 1.324(4) . ? F18 C224 1.321(4) . ? F19 C231 1.321(4) . ? F20 C231 1.329(4) . ? F21 C231 1.319(4) . ? F22 C232 1.310(4) . ? F23 C232 1.309(4) . ? F24 C232 1.337(4) . ? C201 C202 1.394(4) . ? C201 C206 1.397(4) . ? C201 B200 1.640(4) . ? C202 C203 1.391(4) . ? C203 C204 1.383(4) . ? C203 C207 1.498(4) . ? C204 C205 1.382(4) . ? C205 C206 1.391(4) . ? C205 C208 1.497(4) . ? C209 C210 1.398(4) . ? C209 C214 1.401(4) . ? C209 B200 1.633(4) . ? C210 C211 1.394(4) . ? C211 C212 1.382(4) . ? C211 C215 1.493(4) . ? C212 C213 1.381(4) . ? C213 C214 1.388(4) . ? C213 C216 1.505(4) . ? C217 C218 1.400(4) . ? C217 C222 1.400(4) . ? C217 B200 1.638(4) . ? C218 C219 1.389(4) . ? C219 C220 1.380(4) . ? C219 C223 1.504(4) . ? C220 C221 1.386(4) . ? C221 C222 1.385(4) . ? C221 C224 1.497(4) . ? C225 C226 1.394(4) . ? C225 C230 1.401(4) . ? C225 B200 1.634(4) . ? C226 C227 1.388(4) . ? C227 C228 1.387(4) . ? C227 C231 1.491(4) . ? C228 C229 1.380(4) . ? C229 C230 1.390(4) . ? C229 C232 1.498(4) . ? 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 C2 Ir1 C4 158.94(13) . . ? C2 Ir1 C5 157.60(13) . . ? C3 Ir1 C2 37.41(13) . . ? C3 Ir1 C4 144.67(14) . . ? C3 Ir1 C5 154.65(13) . . ? C4 Ir1 C5 35.98(12) . . ? C6 Ir1 C2 82.78(12) . . ? C6 Ir1 C3 93.29(12) . . ? C6 Ir1 C4 76.24(12) . . ? C6 Ir1 C5 107.04(11) . . ? C21 Ir1 C2 92.14(12) . . ? C21 Ir1 C3 83.89(12) . . ? C21 Ir1 C4 108.75(12) . . ? C21 Ir1 C5 76.98(12) . . ? C21 Ir1 C6 174.48(10) . . ? C8 O13 C12 105.1(2) . . ? C9 O16 C15 103.8(2) . . ? C23 O28 C27 104.6(2) . . ? C24 O31 C30 103.9(2) . . ? C6 N7 C8 113.1(2) . . ? C6 N7 C11 137.8(2) . . ? C8 N7 C11 109.1(2) . . ? C6 N10 C9 112.7(2) . . ? C6 N10 C14 139.6(2) . . ? C9 N10 C14 107.6(2) . . ? C21 N22 C23 113.2(2) . . ? C21 N22 C26 138.3(2) . . ? C23 N22 C26 108.3(2) . . ? C21 N25 C24 112.9(2) . . ? C21 N25 C29 138.6(2) . . ? C24 N25 C29 107.3(2) . . ? C3 C2 Ir1 70.67(18) . . ? C2 C3 Ir1 71.93(18) . . ? C5 C4 Ir1 72.36(18) . . ? C4 C5 Ir1 71.66(18) . . ? N7 C6 Ir1 125.0(2) . . ? N7 C6 N10 101.3(2) . . ? N10 C6 Ir1 133.5(2) . . ? O13 C8 N7 113.6(3) . . ? C9 C8 O13 139.8(3) . . ? C9 C8 N7 106.6(3) . . ? O16 C9 N10 113.7(3) . . ? C8 C9 O16 139.9(3) . . ? C8 C9 N10 106.3(3) . . ? N7 C11 C12 98.9(2) . . ? N7 C11 C17 109.8(3) . . ? N7 C11 C18 113.4(3) . . ? C17 C11 C12 110.5(3) . . ? C18 C11 C12 110.5(3) . . ? C18 C11 C17 112.9(3) . . ? O13 C12 C11 107.7(3) . . ? N10 C14 C15 98.3(2) . . ? N10 C14 C19 111.1(3) . . ? N10 C14 C20 113.5(3) . . ? C19 C14 C15 109.1(3) . . ? C19 C14 C20 113.4(3) . . ? C20 C14 C15 110.3(3) . . ? O16 C15 C14 105.2(3) . . ? N22 C21 Ir1 131.1(2) . . ? N22 C21 N25 101.1(2) . . ? N25 C21 Ir1 127.8(2) . . ? O28 C23 N22 114.2(3) . . ? C24 C23 O28 139.5(3) . . ? C24 C23 N22 106.3(3) . . ? O31 C24 N25 113.6(3) . . ? C23 C24 O31 139.9(3) . . ? C23 C24 N25 106.5(3) . . ? N22 C26 C27 98.7(3) . . ? N22 C26 C32 113.8(3) . . ? N22 C26 C33 110.7(3) . . ? C32 C26 C27 109.4(3) . . ? C33 C26 C27 111.8(3) . . ? C33 C26 C32 111.8(3) . . ? O28 C27 C26 107.8(3) . . ? N25 C29 C30 97.9(2) . . ? N25 C29 C34 114.4(3) . . ? N25 C29 C35 109.5(3) . . ? C34 C29 C30 111.6(3) . . ? C34 C29 C35 111.9(3) . . ? C35 C29 C30 110.8(3) . . ? O31 C30 C29 106.1(3) . . ? C202 C201 C206 115.7(2) . . ? C202 C201 B200 121.3(2) . . ? C206 C201 B200 122.5(2) . . ? C203 C202 C201 122.2(3) . . ? C202 C203 C207 118.9(3) . . ? C204 C203 C202 121.0(3) . . ? C204 C203 C207 120.1(3) . . ? C205 C204 C203 118.0(3) . . ? C204 C205 C206 120.8(3) . . ? C204 C205 C208 119.5(3) . . ? C206 C205 C208 119.7(3) . . ? C205 C206 C201 122.3(3) . . ? F1 C207 F3 106.1(3) . . ? F1 C207 C203 112.2(2) . . ? F2 C207 F1 106.7(3) . . ? F2 C207 F3 106.6(2) . . ? F2 C207 C203 112.6(3) . . ? F3 C207 C203 112.1(3) . . ? F4 C208 C205 112.7(3) . . ? F4A C208 C205 112.7(5) . . ? F5 C208 F4 105.3(3) . . ? F5 C208 F6 106.7(3) . . ? F5 C208 C205 113.2(2) . . ? F5A C208 F4A 105.9(6) . . ? F5A C208 F6A 106.0(6) . . ? F5A C208 C205 112.9(6) . . ? F6 C208 F4 105.6(3) . . ? F6 C208 C205 112.7(3) . . ? F6A C208 F4A 105.8(6) . . ? F6A C208 C205 112.9(6) . . ? C210 C209 C214 115.6(2) . . ? C210 C209 B200 122.8(2) . . ? C214 C209 B200 121.0(2) . . ? C211 C210 C209 122.0(3) . . ? C210 C211 C215 119.7(3) . . ? C212 C211 C210 121.0(3) . . ? C212 C211 C215 119.2(3) . . ? C213 C212 C211 118.1(3) . . ? C212 C213 C214 120.8(3) . . ? C212 C213 C216 120.9(3) . . ? C214 C213 C216 118.2(3) . . ? C213 C214 C209 122.4(3) . . ? F7 C215 F8 106.2(3) . . ? F7 C215 F9 106.7(3) . . ? F7 C215 C211 112.9(3) . . ? F8 C215 F9 105.1(3) . . ? F8 C215 C211 113.1(3) . . ? F9 C215 C211 112.2(3) . . ? F10 C216 F11 106.8(3) . . ? F10 C216 F12 107.1(3) . . ? F10 C216 C213 113.0(3) . . ? F11 C216 C213 111.1(3) . . ? F12 C216 F11 106.4(3) . . ? F12 C216 C213 112.0(3) . . ? C218 C217 C222 115.5(2) . . ? C218 C217 B200 122.1(2) . . ? C222 C217 B200 122.0(2) . . ? C219 C218 C217 122.2(3) . . ? C218 C219 C223 120.8(3) . . ? C220 C219 C218 121.1(3) . . ? C220 C219 C223 118.0(3) . . ? C219 C220 C221 117.8(3) . . ? C220 C221 C224 118.2(3) . . ? C222 C221 C220 121.1(3) . . ? C222 C221 C224 120.7(3) . . ? C221 C222 C217 122.3(3) . . ? F13 C223 C219 112.2(3) . . ? F14 C223 F13 104.6(3) . . ? F14 C223 F15 109.6(3) . . ? F14 C223 C219 112.1(3) . . ? F15 C223 F13 104.7(3) . . ? F15 C223 C219 113.2(2) . . ? F16 C224 C221 112.4(3) . . ? F17 C224 F16 105.5(3) . . ? F17 C224 C221 113.3(3) . . ? F18 C224 F16 106.8(3) . . ? F18 C224 F17 105.3(3) . . ? F18 C224 C221 112.9(2) . . ? C226 C225 C230 115.3(2) . . ? C226 C225 B200 121.3(2) . . ? C230 C225 B200 123.4(2) . . ? C227 C226 C225 122.8(3) . . ? C226 C227 C231 118.4(3) . . ? C228 C227 C226 120.7(3) . . ? C228 C227 C231 120.9(3) . . ? C229 C228 C227 117.8(3) . . ? C228 C229 C230 121.1(3) . . ? C228 C229 C232 120.5(3) . . ? C230 C229 C232 118.3(3) . . ? C229 C230 C225 122.2(3) . . ? F19 C231 F20 104.8(3) . . ? F19 C231 C227 113.1(3) . . ? F20 C231 C227 112.3(3) . . ? F21 C231 F19 106.4(3) . . ? F21 C231 F20 105.8(3) . . ? F21 C231 C227 113.8(3) . . ? F22 C232 F24 103.8(3) . . ? F22 C232 C229 113.6(3) . . ? F23 C232 F22 110.3(3) . . ? F23 C232 F24 103.5(3) . . ? F23 C232 C229 112.9(3) . . ? F24 C232 C229 111.9(3) . . ? C209 B200 C201 102.8(2) . . ? C209 B200 C217 113.4(2) . . ? C209 B200 C225 112.7(2) . . ? C217 B200 C201 112.4(2) . . ? C225 B200 C201 111.3(2) . . ? C225 B200 C217 104.5(2) . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_0062abc14 #==================================================================== # [Ir(IBioxMe4)2(COD)][BArF4] #-------------------------------------------------------------------- # Collected and solved by Adrian Chaplin #-------------------------------------------------------------------- # Start Validation Reply Form _vrf_PLAT301_0062abc14 ; PROBLEM: Main Residue Disorder ............ Percentage = 9 Note RESPONSE: The structure contains a significant degree of disorder. See _publ_section_exptl_refinement. ; # End Validation Reply Form #-------------------------------------------------------------------- _publ_contact_author_name 'Adrian B. Chaplin' _publ_contact_author_email a.b.chaplin@warwick.ac.uk _publ_section_exptl_refinement ; Solved with SHELXT-2014 by direct methods. Refined full-matrix least squares on F2 using SHELXL-2014. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions and refined using the riding model. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; #==================================================================== _audit_creation_date 2015-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C30 H44 Ir N4 O4, C32 H12 B F24' _chemical_formula_sum 'C62 H56 B F24 Ir N4 O4' _chemical_formula_weight 1580.11 _chemical_absolute_configuration . _chemical_melting_point 'not measured' 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_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 13.9785(2) _cell_length_b 25.1640(4) _cell_length_c 18.1797(3) _cell_angle_alpha 90 _cell_angle_beta 103.8205(18) _cell_angle_gamma 90 _cell_volume 6209.68(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 48258 _cell_measurement_temperature 149.99(19) _cell_measurement_theta_max 33.9830 _cell_measurement_theta_min 2.8800 _shelx_estimated_absorpt_T_max . _shelx_estimated_absorpt_T_min . _exptl_absorpt_coefficient_mu 2.274 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details . _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.690 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method . _exptl_crystal_description prism _exptl_crystal_F_000 3144 _exptl_crystal_recrystallization_method 'Crystals grown from C6H4F2-heptane at 293 K' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.2 _exptl_special_details . _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_unetI/netI 0.0191 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 80294 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 27.102 _diffrn_reflns_theta_max 27.102 _diffrn_reflns_theta_min 2.923 _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.2833 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -18.00 57.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 -99.0000 90.0000 75 #__ type_ start__ end____ width___ exp.time_ 2 omega 24.00 50.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 57.0000 60.0000 26 #__ type_ start__ end____ width___ exp.time_ 3 omega 42.00 86.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 178.0000 60.0000 44 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 16.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 -99.0000 -180.0000 41 #__ type_ start__ end____ width___ exp.time_ 5 omega -1.00 99.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 38.0000 -90.0000 100 #__ type_ start__ end____ width___ exp.time_ 6 omega -84.00 -59.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 129.0000 131.8730 25 #__ type_ start__ end____ width___ exp.time_ 7 omega -39.00 8.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - -24.4093 -77.0000 -60.0000 47 #__ type_ start__ end____ width___ exp.time_ 8 omega 35.00 113.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 178.0000 -30.0000 78 #__ type_ start__ end____ width___ exp.time_ 9 omega -3.00 46.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 38.0000 30.0000 49 #__ type_ start__ end____ width___ exp.time_ 10 omega -3.00 99.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ frames - 23.3155 38.0000 150.0000 102 ; _diffrn_measurement_device_type 'Oxford Diffraction: Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0118341000 _diffrn_orient_matrix_UB_12 -0.0271478000 _diffrn_orient_matrix_UB_13 -0.0034819000 _diffrn_orient_matrix_UB_21 0.0459650000 _diffrn_orient_matrix_UB_22 0.0075049000 _diffrn_orient_matrix_UB_23 -0.0069687000 _diffrn_orient_matrix_UB_31 0.0218868000 _diffrn_orient_matrix_UB_32 -0.0010684000 _diffrn_orient_matrix_UB_33 0.0394055000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 12693 _reflns_number_total 13673 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)’ _computing_structure_solution 'ShelXT (Sheldrick, 2015)’ _refine_diff_density_max 0.717 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 957 _refine_ls_number_reflns 13673 _refine_ls_number_restraints 399 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0236 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0197P)^2^+7.3323P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.0532 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F1A \\sim C207-F2A \\sim C207-F3A with sigma of 0.01 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A with sigma of 0.01 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim C203-F3A with sigma of 0.01 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim C216-F12A with sigma of 0.01 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim F12A-F10A with sigma of 0.01 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim C213-F12A with sigma of 0.01 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim C232-F24A with sigma of 0.01 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim F24A-F22A with sigma of 0.01 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim C229-F24A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F10A \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F22A \\sim F23 \\sim F23A \\sim F24 \\sim F24A: within 1.7A with sigma of 0.007 and sigma for terminal atoms of 0.014 Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F24A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4. Others Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(1) Sof(F1)=Sof(F2)=Sof(F3)=FVAR(1) Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(2) Sof(F10)=Sof(F11)=Sof(F12)=FVAR(2) Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(3) Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3) 5.a Ternary CH refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7) 5.b Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C16(H16A,H16B), C19(H19A, H19B), C31(H31A,H31B), C34(H34A,H34B) 5.c Aromatic/amide H refined with riding coordinates: C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230) 5.d Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B, H24C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A, H39B,H39C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.25755(2) 0.02381(2) 0.20570(2) 0.01444(3) Uani 1 1 d . . . . . O17 O 0.23784(13) 0.16861(7) 0.42107(10) 0.0321(4) Uani 1 1 d . . . . . O20 O 0.00816(12) 0.14950(7) 0.31503(10) 0.0264(4) Uani 1 1 d . . . . . O32 O 0.53251(13) -0.10414(7) 0.38225(11) 0.0345(4) Uani 1 1 d . . . . . O35 O 0.30746(14) -0.13685(7) 0.40920(11) 0.0353(4) Uani 1 1 d . . . . . N11 N 0.24938(13) 0.10016(7) 0.34044(10) 0.0184(4) Uani 1 1 d . . . . . N14 N 0.10576(13) 0.08989(7) 0.26974(10) 0.0174(4) Uani 1 1 d . . . . . N26 N 0.42114(13) -0.05126(7) 0.30112(10) 0.0196(4) Uani 1 1 d . . . . . N29 N 0.28158(14) -0.07171(7) 0.31887(10) 0.0191(4) Uani 1 1 d . . . . . C2 C 0.17839(17) 0.07770(9) 0.11680(12) 0.0224(5) Uani 1 1 d . . . . . H2 H 0.1289 0.1008 0.1328 0.027 Uiso 1 1 calc R . . . . C3 C 0.27580(18) 0.09476(9) 0.14300(13) 0.0244(5) Uani 1 1 d . . . . . H3 H 0.2826 0.1281 0.1738 0.029 Uiso 1 1 calc R . . . . C4 C 0.35543(19) 0.08755(11) 0.10088(15) 0.0332(6) Uani 1 1 d . . . . . H4A H 0.4200 0.0960 0.1352 0.040 Uiso 1 1 calc R . . . . H4B H 0.3444 0.1129 0.0581 0.040 Uiso 1 1 calc R . . . . C5 C 0.3586(2) 0.03126(12) 0.07044(15) 0.0349(6) Uani 1 1 d . . . . . H5A H 0.3151 0.0292 0.0188 0.042 Uiso 1 1 calc R . . . . H5B H 0.4266 0.0231 0.0668 0.042 Uiso 1 1 calc R . . . . C6 C 0.32612(18) -0.00991(10) 0.12041(13) 0.0263(5) Uani 1 1 d . . . . . H6 H 0.3780 -0.0369 0.1413 0.032 Uiso 1 1 calc R . . . . C7 C 0.23045(18) -0.02930(10) 0.11069(12) 0.0246(5) Uani 1 1 d . . . . . H7 H 0.2274 -0.0676 0.1248 0.030 Uiso 1 1 calc R . . . . C8 C 0.14312(19) -0.01106(11) 0.05044(13) 0.0296(5) Uani 1 1 d . . . . . H8A H 0.0819 -0.0236 0.0633 0.035 Uiso 1 1 calc R . . . . H8B H 0.1462 -0.0272 0.0014 0.035 Uiso 1 1 calc R . . . . C9 C 0.13928(19) 0.04952(11) 0.04215(13) 0.0295(5) Uani 1 1 d . . . . . H9A H 0.1786 0.0604 0.0060 0.035 Uiso 1 1 calc R . . . . H9B H 0.0703 0.0606 0.0209 0.035 Uiso 1 1 calc R . . . . C10 C 0.20058(16) 0.07021(8) 0.28041(11) 0.0163(4) Uani 1 1 d . . . . . C12 C 0.19030(18) 0.13674(9) 0.36457(13) 0.0219(5) Uani 1 1 d . . . . . C13 C 0.09987(17) 0.13026(9) 0.32099(13) 0.0214(5) Uani 1 1 d . . . . . C15 C 0.35264(17) 0.10775(9) 0.38460(13) 0.0244(5) Uani 1 1 d . . . . . C16 C 0.3333(2) 0.14562(12) 0.44681(17) 0.0416(7) Uani 1 1 d . . . . . H16A H 0.3369 0.1256 0.4943 0.050 Uiso 1 1 calc R . . . . H16B H 0.3840 0.1739 0.4572 0.050 Uiso 1 1 calc R . . . . C18 C -0.00009(16) 0.07455(9) 0.23495(13) 0.0205(4) Uani 1 1 d . . . . . C19 C -0.04695(18) 0.12850(10) 0.24323(14) 0.0265(5) Uani 1 1 d . . . . . H19A H -0.0418 0.1525 0.2012 0.032 Uiso 1 1 calc R . . . . H19B H -0.1173 0.1242 0.2433 0.032 Uiso 1 1 calc R . . . . C21 C 0.4130(2) 0.13398(12) 0.33631(17) 0.0389(7) Uani 1 1 d . . . . . H21A H 0.4183 0.1101 0.2949 0.058 Uiso 1 1 calc GR . . . . H21B H 0.4790 0.1418 0.3674 0.058 Uiso 1 1 calc GR . . . . H21C H 0.3810 0.1671 0.3153 0.058 Uiso 1 1 calc GR . . . . C22 C 0.3975(2) 0.05637(10) 0.42021(15) 0.0325(6) Uani 1 1 d . . . . . H22A H 0.3540 0.0404 0.4491 0.049 Uiso 1 1 calc GR . . . . H22B H 0.4619 0.0637 0.4542 0.049 Uiso 1 1 calc GR . . . . H22C H 0.4056 0.0318 0.3804 0.049 Uiso 1 1 calc GR . . . . C23 C -0.02535(17) 0.05564(10) 0.15382(13) 0.0258(5) Uani 1 1 d . . . . . H23A H -0.0164 0.0849 0.1205 0.039 Uiso 1 1 calc GR . . . . H23B H -0.0940 0.0437 0.1400 0.039 Uiso 1 1 calc GR . . . . H23C H 0.0180 0.0261 0.1483 0.039 Uiso 1 1 calc GR . . . . C24 C -0.03343(18) 0.03377(9) 0.28596(14) 0.0257(5) Uani 1 1 d . . . . . H24A H -0.0025 -0.0006 0.2811 0.038 Uiso 1 1 calc GR . . . . H24B H -0.1052 0.0300 0.2707 0.038 Uiso 1 1 calc GR . . . . H24C H -0.0139 0.0457 0.3387 0.038 Uiso 1 1 calc GR . . . . C25 C 0.32295(16) -0.03693(8) 0.27846(12) 0.0166(4) Uani 1 1 d . . . . . C27 C 0.43655(18) -0.09119(10) 0.35573(13) 0.0252(5) Uani 1 1 d . . . . . C28 C 0.34879(19) -0.10408(9) 0.36671(13) 0.0256(5) Uani 1 1 d . . . . . C30 C 0.51876(16) -0.04145(10) 0.28246(14) 0.0253(5) Uani 1 1 d . . . . . C31 C 0.58379(19) -0.05944(11) 0.35912(16) 0.0346(6) Uani 1 1 d . . . . . H31A H 0.6498 -0.0703 0.3536 0.042 Uiso 1 1 calc R . . . . H31B H 0.5916 -0.0304 0.3968 0.042 Uiso 1 1 calc R . . . . C33 C 0.18289(17) -0.08110(9) 0.33246(13) 0.0224(5) Uani 1 1 d . . . . . C34 C 0.20312(19) -0.13568(10) 0.37244(15) 0.0310(6) Uani 1 1 d . . . . . H34A H 0.1632 -0.1398 0.4103 0.037 Uiso 1 1 calc R . . . . H34B H 0.1863 -0.1649 0.3351 0.037 Uiso 1 1 calc R . . . . C36 C 0.53465(19) -0.07972(11) 0.22110(16) 0.0333(6) Uani 1 1 d . . . . . H36A H 0.5138 -0.1155 0.2317 0.050 Uiso 1 1 calc GR . . . . H36B H 0.6046 -0.0803 0.2207 0.050 Uiso 1 1 calc GR . . . . H36C H 0.4957 -0.0679 0.1716 0.050 Uiso 1 1 calc GR . . . . C37 C 0.53610(19) 0.01590(10) 0.26512(16) 0.0322(6) Uani 1 1 d . . . . . H37A H 0.4841 0.0278 0.2220 0.048 Uiso 1 1 calc GR . . . . H37B H 0.6002 0.0193 0.2526 0.048 Uiso 1 1 calc GR . . . . H37C H 0.5353 0.0379 0.3095 0.048 Uiso 1 1 calc GR . . . . C38 C 0.10461(17) -0.08494(10) 0.25942(14) 0.0261(5) Uani 1 1 d . . . . . H38A H 0.0997 -0.0509 0.2325 0.039 Uiso 1 1 calc GR . . . . H38B H 0.0411 -0.0934 0.2706 0.039 Uiso 1 1 calc GR . . . . H38C H 0.1222 -0.1130 0.2277 0.039 Uiso 1 1 calc GR . . . . C39 C 0.16383(19) -0.03894(10) 0.38705(14) 0.0261(5) Uani 1 1 d . . . . . H39A H 0.2159 -0.0404 0.4339 0.039 Uiso 1 1 calc GR . . . . H39B H 0.0999 -0.0455 0.3986 0.039 Uiso 1 1 calc GR . . . . H39C H 0.1635 -0.0038 0.3639 0.039 Uiso 1 1 calc GR . . . . F1 F 0.2308(5) 0.4199(3) 0.6526(3) 0.0608(19) Uani 0.561(16) 1 d D U P A 1 F1A F 0.1139(6) 0.4456(3) 0.5461(7) 0.076(3) Uani 0.439(16) 1 d D U P A 2 F2 F 0.2063(7) 0.4112(3) 0.5350(4) 0.0650(19) Uani 0.561(16) 1 d D U P A 1 F2A F 0.2033(8) 0.4312(4) 0.6552(3) 0.062(2) Uani 0.439(16) 1 d D U P A 2 F3 F 0.1043(3) 0.45219(16) 0.5818(6) 0.067(2) Uani 0.561(16) 1 d D U P A 1 F3A F 0.2399(7) 0.3991(4) 0.5603(8) 0.076(3) Uani 0.439(16) 1 d D U P A 2 F4 F 0.10345(18) 0.29075(9) 0.79966(9) 0.0700(7) Uani 1 1 d . U . . . F5 F 0.1140(2) 0.21814(10) 0.74429(12) 0.0952(10) Uani 1 1 d . U . . . F6 F -0.02368(16) 0.24871(10) 0.74911(11) 0.0723(7) Uani 1 1 d . U . . . F7 F -0.24370(13) 0.44785(6) 0.36150(11) 0.0481(5) Uani 1 1 d . U . . . F8 F -0.39763(13) 0.43544(7) 0.34686(10) 0.0461(4) Uani 1 1 d . U . . . F9 F -0.32252(16) 0.40114(7) 0.26918(9) 0.0528(5) Uani 1 1 d . U . . . F10 F -0.4946(6) 0.3044(4) 0.4997(8) 0.088(3) Uani 0.505(19) 1 d D U P B 1 F10A F -0.3665(5) 0.2573(4) 0.5803(4) 0.067(2) Uani 0.495(19) 1 d D U P B 2 F11 F -0.3756(7) 0.2748(5) 0.5863(3) 0.075(2) Uani 0.505(19) 1 d D U P B 1 F11A F -0.4665(8) 0.2394(4) 0.4764(6) 0.085(3) Uani 0.495(19) 1 d D U P B 2 F12 F -0.4385(6) 0.2278(2) 0.4912(5) 0.063(2) Uani 0.505(19) 1 d D U P B 1 F12A F -0.4692(6) 0.3147(2) 0.5302(6) 0.059(2) Uani 0.495(19) 1 d D U P B 2 F13 F 0.27122(11) 0.28411(8) 0.38590(10) 0.0496(5) Uani 1 1 d . U . . . F14 F 0.23113(13) 0.33451(9) 0.29046(13) 0.0678(7) Uani 1 1 d . U . . . F15 F 0.24960(14) 0.25149(10) 0.27643(13) 0.0722(7) Uani 1 1 d . U . . . F16 F -0.18803(14) 0.31197(7) 0.15191(9) 0.0485(4) Uani 1 1 d . U . . . F17 F -0.08904(13) 0.26744(9) 0.10484(9) 0.0552(5) Uani 1 1 d . U . . . F18 F -0.19010(13) 0.22773(7) 0.15799(9) 0.0485(5) Uani 1 1 d . U . . . F19 F 0.17531(11) 0.11637(6) 0.57181(11) 0.0493(5) Uani 1 1 d . U . . . F20 F 0.08350(12) 0.05309(7) 0.59173(10) 0.0442(4) Uani 1 1 d . U . . . F21 F 0.13583(13) 0.05400(7) 0.49205(9) 0.0475(5) Uani 1 1 d . U . . . F22 F -0.3261(2) 0.1030(2) 0.4070(4) 0.0502(12) Uani 0.750(15) 1 d D U P C 1 F22A F -0.2291(7) 0.0334(3) 0.3782(10) 0.042(3) Uani 0.250(15) 1 d D U P C 2 F23 F -0.2623(4) 0.0889(2) 0.31450(13) 0.0426(11) Uani 0.750(15) 1 d D U P C 1 F23A F -0.3126(7) 0.0828(7) 0.4318(7) 0.049(3) Uani 0.250(15) 1 d D U P C 2 F24 F -0.2425(3) 0.03304(11) 0.4042(3) 0.0444(11) Uani 0.750(15) 1 d D U P C 1 F24A F -0.2930(10) 0.1037(5) 0.3246(6) 0.051(3) Uani 0.250(15) 1 d D U P C 2 C201 C -0.00138(15) 0.29027(8) 0.52855(12) 0.0167(4) Uani 1 1 d . . . . . C202 C 0.05126(16) 0.33732(9) 0.52850(12) 0.0187(4) Uani 1 1 d . . . . . H202 H 0.0493 0.3545 0.4816 0.022 Uiso 1 1 calc R . . . . C203 C 0.10673(16) 0.35997(9) 0.59504(13) 0.0211(4) Uani 1 1 d D . . . . C204 C 0.11122(17) 0.33655(10) 0.66462(13) 0.0236(5) Uani 1 1 d . . . . . H204 H 0.1496 0.3517 0.7100 0.028 Uiso 1 1 calc R . . . . C205 C 0.05823(17) 0.29042(9) 0.66621(12) 0.0216(5) Uani 1 1 d . . . . . C206 C 0.00273(16) 0.26820(9) 0.59987(12) 0.0187(4) Uani 1 1 d . . . . . H206 H -0.0339 0.2368 0.6030 0.022 Uiso 1 1 calc R . . . . C207 C 0.16278(18) 0.40964(10) 0.59038(13) 0.0315(6) Uani 1 1 d D . . . . C208 C 0.0636(2) 0.26223(11) 0.73928(14) 0.0332(6) Uani 1 1 d . . . . . C209 C -0.17846(15) 0.29152(8) 0.44166(11) 0.0154(4) Uani 1 1 d . . . . . C210 C -0.20322(16) 0.33767(8) 0.39856(12) 0.0171(4) Uani 1 1 d . . . . . H210 H -0.1565 0.3525 0.3741 0.020 Uiso 1 1 calc R . . . . C211 C -0.29363(16) 0.36258(9) 0.39025(12) 0.0198(4) Uani 1 1 d . . . . . C212 C -0.36341(17) 0.34311(9) 0.42580(14) 0.0249(5) Uani 1 1 d . . . . . H212 H -0.4259 0.3597 0.4192 0.030 Uiso 1 1 calc R . . . . C213 C -0.33920(17) 0.29872(9) 0.47120(14) 0.0266(5) Uani 1 1 d D . . . . C214 C -0.24871(17) 0.27360(9) 0.47917(13) 0.0215(5) Uani 1 1 d . . . . . H214 H -0.2342 0.2433 0.5111 0.026 Uiso 1 1 calc R . . . . C215 C -0.31433(19) 0.41115(10) 0.34198(14) 0.0282(5) Uani 1 1 d . . . . . C216 C -0.4113(2) 0.27726(11) 0.51268(17) 0.0439(7) Uani 1 1 d D . . . . C217 C -0.02761(16) 0.27206(8) 0.37620(12) 0.0162(4) Uani 1 1 d . . . . . C218 C 0.07271(16) 0.27662(8) 0.37841(13) 0.0191(4) Uani 1 1 d . . . . . H218 H 0.1188 0.2781 0.4262 0.023 Uiso 1 1 calc R . . . . C219 C 0.10703(17) 0.27909(9) 0.31275(13) 0.0216(5) Uani 1 1 d . . . . . C220 C 0.04262(18) 0.27677(9) 0.24176(13) 0.0224(5) Uani 1 1 d . . . . . H220 H 0.0662 0.2788 0.1970 0.027 Uiso 1 1 calc R . . . . C221 C -0.05688(17) 0.27150(9) 0.23802(12) 0.0204(4) Uani 1 1 d . . . . . C222 C -0.09104(16) 0.26916(8) 0.30394(12) 0.0178(4) Uani 1 1 d . . . . . H222 H -0.1598 0.2655 0.2997 0.021 Uiso 1 1 calc R . . . . C223 C 0.21403(19) 0.28691(11) 0.31689(15) 0.0321(6) Uani 1 1 d . . . . . C224 C -0.13013(19) 0.26950(10) 0.16346(13) 0.0271(5) Uani 1 1 d . . . . . C225 C -0.07396(15) 0.19915(8) 0.46022(11) 0.0150(4) Uani 1 1 d . . . . . C226 C 0.01043(15) 0.17040(8) 0.49612(12) 0.0162(4) Uani 1 1 d . . . . . H226 H 0.0687 0.1893 0.5194 0.019 Uiso 1 1 calc R . . . . C227 C 0.01128(15) 0.11541(8) 0.49867(11) 0.0156(4) Uani 1 1 d . . . . . C228 C -0.07177(16) 0.08608(8) 0.46466(12) 0.0167(4) Uani 1 1 d . . . . . H228 H -0.0713 0.0483 0.4663 0.020 Uiso 1 1 calc R . . . . C229 C -0.15515(15) 0.11375(8) 0.42832(11) 0.0164(4) Uani 1 1 d D . . . . C230 C -0.15601(15) 0.16903(8) 0.42616(11) 0.0163(4) Uani 1 1 d . . . . . H230 H -0.2145 0.1868 0.4006 0.020 Uiso 1 1 calc R . . . . C231 C 0.10129(16) 0.08572(9) 0.53863(13) 0.0204(4) Uani 1 1 d . . . . . C232 C -0.24595(16) 0.08434(8) 0.38987(12) 0.0220(5) Uani 1 1 d D . . . . B200 B -0.07008(17) 0.26377(9) 0.45203(13) 0.0147(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 0.01488(4) 0.01510(4) 0.01276(4) -0.00032(3) 0.00213(3) -0.00048(3) O17 0.0320(10) 0.0294(9) 0.0309(9) -0.0167(8) 0.0000(8) -0.0004(8) O20 0.0244(8) 0.0232(9) 0.0311(9) -0.0083(7) 0.0054(7) 0.0049(7) O32 0.0247(9) 0.0356(10) 0.0377(10) 0.0088(8) -0.0036(8) 0.0093(8) O35 0.0407(11) 0.0311(10) 0.0355(10) 0.0173(8) 0.0119(8) 0.0059(8) N11 0.0195(9) 0.0171(9) 0.0176(9) -0.0022(7) 0.0025(7) -0.0003(7) N14 0.0191(9) 0.0138(8) 0.0183(9) -0.0030(7) 0.0025(7) -0.0007(7) N26 0.0160(9) 0.0207(9) 0.0210(9) 0.0010(7) 0.0021(7) 0.0016(7) N29 0.0202(9) 0.0178(9) 0.0191(9) 0.0027(7) 0.0043(7) 0.0034(7) C2 0.0239(11) 0.0235(12) 0.0189(10) 0.0077(9) 0.0031(9) 0.0028(9) C3 0.0290(12) 0.0208(11) 0.0232(11) 0.0068(9) 0.0057(10) -0.0031(9) C4 0.0275(13) 0.0443(16) 0.0287(13) 0.0116(11) 0.0085(10) -0.0077(11) C5 0.0274(13) 0.0561(18) 0.0243(12) 0.0002(12) 0.0121(10) 0.0001(12) C6 0.0265(12) 0.0344(14) 0.0185(11) -0.0037(10) 0.0064(9) 0.0061(10) C7 0.0306(12) 0.0259(12) 0.0166(10) -0.0075(9) 0.0043(9) 0.0001(10) C8 0.0289(13) 0.0389(15) 0.0186(11) -0.0083(10) 0.0010(10) -0.0037(11) C9 0.0253(12) 0.0442(15) 0.0166(11) 0.0049(10) 0.0000(9) 0.0007(11) C10 0.0186(10) 0.0147(10) 0.0146(9) 0.0008(8) 0.0022(8) 0.0005(8) C12 0.0285(12) 0.0165(11) 0.0203(11) -0.0036(9) 0.0052(9) 0.0000(9) C13 0.0244(11) 0.0167(11) 0.0235(11) -0.0038(9) 0.0066(9) 0.0030(9) C15 0.0207(11) 0.0237(12) 0.0250(11) -0.0062(9) -0.0024(9) -0.0017(9) C16 0.0331(15) 0.0440(17) 0.0395(15) -0.0218(13) -0.0073(12) 0.0068(12) C18 0.0159(10) 0.0224(11) 0.0226(11) -0.0034(9) 0.0035(8) 0.0010(9) C19 0.0223(12) 0.0254(12) 0.0297(12) -0.0040(10) 0.0020(10) 0.0041(9) C21 0.0235(13) 0.0437(16) 0.0462(16) 0.0032(13) 0.0019(12) -0.0096(12) C22 0.0325(14) 0.0295(14) 0.0280(13) -0.0030(10) -0.0072(11) 0.0028(11) C23 0.0198(11) 0.0317(13) 0.0244(12) -0.0051(10) 0.0022(9) -0.0009(9) C24 0.0228(12) 0.0247(12) 0.0309(13) -0.0011(10) 0.0093(10) -0.0004(9) C25 0.0174(10) 0.0168(10) 0.0154(10) -0.0040(8) 0.0033(8) 0.0010(8) C27 0.0250(12) 0.0239(12) 0.0237(11) 0.0034(9) 0.0001(9) 0.0073(9) C28 0.0315(13) 0.0213(12) 0.0232(11) 0.0067(9) 0.0048(10) 0.0058(10) C30 0.0144(11) 0.0270(12) 0.0330(13) -0.0006(10) 0.0023(9) 0.0015(9) C31 0.0195(12) 0.0389(15) 0.0401(15) 0.0030(12) -0.0032(11) 0.0045(11) C33 0.0256(12) 0.0195(11) 0.0252(11) 0.0032(9) 0.0120(9) 0.0006(9) C34 0.0365(14) 0.0240(12) 0.0368(14) 0.0092(11) 0.0172(12) 0.0012(10) C36 0.0247(13) 0.0361(15) 0.0409(15) -0.0031(12) 0.0112(11) 0.0076(11) C37 0.0227(12) 0.0316(14) 0.0394(14) -0.0007(11) 0.0019(11) -0.0085(10) C38 0.0216(11) 0.0236(12) 0.0343(13) -0.0031(10) 0.0086(10) -0.0017(9) C39 0.0338(13) 0.0235(12) 0.0252(12) 0.0020(9) 0.0151(10) 0.0021(10) F1 0.042(3) 0.063(3) 0.061(3) 0.013(2) -0.021(2) -0.034(2) F1A 0.074(4) 0.045(3) 0.090(5) 0.037(3) -0.019(3) -0.036(3) F2 0.099(4) 0.057(3) 0.053(3) -0.018(2) 0.047(3) -0.049(3) F2A 0.100(6) 0.046(3) 0.043(3) -0.028(3) 0.023(3) -0.047(4) F3 0.042(2) 0.0241(19) 0.135(5) 0.009(3) 0.023(3) -0.0034(16) F3A 0.064(4) 0.072(4) 0.110(6) -0.021(4) 0.052(4) -0.036(3) F4 0.1062(18) 0.0763(14) 0.0197(8) 0.0007(9) -0.0004(9) -0.0326(13) F5 0.170(3) 0.0746(16) 0.0526(13) 0.0412(12) 0.0487(15) 0.0732(17) F6 0.0681(14) 0.1109(18) 0.0386(10) 0.0245(11) 0.0140(10) -0.0316(13) F7 0.0493(10) 0.0226(8) 0.0643(11) 0.0165(8) -0.0026(9) -0.0035(7) F8 0.0430(10) 0.0415(10) 0.0533(10) 0.0168(8) 0.0105(8) 0.0269(8) F9 0.0942(15) 0.0397(10) 0.0238(8) 0.0083(7) 0.0125(9) 0.0203(10) F10 0.048(3) 0.089(5) 0.149(6) 0.059(4) 0.065(4) 0.034(3) F10A 0.070(3) 0.075(4) 0.077(4) 0.041(3) 0.058(3) 0.028(3) F11 0.084(4) 0.093(5) 0.065(3) -0.003(3) 0.053(3) -0.016(4) F11A 0.067(4) 0.086(4) 0.116(5) -0.033(4) 0.050(4) -0.047(4) F12 0.044(3) 0.051(3) 0.104(4) 0.020(3) 0.038(3) -0.014(2) F12A 0.058(3) 0.043(3) 0.097(4) 0.003(3) 0.061(3) 0.010(2) F13 0.0218(8) 0.0776(13) 0.0477(10) 0.0165(9) 0.0052(7) -0.0068(8) F14 0.0344(10) 0.0689(14) 0.0997(17) 0.0501(12) 0.0150(10) -0.0114(9) F15 0.0349(10) 0.1037(18) 0.0870(15) -0.0344(13) 0.0325(10) 0.0050(11) F16 0.0532(11) 0.0433(10) 0.0385(9) 0.0026(8) -0.0101(8) 0.0193(8) F17 0.0471(10) 0.1008(16) 0.0188(7) -0.0041(9) 0.0103(7) 0.0037(10) F18 0.0533(11) 0.0442(10) 0.0363(9) 0.0035(8) -0.0120(8) -0.0184(8) F19 0.0233(8) 0.0245(8) 0.0832(13) 0.0021(8) -0.0206(8) -0.0003(6) F20 0.0317(8) 0.0531(10) 0.0474(10) 0.0336(8) 0.0084(7) 0.0131(7) F21 0.0501(10) 0.0502(10) 0.0405(9) -0.0036(8) 0.0076(8) 0.0344(9) F22 0.0180(12) 0.053(2) 0.080(3) -0.0275(19) 0.0116(14) -0.0088(12) F22A 0.028(4) 0.023(4) 0.068(7) -0.015(4) 0.000(4) -0.001(3) F23 0.0394(18) 0.058(2) 0.0224(12) 0.0011(11) -0.0086(10) -0.0211(16) F23A 0.028(4) 0.077(7) 0.044(5) -0.015(4) 0.013(3) -0.023(4) F24 0.0382(17) 0.0209(13) 0.059(2) 0.0138(11) -0.0185(15) -0.0158(11) F24A 0.048(5) 0.035(4) 0.049(5) 0.024(4) -0.029(4) -0.021(4) C201 0.0149(10) 0.0151(10) 0.0196(10) 0.0006(8) 0.0030(8) 0.0026(8) C202 0.0193(10) 0.0179(10) 0.0190(10) 0.0020(8) 0.0047(8) -0.0004(8) C203 0.0185(11) 0.0187(11) 0.0261(11) -0.0029(9) 0.0052(9) -0.0023(8) C204 0.0207(11) 0.0278(12) 0.0200(11) -0.0064(9) 0.0006(9) -0.0006(9) C205 0.0233(11) 0.0230(11) 0.0180(10) 0.0004(9) 0.0041(9) 0.0029(9) C206 0.0203(11) 0.0159(10) 0.0202(10) 0.0000(8) 0.0052(8) -0.0004(8) C207 0.0311(14) 0.0300(13) 0.0319(13) -0.0052(11) 0.0045(11) -0.0120(11) C208 0.0435(16) 0.0343(14) 0.0204(12) 0.0023(10) 0.0048(11) -0.0003(12) C209 0.0161(10) 0.0142(10) 0.0151(9) -0.0016(8) 0.0018(8) 0.0005(8) C210 0.0198(10) 0.0149(10) 0.0165(10) -0.0017(8) 0.0042(8) -0.0003(8) C211 0.0227(11) 0.0157(10) 0.0189(10) -0.0025(8) 0.0006(9) 0.0031(8) C212 0.0188(11) 0.0215(11) 0.0342(13) -0.0031(10) 0.0059(10) 0.0047(9) C213 0.0237(12) 0.0238(12) 0.0364(13) -0.0009(10) 0.0150(10) 0.0002(9) C214 0.0242(11) 0.0170(11) 0.0249(11) 0.0040(9) 0.0093(9) 0.0029(9) C215 0.0323(13) 0.0238(12) 0.0260(12) 0.0015(10) 0.0019(10) 0.0105(10) C216 0.0358(16) 0.0364(16) 0.069(2) 0.0116(15) 0.0320(15) 0.0053(13) C217 0.0204(10) 0.0095(9) 0.0189(10) 0.0011(8) 0.0050(8) 0.0009(8) C218 0.0189(11) 0.0163(10) 0.0216(11) 0.0018(8) 0.0041(9) 0.0013(8) C219 0.0209(11) 0.0170(11) 0.0287(12) 0.0027(9) 0.0096(9) 0.0018(8) C220 0.0290(12) 0.0189(11) 0.0227(11) 0.0020(9) 0.0126(9) 0.0027(9) C221 0.0276(12) 0.0146(10) 0.0194(10) 0.0004(8) 0.0064(9) 0.0037(9) C222 0.0202(11) 0.0133(10) 0.0204(10) 0.0001(8) 0.0057(8) 0.0023(8) C223 0.0252(13) 0.0382(15) 0.0363(14) 0.0072(12) 0.0139(11) -0.0005(11) C224 0.0324(13) 0.0284(13) 0.0201(11) 0.0010(10) 0.0052(10) 0.0036(10) C225 0.0178(10) 0.0138(10) 0.0136(9) 0.0004(8) 0.0042(8) 0.0001(8) C226 0.0154(10) 0.0156(10) 0.0172(10) -0.0010(8) 0.0030(8) -0.0017(8) C227 0.0181(10) 0.0146(10) 0.0141(9) 0.0010(8) 0.0039(8) 0.0016(8) C228 0.0220(11) 0.0115(10) 0.0168(10) 0.0005(8) 0.0054(8) -0.0005(8) C229 0.0172(10) 0.0169(10) 0.0146(9) 0.0001(8) 0.0029(8) -0.0029(8) C230 0.0164(10) 0.0166(10) 0.0158(10) 0.0020(8) 0.0034(8) 0.0015(8) C231 0.0201(11) 0.0154(10) 0.0244(11) 0.0010(8) 0.0031(9) 0.0010(8) C232 0.0214(11) 0.0188(11) 0.0230(11) 0.0005(9) -0.0004(9) -0.0035(9) B200 0.0143(11) 0.0125(11) 0.0169(11) 0.0020(9) 0.0030(9) 0.0009(8) _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 C2 2.196(2) . ? Ir1 C3 2.166(2) . ? Ir1 C6 2.180(2) . ? Ir1 C7 2.145(2) . ? Ir1 C10 2.088(2) . ? Ir1 C25 2.084(2) . ? O17 C12 1.347(3) . ? O17 C16 1.427(3) . ? O20 C13 1.350(3) . ? O20 C19 1.448(3) . ? O32 C27 1.352(3) . ? O32 C31 1.449(3) . ? O35 C28 1.350(3) . ? O35 C34 1.452(3) . ? N11 C10 1.367(3) . ? N11 C12 1.377(3) . ? N11 C15 1.487(3) . ? N14 C10 1.384(3) . ? N14 C13 1.394(3) . ? N14 C18 1.514(3) . ? N26 C25 1.383(3) . ? N26 C27 1.393(3) . ? N26 C30 1.503(3) . ? N29 C25 1.358(3) . ? N29 C28 1.383(3) . ? N29 C33 1.477(3) . ? C2 C3 1.398(3) . ? C2 C9 1.513(3) . ? C3 C4 1.505(3) . ? C4 C5 1.525(4) . ? C5 C6 1.517(4) . ? C6 C7 1.395(3) . ? C7 C8 1.504(3) . ? C8 C9 1.532(4) . ? C12 C13 1.332(3) . ? C15 C16 1.551(3) . ? C15 C21 1.508(4) . ? C15 C22 1.513(3) . ? C18 C19 1.530(3) . ? C18 C23 1.509(3) . ? C18 C24 1.529(3) . ? C27 C28 1.329(4) . ? C30 C31 1.539(3) . ? C30 C36 1.530(4) . ? C30 C37 1.509(3) . ? C33 C34 1.548(3) . ? C33 C38 1.509(3) . ? C33 C39 1.519(3) . ? F1 C207 1.318(4) . ? F1A C207 1.294(5) . ? F2 C207 1.295(4) . ? F2A C207 1.298(5) . ? F3 C207 1.334(4) . ? F3A C207 1.346(5) . ? F4 C208 1.318(3) . ? F5 C208 1.305(3) . ? F6 C208 1.319(3) . ? F7 C215 1.336(3) . ? F8 C215 1.337(3) . ? F9 C215 1.325(3) . ? F10 C216 1.321(5) . ? F10A C216 1.337(5) . ? F11 C216 1.314(5) . ? F11A C216 1.300(5) . ? F12 C216 1.333(5) . ? F12A C216 1.329(4) . ? F13 C223 1.319(3) . ? F14 C223 1.333(3) . ? F15 C223 1.326(3) . ? F16 C224 1.327(3) . ? F17 C224 1.327(3) . ? F18 C224 1.333(3) . ? F19 C231 1.316(3) . ? F20 C231 1.335(3) . ? F21 C231 1.335(3) . ? F22 C232 1.318(3) . ? F22A C232 1.330(5) . ? F23 C232 1.339(3) . ? F23A C232 1.338(5) . ? F24 C232 1.316(3) . ? F24A C232 1.305(5) . ? C201 C202 1.394(3) . ? C201 C206 1.399(3) . ? C201 B200 1.632(3) . ? C202 C203 1.393(3) . ? C203 C204 1.383(3) . ? C203 C207 1.488(3) . ? C204 C205 1.381(3) . ? C205 C206 1.386(3) . ? C205 C208 1.492(3) . ? C209 C210 1.397(3) . ? C209 C214 1.397(3) . ? C209 B200 1.638(3) . ? C210 C211 1.386(3) . ? C211 C212 1.382(3) . ? C211 C215 1.492(3) . ? C212 C213 1.382(3) . ? C213 C214 1.390(3) . ? C213 C216 1.497(4) . ? C217 C218 1.398(3) . ? C217 C222 1.400(3) . ? C217 B200 1.639(3) . ? C218 C219 1.390(3) . ? C219 C220 1.387(3) . ? C219 C223 1.493(3) . ? C220 C221 1.383(3) . ? C221 C222 1.393(3) . ? C221 C224 1.492(3) . ? C225 C226 1.405(3) . ? C225 C230 1.391(3) . ? C225 B200 1.635(3) . ? C226 C227 1.384(3) . ? C227 C228 1.390(3) . ? C227 C231 1.494(3) . ? C228 C229 1.383(3) . ? C229 C230 1.392(3) . ? C229 C232 1.491(3) . ? 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 C3 Ir1 C2 37.39(9) . . ? C3 Ir1 C6 79.60(10) . . ? C6 Ir1 C2 86.94(9) . . ? C7 Ir1 C2 80.27(9) . . ? C7 Ir1 C3 96.32(9) . . ? C7 Ir1 C6 37.61(9) . . ? C10 Ir1 C2 85.98(8) . . ? C10 Ir1 C3 89.57(9) . . ? C10 Ir1 C6 168.86(9) . . ? C10 Ir1 C7 148.31(9) . . ? C25 Ir1 C2 170.97(8) . . ? C25 Ir1 C3 148.16(9) . . ? C25 Ir1 C6 88.01(9) . . ? C25 Ir1 C7 91.18(9) . . ? C25 Ir1 C10 100.07(8) . . ? C12 O17 C16 105.14(18) . . ? C13 O20 C19 103.42(17) . . ? C27 O32 C31 103.10(18) . . ? C28 O35 C34 104.13(18) . . ? C10 N11 C12 113.59(18) . . ? C10 N11 C15 137.45(19) . . ? C12 N11 C15 108.73(18) . . ? C10 N14 C13 111.98(18) . . ? C10 N14 C18 140.80(18) . . ? C13 N14 C18 104.90(17) . . ? C25 N26 C27 111.96(19) . . ? C25 N26 C30 141.23(19) . . ? C27 N26 C30 106.57(18) . . ? C25 N29 C28 114.01(19) . . ? C25 N29 C33 136.81(18) . . ? C28 N29 C33 108.77(18) . . ? C3 C2 Ir1 70.15(13) . . ? C3 C2 C9 124.3(2) . . ? C9 C2 Ir1 112.43(16) . . ? C2 C3 Ir1 72.46(13) . . ? C2 C3 C4 124.6(2) . . ? C4 C3 Ir1 111.27(17) . . ? C3 C4 C5 112.7(2) . . ? C6 C5 C4 112.2(2) . . ? C5 C6 Ir1 113.91(17) . . ? C7 C6 Ir1 69.82(13) . . ? C7 C6 C5 125.3(2) . . ? C6 C7 Ir1 72.57(13) . . ? C6 C7 C8 124.9(2) . . ? C8 C7 Ir1 110.66(16) . . ? C7 C8 C9 112.3(2) . . ? C2 C9 C8 112.42(19) . . ? N11 C10 Ir1 129.24(15) . . ? N11 C10 N14 101.14(17) . . ? N14 C10 Ir1 127.59(15) . . ? O17 C12 N11 114.6(2) . . ? C13 C12 O17 138.8(2) . . ? C13 C12 N11 106.56(19) . . ? O20 C13 N14 114.46(19) . . ? C12 C13 O20 138.8(2) . . ? C12 C13 N14 106.72(19) . . ? N11 C15 C16 99.03(19) . . ? N11 C15 C21 110.4(2) . . ? N11 C15 C22 111.77(19) . . ? C21 C15 C16 112.0(2) . . ? C21 C15 C22 113.0(2) . . ? C22 C15 C16 109.8(2) . . ? O17 C16 C15 108.8(2) . . ? N14 C18 C19 97.55(17) . . ? N14 C18 C24 109.09(18) . . ? C23 C18 N14 117.76(18) . . ? C23 C18 C19 111.73(19) . . ? C23 C18 C24 110.30(19) . . ? C24 C18 C19 109.65(19) . . ? O20 C19 C18 105.33(18) . . ? N26 C25 Ir1 129.34(16) . . ? N29 C25 Ir1 129.58(15) . . ? N29 C25 N26 101.03(18) . . ? O32 C27 N26 113.5(2) . . ? C28 C27 O32 139.5(2) . . ? C28 C27 N26 107.0(2) . . ? O35 C28 N29 113.6(2) . . ? C27 C28 O35 140.5(2) . . ? C27 C28 N29 105.9(2) . . ? N26 C30 C31 96.83(19) . . ? N26 C30 C36 111.04(19) . . ? N26 C30 C37 113.8(2) . . ? C36 C30 C31 108.5(2) . . ? C37 C30 C31 112.4(2) . . ? C37 C30 C36 113.0(2) . . ? O32 C31 C30 105.37(19) . . ? N29 C33 C34 98.47(18) . . ? N29 C33 C38 111.90(18) . . ? N29 C33 C39 108.31(19) . . ? C38 C33 C34 111.7(2) . . ? C38 C33 C39 114.6(2) . . ? C39 C33 C34 110.71(19) . . ? O35 C34 C33 106.56(19) . . ? C202 C201 C206 115.65(19) . . ? C202 C201 B200 123.34(18) . . ? C206 C201 B200 120.89(19) . . ? C203 C202 C201 122.1(2) . . ? C202 C203 C207 119.0(2) . . ? C204 C203 C202 120.9(2) . . ? C204 C203 C207 120.0(2) . . ? C205 C204 C203 118.0(2) . . ? C204 C205 C206 120.8(2) . . ? C204 C205 C208 120.3(2) . . ? C206 C205 C208 118.8(2) . . ? C205 C206 C201 122.5(2) . . ? F1 C207 F3 103.9(4) . . ? F1 C207 C203 113.4(3) . . ? F1A C207 F2A 108.9(4) . . ? F1A C207 F3A 103.8(4) . . ? F1A C207 C203 114.6(3) . . ? F2 C207 F1 106.5(4) . . ? F2 C207 F3 105.9(4) . . ? F2 C207 C203 114.9(3) . . ? F2A C207 F3A 103.5(4) . . ? F2A C207 C203 114.9(4) . . ? F3 C207 C203 111.4(3) . . ? F3A C207 C203 110.0(4) . . ? F4 C208 F6 104.4(2) . . ? F4 C208 C205 113.8(2) . . ? F5 C208 F4 106.9(3) . . ? F5 C208 F6 105.8(3) . . ? F5 C208 C205 112.2(2) . . ? F6 C208 C205 113.0(2) . . ? C210 C209 B200 121.15(19) . . ? C214 C209 C210 115.66(19) . . ? C214 C209 B200 123.02(19) . . ? C211 C210 C209 122.3(2) . . ? C210 C211 C215 118.6(2) . . ? C212 C211 C210 121.0(2) . . ? C212 C211 C215 120.4(2) . . ? C213 C212 C211 117.8(2) . . ? C212 C213 C214 121.1(2) . . ? C212 C213 C216 119.6(2) . . ? C214 C213 C216 119.3(2) . . ? C213 C214 C209 122.0(2) . . ? F7 C215 F8 105.5(2) . . ? F7 C215 C211 112.5(2) . . ? F8 C215 C211 112.7(2) . . ? F9 C215 F7 106.2(2) . . ? F9 C215 F8 106.5(2) . . ? F9 C215 C211 113.0(2) . . ? F10 C216 F12 104.7(4) . . ? F10 C216 C213 113.2(4) . . ? F10A C216 C213 111.9(4) . . ? F11 C216 F10 108.1(4) . . ? F11 C216 F12 105.4(4) . . ? F11 C216 C213 113.1(4) . . ? F11A C216 F10A 106.4(4) . . ? F11A C216 F12A 108.7(4) . . ? F11A C216 C213 113.4(4) . . ? F12 C216 C213 111.6(4) . . ? F12A C216 F10A 103.0(4) . . ? F12A C216 C213 112.7(3) . . ? C218 C217 C222 115.93(19) . . ? C218 C217 B200 123.27(19) . . ? C222 C217 B200 120.46(19) . . ? C219 C218 C217 121.9(2) . . ? C218 C219 C223 120.7(2) . . ? C220 C219 C218 121.1(2) . . ? C220 C219 C223 118.2(2) . . ? C221 C220 C219 118.1(2) . . ? C220 C221 C222 120.6(2) . . ? C220 C221 C224 120.8(2) . . ? C222 C221 C224 118.6(2) . . ? C221 C222 C217 122.3(2) . . ? F13 C223 F14 105.7(2) . . ? F13 C223 F15 105.6(2) . . ? F13 C223 C219 114.4(2) . . ? F14 C223 C219 111.4(2) . . ? F15 C223 F14 106.3(2) . . ? F15 C223 C219 112.8(2) . . ? F16 C224 F17 105.6(2) . . ? F16 C224 F18 105.9(2) . . ? F16 C224 C221 112.2(2) . . ? F17 C224 F18 107.1(2) . . ? F17 C224 C221 113.3(2) . . ? F18 C224 C221 112.2(2) . . ? C226 C225 B200 120.81(18) . . ? C230 C225 C226 115.96(19) . . ? C230 C225 B200 122.91(18) . . ? C227 C226 C225 122.0(2) . . ? C226 C227 C228 121.09(19) . . ? C226 C227 C231 121.03(19) . . ? C228 C227 C231 117.88(18) . . ? C229 C228 C227 117.67(19) . . ? C228 C229 C230 121.16(19) . . ? C228 C229 C232 120.01(19) . . ? C230 C229 C232 118.83(19) . . ? C225 C230 C229 122.1(2) . . ? F19 C231 F20 106.9(2) . . ? F19 C231 F21 106.1(2) . . ? F19 C231 C227 114.12(18) . . ? F20 C231 F21 104.41(19) . . ? F20 C231 C227 112.23(18) . . ? F21 C231 C227 112.37(18) . . ? F22 C232 F23 105.3(2) . . ? F22 C232 C229 112.9(2) . . ? F22A C232 F23A 103.7(5) . . ? F22A C232 C229 112.9(4) . . ? F23 C232 C229 110.8(2) . . ? F23A C232 C229 112.2(4) . . ? F24 C232 F22 107.2(3) . . ? F24 C232 F23 106.0(3) . . ? F24 C232 C229 114.0(2) . . ? F24A C232 F22A 106.5(5) . . ? F24A C232 F23A 105.1(5) . . ? F24A C232 C229 115.4(4) . . ? C201 B200 C209 105.29(16) . . ? C201 B200 C217 114.03(17) . . ? C201 B200 C225 110.75(17) . . ? C209 B200 C217 111.09(17) . . ? C225 B200 C209 112.62(17) . . ? C225 B200 C217 103.28(16) . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END data_0078abc14 #==================================================================== # [Ir(IBioxMe4)2(CO)2][BArF4] #-------------------------------------------------------------------- # Collected and solved by Adrian Chaplin #-------------------------------------------------------------------- # Start Validation Reply Form _vrf_PLAT301_0078abc14 ; PROBLEM: Main Residue Disorder ............ Percentage = 13 Note RESPONSE: The structure contains a significant degree of disorder. See _publ_section_exptl_refinement. ; # End Validation Reply Form #-------------------------------------------------------------------- _publ_contact_author_name 'Adrian B. Chaplin' _publ_contact_author_email a.b.chaplin@warwick.ac.uk _publ_section_exptl_refinement ; Solved with SHELXT-2014 by direct methods. Refined full-matrix least squares on F2 using SHELXL-2014. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions and refined using the riding model. Rotational disorder of the CF3 groups of the anion was treated by modelling the fluorine atoms over two sites and restraining their geometry. Restraints to thermal parameters were applied where necessary in order to maintain sensible values. ; #==================================================================== _audit_creation_date 2015-06-17 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998) ; _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C24 H32 Ir N4 O6, C32 H12 B F24' _chemical_formula_sum 'C56 H44 B F24 Ir N4 O6' _chemical_formula_weight 1527.96 _chemical_absolute_configuration . _chemical_melting_point 'not measured' 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' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_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 20.5168(3) _cell_length_b 17.3725(3) _cell_length_c 34.3622(8) _cell_angle_alpha 90 _cell_angle_beta 98.034(2) _cell_angle_gamma 90 _cell_volume 12127.4(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 19285 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 31.7780 _cell_measurement_theta_min 3.5910 _shelx_estimated_absorpt_T_max . _shelx_estimated_absorpt_T_min . _exptl_absorpt_coefficient_mu 2.328 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details . _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method . _exptl_crystal_description plate _exptl_crystal_F_000 6032 _exptl_crystal_recrystallization_method 'Crystals grown from C6H4F2-heptane at 293 K' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_special_details . _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_unetI/netI 0.0402 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_number 58266 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 27.103 _diffrn_reflns_theta_max 27.103 _diffrn_reflns_theta_min 3.332 _diffrn_ambient_temperature 150(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.2833 _diffrn_detector_type Ruby _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -29.00 99.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 17.3355 19.0000 -120.0000 128 #__ type_ start__ end____ width___ exp.time_ 2 omega -9.00 93.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 17.3355 38.0000 -60.0000 102 #__ type_ start__ end____ width___ exp.time_ 3 omega 35.00 107.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - 17.3355 178.0000 -120.0000 72 #__ type_ start__ end____ width___ exp.time_ 4 omega -25.00 24.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - -18.2730 -99.0000 -120.0000 49 #__ type_ start__ end____ width___ exp.time_ 5 omega -108.00 -57.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - -18.2730 -178.0000 -90.0000 51 #__ type_ start__ end____ width___ exp.time_ 6 omega -107.00 -106.00 1.0000 7.5000 omega____ theta____ kappa____ phi______ frames - -18.2730 178.0000 150.0000 1 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction: Xcalibur, Ruby, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0310032000 _diffrn_orient_matrix_UB_12 0.0078912000 _diffrn_orient_matrix_UB_13 0.0060346000 _diffrn_orient_matrix_UB_21 -0.0149985000 _diffrn_orient_matrix_UB_22 -0.0009317000 _diffrn_orient_matrix_UB_23 -0.0198838000 _diffrn_orient_matrix_UB_31 -0.0057543000 _diffrn_orient_matrix_UB_32 -0.0400482000 _diffrn_orient_matrix_UB_33 0.0016527000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11165 _reflns_number_total 13358 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.042 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.082 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 948 _refine_ls_number_reflns 13358 _refine_ls_number_restraints 498 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0301 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+10.0796P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.0664 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim C208-F6A with sigma of 0.01 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A with sigma of 0.01 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim C205-F6A with sigma of 0.01 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim C232-F24A with sigma of 0.01 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim F24A-F22A with sigma of 0.01 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim C229-F24A with sigma of 0.01 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim C231-F21A with sigma of 0.01 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim F21A-F19A with sigma of 0.01 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim C227-F21A with sigma of 0.01 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F1A \\sim C207-F2A \\sim C207-F3A with sigma of 0.01 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A with sigma of 0.01 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim C203-F3A with sigma of 0.01 3. Uiso/Uaniso restraints and constraints F1 \\sim F1A \\sim F2 \\sim F2A \\sim F3 \\sim F3A \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A \\sim F7 \\sim F8 \\sim F9 \\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F19A \\sim F20 \\sim F20A \\sim F21 \\sim F21A \\sim F22 \\sim F22A \\sim F23 \\sim F23A \\sim F24 \\sim F24A: within 1.7A with sigma of 0.007 and sigma for terminal atoms of 0.02 Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F19A) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F20A) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F22A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F24A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.02 4. Others Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1) Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1) Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(2) Sof(F22)=Sof(F23)=Sof(F24)=FVAR(2) Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(3) Sof(F19)=Sof(F20)=Sof(F21)=FVAR(3) Fixed Sof: F1(0.5) F1A(0.5) F2(0.5) F2A(0.5) F3(0.5) F3A(0.5) 5.a Secondary CH2 refined with riding coordinates: C12(H12A,H12B), C15(H15A,H15B), C27(H27A,H27B), C30(H30A,H30B) 5.b Aromatic/amide H refined with riding coordinates: C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230) 5.c Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B, H20C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A, H35B,H35C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.18840(2) 0.22150(2) 0.12014(2) 0.02012(4) Uani 1 1 d . . . . . O3 O 0.22052(12) 0.09112(14) 0.17886(7) 0.0470(6) Uani 1 1 d . . . . . O5 O 0.16928(14) 0.32682(16) 0.04903(8) 0.0651(8) Uani 1 1 d . . . . . O13 O 0.43978(10) 0.31598(12) 0.15685(6) 0.0326(5) Uani 1 1 d . . . . . O16 O 0.34485(10) 0.40909(11) 0.21672(6) 0.0275(5) Uani 1 1 d . . . . . O28 O 0.02997(11) 0.00787(12) 0.04270(6) 0.0364(5) Uani 1 1 d . . . . . O31 O -0.06309(10) 0.12518(11) 0.09361(6) 0.0307(5) Uani 1 1 d . . . . . N7 N 0.33413(11) 0.27617(12) 0.13813(7) 0.0225(5) Uani 1 1 d . . . . . N10 N 0.27611(11) 0.33069(12) 0.17629(7) 0.0217(5) Uani 1 1 d . . . . . N22 N 0.09922(11) 0.09936(12) 0.07290(7) 0.0220(5) Uani 1 1 d . . . . . N25 N 0.04192(11) 0.17135(12) 0.10426(6) 0.0196(5) Uani 1 1 d . . . . . C2 C 0.20798(14) 0.14142(17) 0.15818(9) 0.0275(7) Uani 1 1 d . . . . . C4 C 0.17573(16) 0.28961(18) 0.07652(10) 0.0354(8) Uani 1 1 d . . . . . C6 C 0.27080(14) 0.28022(14) 0.14579(8) 0.0223(6) Uani 1 1 d . . . . . C8 C 0.37647(14) 0.32214(15) 0.16305(8) 0.0248(6) Uani 1 1 d . . . . . C9 C 0.33989(14) 0.35699(15) 0.18707(8) 0.0232(6) Uani 1 1 d . . . . . C11 C 0.37087(14) 0.23281(16) 0.11105(9) 0.0288(7) Uani 1 1 d . . . . . C12 C 0.43956(18) 0.2708(2) 0.12249(13) 0.0596(12) Uani 1 1 d . . . . . H12A H 0.4738 0.2304 0.1272 0.072 Uiso 1 1 calc R . . . . H12B H 0.4499 0.3037 0.1006 0.072 Uiso 1 1 calc R . . . . C14 C 0.23114(14) 0.36878(16) 0.20042(8) 0.0258(6) Uani 1 1 d . . . . . C15 C 0.28374(15) 0.40057(18) 0.23348(9) 0.0323(7) Uani 1 1 d . . . . . H15A H 0.2696 0.4509 0.2429 0.039 Uiso 1 1 calc R . . . . H15B H 0.2900 0.3644 0.2560 0.039 Uiso 1 1 calc R . . . . C17 C 0.3715(2) 0.14792(18) 0.12052(11) 0.0477(9) Uani 1 1 d . . . . . H17A H 0.3875 0.1404 0.1485 0.072 Uiso 1 1 calc GR . . . . H17B H 0.4006 0.1210 0.1047 0.072 Uiso 1 1 calc GR . . . . H17C H 0.3268 0.1272 0.1145 0.072 Uiso 1 1 calc GR . . . . C18 C 0.34514(19) 0.2482(2) 0.06868(10) 0.0425(8) Uani 1 1 d . . . . . H18A H 0.3010 0.2261 0.0624 0.064 Uiso 1 1 calc GR . . . . H18B H 0.3745 0.2246 0.0519 0.064 Uiso 1 1 calc GR . . . . H18C H 0.3431 0.3038 0.0641 0.064 Uiso 1 1 calc GR . . . . C19 C 0.18572(16) 0.31169(19) 0.21684(9) 0.0361(7) Uani 1 1 d . . . . . H19A H 0.1537 0.2917 0.1954 0.054 Uiso 1 1 calc GR . . . . H19B H 0.1624 0.3376 0.2361 0.054 Uiso 1 1 calc GR . . . . H19C H 0.2118 0.2690 0.2295 0.054 Uiso 1 1 calc GR . . . . C20 C 0.19354(16) 0.43336(17) 0.17685(10) 0.0354(7) Uani 1 1 d . . . . . H20A H 0.2249 0.4699 0.1681 0.053 Uiso 1 1 calc GR . . . . H20B H 0.1656 0.4601 0.1934 0.053 Uiso 1 1 calc GR . . . . H20C H 0.1660 0.4115 0.1539 0.053 Uiso 1 1 calc GR . . . . C21 C 0.10483(13) 0.16174(14) 0.09725(8) 0.0196(6) Uani 1 1 d . . . . . C23 C 0.03572(14) 0.07099(15) 0.06631(8) 0.0242(6) Uani 1 1 d . . . . . C24 C -0.00068(13) 0.11659(15) 0.08594(8) 0.0233(6) Uani 1 1 d . . . . . C26 C 0.14309(14) 0.04983(16) 0.05295(9) 0.0288(7) Uani 1 1 d . . . . . C27 C 0.08961(16) 0.00931(19) 0.02384(10) 0.0402(8) Uani 1 1 d . . . . . H27A H 0.0817 0.0380 -0.0013 0.048 Uiso 1 1 calc R . . . . H27B H 0.1035 -0.0437 0.0184 0.048 Uiso 1 1 calc R . . . . C29 C 0.00668(14) 0.22142(15) 0.12932(9) 0.0255(6) Uani 1 1 d . . . . . C30 C -0.06442(15) 0.20260(17) 0.10978(10) 0.0330(7) Uani 1 1 d . . . . . H30A H -0.0953 0.2050 0.1295 0.040 Uiso 1 1 calc R . . . . H30B H -0.0790 0.2401 0.0886 0.040 Uiso 1 1 calc R . . . . C32 C 0.1789(2) -0.0056(2) 0.08276(12) 0.0547(11) Uani 1 1 d . . . . . H32A H 0.2102 0.0230 0.1015 0.082 Uiso 1 1 calc GR . . . . H32B H 0.2027 -0.0438 0.0692 0.082 Uiso 1 1 calc GR . . . . H32C H 0.1469 -0.0318 0.0968 0.082 Uiso 1 1 calc GR . . . . C33 C 0.18937(17) 0.0958(2) 0.03144(11) 0.0455(9) Uani 1 1 d . . . . . H33A H 0.1640 0.1324 0.0136 0.068 Uiso 1 1 calc GR . . . . H33B H 0.2135 0.0608 0.0162 0.068 Uiso 1 1 calc GR . . . . H33C H 0.2206 0.1239 0.0505 0.068 Uiso 1 1 calc GR . . . . C34 C 0.01992(17) 0.1941(2) 0.17157(9) 0.0375(8) Uani 1 1 d . . . . . H34A H 0.0065 0.1402 0.1730 0.056 Uiso 1 1 calc GR . . . . H34B H -0.0052 0.2257 0.1878 0.056 Uiso 1 1 calc GR . . . . H34C H 0.0670 0.1988 0.1812 0.056 Uiso 1 1 calc GR . . . . C35 C 0.02326(16) 0.30587(17) 0.12446(10) 0.0365(8) Uani 1 1 d . . . . . H35A H 0.0699 0.3146 0.1343 0.055 Uiso 1 1 calc GR . . . . H35B H -0.0040 0.3376 0.1394 0.055 Uiso 1 1 calc GR . . . . H35C H 0.0146 0.3198 0.0966 0.055 Uiso 1 1 calc GR . . . . F1 F 0.3967(4) 0.9890(4) 0.1600(2) 0.081(3) Uani 0.5 1 d D U P A 1 F1A F 0.3885(4) 0.8863(4) 0.19816(18) 0.072(3) Uani 0.5 1 d D U P A 2 F2 F 0.3260(3) 0.9512(4) 0.19569(19) 0.070(2) Uani 0.5 1 d D U P A 1 F2A F 0.4146(3) 0.9685(4) 0.1580(2) 0.052(2) Uani 0.5 1 d D U P A 2 F3 F 0.4079(3) 0.8829(4) 0.18995(18) 0.056(2) Uani 0.5 1 d D U P A 1 F3A F 0.3275(4) 0.9836(4) 0.1829(2) 0.103(4) Uani 0.5 1 d D U P A 2 F4 F 0.3681(4) 0.9038(4) 0.02079(16) 0.100(3) Uani 0.609(8) 1 d D U P B 1 F4A F 0.2953(5) 0.8163(6) 0.00094(18) 0.092(4) Uani 0.391(8) 1 d D U P B 2 F5 F 0.2658(3) 0.8869(5) 0.00274(12) 0.087(2) Uani 0.609(8) 1 d D U P B 1 F5A F 0.3859(3) 0.8614(6) 0.0267(2) 0.071(3) Uani 0.391(8) 1 d D U P B 2 F6 F 0.3284(3) 0.7929(3) 0.01016(14) 0.0689(17) Uani 0.609(8) 1 d D U P B 1 F6A F 0.3065(6) 0.9353(4) 0.0142(2) 0.088(3) Uani 0.391(8) 1 d D U P B 2 F7 F 0.43318(8) 0.56155(10) 0.22969(5) 0.0387(5) Uani 1 1 d . U . . . F8 F 0.40245(9) 0.67946(10) 0.23214(5) 0.0390(4) Uani 1 1 d . U . . . F9 F 0.34378(9) 0.59034(11) 0.25260(5) 0.0430(5) Uani 1 1 d . U . . . F10 F 0.39249(9) 0.45746(10) 0.09705(5) 0.0409(5) Uani 1 1 d . U . . . F11 F 0.28949(10) 0.42969(10) 0.08798(6) 0.0495(5) Uani 1 1 d . U . . . F12 F 0.32679(10) 0.51885(10) 0.05379(5) 0.0405(5) Uani 1 1 d . U . . . F13 F 0.01378(10) 0.93576(10) 0.20800(6) 0.0438(5) Uani 1 1 d . U . . . F14 F 0.10696(9) 0.97676(10) 0.19452(6) 0.0485(5) Uani 1 1 d . U . . . F15 F 0.03326(9) 0.94029(9) 0.14816(5) 0.0357(4) Uani 1 1 d . U . . . F16 F 0.05837(9) 0.69444(11) 0.27866(5) 0.0400(4) Uani 1 1 d . U . . . F17 F 0.15970(10) 0.66446(13) 0.27953(6) 0.0549(6) Uani 1 1 d . U . . . F18 F 0.08441(12) 0.60016(11) 0.24385(6) 0.0575(6) Uani 1 1 d . U . . . F19 F -0.0097(6) 0.8360(4) 0.0272(2) 0.058(2) Uani 0.55(3) 1 d D U P C 1 F19A F -0.0153(10) 0.7418(6) -0.0223(3) 0.076(4) Uani 0.45(3) 1 d D U P C 2 F20 F -0.0332(5) 0.7483(5) -0.0149(3) 0.068(3) Uani 0.55(3) 1 d D U P C 1 F20A F 0.0579(4) 0.8234(8) -0.0031(4) 0.051(3) Uani 0.45(3) 1 d D U P C 2 F21 F 0.0576(4) 0.8075(7) -0.0113(3) 0.062(3) Uani 0.55(3) 1 d D U P C 1 F21A F -0.0291(9) 0.8196(10) 0.0230(4) 0.080(4) Uani 0.45(3) 1 d D U P C 2 F22 F -0.03435(16) 0.5086(2) 0.0587(2) 0.0739(17) Uani 0.685(8) 1 d D U P D 1 F22A F 0.0785(3) 0.4633(3) 0.0770(4) 0.065(3) Uani 0.315(8) 1 d D U P D 2 F23 F 0.0574(3) 0.4662(2) 0.0486(2) 0.097(2) Uani 0.685(8) 1 d D U P D 1 F23A F -0.0050(7) 0.5026(4) 0.0983(4) 0.082(4) Uani 0.315(8) 1 d D U P D 2 F24 F 0.0383(4) 0.4864(3) 0.10623(13) 0.100(2) Uani 0.685(8) 1 d D U P D 1 F24A F -0.0056(7) 0.4894(5) 0.0377(3) 0.087(4) Uani 0.315(8) 1 d D U P D 2 C201 C 0.24255(13) 0.78931(13) 0.11375(8) 0.0187(6) Uani 1 1 d . . . . . C202 C 0.27773(13) 0.83534(14) 0.14303(8) 0.0221(6) Uani 1 1 d . . . . . H202 H 0.2681 0.8311 0.1692 0.027 Uiso 1 1 calc R . . . . C203 C 0.32599(13) 0.88681(15) 0.13529(8) 0.0252(6) Uani 1 1 d D . . . . C204 C 0.34063(14) 0.89639(16) 0.09764(9) 0.0264(6) Uani 1 1 d . . . . . H204 H 0.3735 0.9318 0.0922 0.032 Uiso 1 1 calc R . . . . C205 C 0.30582(13) 0.85255(15) 0.06781(8) 0.0253(6) Uani 1 1 d D . . . . C206 C 0.25869(13) 0.79969(15) 0.07584(8) 0.0219(6) Uani 1 1 d . . . . . H206 H 0.2367 0.7696 0.0549 0.026 Uiso 1 1 calc R . . . . C207 C 0.36369(15) 0.92964(16) 0.16896(10) 0.0381(8) Uani 1 1 d D . . . . C208 C 0.31949(16) 0.86286(18) 0.02665(10) 0.0439(9) Uani 1 1 d D . . . . C209 C 0.24973(13) 0.65114(14) 0.13833(8) 0.0185(5) Uani 1 1 d . . . . . C210 C 0.28931(13) 0.65101(14) 0.17500(8) 0.0209(6) Uani 1 1 d . . . . . H210 H 0.2798 0.6868 0.1943 0.025 Uiso 1 1 calc R . . . . C211 C 0.34192(13) 0.60070(15) 0.18427(8) 0.0200(6) Uani 1 1 d . . . . . C212 C 0.35774(13) 0.54737(15) 0.15709(8) 0.0217(6) Uani 1 1 d . . . . . H212 H 0.3935 0.5128 0.1632 0.026 Uiso 1 1 calc R . . . . C213 C 0.31909(13) 0.54651(14) 0.12038(8) 0.0207(6) Uani 1 1 d . . . . . C214 C 0.26695(13) 0.59710(14) 0.11125(8) 0.0201(6) Uani 1 1 d . . . . . H214 H 0.2421 0.5951 0.0858 0.024 Uiso 1 1 calc R . . . . C215 C 0.38071(14) 0.60696(16) 0.22438(8) 0.0270(6) Uani 1 1 d . . . . . C216 C 0.33252(15) 0.48921(16) 0.09006(9) 0.0284(7) Uani 1 1 d . . . . . C217 C 0.15714(12) 0.74662(15) 0.16217(8) 0.0185(5) Uani 1 1 d . . . . . C218 C 0.12665(13) 0.81960(14) 0.16097(8) 0.0208(6) Uani 1 1 d . . . . . H218 H 0.1328 0.8536 0.1401 0.025 Uiso 1 1 calc R . . . . C219 C 0.08844(13) 0.84376(15) 0.18856(8) 0.0218(6) Uani 1 1 d . . . . . C220 C 0.07893(14) 0.79647(16) 0.21998(8) 0.0240(6) Uani 1 1 d . . . . . H220 H 0.0533 0.8132 0.2394 0.029 Uiso 1 1 calc R . . . . C221 C 0.10802(13) 0.72416(15) 0.22209(8) 0.0231(6) Uani 1 1 d . . . . . C222 C 0.14566(13) 0.70019(15) 0.19371(8) 0.0212(6) Uani 1 1 d . . . . . H222 H 0.1644 0.6501 0.1958 0.025 Uiso 1 1 calc R . . . . C223 C 0.05998(15) 0.92355(16) 0.18509(9) 0.0284(7) Uani 1 1 d . . . . . C224 C 0.10181(15) 0.67120(18) 0.25549(9) 0.0320(7) Uani 1 1 d . . . . . C225 C 0.13609(13) 0.69235(15) 0.09234(7) 0.0185(5) Uani 1 1 d . . . . . C226 C 0.10258(13) 0.74199(15) 0.06470(8) 0.0203(6) Uani 1 1 d . . . . . H226 H 0.1180 0.7933 0.0632 0.024 Uiso 1 1 calc R . . . . C227 C 0.04734(13) 0.71923(15) 0.03910(8) 0.0220(6) Uani 1 1 d D . . . . C228 C 0.02277(14) 0.64528(16) 0.04032(8) 0.0264(6) Uani 1 1 d . . . . . H228 H -0.0148 0.6295 0.0227 0.032 Uiso 1 1 calc R . . . . C229 C 0.05446(14) 0.59495(15) 0.06787(8) 0.0275(6) Uani 1 1 d D . . . . C230 C 0.10955(14) 0.61798(15) 0.09323(8) 0.0239(6) Uani 1 1 d . . . . . H230 H 0.1301 0.5821 0.1119 0.029 Uiso 1 1 calc R . . . . C231 C 0.01554(14) 0.77585(16) 0.00966(9) 0.0332(7) Uani 1 1 d D . . . . C232 C 0.02994(15) 0.51428(18) 0.07001(10) 0.0429(9) Uani 1 1 d D . . . . B200 B 0.19570(15) 0.71954(16) 0.12637(9) 0.0183(6) 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 0.01449(6) 0.02259(6) 0.02289(6) -0.00450(4) 0.00120(4) -0.00230(4) O3 0.0458(15) 0.0513(14) 0.0412(14) 0.0135(12) -0.0037(12) -0.0078(12) O5 0.0615(19) 0.0685(18) 0.0586(18) 0.0311(15) -0.0154(15) -0.0209(15) O13 0.0163(11) 0.0413(12) 0.0399(13) -0.0047(10) 0.0032(9) -0.0058(9) O16 0.0251(11) 0.0297(10) 0.0268(11) -0.0079(8) -0.0002(9) -0.0067(8) O28 0.0317(13) 0.0363(12) 0.0407(13) -0.0168(10) 0.0033(10) -0.0131(10) O31 0.0175(10) 0.0376(11) 0.0377(12) -0.0044(9) 0.0062(9) -0.0073(9) N7 0.0166(12) 0.0265(12) 0.0241(12) -0.0043(10) 0.0026(10) -0.0016(10) N10 0.0155(11) 0.0248(11) 0.0242(12) -0.0031(9) 0.0008(10) -0.0021(9) N22 0.0174(12) 0.0221(11) 0.0257(13) -0.0047(9) -0.0001(10) 0.0010(9) N25 0.0169(12) 0.0194(11) 0.0224(12) -0.0023(9) 0.0021(9) -0.0024(9) C2 0.0198(15) 0.0360(16) 0.0256(16) -0.0057(13) -0.0007(12) -0.0093(12) C4 0.0267(17) 0.0373(18) 0.0391(19) 0.0010(15) -0.0058(15) -0.0119(14) C6 0.0210(14) 0.0211(13) 0.0247(14) -0.0011(11) 0.0023(12) -0.0037(11) C8 0.0175(14) 0.0264(14) 0.0299(16) -0.0014(12) 0.0009(12) -0.0051(11) C9 0.0185(14) 0.0254(14) 0.0239(15) -0.0005(11) -0.0037(12) -0.0068(11) C11 0.0194(15) 0.0345(17) 0.0337(17) -0.0054(13) 0.0073(13) -0.0007(12) C12 0.0268(19) 0.088(3) 0.067(3) -0.040(2) 0.0152(19) -0.0136(19) C14 0.0226(15) 0.0291(15) 0.0258(15) -0.0060(12) 0.0039(12) -0.0043(12) C15 0.0275(17) 0.0386(17) 0.0299(17) -0.0093(13) 0.0004(14) -0.0046(14) C17 0.061(3) 0.0362(18) 0.051(2) 0.0055(16) 0.0261(19) 0.0165(17) C18 0.051(2) 0.0470(19) 0.0324(18) -0.0007(15) 0.0165(17) 0.0118(17) C19 0.0356(19) 0.0434(18) 0.0321(18) -0.0085(14) 0.0150(15) -0.0083(15) C20 0.0291(17) 0.0354(17) 0.0413(19) -0.0049(14) 0.0031(15) 0.0065(14) C21 0.0176(14) 0.0185(12) 0.0216(14) 0.0012(10) -0.0010(11) -0.0005(11) C23 0.0206(15) 0.0237(14) 0.0264(15) -0.0033(11) -0.0030(12) -0.0066(11) C24 0.0163(14) 0.0269(14) 0.0255(15) 0.0037(11) -0.0013(12) -0.0055(11) C26 0.0233(16) 0.0291(15) 0.0332(17) -0.0110(13) 0.0013(13) 0.0040(12) C27 0.0313(19) 0.0427(19) 0.046(2) -0.0231(15) 0.0047(16) -0.0070(15) C29 0.0189(14) 0.0276(14) 0.0312(16) -0.0015(12) 0.0080(12) -0.0018(12) C30 0.0189(15) 0.0382(17) 0.0429(19) 0.0014(14) 0.0077(14) 0.0005(13) C32 0.059(3) 0.044(2) 0.058(3) -0.0068(18) 0.000(2) 0.0283(19) C33 0.039(2) 0.052(2) 0.048(2) -0.0247(17) 0.0174(17) -0.0096(16) C34 0.0329(19) 0.0518(19) 0.0296(17) -0.0023(15) 0.0108(15) -0.0058(15) C35 0.0311(18) 0.0259(15) 0.055(2) -0.0063(14) 0.0134(16) 0.0024(13) F1 0.125(8) 0.049(4) 0.060(4) 0.010(3) -0.015(4) -0.056(5) F1A 0.103(7) 0.071(5) 0.033(3) 0.014(3) -0.020(4) -0.054(4) F2 0.049(4) 0.088(5) 0.073(4) -0.061(4) 0.009(3) -0.017(3) F2A 0.036(3) 0.057(4) 0.062(4) -0.014(3) 0.001(2) -0.029(3) F3 0.046(3) 0.073(4) 0.043(4) -0.009(3) -0.016(3) 0.013(3) F3A 0.054(4) 0.103(6) 0.151(8) -0.100(6) 0.008(5) -0.005(4) F4 0.120(5) 0.136(6) 0.050(3) -0.015(4) 0.040(4) -0.101(5) F4A 0.115(7) 0.136(7) 0.028(4) -0.016(5) 0.018(5) -0.100(6) F5 0.080(4) 0.146(5) 0.036(2) 0.042(3) 0.016(2) 0.030(4) F5A 0.057(4) 0.104(7) 0.063(5) 0.005(4) 0.046(3) -0.006(4) F6 0.090(4) 0.086(3) 0.035(3) -0.011(2) 0.026(3) 0.007(3) F6A 0.132(8) 0.084(5) 0.063(5) 0.042(4) 0.060(5) 0.043(5) F7 0.0260(10) 0.0508(11) 0.0355(10) 0.0005(8) -0.0088(8) 0.0158(8) F8 0.0410(11) 0.0371(10) 0.0352(10) -0.0061(8) -0.0080(9) -0.0014(8) F9 0.0336(11) 0.0721(13) 0.0234(9) 0.0123(9) 0.0044(8) 0.0063(9) F10 0.0341(11) 0.0432(10) 0.0448(11) -0.0126(8) 0.0036(9) 0.0188(8) F11 0.0480(13) 0.0303(10) 0.0723(15) -0.0213(9) 0.0158(11) -0.0098(9) F12 0.0526(13) 0.0434(10) 0.0259(10) -0.0091(8) 0.0064(9) 0.0141(9) F13 0.0419(12) 0.0425(10) 0.0505(12) -0.0073(9) 0.0188(10) 0.0181(9) F14 0.0379(11) 0.0285(9) 0.0755(15) -0.0142(9) -0.0045(10) -0.0050(8) F15 0.0352(10) 0.0303(9) 0.0403(11) 0.0041(8) 0.0008(8) 0.0108(8) F16 0.0330(11) 0.0610(12) 0.0292(10) 0.0061(8) 0.0155(8) 0.0011(9) F17 0.0336(11) 0.0898(16) 0.0413(12) 0.0324(11) 0.0047(9) 0.0141(11) F18 0.0936(18) 0.0360(11) 0.0498(13) 0.0064(9) 0.0342(12) -0.0105(11) F19 0.069(5) 0.041(3) 0.056(3) 0.003(3) -0.013(3) 0.025(3) F19A 0.118(8) 0.058(4) 0.034(4) 0.010(3) -0.048(5) -0.021(5) F20 0.053(4) 0.057(4) 0.077(5) 0.023(3) -0.047(3) -0.016(3) F20A 0.050(5) 0.046(4) 0.047(5) 0.028(4) -0.026(3) -0.026(3) F21 0.046(4) 0.091(6) 0.048(4) 0.040(4) 0.008(3) 0.009(4) F21A 0.065(6) 0.111(7) 0.070(6) 0.047(5) 0.025(5) 0.059(6) F22 0.040(2) 0.050(2) 0.128(5) 0.012(3) 0.000(3) -0.0244(17) F22A 0.049(5) 0.011(3) 0.136(9) -0.001(4) 0.018(6) -0.008(3) F23 0.108(5) 0.039(2) 0.158(6) -0.044(3) 0.062(4) -0.023(2) F23A 0.095(8) 0.048(4) 0.123(8) 0.007(5) 0.081(6) -0.023(5) F24 0.140(5) 0.060(3) 0.086(3) 0.039(2) -0.034(4) -0.062(3) F24A 0.111(8) 0.050(5) 0.086(6) 0.000(4) -0.037(6) -0.044(6) C201 0.0155(13) 0.0176(13) 0.0222(14) 0.0018(10) 0.0001(11) 0.0058(10) C202 0.0224(15) 0.0207(13) 0.0231(14) 0.0001(11) 0.0031(12) 0.0024(11) C203 0.0211(15) 0.0227(14) 0.0303(16) -0.0010(12) -0.0016(13) 0.0045(11) C204 0.0178(14) 0.0265(14) 0.0359(17) 0.0018(12) 0.0066(13) -0.0013(12) C205 0.0191(15) 0.0308(15) 0.0275(16) 0.0035(12) 0.0091(12) 0.0029(12) C206 0.0177(14) 0.0240(13) 0.0238(15) -0.0020(11) 0.0023(12) 0.0038(11) C207 0.0336(19) 0.0360(18) 0.044(2) -0.0054(15) 0.0025(16) -0.0093(15) C208 0.040(2) 0.057(2) 0.039(2) 0.0061(17) 0.0197(17) -0.0027(18) C209 0.0165(13) 0.0206(13) 0.0187(13) 0.0031(10) 0.0032(11) 0.0007(10) C210 0.0204(14) 0.0212(13) 0.0216(14) 0.0002(11) 0.0043(11) 0.0026(11) C211 0.0169(14) 0.0227(13) 0.0201(14) 0.0050(11) 0.0018(11) -0.0003(11) C212 0.0154(14) 0.0214(13) 0.0291(15) 0.0057(11) 0.0053(12) 0.0037(11) C213 0.0207(14) 0.0175(12) 0.0244(14) 0.0003(11) 0.0051(12) -0.0010(11) C214 0.0199(14) 0.0208(13) 0.0191(14) 0.0003(10) 0.0013(11) -0.0018(11) C215 0.0226(15) 0.0321(15) 0.0260(16) 0.0039(12) 0.0026(13) 0.0064(12) C216 0.0266(16) 0.0253(15) 0.0329(17) -0.0048(12) 0.0024(13) 0.0035(12) C217 0.0131(13) 0.0225(12) 0.0186(14) -0.0014(10) -0.0025(11) -0.0017(10) C218 0.0165(14) 0.0224(14) 0.0224(14) -0.0001(11) -0.0014(11) 0.0010(11) C219 0.0144(13) 0.0258(14) 0.0240(15) -0.0068(11) -0.0013(11) -0.0004(11) C220 0.0172(14) 0.0329(15) 0.0218(15) -0.0063(11) 0.0024(12) -0.0004(11) C221 0.0159(13) 0.0314(15) 0.0219(14) 0.0010(12) 0.0022(11) -0.0011(12) C222 0.0177(14) 0.0228(13) 0.0223(14) -0.0009(11) -0.0003(11) 0.0028(11) C223 0.0227(16) 0.0266(15) 0.0356(18) -0.0079(13) 0.0032(14) 0.0007(12) C224 0.0266(17) 0.0410(18) 0.0297(17) 0.0035(13) 0.0087(14) 0.0001(14) C225 0.0168(14) 0.0235(13) 0.0159(13) 0.0000(10) 0.0048(11) 0.0003(11) C226 0.0177(14) 0.0194(13) 0.0240(15) 0.0000(11) 0.0040(12) -0.0010(11) C227 0.0179(14) 0.0291(14) 0.0189(14) 0.0017(11) 0.0023(11) 0.0016(11) C228 0.0205(15) 0.0341(16) 0.0237(15) -0.0024(12) 0.0002(12) -0.0035(12) C229 0.0249(16) 0.0254(14) 0.0330(17) -0.0018(12) 0.0066(13) -0.0050(12) C230 0.0245(15) 0.0224(13) 0.0246(15) 0.0039(11) 0.0025(12) 0.0026(11) C231 0.0273(17) 0.0390(18) 0.0306(17) 0.0049(14) -0.0057(14) -0.0014(14) C232 0.038(2) 0.0303(17) 0.058(2) 0.0019(16) -0.0042(18) -0.0109(15) B200 0.0180(15) 0.0173(14) 0.0194(15) 0.0009(11) 0.0018(12) 0.0021(12) _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 C2 1.913(3) . ? Ir1 C4 1.899(3) . ? Ir1 C6 2.064(3) . ? Ir1 C21 2.064(2) . ? O3 C2 1.133(3) . ? O5 C4 1.137(4) . ? O13 C8 1.349(3) . ? O13 C12 1.417(4) . ? O16 C9 1.356(3) . ? O16 C15 1.459(4) . ? O28 C23 1.359(3) . ? O28 C27 1.463(4) . ? O31 C24 1.351(3) . ? O31 C30 1.457(4) . ? N7 C6 1.363(4) . ? N7 C8 1.385(3) . ? N7 C11 1.482(4) . ? N10 C6 1.359(3) . ? N10 C9 1.387(3) . ? N10 C14 1.480(4) . ? N22 C21 1.364(3) . ? N22 C23 1.382(3) . ? N22 C26 1.481(4) . ? N25 C21 1.356(3) . ? N25 C24 1.382(3) . ? N25 C29 1.482(4) . ? C8 C9 1.336(4) . ? C11 C12 1.556(4) . ? C11 C17 1.510(4) . ? C11 C18 1.501(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C15 1.555(4) . ? C14 C19 1.522(4) . ? C14 C20 1.528(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C23 C24 1.335(4) . ? C26 C27 1.547(4) . ? C26 C32 1.518(4) . ? C26 C33 1.511(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C29 C30 1.553(4) . ? C29 C34 1.515(4) . ? C29 C35 1.520(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? F1 C207 1.294(5) . ? F1A C207 1.300(5) . ? F2 C207 1.334(5) . ? F2A C207 1.342(5) . ? F3 C207 1.349(5) . ? F3A C207 1.326(5) . ? F4 C208 1.263(4) . ? F4A C208 1.248(5) . ? F5 C208 1.346(4) . ? F5A C208 1.362(5) . ? F6 C208 1.363(4) . ? F6A C208 1.343(5) . ? F7 C215 1.326(3) . ? F8 C215 1.350(3) . ? F9 C215 1.343(3) . ? F10 C216 1.339(3) . ? F11 C216 1.355(3) . ? F12 C216 1.338(3) . ? F13 C223 1.331(4) . ? F14 C223 1.342(3) . ? F15 C223 1.342(3) . ? F16 C224 1.338(4) . ? F17 C224 1.354(3) . ? F18 C224 1.331(4) . ? F19 C231 1.344(5) . ? F19A C231 1.328(6) . ? F20 C231 1.305(5) . ? F20A C231 1.318(5) . ? F21 C231 1.319(5) . ? F21A C231 1.320(6) . ? F22 C232 1.326(4) . ? F22A C232 1.330(5) . ? F23 C232 1.292(4) . ? F23A C232 1.302(5) . ? F24 C232 1.324(4) . ? F24A C232 1.312(5) . ? C201 C202 1.403(4) . ? C201 C206 1.400(4) . ? C201 B200 1.642(4) . ? C202 H202 0.9500 . ? C202 C203 1.387(4) . ? C203 C204 1.379(4) . ? C203 C207 1.497(4) . ? C204 H204 0.9500 . ? C204 C205 1.392(4) . ? C205 C206 1.389(4) . ? C205 C208 1.491(4) . ? C206 H206 0.9500 . ? C209 C210 1.400(4) . ? C209 C214 1.401(4) . ? C209 B200 1.638(4) . ? C210 H210 0.9500 . ? C210 C211 1.391(4) . ? C211 C212 1.386(4) . ? C211 C215 1.496(4) . ? C212 H212 0.9500 . ? C212 C213 1.393(4) . ? C213 C214 1.386(4) . ? C213 C216 1.494(4) . ? C214 H214 0.9500 . ? C217 C218 1.412(4) . ? C217 C222 1.397(4) . ? C217 B200 1.623(4) . ? C218 H218 0.9500 . ? C218 C219 1.378(4) . ? C219 C220 1.392(4) . ? C219 C223 1.502(4) . ? C220 H220 0.9500 . ? C220 C221 1.388(4) . ? C221 C222 1.390(4) . ? C221 C224 1.490(4) . ? C222 H222 0.9500 . ? C225 C226 1.392(4) . ? C225 C230 1.404(4) . ? C225 B200 1.639(4) . ? C226 H226 0.9500 . ? C226 C227 1.391(4) . ? C227 C228 1.383(4) . ? C227 C231 1.494(4) . ? C228 H228 0.9500 . ? C228 C229 1.383(4) . ? C229 C230 1.386(4) . ? C229 C232 1.494(4) . ? C230 H230 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 C2 Ir1 C6 89.22(11) . . ? C2 Ir1 C21 88.77(10) . . ? C4 Ir1 C2 170.13(14) . . ? C4 Ir1 C6 92.45(11) . . ? C4 Ir1 C21 89.87(11) . . ? C6 Ir1 C21 177.15(11) . . ? C8 O13 C12 106.5(2) . . ? C9 O16 C15 104.5(2) . . ? C23 O28 C27 104.0(2) . . ? C24 O31 C30 104.2(2) . . ? C6 N7 C8 112.5(2) . . ? C6 N7 C11 136.8(2) . . ? C8 N7 C11 110.6(2) . . ? C6 N10 C9 112.9(2) . . ? C6 N10 C14 137.0(2) . . ? C9 N10 C14 110.0(2) . . ? C21 N22 C23 112.4(2) . . ? C21 N22 C26 137.8(2) . . ? C23 N22 C26 109.7(2) . . ? C21 N25 C24 113.0(2) . . ? C21 N25 C29 136.8(2) . . ? C24 N25 C29 109.9(2) . . ? O3 C2 Ir1 175.7(3) . . ? O5 C4 Ir1 175.8(3) . . ? N7 C6 Ir1 129.64(19) . . ? N10 C6 Ir1 128.4(2) . . ? N10 C6 N7 101.9(2) . . ? O13 C8 N7 113.0(2) . . ? C9 C8 O13 140.3(3) . . ? C9 C8 N7 106.6(2) . . ? O16 C9 N10 112.9(2) . . ? C8 C9 O16 141.0(3) . . ? C8 C9 N10 106.1(2) . . ? N7 C11 C12 98.5(2) . . ? N7 C11 C17 110.5(3) . . ? N7 C11 C18 112.2(2) . . ? C17 C11 C12 112.3(3) . . ? C18 C11 C12 110.7(3) . . ? C18 C11 C17 111.9(3) . . ? O13 C12 C11 110.0(3) . . ? O13 C12 H12A 109.7 . . ? O13 C12 H12B 109.7 . . ? C11 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N10 C14 C15 98.3(2) . . ? N10 C14 C19 112.2(2) . . ? N10 C14 C20 109.8(2) . . ? C19 C14 C15 111.0(2) . . ? C19 C14 C20 112.6(3) . . ? C20 C14 C15 111.9(2) . . ? O16 C15 C14 107.1(2) . . ? O16 C15 H15A 110.3 . . ? O16 C15 H15B 110.3 . . ? C14 C15 H15A 110.3 . . ? C14 C15 H15B 110.3 . . ? H15A C15 H15B 108.5 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N22 C21 Ir1 128.9(2) . . ? N25 C21 Ir1 129.13(19) . . ? N25 C21 N22 101.9(2) . . ? O28 C23 N22 112.8(2) . . ? C24 C23 O28 140.6(3) . . ? C24 C23 N22 106.7(2) . . ? O31 C24 N25 113.0(2) . . ? C23 C24 O31 141.0(3) . . ? C23 C24 N25 106.0(2) . . ? N22 C26 C27 98.1(2) . . ? N22 C26 C32 108.9(3) . . ? N22 C26 C33 112.6(2) . . ? C32 C26 C27 112.3(3) . . ? C33 C26 C27 111.2(3) . . ? C33 C26 C32 112.8(3) . . ? O28 C27 C26 106.4(2) . . ? O28 C27 H27A 110.4 . . ? O28 C27 H27B 110.4 . . ? C26 C27 H27A 110.4 . . ? C26 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? N25 C29 C30 97.5(2) . . ? N25 C29 C34 109.7(2) . . ? N25 C29 C35 111.6(2) . . ? C34 C29 C30 112.3(2) . . ? C34 C29 C35 113.2(3) . . ? C35 C29 C30 111.5(2) . . ? O31 C30 C29 107.0(2) . . ? O31 C30 H30A 110.3 . . ? O31 C30 H30B 110.3 . . ? C29 C30 H30A 110.3 . . ? C29 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 H33A 109.5 . . ? C26 C33 H33B 109.5 . . ? C26 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C29 C35 H35A 109.5 . . ? C29 C35 H35B 109.5 . . ? C29 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C202 C201 B200 119.5(2) . . ? C206 C201 C202 115.4(2) . . ? C206 C201 B200 124.3(2) . . ? C201 C202 H202 118.7 . . ? C203 C202 C201 122.6(3) . . ? C203 C202 H202 118.7 . . ? C202 C203 C207 118.5(3) . . ? C204 C203 C202 120.9(3) . . ? C204 C203 C207 120.6(3) . . ? C203 C204 H204 121.0 . . ? C203 C204 C205 117.9(3) . . ? C205 C204 H204 121.0 . . ? C204 C205 C208 119.2(3) . . ? C206 C205 C204 121.0(3) . . ? C206 C205 C208 119.8(3) . . ? C201 C206 H206 118.9 . . ? C205 C206 C201 122.1(3) . . ? C205 C206 H206 118.9 . . ? F1 C207 F2 108.2(4) . . ? F1 C207 F3 105.8(4) . . ? F1 C207 C203 116.3(4) . . ? F1A C207 F2A 105.8(4) . . ? F1A C207 F3A 108.1(5) . . ? F1A C207 C203 114.4(4) . . ? F2 C207 F3 102.2(4) . . ? F2 C207 C203 112.7(4) . . ? F2A C207 C203 111.8(4) . . ? F3 C207 C203 110.5(4) . . ? F3A C207 F2A 104.1(4) . . ? F3A C207 C203 112.0(4) . . ? F4 C208 F5 108.9(4) . . ? F4 C208 F6 106.3(4) . . ? F4 C208 C205 118.4(3) . . ? F4A C208 F5A 106.7(5) . . ? F4A C208 F6A 109.9(5) . . ? F4A C208 C205 119.0(4) . . ? F5 C208 F6 99.7(4) . . ? F5 C208 C205 111.7(3) . . ? F5A C208 C205 108.5(4) . . ? F6 C208 C205 109.9(3) . . ? F6A C208 F5A 99.9(4) . . ? F6A C208 C205 111.1(4) . . ? C210 C209 C214 115.4(2) . . ? C210 C209 B200 120.9(2) . . ? C214 C209 B200 123.0(2) . . ? C209 C210 H210 118.6 . . ? C211 C210 C209 122.8(2) . . ? C211 C210 H210 118.6 . . ? C210 C211 C215 117.5(2) . . ? C212 C211 C210 120.9(2) . . ? C212 C211 C215 121.7(2) . . ? C211 C212 H212 121.3 . . ? C211 C212 C213 117.4(2) . . ? C213 C212 H212 121.3 . . ? C212 C213 C216 120.1(2) . . ? C214 C213 C212 121.4(2) . . ? C214 C213 C216 118.5(2) . . ? C209 C214 H214 118.9 . . ? C213 C214 C209 122.2(2) . . ? C213 C214 H214 118.9 . . ? F7 C215 F8 106.8(2) . . ? F7 C215 F9 107.6(2) . . ? F7 C215 C211 113.6(2) . . ? F8 C215 C211 111.6(2) . . ? F9 C215 F8 105.2(2) . . ? F9 C215 C211 111.6(2) . . ? F10 C216 F11 105.7(2) . . ? F10 C216 C213 113.8(2) . . ? F11 C216 C213 111.3(3) . . ? F12 C216 F10 106.5(2) . . ? F12 C216 F11 105.8(2) . . ? F12 C216 C213 113.1(2) . . ? C218 C217 B200 119.9(2) . . ? C222 C217 C218 114.8(3) . . ? C222 C217 B200 125.0(2) . . ? C217 C218 H218 118.5 . . ? C219 C218 C217 123.1(3) . . ? C219 C218 H218 118.5 . . ? C218 C219 C220 120.6(2) . . ? C218 C219 C223 118.6(3) . . ? C220 C219 C223 120.7(3) . . ? C219 C220 H220 121.0 . . ? C221 C220 C219 118.0(3) . . ? C221 C220 H220 121.0 . . ? C220 C221 C222 120.7(3) . . ? C220 C221 C224 121.1(3) . . ? C222 C221 C224 118.1(3) . . ? C217 C222 H222 118.6 . . ? C221 C222 C217 122.8(2) . . ? C221 C222 H222 118.6 . . ? F13 C223 F14 107.1(2) . . ? F13 C223 F15 107.1(2) . . ? F13 C223 C219 113.6(3) . . ? F14 C223 C219 111.0(2) . . ? F15 C223 F14 105.3(2) . . ? F15 C223 C219 112.2(2) . . ? F16 C224 F17 105.3(2) . . ? F16 C224 C221 114.1(3) . . ? F17 C224 C221 111.2(2) . . ? F18 C224 F16 106.6(2) . . ? F18 C224 F17 106.2(3) . . ? F18 C224 C221 112.9(3) . . ? C226 C225 C230 115.4(2) . . ? C226 C225 B200 123.8(2) . . ? C230 C225 B200 120.2(2) . . ? C225 C226 H226 118.8 . . ? C225 C226 C227 122.4(2) . . ? C227 C226 H226 118.8 . . ? C226 C227 C231 118.7(2) . . ? C228 C227 C226 120.9(2) . . ? C228 C227 C231 120.4(2) . . ? C227 C228 H228 121.0 . . ? C229 C228 C227 118.0(3) . . ? C229 C228 H228 121.0 . . ? C228 C229 C230 120.8(3) . . ? C228 C229 C232 119.8(2) . . ? C230 C229 C232 119.4(2) . . ? C225 C230 H230 118.8 . . ? C229 C230 C225 122.4(2) . . ? C229 C230 H230 118.8 . . ? F19 C231 C227 111.6(4) . . ? F19A C231 C227 112.3(5) . . ? F20 C231 F19 105.4(4) . . ? F20 C231 F21 107.5(5) . . ? F20 C231 C227 114.7(4) . . ? F20A C231 F19A 105.3(5) . . ? F20A C231 F21A 106.0(5) . . ? F20A C231 C227 113.1(4) . . ? F21 C231 F19 104.0(4) . . ? F21 C231 C227 112.7(4) . . ? F21A C231 F19A 105.6(5) . . ? F21A C231 C227 113.8(5) . . ? F22 C232 C229 112.5(3) . . ? F22A C232 C229 112.6(4) . . ? F23 C232 F22 106.3(3) . . ? F23 C232 F24 106.8(4) . . ? F23 C232 C229 113.7(3) . . ? F23A C232 F22A 103.8(5) . . ? F23A C232 F24A 106.3(5) . . ? F23A C232 C229 114.0(4) . . ? F24 C232 F22 103.9(4) . . ? F24 C232 C229 112.9(3) . . ? F24A C232 F22A 104.4(5) . . ? F24A C232 C229 114.7(4) . . ? C209 B200 C201 101.6(2) . . ? C209 B200 C225 112.4(2) . . ? C217 B200 C201 110.6(2) . . ? C217 B200 C209 113.9(2) . . ? C217 B200 C225 103.3(2) . . ? C225 B200 C201 115.5(2) . . ? 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 O13 C8 C9 O16 5.9(7) . . . . ? O13 C8 C9 N10 -176.2(3) . . . . ? O28 C23 C24 O31 0.8(7) . . . . ? O28 C23 C24 N25 179.7(3) . . . . ? N7 C8 C9 O16 -177.4(3) . . . . ? N7 C8 C9 N10 0.5(3) . . . . ? N7 C11 C12 O13 10.9(4) . . . . ? N10 C14 C15 O16 25.1(3) . . . . ? N22 C23 C24 O31 -179.4(3) . . . . ? N22 C23 C24 N25 -0.4(3) . . . . ? N22 C26 C27 O28 -28.4(3) . . . . ? N25 C29 C30 O31 27.8(3) . . . . ? C6 N7 C8 O13 177.3(2) . . . . ? C6 N7 C8 C9 -0.4(3) . . . . ? C6 N7 C11 C12 176.9(3) . . . . ? C6 N7 C11 C17 -65.3(4) . . . . ? C6 N7 C11 C18 60.4(4) . . . . ? C6 N10 C9 O16 178.1(2) . . . . ? C6 N10 C9 C8 -0.4(3) . . . . ? C6 N10 C14 C15 167.7(3) . . . . ? C6 N10 C14 C19 50.9(4) . . . . ? C6 N10 C14 C20 -75.2(4) . . . . ? C8 O13 C12 C11 -11.8(4) . . . . ? C8 N7 C6 Ir1 -177.0(2) . . . . ? C8 N7 C6 N10 0.2(3) . . . . ? C8 N7 C11 C12 -6.3(3) . . . . ? C8 N7 C11 C17 111.5(3) . . . . ? C8 N7 C11 C18 -122.8(3) . . . . ? C9 O16 C15 C14 -26.0(3) . . . . ? C9 N10 C6 Ir1 177.38(19) . . . . ? C9 N10 C6 N7 0.1(3) . . . . ? C9 N10 C14 C15 -15.9(3) . . . . ? C9 N10 C14 C19 -132.7(2) . . . . ? C9 N10 C14 C20 101.2(3) . . . . ? C11 N7 C6 Ir1 -0.2(5) . . . . ? C11 N7 C6 N10 177.0(3) . . . . ? C11 N7 C8 O13 -0.4(3) . . . . ? C11 N7 C8 C9 -178.1(2) . . . . ? C12 O13 C8 N7 7.7(4) . . . . ? C12 O13 C8 C9 -175.7(4) . . . . ? C14 N10 C6 Ir1 -6.3(5) . . . . ? C14 N10 C6 N7 176.5(3) . . . . ? C14 N10 C9 O16 0.8(3) . . . . ? C14 N10 C9 C8 -177.7(2) . . . . ? C15 O16 C9 N10 16.1(3) . . . . ? C15 O16 C9 C8 -166.2(4) . . . . ? C17 C11 C12 O13 -105.5(4) . . . . ? C18 C11 C12 O13 128.6(3) . . . . ? C19 C14 C15 O16 142.9(3) . . . . ? C20 C14 C15 O16 -90.3(3) . . . . ? C21 N22 C23 O28 -178.8(2) . . . . ? C21 N22 C23 C24 1.3(3) . . . . ? C21 N22 C26 C27 -165.8(3) . . . . ? C21 N22 C26 C32 77.1(4) . . . . ? C21 N22 C26 C33 -48.7(4) . . . . ? C21 N25 C24 O31 178.7(2) . . . . ? C21 N25 C24 C23 -0.6(3) . . . . ? C21 N25 C29 C30 167.5(3) . . . . ? C21 N25 C29 C34 -75.5(4) . . . . ? C21 N25 C29 C35 50.8(4) . . . . ? C23 O28 C27 C26 28.7(3) . . . . ? C23 N22 C21 Ir1 174.97(19) . . . . ? C23 N22 C21 N25 -1.6(3) . . . . ? C23 N22 C26 C27 18.6(3) . . . . ? C23 N22 C26 C32 -98.5(3) . . . . ? C23 N22 C26 C33 135.6(3) . . . . ? C24 O31 C30 C29 -27.4(3) . . . . ? C24 N25 C21 Ir1 -175.24(19) . . . . ? C24 N25 C21 N22 1.3(3) . . . . ? C24 N25 C29 C30 -19.0(3) . . . . ? C24 N25 C29 C34 98.0(3) . . . . ? C24 N25 C29 C35 -135.7(2) . . . . ? C26 N22 C21 Ir1 -0.6(5) . . . . ? C26 N22 C21 N25 -177.2(3) . . . . ? C26 N22 C23 O28 -2.0(3) . . . . ? C26 N22 C23 C24 178.2(2) . . . . ? C27 O28 C23 N22 -17.1(3) . . . . ? C27 O28 C23 C24 162.8(4) . . . . ? C29 N25 C21 Ir1 -1.8(4) . . . . ? C29 N25 C21 N22 174.7(3) . . . . ? C29 N25 C24 O31 3.5(3) . . . . ? C29 N25 C24 C23 -175.8(2) . . . . ? C30 O31 C24 N25 15.3(3) . . . . ? C30 O31 C24 C23 -165.8(4) . . . . ? C32 C26 C27 O28 86.0(3) . . . . ? C33 C26 C27 O28 -146.5(3) . . . . ? C34 C29 C30 O31 -87.1(3) . . . . ? C35 C29 C30 O31 144.6(3) . . . . ? C201 C202 C203 C204 1.5(4) . . . . ? C201 C202 C203 C207 -176.2(2) . . . . ? C202 C201 C206 C205 -0.6(4) . . . . ? C202 C201 B200 C209 -81.4(3) . . . . ? C202 C201 B200 C217 39.9(3) . . . . ? C202 C201 B200 C225 156.7(2) . . . . ? C202 C203 C204 C205 -0.4(4) . . . . ? C202 C203 C207 F1 -164.5(5) . . . . ? C202 C203 C207 F1A 50.8(5) . . . . ? C202 C203 C207 F2 -38.7(5) . . . . ? C202 C203 C207 F2A 171.0(4) . . . . ? C202 C203 C207 F3 75.0(5) . . . . ? C202 C203 C207 F3A -72.6(5) . . . . ? C203 C204 C205 C206 -1.2(4) . . . . ? C203 C204 C205 C208 178.7(2) . . . . ? C204 C203 C207 F1 17.8(6) . . . . ? C204 C203 C207 F1A -126.9(5) . . . . ? C204 C203 C207 F2 143.6(5) . . . . ? C204 C203 C207 F2A -6.7(5) . . . . ? C204 C203 C207 F3 -102.8(5) . . . . ? C204 C203 C207 F3A 109.7(5) . . . . ? C204 C205 C206 C201 1.8(4) . . . . ? C204 C205 C208 F4 9.0(6) . . . . ? C204 C205 C208 F4A 170.0(8) . . . . ? C204 C205 C208 F5 -118.9(5) . . . . ? C204 C205 C208 F5A 47.8(6) . . . . ? C204 C205 C208 F6 131.4(4) . . . . ? C204 C205 C208 F6A -61.0(7) . . . . ? C206 C201 C202 C203 -1.0(4) . . . . ? C206 C201 B200 C209 88.1(3) . . . . ? C206 C201 B200 C217 -150.6(2) . . . . ? C206 C201 B200 C225 -33.8(4) . . . . ? C206 C205 C208 F4 -171.1(6) . . . . ? C206 C205 C208 F4A -10.1(8) . . . . ? C206 C205 C208 F5 61.1(5) . . . . ? C206 C205 C208 F5A -132.3(5) . . . . ? C206 C205 C208 F6 -48.7(5) . . . . ? C206 C205 C208 F6A 118.9(7) . . . . ? C207 C203 C204 C205 177.3(2) . . . . ? C208 C205 C206 C201 -178.1(2) . . . . ? C209 C210 C211 C212 -0.1(4) . . . . ? C209 C210 C211 C215 179.5(3) . . . . ? C210 C209 C214 C213 0.7(4) . . . . ? C210 C209 B200 C201 79.6(3) . . . . ? C210 C209 B200 C217 -39.3(3) . . . . ? C210 C209 B200 C225 -156.4(2) . . . . ? C210 C211 C212 C213 0.1(4) . . . . ? C210 C211 C215 F7 -174.6(2) . . . . ? C210 C211 C215 F8 -53.9(3) . . . . ? C210 C211 C215 F9 63.5(3) . . . . ? C211 C212 C213 C214 0.2(4) . . . . ? C211 C212 C213 C216 -178.6(3) . . . . ? C212 C211 C215 F7 4.9(4) . . . . ? C212 C211 C215 F8 125.7(3) . . . . ? C212 C211 C215 F9 -116.9(3) . . . . ? C212 C213 C214 C209 -0.7(4) . . . . ? C212 C213 C216 F10 -18.0(4) . . . . ? C212 C213 C216 F11 101.3(3) . . . . ? C212 C213 C216 F12 -139.7(3) . . . . ? C214 C209 C210 C211 -0.4(4) . . . . ? C214 C209 B200 C201 -89.9(3) . . . . ? C214 C209 B200 C217 151.2(2) . . . . ? C214 C209 B200 C225 34.1(4) . . . . ? C214 C213 C216 F10 163.2(2) . . . . ? C214 C213 C216 F11 -77.5(3) . . . . ? C214 C213 C216 F12 41.5(4) . . . . ? C215 C211 C212 C213 -179.4(3) . . . . ? C216 C213 C214 C209 178.1(3) . . . . ? C217 C218 C219 C220 1.1(4) . . . . ? C217 C218 C219 C223 178.2(2) . . . . ? C218 C217 C222 C221 -0.9(4) . . . . ? C218 C217 B200 C201 45.1(3) . . . . ? C218 C217 B200 C209 158.7(2) . . . . ? C218 C217 B200 C225 -79.0(3) . . . . ? C218 C219 C220 C221 -1.2(4) . . . . ? C218 C219 C223 F13 167.3(2) . . . . ? C218 C219 C223 F14 -71.9(3) . . . . ? C218 C219 C223 F15 45.6(3) . . . . ? C219 C220 C221 C222 0.3(4) . . . . ? C219 C220 C221 C224 178.1(2) . . . . ? C220 C219 C223 F13 -15.6(4) . . . . ? C220 C219 C223 F14 105.2(3) . . . . ? C220 C219 C223 F15 -137.3(3) . . . . ? C220 C221 C222 C217 0.8(4) . . . . ? C220 C221 C224 F16 10.0(4) . . . . ? C220 C221 C224 F17 -108.8(3) . . . . ? C220 C221 C224 F18 131.9(3) . . . . ? C222 C217 C218 C219 0.0(4) . . . . ? C222 C217 B200 C201 -141.2(2) . . . . ? C222 C217 B200 C209 -27.5(3) . . . . ? C222 C217 B200 C225 94.7(3) . . . . ? C222 C221 C224 F16 -172.1(2) . . . . ? C222 C221 C224 F17 69.1(3) . . . . ? C222 C221 C224 F18 -50.2(4) . . . . ? C223 C219 C220 C221 -178.2(2) . . . . ? C224 C221 C222 C217 -177.1(2) . . . . ? C225 C226 C227 C228 0.5(4) . . . . ? C225 C226 C227 C231 -178.4(3) . . . . ? C226 C225 C230 C229 1.1(4) . . . . ? C226 C225 B200 C201 -33.5(4) . . . . ? C226 C225 B200 C209 -149.4(3) . . . . ? C226 C225 B200 C217 87.4(3) . . . . ? C226 C227 C228 C229 0.4(4) . . . . ? C226 C227 C231 F19 -64.6(7) . . . . ? C226 C227 C231 F19A 152.4(11) . . . . ? C226 C227 C231 F20 175.6(8) . . . . ? C226 C227 C231 F20A 33.4(10) . . . . ? C226 C227 C231 F21 52.0(8) . . . . ? C226 C227 C231 F21A -87.6(13) . . . . ? C227 C228 C229 C230 -0.6(4) . . . . ? C227 C228 C229 C232 -179.5(3) . . . . ? C228 C227 C231 F19 116.5(7) . . . . ? C228 C227 C231 F19A -26.5(12) . . . . ? C228 C227 C231 F20 -3.3(9) . . . . ? C228 C227 C231 F20A -145.5(10) . . . . ? C228 C227 C231 F21 -126.9(8) . . . . ? C228 C227 C231 F21A 93.4(12) . . . . ? C228 C229 C230 C225 -0.2(5) . . . . ? C228 C229 C232 F22 -29.5(5) . . . . ? C228 C229 C232 F22A 141.0(8) . . . . ? C228 C229 C232 F23 91.4(6) . . . . ? C228 C229 C232 F23A -101.1(9) . . . . ? C228 C229 C232 F24 -146.7(5) . . . . ? C228 C229 C232 F24A 21.9(9) . . . . ? C230 C225 C226 C227 -1.3(4) . . . . ? C230 C225 B200 C201 155.8(2) . . . . ? C230 C225 B200 C209 39.8(3) . . . . ? C230 C225 B200 C217 -83.4(3) . . . . ? C230 C229 C232 F22 151.6(4) . . . . ? C230 C229 C232 F22A -37.9(8) . . . . ? C230 C229 C232 F23 -87.5(6) . . . . ? C230 C229 C232 F23A 79.9(9) . . . . ? C230 C229 C232 F24 34.4(6) . . . . ? C230 C229 C232 F24A -157.1(9) . . . . ? C231 C227 C228 C229 179.4(3) . . . . ? C232 C229 C230 C225 178.7(3) . . . . ? B200 C201 C202 C203 169.4(2) . . . . ? B200 C201 C206 C205 -170.5(2) . . . . ? B200 C209 C210 C211 -170.6(2) . . . . ? B200 C209 C214 C213 170.8(2) . . . . ? B200 C217 C218 C219 174.3(2) . . . . ? B200 C217 C222 C221 -174.9(2) . . . . ? B200 C225 C226 C227 -172.4(3) . . . . ? B200 C225 C230 C229 172.6(3) . . . . ? _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received' #===END