data_publication_text _publ_requested_journal Organometallics _publ_contact_author_name 'KO, C. C.' _publ_contact_author_address ;Department of Biology and Chemistry, City University of Hong Kong, Kowloon Tong, Kowloon, Hong Kong SAR, People's Republic of China ; _publ_contact_author_email vinccko@cityu.edu.hk loop_ _publ_author_name _publ_author_address 'LO, L. T.-L.' ;Department of Biology and Chemistry, City University of Hong Kong, Kowloon Tong, Kowloon, Hong Kong SAR, People's Republic of China ; 'NG, C.-O.' ;Department of Biology and Chemistry, City University of Hong Kong, Kowloon Tong, Kowloon, Hong Kong SAR, People's Republic of China ; 'FENG, H.' ;Department of Biology and Chemistry, City University of Hong Kong, Kowloon Tong, Kowloon, Hong Kong SAR, People's Republic of China ; 'KO, C. C.' ;Department of Biology and Chemistry, City University of Hong Kong, Kowloon Tong, Kowloon, Hong Kong SAR, People's Republic of China ; data_1_green _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H35 B F4 N4 O0.50 Rh' _chemical_formula_sum 'C32 H35 B F4 N4 O0.50 Rh' _chemical_formula_weight 673.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.0965(4) _cell_length_b 20.8077(4) _cell_length_c 15.4552(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.555(2) _cell_angle_gamma 90.00 _cell_volume 6101.0(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 4.993 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.3158 _exptl_absorpt_correction_T_max 0.6351 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6424 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 55.00 _reflns_number_total 3581 _reflns_number_gt 2681 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3581 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0695 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 1.010925(9) 0.044586(9) 0.363276(11) 0.03540(5) Uani 1 1 d . . . C18 C 0.80249(12) 0.05386(12) 0.46699(14) 0.0413(7) Uani 1 1 d . . . N3 N 0.86868(9) 0.04878(9) 0.43664(11) 0.0361(5) Uani 1 1 d . . . C21 C 0.92278(11) 0.04815(11) 0.40882(14) 0.0369(7) Uani 1 1 d . . . N1 N 1.10899(9) 0.02784(9) 0.32108(11) 0.0361(6) Uani 1 1 d . . . N4 N 1.01690(10) 0.19233(9) 0.37580(11) 0.0424(6) Uani 1 1 d . . . C5 C 1.12780(12) -0.03539(11) 0.31587(13) 0.0346(7) Uani 1 1 d . . . C10 C 0.96340(13) -0.09482(13) 0.38246(15) 0.0461(8) Uani 1 1 d . . . H10 H 0.9201 -0.0768 0.3956 0.055 Uiso 1 1 calc R . . C30 C 1.01540(11) 0.13575(12) 0.36980(14) 0.0398(7) Uani 1 1 d . . . C2 C 1.21821(13) 0.05536(12) 0.26841(14) 0.0422(8) Uani 1 1 d . . . H2 H 1.2487 0.0883 0.2525 0.051 Uiso 1 1 calc R . . C1 C 1.15523(13) 0.07175(12) 0.29711(14) 0.0414(7) Uani 1 1 d . . . H1 H 1.1436 0.1160 0.3003 0.050 Uiso 1 1 calc R . . C4 C 1.19032(12) -0.05324(12) 0.28585(14) 0.0418(7) Uani 1 1 d . . . H4 H 1.2011 -0.0976 0.2812 0.050 Uiso 1 1 calc R . . C3 C 1.23790(12) -0.00774(13) 0.26228(14) 0.0401(7) Uani 1 1 d . . . N2 N 1.01484(9) -0.05454(9) 0.36178(11) 0.0371(6) Uani 1 1 d . . . C6 C 1.07546(12) -0.08163(12) 0.34159(14) 0.0369(7) Uani 1 1 d . . . C17 C 0.77515(13) 0.11580(12) 0.47373(16) 0.0486(8) Uani 1 1 d . . . C19 C 0.79888(13) -0.06681(12) 0.48082(16) 0.0483(8) Uani 1 1 d . . . H19A H 0.7975 -0.0782 0.4191 0.072 Uiso 1 1 calc R . . H19B H 0.7716 -0.0983 0.5103 0.072 Uiso 1 1 calc R . . H19C H 0.8478 -0.0668 0.5079 0.072 Uiso 1 1 calc R . . C13 C 0.76767(12) -0.00114(12) 0.48868(14) 0.0390(7) Uani 1 1 d . . . C28 C 0.90583(13) 0.27847(14) 0.31116(17) 0.0599(9) Uani 1 1 d . . . H28A H 0.8702 0.2824 0.3518 0.090 Uiso 1 1 calc R . . H28B H 0.9091 0.2335 0.2932 0.090 Uiso 1 1 calc R . . H28C H 0.8923 0.3052 0.2598 0.090 Uiso 1 1 calc R . . C22 C 1.02838(12) 0.25696(12) 0.38742(15) 0.0426(8) Uani 1 1 d . . . C27 C 1.09350(14) 0.27677(13) 0.42827(18) 0.0563(9) Uani 1 1 d . . . C15 C 0.67342(15) 0.06673(15) 0.52419(18) 0.0643(10) Uani 1 1 d . . . H15 H 0.6283 0.0711 0.5439 0.077 Uiso 1 1 calc R . . C29 C 1.15046(15) 0.23050(15) 0.46121(18) 0.0660(10) Uani 1 1 d . . . H29A H 1.1295 0.1887 0.4722 0.099 Uiso 1 1 calc R . . H29B H 1.1757 0.2470 0.5154 0.099 Uiso 1 1 calc R . . H29C H 1.1835 0.2255 0.4176 0.099 Uiso 1 1 calc R . . C23 C 0.97562(13) 0.30014(13) 0.35491(17) 0.0510(8) Uani 1 1 d . . . C9 C 0.97097(14) -0.16021(13) 0.38532(15) 0.0495(8) Uani 1 1 d . . . H9 H 0.9332 -0.1866 0.3992 0.059 Uiso 1 1 calc R . . C7 C 1.08631(13) -0.14688(11) 0.34574(15) 0.0425(7) Uani 1 1 d . . . H7 H 1.1301 -0.1642 0.3334 0.051 Uiso 1 1 calc R . . C16 C 0.70923(13) 0.12084(14) 0.50284(18) 0.0598(9) Uani 1 1 d . . . H16 H 0.6886 0.1620 0.5081 0.072 Uiso 1 1 calc R . . C20 C 0.81345(15) 0.17356(13) 0.44689(18) 0.0613(9) Uani 1 1 d . . . H20A H 0.8592 0.1768 0.4825 0.092 Uiso 1 1 calc R . . H20B H 0.7856 0.2121 0.4551 0.092 Uiso 1 1 calc R . . H20C H 0.8208 0.1697 0.3854 0.092 Uiso 1 1 calc R . . C14 C 0.70165(13) 0.00669(14) 0.51754(16) 0.0515(9) Uani 1 1 d . . . H14 H 0.6760 -0.0300 0.5327 0.062 Uiso 1 1 calc R . . C12 C 1.04439(17) -0.25957(13) 0.3735(2) 0.0735(11) Uani 1 1 d . . . H12A H 1.0901 -0.2705 0.3544 0.110 Uiso 1 1 calc R . . H12B H 1.0067 -0.2811 0.3360 0.110 Uiso 1 1 calc R . . H12C H 1.0434 -0.2737 0.4339 0.110 Uiso 1 1 calc R . . C8 C 1.03363(14) -0.18783(13) 0.36794(16) 0.0489(8) Uani 1 1 d . . . C25 C 1.05491(18) 0.38541(16) 0.4032(3) 0.0992(15) Uani 1 1 d . . . H25 H 1.0645 0.4301 0.4096 0.119 Uiso 1 1 calc R . . C26 C 1.10457(17) 0.34183(16) 0.4344(2) 0.0909(13) Uani 1 1 d . . . H26 H 1.1486 0.3570 0.4615 0.109 Uiso 1 1 calc R . . C24 C 0.99137(16) 0.36543(14) 0.3625(2) 0.0793(12) Uani 1 1 d . . . H24 H 0.9577 0.3963 0.3393 0.095 Uiso 1 1 calc R . . F4 F 0.23666(9) 0.20685(8) 0.28852(12) 0.0878(6) Uani 1 1 d . . . F2 F 0.27873(10) 0.26983(11) 0.18987(11) 0.1112(8) Uani 1 1 d . . . F1 F 0.27653(14) 0.30512(9) 0.32398(13) 0.1228(10) Uani 1 1 d . . . C11 C 1.30666(13) -0.02751(14) 0.23320(17) 0.0568(9) Uani 1 1 d . . . H11A H 1.3145 -0.0037 0.1805 0.085 Uiso 1 1 calc R . . H11B H 1.3058 -0.0737 0.2207 0.085 Uiso 1 1 calc R . . H11C H 1.3449 -0.0181 0.2793 0.085 Uiso 1 1 calc R . . F3 F 0.35242(11) 0.23004(14) 0.30146(16) 0.1389(11) Uani 1 1 d . . . B1 B 0.28674(18) 0.2518(2) 0.2766(2) 0.0670(12) Uani 1 1 d . . . O1 O 1.0000 0.5294(3) 0.2500 0.195(3) Uani 1 2 d S . . C31 C 1.0130(5) 0.5675(3) 0.3279(5) 0.333(6) Uani 1 1 d . . . H31A H 1.0529 0.5488 0.3662 0.400 Uiso 1 1 calc R . . H31B H 1.0261 0.6116 0.3123 0.400 Uiso 1 1 calc R . . C32 C 0.9576(4) 0.5695(5) 0.3692(6) 0.442(5) Uani 1 1 d . . . H32A H 0.9400 0.5258 0.3762 0.663 Uiso 1 1 calc R . . H32B H 0.9210 0.5953 0.3359 0.663 Uiso 1 1 calc R . . H32C H 0.9700 0.5890 0.4266 0.663 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.03048(8) 0.03732(9) 0.03839(8) 0.00003(10) 0.00387(7) 0.00277(10) C18 0.0321(12) 0.0559(16) 0.0358(12) 0.0006(12) 0.0028(10) 0.0036(13) N3 0.0310(9) 0.0386(11) 0.0382(10) -0.0021(9) 0.0016(8) 0.0086(10) C21 0.0305(11) 0.0339(13) 0.0445(13) -0.0028(12) -0.0042(10) 0.0160(12) N1 0.0332(10) 0.0432(12) 0.0317(10) 0.0004(9) 0.0028(9) 0.0006(9) N4 0.0455(11) 0.0393(11) 0.0451(11) 0.0033(10) 0.0173(9) 0.0022(11) C5 0.0347(12) 0.0360(13) 0.0326(11) -0.0039(11) 0.0017(10) 0.0079(12) C10 0.0358(13) 0.0527(16) 0.0514(14) -0.0063(13) 0.0113(12) -0.0015(13) C30 0.0308(12) 0.0561(15) 0.0322(11) 0.0114(12) 0.0028(10) 0.0064(13) C2 0.0428(13) 0.0506(15) 0.0331(12) 0.0027(12) 0.0046(11) -0.0027(13) C1 0.0468(14) 0.0413(14) 0.0363(12) 0.0023(11) 0.0051(12) 0.0104(13) C4 0.0423(13) 0.0435(14) 0.0381(12) -0.0065(12) -0.0018(11) 0.0109(13) C3 0.0332(12) 0.0545(15) 0.0321(12) -0.0011(12) 0.0011(11) 0.0060(13) N2 0.0317(10) 0.0417(11) 0.0382(9) -0.0025(10) 0.0054(8) 0.0011(10) C6 0.0367(13) 0.0400(14) 0.0330(12) -0.0030(11) -0.0001(11) 0.0045(12) C17 0.0438(14) 0.0470(16) 0.0556(15) 0.0010(13) 0.0088(12) 0.0067(13) C19 0.0450(14) 0.0486(16) 0.0511(15) -0.0007(13) 0.0053(13) -0.0101(13) C13 0.0363(13) 0.0448(15) 0.0355(13) -0.0007(12) 0.0021(11) 0.0024(12) C28 0.0482(15) 0.0650(18) 0.0698(17) 0.0110(15) 0.0204(13) 0.0094(15) C22 0.0414(13) 0.0371(14) 0.0527(14) -0.0018(12) 0.0198(11) -0.0015(12) C27 0.0509(15) 0.0492(16) 0.0731(16) -0.0127(14) 0.0253(13) -0.0001(14) C15 0.0428(14) 0.091(2) 0.0617(16) -0.0058(16) 0.0180(13) 0.0032(16) C29 0.0516(16) 0.083(2) 0.0625(17) -0.0008(17) 0.0042(15) -0.0007(17) C23 0.0488(14) 0.0447(15) 0.0632(15) -0.0003(14) 0.0228(12) 0.0001(14) C9 0.0532(15) 0.0478(16) 0.0493(14) -0.0023(13) 0.0134(13) 0.0001(14) C7 0.0457(14) 0.0363(14) 0.0481(13) -0.0048(12) 0.0166(12) 0.0031(12) C16 0.0439(14) 0.0594(18) 0.0790(18) 0.0007(16) 0.0197(14) 0.0174(15) C20 0.0564(16) 0.0497(17) 0.0809(18) 0.0028(15) 0.0216(15) 0.0109(15) C14 0.0440(14) 0.0597(17) 0.0523(15) -0.0045(14) 0.0117(13) -0.0066(15) C12 0.0843(19) 0.0419(17) 0.099(2) 0.0003(17) 0.0319(17) 0.0029(17) C8 0.0512(15) 0.0472(15) 0.0497(14) -0.0042(13) 0.0126(13) -0.0016(14) C25 0.076(2) 0.051(2) 0.174(3) -0.017(2) 0.028(2) -0.0101(19) C26 0.061(2) 0.071(2) 0.141(3) -0.031(2) 0.009(2) -0.0066(18) C24 0.0589(18) 0.0443(17) 0.138(3) -0.0044(19) 0.0238(19) 0.0149(16) F4 0.0900(11) 0.0649(11) 0.1148(12) 0.0015(10) 0.0386(10) -0.0311(10) F2 0.1054(12) 0.1585(17) 0.0695(11) -0.0032(12) 0.0094(10) -0.0744(12) F1 0.201(2) 0.0652(12) 0.1024(14) -0.0118(11) 0.0175(15) -0.0214(15) C11 0.0405(14) 0.072(2) 0.0601(16) -0.0027(15) 0.0161(13) 0.0056(14) F3 0.0794(14) 0.188(2) 0.1482(19) 0.0129(18) 0.0097(14) 0.0036(16) B1 0.0501(19) 0.089(3) 0.063(2) -0.002(2) 0.0115(18) -0.014(2) O1 0.195(5) 0.184(5) 0.208(5) 0.000 0.021(4) 0.000 C31 0.415(13) 0.112(4) 0.440(12) -0.082(6) -0.096(11) -0.024(7) C32 0.370(7) 0.430(12) 0.597(10) -0.261(9) 0.364(6) -0.186(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 Rh1 C21 1.899(2) . ? Rh1 C30 1.901(3) . ? Rh1 N2 2.0641(18) . ? Rh1 N1 2.0814(18) . ? C18 C13 1.384(3) . ? C18 C17 1.399(4) . ? C18 N3 1.402(3) . ? N3 C21 1.164(3) . ? N1 C1 1.351(3) . ? N1 C5 1.369(3) . ? N4 C30 1.181(3) . ? N4 C22 1.371(3) . ? C5 C4 1.380(3) . ? C5 C6 1.474(3) . ? C10 N2 1.357(3) . ? C10 C9 1.368(4) . ? C10 H10 0.9500 . ? C2 C1 1.372(3) . ? C2 C3 1.372(4) . ? C2 H2 0.9500 . ? C1 H1 0.9500 . ? C4 C3 1.389(3) . ? C4 H4 0.9500 . ? C3 C11 1.493(3) . ? N2 C6 1.356(3) . ? C6 C7 1.374(3) . ? C17 C16 1.388(4) . ? C17 C20 1.490(4) . ? C19 C13 1.501(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C13 C14 1.394(4) . ? C28 C23 1.494(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C22 C27 1.391(3) . ? C22 C23 1.400(3) . ? C27 C26 1.372(4) . ? C27 C29 1.498(4) . ? C15 C14 1.369(4) . ? C15 C16 1.377(4) . ? C15 H15 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C23 C24 1.393(4) . ? C9 C8 1.381(4) . ? C9 H9 0.9500 . ? C7 C8 1.391(4) . ? C7 H7 0.9500 . ? C16 H16 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C14 H14 0.9500 . ? C12 C8 1.508(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C25 C26 1.360(5) . ? C25 C24 1.366(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C24 H24 0.9500 . ? F4 B1 1.365(4) . ? F2 B1 1.383(4) . ? F1 B1 1.356(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? F3 B1 1.348(4) . ? O1 C31 1.438(8) . ? O1 C31 1.438(8) 2_755 ? C31 C32 1.296(13) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? 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 C21 Rh1 C30 88.72(10) . . ? C21 Rh1 N2 94.47(9) . . ? C30 Rh1 N2 175.01(8) . . ? C21 Rh1 N1 171.94(9) . . ? C30 Rh1 N1 98.45(9) . . ? N2 Rh1 N1 78.12(7) . . ? C13 C18 C17 123.4(2) . . ? C13 C18 N3 119.7(2) . . ? C17 C18 N3 116.9(2) . . ? C21 N3 C18 175.8(2) . . ? N3 C21 Rh1 178.4(2) . . ? C1 N1 C5 116.72(19) . . ? C1 N1 Rh1 127.75(16) . . ? C5 N1 Rh1 115.53(15) . . ? C30 N4 C22 171.9(2) . . ? N1 C5 C4 121.4(2) . . ? N1 C5 C6 114.9(2) . . ? C4 C5 C6 123.6(2) . . ? N2 C10 C9 123.0(2) . . ? N2 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? N4 C30 Rh1 178.0(2) . . ? C1 C2 C3 121.2(2) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? N1 C1 C2 123.0(2) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C5 C4 C3 121.4(2) . . ? C5 C4 H4 119.3 . . ? C3 C4 H4 119.3 . . ? C2 C3 C4 116.2(2) . . ? C2 C3 C11 122.8(2) . . ? C4 C3 C11 121.0(2) . . ? C6 N2 C10 117.2(2) . . ? C6 N2 Rh1 116.82(15) . . ? C10 N2 Rh1 125.91(16) . . ? N2 C6 C7 121.9(2) . . ? N2 C6 C5 114.4(2) . . ? C7 C6 C5 123.7(2) . . ? C16 C17 C18 117.0(2) . . ? C16 C17 C20 121.4(2) . . ? C18 C17 C20 121.5(2) . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C13 C14 117.3(2) . . ? C18 C13 C19 121.8(2) . . ? C14 C13 C19 120.9(2) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C22 C27 118.1(2) . . ? N4 C22 C23 119.0(2) . . ? C27 C22 C23 122.8(2) . . ? C26 C27 C22 116.5(3) . . ? C26 C27 C29 120.7(3) . . ? C22 C27 C29 122.7(2) . . ? C14 C15 C16 121.2(3) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C23 C22 117.1(2) . . ? C24 C23 C28 120.4(2) . . ? C22 C23 C28 122.5(2) . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C6 C7 C8 120.5(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C15 C16 C17 120.6(3) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C14 C13 120.6(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C8 C7 117.4(2) . . ? C9 C8 C12 121.1(3) . . ? C7 C8 C12 121.5(2) . . ? C26 C25 C24 120.5(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 122.5(3) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? F3 B1 F1 107.9(3) . . ? F3 B1 F4 112.0(3) . . ? F1 B1 F4 110.0(3) . . ? F3 B1 F2 111.3(3) . . ? F1 B1 F2 107.1(3) . . ? F4 B1 F2 108.4(3) . . ? C31 O1 C31 113.1(7) . 2_755 ? C32 C31 O1 111.0(7) . . ? C32 C31 H31A 109.4 . . ? O1 C31 H31A 109.4 . . ? C32 C31 H31B 109.4 . . ? O1 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? 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 C13 C18 N3 C21 154(3) . . . . ? C17 C18 N3 C21 -26(3) . . . . ? C18 N3 C21 Rh1 -147(6) . . . . ? C30 Rh1 C21 N3 -180(100) . . . . ? N2 Rh1 C21 N3 -3(7) . . . . ? N1 Rh1 C21 N3 -27(7) . . . . ? C21 Rh1 N1 C1 -159.4(5) . . . . ? C30 Rh1 N1 C1 -6.67(19) . . . . ? N2 Rh1 N1 C1 177.01(18) . . . . ? C21 Rh1 N1 C5 21.8(6) . . . . ? C30 Rh1 N1 C5 174.52(15) . . . . ? N2 Rh1 N1 C5 -1.80(14) . . . . ? C1 N1 C5 C4 -1.3(3) . . . . ? Rh1 N1 C5 C4 177.64(16) . . . . ? C1 N1 C5 C6 -179.27(18) . . . . ? Rh1 N1 C5 C6 -0.3(2) . . . . ? C22 N4 C30 Rh1 111(6) . . . . ? C21 Rh1 C30 N4 26(6) . . . . ? N2 Rh1 C30 N4 -104(6) . . . . ? N1 Rh1 C30 N4 -151(6) . . . . ? C5 N1 C1 C2 0.2(3) . . . . ? Rh1 N1 C1 C2 -178.58(16) . . . . ? C3 C2 C1 N1 0.1(3) . . . . ? N1 C5 C4 C3 2.1(3) . . . . ? C6 C5 C4 C3 179.9(2) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C1 C2 C3 C11 -178.6(2) . . . . ? C5 C4 C3 C2 -1.7(3) . . . . ? C5 C4 C3 C11 177.6(2) . . . . ? C9 C10 N2 C6 1.4(3) . . . . ? C9 C10 N2 Rh1 -175.87(17) . . . . ? C21 Rh1 N2 C6 -172.88(16) . . . . ? C30 Rh1 N2 C6 -43.1(10) . . . . ? N1 Rh1 N2 C6 3.89(14) . . . . ? C21 Rh1 N2 C10 4.35(19) . . . . ? C30 Rh1 N2 C10 134.1(9) . . . . ? N1 Rh1 N2 C10 -178.87(18) . . . . ? C10 N2 C6 C7 -3.1(3) . . . . ? Rh1 N2 C6 C7 174.40(16) . . . . ? C10 N2 C6 C5 177.33(18) . . . . ? Rh1 N2 C6 C5 -5.2(2) . . . . ? N1 C5 C6 N2 3.6(3) . . . . ? C4 C5 C6 N2 -174.34(19) . . . . ? N1 C5 C6 C7 -176.0(2) . . . . ? C4 C5 C6 C7 6.1(3) . . . . ? C13 C18 C17 C16 -0.8(4) . . . . ? N3 C18 C17 C16 179.3(2) . . . . ? C13 C18 C17 C20 -178.0(2) . . . . ? N3 C18 C17 C20 2.1(3) . . . . ? C17 C18 C13 C14 0.8(3) . . . . ? N3 C18 C13 C14 -179.3(2) . . . . ? C17 C18 C13 C19 -179.8(2) . . . . ? N3 C18 C13 C19 0.1(3) . . . . ? C30 N4 C22 C27 -5.0(17) . . . . ? C30 N4 C22 C23 172.5(15) . . . . ? N4 C22 C27 C26 176.4(3) . . . . ? C23 C22 C27 C26 -0.9(4) . . . . ? N4 C22 C27 C29 -1.2(4) . . . . ? C23 C22 C27 C29 -178.6(3) . . . . ? N4 C22 C23 C24 -175.5(2) . . . . ? C27 C22 C23 C24 1.9(4) . . . . ? N4 C22 C23 C28 2.7(4) . . . . ? C27 C22 C23 C28 -180.0(2) . . . . ? N2 C10 C9 C8 1.0(4) . . . . ? N2 C6 C7 C8 2.5(3) . . . . ? C5 C6 C7 C8 -178.0(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C18 C17 C16 C15 0.3(4) . . . . ? C20 C17 C16 C15 177.5(2) . . . . ? C16 C15 C14 C13 -0.1(4) . . . . ? C18 C13 C14 C15 -0.3(3) . . . . ? C19 C13 C14 C15 -179.7(2) . . . . ? C10 C9 C8 C7 -1.7(3) . . . . ? C10 C9 C8 C12 177.9(2) . . . . ? C6 C7 C8 C9 0.0(3) . . . . ? C6 C7 C8 C12 -179.6(2) . . . . ? C24 C25 C26 C27 -1.0(6) . . . . ? C22 C27 C26 C25 0.5(5) . . . . ? C29 C27 C26 C25 178.2(3) . . . . ? C26 C25 C24 C23 2.0(6) . . . . ? C22 C23 C24 C25 -2.4(5) . . . . ? C28 C23 C24 C25 179.4(3) . . . . ? C31 O1 C31 C32 102.2(7) 2_755 . . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 55.00 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.712 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.085 # start Validation Reply Form _vrf_THETM01_1_green ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.5313 RESPONSE: A full set of data was collected, however the diffraction of the crystal was weak at higher theta angles with most of the Intensity < 3 sigma(I) suggesting the data at very high angle were dominated by noise and therefore were omitted. ; _vrf_PLAT029_1_green ; PROBLEM: Low ....... 0.93. RESPONSE: This is also the consequence of the relatively weak diffraction of the crystal at high angle. It is only the very high angle data that is incomplete and at lower angle, the completeness of the data is acceptable. ; _vrf_PLAT232_1_green ; PROBLEM: Hirshfeld Test Diff for N1 -- C1 .. 7.80 su. PROBLEM: Hirshfeld Test Diff for N4 -- C30 .. 10.55 su. PROBLEM: Hirshfeld Test Diff for C14 -- C15 .. 7.76 su. PROBLEM: Hirshfeld Test Diff (M-X) Rh1 -- C30 .. 15.43 su. RESPONSE: (PLAT230 to PLAT232) These are attributed to the disorderness of the atoms or bonds between heavy and light atoms as a result of inadequate modelling of bonding density. ; _vrf_PLAT360_1_green ; PROBLEM: Short C(sp3)-C(sp3) Bond C31 - C32 ... 1.30 Ang. RESPONSE: This is due to the diorderness of the solvent molecule that causes larger anisotropic displacement parameters and unexpected short bond length. ; # end Validation Reply Form