####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_f50327a _database_code_depnum_ccdc_archive 'CCDC 281883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H63 B20 Cl2 Ir2 Rh2 S4' _chemical_formula_weight 1465.39 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.066(4) _cell_length_b 26.140(8) _cell_length_c 18.062(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.633(5) _cell_angle_gamma 90.00 _cell_volume 5165(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1004 _cell_measurement_theta_min 2.411 _cell_measurement_theta_max 22.566 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.884 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2812 _exptl_absorpt_coefficient_mu 6.057 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2638 _exptl_absorpt_correction_T_max 0.6429 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _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 21604 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0866 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9083 _reflns_number_gt 6697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. The solvent molecules were disordered. C33 atoms refined with anisotropic restraint. The C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 atoms of the Cp ring is disordered in some way. These atoms were refined with anisotropic restraints. The 66 restraints refer to anisotropical B parameters of these atoms. The Cp ring was not modelled as disordered. ; _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^)+(0.0342P)^2^+30.4599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9083 _refine_ls_number_parameters 597 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.27499(4) 0.026133(15) 0.15490(2) 0.03248(13) Uani 1 1 d . . . Ir2 Ir 0.57743(4) 0.181983(14) 0.28345(2) 0.02721(12) Uani 1 1 d . . . Rh1 Rh 0.39497(8) 0.22804(3) 0.18218(4) 0.0316(2) Uani 1 1 d . . . Rh2 Rh 0.42976(7) 0.09760(3) 0.20405(4) 0.02790(19) Uani 1 1 d . . . S1 S 0.3765(3) 0.02751(10) 0.27778(14) 0.0331(6) Uani 1 1 d . . . S2 S 0.4769(2) 0.02675(10) 0.12943(14) 0.0325(6) Uani 1 1 d . . . S3 S 0.3698(2) 0.16568(10) 0.27096(13) 0.0317(6) Uani 1 1 d . . . S4 S 0.4020(2) 0.15465(10) 0.10637(13) 0.0323(6) Uani 1 1 d . . . B3 B 0.6434(11) 0.0098(4) 0.2750(6) 0.032(3) Uani 1 1 d . . . H3 H 0.6632 0.0509 0.2817 0.039 Uiso 1 1 calc R . . B4 B 0.6155(13) -0.0289(5) 0.3506(7) 0.043(3) Uani 1 1 d . . . H4 H 0.6156 -0.0134 0.4072 0.052 Uiso 1 1 calc R . . B5 B 0.5104(15) -0.0770(5) 0.3148(9) 0.057(4) Uani 1 1 d . . . H5 H 0.4426 -0.0922 0.3478 0.068 Uiso 1 1 calc R . . B6 B 0.4738(13) -0.0704(5) 0.2185(8) 0.047(4) Uani 1 1 d . . . H6 H 0.3835 -0.0814 0.1886 0.057 Uiso 1 1 calc R . . B7 B 0.7099(13) -0.0270(5) 0.2113(7) 0.042(3) Uani 1 1 d . . . H7 H 0.7718 -0.0098 0.1760 0.050 Uiso 1 1 calc R . . B8 B 0.7517(14) -0.0369(5) 0.3104(8) 0.050(4) Uani 1 1 d . . . H8 H 0.8426 -0.0269 0.3403 0.060 Uiso 1 1 calc R . . B9 B 0.6722(15) -0.0899(6) 0.3358(9) 0.060(4) Uani 1 1 d . . . H9 H 0.7116 -0.1141 0.3831 0.072 Uiso 1 1 calc R . . B10 B 0.5825(15) -0.1165(5) 0.2539(8) 0.055(4) Uani 1 1 d . . . H10 H 0.5641 -0.1577 0.2477 0.066 Uiso 1 1 calc R . . B11 B 0.6088(13) -0.0767(5) 0.1772(9) 0.049(4) Uani 1 1 d . . . H11 H 0.6072 -0.0916 0.1202 0.059 Uiso 1 1 calc R . . B12 B 0.7292(16) -0.0898(5) 0.2506(10) 0.063(5) Uani 1 1 d . . . H12 H 0.8064 -0.1143 0.2416 0.076 Uiso 1 1 calc R . . B13 B 0.5229(14) 0.2299(5) 0.0263(7) 0.046(3) Uani 1 1 d . . . H13 H 0.4374 0.2368 -0.0120 0.055 Uiso 1 1 calc R . . B14 B 0.6126(14) 0.2819(5) 0.0638(7) 0.047(4) Uani 1 1 d . . . H14 H 0.5864 0.3218 0.0503 0.057 Uiso 1 1 calc R . . B15 B 0.6877(12) 0.2623(5) 0.1544(7) 0.039(3) Uani 1 1 d . . . H15 H 0.7118 0.2909 0.1989 0.047 Uiso 1 1 calc R . . B16 B 0.6353(11) 0.2012(5) 0.1791(6) 0.031(3) Uani 1 1 d . . . B17 B 0.6170(14) 0.1752(6) 0.0171(7) 0.051(4) Uani 1 1 d . . . H17 H 0.5930 0.1466 -0.0273 0.061 Uiso 1 1 calc R . . B18 B 0.6686(15) 0.2379(6) -0.0018(7) 0.054(4) Uani 1 1 d . . . H18 H 0.6805 0.2497 -0.0587 0.064 Uiso 1 1 calc R . . B19 B 0.7684(14) 0.2592(6) 0.0787(7) 0.051(4) Uani 1 1 d . . . H19 H 0.8446 0.2853 0.0734 0.061 Uiso 1 1 calc R . . B20 B 0.7792(13) 0.2101(5) 0.1466(7) 0.044(3) Uani 1 1 d . . . H20 H 0.8641 0.2039 0.1858 0.053 Uiso 1 1 calc R . . B21 B 0.6883(12) 0.1569(5) 0.1101(7) 0.039(3) Uani 1 1 d . . . H21 H 0.7102 0.1168 0.1251 0.047 Uiso 1 1 calc R . . B22 B 0.7701(14) 0.1939(6) 0.0508(7) 0.051(4) Uani 1 1 d . . . H22 H 0.8479 0.1772 0.0278 0.061 Uiso 1 1 calc R . . C1 C 0.5038(11) -0.0172(4) 0.2770(6) 0.039(3) Uani 1 1 d . . . C2 C 0.5563(10) -0.0180(4) 0.1985(6) 0.034(2) Uani 1 1 d . . . C3 C 0.5404(10) 0.2422(4) 0.1197(5) 0.034(3) Uani 1 1 d . . . C4 C 0.5455(10) 0.1831(4) 0.0922(5) 0.035(2) Uani 1 1 d . . . C5 C 0.0870(13) 0.0472(6) 0.1363(9) 0.074(4) Uani 1 1 d U . . C6 C 0.0943(13) -0.0026(7) 0.1619(8) 0.070(4) Uani 1 1 d U . . C7 C 0.1350(16) -0.0312(6) 0.1170(10) 0.080(5) Uani 1 1 d U . . C8 C 0.1620(13) -0.0074(6) 0.0567(7) 0.061(4) Uani 1 1 d U . . C9 C 0.1355(13) 0.0452(6) 0.0645(8) 0.072(4) Uani 1 1 d U . . C10 C 0.029(3) 0.0887(11) 0.1755(16) 0.206(13) Uani 1 1 d U . . H10A H -0.0498 0.0778 0.1850 0.308 Uiso 1 1 calc R . . H10B H 0.0204 0.1188 0.1445 0.308 Uiso 1 1 calc R . . H10C H 0.0798 0.0965 0.2221 0.308 Uiso 1 1 calc R . . C11 C 0.052(3) -0.0195(11) 0.2378(16) 0.204(13) Uani 1 1 d U . . H11A H -0.0164 -0.0425 0.2273 0.307 Uiso 1 1 calc R . . H11B H 0.0276 0.0101 0.2634 0.307 Uiso 1 1 calc R . . H11C H 0.1178 -0.0364 0.2687 0.307 Uiso 1 1 calc R . . C12 C 0.141(2) -0.0914(9) 0.1317(14) 0.172(10) Uani 1 1 d U . . H12A H 0.1588 -0.0978 0.1845 0.258 Uiso 1 1 calc R . . H12B H 0.2036 -0.1062 0.1071 0.258 Uiso 1 1 calc R . . H12C H 0.0634 -0.1065 0.1122 0.258 Uiso 1 1 calc R . . C13 C 0.215(2) -0.0320(8) -0.0076(12) 0.141(8) Uani 1 1 d U . . H13A H 0.1993 -0.0681 -0.0083 0.212 Uiso 1 1 calc R . . H13B H 0.3020 -0.0263 -0.0010 0.212 Uiso 1 1 calc R . . H13C H 0.1784 -0.0172 -0.0542 0.212 Uiso 1 1 calc R . . C14 C 0.155(2) 0.0805(9) 0.0022(14) 0.171(10) Uani 1 1 d U . . H14A H 0.1411 0.0623 -0.0445 0.257 Uiso 1 1 calc R . . H14B H 0.2370 0.0933 0.0106 0.257 Uiso 1 1 calc R . . H14C H 0.0985 0.1086 0.0003 0.257 Uiso 1 1 calc R . . C15 C 0.5825(11) 0.2026(4) 0.4066(5) 0.041(3) Uani 1 1 d . . . C16 C 0.6525(12) 0.2403(4) 0.3764(6) 0.044(3) Uani 1 1 d . . . C17 C 0.7520(12) 0.2149(6) 0.3491(6) 0.056(4) Uani 1 1 d . . . C18 C 0.7432(11) 0.1619(5) 0.3641(6) 0.045(3) Uani 1 1 d . . . C19 C 0.6370(11) 0.1543(4) 0.3992(5) 0.038(3) Uani 1 1 d . . . C20 C 0.4790(13) 0.2120(7) 0.4491(7) 0.082(5) Uani 1 1 d . . . H20A H 0.5100 0.2152 0.5014 0.123 Uiso 1 1 calc R . . H20B H 0.4227 0.1839 0.4416 0.123 Uiso 1 1 calc R . . H20C H 0.4378 0.2430 0.4316 0.123 Uiso 1 1 calc R . . C21 C 0.6439(16) 0.2974(5) 0.3836(8) 0.084(5) Uani 1 1 d . . . H21A H 0.5655 0.3063 0.3965 0.126 Uiso 1 1 calc R . . H21B H 0.6535 0.3131 0.3368 0.126 Uiso 1 1 calc R . . H21C H 0.7071 0.3092 0.4221 0.126 Uiso 1 1 calc R . . C22 C 0.8646(14) 0.2407(7) 0.3288(7) 0.093(6) Uani 1 1 d . . . H22A H 0.9256 0.2430 0.3725 0.139 Uiso 1 1 calc R . . H22B H 0.8438 0.2744 0.3100 0.139 Uiso 1 1 calc R . . H22C H 0.8960 0.2210 0.2910 0.139 Uiso 1 1 calc R . . C23 C 0.8423(15) 0.1236(7) 0.3539(10) 0.108(7) Uani 1 1 d . . . H23A H 0.8152 0.1024 0.3113 0.161 Uiso 1 1 calc R . . H23B H 0.8594 0.1026 0.3979 0.161 Uiso 1 1 calc R . . H23C H 0.9151 0.1416 0.3463 0.161 Uiso 1 1 calc R . . C24 C 0.5975(16) 0.1056(5) 0.4313(7) 0.081(5) Uani 1 1 d . . . H24A H 0.6190 0.1062 0.4848 0.122 Uiso 1 1 calc R . . H24B H 0.6375 0.0773 0.4113 0.122 Uiso 1 1 calc R . . H24C H 0.5106 0.1019 0.4184 0.122 Uiso 1 1 calc R . . C25 C 0.4197(12) 0.3097(4) 0.2202(6) 0.047(3) Uani 1 1 d . . . H25 H 0.5031 0.3178 0.2438 0.056 Uiso 1 1 calc R . . C26 C 0.3517(11) 0.2850(4) 0.2666(6) 0.045(3) Uani 1 1 d . . . H26 H 0.3944 0.2792 0.3175 0.054 Uiso 1 1 calc R . . C27 C 0.2126(14) 0.2929(6) 0.2613(10) 0.085(5) Uani 1 1 d . . . H27A H 0.1899 0.2862 0.3102 0.102 Uiso 1 1 calc R . . H27B H 0.1947 0.3285 0.2496 0.102 Uiso 1 1 calc R . . C28 C 0.1355(15) 0.2616(7) 0.2065(9) 0.095(6) Uani 1 1 d . . . H28A H 0.0667 0.2821 0.1840 0.114 Uiso 1 1 calc R . . H28B H 0.1033 0.2334 0.2325 0.114 Uiso 1 1 calc R . . C29 C 0.1992(12) 0.2395(6) 0.1434(8) 0.069(4) Uani 1 1 d . . . H29 H 0.1584 0.2091 0.1196 0.082 Uiso 1 1 calc R . . C30 C 0.2659(13) 0.2667(5) 0.0965(7) 0.059(4) Uani 1 1 d . . . H30 H 0.2621 0.2518 0.0464 0.071 Uiso 1 1 calc R . . C31 C 0.2802(17) 0.3232(5) 0.0979(9) 0.084(5) Uani 1 1 d . . . H31A H 0.3016 0.3340 0.0501 0.100 Uiso 1 1 calc R . . H31B H 0.2017 0.3384 0.1024 0.100 Uiso 1 1 calc R . . C32 C 0.3720(16) 0.3442(5) 0.1579(7) 0.072(4) Uani 1 1 d . . . H32A H 0.3365 0.3738 0.1789 0.087 Uiso 1 1 calc R . . H32B H 0.4408 0.3563 0.1352 0.087 Uiso 1 1 calc R . . C33 C 0.124(5) 0.050(2) 0.469(3) 0.35(3) Uani 1 1 d U . . H33A H 0.1598 0.0557 0.5212 0.417 Uiso 1 1 calc R . . H33B H 0.0366 0.0553 0.4652 0.417 Uiso 1 1 calc R . . Cl1 Cl 0.1528(18) -0.0076(8) 0.4443(7) 0.376(9) Uani 1 1 d . . . Cl2 Cl 0.1875(11) 0.0968(6) 0.4102(7) 0.279(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 0.0266(2) 0.0365(2) 0.0340(2) -0.00563(18) 0.00330(18) -0.00664(18) Ir2 0.0292(2) 0.0292(2) 0.0228(2) -0.00293(15) 0.00264(16) -0.00061(17) Rh1 0.0308(5) 0.0332(5) 0.0299(4) -0.0019(3) 0.0013(4) 0.0040(4) Rh2 0.0272(5) 0.0289(4) 0.0271(4) -0.0029(3) 0.0025(3) -0.0023(3) S1 0.0335(16) 0.0350(14) 0.0308(13) -0.0016(11) 0.0047(12) -0.0031(12) S2 0.0313(16) 0.0338(14) 0.0329(14) -0.0051(11) 0.0069(12) -0.0043(11) S3 0.0282(16) 0.0393(15) 0.0280(13) -0.0068(11) 0.0052(11) 0.0035(11) S4 0.0308(16) 0.0379(15) 0.0263(13) -0.0011(11) -0.0022(11) -0.0032(12) B3 0.028(7) 0.029(6) 0.036(7) -0.003(5) -0.010(5) -0.002(5) B4 0.045(9) 0.038(7) 0.041(7) 0.012(6) -0.013(6) 0.003(6) B5 0.053(11) 0.037(8) 0.080(11) 0.008(7) 0.011(9) 0.000(7) B6 0.038(9) 0.028(7) 0.073(10) -0.001(6) 0.001(7) -0.010(6) B7 0.042(9) 0.035(7) 0.047(8) 0.001(6) 0.003(6) -0.003(6) B8 0.048(10) 0.036(8) 0.065(9) 0.017(6) -0.001(8) 0.002(6) B9 0.060(11) 0.044(9) 0.073(11) 0.011(7) 0.001(9) 0.019(7) B10 0.070(12) 0.029(7) 0.068(10) 0.001(7) 0.022(9) 0.001(7) B11 0.029(8) 0.049(8) 0.071(10) -0.004(7) 0.010(7) 0.008(6) B12 0.062(12) 0.035(8) 0.096(13) -0.007(8) 0.020(10) 0.005(7) B13 0.057(10) 0.041(8) 0.038(7) 0.006(6) -0.003(7) 0.000(7) B14 0.065(11) 0.037(7) 0.040(7) 0.008(6) 0.011(7) -0.018(7) B15 0.038(8) 0.048(8) 0.031(7) -0.007(5) 0.008(6) -0.015(6) B16 0.027(7) 0.041(7) 0.027(6) -0.009(5) 0.009(5) -0.001(5) B17 0.069(11) 0.067(10) 0.022(6) -0.014(6) 0.025(7) -0.014(8) B18 0.072(12) 0.068(10) 0.025(7) 0.001(6) 0.021(7) -0.008(8) B19 0.055(10) 0.067(10) 0.037(7) 0.000(7) 0.025(7) -0.005(8) B20 0.041(9) 0.053(8) 0.042(7) -0.011(6) 0.017(7) -0.017(7) B21 0.030(8) 0.045(8) 0.046(7) -0.009(6) 0.017(6) -0.002(6) B22 0.047(10) 0.077(10) 0.037(7) 0.000(7) 0.031(7) -0.001(7) C1 0.045(8) 0.027(6) 0.047(7) 0.002(5) 0.013(6) -0.009(5) C2 0.035(7) 0.031(6) 0.035(6) -0.012(4) 0.004(5) -0.004(5) C3 0.043(7) 0.034(6) 0.029(5) -0.002(4) 0.014(5) -0.010(5) C4 0.040(7) 0.045(6) 0.018(5) -0.004(4) 0.002(5) -0.006(5) C5 0.047(7) 0.073(7) 0.095(8) -0.053(7) -0.014(6) 0.021(6) C6 0.047(7) 0.097(8) 0.067(7) 0.014(7) 0.011(6) -0.017(6) C7 0.076(8) 0.067(7) 0.091(8) -0.002(7) -0.009(7) -0.014(7) C8 0.047(7) 0.083(8) 0.053(6) -0.022(6) 0.001(6) -0.005(6) C9 0.049(7) 0.079(7) 0.075(7) 0.039(6) -0.030(6) -0.037(6) C10 0.198(15) 0.197(15) 0.216(15) -0.040(10) 0.011(10) 0.018(10) C11 0.194(15) 0.228(16) 0.194(15) 0.019(10) 0.038(10) -0.014(10) C12 0.165(13) 0.154(13) 0.186(13) 0.016(9) -0.009(9) -0.017(9) C13 0.133(12) 0.162(12) 0.126(11) -0.039(9) 0.012(9) 0.006(9) C14 0.162(13) 0.170(13) 0.171(13) 0.027(9) -0.013(9) -0.021(9) C15 0.050(8) 0.049(7) 0.023(5) -0.007(5) 0.002(5) -0.001(6) C16 0.055(8) 0.043(7) 0.029(6) -0.002(5) -0.010(6) 0.004(6) C17 0.044(8) 0.096(11) 0.027(6) -0.017(6) -0.003(6) -0.027(7) C18 0.046(8) 0.051(7) 0.033(6) -0.013(5) -0.011(6) 0.005(6) C19 0.051(8) 0.041(7) 0.018(5) 0.002(4) -0.004(5) -0.005(5) C20 0.054(10) 0.146(15) 0.050(8) -0.039(9) 0.018(7) -0.001(9) C21 0.133(16) 0.038(8) 0.067(9) -0.019(7) -0.034(9) 0.005(8) C22 0.079(12) 0.164(17) 0.031(7) -0.016(9) -0.007(7) -0.063(11) C23 0.065(12) 0.132(15) 0.110(13) -0.066(12) -0.038(10) 0.049(11) C24 0.147(16) 0.044(8) 0.044(8) 0.016(6) -0.013(9) -0.029(9) C25 0.057(9) 0.034(6) 0.049(7) -0.014(5) 0.007(6) 0.010(6) C26 0.049(8) 0.047(7) 0.039(6) -0.013(5) 0.006(6) 0.007(6) C27 0.055(11) 0.083(11) 0.118(14) -0.038(10) 0.021(10) 0.007(8) C28 0.054(11) 0.135(16) 0.100(13) -0.024(11) 0.020(10) 0.022(10) C29 0.028(8) 0.092(11) 0.077(10) -0.024(8) -0.022(7) 0.035(7) C30 0.060(10) 0.065(9) 0.048(8) 0.011(6) -0.004(7) 0.014(7) C31 0.112(15) 0.046(9) 0.084(11) 0.015(8) -0.011(10) 0.024(8) C32 0.108(14) 0.053(9) 0.056(8) 0.005(7) 0.014(9) 0.011(8) C33 0.35(3) 0.35(3) 0.34(3) 0.004(10) 0.053(11) 0.005(10) Cl1 0.49(3) 0.43(2) 0.190(11) 0.037(13) 0.004(14) -0.03(2) Cl2 0.212(12) 0.380(17) 0.253(12) -0.061(11) 0.065(10) -0.009(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 C5 2.129(14) . ? Ir1 C9 2.131(13) . ? Ir1 C6 2.157(14) . ? Ir1 C7 2.189(15) . ? Ir1 C8 2.194(13) . ? Ir1 S1 2.332(3) . ? Ir1 S2 2.347(3) . ? Ir1 Rh2 2.5990(10) . ? Ir2 B16 2.139(11) . ? Ir2 C19 2.217(9) . ? Ir2 C18 2.227(11) . ? Ir2 C17 2.279(12) . ? Ir2 C15 2.281(10) . ? Ir2 S3 2.315(3) . ? Ir2 C16 2.326(11) . ? Ir2 Rh1 2.7862(11) . ? Ir2 Rh2 2.9814(10) . ? Rh1 C3 2.132(10) . ? Rh1 C30 2.190(12) . ? Rh1 C29 2.195(12) . ? Rh1 C26 2.234(10) . ? Rh1 C25 2.246(10) . ? Rh1 S3 2.332(3) . ? Rh1 S4 2.365(3) . ? Rh2 S4 2.295(3) . ? Rh2 S3 2.304(3) . ? Rh2 S1 2.390(3) . ? Rh2 S2 2.393(3) . ? S1 C1 1.833(12) . ? S2 C2 1.835(11) . ? S4 C4 1.805(11) . ? B3 C1 1.704(16) . ? B3 C2 1.722(15) . ? B3 B7 1.744(17) . ? B3 B8 1.762(18) . ? B3 B4 1.764(17) . ? B4 C1 1.702(17) . ? B4 B9 1.747(19) . ? B4 B5 1.77(2) . ? B4 B8 1.78(2) . ? B5 C1 1.702(17) . ? B5 B6 1.73(2) . ? B5 B10 1.78(2) . ? B5 B9 1.80(2) . ? B6 C2 1.714(16) . ? B6 C1 1.746(16) . ? B6 B10 1.75(2) . ? B6 B11 1.775(19) . ? B7 C2 1.697(17) . ? B7 B11 1.763(19) . ? B7 B12 1.787(19) . ? B7 B8 1.798(19) . ? B8 B9 1.74(2) . ? B8 B12 1.75(2) . ? B9 B12 1.75(2) . ? B9 B10 1.79(2) . ? B10 B12 1.78(2) . ? B10 B11 1.79(2) . ? B11 C2 1.705(16) . ? B11 B12 1.77(2) . ? B13 C3 1.699(16) . ? B13 C4 1.700(16) . ? B13 B14 1.757(19) . ? B13 B18 1.77(2) . ? B13 B17 1.79(2) . ? B14 C3 1.725(15) . ? B14 B15 1.795(18) . ? B14 B19 1.80(2) . ? B14 B18 1.824(19) . ? B15 B20 1.72(2) . ? B15 C3 1.738(16) . ? B15 B19 1.743(16) . ? B15 B16 1.778(17) . ? B16 C3 1.750(16) . ? B16 C4 1.791(15) . ? B16 B20 1.793(17) . ? B16 B21 1.860(16) . ? B17 C4 1.684(14) . ? B17 B22 1.78(2) . ? B17 B18 1.79(2) . ? B17 B21 1.810(19) . ? B18 B19 1.78(2) . ? B18 B22 1.78(2) . ? B19 B20 1.767(19) . ? B19 B22 1.78(2) . ? B20 B22 1.770(17) . ? B20 B21 1.783(18) . ? B21 C4 1.707(17) . ? B21 B22 1.786(17) . ? C1 C2 1.610(14) . ? C3 C4 1.627(14) . ? C5 C6 1.38(2) . ? C5 C9 1.48(2) . ? C5 C10 1.49(3) . ? C6 C7 1.24(2) . ? C6 C11 1.58(3) . ? C7 C8 1.33(2) . ? C7 C12 1.60(3) . ? C8 C9 1.42(2) . ? C8 C13 1.52(2) . ? C9 C14 1.49(2) . ? C15 C16 1.413(15) . ? C15 C19 1.413(15) . ? C15 C20 1.491(16) . ? C16 C17 1.435(17) . ? C16 C21 1.503(16) . ? C17 C18 1.418(17) . ? C17 C22 1.509(17) . ? C18 C19 1.430(16) . ? C18 C23 1.515(17) . ? C19 C24 1.493(15) . ? C25 C26 1.369(15) . ? C25 C32 1.477(17) . ? C26 C27 1.542(18) . ? C27 C28 1.46(2) . ? C28 C29 1.538(18) . ? C29 C30 1.400(18) . ? C30 C31 1.485(18) . ? C31 C32 1.48(2) . ? C33 Cl1 1.63(5) . ? C33 Cl2 1.82(5) . ? 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 C5 Ir1 C9 40.6(6) . . ? C5 Ir1 C6 37.5(6) . . ? C9 Ir1 C6 63.6(5) . . ? C5 Ir1 C7 59.9(6) . . ? C9 Ir1 C7 61.5(5) . . ? C6 Ir1 C7 33.0(5) . . ? C5 Ir1 C8 63.3(5) . . ? C9 Ir1 C8 38.2(5) . . ? C6 Ir1 C8 59.1(5) . . ? C7 Ir1 C8 35.2(5) . . ? C5 Ir1 S1 117.7(4) . . ? C9 Ir1 S1 156.3(5) . . ? C6 Ir1 S1 105.5(4) . . ? C7 Ir1 S1 121.7(5) . . ? C8 Ir1 S1 155.5(4) . . ? C5 Ir1 S2 154.6(5) . . ? C9 Ir1 S2 116.7(4) . . ? C6 Ir1 S2 158.7(5) . . ? C7 Ir1 S2 126.4(5) . . ? C8 Ir1 S2 106.7(4) . . ? S1 Ir1 S2 81.37(9) . . ? C5 Ir1 Rh2 116.5(4) . . ? C9 Ir1 Rh2 117.3(4) . . ? C6 Ir1 Rh2 143.1(5) . . ? C7 Ir1 Rh2 176.0(5) . . ? C8 Ir1 Rh2 146.1(4) . . ? S1 Ir1 Rh2 57.69(7) . . ? S2 Ir1 Rh2 57.61(6) . . ? B16 Ir2 C19 145.2(5) . . ? B16 Ir2 C18 107.8(5) . . ? C19 Ir2 C18 37.5(4) . . ? B16 Ir2 C17 91.6(4) . . ? C19 Ir2 C17 61.5(4) . . ? C18 Ir2 C17 36.7(5) . . ? B16 Ir2 C15 146.8(4) . . ? C19 Ir2 C15 36.6(4) . . ? C18 Ir2 C15 61.4(4) . . ? C17 Ir2 C15 60.6(4) . . ? B16 Ir2 S3 112.4(3) . . ? C19 Ir2 S3 100.5(3) . . ? C18 Ir2 S3 136.8(3) . . ? C17 Ir2 S3 150.7(3) . . ? C15 Ir2 S3 91.0(3) . . ? B16 Ir2 C16 111.1(4) . . ? C19 Ir2 C16 60.6(4) . . ? C18 Ir2 C16 60.9(4) . . ? C17 Ir2 C16 36.3(4) . . ? C15 Ir2 C16 35.7(4) . . ? S3 Ir2 C16 115.6(3) . . ? B16 Ir2 Rh1 66.6(3) . . ? C19 Ir2 Rh1 147.5(3) . . ? C18 Ir2 Rh1 167.4(3) . . ? C17 Ir2 Rh1 130.8(4) . . ? C15 Ir2 Rh1 116.6(3) . . ? S3 Ir2 Rh1 53.45(7) . . ? C16 Ir2 Rh1 109.6(3) . . ? B16 Ir2 Rh2 88.0(3) . . ? C19 Ir2 Rh2 106.1(3) . . ? C18 Ir2 Rh2 118.6(3) . . ? C17 Ir2 Rh2 152.9(4) . . ? C15 Ir2 Rh2 125.1(3) . . ? S3 Ir2 Rh2 49.64(6) . . ? C16 Ir2 Rh2 160.4(3) . . ? Rh1 Ir2 Rh2 73.32(3) . . ? C3 Rh1 C30 90.6(5) . . ? C3 Rh1 C29 126.5(5) . . ? C30 Rh1 C29 37.2(5) . . ? C3 Rh1 C26 120.1(4) . . ? C30 Rh1 C26 89.5(5) . . ? C29 Rh1 C26 79.9(5) . . ? C3 Rh1 C25 86.0(4) . . ? C30 Rh1 C25 79.3(5) . . ? C29 Rh1 C25 92.1(5) . . ? C26 Rh1 C25 35.6(4) . . ? C3 Rh1 S3 131.5(3) . . ? C30 Rh1 S3 132.6(4) . . ? C29 Rh1 S3 95.8(4) . . ? C26 Rh1 S3 86.3(3) . . ? C25 Rh1 S3 118.4(3) . . ? C3 Rh1 S4 75.0(3) . . ? C30 Rh1 S4 92.3(4) . . ? C29 Rh1 S4 92.4(4) . . ? C26 Rh1 S4 164.8(3) . . ? C25 Rh1 S4 159.2(3) . . ? S3 Rh1 S4 81.31(9) . . ? C3 Rh1 Ir2 83.8(3) . . ? C30 Rh1 Ir2 174.3(4) . . ? C29 Rh1 Ir2 148.4(4) . . ? C26 Rh1 Ir2 92.8(3) . . ? C25 Rh1 Ir2 99.6(3) . . ? S3 Rh1 Ir2 52.87(7) . . ? S4 Rh1 Ir2 86.91(7) . . ? S4 Rh2 S3 83.43(10) . . ? S4 Rh2 S1 155.57(10) . . ? S3 Rh2 S1 100.67(9) . . ? S4 Rh2 S2 94.88(9) . . ? S3 Rh2 S2 175.70(10) . . ? S1 Rh2 S2 79.25(9) . . ? S4 Rh2 Ir1 101.49(7) . . ? S3 Rh2 Ir1 120.49(8) . . ? S1 Rh2 Ir1 55.55(7) . . ? S2 Rh2 Ir1 55.91(7) . . ? S4 Rh2 Ir2 83.66(7) . . ? S3 Rh2 Ir2 49.95(7) . . ? S1 Rh2 Ir2 117.54(7) . . ? S2 Rh2 Ir2 133.90(7) . . ? Ir1 Rh2 Ir2 168.99(3) . . ? C1 S1 Ir1 104.1(4) . . ? C1 S1 Rh2 103.3(3) . . ? Ir1 S1 Rh2 66.76(7) . . ? C2 S2 Ir1 103.6(3) . . ? C2 S2 Rh2 103.5(3) . . ? Ir1 S2 Rh2 66.48(7) . . ? Rh2 S3 Ir2 80.41(8) . . ? Rh2 S3 Rh1 96.06(9) . . ? Ir2 S3 Rh1 73.68(8) . . ? C4 S4 Rh2 110.9(4) . . ? C4 S4 Rh1 81.6(3) . . ? Rh2 S4 Rh1 95.40(9) . . ? C1 B3 C2 56.1(6) . . ? C1 B3 B7 105.0(8) . . ? C2 B3 B7 58.6(7) . . ? C1 B3 B8 105.9(9) . . ? C2 B3 B8 105.5(9) . . ? B7 B3 B8 61.7(8) . . ? C1 B3 B4 58.7(7) . . ? C2 B3 B4 103.7(8) . . ? B7 B3 B4 109.5(9) . . ? B8 B3 B4 60.6(7) . . ? C1 B4 B9 106.3(10) . . ? C1 B4 B3 58.9(6) . . ? B9 B4 B3 107.2(10) . . ? C1 B4 B5 58.8(7) . . ? B9 B4 B5 61.8(9) . . ? B3 B4 B5 107.9(9) . . ? C1 B4 B8 105.2(9) . . ? B9 B4 B8 59.0(8) . . ? B3 B4 B8 59.6(7) . . ? B5 B4 B8 108.6(10) . . ? C1 B5 B6 61.1(7) . . ? C1 B5 B4 58.7(7) . . ? B6 B5 B4 109.7(10) . . ? C1 B5 B10 106.2(10) . . ? B6 B5 B10 59.8(9) . . ? B4 B5 B10 107.8(11) . . ? C1 B5 B9 103.7(10) . . ? B6 B5 B9 107.8(11) . . ? B4 B5 B9 58.5(8) . . ? B10 B5 B9 60.0(9) . . ? C2 B6 B5 103.9(10) . . ? C2 B6 C1 55.5(6) . . ? B5 B6 C1 58.6(7) . . ? C2 B6 B10 105.5(10) . . ? B5 B6 B10 61.4(8) . . ? C1 B6 B10 105.6(10) . . ? C2 B6 B11 58.5(7) . . ? B5 B6 B11 109.1(11) . . ? C1 B6 B11 103.4(9) . . ? B10 B6 B11 61.0(8) . . ? C2 B7 B3 60.0(7) . . ? C2 B7 B11 59.0(7) . . ? B3 B7 B11 109.2(10) . . ? C2 B7 B12 103.9(9) . . ? B3 B7 B12 106.4(9) . . ? B11 B7 B12 59.7(8) . . ? C2 B7 B8 105.0(9) . . ? B3 B7 B8 59.6(7) . . ? B11 B7 B8 107.3(10) . . ? B12 B7 B8 58.4(8) . . ? B9 B8 B12 60.2(9) . . ? B9 B8 B3 107.7(10) . . ? B12 B8 B3 107.3(11) . . ? B9 B8 B4 59.5(8) . . ? B12 B8 B4 107.1(11) . . ? B3 B8 B4 59.7(7) . . ? B9 B8 B7 108.2(11) . . ? B12 B8 B7 60.5(8) . . ? B3 B8 B7 58.6(7) . . ? B4 B8 B7 106.4(10) . . ? B8 B9 B4 61.4(8) . . ? B8 B9 B12 60.2(9) . . ? B4 B9 B12 108.6(10) . . ? B8 B9 B10 109.3(11) . . ? B4 B9 B10 108.2(10) . . ? B12 B9 B10 60.2(9) . . ? B8 B9 B5 108.7(10) . . ? B4 B9 B5 59.6(8) . . ? B12 B9 B5 107.0(12) . . ? B10 B9 B5 59.4(9) . . ? B6 B10 B12 107.4(10) . . ? B6 B10 B5 58.7(8) . . ? B12 B10 B5 106.8(11) . . ? B6 B10 B11 60.1(8) . . ? B12 B10 B11 59.4(8) . . ? B5 B10 B11 106.3(10) . . ? B6 B10 B9 107.4(10) . . ? B12 B10 B9 58.7(9) . . ? B5 B10 B9 60.6(9) . . ? B11 B10 B9 106.2(10) . . ? C2 B11 B7 58.6(7) . . ? C2 B11 B12 104.5(10) . . ? B7 B11 B12 60.8(8) . . ? C2 B11 B6 59.0(7) . . ? B7 B11 B6 108.3(10) . . ? B12 B11 B6 106.9(11) . . ? C2 B11 B10 104.4(9) . . ? B7 B11 B10 109.0(11) . . ? B12 B11 B10 59.9(9) . . ? B6 B11 B10 59.0(8) . . ? B8 B12 B9 59.6(9) . . ? B8 B12 B11 109.4(11) . . ? B9 B12 B11 109.2(11) . . ? B8 B12 B10 109.6(11) . . ? B9 B12 B10 61.2(9) . . ? B11 B12 B10 60.7(9) . . ? B8 B12 B7 61.1(8) . . ? B9 B12 B7 108.2(10) . . ? B11 B12 B7 59.5(8) . . ? B10 B12 B7 108.5(11) . . ? C3 B13 C4 57.2(6) . . ? C3 B13 B14 59.9(7) . . ? C4 B13 B14 105.8(9) . . ? C3 B13 B18 106.8(10) . . ? C4 B13 B18 103.9(10) . . ? B14 B13 B18 62.2(8) . . ? C3 B13 B17 105.2(9) . . ? C4 B13 B17 57.6(7) . . ? B14 B13 B17 110.5(11) . . ? B18 B13 B17 60.1(8) . . ? C3 B14 B13 58.4(7) . . ? C3 B14 B15 59.1(7) . . ? B13 B14 B15 106.8(9) . . ? C3 B14 B19 103.4(9) . . ? B13 B14 B19 106.0(10) . . ? B15 B14 B19 57.9(7) . . ? C3 B14 B18 103.5(9) . . ? B13 B14 B18 59.4(8) . . ? B15 B14 B18 104.9(10) . . ? B19 B14 B18 58.7(8) . . ? B20 B15 C3 105.2(9) . . ? B20 B15 B19 61.4(8) . . ? C3 B15 B19 105.4(9) . . ? B20 B15 B16 61.7(7) . . ? C3 B15 B16 59.7(7) . . ? B19 B15 B16 112.3(9) . . ? B20 B15 B14 110.5(9) . . ? C3 B15 B14 58.4(7) . . ? B19 B15 B14 61.3(8) . . ? B16 B15 B14 111.1(9) . . ? C3 B16 B15 59.0(7) . . ? C3 B16 C4 54.7(6) . . ? B15 B16 C4 100.2(8) . . ? C3 B16 B20 101.6(8) . . ? B15 B16 B20 57.5(7) . . ? C4 B16 B20 98.6(7) . . ? C3 B16 B21 101.0(8) . . ? B15 B16 B21 104.1(8) . . ? C4 B16 B21 55.7(6) . . ? B20 B16 B21 58.4(6) . . ? C3 B16 Ir2 116.9(7) . . ? B15 B16 Ir2 125.8(7) . . ? C4 B16 Ir2 120.6(7) . . ? B20 B16 Ir2 135.8(8) . . ? B21 B16 Ir2 127.6(7) . . ? C4 B17 B22 103.2(9) . . ? C4 B17 B18 104.1(9) . . ? B22 B17 B18 59.9(9) . . ? C4 B17 B13 58.5(7) . . ? B22 B17 B13 106.6(10) . . ? B18 B17 B13 59.5(8) . . ? C4 B17 B21 58.4(6) . . ? B22 B17 B21 59.7(7) . . ? B18 B17 B21 108.2(10) . . ? B13 B17 B21 107.6(8) . . ? B13 B18 B19 106.4(9) . . ? B13 B18 B22 107.4(9) . . ? B19 B18 B22 60.1(8) . . ? B13 B18 B17 60.5(8) . . ? B19 B18 B17 108.0(10) . . ? B22 B18 B17 59.9(8) . . ? B13 B18 B14 58.4(7) . . ? B19 B18 B14 60.1(8) . . ? B22 B18 B14 108.0(9) . . ? B17 B18 B14 107.7(9) . . ? B15 B19 B20 58.6(7) . . ? B15 B19 B18 109.1(10) . . ? B20 B19 B18 108.0(10) . . ? B15 B19 B22 107.1(9) . . ? B20 B19 B22 59.8(7) . . ? B18 B19 B22 60.0(8) . . ? B15 B19 B14 60.8(7) . . ? B20 B19 B14 107.8(9) . . ? B18 B19 B14 61.2(8) . . ? B22 B19 B14 108.8(10) . . ? B15 B20 B19 60.0(8) . . ? B15 B20 B22 108.8(11) . . ? B19 B20 B22 60.5(8) . . ? B15 B20 B21 110.1(10) . . ? B19 B20 B21 109.5(10) . . ? B22 B20 B21 60.4(7) . . ? B15 B20 B16 60.8(7) . . ? B19 B20 B16 110.5(10) . . ? B22 B20 B16 111.5(10) . . ? B21 B20 B16 62.7(7) . . ? C4 B21 B20 102.3(9) . . ? C4 B21 B22 102.0(9) . . ? B20 B21 B22 59.4(7) . . ? C4 B21 B17 57.1(7) . . ? B20 B21 B17 106.3(10) . . ? B22 B21 B17 59.3(8) . . ? C4 B21 B16 60.1(6) . . ? B20 B21 B16 58.9(7) . . ? B22 B21 B16 107.7(9) . . ? B17 B21 B16 108.7(9) . . ? B20 B22 B17 108.2(9) . . ? B20 B22 B18 107.8(10) . . ? B17 B22 B18 60.2(9) . . ? B20 B22 B19 59.7(7) . . ? B17 B22 B19 108.0(11) . . ? B18 B22 B19 59.9(8) . . ? B20 B22 B21 60.2(7) . . ? B17 B22 B21 61.0(7) . . ? B18 B22 B21 109.5(10) . . ? B19 B22 B21 108.7(8) . . ? C2 C1 B4 111.7(9) . . ? C2 C1 B5 110.0(9) . . ? B4 C1 B5 62.5(8) . . ? C2 C1 B3 62.5(6) . . ? B4 C1 B3 62.4(7) . . ? B5 C1 B3 113.9(10) . . ? C2 C1 B6 61.3(7) . . ? B4 C1 B6 112.3(9) . . ? B5 C1 B6 60.4(8) . . ? B3 C1 B6 114.1(9) . . ? C2 C1 S1 113.2(7) . . ? B4 C1 S1 125.3(8) . . ? B5 C1 S1 124.7(8) . . ? B3 C1 S1 115.9(7) . . ? B6 C1 S1 115.8(8) . . ? C1 C2 B7 111.5(9) . . ? C1 C2 B11 112.9(9) . . ? B7 C2 B11 62.4(7) . . ? C1 C2 B6 63.3(7) . . ? B7 C2 B6 114.5(9) . . ? B11 C2 B6 62.5(7) . . ? C1 C2 B3 61.4(7) . . ? B7 C2 B3 61.3(7) . . ? B11 C2 B3 113.0(9) . . ? B6 C2 B3 114.8(9) . . ? C1 C2 S2 113.0(7) . . ? B7 C2 S2 123.3(7) . . ? B11 C2 S2 124.4(8) . . ? B6 C2 S2 115.9(8) . . ? B3 C2 S2 115.5(7) . . ? C4 C3 B13 61.5(6) . . ? C4 C3 B14 110.6(8) . . ? B13 C3 B14 61.7(7) . . ? C4 C3 B15 108.9(8) . . ? B13 C3 B15 112.1(8) . . ? B14 C3 B15 62.4(7) . . ? C4 C3 B16 63.9(6) . . ? B13 C3 B16 117.5(8) . . ? B14 C3 B16 116.0(9) . . ? B15 C3 B16 61.3(7) . . ? C4 C3 Rh1 93.4(6) . . ? B13 C3 Rh1 120.7(8) . . ? B14 C3 Rh1 150.1(8) . . ? B15 C3 Rh1 127.1(6) . . ? B16 C3 Rh1 90.0(5) . . ? C3 C4 B17 113.8(8) . . ? C3 C4 B13 61.3(7) . . ? B17 C4 B13 64.0(8) . . ? C3 C4 B21 113.3(8) . . ? B17 C4 B21 64.5(8) . . ? B13 C4 B21 117.1(9) . . ? C3 C4 B16 61.4(6) . . ? B17 C4 B16 118.2(9) . . ? B13 C4 B16 115.2(8) . . ? B21 C4 B16 64.2(7) . . ? C3 C4 S4 106.0(7) . . ? B17 C4 S4 126.4(8) . . ? B13 C4 S4 110.8(8) . . ? B21 C4 S4 128.1(8) . . ? B16 C4 S4 111.7(6) . . ? C6 C5 C9 104.5(12) . . ? C6 C5 C10 122.4(19) . . ? C9 C5 C10 132.8(19) . . ? C6 C5 Ir1 72.4(8) . . ? C9 C5 Ir1 69.8(8) . . ? C10 C5 Ir1 126.3(14) . . ? C7 C6 C5 111.1(14) . . ? C7 C6 C11 125.8(19) . . ? C5 C6 C11 123.1(18) . . ? C7 C6 Ir1 74.9(10) . . ? C5 C6 Ir1 70.2(8) . . ? C11 C6 Ir1 123.3(15) . . ? C6 C7 C8 113.9(15) . . ? C6 C7 C12 119.8(18) . . ? C8 C7 C12 126.1(18) . . ? C6 C7 Ir1 72.1(10) . . ? C8 C7 Ir1 72.6(9) . . ? C12 C7 Ir1 127.9(14) . . ? C7 C8 C9 107.3(13) . . ? C7 C8 C13 126.1(17) . . ? C9 C8 C13 126.5(16) . . ? C7 C8 Ir1 72.2(9) . . ? C9 C8 Ir1 68.5(7) . . ? C13 C8 Ir1 123.1(12) . . ? C8 C9 C5 103.2(11) . . ? C8 C9 C14 118.0(17) . . ? C5 C9 C14 138.6(18) . . ? C8 C9 Ir1 73.3(8) . . ? C5 C9 Ir1 69.6(7) . . ? C14 C9 Ir1 123.6(12) . . ? C16 C15 C19 108.6(10) . . ? C16 C15 C20 126.3(11) . . ? C19 C15 C20 124.6(11) . . ? C16 C15 Ir2 73.9(6) . . ? C19 C15 Ir2 69.2(5) . . ? C20 C15 Ir2 129.2(9) . . ? C15 C16 C17 107.7(10) . . ? C15 C16 C21 127.9(12) . . ? C17 C16 C21 123.4(13) . . ? C15 C16 Ir2 70.4(6) . . ? C17 C16 Ir2 70.1(6) . . ? C21 C16 Ir2 133.9(8) . . ? C18 C17 C16 107.9(10) . . ? C18 C17 C22 124.4(14) . . ? C16 C17 C22 125.6(13) . . ? C18 C17 Ir2 69.7(6) . . ? C16 C17 Ir2 73.7(7) . . ? C22 C17 Ir2 135.1(8) . . ? C17 C18 C19 107.7(10) . . ? C17 C18 C23 123.4(13) . . ? C19 C18 C23 128.3(13) . . ? C17 C18 Ir2 73.6(7) . . ? C19 C18 Ir2 70.8(6) . . ? C23 C18 Ir2 128.1(8) . . ? C15 C19 C18 108.1(10) . . ? C15 C19 C24 124.8(11) . . ? C18 C19 C24 126.7(12) . . ? C15 C19 Ir2 74.2(6) . . ? C18 C19 Ir2 71.6(6) . . ? C24 C19 Ir2 125.6(8) . . ? C26 C25 C32 126.1(13) . . ? C26 C25 Rh1 71.7(6) . . ? C32 C25 Rh1 109.5(8) . . ? C25 C26 C27 122.3(12) . . ? C25 C26 Rh1 72.7(6) . . ? C27 C26 Rh1 111.1(8) . . ? C28 C27 C26 116.4(12) . . ? C27 C28 C29 115.3(14) . . ? C30 C29 C28 126.8(14) . . ? C30 C29 Rh1 71.2(7) . . ? C28 C29 Rh1 110.8(9) . . ? C29 C30 C31 124.1(13) . . ? C29 C30 Rh1 71.6(7) . . ? C31 C30 Rh1 113.0(10) . . ? C32 C31 C30 116.2(12) . . ? C31 C32 C25 117.4(12) . . ? Cl1 C33 Cl2 110(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.917 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.179 data_f50324c _database_code_depnum_ccdc_archive 'CCDC 281884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H63 B20 Cl2 Ir2 Rh2 Se4' _chemical_formula_weight 1652.99 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.104(3) _cell_length_b 26.517(6) _cell_length_c 18.003(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.155(4) _cell_angle_gamma 90.00 _cell_volume 5247(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 842 _cell_measurement_theta_min 2.411 _cell_measurement_theta_max 17.773 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.092 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3100 _exptl_absorpt_coefficient_mu 8.578 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2788 _exptl_absorpt_correction_T_max 0.2788 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _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 22009 _diffrn_reflns_av_R_equivalents 0.0857 _diffrn_reflns_av_sigmaI/netI 0.1180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9264 _reflns_number_gt 5833 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. The solvent molecules were disordered. C33 Cl1 Cl2 atoms refined with anisotropic restraint. The C5 C6 C7 C8 C9 C10 C11 C12 C13 C14 C20 C22 C23 C24 atoms of the Cp ring is disordered in some way. These atoms were refined with anisotropic restraints. The 102 restraints refer to anisotropical B parameters of these atoms. The Cp ring was not modelled as disordered. ; _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^)+(0.0584P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9264 _refine_ls_number_parameters 595 _refine_ls_number_restraints 102 _refine_ls_R_factor_all 0.1059 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.27142(5) 0.02713(2) 0.65284(3) 0.03249(17) Uani 1 1 d . . . Ir2 Ir 0.57607(5) 0.18323(2) 0.77832(3) 0.02737(16) Uani 1 1 d . . . Rh1 Rh 0.39416(10) 0.23155(4) 0.67734(6) 0.0315(3) Uani 1 1 d . . . Rh2 Rh 0.42734(10) 0.09840(4) 0.70154(6) 0.0293(3) Uani 1 1 d . . . Se1 Se 0.37286(13) 0.02811(5) 0.78173(8) 0.0348(4) Uani 1 1 d . . . Se2 Se 0.47934(13) 0.02654(5) 0.62305(8) 0.0346(4) Uani 1 1 d . . . Se3 Se 0.35777(13) 0.16762(5) 0.77047(8) 0.0337(4) Uani 1 1 d . . . Se4 Se 0.39294(13) 0.15545(5) 0.59738(7) 0.0334(4) Uani 1 1 d . . . C1 C 0.5116(14) -0.0196(5) 0.7784(8) 0.040(4) Uani 1 1 d . . . C2 C 0.5633(13) -0.0214(5) 0.6990(8) 0.034(3) Uani 1 1 d . . . C3 C 0.5403(14) 0.2444(6) 0.6141(7) 0.041(4) Uani 1 1 d . . . C4 C 0.5484(13) 0.1857(5) 0.5847(7) 0.034(3) Uani 1 1 d . . . C5 C 0.1389(16) 0.0409(7) 0.5556(9) 0.058(5) Uani 1 1 d U . . C6 C 0.0945(18) 0.0548(8) 0.6190(14) 0.080(6) Uani 1 1 d U . . C7 C 0.0879(19) 0.0148(10) 0.6639(11) 0.084(6) Uani 1 1 d U . . C8 C 0.1202(17) -0.0259(7) 0.6297(11) 0.065(5) Uani 1 1 d U . . C9 C 0.1614(16) -0.0103(7) 0.5642(10) 0.060(5) Uani 1 1 d U . . C10 C 0.167(3) 0.0692(12) 0.4866(16) 0.178(13) Uani 1 1 d U . . H10A H 0.1243 0.0537 0.4423 0.267 Uiso 1 1 calc R . . H10B H 0.2530 0.0680 0.4847 0.267 Uiso 1 1 calc R . . H10C H 0.1416 0.1036 0.4892 0.267 Uiso 1 1 calc R . . C11 C 0.056(4) 0.1082(15) 0.631(2) 0.26(2) Uani 1 1 d U . . H11A H -0.0286 0.1121 0.6111 0.394 Uiso 1 1 calc R . . H11B H 0.1035 0.1308 0.6050 0.394 Uiso 1 1 calc R . . H11C H 0.0682 0.1158 0.6833 0.394 Uiso 1 1 calc R . . C12 C 0.033(5) 0.0248(17) 0.739(3) 0.30(3) Uani 1 1 d U . . H12A H -0.0517 0.0164 0.7315 0.452 Uiso 1 1 calc R . . H12B H 0.0433 0.0597 0.7523 0.452 Uiso 1 1 calc R . . H12C H 0.0751 0.0043 0.7783 0.452 Uiso 1 1 calc R . . C13 C 0.115(4) -0.0757(15) 0.665(2) 0.25(2) Uani 1 1 d U . . H13A H 0.1703 -0.0765 0.7110 0.372 Uiso 1 1 calc R . . H13B H 0.1365 -0.1012 0.6317 0.372 Uiso 1 1 calc R . . H13C H 0.0335 -0.0817 0.6756 0.372 Uiso 1 1 calc R . . C14 C 0.206(3) -0.0420(10) 0.5013(15) 0.149(11) Uani 1 1 d U . . H14A H 0.1469 -0.0401 0.4569 0.224 Uiso 1 1 calc R . . H14B H 0.2156 -0.0765 0.5172 0.224 Uiso 1 1 calc R . . H14C H 0.2822 -0.0291 0.4908 0.224 Uiso 1 1 calc R . . C15 C 0.5839(13) 0.2006(6) 0.9031(7) 0.038(4) Uani 1 1 d . . . C16 C 0.6414(16) 0.1543(5) 0.8928(7) 0.045(4) Uani 1 1 d . . . C17 C 0.7437(14) 0.1644(7) 0.8556(9) 0.048(4) Uani 1 1 d . . . C18 C 0.7510(15) 0.2150(7) 0.8443(8) 0.047(4) Uani 1 1 d . . . C19 C 0.6500(15) 0.2385(6) 0.8730(9) 0.047(4) Uani 1 1 d . . . C20 C 0.4852(16) 0.2075(7) 0.9498(9) 0.063(5) Uani 1 1 d U . . H20A H 0.5201 0.2142 1.0008 0.095 Uiso 1 1 calc R . . H20B H 0.4368 0.1774 0.9480 0.095 Uiso 1 1 calc R . . H20C H 0.4348 0.2354 0.9309 0.095 Uiso 1 1 calc R . . C21 C 0.6042(18) 0.1036(6) 0.9260(9) 0.072(6) Uani 1 1 d . . . H21A H 0.6335 0.1027 0.9787 0.108 Uiso 1 1 calc R . . H21B H 0.6389 0.0762 0.9014 0.108 Uiso 1 1 calc R . . H21C H 0.5172 0.1007 0.9183 0.108 Uiso 1 1 calc R . . C22 C 0.8415(18) 0.1274(7) 0.8429(11) 0.083(6) Uani 1 1 d U . . H22A H 0.8121 0.0936 0.8472 0.125 Uiso 1 1 calc R . . H22B H 0.9119 0.1327 0.8796 0.125 Uiso 1 1 calc R . . H22C H 0.8630 0.1322 0.7936 0.125 Uiso 1 1 calc R . . C23 C 0.8607(18) 0.2434(8) 0.8234(10) 0.086(6) Uani 1 1 d U . . H23A H 0.9185 0.2488 0.8677 0.129 Uiso 1 1 calc R . . H23B H 0.8348 0.2753 0.8016 0.129 Uiso 1 1 calc R . . H23C H 0.8979 0.2240 0.7879 0.129 Uiso 1 1 calc R . . C24 C 0.6394(18) 0.2962(7) 0.8860(10) 0.076(6) Uani 1 1 d U . . H24A H 0.5571 0.3044 0.8918 0.114 Uiso 1 1 calc R . . H24B H 0.6619 0.3140 0.8437 0.114 Uiso 1 1 calc R . . H24C H 0.6927 0.3057 0.9305 0.114 Uiso 1 1 calc R . . C25 C 0.4287(16) 0.3107(6) 0.7188(9) 0.052(4) Uani 1 1 d . . . H25 H 0.5114 0.3170 0.7442 0.063 Uiso 1 1 calc R . . C26 C 0.3516(14) 0.2881(6) 0.7632(9) 0.046(4) Uani 1 1 d . . . H26 H 0.3903 0.2807 0.8144 0.055 Uiso 1 1 calc R . . C27 C 0.2184(16) 0.2981(8) 0.7570(10) 0.071(6) Uani 1 1 d . . . H27A H 0.2054 0.3339 0.7480 0.086 Uiso 1 1 calc R . . H27B H 0.1930 0.2906 0.8052 0.086 Uiso 1 1 calc R . . C28 C 0.1361(18) 0.2700(8) 0.6979(11) 0.081(6) Uani 1 1 d . . . H28A H 0.0952 0.2434 0.7217 0.097 Uiso 1 1 calc R . . H28B H 0.0743 0.2929 0.6741 0.097 Uiso 1 1 calc R . . C29 C 0.2002(15) 0.2472(7) 0.6391(10) 0.056(5) Uani 1 1 d . . . H29 H 0.1571 0.2179 0.6150 0.067 Uiso 1 1 calc R . . C30 C 0.2728(15) 0.2719(6) 0.5918(9) 0.054(5) Uani 1 1 d . . . H30 H 0.2675 0.2570 0.5416 0.065 Uiso 1 1 calc R . . C31 C 0.2922(19) 0.3284(6) 0.5935(12) 0.080(6) Uani 1 1 d . . . H31A H 0.3167 0.3384 0.5461 0.095 Uiso 1 1 calc R . . H31B H 0.2148 0.3445 0.5970 0.095 Uiso 1 1 calc R . . C32 C 0.383(2) 0.3484(7) 0.6551(10) 0.083(7) Uani 1 1 d . . . H32A H 0.3482 0.3773 0.6770 0.099 Uiso 1 1 calc R . . H32B H 0.4533 0.3603 0.6333 0.099 Uiso 1 1 calc R . . C33 C 0.123(4) 0.0503(16) 0.963(2) 0.221(18) Uani 1 1 d U . . H33A H 0.1505 0.0562 1.0158 0.265 Uiso 1 1 calc R . . H33B H 0.0359 0.0547 0.9546 0.265 Uiso 1 1 calc R . . B3 B 0.6486(16) 0.0074(6) 0.7762(9) 0.036(4) Uani 1 1 d . . . H3 H 0.6680 0.0479 0.7823 0.043 Uiso 1 1 calc R . . B4 B 0.620(2) -0.0294(7) 0.8517(11) 0.061(6) Uani 1 1 d . . . H4 H 0.6198 -0.0132 0.9080 0.073 Uiso 1 1 calc R . . B5 B 0.5147(19) -0.0776(7) 0.8177(11) 0.053(5) Uani 1 1 d . . . H5 H 0.4472 -0.0917 0.8518 0.063 Uiso 1 1 calc R . . B6 B 0.4790(17) -0.0724(6) 0.7218(11) 0.042(5) Uani 1 1 d . . . H6 H 0.3884 -0.0831 0.6933 0.051 Uiso 1 1 calc R . . B7 B 0.7149(17) -0.0305(7) 0.7120(11) 0.053(5) Uani 1 1 d . . . H7 H 0.7779 -0.0147 0.6762 0.063 Uiso 1 1 calc R . . B8 B 0.7535(19) -0.0375(7) 0.8122(11) 0.054(5) Uani 1 1 d . . . H8 H 0.8427 -0.0268 0.8427 0.065 Uiso 1 1 calc R . . B9 B 0.6737(19) -0.0913(7) 0.8366(12) 0.057(6) Uani 1 1 d . . . H9 H 0.7121 -0.1158 0.8833 0.068 Uiso 1 1 calc R . . B10 B 0.586(2) -0.1177(9) 0.7565(12) 0.065(6) Uani 1 1 d . . . H10 H 0.5680 -0.1584 0.7512 0.078 Uiso 1 1 calc R . . B11 B 0.6101(18) -0.0798(6) 0.6795(13) 0.052(5) Uani 1 1 d . . . H11 H 0.6056 -0.0955 0.6226 0.063 Uiso 1 1 calc R . . B12 B 0.731(2) -0.0915(7) 0.7517(12) 0.064(6) Uani 1 1 d . . . H12 H 0.8085 -0.1156 0.7424 0.077 Uiso 1 1 calc R . . B13 B 0.5253(18) 0.2335(7) 0.5190(9) 0.045(5) Uani 1 1 d . . . H13 H 0.4410 0.2403 0.4802 0.054 Uiso 1 1 calc R . . B14 B 0.6165(18) 0.2834(7) 0.5599(10) 0.046(5) Uani 1 1 d . . . H14 H 0.5919 0.3230 0.5474 0.056 Uiso 1 1 calc R . . B15 B 0.6849(16) 0.2634(7) 0.6502(10) 0.040(4) Uani 1 1 d . . . H15 H 0.7056 0.2910 0.6958 0.048 Uiso 1 1 calc R . . B16 B 0.6331(14) 0.2025(6) 0.6726(8) 0.029(4) Uani 1 1 d . . . B17 B 0.6225(16) 0.1804(7) 0.5094(10) 0.044(5) Uani 1 1 d . . . H17 H 0.6012 0.1532 0.4632 0.053 Uiso 1 1 calc R . . B18 B 0.6722(18) 0.2435(7) 0.4937(10) 0.051(5) Uani 1 1 d . . . H18 H 0.6849 0.2574 0.4377 0.061 Uiso 1 1 calc R . . B19 B 0.7716(19) 0.2618(8) 0.5757(10) 0.054(5) Uani 1 1 d . . . H19 H 0.8486 0.2875 0.5728 0.064 Uiso 1 1 calc R . . B20 B 0.7815(16) 0.2106(7) 0.6416(9) 0.038(4) Uani 1 1 d . . . H20 H 0.8651 0.2030 0.6807 0.046 Uiso 1 1 calc R . . B21 B 0.6880(17) 0.1594(7) 0.6013(10) 0.048(5) Uani 1 1 d . . . H21 H 0.7075 0.1194 0.6142 0.058 Uiso 1 1 calc R . . B22 B 0.7734(19) 0.1975(7) 0.5446(9) 0.052(5) Uani 1 1 d . . . H22 H 0.8514 0.1817 0.5211 0.063 Uiso 1 1 calc R . . Cl1 Cl 0.1865(11) 0.0963(4) 0.9130(6) 0.206(4) Uani 1 1 d U . . Cl2 Cl 0.1537(14) -0.0102(6) 0.9440(8) 0.262(6) 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 0.0242(3) 0.0367(4) 0.0362(3) -0.0040(3) 0.0028(2) -0.0050(3) Ir2 0.0257(3) 0.0304(3) 0.0257(3) -0.0025(2) 0.0025(2) -0.0010(2) Rh1 0.0289(7) 0.0317(7) 0.0331(6) -0.0015(5) 0.0019(5) 0.0038(5) Rh2 0.0263(6) 0.0287(6) 0.0322(6) -0.0005(5) 0.0014(5) -0.0019(5) Se1 0.0330(9) 0.0363(9) 0.0355(8) 0.0000(7) 0.0062(6) -0.0016(7) Se2 0.0301(8) 0.0382(9) 0.0357(8) -0.0037(7) 0.0056(6) -0.0035(7) Se3 0.0276(8) 0.0384(9) 0.0357(8) -0.0019(6) 0.0067(6) 0.0000(6) Se4 0.0310(9) 0.0362(9) 0.0316(8) -0.0015(6) -0.0009(6) -0.0032(6) C1 0.042(10) 0.030(9) 0.053(10) -0.003(7) 0.022(8) 0.005(7) C2 0.030(8) 0.038(9) 0.038(8) -0.010(7) 0.014(7) -0.005(7) C3 0.040(10) 0.053(10) 0.029(8) -0.005(7) -0.003(7) 0.013(8) C4 0.042(9) 0.034(8) 0.024(7) -0.011(6) -0.002(6) -0.009(7) C5 0.048(8) 0.070(9) 0.050(8) 0.027(7) -0.009(6) -0.019(7) C6 0.061(9) 0.059(9) 0.113(10) -0.035(8) -0.007(8) 0.013(7) C7 0.069(10) 0.120(11) 0.067(9) -0.009(8) 0.023(8) -0.018(8) C8 0.056(8) 0.050(8) 0.078(9) 0.031(7) -0.026(7) -0.023(7) C9 0.050(8) 0.070(9) 0.056(8) -0.038(7) -0.004(7) 0.004(7) C10 0.170(16) 0.184(16) 0.175(15) 0.018(10) 0.004(10) -0.024(10) C11 0.25(2) 0.25(2) 0.28(2) -0.018(10) 0.021(10) 0.008(10) C12 0.29(3) 0.32(3) 0.29(3) -0.008(10) 0.047(11) -0.006(10) C13 0.24(2) 0.24(2) 0.26(2) 0.025(10) 0.021(10) -0.020(10) C14 0.142(14) 0.151(14) 0.154(13) -0.043(9) 0.015(9) 0.015(9) C15 0.030(9) 0.054(10) 0.028(8) -0.009(7) 0.001(6) 0.000(7) C16 0.071(13) 0.032(9) 0.024(8) -0.001(7) -0.018(8) 0.012(8) C17 0.026(9) 0.068(12) 0.052(10) -0.021(9) 0.009(8) 0.006(8) C18 0.044(11) 0.065(12) 0.028(8) 0.001(8) -0.006(7) -0.024(9) C19 0.041(10) 0.045(10) 0.052(10) -0.007(8) -0.005(8) 0.006(8) C20 0.051(8) 0.083(9) 0.058(8) -0.015(7) 0.013(7) 0.002(7) C21 0.108(18) 0.054(12) 0.046(11) 0.012(9) -0.016(10) -0.021(11) C22 0.073(10) 0.091(10) 0.084(9) -0.021(8) 0.004(8) 0.011(8) C23 0.082(10) 0.104(10) 0.067(9) -0.001(8) -0.004(8) -0.024(8) C24 0.086(10) 0.063(9) 0.073(9) -0.009(7) -0.009(8) -0.002(8) C25 0.046(11) 0.043(10) 0.069(12) -0.020(9) 0.008(9) 0.000(8) C26 0.037(10) 0.043(10) 0.055(10) -0.023(8) 0.001(8) 0.010(8) C27 0.054(13) 0.093(15) 0.073(13) -0.021(11) 0.027(10) 0.006(11) C28 0.063(14) 0.100(17) 0.078(14) -0.014(12) 0.005(11) 0.033(12) C29 0.041(11) 0.058(12) 0.066(12) -0.006(9) -0.002(9) 0.002(8) C30 0.051(12) 0.069(13) 0.038(10) 0.001(9) -0.008(8) 0.023(9) C31 0.079(16) 0.034(11) 0.119(18) 0.020(11) -0.008(13) 0.004(10) C32 0.14(2) 0.042(12) 0.066(13) -0.005(10) 0.018(13) -0.004(12) C33 0.23(2) 0.22(2) 0.214(19) 0.009(10) 0.035(10) 0.001(10) B3 0.043(11) 0.023(9) 0.043(10) 0.003(7) 0.003(8) -0.020(8) B4 0.103(19) 0.032(11) 0.041(11) 0.017(9) -0.011(11) 0.014(11) B5 0.061(14) 0.026(10) 0.070(14) -0.001(9) 0.007(11) -0.013(9) B6 0.037(11) 0.016(9) 0.076(13) 0.000(8) 0.017(9) -0.018(8) B7 0.028(11) 0.057(13) 0.073(14) 0.004(11) 0.007(10) 0.017(9) B8 0.048(13) 0.048(13) 0.063(13) -0.004(10) -0.005(10) 0.006(9) B9 0.065(15) 0.038(12) 0.069(14) 0.018(10) 0.015(11) 0.012(10) B10 0.056(15) 0.059(14) 0.085(16) -0.001(12) 0.027(12) -0.007(11) B11 0.044(12) 0.022(10) 0.093(16) -0.005(10) 0.016(11) 0.011(8) B12 0.071(17) 0.040(12) 0.086(16) 0.014(11) 0.026(13) 0.011(11) B13 0.060(14) 0.051(12) 0.021(9) 0.004(8) -0.004(8) -0.013(10) B14 0.058(14) 0.036(11) 0.045(11) 0.013(9) 0.009(9) 0.004(9) B15 0.036(11) 0.038(11) 0.049(11) -0.005(8) 0.016(9) -0.007(8) B16 0.017(9) 0.045(10) 0.025(8) -0.004(7) 0.001(7) -0.005(7) B17 0.034(11) 0.056(12) 0.042(10) -0.014(9) 0.007(8) 0.011(9) B18 0.059(14) 0.062(14) 0.031(10) -0.010(9) 0.007(9) -0.023(11) B19 0.057(14) 0.071(15) 0.035(10) 0.005(10) 0.014(9) -0.011(11) B20 0.034(11) 0.046(11) 0.036(10) -0.002(8) 0.010(8) -0.006(8) B21 0.049(13) 0.050(12) 0.048(11) -0.029(9) 0.016(9) -0.014(10) B22 0.071(15) 0.062(14) 0.031(10) 0.001(9) 0.034(10) -0.004(11) Cl1 0.195(8) 0.223(8) 0.208(8) -0.018(7) 0.060(6) 0.013(7) Cl2 0.283(10) 0.271(9) 0.234(9) 0.015(8) 0.043(8) -0.011(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 C7 2.10(2) . ? Ir1 C6 2.105(19) . ? Ir1 C9 2.114(15) . ? Ir1 C5 2.152(15) . ? Ir1 C8 2.184(16) . ? Ir1 Se1 2.4316(16) . ? Ir1 Se2 2.4433(16) . ? Ir1 Rh2 2.6281(12) . ? Ir2 B16 2.151(15) . ? Ir2 C17 2.217(16) . ? Ir2 C16 2.222(13) . ? Ir2 C15 2.283(13) . ? Ir2 C18 2.289(14) . ? Ir2 C19 2.309(15) . ? Ir2 Se3 2.4435(16) . ? Ir2 Rh1 2.8258(13) . ? Ir2 Rh2 3.0085(13) . ? Rh1 C3 2.138(15) . ? Rh1 C30 2.178(15) . ? Rh1 C29 2.205(16) . ? Rh1 C25 2.243(15) . ? Rh1 C26 2.252(14) . ? Rh1 Se3 2.4578(18) . ? Rh1 Se4 2.4777(18) . ? Rh2 Se4 2.3975(18) . ? Rh2 Se3 2.4038(18) . ? Rh2 Se1 2.4841(18) . ? Rh2 Se2 2.4883(18) . ? Se1 C1 2.001(14) . ? Se2 C2 1.998(14) . ? Se4 C4 1.947(14) . ? C1 C2 1.614(19) . ? C1 B4 1.67(2) . ? C1 B3 1.69(2) . ? C1 B5 1.69(2) . ? C1 B6 1.74(2) . ? C2 B7 1.68(2) . ? C2 B11 1.69(2) . ? C2 B6 1.727(19) . ? C2 B3 1.74(2) . ? C3 C4 1.648(19) . ? C3 B15 1.72(2) . ? C3 B13 1.72(2) . ? C3 B14 1.72(2) . ? C3 B16 1.76(2) . ? C4 B21 1.69(2) . ? C4 B17 1.69(2) . ? C4 B13 1.73(2) . ? C4 B16 1.778(18) . ? C5 C6 1.36(2) . ? C5 C9 1.39(2) . ? C5 C10 1.52(3) . ? C6 C7 1.34(3) . ? C6 C11 1.50(4) . ? C7 C8 1.32(3) . ? C7 C12 1.58(4) . ? C8 C9 1.39(2) . ? C8 C13 1.47(4) . ? C9 C14 1.55(3) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C19 1.40(2) . ? C15 C16 1.41(2) . ? C15 C20 1.48(2) . ? C16 C17 1.42(2) . ? C16 C21 1.55(2) . ? C17 C18 1.36(2) . ? C17 C22 1.51(2) . ? C18 C19 1.44(2) . ? C18 C23 1.52(2) . ? C19 C24 1.55(2) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.39(2) . ? C25 C32 1.55(2) . ? C25 H25 0.9800 . ? C26 C27 1.49(2) . ? C26 H26 0.9800 . ? C27 C28 1.50(2) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.48(2) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.41(2) . ? C29 H29 0.9800 . ? C30 C31 1.51(2) . ? C30 H30 0.9800 . ? C31 C32 1.49(2) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 Cl2 1.68(4) . ? C33 Cl1 1.72(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? B3 B8 1.73(3) . ? B3 B4 1.74(2) . ? B3 B7 1.77(3) . ? B3 H3 1.1000 . ? B4 B8 1.75(3) . ? B4 B5 1.78(3) . ? B4 B9 1.78(3) . ? B4 H4 1.1000 . ? B5 B6 1.72(3) . ? B5 B9 1.79(3) . ? B5 B10 1.79(3) . ? B5 H5 1.1000 . ? B6 B10 1.74(3) . ? B6 B11 1.75(3) . ? B6 H6 1.1000 . ? B7 B12 1.77(3) . ? B7 B11 1.79(3) . ? B7 B8 1.80(3) . ? B7 H7 1.1000 . ? B8 B9 1.77(3) . ? B8 B12 1.79(3) . ? B8 H8 1.1000 . ? B9 B12 1.74(3) . ? B9 B10 1.76(3) . ? B9 H9 1.1000 . ? B10 B11 1.76(3) . ? B10 B12 1.77(3) . ? B10 H10 1.1000 . ? B11 B12 1.76(3) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? B13 B14 1.76(3) . ? B13 B18 1.77(3) . ? B13 B17 1.80(3) . ? B13 H13 1.1000 . ? B14 B18 1.77(3) . ? B14 B15 1.78(2) . ? B14 B19 1.80(3) . ? B14 H14 1.1000 . ? B15 B19 1.76(2) . ? B15 B16 1.78(2) . ? B15 B20 1.78(2) . ? B15 H15 1.1000 . ? B16 B20 1.83(2) . ? B16 B21 1.88(2) . ? B17 B22 1.77(3) . ? B17 B21 1.80(3) . ? B17 B18 1.80(3) . ? B17 H17 1.1000 . ? B18 B19 1.78(3) . ? B18 B22 1.82(3) . ? B18 H18 1.1000 . ? B19 B22 1.80(3) . ? B19 B20 1.80(2) . ? B19 H19 1.1000 . ? B20 B22 1.77(2) . ? B20 B21 1.80(2) . ? B20 H20 1.1000 . ? B21 B22 1.80(3) . ? B21 H21 1.1000 . ? B22 H22 1.1000 . ? 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 C7 Ir1 C6 37.3(8) . . ? C7 Ir1 C9 62.2(8) . . ? C6 Ir1 C9 62.0(7) . . ? C7 Ir1 C5 62.8(7) . . ? C6 Ir1 C5 37.1(7) . . ? C9 Ir1 C5 37.9(6) . . ? C7 Ir1 C8 35.7(7) . . ? C6 Ir1 C8 60.6(7) . . ? C9 Ir1 C8 37.6(7) . . ? C5 Ir1 C8 62.3(6) . . ? C7 Ir1 Se1 103.6(6) . . ? C6 Ir1 Se1 124.0(6) . . ? C9 Ir1 Se1 149.9(6) . . ? C5 Ir1 Se1 160.9(6) . . ? C8 Ir1 Se1 115.4(5) . . ? C7 Ir1 Se2 168.3(7) . . ? C6 Ir1 Se2 144.2(7) . . ? C9 Ir1 Se2 107.1(5) . . ? C5 Ir1 Se2 112.4(5) . . ? C8 Ir1 Se2 132.8(6) . . ? Se1 Ir1 Se2 83.41(5) . . ? C7 Ir1 Rh2 133.0(7) . . ? C6 Ir1 Rh2 112.9(5) . . ? C9 Ir1 Rh2 150.7(6) . . ? C5 Ir1 Rh2 119.4(4) . . ? C8 Ir1 Rh2 168.1(6) . . ? Se1 Ir1 Rh2 58.65(4) . . ? Se2 Ir1 Rh2 58.63(4) . . ? B16 Ir2 C17 106.5(6) . . ? B16 Ir2 C16 143.6(6) . . ? C17 Ir2 C16 37.4(6) . . ? B16 Ir2 C15 148.0(6) . . ? C17 Ir2 C15 61.1(5) . . ? C16 Ir2 C15 36.4(5) . . ? B16 Ir2 C18 92.1(5) . . ? C17 Ir2 C18 35.1(6) . . ? C16 Ir2 C18 60.3(6) . . ? C15 Ir2 C18 60.3(5) . . ? B16 Ir2 C19 112.6(6) . . ? C17 Ir2 C19 60.1(6) . . ? C16 Ir2 C19 60.0(5) . . ? C15 Ir2 C19 35.4(5) . . ? C18 Ir2 C19 36.6(5) . . ? B16 Ir2 Se3 113.8(4) . . ? C17 Ir2 Se3 137.3(5) . . ? C16 Ir2 Se3 100.7(5) . . ? C15 Ir2 Se3 89.4(4) . . ? C18 Ir2 Se3 148.7(4) . . ? C19 Ir2 Se3 113.3(4) . . ? B16 Ir2 Rh1 66.2(4) . . ? C17 Ir2 Rh1 165.0(5) . . ? C16 Ir2 Rh1 149.6(4) . . ? C15 Ir2 Rh1 117.7(4) . . ? C18 Ir2 Rh1 130.1(4) . . ? C19 Ir2 Rh1 109.5(4) . . ? Se3 Ir2 Rh1 55.03(4) . . ? B16 Ir2 Rh2 89.0(4) . . ? C17 Ir2 Rh2 118.5(4) . . ? C16 Ir2 Rh2 104.7(4) . . ? C15 Ir2 Rh2 123.0(4) . . ? C18 Ir2 Rh2 152.1(5) . . ? C19 Ir2 Rh2 158.2(4) . . ? Se3 Ir2 Rh2 51.04(4) . . ? Rh1 Ir2 Rh2 75.39(4) . . ? C3 Rh1 C30 89.2(6) . . ? C3 Rh1 C29 125.8(6) . . ? C30 Rh1 C29 37.6(6) . . ? C3 Rh1 C25 85.5(6) . . ? C30 Rh1 C25 80.5(6) . . ? C29 Rh1 C25 92.4(6) . . ? C3 Rh1 C26 120.6(6) . . ? C30 Rh1 C26 89.4(6) . . ? C29 Rh1 C26 78.4(6) . . ? C25 Rh1 C26 35.9(5) . . ? C3 Rh1 Se3 133.1(4) . . ? C30 Rh1 Se3 132.5(5) . . ? C29 Rh1 Se3 95.4(5) . . ? C25 Rh1 Se3 117.1(4) . . ? C26 Rh1 Se3 85.4(4) . . ? C3 Rh1 Se4 76.2(4) . . ? C30 Rh1 Se4 92.1(4) . . ? C29 Rh1 Se4 92.7(4) . . ? C25 Rh1 Se4 160.4(4) . . ? C26 Rh1 Se4 163.2(4) . . ? Se3 Rh1 Se4 81.18(6) . . ? C3 Rh1 Ir2 83.5(4) . . ? C30 Rh1 Ir2 172.7(5) . . ? C29 Rh1 Ir2 149.7(5) . . ? C25 Rh1 Ir2 97.9(4) . . ? C26 Rh1 Ir2 93.5(4) . . ? Se3 Rh1 Ir2 54.56(4) . . ? Se4 Rh1 Ir2 87.08(5) . . ? Se4 Rh2 Se3 83.96(6) . . ? Se4 Rh2 Se1 154.56(7) . . ? Se3 Rh2 Se1 98.64(6) . . ? Se4 Rh2 Se2 93.62(6) . . ? Se3 Rh2 Se2 174.46(7) . . ? Se1 Rh2 Se2 81.42(6) . . ? Se4 Rh2 Ir1 99.70(5) . . ? Se3 Rh2 Ir1 118.46(6) . . ? Se1 Rh2 Ir1 56.72(4) . . ? Se2 Rh2 Ir1 56.97(4) . . ? Se4 Rh2 Ir2 84.47(5) . . ? Se3 Rh2 Ir2 52.23(4) . . ? Se1 Rh2 Ir2 117.19(5) . . ? Se2 Rh2 Ir2 132.61(5) . . ? Ir1 Rh2 Ir2 169.63(5) . . ? C1 Se1 Ir1 102.6(4) . . ? C1 Se1 Rh2 101.8(4) . . ? Ir1 Se1 Rh2 64.63(4) . . ? C2 Se2 Ir1 102.6(4) . . ? C2 Se2 Rh2 102.8(4) . . ? Ir1 Se2 Rh2 64.39(4) . . ? Rh2 Se3 Ir2 76.72(5) . . ? Rh2 Se3 Rh1 94.50(6) . . ? Ir2 Se3 Rh1 70.42(5) . . ? C4 Se4 Rh2 107.8(4) . . ? C4 Se4 Rh1 78.5(4) . . ? Rh2 Se4 Rh1 94.15(6) . . ? C2 C1 B4 112.8(13) . . ? C2 C1 B3 63.7(9) . . ? B4 C1 B3 62.3(11) . . ? C2 C1 B5 110.8(12) . . ? B4 C1 B5 63.8(10) . . ? B3 C1 B5 115.5(12) . . ? C2 C1 B6 61.9(9) . . ? B4 C1 B6 113.8(12) . . ? B3 C1 B6 116.2(11) . . ? B5 C1 B6 60.3(10) . . ? C2 C1 Se1 114.7(9) . . ? B4 C1 Se1 122.9(11) . . ? B3 C1 Se1 115.6(9) . . ? B5 C1 Se1 122.2(11) . . ? B6 C1 Se1 115.5(10) . . ? C1 C2 B7 110.8(12) . . ? C1 C2 B11 111.7(12) . . ? B7 C2 B11 64.2(11) . . ? C1 C2 B6 62.6(9) . . ? B7 C2 B6 114.8(12) . . ? B11 C2 B6 61.5(10) . . ? C1 C2 B3 60.2(9) . . ? B7 C2 B3 62.2(10) . . ? B11 C2 B3 114.8(13) . . ? B6 C2 B3 113.9(11) . . ? C1 C2 Se2 113.4(9) . . ? B7 C2 Se2 123.2(10) . . ? B11 C2 Se2 124.7(11) . . ? B6 C2 Se2 116.4(10) . . ? B3 C2 Se2 114.6(9) . . ? C4 C3 B15 107.8(11) . . ? C4 C3 B13 61.6(9) . . ? B15 C3 B13 112.2(12) . . ? C4 C3 B14 109.3(11) . . ? B15 C3 B14 62.0(10) . . ? B13 C3 B14 61.6(9) . . ? C4 C3 B16 62.8(8) . . ? B15 C3 B16 61.5(9) . . ? B13 C3 B16 117.1(11) . . ? B14 C3 B16 115.1(12) . . ? C4 C3 Rh1 95.8(9) . . ? B15 C3 Rh1 125.7(9) . . ? B13 C3 Rh1 122.0(10) . . ? B14 C3 Rh1 150.2(10) . . ? B16 C3 Rh1 90.3(8) . . ? C3 C4 B21 115.1(11) . . ? C3 C4 B17 113.1(11) . . ? B21 C4 B17 64.4(10) . . ? C3 C4 B13 61.2(9) . . ? B21 C4 B13 117.9(12) . . ? B17 C4 B13 63.5(10) . . ? C3 C4 B16 61.6(8) . . ? B21 C4 B16 65.8(9) . . ? B17 C4 B16 118.7(11) . . ? B13 C4 B16 115.7(10) . . ? C3 C4 Se4 105.2(9) . . ? B21 C4 Se4 128.0(10) . . ? B17 C4 Se4 126.9(9) . . ? B13 C4 Se4 109.5(9) . . ? B16 C4 Se4 111.4(8) . . ? C6 C5 C9 104.7(16) . . ? C6 C5 C10 134(2) . . ? C9 C5 C10 121(2) . . ? C6 C5 Ir1 69.6(10) . . ? C9 C5 Ir1 69.6(9) . . ? C10 C5 Ir1 123.5(15) . . ? C7 C6 C5 110.4(18) . . ? C7 C6 C11 128(3) . . ? C5 C6 C11 121(3) . . ? C7 C6 Ir1 71.2(13) . . ? C5 C6 Ir1 73.3(11) . . ? C11 C6 Ir1 124(2) . . ? C8 C7 C6 108.9(19) . . ? C8 C7 C12 134(3) . . ? C6 C7 C12 116(3) . . ? C8 C7 Ir1 75.6(13) . . ? C6 C7 Ir1 71.5(12) . . ? C12 C7 Ir1 123(2) . . ? C7 C8 C9 107.4(17) . . ? C7 C8 C13 120(3) . . ? C9 C8 C13 132(3) . . ? C7 C8 Ir1 68.7(12) . . ? C9 C8 Ir1 68.5(9) . . ? C13 C8 Ir1 125.0(19) . . ? C5 C9 C8 108.1(16) . . ? C5 C9 C14 121(2) . . ? C8 C9 C14 130(2) . . ? C5 C9 Ir1 72.5(9) . . ? C8 C9 Ir1 73.9(9) . . ? C14 C9 Ir1 126.8(15) . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C19 C15 C16 107.6(14) . . ? C19 C15 C20 127.0(15) . . ? C16 C15 C20 124.5(15) . . ? C19 C15 Ir2 73.3(8) . . ? C16 C15 Ir2 69.4(8) . . ? C20 C15 Ir2 130.9(11) . . ? C15 C16 C17 107.8(14) . . ? C15 C16 C21 123.7(16) . . ? C17 C16 C21 128.2(15) . . ? C15 C16 Ir2 74.2(8) . . ? C17 C16 Ir2 71.2(9) . . ? C21 C16 Ir2 126.0(10) . . ? C18 C17 C16 108.9(14) . . ? C18 C17 C22 124.0(17) . . ? C16 C17 C22 126.2(17) . . ? C18 C17 Ir2 75.3(10) . . ? C16 C17 Ir2 71.5(8) . . ? C22 C17 Ir2 127.6(12) . . ? C17 C18 C19 107.8(14) . . ? C17 C18 C23 126.2(17) . . ? C19 C18 C23 124.4(17) . . ? C17 C18 Ir2 69.6(9) . . ? C19 C18 Ir2 72.5(9) . . ? C23 C18 Ir2 134.7(11) . . ? C15 C19 C18 107.9(14) . . ? C15 C19 C24 126.4(15) . . ? C18 C19 C24 123.9(16) . . ? C15 C19 Ir2 71.3(8) . . ? C18 C19 Ir2 71.0(8) . . ? C24 C19 Ir2 135.1(11) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C32 122.8(17) . . ? C26 C25 Rh1 72.4(9) . . ? C32 C25 Rh1 109.5(11) . . ? C26 C25 H25 114.8 . . ? C32 C25 H25 114.8 . . ? Rh1 C25 H25 114.8 . . ? C25 C26 C27 124.6(16) . . ? C25 C26 Rh1 71.7(9) . . ? C27 C26 Rh1 111.7(10) . . ? C25 C26 H26 113.8 . . ? C27 C26 H26 113.8 . . ? Rh1 C26 H26 113.8 . . ? C26 C27 C28 117.5(15) . . ? C26 C27 H27A 107.9 . . ? C28 C27 H27A 107.9 . . ? C26 C27 H27B 107.9 . . ? C28 C27 H27B 107.9 . . ? H27A C27 H27B 107.2 . . ? C29 C28 C27 113.8(16) . . ? C29 C28 H28A 108.8 . . ? C27 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C28 127.7(17) . . ? C30 C29 Rh1 70.1(9) . . ? C28 C29 Rh1 113.6(12) . . ? C30 C29 H29 112.6 . . ? C28 C29 H29 112.6 . . ? Rh1 C29 H29 112.6 . . ? C29 C30 C31 122.6(16) . . ? C29 C30 Rh1 72.2(9) . . ? C31 C30 Rh1 113.5(12) . . ? C29 C30 H30 113.9 . . ? C31 C30 H30 113.9 . . ? Rh1 C30 H30 113.9 . . ? C32 C31 C30 116.6(15) . . ? C32 C31 H31A 108.1 . . ? C30 C31 H31A 108.1 . . ? C32 C31 H31B 108.1 . . ? C30 C31 H31B 108.1 . . ? H31A C31 H31B 107.3 . . ? C31 C32 C25 115.9(15) . . ? C31 C32 H32A 108.3 . . ? C25 C32 H32A 108.3 . . ? C31 C32 H32B 108.3 . . ? C25 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? Cl2 C33 Cl1 118(2) . . ? Cl2 C33 H33A 107.9 . . ? Cl1 C33 H33A 107.9 . . ? Cl2 C33 H33B 107.9 . . ? Cl1 C33 H33B 107.9 . . ? H33A C33 H33B 107.2 . . ? C1 B3 B8 105.2(12) . . ? C1 B3 B4 58.5(10) . . ? B8 B3 B4 60.6(11) . . ? C1 B3 C2 56.1(8) . . ? B8 B3 C2 105.0(12) . . ? B4 B3 C2 103.8(11) . . ? C1 B3 B7 103.6(11) . . ? B8 B3 B7 62.1(11) . . ? B4 B3 B7 109.4(13) . . ? C2 B3 B7 57.3(9) . . ? C1 B3 H3 125.3 . . ? B8 B3 H3 121.7 . . ? B4 B3 H3 121.7 . . ? C2 B3 H3 125.7 . . ? B7 B3 H3 121.7 . . ? C1 B4 B3 59.2(9) . . ? C1 B4 B8 104.7(13) . . ? B3 B4 B8 59.3(11) . . ? C1 B4 B5 58.5(10) . . ? B3 B4 B5 108.5(13) . . ? B8 B4 B5 108.9(14) . . ? C1 B4 B9 103.9(14) . . ? B3 B4 B9 107.0(15) . . ? B8 B4 B9 60.0(11) . . ? B5 B4 B9 60.2(11) . . ? C1 B4 H4 125.0 . . ? B3 B4 H4 121.7 . . ? B8 B4 H4 122.2 . . ? B5 B4 H4 120.8 . . ? B9 B4 H4 123.0 . . ? C1 B5 B6 61.2(10) . . ? C1 B5 B4 57.6(9) . . ? B6 B5 B4 109.5(13) . . ? C1 B5 B9 103.0(13) . . ? B6 B5 B9 106.7(14) . . ? B4 B5 B9 59.9(11) . . ? C1 B5 B10 105.4(14) . . ? B6 B5 B10 59.4(11) . . ? B4 B5 B10 108.2(15) . . ? B9 B5 B10 59.1(12) . . ? C1 B5 H5 124.5 . . ? B6 B5 H5 120.6 . . ? B4 B5 H5 121.1 . . ? B9 B5 H5 123.9 . . ? B10 B5 H5 122.5 . . ? B5 B6 C2 104.2(12) . . ? B5 B6 C1 58.5(10) . . ? C2 B6 C1 55.5(8) . . ? B5 B6 B10 62.4(12) . . ? C2 B6 B10 105.0(13) . . ? C1 B6 B10 105.6(14) . . ? B5 B6 B11 109.9(15) . . ? C2 B6 B11 58.1(9) . . ? C1 B6 B11 103.3(12) . . ? B10 B6 B11 60.7(11) . . ? B5 B6 H6 120.9 . . ? C2 B6 H6 125.6 . . ? C1 B6 H6 125.6 . . ? B10 B6 H6 121.5 . . ? B11 B6 H6 122.0 . . ? C2 B7 B12 103.4(14) . . ? C2 B7 B3 60.5(9) . . ? B12 B7 B3 106.5(14) . . ? C2 B7 B11 58.0(9) . . ? B12 B7 B11 59.3(11) . . ? B3 B7 B11 108.4(13) . . ? C2 B7 B8 104.1(13) . . ? B12 B7 B8 60.3(11) . . ? B3 B7 B8 57.8(10) . . ? B11 B7 B8 107.6(14) . . ? C2 B7 H7 124.7 . . ? B12 B7 H7 123.3 . . ? B3 B7 H7 121.7 . . ? B11 B7 H7 121.6 . . ? B8 B7 H7 123.1 . . ? B3 B8 B4 60.0(10) . . ? B3 B8 B9 108.3(14) . . ? B4 B8 B9 60.9(11) . . ? B3 B8 B12 107.2(13) . . ? B4 B8 B12 107.1(15) . . ? B9 B8 B12 58.5(11) . . ? B3 B8 B7 60.1(10) . . ? B4 B8 B7 107.4(13) . . ? B9 B8 B7 106.0(14) . . ? B12 B8 B7 58.8(11) . . ? B3 B8 H8 121.4 . . ? B4 B8 H8 121.5 . . ? B9 B8 H8 122.2 . . ? B12 B8 H8 123.0 . . ? B7 B8 H8 122.8 . . ? B12 B9 B10 60.7(12) . . ? B12 B9 B8 61.6(11) . . ? B10 B9 B8 110.8(15) . . ? B12 B9 B4 108.2(14) . . ? B10 B9 B4 109.4(15) . . ? B8 B9 B4 59.1(11) . . ? B12 B9 B5 108.1(15) . . ? B10 B9 B5 60.7(11) . . ? B8 B9 B5 107.8(13) . . ? B4 B9 B5 59.8(11) . . ? B12 B9 H9 121.2 . . ? B10 B9 H9 119.9 . . ? B8 B9 H9 120.8 . . ? B4 B9 H9 122.0 . . ? B5 B9 H9 122.1 . . ? B6 B10 B11 59.8(11) . . ? B6 B10 B9 106.8(15) . . ? B11 B10 B9 106.8(15) . . ? B6 B10 B12 107.1(15) . . ? B11 B10 B12 59.9(11) . . ? B9 B10 B12 58.9(12) . . ? B6 B10 B5 58.3(11) . . ? B11 B10 B5 106.0(15) . . ? B9 B10 B5 60.3(11) . . ? B12 B10 B5 106.5(15) . . ? B6 B10 H10 122.6 . . ? B11 B10 H10 122.4 . . ? B9 B10 H10 122.2 . . ? B12 B10 H10 122.4 . . ? B5 B10 H10 123.0 . . ? C2 B11 B6 60.4(9) . . ? C2 B11 B12 103.5(14) . . ? B6 B11 B12 107.1(15) . . ? C2 B11 B10 105.9(14) . . ? B6 B11 B10 59.5(11) . . ? B12 B11 B10 60.3(12) . . ? C2 B11 B7 57.8(9) . . ? B6 B11 B7 108.5(13) . . ? B12 B11 B7 59.6(11) . . ? B10 B11 B7 108.7(15) . . ? C2 B11 H11 124.5 . . ? B6 B11 H11 121.2 . . ? B12 B11 H11 123.3 . . ? B10 B11 H11 121.7 . . ? B7 B11 H11 121.5 . . ? B9 B12 B11 108.0(16) . . ? B9 B12 B7 108.8(15) . . ? B11 B12 B7 61.1(11) . . ? B9 B12 B10 60.4(12) . . ? B11 B12 B10 59.9(12) . . ? B7 B12 B10 109.6(15) . . ? B9 B12 B8 59.9(12) . . ? B11 B12 B8 109.4(14) . . ? B7 B12 B8 60.8(11) . . ? B10 B12 B8 109.2(15) . . ? B9 B12 H12 121.9 . . ? B11 B12 H12 121.3 . . ? B7 B12 H12 120.6 . . ? B10 B12 H12 121.0 . . ? B8 B12 H12 120.9 . . ? C3 B13 C4 57.1(8) . . ? C3 B13 B14 59.3(9) . . ? C4 B13 B14 104.1(11) . . ? C3 B13 B18 105.5(12) . . ? C4 B13 B18 103.5(13) . . ? B14 B13 B18 60.0(10) . . ? C3 B13 B17 104.6(12) . . ? C4 B13 B17 57.2(9) . . ? B14 B13 B17 108.1(13) . . ? B18 B13 B17 60.5(11) . . ? C3 B13 H13 123.9 . . ? C4 B13 H13 125.8 . . ? B14 B13 H13 122.0 . . ? B18 B13 H13 122.9 . . ? B17 B13 H13 122.4 . . ? C3 B14 B13 59.1(9) . . ? C3 B14 B18 105.6(12) . . ? B13 B14 B18 60.3(10) . . ? C3 B14 B15 58.8(9) . . ? B13 B14 B15 107.6(12) . . ? B18 B14 B15 107.0(13) . . ? C3 B14 B19 104.8(12) . . ? B13 B14 B19 107.9(13) . . ? B18 B14 B19 59.9(10) . . ? B15 B14 B19 58.9(10) . . ? C3 B14 H14 124.1 . . ? B13 B14 H14 121.3 . . ? B18 B14 H14 122.3 . . ? B15 B14 H14 122.3 . . ? B19 B14 H14 122.8 . . ? C3 B15 B19 106.8(12) . . ? C3 B15 B14 59.1(10) . . ? B19 B15 B14 61.2(10) . . ? C3 B15 B16 60.3(9) . . ? B19 B15 B16 112.5(12) . . ? B14 B15 B16 111.7(12) . . ? C3 B15 B20 106.2(12) . . ? B19 B15 B20 61.0(10) . . ? B14 B15 B20 109.9(12) . . ? B16 B15 B20 61.7(9) . . ? C3 B15 H15 124.2 . . ? B19 B15 H15 120.4 . . ? B14 B15 H15 120.1 . . ? B16 B15 H15 118.3 . . ? B20 B15 H15 121.5 . . ? C3 B16 C4 55.6(8) . . ? C3 B16 B15 58.2(9) . . ? C4 B16 B15 99.9(11) . . ? C3 B16 B20 102.8(11) . . ? C4 B16 B20 98.3(10) . . ? B15 B16 B20 59.3(9) . . ? C3 B16 B21 101.2(10) . . ? C4 B16 B21 54.8(8) . . ? B15 B16 B21 104.5(11) . . ? B20 B16 B21 58.0(9) . . ? C3 B16 Ir2 117.3(9) . . ? C4 B16 Ir2 122.9(9) . . ? B15 B16 Ir2 124.2(10) . . ? B20 B16 Ir2 133.6(10) . . ? B21 B16 Ir2 128.5(10) . . ? C4 B17 B22 103.7(11) . . ? C4 B17 B13 59.3(9) . . ? B22 B17 B13 108.4(13) . . ? C4 B17 B21 57.8(9) . . ? B22 B17 B21 60.7(10) . . ? B13 B17 B21 108.9(12) . . ? C4 B17 B18 104.1(12) . . ? B22 B17 B18 61.2(11) . . ? B13 B17 B18 59.1(10) . . ? B21 B17 B18 109.8(13) . . ? C4 B17 H17 125.8 . . ? B22 B17 H17 122.1 . . ? B13 B17 H17 121.2 . . ? B21 B17 H17 120.6 . . ? B18 B17 H17 121.9 . . ? B14 B18 B13 59.7(10) . . ? B14 B18 B19 60.9(10) . . ? B13 B18 B19 108.2(13) . . ? B14 B18 B17 107.8(13) . . ? B13 B18 B17 60.4(10) . . ? B19 B18 B17 107.0(13) . . ? B14 B18 B22 108.2(12) . . ? B13 B18 B22 107.2(13) . . ? B19 B18 B22 59.9(11) . . ? B17 B18 B22 58.5(10) . . ? B14 B18 H18 121.3 . . ? B13 B18 H18 121.8 . . ? B19 B18 H18 121.6 . . ? B17 B18 H18 122.5 . . ? B22 B18 H18 122.4 . . ? B15 B19 B18 107.2(14) . . ? B15 B19 B22 106.9(13) . . ? B18 B19 B22 61.0(11) . . ? B15 B19 B20 60.2(10) . . ? B18 B19 B20 108.3(14) . . ? B22 B19 B20 59.1(10) . . ? B15 B19 B14 59.9(10) . . ? B18 B19 B14 59.2(11) . . ? B22 B19 B14 107.8(14) . . ? B20 B19 B14 108.2(13) . . ? B15 B19 H19 122.3 . . ? B18 B19 H19 121.6 . . ? B22 B19 H19 122.0 . . ? B20 B19 H19 121.6 . . ? B14 B19 H19 121.9 . . ? B22 B20 B15 106.9(13) . . ? B22 B20 B19 60.4(10) . . ? B15 B20 B19 58.8(10) . . ? B22 B20 B21 60.6(10) . . ? B15 B20 B21 107.9(13) . . ? B19 B20 B21 109.0(13) . . ? B22 B20 B16 110.9(12) . . ? B15 B20 B16 59.0(9) . . ? B19 B20 B16 108.5(13) . . ? B21 B20 B16 62.6(9) . . ? B22 B20 H20 121.0 . . ? B15 B20 H20 123.5 . . ? B19 B20 H20 121.8 . . ? B21 B20 H20 120.4 . . ? B16 B20 H20 120.0 . . ? C4 B21 B20 102.8(12) . . ? C4 B21 B17 57.8(10) . . ? B20 B21 B17 105.8(13) . . ? C4 B21 B22 102.2(14) . . ? B20 B21 B22 59.0(10) . . ? B17 B21 B22 58.7(11) . . ? C4 B21 B16 59.4(8) . . ? B20 B21 B16 59.4(8) . . ? B17 B21 B16 108.1(13) . . ? B22 B21 B16 107.0(12) . . ? C4 B21 H21 125.8 . . ? B20 B21 H21 123.8 . . ? B17 B21 H21 122.3 . . ? B22 B21 H21 123.8 . . ? B16 B21 H21 121.0 . . ? B17 B22 B20 108.5(12) . . ? B17 B22 B19 107.8(14) . . ? B20 B22 B19 60.5(10) . . ? B17 B22 B21 60.6(11) . . ? B20 B22 B21 60.4(9) . . ? B19 B22 B21 109.0(12) . . ? B17 B22 B18 60.3(11) . . ? B20 B22 B18 107.9(13) . . ? B19 B22 B18 59.1(10) . . ? B21 B22 B18 109.0(14) . . ? B17 B22 H22 121.5 . . ? B20 B22 H22 121.4 . . ? B19 B22 H22 121.8 . . ? B21 B22 H22 120.7 . . ? B18 B22 H22 121.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.399 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.241