# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_d:complex1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H44 Cl2 Rh2 S2' _chemical_formula_sum 'C34 H44 Cl2 Rh2 S2' _chemical_formula_weight 793.53 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P n' _symmetry_space_group_name_Hall 'P -2yac' _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 8.7743(7) _cell_length_b 14.8192(13) _cell_length_c 13.3856(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.358(10) _cell_angle_gamma 90.00 _cell_volume 1740.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 25.85 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 1.243 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_T_max 0.799 _exptl_absorpt_process_details 'Walker, N. & Stuart, D. (1983)' _exptl_special_details ; A crystal was mounted at 173K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using MoK\a graphite monochromated radiation. Image plate distance 70mm, \f oscillation scans 0 - 200\%, step \D\f = 1.2\%, 5 minutes per frame. ; _diffrn_ambient_temperature 173(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9057 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 26.09 _reflns_number_total 6136 _reflns_number_gt 4955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie, 2000)' _computing_cell_refinement 'CELL (Stoe & Cie, 2000)' _computing_data_reduction 'INTEGRATE (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-32 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0510P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(4) _refine_ls_number_reflns 6136 _refine_ls_number_parameters 371 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0752 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _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 C1 C 1.0600(11) 0.3334(14) 0.1026(9) 0.123(6) Uani 1 1 d . . . C2 C 0.998(2) 0.2695(7) 0.0314(11) 0.139(7) Uani 1 1 d . . . C3 C 0.8564(16) 0.3072(10) 0.0051(5) 0.099(4) Uani 1 1 d . . . C4 C 0.8402(13) 0.3818(8) 0.0532(9) 0.091(3) Uani 1 1 d . . . C5 C 0.9531(19) 0.4003(7) 0.1090(7) 0.102(4) Uani 1 1 d . . . C6 C 1.2150(18) 0.324(3) 0.1454(19) 0.49(4) Uani 1 1 d . . . H6A H 1.2655 0.3812 0.1446 0.734 Uiso 1 1 calc R . . H6B H 1.2710 0.2813 0.1064 0.734 Uiso 1 1 calc R . . H6C H 1.2097 0.3025 0.2129 0.734 Uiso 1 1 calc R . . C7 C 1.048(4) 0.1843(11) -0.019(2) 0.46(3) Uani 1 1 d . . . H7A H 0.9657 0.1600 -0.0584 0.684 Uiso 1 1 calc R . . H7B H 1.0794 0.1410 0.0312 0.684 Uiso 1 1 calc R . . H7C H 1.1327 0.1973 -0.0608 0.684 Uiso 1 1 calc R . . C8 C 0.734(3) 0.282(2) -0.0668(10) 0.31(2) Uani 1 1 d . . . H8A H 0.6415 0.2712 -0.0317 0.458 Uiso 1 1 calc R . . H8B H 0.7624 0.2281 -0.1016 0.458 Uiso 1 1 calc R . . H8C H 0.7178 0.3300 -0.1140 0.458 Uiso 1 1 calc R . . C9 C 0.715(3) 0.4520(17) 0.054(2) 0.296(19) Uani 1 1 d . . . H9A H 0.6370 0.4335 0.0983 0.444 Uiso 1 1 calc R . . H9B H 0.6719 0.4582 -0.0127 0.444 Uiso 1 1 calc R . . H9C H 0.7565 0.5089 0.0752 0.444 Uiso 1 1 calc R . . C10 C 0.985(4) 0.4806(14) 0.1739(15) 0.36(3) Uani 1 1 d . . . H10A H 0.9328 0.5323 0.1467 0.537 Uiso 1 1 calc R . . H10B H 1.0929 0.4921 0.1764 0.537 Uiso 1 1 calc R . . H10C H 0.9504 0.4689 0.2401 0.537 Uiso 1 1 calc R . . C11 C 1.0439(11) 0.0450(6) 0.4895(7) 0.088(3) Uani 1 1 d . . . C12 C 1.1516(10) 0.0683(6) 0.4204(5) 0.068(2) Uani 1 1 d . . . C13 C 1.1854(8) 0.1606(5) 0.4313(5) 0.0602(18) Uani 1 1 d . . . C14 C 1.1001(10) 0.1919(6) 0.5121(5) 0.069(2) Uani 1 1 d . . . C15 C 1.0152(10) 0.1210(9) 0.5462(5) 0.083(3) Uani 1 1 d . . . C16 C 0.9729(17) -0.0457(9) 0.5066(13) 0.195(9) Uani 1 1 d . . . H16A H 0.9986 -0.0661 0.5729 0.292 Uiso 1 1 calc R . . H16B H 1.0107 -0.0881 0.4588 0.292 Uiso 1 1 calc R . . H16C H 0.8642 -0.0410 0.4988 0.292 Uiso 1 1 calc R . . C17 C 1.2227(17) 0.0048(12) 0.3444(10) 0.181(9) Uani 1 1 d . . . H17A H 1.3264 -0.0078 0.3644 0.272 Uiso 1 1 calc R . . H17B H 1.2205 0.0328 0.2798 0.272 Uiso 1 1 calc R . . H17C H 1.1659 -0.0506 0.3415 0.272 Uiso 1 1 calc R . . C18 C 1.3040(12) 0.2110(11) 0.3762(9) 0.137(5) Uani 1 1 d . . . H18A H 1.2763 0.2736 0.3722 0.205 Uiso 1 1 calc R . . H18B H 1.3117 0.1867 0.3101 0.205 Uiso 1 1 calc R . . H18C H 1.4005 0.2052 0.4110 0.205 Uiso 1 1 calc R . . C19 C 1.1108(18) 0.2856(9) 0.5548(10) 0.168(8) Uani 1 1 d . . . H19A H 1.0137 0.3029 0.5804 0.253 Uiso 1 1 calc R . . H19B H 1.1393 0.3271 0.5034 0.253 Uiso 1 1 calc R . . H19C H 1.1862 0.2867 0.6080 0.253 Uiso 1 1 calc R . . C20 C 0.9123(14) 0.1214(16) 0.6328(8) 0.210(11) Uani 1 1 d . . . H20A H 0.8587 0.0650 0.6356 0.314 Uiso 1 1 calc R . . H20B H 0.8402 0.1698 0.6254 0.314 Uiso 1 1 calc R . . H20C H 0.9714 0.1297 0.6934 0.314 Uiso 1 1 calc R . . C21 C 0.7117(8) 0.3287(5) 0.3907(5) 0.0563(17) Uani 1 1 d . . . H21A H 0.6315 0.2900 0.3639 0.068 Uiso 1 1 calc R . . H21B H 0.7182 0.3195 0.4625 0.068 Uiso 1 1 calc R . . C22 C 0.6724(8) 0.4249(5) 0.3693(5) 0.0576(17) Uani 1 1 d . . . C23 C 0.7608(11) 0.4942(5) 0.4088(6) 0.077(2) Uani 1 1 d . . . H23 H 0.8444 0.4807 0.4501 0.093 Uiso 1 1 calc R . . C24 C 0.7255(14) 0.5849(6) 0.3872(7) 0.089(3) Uani 1 1 d . . . H24 H 0.7832 0.6312 0.4157 0.107 Uiso 1 1 calc R . . C25 C 0.6065(15) 0.6039(6) 0.3243(8) 0.098(3) Uani 1 1 d . . . H25 H 0.5849 0.6637 0.3081 0.118 Uiso 1 1 calc R . . C26 C 0.5184(13) 0.5371(7) 0.2847(8) 0.099(3) Uani 1 1 d . . . H26 H 0.4352 0.5506 0.2430 0.119 Uiso 1 1 calc R . . C27 C 0.5549(10) 0.4475(6) 0.3078(7) 0.081(2) Uani 1 1 d . . . H27 H 0.4956 0.4017 0.2795 0.097 Uiso 1 1 calc R . . C28 C 0.8007(8) 0.0477(5) 0.1743(5) 0.0529(16) Uani 1 1 d . . . H28A H 0.7090 0.0577 0.2119 0.063 Uiso 1 1 calc R . . H28B H 0.7759 0.0578 0.1042 0.063 Uiso 1 1 calc R . . C29 C 0.8531(8) -0.0487(4) 0.1888(4) 0.0506(15) Uani 1 1 d . . . C30 C 0.8095(10) -0.0984(5) 0.2700(6) 0.076(2) Uani 1 1 d . . . H30 H 0.7449 -0.0728 0.3163 0.091 Uiso 1 1 calc R . . C31 C 0.8612(13) -0.1870(6) 0.2840(7) 0.096(3) Uani 1 1 d . . . H31 H 0.8323 -0.2197 0.3397 0.115 Uiso 1 1 calc R . . C32 C 0.9543(12) -0.2250(6) 0.2155(7) 0.083(2) Uani 1 1 d . . . H32 H 0.9878 -0.2841 0.2240 0.100 Uiso 1 1 calc R . . C33 C 0.9981(10) -0.1767(6) 0.1350(6) 0.072(2) Uani 1 1 d . . . H33 H 1.0594 -0.2034 0.0875 0.087 Uiso 1 1 calc R . . C34 C 0.9523(8) -0.0888(5) 0.1234(5) 0.0616(18) Uani 1 1 d . . . H34 H 0.9888 -0.0553 0.0703 0.074 Uiso 1 1 calc R . . Cl1 Cl 0.59908(19) 0.23779(12) 0.16738(13) 0.0594(4) Uani 1 1 d . . . Cl2 Cl 0.69067(18) 0.10306(12) 0.40853(11) 0.0555(4) Uani 1 1 d . . . S1 S 0.89277(19) 0.29707(12) 0.33590(12) 0.0449(4) Uani 1 1 d . . . S2 S 0.94619(18) 0.12733(11) 0.21521(11) 0.0429(4) Uani 1 1 d . . . Rh1 Rh 0.86378(5) 0.27193(3) 0.16144(3) 0.04228(13) Uani 1 1 d . . . Rh2 Rh 0.94980(4) 0.14843(3) 0.39066(3) 0.04239(13) 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 C1 0.046(6) 0.233(17) 0.092(7) 0.109(10) -0.004(5) -0.027(7) C2 0.236(16) 0.057(6) 0.130(9) 0.047(6) 0.150(11) 0.060(8) C3 0.148(11) 0.109(9) 0.040(4) 0.008(5) 0.004(5) -0.076(8) C4 0.092(8) 0.087(7) 0.093(7) 0.041(6) 0.018(6) 0.007(6) C5 0.159(13) 0.084(7) 0.065(5) -0.001(5) 0.026(7) -0.060(8) C6 0.069(10) 1.06(9) 0.33(3) 0.54(5) -0.057(13) -0.13(2) C7 0.86(7) 0.102(11) 0.43(4) 0.120(17) 0.56(5) 0.19(2) C8 0.32(3) 0.51(4) 0.086(8) 0.111(16) -0.083(13) -0.28(3) C9 0.25(2) 0.27(3) 0.37(3) 0.24(3) 0.18(2) 0.19(2) C10 0.69(6) 0.189(19) 0.202(17) -0.115(16) 0.24(3) -0.31(3) C11 0.096(7) 0.071(6) 0.093(6) 0.052(5) -0.051(5) -0.031(5) C12 0.071(5) 0.064(5) 0.067(4) -0.008(4) -0.035(4) 0.025(4) C13 0.055(4) 0.070(5) 0.056(4) 0.023(3) -0.005(3) -0.001(3) C14 0.069(5) 0.073(5) 0.064(4) -0.012(4) -0.019(4) 0.018(4) C15 0.051(5) 0.153(10) 0.044(4) 0.020(5) -0.013(3) -0.016(5) C16 0.156(13) 0.113(10) 0.308(19) 0.142(12) -0.145(13) -0.086(9) C17 0.172(14) 0.214(17) 0.155(11) -0.089(11) -0.069(10) 0.149(14) C18 0.057(6) 0.224(15) 0.129(8) 0.096(9) -0.004(5) -0.032(7) C19 0.192(15) 0.118(11) 0.188(13) -0.095(10) -0.144(12) 0.064(10) C20 0.073(8) 0.48(3) 0.072(6) 0.097(12) 0.002(5) 0.015(12) C21 0.056(4) 0.049(4) 0.064(4) -0.003(3) 0.020(3) 0.000(3) C22 0.060(5) 0.048(4) 0.066(4) -0.001(3) 0.023(3) 0.005(3) C23 0.101(7) 0.048(5) 0.083(5) -0.010(4) 0.014(5) 0.005(4) C24 0.132(9) 0.052(5) 0.084(5) -0.010(4) 0.008(6) 0.012(5) C25 0.146(10) 0.049(5) 0.101(7) -0.003(5) 0.045(7) 0.025(6) C26 0.105(8) 0.072(7) 0.121(7) 0.000(6) 0.000(6) 0.041(6) C27 0.075(6) 0.055(5) 0.112(6) -0.008(4) -0.002(5) 0.008(4) C28 0.055(4) 0.048(4) 0.055(3) -0.002(3) -0.003(3) -0.008(3) C29 0.058(4) 0.045(4) 0.048(3) -0.010(3) -0.006(3) -0.008(3) C30 0.096(6) 0.057(5) 0.076(5) 0.008(4) 0.032(4) -0.002(4) C31 0.149(9) 0.054(5) 0.087(5) 0.019(4) 0.034(6) -0.008(5) C32 0.093(7) 0.049(5) 0.107(6) -0.014(5) -0.001(5) 0.004(4) C33 0.078(6) 0.061(5) 0.078(5) -0.013(4) -0.003(4) 0.011(4) C34 0.064(5) 0.059(5) 0.062(4) -0.007(3) 0.012(3) -0.005(3) Cl1 0.0457(10) 0.0557(10) 0.0766(10) -0.0009(8) -0.0004(7) -0.0016(7) Cl2 0.0445(9) 0.0655(11) 0.0569(8) 0.0076(7) 0.0068(7) -0.0048(7) S1 0.0452(9) 0.0429(9) 0.0468(8) -0.0007(7) 0.0041(7) -0.0021(7) S2 0.0429(9) 0.0423(9) 0.0438(8) 0.0009(6) 0.0043(6) 0.0003(7) Rh1 0.0428(3) 0.0408(3) 0.0433(2) 0.0035(2) 0.00392(18) 0.0000(2) Rh2 0.0400(3) 0.0449(3) 0.0423(2) 0.0046(2) 0.00089(18) -0.0021(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.369(19) . ? C1 C2 1.44(2) . ? C1 C6 1.470(18) . ? C1 Rh1 2.116(8) . ? C2 C3 1.40(2) . ? C2 C7 1.502(17) . ? C2 Rh1 2.123(7) . ? C3 C4 1.289(16) . ? C3 C8 1.475(17) . ? C3 Rh1 2.157(7) . ? C4 C5 1.256(16) . ? C4 C9 1.513(17) . ? C4 Rh1 2.186(9) . ? C5 C10 1.496(17) . ? C5 Rh1 2.180(9) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.381(13) . ? C11 C15 1.384(14) . ? C11 C16 1.502(13) . ? C11 Rh2 2.175(7) . ? C12 C13 1.407(11) . ? C12 C17 1.529(12) . ? C12 Rh2 2.161(7) . ? C13 C14 1.408(11) . ? C13 C18 1.491(11) . ? C13 Rh2 2.132(7) . ? C14 C15 1.373(13) . ? C14 C19 1.504(13) . ? C14 Rh2 2.167(7) . ? C15 C20 1.487(13) . ? C15 Rh2 2.185(7) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.494(10) . ? C21 S1 1.827(6) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.347(11) . ? C22 C23 1.384(11) . ? C23 C24 1.407(12) . ? C23 H23 0.9300 . ? C24 C25 1.355(15) . ? C24 H24 0.9300 . ? C25 C26 1.357(16) . ? C25 H25 0.9300 . ? C26 C27 1.398(13) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.512(10) . ? C28 S2 1.814(7) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.374(9) . ? C29 C34 1.383(9) . ? C30 C31 1.401(13) . ? C30 H30 0.9300 . ? C31 C32 1.364(13) . ? C31 H31 0.9300 . ? C32 C33 1.356(12) . ? C32 H32 0.9300 . ? C33 C34 1.372(11) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? Cl1 Rh1 2.3802(17) . ? Cl2 Rh2 2.3884(16) . ? S1 Rh2 2.3711(18) . ? S1 Rh1 2.3725(17) . ? S2 Rh1 2.3681(17) . ? S2 Rh2 2.3688(15) . ? 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 C1 C2 105.5(10) . . ? C5 C1 C6 132(3) . . ? C2 C1 C6 122(3) . . ? C5 C1 Rh1 74.0(5) . . ? C2 C1 Rh1 70.4(6) . . ? C6 C1 Rh1 124.6(7) . . ? C3 C2 C1 102.9(9) . . ? C3 C2 C7 120(3) . . ? C1 C2 C7 137(3) . . ? C3 C2 Rh1 72.2(5) . . ? C1 C2 Rh1 69.8(5) . . ? C7 C2 Rh1 123.8(7) . . ? C4 C3 C2 109.0(10) . . ? C4 C3 C8 117(2) . . ? C2 C3 C8 134(2) . . ? C4 C3 Rh1 74.0(5) . . ? C2 C3 Rh1 69.6(5) . . ? C8 C3 Rh1 125.2(8) . . ? C5 C4 C3 112.9(11) . . ? C5 C4 C9 114.3(19) . . ? C3 C4 C9 132.8(19) . . ? C5 C4 Rh1 73.0(6) . . ? C3 C4 Rh1 71.5(6) . . ? C9 C4 Rh1 124.6(8) . . ? C4 C5 C1 109.7(11) . . ? C4 C5 C10 131(2) . . ? C1 C5 C10 120(2) . . ? C4 C5 Rh1 73.6(6) . . ? C1 C5 Rh1 68.9(6) . . ? C10 C5 Rh1 124.9(8) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 . . ? C12 C11 C15 107.5(7) . . ? C12 C11 C16 128.1(13) . . ? C15 C11 C16 124.3(13) . . ? C12 C11 Rh2 70.9(4) . . ? C15 C11 Rh2 71.9(5) . . ? C16 C11 Rh2 124.8(6) . . ? C11 C12 C13 108.6(7) . . ? C11 C12 C17 126.0(11) . . ? C13 C12 C17 125.4(11) . . ? C11 C12 Rh2 72.0(5) . . ? C13 C12 Rh2 69.8(4) . . ? C17 C12 Rh2 124.1(6) . . ? C12 C13 C14 106.6(7) . . ? C12 C13 C18 125.7(10) . . ? C14 C13 C18 127.2(10) . . ? C12 C13 Rh2 72.0(4) . . ? C14 C13 Rh2 72.2(5) . . ? C18 C13 Rh2 126.9(6) . . ? C15 C14 C13 107.7(8) . . ? C15 C14 C19 127.6(11) . . ? C13 C14 C19 124.6(11) . . ? C15 C14 Rh2 72.3(5) . . ? C13 C14 Rh2 69.6(4) . . ? C19 C14 Rh2 126.3(6) . . ? C14 C15 C11 109.5(7) . . ? C14 C15 C20 126.9(13) . . ? C11 C15 C20 123.6(13) . . ? C14 C15 Rh2 70.9(4) . . ? C11 C15 Rh2 71.1(4) . . ? C20 C15 Rh2 126.3(7) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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 . . ? C22 C21 S1 111.5(4) . . ? C22 C21 H21A 109.3 . . ? S1 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? S1 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C27 C22 C23 117.6(7) . . ? C27 C22 C21 121.6(7) . . ? C23 C22 C21 120.7(7) . . ? C22 C23 C24 120.8(9) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C25 C24 C23 119.3(9) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C24 C25 C26 120.9(9) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C27 118.8(10) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C22 C27 C26 122.6(9) . . ? C22 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C29 C28 S2 111.5(5) . . ? C29 C28 H28A 109.3 . . ? S2 C28 H28A 109.3 . . ? C29 C28 H28B 109.3 . . ? S2 C28 H28B 109.3 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C34 117.5(7) . . ? C30 C29 C28 121.2(6) . . ? C34 C29 C28 121.2(6) . . ? C29 C30 C31 120.8(7) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 119.6(8) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C33 C32 C31 120.2(8) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C34 120.1(7) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C29 121.6(7) . . ? C33 C34 H34 119.2 . . ? C29 C34 H34 119.2 . . ? C21 S1 Rh2 107.0(2) . . ? C21 S1 Rh1 111.2(3) . . ? Rh2 S1 Rh1 100.10(7) . . ? C28 S2 Rh1 106.8(2) . . ? C28 S2 Rh2 112.2(2) . . ? Rh1 S2 Rh2 100.29(6) . . ? C1 Rh1 C2 39.8(6) . . ? C1 Rh1 C3 62.7(4) . . ? C2 Rh1 C3 38.1(5) . . ? C1 Rh1 C5 37.1(5) . . ? C2 Rh1 C5 62.7(4) . . ? C3 Rh1 C5 58.6(4) . . ? C1 Rh1 C4 59.9(4) . . ? C2 Rh1 C4 61.0(4) . . ? C3 Rh1 C4 34.5(5) . . ? C5 Rh1 C4 33.4(4) . . ? C1 Rh1 S2 104.9(5) . . ? C2 Rh1 S2 93.6(3) . . ? C3 Rh1 S2 121.1(4) . . ? C5 Rh1 S2 141.1(5) . . ? C4 Rh1 S2 154.0(3) . . ? C1 Rh1 S1 103.3(4) . . ? C2 Rh1 S1 139.6(7) . . ? C3 Rh1 S1 156.5(3) . . ? C5 Rh1 S1 98.6(3) . . ? C4 Rh1 S1 122.8(4) . . ? S2 Rh1 S1 79.52(6) . . ? C1 Rh1 Cl1 155.1(3) . . ? C2 Rh1 Cl1 125.7(7) . . ? C3 Rh1 Cl1 94.4(3) . . ? C5 Rh1 Cl1 123.7(5) . . ? C4 Rh1 Cl1 95.9(3) . . ? S2 Rh1 Cl1 95.09(6) . . ? S1 Rh1 Cl1 94.73(6) . . ? C13 Rh2 C12 38.2(3) . . ? C13 Rh2 C14 38.2(3) . . ? C12 Rh2 C14 62.9(3) . . ? C13 Rh2 C11 63.4(3) . . ? C12 Rh2 C11 37.1(4) . . ? C14 Rh2 C11 62.5(3) . . ? C13 Rh2 C15 62.7(3) . . ? C12 Rh2 C15 61.7(3) . . ? C14 Rh2 C15 36.8(3) . . ? C11 Rh2 C15 37.0(4) . . ? C13 Rh2 S2 104.7(2) . . ? C12 Rh2 S2 95.8(2) . . ? C14 Rh2 S2 141.0(2) . . ? C11 Rh2 S2 120.4(3) . . ? C15 Rh2 S2 156.5(3) . . ? C13 Rh2 S1 101.4(2) . . ? C12 Rh2 S1 137.2(3) . . ? C14 Rh2 S1 94.3(2) . . ? C11 Rh2 S1 156.5(3) . . ? C15 Rh2 S1 121.1(4) . . ? S2 Rh2 S1 79.53(5) . . ? C13 Rh2 Cl2 156.54(17) . . ? C12 Rh2 Cl2 127.2(3) . . ? C14 Rh2 Cl2 124.9(2) . . ? C11 Rh2 Cl2 95.1(3) . . ? C15 Rh2 Cl2 94.7(2) . . ? S2 Rh2 Cl2 94.11(6) . . ? S1 Rh2 Cl2 95.63(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.9(9) . . . . ? C6 C1 C2 C3 -175.5(8) . . . . ? Rh1 C1 C2 C3 65.3(6) . . . . ? C5 C1 C2 C7 175.4(10) . . . . ? C6 C1 C2 C7 0.7(16) . . . . ? Rh1 C1 C2 C7 -118.4(11) . . . . ? C5 C1 C2 Rh1 -66.2(6) . . . . ? C6 C1 C2 Rh1 119.2(9) . . . . ? C1 C2 C3 C4 0.4(9) . . . . ? C7 C2 C3 C4 -176.7(9) . . . . ? Rh1 C2 C3 C4 64.0(6) . . . . ? C1 C2 C3 C8 176.7(11) . . . . ? C7 C2 C3 C8 -0.4(16) . . . . ? Rh1 C2 C3 C8 -119.7(12) . . . . ? C1 C2 C3 Rh1 -63.6(5) . . . . ? C7 C2 C3 Rh1 119.3(9) . . . . ? C2 C3 C4 C5 0.3(11) . . . . ? C8 C3 C4 C5 -176.6(9) . . . . ? Rh1 C3 C4 C5 61.6(7) . . . . ? C2 C3 C4 C9 178.4(11) . . . . ? C8 C3 C4 C9 1.4(16) . . . . ? Rh1 C3 C4 C9 -120.4(12) . . . . ? C2 C3 C4 Rh1 -61.2(6) . . . . ? C8 C3 C4 Rh1 121.8(9) . . . . ? C3 C4 C5 C1 -1.0(11) . . . . ? C9 C4 C5 C1 -179.4(9) . . . . ? Rh1 C4 C5 C1 59.7(6) . . . . ? C3 C4 C5 C10 177.2(10) . . . . ? C9 C4 C5 C10 -1.3(16) . . . . ? Rh1 C4 C5 C10 -122.2(11) . . . . ? C3 C4 C5 Rh1 -60.7(7) . . . . ? C9 C4 C5 Rh1 120.9(9) . . . . ? C2 C1 C5 C4 1.2(10) . . . . ? C6 C1 C5 C4 174.9(10) . . . . ? Rh1 C1 C5 C4 -62.6(7) . . . . ? C2 C1 C5 C10 -177.2(9) . . . . ? C6 C1 C5 C10 -3.4(15) . . . . ? Rh1 C1 C5 C10 119.0(9) . . . . ? C2 C1 C5 Rh1 63.7(6) . . . . ? C6 C1 C5 Rh1 -122.5(10) . . . . ? C15 C11 C12 C13 -2.5(8) . . . . ? C16 C11 C12 C13 -179.8(8) . . . . ? Rh2 C11 C12 C13 60.5(5) . . . . ? C15 C11 C12 C17 177.5(8) . . . . ? C16 C11 C12 C17 0.2(14) . . . . ? Rh2 C11 C12 C17 -119.5(8) . . . . ? C15 C11 C12 Rh2 -63.0(6) . . . . ? C16 C11 C12 Rh2 119.7(9) . . . . ? C11 C12 C13 C14 2.5(8) . . . . ? C17 C12 C13 C14 -177.5(8) . . . . ? Rh2 C12 C13 C14 64.4(5) . . . . ? C11 C12 C13 C18 175.3(8) . . . . ? C17 C12 C13 C18 -4.7(12) . . . . ? Rh2 C12 C13 C18 -122.9(8) . . . . ? C11 C12 C13 Rh2 -61.8(5) . . . . ? C17 C12 C13 Rh2 118.2(8) . . . . ? C12 C13 C14 C15 -1.6(9) . . . . ? C18 C13 C14 C15 -174.2(8) . . . . ? Rh2 C13 C14 C15 62.7(6) . . . . ? C12 C13 C14 C19 175.1(7) . . . . ? C18 C13 C14 C19 2.5(13) . . . . ? Rh2 C13 C14 C19 -120.7(8) . . . . ? C12 C13 C14 Rh2 -64.2(5) . . . . ? C18 C13 C14 Rh2 123.2(9) . . . . ? C13 C14 C15 C11 0.0(9) . . . . ? C19 C14 C15 C11 -176.5(8) . . . . ? Rh2 C14 C15 C11 60.9(6) . . . . ? C13 C14 C15 C20 177.6(9) . . . . ? C19 C14 C15 C20 1.0(15) . . . . ? Rh2 C14 C15 C20 -121.5(10) . . . . ? C13 C14 C15 Rh2 -60.9(5) . . . . ? C19 C14 C15 Rh2 122.6(9) . . . . ? C12 C11 C15 C14 1.5(9) . . . . ? C16 C11 C15 C14 179.0(8) . . . . ? Rh2 C11 C15 C14 -60.8(6) . . . . ? C12 C11 C15 C20 -176.1(8) . . . . ? C16 C11 C15 C20 1.3(14) . . . . ? Rh2 C11 C15 C20 121.6(9) . . . . ? C12 C11 C15 Rh2 62.3(5) . . . . ? C16 C11 C15 Rh2 -120.2(9) . . . . ? S1 C21 C22 C27 111.2(7) . . . . ? S1 C21 C22 C23 -65.8(7) . . . . ? C27 C22 C23 C24 1.7(11) . . . . ? C21 C22 C23 C24 178.8(7) . . . . ? C22 C23 C24 C25 -2.2(13) . . . . ? C23 C24 C25 C26 2.1(14) . . . . ? C24 C25 C26 C27 -1.7(15) . . . . ? C23 C22 C27 C26 -1.3(12) . . . . ? C21 C22 C27 C26 -178.4(7) . . . . ? C25 C26 C27 C22 1.3(14) . . . . ? S2 C28 C29 C30 99.2(7) . . . . ? S2 C28 C29 C34 -77.8(7) . . . . ? C34 C29 C30 C31 -1.6(13) . . . . ? C28 C29 C30 C31 -178.6(8) . . . . ? C29 C30 C31 C32 -0.9(16) . . . . ? C30 C31 C32 C33 0.9(16) . . . . ? C31 C32 C33 C34 1.7(14) . . . . ? C32 C33 C34 C29 -4.3(12) . . . . ? C30 C29 C34 C33 4.2(11) . . . . ? C28 C29 C34 C33 -178.8(7) . . . . ? C22 C21 S1 Rh2 174.3(5) . . . . ? C22 C21 S1 Rh1 -77.3(6) . . . . ? C29 C28 S2 Rh1 170.2(4) . . . . ? C29 C28 S2 Rh2 -80.8(4) . . . . ? C5 C1 Rh1 C2 113.4(9) . . . . ? C6 C1 Rh1 C2 -116(3) . . . . ? C5 C1 Rh1 C3 73.2(7) . . . . ? C2 C1 Rh1 C3 -40.3(7) . . . . ? C6 C1 Rh1 C3 -156(3) . . . . ? C2 C1 Rh1 C5 -113.4(9) . . . . ? C6 C1 Rh1 C5 131(3) . . . . ? C5 C1 Rh1 C4 33.7(6) . . . . ? C2 C1 Rh1 C4 -79.7(8) . . . . ? C6 C1 Rh1 C4 165(3) . . . . ? C5 C1 Rh1 S2 -169.2(7) . . . . ? C2 C1 Rh1 S2 77.4(9) . . . . ? C6 C1 Rh1 S2 -38(3) . . . . ? C5 C1 Rh1 S1 -86.7(7) . . . . ? C2 C1 Rh1 S1 159.9(8) . . . . ? C6 C1 Rh1 S1 44(3) . . . . ? C5 C1 Rh1 Cl1 48(2) . . . . ? C2 C1 Rh1 Cl1 -65(2) . . . . ? C6 C1 Rh1 Cl1 179(2) . . . . ? C3 C2 Rh1 C1 -111.6(9) . . . . ? C7 C2 Rh1 C1 134(3) . . . . ? C1 C2 Rh1 C3 111.6(9) . . . . ? C7 C2 Rh1 C3 -114(3) . . . . ? C3 C2 Rh1 C5 -73.0(7) . . . . ? C1 C2 Rh1 C5 38.6(7) . . . . ? C7 C2 Rh1 C5 173(3) . . . . ? C3 C2 Rh1 C4 -35.0(6) . . . . ? C1 C2 Rh1 C4 76.6(8) . . . . ? C7 C2 Rh1 C4 -149(3) . . . . ? C3 C2 Rh1 S2 139.3(8) . . . . ? C1 C2 Rh1 S2 -109.1(9) . . . . ? C7 C2 Rh1 S2 25(3) . . . . ? C3 C2 Rh1 S1 -142.7(8) . . . . ? C1 C2 Rh1 S1 -31.1(10) . . . . ? C7 C2 Rh1 S1 103(3) . . . . ? C3 C2 Rh1 Cl1 40.4(9) . . . . ? C1 C2 Rh1 Cl1 152.0(9) . . . . ? C7 C2 Rh1 Cl1 -74(3) . . . . ? C4 C3 Rh1 C1 -75.8(8) . . . . ? C2 C3 Rh1 C1 42.1(8) . . . . ? C8 C3 Rh1 C1 172(2) . . . . ? C4 C3 Rh1 C2 -117.9(10) . . . . ? C8 C3 Rh1 C2 130(3) . . . . ? C4 C3 Rh1 C5 -33.2(7) . . . . ? C2 C3 Rh1 C5 84.7(9) . . . . ? C8 C3 Rh1 C5 -145(2) . . . . ? C2 C3 Rh1 C4 117.9(10) . . . . ? C8 C3 Rh1 C4 -112(2) . . . . ? C4 C3 Rh1 S2 -167.3(7) . . . . ? C2 C3 Rh1 S2 -49.4(9) . . . . ? C8 C3 Rh1 S2 80(2) . . . . ? C4 C3 Rh1 S1 -18.6(16) . . . . ? C2 C3 Rh1 S1 99.2(15) . . . . ? C8 C3 Rh1 S1 -130.9(19) . . . . ? C4 C3 Rh1 Cl1 94.1(7) . . . . ? C2 C3 Rh1 Cl1 -148.1(9) . . . . ? C8 C3 Rh1 Cl1 -18(2) . . . . ? C4 C5 Rh1 C1 119.4(10) . . . . ? C10 C5 Rh1 C1 -112(3) . . . . ? C4 C5 Rh1 C2 78.0(9) . . . . ? C1 C5 Rh1 C2 -41.4(8) . . . . ? C10 C5 Rh1 C2 -153(3) . . . . ? C4 C5 Rh1 C3 34.3(7) . . . . ? C1 C5 Rh1 C3 -85.1(8) . . . . ? C10 C5 Rh1 C3 163(3) . . . . ? C1 C5 Rh1 C4 -119.4(10) . . . . ? C10 C5 Rh1 C4 129(3) . . . . ? C4 C5 Rh1 S2 136.2(8) . . . . ? C1 C5 Rh1 S2 16.8(10) . . . . ? C10 C5 Rh1 S2 -95(2) . . . . ? C4 C5 Rh1 S1 -139.9(7) . . . . ? C1 C5 Rh1 S1 100.7(8) . . . . ? C10 C5 Rh1 S1 -11(2) . . . . ? C4 C5 Rh1 Cl1 -38.3(8) . . . . ? C1 C5 Rh1 Cl1 -157.7(8) . . . . ? C10 C5 Rh1 Cl1 90(2) . . . . ? C5 C4 Rh1 C1 -37.4(8) . . . . ? C3 C4 Rh1 C1 84.6(9) . . . . ? C9 C4 Rh1 C1 -146(2) . . . . ? C5 C4 Rh1 C2 -83.5(10) . . . . ? C3 C4 Rh1 C2 38.6(8) . . . . ? C9 C4 Rh1 C2 168(2) . . . . ? C5 C4 Rh1 C3 -122.1(10) . . . . ? C9 C4 Rh1 C3 130(2) . . . . ? C3 C4 Rh1 C5 122.1(10) . . . . ? C9 C4 Rh1 C5 -108(2) . . . . ? C5 C4 Rh1 S2 -96.6(13) . . . . ? C3 C4 Rh1 S2 25.5(14) . . . . ? C9 C4 Rh1 S2 155.2(18) . . . . ? C5 C4 Rh1 S1 49.2(8) . . . . ? C3 C4 Rh1 S1 171.3(7) . . . . ? C9 C4 Rh1 S1 -59(2) . . . . ? C5 C4 Rh1 Cl1 148.7(8) . . . . ? C3 C4 Rh1 Cl1 -89.2(8) . . . . ? C9 C4 Rh1 Cl1 41(2) . . . . ? C28 S2 Rh1 C1 -136.1(5) . . . . ? Rh2 S2 Rh1 C1 106.8(5) . . . . ? C28 S2 Rh1 C2 -97.4(7) . . . . ? Rh2 S2 Rh1 C2 145.5(7) . . . . ? C28 S2 Rh1 C3 -69.3(4) . . . . ? Rh2 S2 Rh1 C3 173.5(3) . . . . ? C28 S2 Rh1 C5 -146.5(4) . . . . ? Rh2 S2 Rh1 C5 96.4(4) . . . . ? C28 S2 Rh1 C4 -85.9(9) . . . . ? Rh2 S2 Rh1 C4 157.0(8) . . . . ? C28 S2 Rh1 S1 122.8(2) . . . . ? Rh2 S2 Rh1 S1 5.68(6) . . . . ? C28 S2 Rh1 Cl1 28.9(2) . . . . ? Rh2 S2 Rh1 Cl1 -88.20(7) . . . . ? C21 S1 Rh1 C1 138.5(6) . . . . ? Rh2 S1 Rh1 C1 -108.7(5) . . . . ? C21 S1 Rh1 C2 158.3(4) . . . . ? Rh2 S1 Rh1 C2 -88.8(4) . . . . ? C21 S1 Rh1 C3 88.4(11) . . . . ? Rh2 S1 Rh1 C3 -158.7(10) . . . . ? C21 S1 Rh1 C5 100.9(5) . . . . ? Rh2 S1 Rh1 C5 -146.2(5) . . . . ? C21 S1 Rh1 C4 76.0(4) . . . . ? Rh2 S1 Rh1 C4 -171.2(3) . . . . ? C21 S1 Rh1 S2 -118.5(2) . . . . ? Rh2 S1 Rh1 S2 -5.67(6) . . . . ? C21 S1 Rh1 Cl1 -24.2(2) . . . . ? Rh2 S1 Rh1 Cl1 88.64(7) . . . . ? C14 C13 Rh2 C12 -114.9(6) . . . . ? C18 C13 Rh2 C12 121.6(12) . . . . ? C12 C13 Rh2 C14 114.9(6) . . . . ? C18 C13 Rh2 C14 -123.5(12) . . . . ? C12 C13 Rh2 C11 36.4(5) . . . . ? C14 C13 Rh2 C11 -78.5(6) . . . . ? C18 C13 Rh2 C11 158.0(12) . . . . ? C12 C13 Rh2 C15 78.1(6) . . . . ? C14 C13 Rh2 C15 -36.7(6) . . . . ? C18 C13 Rh2 C15 -160.3(12) . . . . ? C12 C13 Rh2 S2 -80.6(4) . . . . ? C14 C13 Rh2 S2 164.6(4) . . . . ? C18 C13 Rh2 S2 41.0(11) . . . . ? C12 C13 Rh2 S1 -162.6(4) . . . . ? C14 C13 Rh2 S1 82.5(4) . . . . ? C18 C13 Rh2 S1 -41.0(11) . . . . ? C12 C13 Rh2 Cl2 61.9(8) . . . . ? C14 C13 Rh2 Cl2 -53.0(8) . . . . ? C18 C13 Rh2 Cl2 -176.6(9) . . . . ? C11 C12 Rh2 C13 118.5(7) . . . . ? C17 C12 Rh2 C13 -119.7(13) . . . . ? C11 C12 Rh2 C14 79.4(6) . . . . ? C13 C12 Rh2 C14 -39.1(4) . . . . ? C17 C12 Rh2 C14 -158.8(13) . . . . ? C13 C12 Rh2 C11 -118.5(7) . . . . ? C17 C12 Rh2 C11 121.8(14) . . . . ? C11 C12 Rh2 C15 37.7(5) . . . . ? C13 C12 Rh2 C15 -80.8(5) . . . . ? C17 C12 Rh2 C15 159.5(13) . . . . ? C11 C12 Rh2 S2 -135.0(5) . . . . ? C13 C12 Rh2 S2 106.5(4) . . . . ? C17 C12 Rh2 S2 -13.3(12) . . . . ? C11 C12 Rh2 S1 144.1(5) . . . . ? C13 C12 Rh2 S1 25.6(5) . . . . ? C17 C12 Rh2 S1 -94.2(12) . . . . ? C11 C12 Rh2 Cl2 -35.4(6) . . . . ? C13 C12 Rh2 Cl2 -153.9(4) . . . . ? C17 C12 Rh2 Cl2 86.4(12) . . . . ? C15 C14 Rh2 C13 -117.4(8) . . . . ? C19 C14 Rh2 C13 118.5(13) . . . . ? C15 C14 Rh2 C12 -78.3(7) . . . . ? C13 C14 Rh2 C12 39.1(4) . . . . ? C19 C14 Rh2 C12 157.6(12) . . . . ? C15 C14 Rh2 C11 -36.3(6) . . . . ? C13 C14 Rh2 C11 81.1(5) . . . . ? C19 C14 Rh2 C11 -160.3(13) . . . . ? C13 C14 Rh2 C15 117.4(8) . . . . ? C19 C14 Rh2 C15 -124.1(13) . . . . ? C15 C14 Rh2 S2 -141.5(6) . . . . ? C13 C14 Rh2 S2 -24.1(6) . . . . ? C19 C14 Rh2 S2 94.4(11) . . . . ? C15 C14 Rh2 S1 139.8(6) . . . . ? C13 C14 Rh2 S1 -102.9(4) . . . . ? C19 C14 Rh2 S1 15.7(11) . . . . ? C15 C14 Rh2 Cl2 39.8(7) . . . . ? C13 C14 Rh2 Cl2 157.2(3) . . . . ? C19 C14 Rh2 Cl2 -84.3(12) . . . . ? C12 C11 Rh2 C13 -37.5(5) . . . . ? C15 C11 Rh2 C13 79.1(5) . . . . ? C16 C11 Rh2 C13 -161.2(15) . . . . ? C15 C11 Rh2 C12 116.6(7) . . . . ? C16 C11 Rh2 C12 -123.7(16) . . . . ? C12 C11 Rh2 C14 -80.6(5) . . . . ? C15 C11 Rh2 C14 36.0(5) . . . . ? C16 C11 Rh2 C14 155.7(15) . . . . ? C12 C11 Rh2 C15 -116.6(7) . . . . ? C16 C11 Rh2 C15 119.7(16) . . . . ? C12 C11 Rh2 S2 54.6(5) . . . . ? C15 C11 Rh2 S2 171.2(4) . . . . ? C16 C11 Rh2 S2 -69.1(14) . . . . ? C12 C11 Rh2 S1 -90.6(10) . . . . ? C15 C11 Rh2 S1 26.0(11) . . . . ? C16 C11 Rh2 S1 145.6(11) . . . . ? C12 C11 Rh2 Cl2 152.4(5) . . . . ? C15 C11 Rh2 Cl2 -91.0(5) . . . . ? C16 C11 Rh2 Cl2 28.7(14) . . . . ? C14 C15 Rh2 C13 38.2(5) . . . . ? C11 C15 Rh2 C13 -81.2(5) . . . . ? C20 C15 Rh2 C13 160.5(15) . . . . ? C14 C15 Rh2 C12 81.6(6) . . . . ? C11 C15 Rh2 C12 -37.8(5) . . . . ? C20 C15 Rh2 C12 -156.1(15) . . . . ? C11 C15 Rh2 C14 -119.4(7) . . . . ? C20 C15 Rh2 C14 122.3(17) . . . . ? C14 C15 Rh2 C11 119.4(7) . . . . ? C20 C15 Rh2 C11 -118.3(16) . . . . ? C14 C15 Rh2 S2 100.1(9) . . . . ? C11 C15 Rh2 S2 -19.3(10) . . . . ? C20 C15 Rh2 S2 -137.6(12) . . . . ? C14 C15 Rh2 S1 -48.8(6) . . . . ? C11 C15 Rh2 S1 -168.2(5) . . . . ? C20 C15 Rh2 S1 73.5(14) . . . . ? C14 C15 Rh2 Cl2 -148.2(5) . . . . ? C11 C15 Rh2 Cl2 92.3(5) . . . . ? C20 C15 Rh2 Cl2 -25.9(14) . . . . ? C28 S2 Rh2 C13 142.1(3) . . . . ? Rh1 S2 Rh2 C13 -104.8(2) . . . . ? C28 S2 Rh2 C12 104.3(4) . . . . ? Rh1 S2 Rh2 C12 -142.7(3) . . . . ? C28 S2 Rh2 C14 157.3(4) . . . . ? Rh1 S2 Rh2 C14 -89.6(4) . . . . ? C28 S2 Rh2 C11 74.6(4) . . . . ? Rh1 S2 Rh2 C11 -172.3(3) . . . . ? C28 S2 Rh2 C15 88.0(7) . . . . ? Rh1 S2 Rh2 C15 -158.9(6) . . . . ? C28 S2 Rh2 S1 -118.7(3) . . . . ? Rh1 S2 Rh2 S1 -5.69(6) . . . . ? C28 S2 Rh2 Cl2 -23.8(3) . . . . ? Rh1 S2 Rh2 Cl2 89.29(6) . . . . ? C21 S1 Rh2 C13 -135.2(3) . . . . ? Rh1 S1 Rh2 C13 108.8(2) . . . . ? C21 S1 Rh2 C12 -151.0(4) . . . . ? Rh1 S1 Rh2 C12 93.0(3) . . . . ? C21 S1 Rh2 C14 -97.2(3) . . . . ? Rh1 S1 Rh2 C14 146.8(2) . . . . ? C21 S1 Rh2 C11 -88.3(8) . . . . ? Rh1 S1 Rh2 C11 155.7(8) . . . . ? C21 S1 Rh2 C15 -70.4(4) . . . . ? Rh1 S1 Rh2 C15 173.6(3) . . . . ? C21 S1 Rh2 S2 121.7(3) . . . . ? Rh1 S1 Rh2 S2 5.67(6) . . . . ? C21 S1 Rh2 Cl2 28.5(3) . . . . ? Rh1 S1 Rh2 Cl2 -87.49(6) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 26.09 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.416 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 939466' ####################################################################### # # 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_d:complex2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 Cl2 Rh2 S2' _chemical_formula_sum 'C36 H48 Cl2 Rh2 S2' _chemical_formula_weight 821.58 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 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 21.115(4) _cell_length_b 17.085(3) _cell_length_c 20.881(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.72(3) _cell_angle_gamma 90.00 _cell_volume 7318(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.60 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 1.185 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.167 _exptl_absorpt_correction_T_max 0.639 _exptl_absorpt_process_details 'Walker, N. & Stuart, D. (1983)' _exptl_special_details ; A crystal was mounted at 173K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using MoK\a graphite monochromated radiation. Image plate distance 70mm, \f oscillation scans 0 - 200\%, step \D\f = 1.0\%, 5 minutes per frame. ; _diffrn_ambient_temperature 173(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12856 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0911 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 26.11 _reflns_number_total 6414 _reflns_number_gt 3199 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie, 2000)' _computing_cell_refinement 'CELL (Stoe & Cie, 2000)' _computing_data_reduction 'INTEGRATE (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-32 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0344P)^2^] 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 6414 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0873 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0774 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 0.764 _refine_ls_restrained_S_all 0.764 _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 C1 C 0.3431(5) 0.6046(4) 0.1607(4) 0.091(3) Uani 1 1 d . . . C2 C 0.3365(4) 0.5379(4) 0.1960(3) 0.077(2) Uani 1 1 d . . . C3 C 0.2727(4) 0.5122(2) 0.1753(3) 0.067(2) Uani 1 1 d . . . C4 C 0.2391(4) 0.5617(3) 0.1237(2) 0.0681(19) Uani 1 1 d . . . C5 C 0.2819(6) 0.6188(3) 0.1157(3) 0.100(3) Uani 1 1 d . . . C6 C 0.4051(6) 0.6519(6) 0.1627(6) 0.204(7) Uani 1 1 d . . . H6A H 0.4053 0.6977 0.1893 0.305 Uiso 1 1 calc R . . H6B H 0.4063 0.6672 0.1188 0.305 Uiso 1 1 calc R . . H6C H 0.4426 0.6204 0.1813 0.305 Uiso 1 1 calc R . . C7 C 0.3880(6) 0.4967(6) 0.2473(4) 0.182(6) Uani 1 1 d . . . H7A H 0.3789 0.4416 0.2461 0.273 Uiso 1 1 calc R . . H7B H 0.3878 0.5169 0.2902 0.273 Uiso 1 1 calc R . . H7C H 0.4300 0.5053 0.2384 0.273 Uiso 1 1 calc R . . C8 C 0.2436(6) 0.4388(3) 0.1992(4) 0.154(5) Uani 1 1 d . . . H8A H 0.2610 0.4326 0.2457 0.232 Uiso 1 1 calc R . . H8B H 0.2545 0.3938 0.1764 0.232 Uiso 1 1 calc R . . H8C H 0.1971 0.4439 0.1903 0.232 Uiso 1 1 calc R . . C9 C 0.1694(5) 0.5505(5) 0.0853(4) 0.147(4) Uani 1 1 d . . . H9A H 0.1531 0.5987 0.0639 0.221 Uiso 1 1 calc R . . H9B H 0.1430 0.5353 0.1148 0.221 Uiso 1 1 calc R . . H9C H 0.1677 0.5104 0.0527 0.221 Uiso 1 1 calc R . . C10 C 0.2684(8) 0.6836(4) 0.0644(3) 0.186(7) Uani 1 1 d . . . H10A H 0.2252 0.6775 0.0371 0.279 Uiso 1 1 calc R . . H10B H 0.2995 0.6808 0.0377 0.279 Uiso 1 1 calc R . . H10C H 0.2719 0.7335 0.0862 0.279 Uiso 1 1 calc R . . C11 C 0.1147(3) 0.5762(3) 0.3921(3) 0.0604(16) Uani 1 1 d . . . C12 C 0.1464(3) 0.5118(2) 0.3650(3) 0.0554(15) Uani 1 1 d . . . C13 C 0.2092(3) 0.5033(2) 0.4029(2) 0.0575(16) Uani 1 1 d . . . C14 C 0.2204(3) 0.5628(2) 0.4538(2) 0.0558(16) Uani 1 1 d . . . C15 C 0.1612(3) 0.6052(2) 0.4472(2) 0.0555(15) Uani 1 1 d . . . C16 C 0.0471(4) 0.6024(3) 0.3702(4) 0.095(2) Uani 1 1 d . . . H16A H 0.0198 0.5711 0.3909 0.142 Uiso 1 1 calc R . . H16B H 0.0330 0.5971 0.3232 0.142 Uiso 1 1 calc R . . H16C H 0.0440 0.6563 0.3822 0.142 Uiso 1 1 calc R . . C17 C 0.1110(4) 0.4592(3) 0.3088(3) 0.082(2) Uani 1 1 d . . . H17A H 0.1423 0.4319 0.2905 0.124 Uiso 1 1 calc R . . H17B H 0.0836 0.4905 0.2753 0.124 Uiso 1 1 calc R . . H17C H 0.0848 0.4219 0.3254 0.124 Uiso 1 1 calc R . . C18 C 0.2571(4) 0.4409(2) 0.3967(3) 0.075(2) Uani 1 1 d . . . H18A H 0.2615 0.4048 0.4327 0.113 Uiso 1 1 calc R . . H18B H 0.2986 0.4644 0.3975 0.113 Uiso 1 1 calc R . . H18C H 0.2418 0.4136 0.3558 0.113 Uiso 1 1 calc R . . C19 C 0.2829(4) 0.5735(3) 0.5053(3) 0.076(2) Uani 1 1 d . . . H19A H 0.2841 0.6251 0.5236 0.114 Uiso 1 1 calc R . . H19B H 0.3192 0.5666 0.4856 0.114 Uiso 1 1 calc R . . H19C H 0.2852 0.5354 0.5396 0.114 Uiso 1 1 calc R . . C20 C 0.1487(4) 0.6689(3) 0.4919(3) 0.079(2) Uani 1 1 d . . . H20A H 0.1895 0.6882 0.5179 0.118 Uiso 1 1 calc R . . H20B H 0.1232 0.6486 0.5205 0.118 Uiso 1 1 calc R . . H20C H 0.1254 0.7109 0.4660 0.118 Uiso 1 1 calc R . . C21 C 0.1248(3) 0.7232(2) 0.2193(2) 0.0701(19) Uani 1 1 d . . . H21A H 0.0888 0.7278 0.2406 0.084 Uiso 1 1 calc R . . H21B H 0.1555 0.7649 0.2359 0.084 Uiso 1 1 calc R . . C22 C 0.1007(4) 0.7321(3) 0.1494(3) 0.0744(19) Uani 1 1 d . . . H22A H 0.0741 0.6870 0.1323 0.089 Uiso 1 1 calc R . . H22B H 0.1374 0.7332 0.1288 0.089 Uiso 1 1 calc R . . C23 C 0.0598(4) 0.8073(3) 0.1301(3) 0.080(2) Uani 1 1 d . . . C24 C -0.0020(5) 0.8174(3) 0.1426(4) 0.099(3) Uani 1 1 d . . . H24 H -0.0182 0.7799 0.1668 0.119 Uiso 1 1 calc R . . C25 C -0.0394(5) 0.8827(4) 0.1191(4) 0.106(3) Uani 1 1 d . . . H25 H -0.0816 0.8875 0.1249 0.127 Uiso 1 1 calc R . . C26 C -0.0138(6) 0.9386(4) 0.0880(4) 0.112(4) Uani 1 1 d . . . H26 H -0.0380 0.9835 0.0738 0.135 Uiso 1 1 calc R . . C27 C 0.0467(6) 0.9313(4) 0.0770(5) 0.128(4) Uani 1 1 d . . . H27 H 0.0636 0.9704 0.0548 0.154 Uiso 1 1 calc R . . C28 C 0.0831(5) 0.8644(3) 0.0992(4) 0.117(3) Uani 1 1 d . . . H28 H 0.1248 0.8597 0.0921 0.140 Uiso 1 1 calc R . . C29 C 0.3499(3) 0.6934(2) 0.3696(2) 0.0527(13) Uani 1 1 d . . . H29A H 0.3274 0.7416 0.3537 0.063 Uiso 1 1 calc R . . H29B H 0.3547 0.6911 0.4169 0.063 Uiso 1 1 calc R . . C30 C 0.4167(3) 0.6944(3) 0.3551(3) 0.0699(17) Uani 1 1 d . . . H30A H 0.4404 0.6475 0.3729 0.084 Uiso 1 1 calc R . . H30B H 0.4123 0.6946 0.3078 0.084 Uiso 1 1 calc R . . C31 C 0.4542(3) 0.7653(3) 0.3850(3) 0.0637(16) Uani 1 1 d . . . C32 C 0.4996(4) 0.7615(3) 0.4432(3) 0.079(2) Uani 1 1 d . . . H32 H 0.5093 0.7134 0.4640 0.095 Uiso 1 1 calc R . . C33 C 0.5318(5) 0.8281(4) 0.4724(3) 0.103(3) Uani 1 1 d . . . H33 H 0.5631 0.8241 0.5119 0.123 Uiso 1 1 calc R . . C34 C 0.5176(5) 0.8986(4) 0.4434(4) 0.098(3) Uani 1 1 d . . . H34 H 0.5383 0.9435 0.4633 0.118 Uiso 1 1 calc R . . C35 C 0.4728(5) 0.9033(4) 0.3848(4) 0.103(3) Uani 1 1 d . . . H35 H 0.4640 0.9516 0.3641 0.124 Uiso 1 1 calc R . . C36 C 0.4403(4) 0.8378(3) 0.3557(3) 0.087(2) Uani 1 1 d . . . H36 H 0.4089 0.8423 0.3162 0.104 Uiso 1 1 calc R . . S1 S 0.16514(7) 0.62836(5) 0.24063(5) 0.0493(3) Uani 1 1 d . . . S2 S 0.30150(7) 0.61129(6) 0.33142(5) 0.0449(3) Uani 1 1 d . . . Cl1 Cl 0.28248(9) 0.76634(6) 0.21847(6) 0.0699(5) Uani 1 1 d . . . Cl2 Cl 0.20050(8) 0.75635(5) 0.37206(6) 0.0573(4) Uani 1 1 d . . . Rh1 Rh 0.26988(2) 0.627453(16) 0.215589(18) 0.04661(12) Uani 1 1 d . . . Rh2 Rh 0.19845(2) 0.618261(17) 0.357521(17) 0.04337(12) 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 C1 0.094(8) 0.111(5) 0.092(5) -0.033(4) 0.071(5) -0.028(5) C2 0.072(7) 0.104(4) 0.053(3) -0.018(3) 0.012(4) 0.031(4) C3 0.113(7) 0.043(2) 0.060(3) -0.007(2) 0.048(4) 0.006(3) C4 0.074(6) 0.074(3) 0.049(3) -0.025(3) -0.001(3) 0.021(3) C5 0.202(11) 0.054(3) 0.057(3) 0.002(3) 0.057(5) 0.006(4) C6 0.156(15) 0.266(11) 0.250(12) -0.145(10) 0.170(11) -0.135(10) C7 0.161(13) 0.266(10) 0.100(6) -0.035(6) -0.008(7) 0.157(11) C8 0.292(15) 0.049(3) 0.180(7) -0.033(4) 0.170(9) -0.029(4) C9 0.086(9) 0.194(8) 0.134(7) -0.103(6) -0.031(6) 0.030(6) C10 0.41(2) 0.096(4) 0.079(5) 0.025(4) 0.114(8) 0.038(7) C11 0.046(5) 0.069(3) 0.074(4) 0.001(2) 0.030(3) -0.007(3) C12 0.054(5) 0.050(2) 0.066(3) -0.003(2) 0.022(3) -0.010(2) C13 0.074(6) 0.044(2) 0.062(3) 0.007(2) 0.031(3) -0.001(2) C14 0.061(5) 0.056(2) 0.051(3) 0.008(2) 0.015(3) -0.010(3) C15 0.056(5) 0.058(2) 0.057(3) -0.007(2) 0.023(3) -0.004(3) C16 0.062(7) 0.087(4) 0.137(6) 0.003(4) 0.026(5) -0.009(3) C17 0.091(7) 0.075(3) 0.085(4) -0.022(3) 0.027(4) -0.034(3) C18 0.082(6) 0.057(3) 0.095(4) 0.014(3) 0.038(4) 0.014(3) C19 0.077(6) 0.089(3) 0.061(3) 0.011(3) 0.014(4) -0.009(3) C20 0.096(7) 0.071(3) 0.083(4) -0.019(3) 0.047(4) -0.002(3) C21 0.071(6) 0.061(3) 0.066(3) -0.007(2) -0.008(3) 0.007(3) C22 0.066(6) 0.076(3) 0.078(4) 0.003(3) 0.012(4) 0.000(3) C23 0.079(7) 0.066(3) 0.078(4) 0.008(3) -0.016(4) -0.011(3) C24 0.118(10) 0.078(4) 0.101(5) 0.007(3) 0.025(5) 0.010(4) C25 0.091(9) 0.101(5) 0.121(6) -0.003(4) 0.017(5) 0.026(5) C26 0.135(11) 0.079(4) 0.102(6) 0.010(4) -0.012(7) 0.028(5) C27 0.128(12) 0.088(5) 0.151(8) 0.031(5) 0.000(8) -0.011(5) C28 0.078(8) 0.079(4) 0.167(7) 0.023(4) -0.022(6) -0.016(4) C29 0.034(4) 0.062(2) 0.061(3) -0.008(2) 0.009(3) -0.007(2) C30 0.045(5) 0.078(3) 0.084(4) -0.012(3) 0.010(3) -0.003(3) C31 0.032(5) 0.081(3) 0.075(4) -0.005(3) 0.006(3) -0.007(3) C32 0.058(6) 0.094(4) 0.082(4) 0.004(3) 0.007(4) -0.007(3) C33 0.083(8) 0.135(5) 0.081(5) -0.004(4) -0.002(4) -0.031(5) C34 0.081(8) 0.110(5) 0.103(5) -0.019(4) 0.018(5) -0.040(4) C35 0.086(8) 0.093(4) 0.122(6) 0.010(4) 0.007(5) -0.036(4) C36 0.068(7) 0.093(4) 0.089(4) 0.010(3) -0.001(4) -0.022(4) S1 0.0439(10) 0.0490(5) 0.0509(6) -0.0044(5) 0.0034(6) 0.0017(5) S2 0.0387(9) 0.0501(5) 0.0458(6) -0.0003(4) 0.0096(6) 0.0005(5) Cl1 0.0940(16) 0.0460(5) 0.0701(8) 0.0035(5) 0.0204(9) -0.0099(6) Cl2 0.0605(11) 0.0446(5) 0.0670(7) -0.0100(5) 0.0152(7) -0.0033(5) Rh1 0.0548(3) 0.04332(16) 0.04270(18) -0.00013(14) 0.01360(18) -0.00119(17) Rh2 0.0403(3) 0.04244(16) 0.0485(2) -0.00441(14) 0.01275(18) -0.00317(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(9) . ? C1 C5 1.427(12) . ? C1 C6 1.530(12) . ? C1 Rh1 2.168(7) . ? C2 C3 1.386(10) . ? C2 C7 1.508(9) . ? C2 Rh1 2.182(6) . ? C3 C4 1.419(7) . ? C3 C8 1.532(8) . ? C3 Rh1 2.147(4) . ? C4 C5 1.368(10) . ? C4 C9 1.512(11) . ? C4 Rh1 2.184(4) . ? C5 C10 1.519(8) . ? C5 Rh1 2.166(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C15 1.414(8) . ? C11 C16 1.462(9) . ? C11 C12 1.470(7) . ? C11 Rh2 2.184(6) . ? C12 C13 1.381(8) . ? C12 C17 1.525(7) . ? C12 Rh2 2.150(5) . ? C13 C14 1.448(6) . ? C13 C18 1.496(8) . ? C13 Rh2 2.169(4) . ? C14 C15 1.423(8) . ? C14 C19 1.502(8) . ? C14 Rh2 2.170(4) . ? C15 C20 1.499(6) . ? C15 Rh2 2.206(5) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.436(7) . ? C21 S1 1.835(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.546(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C28 1.328(10) . ? C23 C24 1.401(11) . ? C24 C25 1.387(10) . ? C24 H24 0.9300 . ? C25 C26 1.339(13) . ? C25 H25 0.9300 . ? C26 C27 1.357(14) . ? C26 H26 0.9300 . ? C27 C28 1.393(11) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.511(8) . ? C29 S2 1.806(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.499(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.359(8) . ? C31 C36 1.382(7) . ? C32 C33 1.390(8) . ? C32 H32 0.9300 . ? C33 C34 1.350(9) . ? C33 H33 0.9300 . ? C34 C35 1.360(10) . ? C34 H34 0.9300 . ? C35 C36 1.377(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? S1 Rh2 2.3807(13) . ? S1 Rh1 2.3903(17) . ? S2 Rh1 2.3676(13) . ? S2 Rh2 2.3682(15) . ? Cl1 Rh1 2.3869(11) . ? Cl2 Rh2 2.3778(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.6(7) . . ? C2 C1 C6 127.9(11) . . ? C5 C1 C6 124.3(9) . . ? C2 C1 Rh1 72.1(4) . . ? C5 C1 Rh1 70.7(4) . . ? C6 C1 Rh1 127.1(5) . . ? C1 C2 C3 108.0(6) . . ? C1 C2 C7 128.2(10) . . ? C3 C2 C7 123.8(8) . . ? C1 C2 Rh1 70.9(4) . . ? C3 C2 Rh1 69.9(4) . . ? C7 C2 Rh1 125.6(4) . . ? C2 C3 C4 108.8(5) . . ? C2 C3 C8 126.4(7) . . ? C4 C3 C8 124.6(8) . . ? C2 C3 Rh1 72.7(3) . . ? C4 C3 Rh1 72.3(2) . . ? C8 C3 Rh1 125.0(4) . . ? C5 C4 C3 107.0(7) . . ? C5 C4 C9 127.8(7) . . ? C3 C4 C9 125.2(7) . . ? C5 C4 Rh1 70.9(3) . . ? C3 C4 Rh1 69.5(3) . . ? C9 C4 Rh1 125.5(5) . . ? C4 C5 C1 108.6(5) . . ? C4 C5 C10 126.0(9) . . ? C1 C5 C10 125.3(9) . . ? C4 C5 Rh1 72.4(3) . . ? C1 C5 Rh1 70.9(3) . . ? C10 C5 Rh1 125.7(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 . . ? C15 C11 C16 125.9(5) . . ? C15 C11 C12 106.4(6) . . ? C16 C11 C12 127.6(6) . . ? C15 C11 Rh2 72.1(3) . . ? C16 C11 Rh2 127.1(4) . . ? C12 C11 Rh2 68.9(3) . . ? C13 C12 C11 108.7(5) . . ? C13 C12 C17 127.5(5) . . ? C11 C12 C17 123.5(6) . . ? C13 C12 Rh2 72.1(3) . . ? C11 C12 Rh2 71.4(3) . . ? C17 C12 Rh2 127.5(4) . . ? C12 C13 C14 108.4(5) . . ? C12 C13 C18 126.9(5) . . ? C14 C13 C18 124.6(6) . . ? C12 C13 Rh2 70.6(3) . . ? C14 C13 Rh2 70.6(2) . . ? C18 C13 Rh2 127.6(4) . . ? C15 C14 C13 107.4(5) . . ? C15 C14 C19 127.5(5) . . ? C13 C14 C19 125.0(6) . . ? C15 C14 Rh2 72.4(3) . . ? C13 C14 Rh2 70.4(3) . . ? C19 C14 Rh2 124.7(4) . . ? C11 C15 C14 109.0(4) . . ? C11 C15 C20 124.8(6) . . ? C14 C15 C20 126.2(5) . . ? C11 C15 Rh2 70.4(3) . . ? C14 C15 Rh2 69.7(3) . . ? C20 C15 Rh2 127.3(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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 . . ? C22 C21 S1 111.8(4) . . ? C22 C21 H21A 109.2 . . ? S1 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? S1 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C21 C22 C23 113.2(5) . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? C28 C23 C24 117.9(7) . . ? C28 C23 C22 119.3(9) . . ? C24 C23 C22 122.8(6) . . ? C25 C24 C23 120.7(8) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C26 C25 C24 118.9(10) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 121.4(8) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C28 119.0(9) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C23 C28 C27 121.8(11) . . ? C23 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C30 C29 S2 112.2(3) . . ? C30 C29 H29A 109.2 . . ? S2 C29 H29A 109.2 . . ? C30 C29 H29B 109.2 . . ? S2 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C31 C30 C29 110.6(5) . . ? C31 C30 H30A 109.5 . . ? C29 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C36 117.9(5) . . ? C32 C31 C30 121.7(5) . . ? C36 C31 C30 120.3(5) . . ? C31 C32 C33 121.5(6) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 120.0(7) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.3(6) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 121.1(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C31 120.1(6) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C21 S1 Rh2 108.64(17) . . ? C21 S1 Rh1 110.7(2) . . ? Rh2 S1 Rh1 99.22(6) . . ? C29 S2 Rh1 110.69(16) . . ? C29 S2 Rh2 108.31(19) . . ? Rh1 S2 Rh2 100.22(6) . . ? C3 Rh1 C5 62.57(18) . . ? C3 Rh1 C1 62.5(2) . . ? C5 Rh1 C1 38.5(3) . . ? C3 Rh1 C2 37.3(2) . . ? C5 Rh1 C2 62.8(3) . . ? C1 Rh1 C2 37.0(3) . . ? C3 Rh1 C4 38.2(2) . . ? C5 Rh1 C4 36.7(3) . . ? C1 Rh1 C4 62.9(3) . . ? C2 Rh1 C4 63.0(2) . . ? C3 Rh1 S2 105.44(15) . . ? C5 Rh1 S2 155.1(3) . . ? C1 Rh1 S2 117.1(3) . . ? C2 Rh1 S2 94.13(16) . . ? C4 Rh1 S2 142.18(15) . . ? C3 Rh1 Cl1 155.23(14) . . ? C5 Rh1 Cl1 93.12(14) . . ? C1 Rh1 Cl1 95.94(18) . . ? C2 Rh1 Cl1 128.9(2) . . ? C4 Rh1 Cl1 122.81(15) . . ? S2 Rh1 Cl1 95.01(4) . . ? C3 Rh1 S1 101.8(2) . . ? C5 Rh1 S1 122.5(3) . . ? C1 Rh1 S1 158.4(2) . . ? C2 Rh1 S1 135.8(2) . . ? C4 Rh1 S1 95.6(2) . . ? S2 Rh1 S1 80.13(5) . . ? Cl1 Rh1 S1 95.25(5) . . ? C12 Rh2 C13 37.3(2) . . ? C12 Rh2 C14 64.2(2) . . ? C13 Rh2 C14 39.00(17) . . ? C12 Rh2 C11 39.6(2) . . ? C13 Rh2 C11 64.3(2) . . ? C14 Rh2 C11 64.1(2) . . ? C12 Rh2 C15 64.03(18) . . ? C13 Rh2 C15 63.85(18) . . ? C14 Rh2 C15 37.9(2) . . ? C11 Rh2 C15 37.6(2) . . ? C12 Rh2 S2 119.17(16) . . ? C13 Rh2 S2 92.77(18) . . ? C14 Rh2 S2 100.66(18) . . ? C11 Rh2 S2 156.89(14) . . ? C15 Rh2 S2 136.19(17) . . ? C12 Rh2 Cl2 145.54(16) . . ? C13 Rh2 Cl2 147.76(13) . . ? C14 Rh2 Cl2 108.76(12) . . ? C11 Rh2 Cl2 106.02(13) . . ? C15 Rh2 Cl2 89.51(11) . . ? S2 Rh2 Cl2 95.12(5) . . ? C12 Rh2 S1 95.95(14) . . ? C13 Rh2 S1 119.23(13) . . ? C14 Rh2 S1 158.02(12) . . ? C11 Rh2 S1 107.27(16) . . ? C15 Rh2 S1 143.04(17) . . ? S2 Rh2 S1 80.32(5) . . ? Cl2 Rh2 S1 92.93(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -1.7(7) . . . . ? C6 C1 C2 C3 -176.2(6) . . . . ? Rh1 C1 C2 C3 60.4(4) . . . . ? C5 C1 C2 C7 177.1(6) . . . . ? C6 C1 C2 C7 2.7(11) . . . . ? Rh1 C1 C2 C7 -120.7(6) . . . . ? C5 C1 C2 Rh1 -62.1(4) . . . . ? C6 C1 C2 Rh1 123.4(7) . . . . ? C1 C2 C3 C4 2.7(6) . . . . ? C7 C2 C3 C4 -176.2(5) . . . . ? Rh1 C2 C3 C4 63.8(3) . . . . ? C1 C2 C3 C8 177.8(5) . . . . ? C7 C2 C3 C8 -1.1(9) . . . . ? Rh1 C2 C3 C8 -121.1(5) . . . . ? C1 C2 C3 Rh1 -61.1(4) . . . . ? C7 C2 C3 Rh1 120.0(6) . . . . ? C2 C3 C4 C5 -2.6(6) . . . . ? C8 C3 C4 C5 -177.9(5) . . . . ? Rh1 C3 C4 C5 61.4(4) . . . . ? C2 C3 C4 C9 176.3(6) . . . . ? C8 C3 C4 C9 1.1(8) . . . . ? Rh1 C3 C4 C9 -119.7(6) . . . . ? C2 C3 C4 Rh1 -64.0(4) . . . . ? C8 C3 C4 Rh1 120.7(5) . . . . ? C3 C4 C5 C1 1.6(6) . . . . ? C9 C4 C5 C1 -177.4(6) . . . . ? Rh1 C4 C5 C1 62.0(4) . . . . ? C3 C4 C5 C10 177.8(6) . . . . ? C9 C4 C5 C10 -1.1(10) . . . . ? Rh1 C4 C5 C10 -121.8(7) . . . . ? C3 C4 C5 Rh1 -60.4(4) . . . . ? C9 C4 C5 Rh1 120.6(6) . . . . ? C2 C1 C5 C4 0.1(7) . . . . ? C6 C1 C5 C4 174.8(6) . . . . ? Rh1 C1 C5 C4 -63.0(4) . . . . ? C2 C1 C5 C10 -176.2(6) . . . . ? C6 C1 C5 C10 -1.5(10) . . . . ? Rh1 C1 C5 C10 120.7(6) . . . . ? C2 C1 C5 Rh1 63.0(4) . . . . ? C6 C1 C5 Rh1 -122.3(7) . . . . ? C15 C11 C12 C13 0.1(6) . . . . ? C16 C11 C12 C13 -175.9(6) . . . . ? Rh2 C11 C12 C13 62.8(4) . . . . ? C15 C11 C12 C17 174.0(4) . . . . ? C16 C11 C12 C17 -2.0(9) . . . . ? Rh2 C11 C12 C17 -123.2(5) . . . . ? C15 C11 C12 Rh2 -62.8(3) . . . . ? C16 C11 C12 Rh2 121.3(6) . . . . ? C11 C12 C13 C14 -1.7(6) . . . . ? C17 C12 C13 C14 -175.3(5) . . . . ? Rh2 C12 C13 C14 60.8(3) . . . . ? C11 C12 C13 C18 174.5(5) . . . . ? C17 C12 C13 C18 0.9(9) . . . . ? Rh2 C12 C13 C18 -123.0(5) . . . . ? C11 C12 C13 Rh2 -62.4(3) . . . . ? C17 C12 C13 Rh2 124.0(5) . . . . ? C12 C13 C14 C15 2.6(5) . . . . ? C18 C13 C14 C15 -173.7(5) . . . . ? Rh2 C13 C14 C15 63.4(3) . . . . ? C12 C13 C14 C19 180.0(5) . . . . ? C18 C13 C14 C19 3.6(8) . . . . ? Rh2 C13 C14 C19 -119.2(5) . . . . ? C12 C13 C14 Rh2 -60.8(3) . . . . ? C18 C13 C14 Rh2 122.9(5) . . . . ? C16 C11 C15 C14 177.6(5) . . . . ? C12 C11 C15 C14 1.6(5) . . . . ? Rh2 C11 C15 C14 -59.1(4) . . . . ? C16 C11 C15 C20 -0.8(9) . . . . ? C12 C11 C15 C20 -176.9(5) . . . . ? Rh2 C11 C15 C20 122.4(5) . . . . ? C16 C11 C15 Rh2 -123.2(6) . . . . ? C12 C11 C15 Rh2 60.7(3) . . . . ? C13 C14 C15 C11 -2.6(5) . . . . ? C19 C14 C15 C11 -179.8(5) . . . . ? Rh2 C14 C15 C11 59.6(3) . . . . ? C13 C14 C15 C20 175.8(5) . . . . ? C19 C14 C15 C20 -1.4(8) . . . . ? Rh2 C14 C15 C20 -122.0(5) . . . . ? C13 C14 C15 Rh2 -62.1(3) . . . . ? C19 C14 C15 Rh2 120.6(5) . . . . ? S1 C21 C22 C23 173.6(5) . . . . ? C21 C22 C23 C28 111.8(7) . . . . ? C21 C22 C23 C24 -69.7(8) . . . . ? C28 C23 C24 C25 4.4(11) . . . . ? C22 C23 C24 C25 -174.1(6) . . . . ? C23 C24 C25 C26 -4.3(11) . . . . ? C24 C25 C26 C27 2.5(13) . . . . ? C25 C26 C27 C28 -0.8(15) . . . . ? C24 C23 C28 C27 -2.6(11) . . . . ? C22 C23 C28 C27 175.9(7) . . . . ? C26 C27 C28 C23 0.9(13) . . . . ? S2 C29 C30 C31 177.4(4) . . . . ? C29 C30 C31 C32 99.4(7) . . . . ? C29 C30 C31 C36 -76.5(7) . . . . ? C36 C31 C32 C33 -0.6(11) . . . . ? C30 C31 C32 C33 -176.6(7) . . . . ? C31 C32 C33 C34 0.9(12) . . . . ? C32 C33 C34 C35 -1.6(13) . . . . ? C33 C34 C35 C36 2.0(14) . . . . ? C34 C35 C36 C31 -1.8(13) . . . . ? C32 C31 C36 C35 1.1(11) . . . . ? C30 C31 C36 C35 177.1(8) . . . . ? C22 C21 S1 Rh2 -177.4(4) . . . . ? C22 C21 S1 Rh1 74.6(5) . . . . ? C30 C29 S2 Rh1 -70.5(4) . . . . ? C30 C29 S2 Rh2 -179.5(3) . . . . ? C2 C3 Rh1 C5 80.3(5) . . . . ? C4 C3 Rh1 C5 -36.7(5) . . . . ? C8 C3 Rh1 C5 -157.0(9) . . . . ? C2 C3 Rh1 C1 36.7(4) . . . . ? C4 C3 Rh1 C1 -80.3(5) . . . . ? C8 C3 Rh1 C1 159.4(9) . . . . ? C4 C3 Rh1 C2 -117.0(5) . . . . ? C8 C3 Rh1 C2 122.7(9) . . . . ? C2 C3 Rh1 C4 117.0(5) . . . . ? C8 C3 Rh1 C4 -120.3(10) . . . . ? C2 C3 Rh1 S2 -76.2(3) . . . . ? C4 C3 Rh1 S2 166.8(4) . . . . ? C8 C3 Rh1 S2 46.5(8) . . . . ? C2 C3 Rh1 Cl1 68.4(7) . . . . ? C4 C3 Rh1 Cl1 -48.6(8) . . . . ? C8 C3 Rh1 Cl1 -168.9(5) . . . . ? C2 C3 Rh1 S1 -159.1(3) . . . . ? C4 C3 Rh1 S1 84.0(4) . . . . ? C8 C3 Rh1 S1 -36.3(8) . . . . ? C4 C5 Rh1 C3 38.3(4) . . . . ? C1 C5 Rh1 C3 -79.4(4) . . . . ? C10 C5 Rh1 C3 160.3(11) . . . . ? C4 C5 Rh1 C1 117.7(5) . . . . ? C10 C5 Rh1 C1 -120.2(11) . . . . ? C4 C5 Rh1 C2 80.5(4) . . . . ? C1 C5 Rh1 C2 -37.2(4) . . . . ? C10 C5 Rh1 C2 -157.4(11) . . . . ? C1 C5 Rh1 C4 -117.7(5) . . . . ? C10 C5 Rh1 C4 122.1(12) . . . . ? C4 C5 Rh1 S2 104.3(7) . . . . ? C1 C5 Rh1 S2 -13.4(7) . . . . ? C10 C5 Rh1 S2 -133.6(8) . . . . ? C4 C5 Rh1 Cl1 -146.7(4) . . . . ? C1 C5 Rh1 Cl1 95.6(4) . . . . ? C10 C5 Rh1 Cl1 -24.6(10) . . . . ? C4 C5 Rh1 S1 -48.5(5) . . . . ? C1 C5 Rh1 S1 -166.1(3) . . . . ? C10 C5 Rh1 S1 73.6(10) . . . . ? C2 C1 Rh1 C3 -37.0(4) . . . . ? C5 C1 Rh1 C3 79.7(4) . . . . ? C6 C1 Rh1 C3 -161.4(11) . . . . ? C2 C1 Rh1 C5 -116.7(6) . . . . ? C6 C1 Rh1 C5 118.9(12) . . . . ? C5 C1 Rh1 C2 116.7(6) . . . . ? C6 C1 Rh1 C2 -124.4(13) . . . . ? C2 C1 Rh1 C4 -80.3(4) . . . . ? C5 C1 Rh1 C4 36.4(3) . . . . ? C6 C1 Rh1 C4 155.4(11) . . . . ? C2 C1 Rh1 S2 57.0(5) . . . . ? C5 C1 Rh1 S2 173.7(3) . . . . ? C6 C1 Rh1 S2 -67.3(10) . . . . ? C2 C1 Rh1 Cl1 155.7(4) . . . . ? C5 C1 Rh1 Cl1 -87.5(3) . . . . ? C6 C1 Rh1 Cl1 31.4(10) . . . . ? C2 C1 Rh1 S1 -83.4(9) . . . . ? C5 C1 Rh1 S1 33.3(8) . . . . ? C6 C1 Rh1 S1 152.3(8) . . . . ? C1 C2 Rh1 C3 118.3(6) . . . . ? C7 C2 Rh1 C3 -117.9(11) . . . . ? C1 C2 Rh1 C5 38.6(4) . . . . ? C3 C2 Rh1 C5 -79.6(4) . . . . ? C7 C2 Rh1 C5 162.5(10) . . . . ? C3 C2 Rh1 C1 -118.3(6) . . . . ? C7 C2 Rh1 C1 123.8(11) . . . . ? C1 C2 Rh1 C4 80.0(5) . . . . ? C3 C2 Rh1 C4 -38.2(3) . . . . ? C7 C2 Rh1 C4 -156.1(10) . . . . ? C1 C2 Rh1 S2 -131.5(5) . . . . ? C3 C2 Rh1 S2 110.2(3) . . . . ? C7 C2 Rh1 S2 -7.7(9) . . . . ? C1 C2 Rh1 Cl1 -31.7(5) . . . . ? C3 C2 Rh1 Cl1 -149.9(3) . . . . ? C7 C2 Rh1 Cl1 92.2(9) . . . . ? C1 C2 Rh1 S1 148.4(4) . . . . ? C3 C2 Rh1 S1 30.1(4) . . . . ? C7 C2 Rh1 S1 -87.8(9) . . . . ? C5 C4 Rh1 C3 -117.3(7) . . . . ? C9 C4 Rh1 C3 119.3(9) . . . . ? C3 C4 Rh1 C5 117.3(7) . . . . ? C9 C4 Rh1 C5 -123.4(8) . . . . ? C5 C4 Rh1 C1 -38.2(4) . . . . ? C3 C4 Rh1 C1 79.1(5) . . . . ? C9 C4 Rh1 C1 -161.6(7) . . . . ? C5 C4 Rh1 C2 -80.0(5) . . . . ? C3 C4 Rh1 C2 37.4(4) . . . . ? C9 C4 Rh1 C2 156.6(8) . . . . ? C5 C4 Rh1 S2 -138.3(4) . . . . ? C3 C4 Rh1 S2 -21.0(6) . . . . ? C9 C4 Rh1 S2 98.3(6) . . . . ? C5 C4 Rh1 Cl1 40.7(5) . . . . ? C3 C4 Rh1 Cl1 158.1(4) . . . . ? C9 C4 Rh1 Cl1 -82.7(7) . . . . ? C5 C4 Rh1 S1 140.6(5) . . . . ? C3 C4 Rh1 S1 -102.0(4) . . . . ? C9 C4 Rh1 S1 17.2(7) . . . . ? C29 S2 Rh1 C3 143.6(3) . . . . ? Rh2 S2 Rh1 C3 -102.2(2) . . . . ? C29 S2 Rh1 C5 86.3(5) . . . . ? Rh2 S2 Rh1 C5 -159.6(4) . . . . ? C29 S2 Rh1 C1 77.0(3) . . . . ? Rh2 S2 Rh1 C1 -168.85(19) . . . . ? C29 S2 Rh1 C2 107.4(3) . . . . ? Rh2 S2 Rh1 C2 -138.4(2) . . . . ? C29 S2 Rh1 C4 156.9(4) . . . . ? Rh2 S2 Rh1 C4 -89.0(3) . . . . ? C29 S2 Rh1 Cl1 -22.3(2) . . . . ? Rh2 S2 Rh1 Cl1 91.86(5) . . . . ? C29 S2 Rh1 S1 -116.8(2) . . . . ? Rh2 S2 Rh1 S1 -2.61(3) . . . . ? C21 S1 Rh1 C3 -139.5(2) . . . . ? Rh2 S1 Rh1 C3 106.47(16) . . . . ? C21 S1 Rh1 C5 -74.6(2) . . . . ? Rh2 S1 Rh1 C5 171.32(16) . . . . ? C21 S1 Rh1 C1 -98.5(6) . . . . ? Rh2 S1 Rh1 C1 147.4(6) . . . . ? C21 S1 Rh1 C2 -157.6(3) . . . . ? Rh2 S1 Rh1 C2 88.3(2) . . . . ? C21 S1 Rh1 C4 -101.3(2) . . . . ? Rh2 S1 Rh1 C4 144.65(14) . . . . ? C21 S1 Rh1 S2 116.62(17) . . . . ? Rh2 S1 Rh1 S2 2.59(3) . . . . ? C21 S1 Rh1 Cl1 22.43(17) . . . . ? Rh2 S1 Rh1 Cl1 -91.60(4) . . . . ? C11 C12 Rh2 C13 117.7(4) . . . . ? C17 C12 Rh2 C13 -123.9(7) . . . . ? C13 C12 Rh2 C14 -37.9(3) . . . . ? C11 C12 Rh2 C14 79.8(3) . . . . ? C17 C12 Rh2 C14 -161.8(6) . . . . ? C13 C12 Rh2 C11 -117.7(4) . . . . ? C17 C12 Rh2 C11 118.4(7) . . . . ? C13 C12 Rh2 C15 -80.2(3) . . . . ? C11 C12 Rh2 C15 37.4(3) . . . . ? C17 C12 Rh2 C15 155.9(6) . . . . ? C13 C12 Rh2 S2 50.1(3) . . . . ? C11 C12 Rh2 S2 167.8(3) . . . . ? C17 C12 Rh2 S2 -73.8(6) . . . . ? C13 C12 Rh2 Cl2 -123.6(3) . . . . ? C11 C12 Rh2 Cl2 -6.0(5) . . . . ? C17 C12 Rh2 Cl2 112.5(5) . . . . ? C13 C12 Rh2 S1 132.3(3) . . . . ? C11 C12 Rh2 S1 -110.0(3) . . . . ? C17 C12 Rh2 S1 8.4(6) . . . . ? C14 C13 Rh2 C12 -118.6(5) . . . . ? C18 C13 Rh2 C12 122.2(6) . . . . ? C12 C13 Rh2 C14 118.6(5) . . . . ? C18 C13 Rh2 C14 -119.2(7) . . . . ? C12 C13 Rh2 C11 38.8(3) . . . . ? C14 C13 Rh2 C11 -79.8(4) . . . . ? C18 C13 Rh2 C11 161.0(6) . . . . ? C12 C13 Rh2 C15 80.8(4) . . . . ? C14 C13 Rh2 C15 -37.8(4) . . . . ? C18 C13 Rh2 C15 -157.0(6) . . . . ? C12 C13 Rh2 S2 -137.9(3) . . . . ? C14 C13 Rh2 S2 103.6(3) . . . . ? C18 C13 Rh2 S2 -15.6(5) . . . . ? C12 C13 Rh2 Cl2 118.0(3) . . . . ? C14 C13 Rh2 Cl2 -0.6(6) . . . . ? C18 C13 Rh2 Cl2 -119.8(4) . . . . ? C12 C13 Rh2 S1 -57.4(3) . . . . ? C14 C13 Rh2 S1 -176.0(3) . . . . ? C18 C13 Rh2 S1 64.8(6) . . . . ? C15 C14 Rh2 C12 -80.2(3) . . . . ? C13 C14 Rh2 C12 36.3(3) . . . . ? C19 C14 Rh2 C12 155.9(5) . . . . ? C15 C14 Rh2 C13 -116.5(5) . . . . ? C19 C14 Rh2 C13 119.7(7) . . . . ? C15 C14 Rh2 C11 -35.9(3) . . . . ? C13 C14 Rh2 C11 80.5(4) . . . . ? C19 C14 Rh2 C11 -159.8(5) . . . . ? C13 C14 Rh2 C15 116.5(5) . . . . ? C19 C14 Rh2 C15 -123.9(5) . . . . ? C15 C14 Rh2 S2 162.4(3) . . . . ? C13 C14 Rh2 S2 -81.1(4) . . . . ? C19 C14 Rh2 S2 38.5(5) . . . . ? C15 C14 Rh2 Cl2 63.2(3) . . . . ? C13 C14 Rh2 Cl2 179.7(3) . . . . ? C19 C14 Rh2 Cl2 -60.7(5) . . . . ? C15 C14 Rh2 S1 -107.1(4) . . . . ? C13 C14 Rh2 S1 9.4(7) . . . . ? C19 C14 Rh2 S1 129.0(4) . . . . ? C15 C11 Rh2 C12 116.3(5) . . . . ? C16 C11 Rh2 C12 -121.9(7) . . . . ? C15 C11 Rh2 C13 79.8(3) . . . . ? C16 C11 Rh2 C13 -158.4(6) . . . . ? C12 C11 Rh2 C13 -36.5(3) . . . . ? C15 C11 Rh2 C14 36.3(3) . . . . ? C16 C11 Rh2 C14 158.1(6) . . . . ? C12 C11 Rh2 C14 -80.1(3) . . . . ? C16 C11 Rh2 C15 121.8(6) . . . . ? C12 C11 Rh2 C15 -116.3(5) . . . . ? C15 C11 Rh2 S2 88.2(4) . . . . ? C16 C11 Rh2 S2 -149.9(4) . . . . ? C12 C11 Rh2 S2 -28.1(6) . . . . ? C15 C11 Rh2 Cl2 -67.2(3) . . . . ? C16 C11 Rh2 Cl2 54.6(5) . . . . ? C12 C11 Rh2 Cl2 176.5(3) . . . . ? C15 C11 Rh2 S1 -165.5(3) . . . . ? C16 C11 Rh2 S1 -43.7(5) . . . . ? C12 C11 Rh2 S1 78.2(3) . . . . ? C11 C15 Rh2 C12 -39.5(3) . . . . ? C14 C15 Rh2 C12 80.6(3) . . . . ? C20 C15 Rh2 C12 -158.8(6) . . . . ? C11 C15 Rh2 C13 -81.2(3) . . . . ? C14 C15 Rh2 C13 38.9(3) . . . . ? C20 C15 Rh2 C13 159.5(6) . . . . ? C11 C15 Rh2 C14 -120.1(4) . . . . ? C20 C15 Rh2 C14 120.6(7) . . . . ? C14 C15 Rh2 C11 120.1(4) . . . . ? C20 C15 Rh2 C11 -119.3(7) . . . . ? C11 C15 Rh2 S2 -145.5(3) . . . . ? C14 C15 Rh2 S2 -25.4(3) . . . . ? C20 C15 Rh2 S2 95.2(5) . . . . ? C11 C15 Rh2 Cl2 117.6(3) . . . . ? C14 C15 Rh2 Cl2 -122.3(3) . . . . ? C20 C15 Rh2 Cl2 -1.7(5) . . . . ? C11 C15 Rh2 S1 23.4(4) . . . . ? C14 C15 Rh2 S1 143.5(3) . . . . ? C20 C15 Rh2 S1 -95.9(5) . . . . ? C29 S2 Rh2 C12 -150.0(2) . . . . ? Rh1 S2 Rh2 C12 94.07(17) . . . . ? C29 S2 Rh2 C13 -122.2(2) . . . . ? Rh1 S2 Rh2 C13 121.81(14) . . . . ? C29 S2 Rh2 C14 -83.7(2) . . . . ? Rh1 S2 Rh2 C14 160.31(12) . . . . ? C29 S2 Rh2 C11 -129.9(4) . . . . ? Rh1 S2 Rh2 C11 114.2(4) . . . . ? C29 S2 Rh2 C15 -68.2(2) . . . . ? Rh1 S2 Rh2 C15 175.87(15) . . . . ? C29 S2 Rh2 Cl2 26.49(17) . . . . ? Rh1 S2 Rh2 Cl2 -89.48(4) . . . . ? C29 S2 Rh2 S1 118.59(17) . . . . ? Rh1 S2 Rh2 S1 2.62(3) . . . . ? C21 S1 Rh2 C12 123.2(3) . . . . ? Rh1 S1 Rh2 C12 -121.23(17) . . . . ? C21 S1 Rh2 C13 154.1(3) . . . . ? Rh1 S1 Rh2 C13 -90.3(2) . . . . ? C21 S1 Rh2 C14 147.3(5) . . . . ? Rh1 S1 Rh2 C14 -97.1(5) . . . . ? C21 S1 Rh2 C11 84.3(3) . . . . ? Rh1 S1 Rh2 C11 -160.12(14) . . . . ? C21 S1 Rh2 C15 69.6(3) . . . . ? Rh1 S1 Rh2 C15 -174.81(18) . . . . ? C21 S1 Rh2 S2 -118.2(2) . . . . ? Rh1 S1 Rh2 S2 -2.59(3) . . . . ? C21 S1 Rh2 Cl2 -23.5(2) . . . . ? Rh1 S1 Rh2 Cl2 92.11(5) . . . . ? _diffrn_measured_fraction_theta_max 0.881 _diffrn_reflns_theta_full 26.11 _diffrn_measured_fraction_theta_full 0.881 _refine_diff_density_max 0.648 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.075 _database_code_depnum_ccdc_archive 'CCDC 939467' ####################################################################### # # 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_d:complex6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H57 Ir2 S3, Cl, H Cl' _chemical_formula_sum 'C44 H58 Cl2 Ir2 S3' _chemical_formula_weight 1138.38 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.350(2) _cell_length_b 12.320(2) _cell_length_c 17.097(3) _cell_angle_alpha 88.82(3) _cell_angle_beta 76.00(3) _cell_angle_gamma 71.04(3) _cell_volume 2189.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.85 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 6.366 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.332 _exptl_absorpt_correction_T_max 0.759 _exptl_absorpt_process_details 'Walker, N. & Stuart, D. (1983)' _exptl_special_details ; A crystal was mounted at 173K on a Stoe Image Plate Diffraction System (Stoe & Cie, 2000) using MoK\a graphite monochromated radiation. Image plate distance 70mm, \f oscillation scans 0 - 200\%, step \D\f = 1.2\%, 5 minutes per frame. ; _diffrn_ambient_temperature 173(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 'STOE IPDS' _diffrn_measurement_method 'phi oscillation' _diffrn_detector_area_resol_mean 0.81\%A _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13000 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.13 _reflns_number_total 7921 _reflns_number_gt 5142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE (Stoe & Cie, 2000)' _computing_cell_refinement 'CELL (Stoe & Cie, 2000)' _computing_data_reduction 'INTEGRATE (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-32 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0220P)^2^] 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 7921 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 0.816 _refine_ls_restrained_S_all 0.816 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0926(6) 0.7258(6) 0.1852(4) 0.0537(19) Uani 1 1 d . . . C2 C 0.0575(6) 0.8458(6) 0.1699(4) 0.0499(18) Uani 1 1 d . . . C3 C 0.0326(6) 0.9100(6) 0.2458(4) 0.0521(18) Uani 1 1 d . . . C4 C 0.0536(6) 0.8309(6) 0.3064(4) 0.0501(18) Uani 1 1 d . . . C5 C 0.0925(6) 0.7160(6) 0.2693(4) 0.0500(18) Uani 1 1 d . . . C6 C 0.1211(8) 0.6289(7) 0.1254(4) 0.071(2) Uani 1 1 d . . . H6A H 0.1746 0.6408 0.0754 0.106 Uiso 1 1 calc R . . H6B H 0.0421 0.6254 0.1164 0.106 Uiso 1 1 calc R . . H6C H 0.1650 0.5580 0.1458 0.106 Uiso 1 1 calc R . . C7 C 0.0353(7) 0.8993(8) 0.0923(5) 0.077(3) Uani 1 1 d . . . H7A H 0.0896 0.8469 0.0472 0.116 Uiso 1 1 calc R . . H7B H 0.0552 0.9695 0.0885 0.116 Uiso 1 1 calc R . . H7C H -0.0532 0.9154 0.0917 0.116 Uiso 1 1 calc R . . C8 C -0.0185(8) 1.0386(6) 0.2571(6) 0.084(3) Uani 1 1 d . . . H8A H -0.0079 1.0623 0.3073 0.127 Uiso 1 1 calc R . . H8B H -0.1081 1.0653 0.2577 0.127 Uiso 1 1 calc R . . H8C H 0.0278 1.0706 0.2134 0.127 Uiso 1 1 calc R . . C9 C 0.0334(8) 0.8592(8) 0.3947(4) 0.078(3) Uani 1 1 d . . . H9A H 0.0270 0.9380 0.4027 0.117 Uiso 1 1 calc R . . H9B H 0.1048 0.8101 0.4133 0.117 Uiso 1 1 calc R . . H9C H -0.0445 0.8477 0.4245 0.117 Uiso 1 1 calc R . . C10 C 0.1107(8) 0.6079(6) 0.3127(5) 0.072(2) Uani 1 1 d . . . H10A H 0.1419 0.6153 0.3591 0.108 Uiso 1 1 calc R . . H10B H 0.1720 0.5446 0.2773 0.108 Uiso 1 1 calc R . . H10C H 0.0301 0.5941 0.3298 0.108 Uiso 1 1 calc R . . C11 C 0.7371(5) 0.6920(5) 0.0889(4) 0.0434(16) Uani 1 1 d . . . C12 C 0.6952(6) 0.8081(6) 0.0662(4) 0.0505(19) Uani 1 1 d . . . C13 C 0.6746(7) 0.8811(6) 0.1337(5) 0.063(2) Uani 1 1 d . . . C14 C 0.6970(7) 0.8134(8) 0.1999(4) 0.066(2) Uani 1 1 d . . . C15 C 0.7388(6) 0.6934(7) 0.1711(4) 0.060(2) Uani 1 1 d . . . C16 C 0.7795(8) 0.5868(8) 0.0343(6) 0.100(3) Uani 1 1 d . . . H16A H 0.7870 0.5207 0.0659 0.151 Uiso 1 1 calc R . . H16B H 0.8614 0.5791 -0.0017 0.151 Uiso 1 1 calc R . . H16C H 0.7174 0.5927 0.0036 0.151 Uiso 1 1 calc R . . C17 C 0.6868(7) 0.8466(9) -0.0167(5) 0.101(4) Uani 1 1 d . . . H17A H 0.5992 0.8901 -0.0157 0.152 Uiso 1 1 calc R . . H17B H 0.7159 0.7806 -0.0540 0.152 Uiso 1 1 calc R . . H17C H 0.7399 0.8939 -0.0335 0.152 Uiso 1 1 calc R . . C18 C 0.6403(9) 1.0097(7) 0.1317(8) 0.133(5) Uani 1 1 d . . . H18A H 0.7051 1.0280 0.0914 0.199 Uiso 1 1 calc R . . H18B H 0.6355 1.0416 0.1836 0.199 Uiso 1 1 calc R . . H18C H 0.5586 1.0414 0.1189 0.199 Uiso 1 1 calc R . . C19 C 0.6978(10) 0.8562(12) 0.2819(6) 0.144(6) Uani 1 1 d . . . H19A H 0.7759 0.8727 0.2782 0.215 Uiso 1 1 calc R . . H19B H 0.6925 0.7982 0.3197 0.215 Uiso 1 1 calc R . . H19C H 0.6254 0.9248 0.3000 0.215 Uiso 1 1 calc R . . C20 C 0.7844(8) 0.5906(9) 0.2183(7) 0.132(5) Uani 1 1 d . . . H20A H 0.7562 0.5302 0.2037 0.198 Uiso 1 1 calc R . . H20B H 0.7496 0.6116 0.2751 0.198 Uiso 1 1 calc R . . H20C H 0.8767 0.5644 0.2065 0.198 Uiso 1 1 calc R . . C21 C 0.4041(6) 0.7367(5) 0.0116(3) 0.0452(16) Uani 1 1 d . . . H21A H 0.3138 0.7703 0.0124 0.054 Uiso 1 1 calc R . . H21B H 0.4439 0.7957 -0.0019 0.054 Uiso 1 1 calc R . . C22 C 0.4653(9) 0.6410(6) -0.0502(4) 0.081(3) Uani 1 1 d . . . H22A H 0.4220 0.5844 -0.0372 0.098 Uiso 1 1 calc R . . H22B H 0.5538 0.6047 -0.0475 0.098 Uiso 1 1 calc R . . C23 C 0.4649(7) 0.6725(5) -0.1352(3) 0.0463(17) Uani 1 1 d . . . C24 C 0.5743(8) 0.6757(6) -0.1885(4) 0.065(2) Uani 1 1 d . . . H24 H 0.6496 0.6601 -0.1714 0.078 Uiso 1 1 calc R . . C25 C 0.5752(11) 0.7016(7) -0.2677(5) 0.088(3) Uani 1 1 d . . . H25 H 0.6508 0.7025 -0.3037 0.106 Uiso 1 1 calc R . . C26 C 0.4650(15) 0.7257(8) -0.2925(5) 0.102(4) Uani 1 1 d . . . H26 H 0.4641 0.7463 -0.3450 0.122 Uiso 1 1 calc R . . C27 C 0.3555(11) 0.7197(7) -0.2405(6) 0.094(3) Uani 1 1 d . . . H27 H 0.2808 0.7331 -0.2581 0.113 Uiso 1 1 calc R . . C28 C 0.3565(8) 0.6938(6) -0.1626(5) 0.064(2) Uani 1 1 d . . . H28 H 0.2814 0.6905 -0.1273 0.077 Uiso 1 1 calc R . . C29 C 0.3127(7) 1.0436(5) 0.2477(4) 0.0507(17) Uani 1 1 d . . . H29A H 0.3861 1.0706 0.2362 0.061 Uiso 1 1 calc R . . H29B H 0.2391 1.1079 0.2419 0.061 Uiso 1 1 calc R . . C30 C 0.2892(12) 1.0170(8) 0.3318(5) 0.101(3) Uani 1 1 d . . . H30A H 0.3621 0.9525 0.3381 0.121 Uiso 1 1 calc R . . H30B H 0.2145 0.9918 0.3443 0.121 Uiso 1 1 calc R . . C31 C 0.2674(8) 1.1107(6) 0.3928(4) 0.061(2) Uani 1 1 d . . . C32 C 0.1730(7) 1.2141(8) 0.4039(4) 0.069(2) Uani 1 1 d . . . H32 H 0.1160 1.2311 0.3709 0.083 Uiso 1 1 calc R . . C33 C 0.1595(10) 1.2948(7) 0.4631(5) 0.085(3) Uani 1 1 d . . . H33 H 0.0921 1.3643 0.4712 0.102 Uiso 1 1 calc R . . C34 C 0.2447(13) 1.2720(11) 0.5090(5) 0.101(4) Uani 1 1 d . . . H34 H 0.2391 1.3270 0.5474 0.121 Uiso 1 1 calc R . . C35 C 0.3370(13) 1.1700(13) 0.4989(6) 0.127(5) Uani 1 1 d . . . H35 H 0.3938 1.1530 0.5321 0.153 Uiso 1 1 calc R . . C36 C 0.3495(10) 1.0914(8) 0.4417(5) 0.096(3) Uani 1 1 d . . . H36 H 0.4163 1.0217 0.4353 0.116 Uiso 1 1 calc R . . C37 C 0.4514(6) 0.5896(5) 0.2956(3) 0.0432(16) Uani 1 1 d . . . H37A H 0.3797 0.5619 0.2984 0.052 Uiso 1 1 calc R . . H37B H 0.5208 0.5486 0.2501 0.052 Uiso 1 1 calc R . . C38 C 0.4960(6) 0.5668(6) 0.3734(3) 0.0514(18) Uani 1 1 d . . . H38A H 0.5345 0.4845 0.3762 0.062 Uiso 1 1 calc R . . H38B H 0.5616 0.6016 0.3722 0.062 Uiso 1 1 calc R . . C39 C 0.3885(6) 0.6132(6) 0.4480(4) 0.0456(16) Uani 1 1 d . . . C40 C 0.3648(7) 0.7200(7) 0.4847(4) 0.0606(19) Uani 1 1 d . . . H40 H 0.4155 0.7647 0.4633 0.073 Uiso 1 1 calc R . . C41 C 0.2659(9) 0.7595(8) 0.5531(5) 0.084(3) Uani 1 1 d . . . H41 H 0.2509 0.8313 0.5772 0.101 Uiso 1 1 calc R . . C42 C 0.1890(8) 0.6964(9) 0.5867(5) 0.079(3) Uani 1 1 d . . . H42 H 0.1229 0.7240 0.6331 0.095 Uiso 1 1 calc R . . C43 C 0.2123(8) 0.5924(9) 0.5501(5) 0.080(3) Uani 1 1 d . . . H43 H 0.1609 0.5482 0.5714 0.096 Uiso 1 1 calc R . . C44 C 0.3111(7) 0.5510(7) 0.4816(4) 0.065(2) Uani 1 1 d . . . H44 H 0.3253 0.4791 0.4579 0.078 Uiso 1 1 calc R . . S1 S 0.41931(15) 0.68841(13) 0.11229(8) 0.0357(4) Uani 1 1 d . . . S2 S 0.34283(14) 0.93271(12) 0.16857(8) 0.0359(4) Uani 1 1 d . . . S3 S 0.40172(14) 0.74467(12) 0.28095(8) 0.0359(3) Uani 1 1 d . . . Cl1 Cl -0.0224(2) 1.2690(3) 0.08046(16) 0.1148(10) Uani 1 1 d . . . Cl2 Cl 0.0665(2) 1.3381(2) 0.22165(14) 0.0923(7) Uani 1 1 d . . . H1CL H 0.0593 1.3838 0.2677 0.050 Uiso 1 1 d . . . Ir1 Ir 0.23355(2) 0.798073(19) 0.211509(13) 0.03452(7) Uani 1 1 d . . . Ir2 Ir 0.54157(2) 0.783465(19) 0.162213(13) 0.03450(8) 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 C1 0.043(4) 0.053(4) 0.060(4) -0.006(4) -0.003(3) -0.015(4) C2 0.032(3) 0.066(5) 0.057(4) 0.006(3) -0.019(3) -0.018(3) C3 0.031(3) 0.056(4) 0.061(4) -0.011(4) -0.002(3) -0.008(3) C4 0.031(3) 0.060(5) 0.052(4) -0.014(3) 0.010(3) -0.020(3) C5 0.046(4) 0.061(5) 0.046(4) 0.009(3) -0.006(3) -0.024(4) C6 0.070(5) 0.079(6) 0.070(5) -0.017(4) -0.013(4) -0.036(5) C7 0.061(5) 0.092(6) 0.083(5) 0.021(5) -0.041(4) -0.016(5) C8 0.056(5) 0.053(5) 0.122(7) -0.016(5) -0.008(5) 0.003(4) C9 0.074(5) 0.102(7) 0.050(4) -0.013(4) 0.011(4) -0.037(5) C10 0.068(5) 0.069(5) 0.080(5) 0.021(4) -0.006(4) -0.036(4) C11 0.024(3) 0.038(4) 0.057(4) -0.005(3) 0.003(3) -0.005(3) C12 0.027(3) 0.061(5) 0.055(4) 0.016(4) 0.001(3) -0.012(3) C13 0.040(4) 0.049(4) 0.091(6) -0.003(4) -0.005(4) -0.011(4) C14 0.042(4) 0.110(7) 0.053(4) -0.013(4) -0.012(3) -0.034(5) C15 0.031(3) 0.071(5) 0.074(5) 0.036(4) -0.018(3) -0.010(4) C16 0.053(5) 0.082(6) 0.138(8) -0.041(6) 0.008(5) -0.005(5) C17 0.048(5) 0.159(9) 0.083(6) 0.064(6) -0.005(4) -0.028(5) C18 0.063(6) 0.043(5) 0.277(15) 0.003(7) -0.007(8) -0.022(5) C19 0.078(7) 0.277(17) 0.087(7) -0.071(8) -0.016(5) -0.071(9) C20 0.051(5) 0.150(10) 0.187(10) 0.128(9) -0.046(6) -0.018(6) C21 0.050(4) 0.049(4) 0.033(3) 0.002(3) -0.012(3) -0.010(3) C22 0.143(8) 0.048(4) 0.042(4) -0.002(3) -0.026(4) -0.015(5) C23 0.073(5) 0.033(3) 0.033(3) -0.005(3) -0.015(3) -0.017(3) C24 0.064(5) 0.069(5) 0.060(5) -0.011(4) -0.011(4) -0.022(4) C25 0.115(8) 0.067(6) 0.061(5) -0.015(4) 0.038(5) -0.043(6) C26 0.191(13) 0.067(6) 0.046(5) 0.015(4) -0.030(7) -0.042(8) C27 0.128(9) 0.063(6) 0.096(7) -0.008(5) -0.076(7) -0.004(6) C28 0.061(5) 0.067(5) 0.070(5) -0.011(4) -0.003(4) -0.038(4) C29 0.051(4) 0.032(3) 0.063(4) -0.013(3) 0.000(3) -0.015(3) C30 0.182(11) 0.082(6) 0.062(5) 0.001(4) -0.024(6) -0.080(7) C31 0.087(6) 0.054(4) 0.044(4) -0.004(3) -0.011(4) -0.026(4) C32 0.062(5) 0.092(6) 0.058(4) 0.009(4) -0.017(4) -0.031(5) C33 0.098(7) 0.057(5) 0.074(6) -0.005(5) 0.007(5) -0.010(5) C34 0.155(11) 0.119(9) 0.062(6) -0.017(6) -0.003(6) -0.108(9) C35 0.128(10) 0.166(12) 0.087(7) -0.019(8) -0.052(7) -0.028(9) C36 0.116(8) 0.082(7) 0.068(5) -0.013(5) -0.022(5) 0.000(6) C37 0.052(4) 0.030(3) 0.046(3) 0.004(3) -0.012(3) -0.012(3) C38 0.046(4) 0.055(4) 0.042(3) 0.009(3) -0.012(3) -0.001(3) C39 0.050(4) 0.048(4) 0.046(3) 0.010(3) -0.023(3) -0.019(3) C40 0.075(5) 0.068(5) 0.052(4) 0.003(4) -0.021(4) -0.037(4) C41 0.106(7) 0.083(6) 0.056(5) -0.016(4) -0.023(5) -0.018(6) C42 0.067(5) 0.105(7) 0.051(4) 0.000(5) -0.012(4) -0.013(6) C43 0.073(6) 0.095(7) 0.071(5) 0.014(5) -0.011(5) -0.033(5) C44 0.076(5) 0.063(5) 0.059(4) 0.006(4) -0.019(4) -0.028(4) S1 0.0402(8) 0.0339(8) 0.0317(7) -0.0002(6) -0.0075(6) -0.0113(7) S2 0.0384(8) 0.0304(8) 0.0371(7) 0.0049(6) -0.0093(6) -0.0089(7) S3 0.0411(8) 0.0352(8) 0.0318(7) 0.0026(6) -0.0103(6) -0.0124(7) Cl1 0.0681(15) 0.161(3) 0.1148(19) -0.0181(18) -0.0271(14) -0.0327(17) Cl2 0.1031(17) 0.0806(15) 0.0958(15) 0.0096(12) -0.0433(14) -0.0206(14) Ir1 0.03510(14) 0.03456(15) 0.03405(13) 0.00028(11) -0.00774(11) -0.01219(12) Ir2 0.03375(14) 0.03317(15) 0.03572(13) 0.00317(11) -0.00820(11) -0.01027(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.437(10) . ? C1 C5 1.440(9) . ? C1 C6 1.488(10) . ? C1 Ir1 2.202(8) . ? C2 C3 1.453(9) . ? C2 C7 1.510(9) . ? C2 Ir1 2.179(6) . ? C3 C4 1.417(9) . ? C3 C8 1.498(10) . ? C3 Ir1 2.189(6) . ? C4 C5 1.448(10) . ? C4 C9 1.501(9) . ? C4 Ir1 2.203(6) . ? C5 C10 1.491(9) . ? C5 Ir1 2.193(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C15 1.410(9) . ? C11 C12 1.431(9) . ? C11 C16 1.486(10) . ? C11 Ir2 2.203(5) . ? C12 C13 1.404(10) . ? C12 C17 1.501(9) . ? C12 Ir2 2.183(6) . ? C13 C14 1.415(10) . ? C13 C18 1.506(11) . ? C13 Ir2 2.183(8) . ? C14 C15 1.454(11) . ? C14 C19 1.512(11) . ? C14 Ir2 2.155(7) . ? C15 C20 1.504(9) . ? C15 Ir2 2.193(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.468(8) . ? C21 S1 1.839(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.496(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.363(10) . ? C23 C28 1.367(10) . ? C24 C25 1.383(11) . ? C24 H24 0.9300 . ? C25 C26 1.358(14) . ? C25 H25 0.9300 . ? C26 C27 1.364(15) . ? C26 H26 0.9300 . ? C27 C28 1.365(11) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.448(9) . ? C29 S2 1.834(6) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.491(10) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.353(10) . ? C31 C36 1.360(11) . ? C32 C33 1.379(12) . ? C32 H32 0.9300 . ? C33 C34 1.346(13) . ? C33 H33 0.9300 . ? C34 C35 1.332(14) . ? C34 H34 0.9300 . ? C35 C36 1.340(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.524(8) . ? C37 S3 1.839(6) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.505(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C44 1.365(10) . ? C39 C40 1.387(9) . ? C40 C41 1.377(11) . ? C40 H40 0.9300 . ? C41 C42 1.370(12) . ? C41 H41 0.9300 . ? C42 C43 1.356(12) . ? C42 H42 0.9300 . ? C43 C44 1.380(10) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? S1 Ir1 2.3793(18) . ? S1 Ir2 2.3866(18) . ? S2 Ir1 2.3822(17) . ? S2 Ir2 2.3823(17) . ? S3 Ir1 2.3945(15) . ? S3 Ir2 2.4007(16) . ? Cl2 H1CL 0.9486 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.8(6) . . ? C2 C1 C6 126.2(6) . . ? C5 C1 C6 126.0(7) . . ? C2 C1 Ir1 70.0(4) . . ? C5 C1 Ir1 70.5(4) . . ? C6 C1 Ir1 125.9(5) . . ? C1 C2 C3 107.7(6) . . ? C1 C2 C7 127.3(7) . . ? C3 C2 C7 124.7(7) . . ? C1 C2 Ir1 71.7(4) . . ? C3 C2 Ir1 70.9(4) . . ? C7 C2 Ir1 127.9(5) . . ? C4 C3 C2 108.4(6) . . ? C4 C3 C8 127.2(7) . . ? C2 C3 C8 124.2(7) . . ? C4 C3 Ir1 71.7(3) . . ? C2 C3 Ir1 70.2(3) . . ? C8 C3 Ir1 128.1(5) . . ? C3 C4 C5 108.0(6) . . ? C3 C4 C9 126.8(7) . . ? C5 C4 C9 125.2(6) . . ? C3 C4 Ir1 70.6(3) . . ? C5 C4 Ir1 70.4(3) . . ? C9 C4 Ir1 126.9(5) . . ? C1 C5 C4 108.1(6) . . ? C1 C5 C10 125.7(7) . . ? C4 C5 C10 125.7(6) . . ? C1 C5 Ir1 71.2(4) . . ? C4 C5 Ir1 71.2(4) . . ? C10 C5 Ir1 129.8(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 . . ? C15 C11 C12 108.7(6) . . ? C15 C11 C16 125.2(7) . . ? C12 C11 C16 126.1(7) . . ? C15 C11 Ir2 70.9(3) . . ? C12 C11 Ir2 70.2(3) . . ? C16 C11 Ir2 127.5(5) . . ? C13 C12 C11 107.9(6) . . ? C13 C12 C17 125.2(7) . . ? C11 C12 C17 126.7(7) . . ? C13 C12 Ir2 71.2(4) . . ? C11 C12 Ir2 71.7(3) . . ? C17 C12 Ir2 127.2(5) . . ? C12 C13 C14 108.9(6) . . ? C12 C13 C18 123.7(8) . . ? C14 C13 C18 127.4(9) . . ? C12 C13 Ir2 71.2(4) . . ? C14 C13 Ir2 69.9(4) . . ? C18 C13 Ir2 127.0(5) . . ? C13 C14 C15 107.5(6) . . ? C13 C14 C19 126.3(10) . . ? C15 C14 C19 125.5(9) . . ? C13 C14 Ir2 72.0(4) . . ? C15 C14 Ir2 71.9(4) . . ? C19 C14 Ir2 128.6(6) . . ? C11 C15 C14 107.0(5) . . ? C11 C15 C20 126.5(8) . . ? C14 C15 C20 126.3(8) . . ? C11 C15 Ir2 71.7(3) . . ? C14 C15 Ir2 69.1(4) . . ? C20 C15 Ir2 127.6(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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 . . ? C22 C21 S1 111.3(4) . . ? C22 C21 H21A 109.4 . . ? S1 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? S1 C21 H21B 109.4 . . ? H21A C21 H21B 108.0 . . ? C21 C22 C23 115.6(5) . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? C21 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.4 . . ? C24 C23 C28 118.0(6) . . ? C24 C23 C22 120.9(7) . . ? C28 C23 C22 121.0(7) . . ? C23 C24 C25 121.1(8) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 119.5(8) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 120.2(8) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 119.4(9) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C23 121.7(8) . . ? C27 C28 H28 119.1 . . ? C23 C28 H28 119.1 . . ? C30 C29 S2 120.1(5) . . ? C30 C29 H29A 107.3 . . ? S2 C29 H29A 107.3 . . ? C30 C29 H29B 107.3 . . ? S2 C29 H29B 107.3 . . ? H29A C29 H29B 106.9 . . ? C29 C30 C31 117.3(7) . . ? C29 C30 H30A 108.0 . . ? C31 C30 H30A 108.0 . . ? C29 C30 H30B 108.0 . . ? C31 C30 H30B 108.0 . . ? H30A C30 H30B 107.2 . . ? C32 C31 C36 116.7(7) . . ? C32 C31 C30 125.7(8) . . ? C36 C31 C30 117.5(8) . . ? C31 C32 C33 121.5(8) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 119.3(8) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 119.4(10) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C34 C35 C36 121.1(10) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 121.9(9) . . ? C35 C36 H36 119.1 . . ? C31 C36 H36 119.1 . . ? C38 C37 S3 109.8(5) . . ? C38 C37 H37A 109.7 . . ? S3 C37 H37A 109.7 . . ? C38 C37 H37B 109.7 . . ? S3 C37 H37B 109.7 . . ? H37A C37 H37B 108.2 . . ? C39 C38 C37 113.0(5) . . ? C39 C38 H38A 109.0 . . ? C37 C38 H38A 109.0 . . ? C39 C38 H38B 109.0 . . ? C37 C38 H38B 109.0 . . ? H38A C38 H38B 107.8 . . ? C44 C39 C40 117.9(7) . . ? C44 C39 C38 120.8(7) . . ? C40 C39 C38 121.3(6) . . ? C41 C40 C39 119.7(8) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C42 C41 C40 122.1(9) . . ? C42 C41 H41 118.9 . . ? C40 C41 H41 118.9 . . ? C43 C42 C41 117.8(8) . . ? C43 C42 H42 121.1 . . ? C41 C42 H42 121.1 . . ? C42 C43 C44 121.1(9) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C39 C44 C43 121.5(8) . . ? C39 C44 H44 119.3 . . ? C43 C44 H44 119.3 . . ? C21 S1 Ir1 109.43(19) . . ? C21 S1 Ir2 109.3(2) . . ? Ir1 S1 Ir2 88.89(6) . . ? C29 S2 Ir1 113.0(2) . . ? C29 S2 Ir2 110.5(2) . . ? Ir1 S2 Ir2 88.92(5) . . ? C37 S3 Ir1 110.6(2) . . ? C37 S3 Ir2 110.2(2) . . ? Ir1 S3 Ir2 88.20(5) . . ? C2 Ir1 C3 38.9(3) . . ? C2 Ir1 C5 64.2(2) . . ? C3 Ir1 C5 63.9(3) . . ? C2 Ir1 C1 38.3(3) . . ? C3 Ir1 C1 64.2(3) . . ? C5 Ir1 C1 38.2(2) . . ? C2 Ir1 C4 64.2(2) . . ? C3 Ir1 C4 37.6(2) . . ? C5 Ir1 C4 38.5(2) . . ? C1 Ir1 C4 64.1(3) . . ? C2 Ir1 S1 113.46(18) . . ? C3 Ir1 S1 150.92(19) . . ? C5 Ir1 S1 118.71(19) . . ? C1 Ir1 S1 99.28(18) . . ? C4 Ir1 S1 157.0(2) . . ? C2 Ir1 S2 109.26(19) . . ? C3 Ir1 S2 101.8(2) . . ? C5 Ir1 S2 164.33(18) . . ? C1 Ir1 S2 143.32(18) . . ? C4 Ir1 S2 126.1(2) . . ? S1 Ir1 S2 76.84(6) . . ? C2 Ir1 S3 169.47(17) . . ? C3 Ir1 S3 133.07(19) . . ? C5 Ir1 S3 107.12(17) . . ? C1 Ir1 S3 137.64(18) . . ? C4 Ir1 S3 105.37(19) . . ? S1 Ir1 S3 75.54(5) . . ? S2 Ir1 S3 77.49(5) . . ? C14 Ir2 C13 38.1(3) . . ? C14 Ir2 C12 63.8(3) . . ? C13 Ir2 C12 37.5(3) . . ? C14 Ir2 C15 39.1(3) . . ? C13 Ir2 C15 63.9(3) . . ? C12 Ir2 C15 63.7(2) . . ? C14 Ir2 C11 63.8(3) . . ? C13 Ir2 C11 63.0(3) . . ? C12 Ir2 C11 38.1(2) . . ? C15 Ir2 C11 37.4(3) . . ? C14 Ir2 S2 122.1(2) . . ? C13 Ir2 S2 100.38(18) . . ? C12 Ir2 S2 110.87(16) . . ? C15 Ir2 S2 161.1(2) . . ? C11 Ir2 S2 146.36(16) . . ? C14 Ir2 S1 161.2(2) . . ? C13 Ir2 S1 146.9(2) . . ? C12 Ir2 S1 112.0(2) . . ? C15 Ir2 S1 122.2(2) . . ? C11 Ir2 S1 101.13(19) . . ? S2 Ir2 S1 76.70(6) . . ? C14 Ir2 S3 106.9(2) . . ? C13 Ir2 S3 137.0(2) . . ? C12 Ir2 S3 169.76(17) . . ? C15 Ir2 S3 106.54(17) . . ? C11 Ir2 S3 135.27(16) . . ? S2 Ir2 S3 77.37(6) . . ? S1 Ir2 S3 75.29(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 C5 C1 C2 C3 -1.4(8) . . . . ? C6 C1 C2 C3 177.3(7) . . . . ? Ir1 C1 C2 C3 -62.2(4) . . . . ? C5 C1 C2 C7 -175.2(6) . . . . ? C6 C1 C2 C7 3.6(12) . . . . ? Ir1 C1 C2 C7 124.1(7) . . . . ? C5 C1 C2 Ir1 60.7(5) . . . . ? C6 C1 C2 Ir1 -120.5(7) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C7 C2 C3 C4 174.7(6) . . . . ? Ir1 C2 C3 C4 -61.9(4) . . . . ? C1 C2 C3 C8 -174.1(7) . . . . ? C7 C2 C3 C8 -0.1(11) . . . . ? Ir1 C2 C3 C8 123.3(7) . . . . ? C1 C2 C3 Ir1 62.7(5) . . . . ? C7 C2 C3 Ir1 -123.4(7) . . . . ? C2 C3 C4 C5 0.2(7) . . . . ? C8 C3 C4 C5 174.9(7) . . . . ? Ir1 C3 C4 C5 -60.7(4) . . . . ? C2 C3 C4 C9 -176.9(7) . . . . ? C8 C3 C4 C9 -2.3(12) . . . . ? Ir1 C3 C4 C9 122.1(7) . . . . ? C2 C3 C4 Ir1 61.0(4) . . . . ? C8 C3 C4 Ir1 -124.4(8) . . . . ? C2 C1 C5 C4 1.6(8) . . . . ? C6 C1 C5 C4 -177.2(7) . . . . ? Ir1 C1 C5 C4 62.0(5) . . . . ? C2 C1 C5 C10 173.6(6) . . . . ? C6 C1 C5 C10 -5.2(12) . . . . ? Ir1 C1 C5 C10 -126.0(7) . . . . ? C2 C1 C5 Ir1 -60.4(5) . . . . ? C6 C1 C5 Ir1 120.8(7) . . . . ? C3 C4 C5 C1 -1.1(7) . . . . ? C9 C4 C5 C1 176.1(7) . . . . ? Ir1 C4 C5 C1 -62.0(5) . . . . ? C3 C4 C5 C10 -173.1(7) . . . . ? C9 C4 C5 C10 4.1(11) . . . . ? Ir1 C4 C5 C10 126.0(7) . . . . ? C3 C4 C5 Ir1 60.9(4) . . . . ? C9 C4 C5 Ir1 -121.9(7) . . . . ? C15 C11 C12 C13 1.7(8) . . . . ? C16 C11 C12 C13 -175.0(7) . . . . ? Ir2 C11 C12 C13 62.4(5) . . . . ? C15 C11 C12 C17 176.1(6) . . . . ? C16 C11 C12 C17 -0.7(11) . . . . ? Ir2 C11 C12 C17 -123.2(7) . . . . ? C15 C11 C12 Ir2 -60.7(5) . . . . ? C16 C11 C12 Ir2 122.6(7) . . . . ? C11 C12 C13 C14 -2.7(8) . . . . ? C17 C12 C13 C14 -177.2(6) . . . . ? Ir2 C12 C13 C14 60.0(5) . . . . ? C11 C12 C13 C18 174.7(7) . . . . ? C17 C12 C13 C18 0.3(12) . . . . ? Ir2 C12 C13 C18 -122.5(8) . . . . ? C11 C12 C13 Ir2 -62.8(4) . . . . ? C17 C12 C13 Ir2 122.8(7) . . . . ? C12 C13 C14 C15 2.7(8) . . . . ? C18 C13 C14 C15 -174.7(7) . . . . ? Ir2 C13 C14 C15 63.5(5) . . . . ? C12 C13 C14 C19 173.9(7) . . . . ? C18 C13 C14 C19 -3.4(13) . . . . ? Ir2 C13 C14 C19 -125.2(8) . . . . ? C12 C13 C14 Ir2 -60.9(5) . . . . ? C18 C13 C14 Ir2 121.8(8) . . . . ? C12 C11 C15 C14 -0.1(7) . . . . ? C16 C11 C15 C14 176.7(7) . . . . ? Ir2 C11 C15 C14 -60.4(5) . . . . ? C12 C11 C15 C20 -176.0(7) . . . . ? C16 C11 C15 C20 0.8(11) . . . . ? Ir2 C11 C15 C20 123.7(7) . . . . ? C12 C11 C15 Ir2 60.3(4) . . . . ? C16 C11 C15 Ir2 -123.0(7) . . . . ? C13 C14 C15 C11 -1.6(8) . . . . ? C19 C14 C15 C11 -172.9(7) . . . . ? Ir2 C14 C15 C11 62.1(5) . . . . ? C13 C14 C15 C20 174.3(7) . . . . ? C19 C14 C15 C20 3.0(12) . . . . ? Ir2 C14 C15 C20 -122.0(7) . . . . ? C13 C14 C15 Ir2 -63.6(5) . . . . ? C19 C14 C15 Ir2 125.0(8) . . . . ? S1 C21 C22 C23 -176.6(6) . . . . ? C21 C22 C23 C24 105.8(9) . . . . ? C21 C22 C23 C28 -77.3(10) . . . . ? C28 C23 C24 C25 1.1(11) . . . . ? C22 C23 C24 C25 178.2(7) . . . . ? C23 C24 C25 C26 0.8(13) . . . . ? C24 C25 C26 C27 -2.7(15) . . . . ? C25 C26 C27 C28 2.6(15) . . . . ? C26 C27 C28 C23 -0.6(13) . . . . ? C24 C23 C28 C27 -1.2(11) . . . . ? C22 C23 C28 C27 -178.3(7) . . . . ? S2 C29 C30 C31 179.1(7) . . . . ? C29 C30 C31 C32 59.0(13) . . . . ? C29 C30 C31 C36 -120.7(10) . . . . ? C36 C31 C32 C33 -1.3(12) . . . . ? C30 C31 C32 C33 179.0(8) . . . . ? C31 C32 C33 C34 2.4(13) . . . . ? C32 C33 C34 C35 -3.0(15) . . . . ? C33 C34 C35 C36 2.6(19) . . . . ? C34 C35 C36 C31 -2(2) . . . . ? C32 C31 C36 C35 0.9(15) . . . . ? C30 C31 C36 C35 -179.4(10) . . . . ? S3 C37 C38 C39 67.7(7) . . . . ? C37 C38 C39 C44 84.3(7) . . . . ? C37 C38 C39 C40 -95.8(7) . . . . ? C44 C39 C40 C41 0.2(10) . . . . ? C38 C39 C40 C41 -179.7(6) . . . . ? C39 C40 C41 C42 0.1(11) . . . . ? C40 C41 C42 C43 -0.4(12) . . . . ? C41 C42 C43 C44 0.6(12) . . . . ? C40 C39 C44 C43 0.0(10) . . . . ? C38 C39 C44 C43 179.9(6) . . . . ? C42 C43 C44 C39 -0.4(12) . . . . ? C22 C21 S1 Ir1 -146.6(6) . . . . ? C22 C21 S1 Ir2 117.5(6) . . . . ? C30 C29 S2 Ir1 31.2(8) . . . . ? C30 C29 S2 Ir2 -66.7(7) . . . . ? C38 C37 S3 Ir1 -148.7(4) . . . . ? C38 C37 S3 Ir2 115.4(4) . . . . ? C1 C2 Ir1 C3 -116.9(6) . . . . ? C7 C2 Ir1 C3 119.6(9) . . . . ? C1 C2 Ir1 C5 -37.3(4) . . . . ? C3 C2 Ir1 C5 79.7(4) . . . . ? C7 C2 Ir1 C5 -160.7(8) . . . . ? C3 C2 Ir1 C1 116.9(6) . . . . ? C7 C2 Ir1 C1 -123.5(8) . . . . ? C1 C2 Ir1 C4 -80.2(4) . . . . ? C3 C2 Ir1 C4 36.7(4) . . . . ? C7 C2 Ir1 C4 156.3(8) . . . . ? C1 C2 Ir1 S1 74.6(4) . . . . ? C3 C2 Ir1 S1 -168.5(4) . . . . ? C7 C2 Ir1 S1 -48.9(7) . . . . ? C1 C2 Ir1 S2 158.2(3) . . . . ? C3 C2 Ir1 S2 -84.9(4) . . . . ? C7 C2 Ir1 S2 34.7(7) . . . . ? C1 C2 Ir1 S3 -73.2(12) . . . . ? C3 C2 Ir1 S3 43.8(13) . . . . ? C7 C2 Ir1 S3 163.4(8) . . . . ? C4 C3 Ir1 C2 118.2(6) . . . . ? C8 C3 Ir1 C2 -118.5(8) . . . . ? C4 C3 Ir1 C5 37.6(4) . . . . ? C2 C3 Ir1 C5 -80.6(4) . . . . ? C8 C3 Ir1 C5 160.9(8) . . . . ? C4 C3 Ir1 C1 80.3(4) . . . . ? C2 C3 Ir1 C1 -37.8(4) . . . . ? C8 C3 Ir1 C1 -156.3(8) . . . . ? C2 C3 Ir1 C4 -118.2(6) . . . . ? C8 C3 Ir1 C4 123.3(9) . . . . ? C4 C3 Ir1 S1 140.3(4) . . . . ? C2 C3 Ir1 S1 22.1(7) . . . . ? C8 C3 Ir1 S1 -96.4(8) . . . . ? C4 C3 Ir1 S2 -135.7(4) . . . . ? C2 C3 Ir1 S2 106.2(4) . . . . ? C8 C3 Ir1 S2 -12.3(7) . . . . ? C4 C3 Ir1 S3 -51.9(5) . . . . ? C2 C3 Ir1 S3 -170.0(3) . . . . ? C8 C3 Ir1 S3 71.5(7) . . . . ? C1 C5 Ir1 C2 37.3(4) . . . . ? C4 C5 Ir1 C2 -80.2(4) . . . . ? C10 C5 Ir1 C2 158.5(8) . . . . ? C1 C5 Ir1 C3 80.7(4) . . . . ? C4 C5 Ir1 C3 -36.8(4) . . . . ? C10 C5 Ir1 C3 -158.1(8) . . . . ? C4 C5 Ir1 C1 -117.5(5) . . . . ? C10 C5 Ir1 C1 121.2(9) . . . . ? C1 C5 Ir1 C4 117.5(5) . . . . ? C10 C5 Ir1 C4 -121.3(8) . . . . ? C1 C5 Ir1 S1 -66.5(4) . . . . ? C4 C5 Ir1 S1 175.9(3) . . . . ? C10 C5 Ir1 S1 54.7(7) . . . . ? C1 C5 Ir1 S2 105.9(7) . . . . ? C4 C5 Ir1 S2 -11.7(9) . . . . ? C10 C5 Ir1 S2 -132.9(6) . . . . ? C1 C5 Ir1 S3 -149.1(3) . . . . ? C4 C5 Ir1 S3 93.3(4) . . . . ? C10 C5 Ir1 S3 -27.9(7) . . . . ? C5 C1 Ir1 C2 -118.2(6) . . . . ? C6 C1 Ir1 C2 120.9(8) . . . . ? C2 C1 Ir1 C3 38.4(4) . . . . ? C5 C1 Ir1 C3 -79.8(4) . . . . ? C6 C1 Ir1 C3 159.3(7) . . . . ? C2 C1 Ir1 C5 118.2(6) . . . . ? C6 C1 Ir1 C5 -120.9(8) . . . . ? C2 C1 Ir1 C4 80.4(4) . . . . ? C5 C1 Ir1 C4 -37.8(4) . . . . ? C6 C1 Ir1 C4 -158.7(7) . . . . ? C2 C1 Ir1 S1 -116.4(4) . . . . ? C5 C1 Ir1 S1 125.4(4) . . . . ? C6 C1 Ir1 S1 4.5(6) . . . . ? C2 C1 Ir1 S2 -36.0(5) . . . . ? C5 C1 Ir1 S2 -154.2(3) . . . . ? C6 C1 Ir1 S2 84.9(7) . . . . ? C2 C1 Ir1 S3 165.0(3) . . . . ? C5 C1 Ir1 S3 46.7(5) . . . . ? C6 C1 Ir1 S3 -74.2(7) . . . . ? C3 C4 Ir1 C2 -37.9(4) . . . . ? C5 C4 Ir1 C2 80.3(4) . . . . ? C9 C4 Ir1 C2 -159.9(8) . . . . ? C5 C4 Ir1 C3 118.3(6) . . . . ? C9 C4 Ir1 C3 -122.0(8) . . . . ? C3 C4 Ir1 C5 -118.3(6) . . . . ? C9 C4 Ir1 C5 119.8(8) . . . . ? C3 C4 Ir1 C1 -80.6(4) . . . . ? C5 C4 Ir1 C1 37.6(4) . . . . ? C9 C4 Ir1 C1 157.4(7) . . . . ? C3 C4 Ir1 S1 -127.4(5) . . . . ? C5 C4 Ir1 S1 -9.2(7) . . . . ? C9 C4 Ir1 S1 110.6(7) . . . . ? C3 C4 Ir1 S2 57.9(5) . . . . ? C5 C4 Ir1 S2 176.1(3) . . . . ? C9 C4 Ir1 S2 -64.1(7) . . . . ? C3 C4 Ir1 S3 143.4(4) . . . . ? C5 C4 Ir1 S3 -98.3(4) . . . . ? C9 C4 Ir1 S3 21.5(7) . . . . ? C21 S1 Ir1 C2 34.4(3) . . . . ? Ir2 S1 Ir1 C2 144.5(2) . . . . ? C21 S1 Ir1 C3 19.5(5) . . . . ? Ir2 S1 Ir1 C3 129.6(4) . . . . ? C21 S1 Ir1 C5 106.7(3) . . . . ? Ir2 S1 Ir1 C5 -143.12(19) . . . . ? C21 S1 Ir1 C1 71.6(3) . . . . ? Ir2 S1 Ir1 C1 -178.25(18) . . . . ? C21 S1 Ir1 C4 113.2(5) . . . . ? Ir2 S1 Ir1 C4 -136.6(5) . . . . ? C21 S1 Ir1 S2 -71.2(2) . . . . ? Ir2 S1 Ir1 S2 38.98(5) . . . . ? C21 S1 Ir1 S3 -151.4(3) . . . . ? Ir2 S1 Ir1 S3 -41.27(5) . . . . ? C29 S2 Ir1 C2 98.5(3) . . . . ? Ir2 S2 Ir1 C2 -149.6(2) . . . . ? C29 S2 Ir1 C3 58.8(3) . . . . ? Ir2 S2 Ir1 C3 170.70(19) . . . . ? C29 S2 Ir1 C5 35.9(7) . . . . ? Ir2 S2 Ir1 C5 147.8(6) . . . . ? C29 S2 Ir1 C1 121.1(4) . . . . ? Ir2 S2 Ir1 C1 -127.0(3) . . . . ? C29 S2 Ir1 C4 26.9(3) . . . . ? Ir2 S2 Ir1 C4 138.8(2) . . . . ? C29 S2 Ir1 S1 -151.0(2) . . . . ? Ir2 S2 Ir1 S1 -39.06(5) . . . . ? C29 S2 Ir1 S3 -73.1(2) . . . . ? Ir2 S2 Ir1 S3 38.77(5) . . . . ? C37 S3 Ir1 C2 79.7(11) . . . . ? Ir2 S3 Ir1 C2 -169.4(11) . . . . ? C37 S3 Ir1 C3 116.1(3) . . . . ? Ir2 S3 Ir1 C3 -133.0(3) . . . . ? C37 S3 Ir1 C5 46.2(3) . . . . ? Ir2 S3 Ir1 C5 157.1(2) . . . . ? C37 S3 Ir1 C1 18.0(3) . . . . ? Ir2 S3 Ir1 C1 128.9(3) . . . . ? C37 S3 Ir1 C4 86.2(3) . . . . ? Ir2 S3 Ir1 C4 -162.8(2) . . . . ? C37 S3 Ir1 S1 -69.9(2) . . . . ? Ir2 S3 Ir1 S1 40.99(5) . . . . ? C37 S3 Ir1 S2 -149.4(2) . . . . ? Ir2 S3 Ir1 S2 -38.43(5) . . . . ? C15 C14 Ir2 C13 -116.0(6) . . . . ? C19 C14 Ir2 C13 122.5(12) . . . . ? C13 C14 Ir2 C12 36.3(4) . . . . ? C15 C14 Ir2 C12 -79.7(4) . . . . ? C19 C14 Ir2 C12 158.9(11) . . . . ? C13 C14 Ir2 C15 116.0(6) . . . . ? C19 C14 Ir2 C15 -121.4(12) . . . . ? C13 C14 Ir2 C11 79.0(4) . . . . ? C15 C14 Ir2 C11 -37.1(4) . . . . ? C19 C14 Ir2 C11 -158.5(11) . . . . ? C13 C14 Ir2 S2 -62.9(4) . . . . ? C15 C14 Ir2 S2 -178.9(3) . . . . ? C19 C14 Ir2 S2 59.6(11) . . . . ? C13 C14 Ir2 S1 117.7(7) . . . . ? C15 C14 Ir2 S1 1.6(9) . . . . ? C19 C14 Ir2 S1 -119.8(9) . . . . ? C13 C14 Ir2 S3 -148.4(4) . . . . ? C15 C14 Ir2 S3 95.6(4) . . . . ? C19 C14 Ir2 S3 -25.8(11) . . . . ? C12 C13 Ir2 C14 119.2(6) . . . . ? C18 C13 Ir2 C14 -122.3(11) . . . . ? C14 C13 Ir2 C12 -119.2(6) . . . . ? C18 C13 Ir2 C12 118.5(11) . . . . ? C12 C13 Ir2 C15 80.1(4) . . . . ? C14 C13 Ir2 C15 -39.1(4) . . . . ? C18 C13 Ir2 C15 -161.4(10) . . . . ? C12 C13 Ir2 C11 38.1(4) . . . . ? C14 C13 Ir2 C11 -81.1(4) . . . . ? C18 C13 Ir2 C11 156.6(10) . . . . ? C12 C13 Ir2 S2 -110.9(3) . . . . ? C14 C13 Ir2 S2 129.9(4) . . . . ? C18 C13 Ir2 S2 7.7(9) . . . . ? C12 C13 Ir2 S1 -29.3(6) . . . . ? C14 C13 Ir2 S1 -148.5(4) . . . . ? C18 C13 Ir2 S1 89.2(10) . . . . ? C12 C13 Ir2 S3 166.6(3) . . . . ? C14 C13 Ir2 S3 47.4(5) . . . . ? C18 C13 Ir2 S3 -74.9(10) . . . . ? C13 C12 Ir2 C14 -36.9(4) . . . . ? C11 C12 Ir2 C14 80.1(5) . . . . ? C17 C12 Ir2 C14 -157.2(8) . . . . ? C11 C12 Ir2 C13 117.0(6) . . . . ? C17 C12 Ir2 C13 -120.4(9) . . . . ? C13 C12 Ir2 C15 -80.6(5) . . . . ? C11 C12 Ir2 C15 36.4(4) . . . . ? C17 C12 Ir2 C15 159.0(9) . . . . ? C13 C12 Ir2 C11 -117.0(6) . . . . ? C17 C12 Ir2 C11 122.7(10) . . . . ? C13 C12 Ir2 S2 79.6(4) . . . . ? C11 C12 Ir2 S2 -163.4(4) . . . . ? C17 C12 Ir2 S2 -40.7(8) . . . . ? C13 C12 Ir2 S1 163.2(3) . . . . ? C11 C12 Ir2 S1 -79.8(4) . . . . ? C17 C12 Ir2 S1 42.9(8) . . . . ? C13 C12 Ir2 S3 -63.0(13) . . . . ? C11 C12 Ir2 S3 54.0(14) . . . . ? C17 C12 Ir2 S3 176.7(9) . . . . ? C11 C15 Ir2 C14 -117.1(6) . . . . ? C20 C15 Ir2 C14 120.4(10) . . . . ? C11 C15 Ir2 C13 -79.0(4) . . . . ? C14 C15 Ir2 C13 38.1(4) . . . . ? C20 C15 Ir2 C13 158.5(10) . . . . ? C11 C15 Ir2 C12 -37.0(4) . . . . ? C14 C15 Ir2 C12 80.1(4) . . . . ? C20 C15 Ir2 C12 -159.5(10) . . . . ? C14 C15 Ir2 C11 117.1(6) . . . . ? C20 C15 Ir2 C11 -122.5(11) . . . . ? C11 C15 Ir2 S2 -114.4(6) . . . . ? C14 C15 Ir2 S2 2.8(8) . . . . ? C20 C15 Ir2 S2 123.2(8) . . . . ? C11 C15 Ir2 S1 63.5(4) . . . . ? C14 C15 Ir2 S1 -179.4(3) . . . . ? C20 C15 Ir2 S1 -59.0(9) . . . . ? C11 C15 Ir2 S3 146.2(4) . . . . ? C14 C15 Ir2 S3 -96.6(4) . . . . ? C20 C15 Ir2 S3 23.8(9) . . . . ? C15 C11 Ir2 C14 38.7(5) . . . . ? C12 C11 Ir2 C14 -80.3(5) . . . . ? C16 C11 Ir2 C14 158.8(8) . . . . ? C15 C11 Ir2 C13 81.5(5) . . . . ? C12 C11 Ir2 C13 -37.5(4) . . . . ? C16 C11 Ir2 C13 -158.4(8) . . . . ? C15 C11 Ir2 C12 119.0(7) . . . . ? C16 C11 Ir2 C12 -120.8(8) . . . . ? C12 C11 Ir2 C15 -119.0(7) . . . . ? C16 C11 Ir2 C15 120.1(8) . . . . ? C15 C11 Ir2 S2 147.9(4) . . . . ? C12 C11 Ir2 S2 28.9(6) . . . . ? C16 C11 Ir2 S2 -92.0(7) . . . . ? C15 C11 Ir2 S1 -129.5(4) . . . . ? C12 C11 Ir2 S1 111.5(4) . . . . ? C16 C11 Ir2 S1 -9.3(7) . . . . ? C15 C11 Ir2 S3 -49.2(5) . . . . ? C12 C11 Ir2 S3 -168.2(3) . . . . ? C16 C11 Ir2 S3 70.9(7) . . . . ? C29 S2 Ir2 C14 -26.6(3) . . . . ? Ir1 S2 Ir2 C14 -140.9(2) . . . . ? C29 S2 Ir2 C13 -60.5(3) . . . . ? Ir1 S2 Ir2 C13 -174.8(2) . . . . ? C29 S2 Ir2 C12 -98.1(3) . . . . ? Ir1 S2 Ir2 C12 147.7(2) . . . . ? C29 S2 Ir2 C15 -28.7(6) . . . . ? Ir1 S2 Ir2 C15 -142.9(5) . . . . ? C29 S2 Ir2 C11 -116.6(4) . . . . ? Ir1 S2 Ir2 C11 129.1(3) . . . . ? C29 S2 Ir2 S1 153.2(2) . . . . ? Ir1 S2 Ir2 S1 38.94(5) . . . . ? C29 S2 Ir2 S3 75.6(2) . . . . ? Ir1 S2 Ir2 S3 -38.67(5) . . . . ? C21 S1 Ir2 C14 -109.3(6) . . . . ? Ir1 S1 Ir2 C14 140.5(6) . . . . ? C21 S1 Ir2 C13 -17.4(4) . . . . ? Ir1 S1 Ir2 C13 -127.7(3) . . . . ? C21 S1 Ir2 C12 -36.2(3) . . . . ? Ir1 S1 Ir2 C12 -146.43(17) . . . . ? C21 S1 Ir2 C15 -108.1(3) . . . . ? Ir1 S1 Ir2 C15 141.7(2) . . . . ? C21 S1 Ir2 C11 -74.4(3) . . . . ? Ir1 S1 Ir2 C11 175.37(17) . . . . ? C21 S1 Ir2 S2 71.2(2) . . . . ? Ir1 S1 Ir2 S2 -39.00(5) . . . . ? C21 S1 Ir2 S3 151.4(2) . . . . ? Ir1 S1 Ir2 S3 41.19(5) . . . . ? C37 S3 Ir2 C14 -90.1(3) . . . . ? Ir1 S3 Ir2 C14 158.5(3) . . . . ? C37 S3 Ir2 C13 -118.4(3) . . . . ? Ir1 S3 Ir2 C13 130.2(3) . . . . ? C37 S3 Ir2 C12 -65.7(12) . . . . ? Ir1 S3 Ir2 C12 -177.1(12) . . . . ? C37 S3 Ir2 C15 -49.3(3) . . . . ? Ir1 S3 Ir2 C15 -160.6(3) . . . . ? C37 S3 Ir2 C11 -20.6(4) . . . . ? Ir1 S3 Ir2 C11 -132.0(3) . . . . ? C37 S3 Ir2 S2 149.8(2) . . . . ? Ir1 S3 Ir2 S2 38.45(5) . . . . ? C37 S3 Ir2 S1 70.5(2) . . . . ? Ir1 S3 Ir2 S1 -40.89(5) . . . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 26.13 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.689 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.122 _database_code_depnum_ccdc_archive 'CCDC 939468'