Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Milstein, David' 'Dorta, Reto' 'Rozenberg, Haim' _publ_contact_author_name 'Prof David Milstein' _publ_contact_author_address ; Departments of Organic Chemistry and Chemical Services The Weizmann Institute of Science Rehovot Israel 76100 ISRAEL ; _publ_contact_author_email 'DAVID.MILSTEIN@WEIZMANN.AC.IL' _publ_section_title ; The first fully characterised neutral and cationic rhodium(I)-complexes containing DMSO as the only dative ligand; S-, 0- and bridging S,0-binding modes ; data_m248 _database_code_CSD 177298 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H18 Cl O3 Rh S3' _chemical_formula_weight 372.74 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' 'O' 'O' 0.0106 0.0060 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 5.7250(11) _cell_length_b 15.932(3) _cell_length_c 14.368(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.58(3) _cell_angle_gamma 90.00 _cell_volume 1310.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 24.10 _exptl_crystal_description parallelogram _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 1.966 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2076 _diffrn_reflns_av_R_equivalents 0.040 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 24.10 _reflns_number_total 2076 _reflns_number_gt 1922 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+6.7827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2076 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.31933(5) 0.431116(18) 0.22535(2) 0.01119(12) Uani 1 1 d . . . Cl2 Cl 0.30213(18) 0.54348(6) 0.11896(7) 0.0201(2) Uani 1 1 d . . . S3 S 0.53022(17) 0.51760(6) 0.31975(7) 0.0134(2) Uani 1 1 d . . . O30 O 0.6510(5) 0.48145(18) 0.4025(2) 0.0192(6) Uani 1 1 d . . . C31 C 0.3523(7) 0.6027(3) 0.3586(3) 0.0189(9) Uani 1 1 d . . . H31A H 0.2429 0.5825 0.4035 0.028 Uiso 1 1 calc R . . H31B H 0.2690 0.6263 0.3065 0.028 Uiso 1 1 calc R . . H31C H 0.4496 0.6450 0.3866 0.028 Uiso 1 1 calc R . . C32 C 0.7483(7) 0.5738(3) 0.2573(3) 0.0201(10) Uani 1 1 d . . . H32A H 0.8179 0.6153 0.2973 0.030 Uiso 1 1 calc R . . H32B H 0.6778 0.6009 0.2044 0.030 Uiso 1 1 calc R . . H32C H 0.8663 0.5355 0.2368 0.030 Uiso 1 1 calc R . . S4 S 0.26874(17) 0.33568(6) 0.33489(7) 0.0139(2) Uani 1 1 d . . . O40 O 0.0980(5) 0.26789(18) 0.3157(2) 0.0211(7) Uani 1 1 d . . . C41 C 0.1756(7) 0.3847(3) 0.4401(3) 0.0180(9) Uani 1 1 d . . . H41A H 0.0372 0.4171 0.4279 0.027 Uiso 1 1 calc R . . H41B H 0.2970 0.4209 0.4632 0.027 Uiso 1 1 calc R . . H41C H 0.1424 0.3424 0.4857 0.027 Uiso 1 1 calc R . . C42 C 0.5310(7) 0.2860(3) 0.3746(3) 0.0223(10) Uani 1 1 d . . . H42A H 0.4974 0.2513 0.4275 0.033 Uiso 1 1 calc R . . H42B H 0.6433 0.3280 0.3921 0.033 Uiso 1 1 calc R . . H42C H 0.5933 0.2520 0.3257 0.033 Uiso 1 1 calc R . . S5 S 0.16762(17) 0.34105(6) 0.11648(7) 0.0132(2) Uani 1 1 d . . . O50 O 0.2762(5) 0.25620(17) 0.1129(2) 0.0220(7) Uani 1 1 d . . . C51 C 0.1813(8) 0.3806(3) 0.0011(3) 0.0197(9) Uani 1 1 d . . . H51A H 0.3389 0.3967 -0.0123 0.029 Uiso 1 1 calc R . . H51B H 0.0807 0.4285 -0.0049 0.029 Uiso 1 1 calc R . . H51C H 0.1317 0.3378 -0.0418 0.029 Uiso 1 1 calc R . . C52 C -0.1407(7) 0.3276(3) 0.1258(4) 0.0274(11) Uani 1 1 d . . . H52A H -0.1960 0.2924 0.0761 0.041 Uiso 1 1 calc R . . H52B H -0.2161 0.3813 0.1219 0.041 Uiso 1 1 calc R . . H52C H -0.1758 0.3019 0.1844 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01178(18) 0.00988(18) 0.01192(19) -0.00047(12) 0.00051(12) -0.00077(12) Cl2 0.0244(5) 0.0161(5) 0.0198(6) 0.0047(4) -0.0037(4) -0.0037(4) S3 0.0122(5) 0.0129(5) 0.0152(5) -0.0018(4) 0.0001(4) -0.0014(4) O30 0.0193(15) 0.0183(15) 0.0199(16) 0.0022(13) -0.0048(12) -0.0002(12) C31 0.016(2) 0.016(2) 0.025(2) -0.0066(18) 0.0015(18) 0.0013(17) C32 0.015(2) 0.020(2) 0.026(2) 0.0012(19) 0.0034(18) -0.0068(17) S4 0.0146(5) 0.0122(5) 0.0149(5) 0.0010(4) 0.0010(4) -0.0006(4) O40 0.0224(16) 0.0160(15) 0.0248(17) -0.0008(13) -0.0011(13) -0.0067(12) C41 0.022(2) 0.022(2) 0.010(2) 0.0002(17) 0.0043(17) 0.0016(18) C42 0.018(2) 0.016(2) 0.033(3) 0.005(2) 0.0014(19) 0.0037(18) S5 0.0136(5) 0.0112(5) 0.0147(5) -0.0019(4) -0.0010(4) 0.0009(4) O50 0.0322(17) 0.0107(14) 0.0231(17) -0.0025(13) -0.0041(14) 0.0058(13) C51 0.027(2) 0.018(2) 0.014(2) 0.0025(18) -0.0017(18) 0.0026(18) C52 0.012(2) 0.034(3) 0.036(3) -0.009(2) -0.001(2) -0.0073(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 S4 2.2095(11) . ? Rh1 S3 2.2722(11) . ? Rh1 S5 2.2874(11) . ? Rh1 Cl2 2.3555(11) . ? S3 O30 1.485(3) . ? S3 C32 1.786(4) . ? S3 C31 1.788(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? S4 O40 1.481(3) . ? S4 C42 1.786(4) . ? S4 C41 1.788(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? S5 O50 1.489(3) . ? S5 C51 1.776(4) . ? S5 C52 1.784(4) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? 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 S4 Rh1 S3 93.72(4) . . ? S4 Rh1 S5 90.22(4) . . ? S3 Rh1 S5 169.86(4) . . ? S4 Rh1 Cl2 168.63(4) . . ? S3 Rh1 Cl2 86.84(4) . . ? S5 Rh1 Cl2 91.14(4) . . ? O30 S3 C32 105.92(19) . . ? O30 S3 C31 107.86(19) . . ? C32 S3 C31 100.4(2) . . ? O30 S3 Rh1 118.86(12) . . ? C32 S3 Rh1 111.98(15) . . ? C31 S3 Rh1 110.18(14) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O40 S4 C42 106.72(19) . . ? O40 S4 C41 105.90(19) . . ? C42 S4 C41 100.4(2) . . ? O40 S4 Rh1 117.40(13) . . ? C42 S4 Rh1 114.63(16) . . ? C41 S4 Rh1 110.14(15) . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O50 S5 C51 105.51(19) . . ? O50 S5 C52 107.9(2) . . ? C51 S5 C52 99.5(2) . . ? O50 S5 Rh1 115.93(13) . . ? C51 S5 Rh1 113.32(15) . . ? C52 S5 Rh1 113.14(16) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S4 Rh1 S3 O30 22.94(15) . . . . ? S5 Rh1 S3 O30 -89.7(3) . . . . ? Cl2 Rh1 S3 O30 -168.44(15) . . . . ? S4 Rh1 S3 C32 147.01(16) . . . . ? S5 Rh1 S3 C32 34.4(3) . . . . ? Cl2 Rh1 S3 C32 -44.37(16) . . . . ? S4 Rh1 S3 C31 -102.20(17) . . . . ? S5 Rh1 S3 C31 145.2(2) . . . . ? Cl2 Rh1 S3 C31 66.41(17) . . . . ? S3 Rh1 S4 O40 168.94(14) . . . . ? S5 Rh1 S4 O40 -20.41(15) . . . . ? Cl2 Rh1 S4 O40 76.5(2) . . . . ? S3 Rh1 S4 C42 -64.60(18) . . . . ? S5 Rh1 S4 C42 106.05(18) . . . . ? Cl2 Rh1 S4 C42 -157.1(2) . . . . ? S3 Rh1 S4 C41 47.69(16) . . . . ? S5 Rh1 S4 C41 -141.66(16) . . . . ? Cl2 Rh1 S4 C41 -44.8(3) . . . . ? S4 Rh1 S5 O50 -52.76(15) . . . . ? S3 Rh1 S5 O50 60.2(3) . . . . ? Cl2 Rh1 S5 O50 138.53(15) . . . . ? S4 Rh1 S5 C51 -175.00(16) . . . . ? S3 Rh1 S5 C51 -62.1(3) . . . . ? Cl2 Rh1 S5 C51 16.29(16) . . . . ? S4 Rh1 S5 C52 72.64(19) . . . . ? S3 Rh1 S5 C52 -174.4(3) . . . . ? Cl2 Rh1 S5 C52 -96.06(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.424 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.108 data_m244 _database_code_CSD 177299 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17.50 H32 Cl2 O3 Rh2 S3' _chemical_formula_weight 663.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.1740(12) _cell_length_b 12.026(2) _cell_length_c 17.111(3) _cell_angle_alpha 88.14(3) _cell_angle_beta 87.25(3) _cell_angle_gamma 82.67(3) _cell_volume 1258.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 28.28 _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 1.788 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6132 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0589 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 28.28 _reflns_number_total 6132 _reflns_number_gt 5019 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0217P)^2^+0.6973P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6132 _refine_ls_number_parameters 286 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0685 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.29762(4) 0.546436(18) 0.198833(12) 0.01472(7) Uani 1 1 d . . . Rh2 Rh 0.50139(4) 0.238119(18) 0.140853(13) 0.01605(7) Uani 1 1 d . . . Cl4 Cl 0.33503(13) 0.41637(6) 0.09557(4) 0.02178(16) Uani 1 1 d . . . Cl5 Cl 0.36174(12) 0.16339(6) 0.03135(4) 0.02111(16) Uani 1 1 d . . . S3 S 0.05999(12) 0.65815(6) 0.13595(4) 0.01587(15) Uani 1 1 d . . . S6 S 0.66639(14) 0.07012(6) 0.16990(5) 0.02333(18) Uani 1 1 d . . . S7 S 0.62082(12) 0.31535(6) 0.23962(4) 0.01805(16) Uani 1 1 d . . . O30 O -0.0415(3) 0.76408(17) 0.17117(12) 0.0212(5) Uani 1 1 d . . . O60 O 0.7816(5) 0.05391(19) 0.24407(14) 0.0434(7) Uani 1 1 d . . . O70 O 0.5533(3) 0.44017(16) 0.25075(12) 0.0205(5) Uani 1 1 d . . . C20 C 0.1819(5) 0.6165(2) 0.30834(16) 0.0177(6) Uani 1 1 d . . . H20 H 0.0329 0.6557 0.3070 0.021 Uiso 1 1 calc R . . C21 C 0.2179(5) 0.5410(2) 0.37974(17) 0.0217(7) Uani 1 1 d . . . H21A H 0.3718 0.5123 0.3818 0.026 Uiso 1 1 calc R . . H21B H 0.1362 0.4777 0.3765 0.026 Uiso 1 1 calc R . . C22 C 0.1431(5) 0.6063(3) 0.45494(17) 0.0227(7) Uani 1 1 d . . . H22A H -0.0154 0.6186 0.4582 0.027 Uiso 1 1 calc R . . H22B H 0.1906 0.5601 0.5000 0.027 Uiso 1 1 calc R . . C23 C 0.2295(5) 0.7199(3) 0.45944(18) 0.0229(7) Uani 1 1 d . . . H23A H 0.1764 0.7533 0.5087 0.028 Uiso 1 1 calc R . . H23B H 0.1675 0.7688 0.4178 0.028 Uiso 1 1 calc R . . C24 C 0.4799(5) 0.7171(3) 0.45312(18) 0.0237(7) Uani 1 1 d . . . H24A H 0.5225 0.7641 0.4933 0.028 Uiso 1 1 calc R . . H24B H 0.5456 0.6410 0.4643 0.028 Uiso 1 1 calc R . . C25 C 0.5754(5) 0.7558(3) 0.37379(17) 0.0220(7) Uani 1 1 d . . . H25A H 0.4980 0.8286 0.3600 0.026 Uiso 1 1 calc R . . H25B H 0.7270 0.7659 0.3801 0.026 Uiso 1 1 calc R . . C26 C 0.5665(5) 0.6777(3) 0.30508(17) 0.0193(6) Uani 1 1 d . . . H26A H 0.6633 0.6994 0.2625 0.023 Uiso 1 1 calc R . . H26B H 0.6197 0.6015 0.3216 0.023 Uiso 1 1 calc R . . C27 C 0.3390(5) 0.6801(3) 0.27541(17) 0.0185(6) Uani 1 1 d . . . H27 H 0.2771 0.7542 0.2558 0.022 Uiso 1 1 calc R . . C31 C -0.1596(5) 0.5883(3) 0.10602(18) 0.0219(7) Uani 1 1 d . . . H31A H -0.2445 0.5672 0.1513 0.033 Uiso 1 1 calc R . . H31B H -0.1015 0.5223 0.0781 0.033 Uiso 1 1 calc R . . H31C H -0.2509 0.6377 0.0726 0.033 Uiso 1 1 calc R . . C32 C 0.1771(5) 0.6943(3) 0.04241(17) 0.0233(7) Uani 1 1 d . . . H32A H 0.0650 0.7327 0.0108 0.035 Uiso 1 1 calc R . . H32B H 0.2418 0.6273 0.0170 0.035 Uiso 1 1 calc R . . H32C H 0.2873 0.7423 0.0492 0.035 Uiso 1 1 calc R . . C61 C 0.4934(6) -0.0379(3) 0.1683(2) 0.0302(8) Uani 1 1 d . . . H61A H 0.5766 -0.1091 0.1798 0.045 Uiso 1 1 calc R . . H61B H 0.4350 -0.0390 0.1173 0.045 Uiso 1 1 calc R . . H61C H 0.3757 -0.0236 0.2068 0.045 Uiso 1 1 calc R . . C62 C 0.8604(5) 0.0243(3) 0.0938(2) 0.0287(7) Uani 1 1 d . . . H62A H 0.9710 0.0738 0.0890 0.043 Uiso 1 1 calc R . . H62B H 0.7881 0.0249 0.0453 0.043 Uiso 1 1 calc R . . H62C H 0.9268 -0.0504 0.1059 0.043 Uiso 1 1 calc R . . C71 C 0.9120(5) 0.3032(3) 0.2420(2) 0.0307(8) Uani 1 1 d . . . H71A H 0.9693 0.3394 0.1960 0.046 Uiso 1 1 calc R . . H71B H 0.9710 0.2254 0.2433 0.046 Uiso 1 1 calc R . . H71C H 0.9521 0.3385 0.2878 0.046 Uiso 1 1 calc R . . C72 C 0.5548(6) 0.2565(3) 0.33357(18) 0.0312(8) Uani 1 1 d . . . H72A H 0.6235 0.2927 0.3731 0.047 Uiso 1 1 calc R . . H72B H 0.6062 0.1777 0.3348 0.047 Uiso 1 1 calc R . . H72C H 0.3992 0.2673 0.3433 0.047 Uiso 1 1 calc R . . C81 C -0.186(3) 0.9681(15) 0.4857(12) 0.033(4) Uani 0.50 1 d P . . C82 C -0.108(2) 0.9925(9) 0.4106(7) 0.051(4) Uani 0.50 1 d P . . C83 C 0.107(2) 1.0320(9) 0.3972(7) 0.049(4) Uani 0.50 1 d P . . C84 C 0.2292(19) 1.0405(8) 0.4661(8) 0.050(3) Uani 0.50 1 d P . . C85 C 0.136(3) 1.0165(13) 0.5415(11) 0.029(4) Uani 0.50 1 d P . . C86 C -0.0689(13) 0.9807(6) 0.5541(6) 0.0270(16) Uani 0.50 1 d P . . C87 C -0.159(2) 0.9560(13) 0.6373(7) 0.054(3) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01560(12) 0.01367(12) 0.01474(12) -0.00065(9) -0.00221(9) -0.00062(9) Rh2 0.01903(13) 0.01356(12) 0.01520(13) -0.00076(9) -0.00288(9) 0.00022(9) Cl4 0.0305(4) 0.0168(4) 0.0166(4) -0.0027(3) -0.0069(3) 0.0052(3) Cl5 0.0241(4) 0.0188(4) 0.0210(4) -0.0020(3) -0.0067(3) -0.0026(3) S3 0.0161(4) 0.0154(3) 0.0157(3) 0.0006(3) -0.0012(3) -0.0006(3) S6 0.0326(5) 0.0151(4) 0.0216(4) -0.0014(3) -0.0078(3) 0.0028(3) S7 0.0211(4) 0.0154(3) 0.0170(4) -0.0008(3) -0.0048(3) 0.0021(3) O30 0.0240(12) 0.0161(10) 0.0226(11) -0.0024(9) -0.0038(9) 0.0033(9) O60 0.073(2) 0.0224(13) 0.0328(14) -0.0029(11) -0.0310(13) 0.0126(13) O70 0.0266(12) 0.0139(10) 0.0206(11) -0.0055(8) -0.0087(9) 0.0032(9) C20 0.0234(16) 0.0145(14) 0.0144(14) -0.0050(11) 0.0008(12) 0.0015(12) C21 0.0251(17) 0.0182(15) 0.0228(16) 0.0007(13) -0.0030(13) -0.0065(13) C22 0.0250(17) 0.0269(17) 0.0163(15) 0.0005(13) 0.0009(12) -0.0043(14) C23 0.0273(17) 0.0241(16) 0.0167(15) -0.0057(13) -0.0004(13) 0.0007(14) C24 0.0276(18) 0.0234(16) 0.0204(16) -0.0055(13) -0.0034(13) -0.0028(14) C25 0.0221(16) 0.0220(16) 0.0230(16) -0.0039(13) -0.0038(13) -0.0053(13) C26 0.0180(15) 0.0195(15) 0.0217(16) -0.0029(12) -0.0007(12) -0.0064(12) C27 0.0194(16) 0.0176(15) 0.0185(15) -0.0046(12) 0.0000(12) -0.0011(12) C31 0.0168(15) 0.0255(16) 0.0242(16) 0.0013(13) -0.0053(13) -0.0040(13) C32 0.0223(17) 0.0257(17) 0.0207(16) 0.0066(13) 0.0020(13) -0.0010(13) C61 0.038(2) 0.0185(16) 0.0331(19) 0.0028(14) 0.0096(15) -0.0026(15) C62 0.0221(17) 0.0220(17) 0.042(2) -0.0052(15) -0.0026(15) 0.0005(14) C71 0.0214(17) 0.0259(17) 0.044(2) -0.0056(16) -0.0109(15) 0.0036(14) C72 0.050(2) 0.0260(18) 0.0158(16) 0.0017(14) -0.0035(15) 0.0011(16) C81 0.019(8) 0.018(5) 0.065(13) 0.007(8) -0.003(7) -0.011(5) C82 0.090(10) 0.020(4) 0.038(6) 0.002(5) -0.007(6) 0.010(4) C83 0.084(11) 0.032(6) 0.022(7) -0.008(6) -0.007(7) 0.024(6) C84 0.050(7) 0.019(4) 0.076(8) 0.007(5) 0.044(6) 0.001(4) C85 0.014(7) 0.017(7) 0.058(12) -0.004(8) -0.012(7) -0.004(4) C86 0.019(4) 0.021(4) 0.040(5) -0.004(4) -0.006(4) 0.004(3) C87 0.056(7) 0.076(8) 0.026(6) 0.010(6) 0.003(6) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O70 2.112(2) . ? Rh1 C20 2.133(3) . ? Rh1 C27 2.154(3) . ? Rh1 S3 2.1610(10) . ? Rh1 Cl4 2.3812(10) . ? Rh2 S7 2.1584(9) . ? Rh2 S6 2.1965(10) . ? Rh2 Cl5 2.3503(9) . ? Rh2 Cl4 2.3785(10) . ? S3 O30 1.479(2) . ? S3 C32 1.788(3) . ? S3 C31 1.787(3) . ? S6 O60 1.480(2) . ? S6 C62 1.779(4) . ? S6 C61 1.785(3) . ? S7 O70 1.521(2) . ? S7 C72 1.786(3) . ? S7 C71 1.787(3) . ? C20 C27 1.397(4) . ? C20 C21 1.506(4) . ? C20 H20 0.9800 . ? C21 C22 1.550(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.535(4) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.540(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.536(4) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.536(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.513(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 H27 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C81 C85 0.583(17) 2_576 ? C81 C84 0.863(17) 2_576 ? C81 C82 1.384(17) . ? C81 C86 1.43(2) . ? C81 C86 1.853(16) 2_576 ? C82 C85 0.834(16) 2_576 ? C82 C86 1.354(15) 2_576 ? C82 C83 1.47(2) . ? C83 C87 0.678(12) 2_576 ? C83 C86 0.869(12) 2_576 ? C83 C84 1.443(18) . ? C84 C81 0.863(17) 2_576 ? C84 C86 1.126(13) 2_576 ? C84 C85 1.424(16) . ? C84 C87 1.839(17) 2_576 ? C85 C81 0.583(17) 2_576 ? C85 C82 0.834(16) 2_576 ? C85 C86 1.393(15) . ? C85 C86 1.71(2) 2_576 ? C86 C83 0.869(12) 2_576 ? C86 C84 1.126(13) 2_576 ? C86 C82 1.354(15) 2_576 ? C86 C87 1.537(12) . ? C86 C85 1.71(2) 2_576 ? C86 C81 1.853(16) 2_576 ? C87 C83 0.678(12) 2_576 ? C87 C84 1.839(17) 2_576 ? 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 O70 Rh1 C20 92.48(10) . . ? O70 Rh1 C27 91.28(10) . . ? C20 Rh1 C27 38.04(11) . . ? O70 Rh1 S3 174.08(6) . . ? C20 Rh1 S3 91.99(9) . . ? C27 Rh1 S3 89.85(9) . . ? O70 Rh1 Cl4 86.06(6) . . ? C20 Rh1 Cl4 157.34(8) . . ? C27 Rh1 Cl4 164.39(8) . . ? S3 Rh1 Cl4 91.30(3) . . ? S7 Rh2 S6 94.24(4) . . ? S7 Rh2 Cl5 176.96(3) . . ? S6 Rh2 Cl5 88.81(4) . . ? S7 Rh2 Cl4 90.14(4) . . ? S6 Rh2 Cl4 174.01(3) . . ? Cl5 Rh2 Cl4 86.83(3) . . ? Rh2 Cl4 Rh1 110.23(3) . . ? O30 S3 C32 106.93(14) . . ? O30 S3 C31 106.36(14) . . ? C32 S3 C31 100.01(15) . . ? O30 S3 Rh1 120.19(9) . . ? C32 S3 Rh1 109.32(11) . . ? C31 S3 Rh1 112.04(11) . . ? O60 S6 C62 106.77(16) . . ? O60 S6 C61 106.56(16) . . ? C62 S6 C61 99.61(16) . . ? O60 S6 Rh2 118.15(11) . . ? C62 S6 Rh2 110.15(12) . . ? C61 S6 Rh2 113.81(12) . . ? O70 S7 C72 102.53(15) . . ? O70 S7 C71 102.56(14) . . ? C72 S7 C71 100.67(17) . . ? O70 S7 Rh2 118.40(9) . . ? C72 S7 Rh2 115.79(12) . . ? C71 S7 Rh2 114.47(13) . . ? S7 O70 Rh1 128.59(12) . . ? C27 C20 C21 123.4(3) . . ? C27 C20 Rh1 71.77(17) . . ? C21 C20 Rh1 116.4(2) . . ? C27 C20 H20 113.0 . . ? C21 C20 H20 113.0 . . ? Rh1 C20 H20 113.0 . . ? C20 C21 C22 110.4(2) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C21 114.6(2) . . ? C23 C22 H22A 108.6 . . ? C21 C22 H22A 108.6 . . ? C23 C22 H22B 108.6 . . ? C21 C22 H22B 108.6 . . ? H22A C22 H22B 107.6 . . ? C22 C23 C24 116.0(3) . . ? C22 C23 H23A 108.3 . . ? C24 C23 H23A 108.3 . . ? C22 C23 H23B 108.3 . . ? C24 C23 H23B 108.3 . . ? H23A C23 H23B 107.4 . . ? C25 C24 C23 115.8(3) . . ? C25 C24 H24A 108.3 . . ? C23 C24 H24A 108.3 . . ? C25 C24 H24B 108.3 . . ? C23 C24 H24B 108.3 . . ? H24A C24 H24B 107.4 . . ? C26 C25 C24 116.3(2) . . ? C26 C25 H25A 108.2 . . ? C24 C25 H25A 108.2 . . ? C26 C25 H25B 108.2 . . ? C24 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C25 113.1(3) . . ? C27 C26 H26A 109.0 . . ? C25 C26 H26A 109.0 . . ? C27 C26 H26B 109.0 . . ? C25 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? C20 C27 C26 124.2(3) . . ? C20 C27 Rh1 70.19(16) . . ? C26 C27 Rh1 115.2(2) . . ? C20 C27 H27 113.4 . . ? C26 C27 H27 113.4 . . ? Rh1 C27 H27 113.4 . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? S6 C61 H61A 109.5 . . ? S6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? S6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? S6 C62 H62A 109.5 . . ? S6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? S6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? S7 C71 H71A 109.5 . . ? S7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? S7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? S7 C72 H72A 109.5 . . ? S7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? S7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C85 C81 C84 160(4) 2_576 2_576 ? C85 C81 C82 15(3) 2_576 . ? C84 C81 C82 174(2) 2_576 . ? C85 C81 C86 109(3) 2_576 . ? C84 C81 C86 52.1(13) 2_576 . ? C82 C81 C86 123.6(13) . . ? C85 C81 C86 32(3) 2_576 2_576 ? C84 C81 C86 128.7(17) 2_576 2_576 ? C82 C81 C86 46.7(8) . 2_576 ? C86 C81 C86 76.8(9) . 2_576 ? C85 C82 C86 74.9(14) 2_576 2_576 ? C85 C82 C81 10.5(16) 2_576 . ? C86 C82 C81 85.2(11) 2_576 . ? C85 C82 C83 110.3(16) 2_576 . ? C86 C82 C83 35.5(6) 2_576 . ? C81 C82 C83 120.6(12) . . ? C87 C83 C86 167(3) 2_576 2_576 ? C87 C83 C84 115(2) 2_576 . ? C86 C83 C84 51.2(8) 2_576 . ? C87 C83 C82 129(2) 2_576 . ? C86 C83 C82 64.7(12) 2_576 . ? C84 C83 C82 115.9(11) . . ? C81 C84 C86 90.7(13) 2_576 2_576 ? C81 C84 C85 8.2(16) 2_576 . ? C86 C84 C85 83.1(11) 2_576 . ? C81 C84 C83 127.6(16) 2_576 . ? C86 C84 C83 37.0(8) 2_576 . ? C85 C84 C83 120.1(14) . . ? C81 C84 C87 147.0(15) 2_576 2_576 ? C86 C84 C87 56.4(8) 2_576 2_576 ? C85 C84 C87 139.5(13) . 2_576 ? C83 C84 C87 19.4(7) . 2_576 ? C81 C85 C82 154(4) 2_576 2_576 ? C81 C85 C86 135(4) 2_576 . ? C82 C85 C86 69.8(13) 2_576 . ? C81 C85 C84 12(3) 2_576 . ? C82 C85 C84 166(2) 2_576 . ? C86 C85 C84 123.8(15) . . ? C81 C85 C86 52(3) 2_576 2_576 ? C82 C85 C86 152.6(16) 2_576 2_576 ? C86 C85 C86 82.9(10) . 2_576 ? C84 C85 C86 40.9(8) . 2_576 ? C83 C86 C84 91.7(13) 2_576 2_576 ? C83 C86 C82 79.9(14) 2_576 2_576 ? C84 C86 C82 171.2(11) 2_576 2_576 ? C83 C86 C85 115.2(15) 2_576 . ? C84 C86 C85 153.0(11) 2_576 . ? C82 C86 C85 35.3(8) 2_576 . ? C83 C86 C81 128.9(14) 2_576 . ? C84 C86 C81 37.2(6) 2_576 . ? C82 C86 C81 151.3(10) 2_576 . ? C85 C86 C81 115.9(10) . . ? C83 C86 C87 5.8(13) 2_576 . ? C84 C86 C87 85.9(10) 2_576 . ? C82 C86 C87 85.7(9) 2_576 . ? C85 C86 C87 121.0(11) . . ? C81 C86 C87 123.1(10) . . ? C83 C86 C85 147.7(14) 2_576 2_576 ? C84 C86 C85 56.0(7) 2_576 2_576 ? C82 C86 C85 132.4(8) 2_576 2_576 ? C85 C86 C85 97.1(10) . 2_576 ? C81 C86 C85 18.9(6) . 2_576 ? C87 C86 C85 141.9(10) . 2_576 ? C83 C86 C81 128.0(15) 2_576 2_576 ? C84 C86 C81 140.2(11) 2_576 2_576 ? C82 C86 C81 48.1(8) 2_576 2_576 ? C85 C86 C81 12.8(12) . 2_576 ? C81 C86 C81 103.2(9) . 2_576 ? C87 C86 C81 133.7(11) . 2_576 ? C85 C86 C81 84.3(7) 2_576 2_576 ? C83 C87 C86 7.5(16) 2_576 . ? C83 C87 C84 45.1(18) 2_576 2_576 ? C86 C87 C84 37.6(5) . 2_576 ? 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 S7 Rh2 Cl4 Rh1 -18.42(4) . . . . ? S6 Rh2 Cl4 Rh1 -155.4(3) . . . . ? Cl5 Rh2 Cl4 Rh1 161.38(4) . . . . ? O70 Rh1 Cl4 Rh2 22.67(6) . . . . ? C20 Rh1 Cl4 Rh2 -64.3(2) . . . . ? C27 Rh1 Cl4 Rh2 103.3(3) . . . . ? S3 Rh1 Cl4 Rh2 -162.63(3) . . . . ? O70 Rh1 S3 O30 -117.6(6) . . . . ? C20 Rh1 S3 O30 21.40(13) . . . . ? C27 Rh1 S3 O30 -16.59(13) . . . . ? Cl4 Rh1 S3 O30 178.98(10) . . . . ? O70 Rh1 S3 C32 6.5(6) . . . . ? C20 Rh1 S3 C32 145.52(14) . . . . ? C27 Rh1 S3 C32 107.53(14) . . . . ? Cl4 Rh1 S3 C32 -56.90(12) . . . . ? O70 Rh1 S3 C31 116.4(6) . . . . ? C20 Rh1 S3 C31 -104.56(14) . . . . ? C27 Rh1 S3 C31 -142.55(14) . . . . ? Cl4 Rh1 S3 C31 53.02(12) . . . . ? S7 Rh2 S6 O60 5.50(15) . . . . ? Cl5 Rh2 S6 O60 -174.52(14) . . . . ? Cl4 Rh2 S6 O60 142.3(3) . . . . ? S7 Rh2 S6 C62 -117.52(12) . . . . ? Cl5 Rh2 S6 C62 62.46(12) . . . . ? Cl4 Rh2 S6 C62 19.3(3) . . . . ? S7 Rh2 S6 C61 131.61(13) . . . . ? Cl5 Rh2 S6 C61 -48.41(13) . . . . ? Cl4 Rh2 S6 C61 -91.6(3) . . . . ? S6 Rh2 S7 O70 -179.60(11) . . . . ? Cl5 Rh2 S7 O70 0.8(6) . . . . ? Cl4 Rh2 S7 O70 4.50(11) . . . . ? S6 Rh2 S7 C72 -57.24(14) . . . . ? Cl5 Rh2 S7 C72 123.2(6) . . . . ? Cl4 Rh2 S7 C72 126.85(14) . . . . ? S6 Rh2 S7 C71 59.23(13) . . . . ? Cl5 Rh2 S7 C71 -120.3(6) . . . . ? Cl4 Rh2 S7 C71 -116.67(13) . . . . ? C72 S7 O70 Rh1 -112.91(19) . . . . ? C71 S7 O70 Rh1 142.98(18) . . . . ? Rh2 S7 O70 Rh1 15.91(19) . . . . ? C20 Rh1 O70 S7 132.19(17) . . . . ? C27 Rh1 O70 S7 170.23(17) . . . . ? S3 Rh1 O70 S7 -88.8(6) . . . . ? Cl4 Rh1 O70 S7 -25.16(15) . . . . ? O70 Rh1 C20 C27 88.91(17) . . . . ? S3 Rh1 C20 C27 -87.21(17) . . . . ? Cl4 Rh1 C20 C27 174.63(17) . . . . ? O70 Rh1 C20 C21 -30.1(2) . . . . ? C27 Rh1 C20 C21 -119.0(3) . . . . ? S3 Rh1 C20 C21 153.8(2) . . . . ? Cl4 Rh1 C20 C21 55.7(4) . . . . ? C27 C20 C21 C22 90.5(3) . . . . ? Rh1 C20 C21 C22 175.3(2) . . . . ? C20 C21 C22 C23 -48.7(4) . . . . ? C21 C22 C23 C24 -56.9(4) . . . . ? C22 C23 C24 C25 103.3(3) . . . . ? C23 C24 C25 C26 -70.1(4) . . . . ? C24 C25 C26 C27 73.5(3) . . . . ? C21 C20 C27 C26 2.5(5) . . . . ? Rh1 C20 C27 C26 -107.6(3) . . . . ? C21 C20 C27 Rh1 110.1(3) . . . . ? C25 C26 C27 C20 -83.8(4) . . . . ? C25 C26 C27 Rh1 -166.15(19) . . . . ? O70 Rh1 C27 C20 -92.39(18) . . . . ? S3 Rh1 C27 C20 93.42(17) . . . . ? Cl4 Rh1 C27 C20 -172.3(2) . . . . ? O70 Rh1 C27 C26 27.0(2) . . . . ? C20 Rh1 C27 C26 119.3(3) . . . . ? S3 Rh1 C27 C26 -147.2(2) . . . . ? Cl4 Rh1 C27 C26 -53.0(4) . . . . ? C84 C81 C82 C85 33(17) 2_576 . . 2_576 ? C86 C81 C82 C85 -11(8) . . . 2_576 ? C86 C81 C82 C85 -11(10) 2_576 . . 2_576 ? C85 C81 C82 C86 11(10) 2_576 . . 2_576 ? C84 C81 C82 C86 44(21) 2_576 . . 2_576 ? C86 C81 C82 C86 1(2) . . . 2_576 ? C85 C81 C82 C83 12(10) 2_576 . . . ? C84 C81 C82 C83 44(22) 2_576 . . . ? C86 C81 C82 C83 1(3) . . . . ? C86 C81 C82 C83 0.5(9) 2_576 . . . ? C85 C82 C83 C87 180(3) 2_576 . . 2_576 ? C86 C82 C83 C87 178(3) 2_576 . . 2_576 ? C81 C82 C83 C87 178(3) . . . 2_576 ? C85 C82 C83 C86 1.4(15) 2_576 . . 2_576 ? C81 C82 C83 C86 -0.8(15) . . . 2_576 ? C85 C82 C83 C84 3.6(16) 2_576 . . . ? C86 C82 C83 C84 2.2(8) 2_576 . . . ? C81 C82 C83 C84 1.4(19) . . . . ? C87 C83 C84 C81 176(2) 2_576 . . 2_576 ? C86 C83 C84 C81 -4.4(18) 2_576 . . 2_576 ? C82 C83 C84 C81 -7.0(18) . . . 2_576 ? C87 C83 C84 C86 -179(3) 2_576 . . 2_576 ? C82 C83 C84 C86 -2.5(10) . . . 2_576 ? C87 C83 C84 C85 -180(2) 2_576 . . . ? C86 C83 C84 C85 -0.4(13) 2_576 . . . ? C82 C83 C84 C85 -2.9(17) . . . . ? C86 C83 C84 C87 179(3) 2_576 . . 2_576 ? C82 C83 C84 C87 177(3) . . . 2_576 ? C86 C84 C85 C81 -157(12) 2_576 . . 2_576 ? C83 C84 C85 C81 -157(12) . . . 2_576 ? C87 C84 C85 C81 -157(12) 2_576 . . 2_576 ? C81 C84 C85 C82 -18(9) 2_576 . . 2_576 ? C86 C84 C85 C82 -175(8) 2_576 . . 2_576 ? C83 C84 C85 C82 -174(8) . . . 2_576 ? C87 C84 C85 C82 -175(7) 2_576 . . 2_576 ? C81 C84 C85 C86 159(14) 2_576 . . . ? C86 C84 C85 C86 2.0(18) 2_576 . . . ? C83 C84 C85 C86 2(2) . . . . ? C87 C84 C85 C86 2(3) 2_576 . . . ? C81 C84 C85 C86 157(12) 2_576 . . 2_576 ? C83 C84 C85 C86 0.2(8) . . . 2_576 ? C87 C84 C85 C86 0.0(15) 2_576 . . 2_576 ? C81 C85 C86 C83 -175(5) 2_576 . . 2_576 ? C82 C85 C86 C83 -1.5(16) 2_576 . . 2_576 ? C84 C85 C86 C83 179.3(14) . . . 2_576 ? C86 C85 C86 C83 -179.4(12) 2_576 . . 2_576 ? C81 C85 C86 C84 2(7) 2_576 . . 2_576 ? C82 C85 C86 C84 175(2) 2_576 . . 2_576 ? C84 C85 C86 C84 -4(4) . . . 2_576 ? C86 C85 C86 C84 -3(3) 2_576 . . 2_576 ? C81 C85 C86 C82 -173(6) 2_576 . . 2_576 ? C84 C85 C86 C82 -179(2) . . . 2_576 ? C86 C85 C86 C82 -177.9(15) 2_576 . . 2_576 ? C81 C85 C86 C81 6(7) 2_576 . . . ? C82 C85 C86 C81 179.4(13) 2_576 . . . ? C84 C85 C86 C81 0(3) . . . . ? C86 C85 C86 C81 1.6(16) 2_576 . . . ? C81 C85 C86 C87 -174(5) 2_576 . . . ? C82 C85 C86 C87 -1.0(16) 2_576 . . . ? C84 C85 C86 C87 179.9(14) . . . . ? C86 C85 C86 C87 -178.8(12) 2_576 . . . ? C81 C85 C86 C85 5(5) 2_576 . . 2_576 ? C82 C85 C86 C85 177.9(15) 2_576 . . 2_576 ? C84 C85 C86 C85 -1.3(12) . . . 2_576 ? C86 C85 C86 C85 0.003(2) 2_576 . . 2_576 ? C82 C85 C86 C81 173(6) 2_576 . . 2_576 ? C84 C85 C86 C81 -6(4) . . . 2_576 ? C86 C85 C86 C81 -5(5) 2_576 . . 2_576 ? C85 C81 C86 C83 176(3) 2_576 . . 2_576 ? C84 C81 C86 C83 4.5(19) 2_576 . . 2_576 ? C82 C81 C86 C83 179.2(15) . . . 2_576 ? C86 C81 C86 C83 179.6(14) 2_576 . . 2_576 ? C85 C81 C86 C84 172(5) 2_576 . . 2_576 ? C82 C81 C86 C84 175(3) . . . 2_576 ? C86 C81 C86 C84 175.1(15) 2_576 . . 2_576 ? C85 C81 C86 C82 -4(6) 2_576 . . 2_576 ? C84 C81 C86 C82 -176(2) 2_576 . . 2_576 ? C82 C81 C86 C82 -1(4) . . . 2_576 ? C86 C81 C86 C82 -1(3) 2_576 . . 2_576 ? C85 C81 C86 C85 -5(5) 2_576 . . . ? C84 C81 C86 C85 -176.6(13) 2_576 . . . ? C82 C81 C86 C85 -2(3) . . . . ? C86 C81 C86 C85 -1.5(15) 2_576 . . . ? C85 C81 C86 C87 176(3) 2_576 . . . ? C84 C81 C86 C87 3.8(16) 2_576 . . . ? C82 C81 C86 C87 178.5(15) . . . . ? C86 C81 C86 C87 178.9(12) 2_576 . . . ? C84 C81 C86 C85 -172(5) 2_576 . . 2_576 ? C82 C81 C86 C85 3(2) . . . 2_576 ? C86 C81 C86 C85 3(3) 2_576 . . 2_576 ? C85 C81 C86 C81 -3(3) 2_576 . . 2_576 ? C84 C81 C86 C81 -175.1(15) 2_576 . . 2_576 ? C82 C81 C86 C81 -0.4(15) . . . 2_576 ? C86 C81 C86 C81 0.0 2_576 . . 2_576 ? C84 C86 C87 C83 177(10) 2_576 . . 2_576 ? C82 C86 C87 C83 -5(10) 2_576 . . 2_576 ? C85 C86 C87 C83 -5(11) . . . 2_576 ? C81 C86 C87 C83 175(10) . . . 2_576 ? C85 C86 C87 C83 177(10) 2_576 . . 2_576 ? C81 C86 C87 C83 -7(11) 2_576 . . 2_576 ? C83 C86 C87 C84 -177(10) 2_576 . . 2_576 ? C82 C86 C87 C84 177.6(10) 2_576 . . 2_576 ? C85 C86 C87 C84 178.1(15) . . . 2_576 ? C81 C86 C87 C84 -2.3(10) . . . 2_576 ? C85 C86 C87 C84 0.0(15) 2_576 . . 2_576 ? C81 C86 C87 C84 176.3(14) 2_576 . . 2_576 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.708 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.122 data_m295 _database_code_CSD 177300 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H48 B2 Cl0 F8 O4 Rh2 S4' _chemical_formula_weight 908.30 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' 'O' 'O' 0.0106 0.0060 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 12.317(3) _cell_length_b 24.171(5) _cell_length_c 11.808(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3515.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 28.28 _exptl_crystal_description parallelogram _exptl_crystal_colour yellow _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 1.248 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4561 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4561 _reflns_number_gt 4229 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0479P)^2^+3.1178P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(3) _refine_ls_number_reflns 4561 _refine_ls_number_parameters 405 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.69648(2) 0.428290(12) 0.51458(3) 0.01872(8) Uani 1 1 d . . . S11 S 0.49663(10) 0.36579(5) 0.38710(12) 0.0303(3) Uani 1 1 d . . . O11 O 0.6183(3) 0.36778(15) 0.4154(3) 0.0321(8) Uani 1 1 d . . . C11A C 0.4929(4) 0.3420(2) 0.2449(5) 0.0325(11) Uani 1 1 d . . . H11A H 0.5253 0.3692 0.1963 0.049 Uiso 1 1 calc R . . H11B H 0.4189 0.3360 0.2226 0.049 Uiso 1 1 calc R . . H11C H 0.5325 0.3079 0.2391 0.049 Uiso 1 1 calc R . . C11B C 0.4477(5) 0.3054(3) 0.4567(5) 0.0468(15) Uani 1 1 d . . . H11D H 0.4836 0.2734 0.4266 0.070 Uiso 1 1 calc R . . H11E H 0.3709 0.3021 0.4447 0.070 Uiso 1 1 calc R . . H11F H 0.4622 0.3082 0.5364 0.070 Uiso 1 1 calc R . . S12 S 0.88420(10) 0.33069(6) 0.44546(14) 0.0344(3) Uani 1 1 d . . . O12 O 0.8450(2) 0.38363(14) 0.5031(5) 0.0365(8) Uani 1 1 d . . . C12A C 0.7939(5) 0.2777(2) 0.4926(5) 0.0398(14) Uani 1 1 d . . . H12A H 0.7971 0.2751 0.5737 0.060 Uiso 1 1 calc R . . H12B H 0.8149 0.2430 0.4598 0.060 Uiso 1 1 calc R . . H12C H 0.7212 0.2866 0.4697 0.060 Uiso 1 1 calc R . . C12B C 0.8461(4) 0.3345(2) 0.3007(5) 0.0341(12) Uani 1 1 d . . . H12D H 0.7698 0.3420 0.2952 0.051 Uiso 1 1 calc R . . H12E H 0.8621 0.3000 0.2641 0.051 Uiso 1 1 calc R . . H12F H 0.8860 0.3637 0.2643 0.051 Uiso 1 1 calc R . . C11 C 0.5803(4) 0.4894(2) 0.4824(4) 0.0282(12) Uani 1 1 d . . . H11 H 0.5687 0.4710 0.4143 0.034 Uiso 1 1 calc R . . C12 C 0.5529(4) 0.46177(19) 0.5819(4) 0.0225(9) Uani 1 1 d . . . H12 H 0.5254 0.4261 0.5763 0.027 Uiso 1 1 calc R . . C13 C 0.5658(5) 0.4867(3) 0.6979(5) 0.0435(14) Uani 1 1 d . . . H13A H 0.5238 0.4650 0.7513 0.052 Uiso 1 1 calc R . . H13B H 0.5356 0.5238 0.6970 0.052 Uiso 1 1 calc R . . C14 C 0.6823(5) 0.4898(3) 0.7394(5) 0.0432(15) Uani 1 1 d . . . H14A H 0.6991 0.5280 0.7577 0.052 Uiso 1 1 calc R . . H14B H 0.6886 0.4684 0.8085 0.052 Uiso 1 1 calc R . . C15 C 0.7641(4) 0.4692(2) 0.6565(5) 0.0310(11) Uani 1 1 d . . . H15 H 0.7988 0.4358 0.6715 0.037 Uiso 1 1 calc R . . C16 C 0.7913(4) 0.4978(2) 0.5566(5) 0.0303(11) Uani 1 1 d . . . H16 H 0.8434 0.4824 0.5090 0.036 Uiso 1 1 calc R . . C17 C 0.7408(6) 0.5519(2) 0.5228(6) 0.0492(15) Uani 1 1 d . . . H17A H 0.7862 0.5691 0.4658 0.059 Uiso 1 1 calc R . . H17B H 0.7396 0.5761 0.5883 0.059 Uiso 1 1 calc R . . C18 C 0.6273(5) 0.5470(3) 0.4770(8) 0.064(3) Uani 1 1 d . . . H18A H 0.6273 0.5592 0.3988 0.077 Uiso 1 1 calc R . . H18B H 0.5805 0.5718 0.5193 0.077 Uiso 1 1 calc R . . Rh2 Rh 0.33048(3) 0.082300(12) 0.50572(3) 0.01932(8) Uani 1 1 d . . . S21 S 0.52674(10) 0.12639(5) 0.67076(11) 0.0255(2) Uani 1 1 d . . . O21 O 0.4091(3) 0.13154(14) 0.6286(3) 0.0304(8) Uani 1 1 d . . . C21A C 0.5976(5) 0.1800(3) 0.5994(5) 0.0453(15) Uani 1 1 d . . . H21A H 0.5997 0.1721 0.5197 0.068 Uiso 1 1 calc R . . H21B H 0.6703 0.1824 0.6282 0.068 Uiso 1 1 calc R . . H21C H 0.5610 0.2146 0.6116 0.068 Uiso 1 1 calc R . . C21B C 0.5214(4) 0.1567(2) 0.8082(5) 0.0318(11) Uani 1 1 d . . . H21D H 0.4935 0.1937 0.8026 0.048 Uiso 1 1 calc R . . H21E H 0.5931 0.1577 0.8400 0.048 Uiso 1 1 calc R . . H21F H 0.4748 0.1350 0.8560 0.048 Uiso 1 1 calc R . . S22 S 0.22367(9) 0.19686(5) 0.57199(11) 0.0231(2) Uani 1 1 d . . . O22 O 0.2002(2) 0.13910(13) 0.5242(4) 0.0282(8) Uani 1 1 d . . . C22A C 0.1083(4) 0.23532(19) 0.5284(5) 0.0306(11) Uani 1 1 d . . . H22A H 0.1083 0.2387 0.4474 0.046 Uiso 1 1 calc R . . H22B H 0.1106 0.2715 0.5619 0.046 Uiso 1 1 calc R . . H22C H 0.0435 0.2166 0.5523 0.046 Uiso 1 1 calc R . . C22B C 0.1933(4) 0.1914(2) 0.7200(5) 0.0313(11) Uani 1 1 d . . . H22D H 0.1225 0.1755 0.7295 0.047 Uiso 1 1 calc R . . H22E H 0.1949 0.2275 0.7537 0.047 Uiso 1 1 calc R . . H22F H 0.2463 0.1682 0.7560 0.047 Uiso 1 1 calc R . . C21 C 0.4356(3) 0.01361(18) 0.5210(6) 0.0277(10) Uani 1 1 d . . . H21 H 0.4458 0.0233 0.5964 0.033 Uiso 1 1 calc R . . C22 C 0.4717(4) 0.0497(2) 0.4363(5) 0.0284(10) Uani 1 1 d . . . H22 H 0.5050 0.0823 0.4596 0.034 Uiso 1 1 calc R . . C23 C 0.4614(5) 0.0403(3) 0.3103(5) 0.0401(13) Uani 1 1 d . . . H23A H 0.5082 0.0099 0.2882 0.048 Uiso 1 1 calc R . . H23B H 0.4859 0.0732 0.2705 0.048 Uiso 1 1 calc R . . C24 C 0.3448(5) 0.0273(2) 0.2748(5) 0.0386(13) Uani 1 1 d . . . H24A H 0.3317 0.0425 0.2000 0.046 Uiso 1 1 calc R . . H24B H 0.3358 -0.0125 0.2700 0.046 Uiso 1 1 calc R . . C25 C 0.2612(4) 0.0506(2) 0.3571(4) 0.0297(11) Uani 1 1 d . . . H25 H 0.2352 0.0861 0.3439 0.036 Uiso 1 1 calc R . . C26 C 0.2209(4) 0.0219(2) 0.4514(5) 0.0280(10) Uani 1 1 d . . . H26 H 0.1677 0.0392 0.4946 0.034 Uiso 1 1 calc R . . C27 C 0.2580(5) -0.03533(19) 0.4884(5) 0.0361(13) Uani 1 1 d . . . H27A H 0.2281 -0.0433 0.5626 0.043 Uiso 1 1 calc R . . H27B H 0.2294 -0.0626 0.4359 0.043 Uiso 1 1 calc R . . C28 C 0.3802(4) -0.0410(2) 0.4934(6) 0.0372(13) Uani 1 1 d . . . H28A H 0.4065 -0.0544 0.4211 0.045 Uiso 1 1 calc R . . H28B H 0.3992 -0.0681 0.5507 0.045 Uiso 1 1 calc R . . B1 B 0.3432(4) 0.3259(2) 0.7481(5) 0.0257(11) Uani 1 1 d . . . F1 F 0.4037(3) 0.37256(13) 0.7264(3) 0.0430(8) Uani 1 1 d . . . F2 F 0.2652(3) 0.31934(13) 0.6635(3) 0.0385(8) Uani 1 1 d . . . F3 F 0.4110(3) 0.27980(13) 0.7485(3) 0.0373(7) Uani 1 1 d . . . F4 F 0.2915(3) 0.33021(16) 0.8517(3) 0.0538(10) Uani 1 1 d . . . B2 B 0.6384(5) 0.1820(3) 0.2615(6) 0.0319(13) Uani 1 1 d . . . F5 F 0.6833(4) 0.23395(18) 0.2577(4) 0.0711(14) Uani 1 1 d . . . F6 F 0.6088(3) 0.16727(16) 0.1540(3) 0.0548(10) Uani 1 1 d . . . F7 F 0.5484(3) 0.1823(2) 0.3313(4) 0.0714(14) Uani 1 1 d . . . F8 F 0.7124(4) 0.1465(2) 0.3058(6) 0.097(2) 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 Rh1 0.01658(14) 0.01824(14) 0.02132(17) -0.00202(17) -0.00139(17) 0.00069(11) S11 0.0194(5) 0.0333(6) 0.0382(7) -0.0157(6) -0.0045(5) 0.0029(5) O11 0.0189(16) 0.0347(19) 0.043(2) -0.0195(16) -0.0068(15) 0.0034(14) C11A 0.035(3) 0.034(3) 0.029(3) 0.000(2) -0.006(2) -0.010(2) C11B 0.036(3) 0.071(4) 0.033(3) 0.003(3) 0.003(2) -0.012(3) S12 0.0254(6) 0.0270(6) 0.0510(8) -0.0069(6) -0.0064(6) 0.0076(5) O12 0.0204(15) 0.0327(17) 0.056(2) -0.017(2) -0.008(2) 0.0089(13) C12A 0.051(3) 0.028(2) 0.041(4) 0.002(2) -0.008(3) 0.003(2) C12B 0.029(3) 0.035(3) 0.039(3) -0.001(2) 0.009(2) 0.001(2) C11 0.025(2) 0.027(2) 0.032(3) 0.0081(19) 0.0017(18) 0.011(2) C12 0.023(2) 0.016(2) 0.028(2) -0.0033(18) 0.0073(19) 0.0017(18) C13 0.051(4) 0.049(3) 0.030(3) -0.013(3) 0.003(3) 0.008(3) C14 0.060(4) 0.052(4) 0.017(3) -0.002(2) -0.006(2) -0.004(3) C15 0.033(3) 0.025(2) 0.036(3) -0.005(2) -0.016(2) 0.000(2) C16 0.029(2) 0.028(2) 0.034(3) -0.012(2) 0.001(2) -0.012(2) C17 0.081(4) 0.027(2) 0.039(3) 0.000(3) -0.011(4) -0.016(3) C18 0.034(3) 0.037(3) 0.122(8) 0.040(4) 0.030(4) 0.010(3) Rh2 0.02010(15) 0.01508(14) 0.02279(17) -0.00276(17) 0.00053(18) 0.00148(10) S21 0.0232(5) 0.0218(5) 0.0314(6) -0.0037(5) -0.0024(5) 0.0025(5) O21 0.0228(16) 0.0256(17) 0.043(2) -0.0128(16) -0.0078(15) 0.0050(14) C21A 0.043(3) 0.055(4) 0.037(3) 0.009(3) -0.005(3) -0.022(3) C21B 0.035(3) 0.028(2) 0.032(3) 0.000(2) -0.005(2) 0.002(2) S22 0.0235(5) 0.0175(5) 0.0284(6) -0.0030(4) 0.0013(5) 0.0004(4) O22 0.0180(13) 0.0223(14) 0.044(2) -0.0055(18) -0.0021(16) 0.0044(11) C22A 0.033(2) 0.023(2) 0.036(3) -0.006(2) -0.005(2) 0.0042(19) C22B 0.038(3) 0.026(3) 0.030(3) 0.002(2) 0.003(2) 0.003(2) C21 0.030(2) 0.0217(19) 0.032(3) -0.003(2) -0.003(2) 0.0154(17) C22 0.024(2) 0.024(2) 0.038(3) -0.006(2) 0.007(2) 0.005(2) C23 0.044(3) 0.044(3) 0.033(3) -0.002(2) 0.015(2) 0.005(3) C24 0.053(3) 0.036(3) 0.027(3) -0.006(2) 0.002(3) 0.010(3) C25 0.037(3) 0.025(2) 0.027(3) -0.006(2) -0.008(2) 0.003(2) C26 0.026(2) 0.024(2) 0.034(3) -0.011(2) -0.002(2) 0.000(2) C27 0.049(3) 0.023(2) 0.036(3) 0.000(2) 0.006(2) -0.010(2) C28 0.048(3) 0.019(2) 0.044(4) -0.001(2) 0.005(3) 0.007(2) B1 0.024(3) 0.022(2) 0.031(3) 0.002(2) 0.001(2) -0.002(2) F1 0.0378(17) 0.0317(16) 0.059(2) 0.0090(16) -0.0011(17) -0.0126(14) F2 0.0335(17) 0.0360(16) 0.046(2) -0.0025(15) -0.0099(15) -0.0023(14) F3 0.0375(16) 0.0297(16) 0.0446(19) 0.0024(14) -0.0024(14) 0.0079(13) F4 0.063(2) 0.057(2) 0.042(2) -0.0027(18) 0.0250(19) -0.0011(19) B2 0.025(3) 0.034(3) 0.037(3) 0.008(3) -0.001(2) -0.003(2) F5 0.116(4) 0.048(2) 0.050(3) -0.001(2) -0.007(3) -0.037(2) F6 0.065(3) 0.054(2) 0.046(2) -0.0152(19) -0.0016(19) -0.010(2) F7 0.044(2) 0.127(4) 0.043(2) 0.006(3) 0.0058(19) -0.007(2) F8 0.048(3) 0.110(4) 0.134(5) 0.078(4) -0.003(3) 0.022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C11 2.092(5) . ? Rh1 C12 2.101(4) . ? Rh1 C16 2.106(5) . ? Rh1 O11 2.107(3) . ? Rh1 C15 2.117(5) . ? Rh1 O12 2.128(3) . ? S11 O11 1.536(3) . ? S11 C11A 1.775(6) . ? S11 C11B 1.780(7) . ? C11A H11A 0.9600 . ? C11A H11B 0.9600 . ? C11A H11C 0.9600 . ? C11B H11D 0.9600 . ? C11B H11E 0.9600 . ? C11B H11F 0.9600 . ? S12 O12 1.528(4) . ? S12 C12B 1.775(6) . ? S12 C12A 1.785(6) . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C11 C12 1.393(7) . ? C11 C18 1.510(8) . ? C11 H11 0.9300 . ? C12 C13 1.504(7) . ? C12 H12 0.9300 . ? C13 C14 1.519(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.489(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.408(8) . ? C15 H15 0.9300 . ? C16 C17 1.501(8) . ? C16 H16 0.9300 . ? C17 C18 1.503(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? Rh2 C22 2.079(5) . ? Rh2 C26 2.088(5) . ? Rh2 C25 2.097(5) . ? Rh2 O21 2.112(3) . ? Rh2 C21 2.113(4) . ? Rh2 O22 2.123(3) . ? S21 O21 1.537(3) . ? S21 C21A 1.776(6) . ? S21 C21B 1.781(6) . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? S22 O22 1.533(3) . ? S22 C22A 1.775(5) . ? S22 C22B 1.792(6) . ? C22A H22A 0.9600 . ? C22A H22B 0.9600 . ? C22A H22C 0.9600 . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C21 C22 1.399(8) . ? C21 C28 1.521(7) . ? C21 H21 0.9300 . ? C22 C23 1.510(8) . ? C22 H22 0.9300 . ? C23 C24 1.530(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.524(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.402(8) . ? C25 H25 0.9300 . ? C26 C27 1.522(7) . ? C26 H26 0.9300 . ? C27 C28 1.512(8) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? B1 F1 1.377(6) . ? B1 F4 1.383(7) . ? B1 F3 1.392(6) . ? B1 F2 1.395(7) . ? B2 F8 1.356(8) . ? B2 F6 1.367(8) . ? B2 F5 1.374(7) . ? B2 F7 1.381(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh1 C12 38.80(19) . . ? C11 Rh1 C16 81.9(2) . . ? C12 Rh1 C16 94.0(2) . . ? C11 Rh1 O11 94.40(18) . . ? C12 Rh1 O11 95.34(16) . . ? C16 Rh1 O11 159.81(19) . . ? C11 Rh1 C15 94.7(2) . . ? C12 Rh1 C15 81.4(2) . . ? C16 Rh1 C15 39.0(2) . . ? O11 Rh1 C15 160.81(19) . . ? C11 Rh1 O12 159.2(2) . . ? C12 Rh1 O12 160.5(2) . . ? C16 Rh1 O12 86.73(17) . . ? O11 Rh1 O12 90.31(14) . . ? C15 Rh1 O12 87.10(19) . . ? O11 S11 C11A 104.0(2) . . ? O11 S11 C11B 104.8(3) . . ? C11A S11 C11B 99.4(3) . . ? S11 O11 Rh1 126.1(2) . . ? S11 C11A H11A 109.5 . . ? S11 C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? S11 C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? S11 C11B H11D 109.5 . . ? S11 C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? S11 C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? O12 S12 C12B 107.6(3) . . ? O12 S12 C12A 105.4(3) . . ? C12B S12 C12A 100.0(3) . . ? S12 O12 Rh1 136.5(2) . . ? S12 C12A H12A 109.5 . . ? S12 C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? S12 C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? S12 C12B H12D 109.5 . . ? S12 C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? S12 C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C12 C11 C18 124.8(6) . . ? C12 C11 Rh1 70.9(3) . . ? C18 C11 Rh1 113.4(4) . . ? C12 C11 H11 117.6 . . ? C18 C11 H11 117.6 . . ? Rh1 C11 H11 85.7 . . ? C11 C12 C13 123.4(5) . . ? C11 C12 Rh1 70.3(3) . . ? C13 C12 Rh1 114.2(4) . . ? C11 C12 H12 118.3 . . ? C13 C12 H12 118.3 . . ? Rh1 C12 H12 85.6 . . ? C12 C13 C14 114.4(5) . . ? C12 C13 H13A 108.7 . . ? C14 C13 H13A 108.7 . . ? C12 C13 H13B 108.7 . . ? C14 C13 H13B 108.7 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 114.2(5) . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C16 C15 C14 123.2(5) . . ? C16 C15 Rh1 70.1(3) . . ? C14 C15 Rh1 114.2(4) . . ? C16 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? Rh1 C15 H15 85.8 . . ? C15 C16 C17 123.4(5) . . ? C15 C16 Rh1 70.9(3) . . ? C17 C16 Rh1 113.7(4) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? Rh1 C16 H16 85.5 . . ? C16 C17 C18 114.5(4) . . ? C16 C17 H17A 108.6 . . ? C18 C17 H17A 108.6 . . ? C16 C17 H17B 108.6 . . ? C18 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C17 C18 C11 114.4(5) . . ? C17 C18 H18A 108.7 . . ? C11 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? C11 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C22 Rh2 C26 98.9(2) . . ? C22 Rh2 C25 82.6(2) . . ? C26 Rh2 C25 39.1(2) . . ? C22 Rh2 O21 95.79(17) . . ? C26 Rh2 O21 154.32(19) . . ? C25 Rh2 O21 165.42(18) . . ? C22 Rh2 C21 39.0(2) . . ? C26 Rh2 C21 82.71(19) . . ? C25 Rh2 C21 91.9(2) . . ? O21 Rh2 C21 95.93(18) . . ? C22 Rh2 O22 156.70(19) . . ? C26 Rh2 O22 89.72(16) . . ? C25 Rh2 O22 90.86(18) . . ? O21 Rh2 O22 84.92(14) . . ? C21 Rh2 O22 164.23(19) . . ? O21 S21 C21A 104.5(3) . . ? O21 S21 C21B 103.1(2) . . ? C21A S21 C21B 98.6(3) . . ? S21 O21 Rh2 127.5(2) . . ? S21 C21A H21A 109.5 . . ? S21 C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? S21 C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? S21 C21B H21D 109.5 . . ? S21 C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? S21 C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? O22 S22 C22A 102.7(2) . . ? O22 S22 C22B 104.6(3) . . ? C22A S22 C22B 98.9(3) . . ? S22 O22 Rh2 118.98(18) . . ? S22 C22A H22A 109.5 . . ? S22 C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? S22 C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? S22 C22B H22D 109.5 . . ? S22 C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? S22 C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C22 C21 C28 122.0(5) . . ? C22 C21 Rh2 69.2(3) . . ? C28 C21 Rh2 112.9(3) . . ? C22 C21 H21 119.0 . . ? C28 C21 H21 119.0 . . ? Rh2 C21 H21 88.0 . . ? C21 C22 C23 125.8(5) . . ? C21 C22 Rh2 71.8(3) . . ? C23 C22 Rh2 112.0(4) . . ? C21 C22 H22 117.1 . . ? C23 C22 H22 117.1 . . ? Rh2 C22 H22 86.0 . . ? C22 C23 C24 112.3(5) . . ? C22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C25 C24 C23 112.5(5) . . ? C25 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? C25 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C24 124.3(5) . . ? C26 C25 Rh2 70.1(3) . . ? C24 C25 Rh2 113.2(4) . . ? C26 C25 H25 117.9 . . ? C24 C25 H25 117.9 . . ? Rh2 C25 H25 86.7 . . ? C25 C26 C27 124.8(5) . . ? C25 C26 Rh2 70.8(3) . . ? C27 C26 Rh2 110.7(4) . . ? C25 C26 H26 117.6 . . ? C27 C26 H26 117.6 . . ? Rh2 C26 H26 88.5 . . ? C28 C27 C26 113.1(4) . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C21 112.1(4) . . ? C27 C28 H28A 109.2 . . ? C21 C28 H28A 109.2 . . ? C27 C28 H28B 109.2 . . ? C21 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? F1 B1 F4 110.6(5) . . ? F1 B1 F3 109.4(4) . . ? F4 B1 F3 109.6(5) . . ? F1 B1 F2 109.4(5) . . ? F4 B1 F2 108.9(4) . . ? F3 B1 F2 109.0(4) . . ? F8 B2 F6 111.9(6) . . ? F8 B2 F5 108.6(5) . . ? F6 B2 F5 108.3(5) . . ? F8 B2 F7 108.3(5) . . ? F6 B2 F7 109.9(5) . . ? F5 B2 F7 109.8(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 C11A S11 O11 Rh1 142.3(3) . . . . ? C11B S11 O11 Rh1 -113.9(3) . . . . ? C11 Rh1 O11 S11 -25.1(3) . . . . ? C12 Rh1 O11 S11 13.9(3) . . . . ? C16 Rh1 O11 S11 -103.4(5) . . . . ? C15 Rh1 O11 S11 93.1(6) . . . . ? O12 Rh1 O11 S11 175.2(3) . . . . ? C12B S12 O12 Rh1 51.3(5) . . . . ? C12A S12 O12 Rh1 -54.7(5) . . . . ? C11 Rh1 O12 S12 -101.7(6) . . . . ? C12 Rh1 O12 S12 108.8(6) . . . . ? C16 Rh1 O12 S12 -158.4(5) . . . . ? O11 Rh1 O12 S12 1.6(5) . . . . ? C15 Rh1 O12 S12 162.6(5) . . . . ? C16 Rh1 C11 C12 -106.9(3) . . . . ? O11 Rh1 C11 C12 93.0(3) . . . . ? C15 Rh1 C11 C12 -70.1(3) . . . . ? O12 Rh1 C11 C12 -164.4(5) . . . . ? C12 Rh1 C11 C18 120.6(6) . . . . ? C16 Rh1 C11 C18 13.7(5) . . . . ? O11 Rh1 C11 C18 -146.4(5) . . . . ? C15 Rh1 C11 C18 50.5(5) . . . . ? O12 Rh1 C11 C18 -43.8(8) . . . . ? C18 C11 C12 C13 0.9(8) . . . . ? Rh1 C11 C12 C13 106.6(5) . . . . ? C18 C11 C12 Rh1 -105.7(5) . . . . ? C16 Rh1 C12 C11 71.7(3) . . . . ? O11 Rh1 C12 C11 -90.4(3) . . . . ? C15 Rh1 C12 C11 108.7(3) . . . . ? O12 Rh1 C12 C11 163.3(4) . . . . ? C11 Rh1 C12 C13 -118.6(5) . . . . ? C16 Rh1 C12 C13 -46.9(4) . . . . ? O11 Rh1 C12 C13 151.0(4) . . . . ? C15 Rh1 C12 C13 -9.9(4) . . . . ? O12 Rh1 C12 C13 44.7(7) . . . . ? C11 C12 C13 C14 -74.2(7) . . . . ? Rh1 C12 C13 C14 7.3(7) . . . . ? C12 C13 C14 C15 1.8(8) . . . . ? C13 C14 C15 C16 71.3(7) . . . . ? C13 C14 C15 Rh1 -10.0(7) . . . . ? C11 Rh1 C15 C16 -70.8(3) . . . . ? C12 Rh1 C15 C16 -107.4(3) . . . . ? O11 Rh1 C15 C16 171.0(4) . . . . ? O12 Rh1 C15 C16 88.4(3) . . . . ? C11 Rh1 C15 C14 47.6(4) . . . . ? C12 Rh1 C15 C14 11.0(4) . . . . ? C16 Rh1 C15 C14 118.4(5) . . . . ? O11 Rh1 C15 C14 -70.6(7) . . . . ? O12 Rh1 C15 C14 -153.2(4) . . . . ? C14 C15 C16 C17 -0.3(8) . . . . ? Rh1 C15 C16 C17 106.3(5) . . . . ? C14 C15 C16 Rh1 -106.6(5) . . . . ? C11 Rh1 C16 C15 108.0(3) . . . . ? C12 Rh1 C16 C15 71.1(3) . . . . ? O11 Rh1 C16 C15 -171.4(4) . . . . ? O12 Rh1 C16 C15 -89.4(3) . . . . ? C11 Rh1 C16 C17 -11.0(4) . . . . ? C12 Rh1 C16 C17 -47.9(5) . . . . ? O11 Rh1 C16 C17 69.6(7) . . . . ? C15 Rh1 C16 C17 -119.0(6) . . . . ? O12 Rh1 C16 C17 151.6(5) . . . . ? C15 C16 C17 C18 -75.8(8) . . . . ? Rh1 C16 C17 C18 6.3(8) . . . . ? C16 C17 C18 C11 5.1(10) . . . . ? C12 C11 C18 C17 68.2(8) . . . . ? Rh1 C11 C18 C17 -14.1(8) . . . . ? C21A S21 O21 Rh2 101.9(4) . . . . ? C21B S21 O21 Rh2 -155.4(3) . . . . ? C22 Rh2 O21 S21 -17.3(3) . . . . ? C26 Rh2 O21 S21 107.4(4) . . . . ? C25 Rh2 O21 S21 -100.3(7) . . . . ? C21 Rh2 O21 S21 21.9(3) . . . . ? O22 Rh2 O21 S21 -173.9(3) . . . . ? C22A S22 O22 Rh2 161.2(3) . . . . ? C22B S22 O22 Rh2 -96.0(3) . . . . ? C22 Rh2 O22 S22 -71.1(6) . . . . ? C26 Rh2 O22 S22 176.6(3) . . . . ? C25 Rh2 O22 S22 -144.3(3) . . . . ? O21 Rh2 O22 S22 21.7(3) . . . . ? C21 Rh2 O22 S22 115.5(6) . . . . ? C26 Rh2 C21 C22 113.9(3) . . . . ? C25 Rh2 C21 C22 75.8(3) . . . . ? O21 Rh2 C21 C22 -91.9(3) . . . . ? O22 Rh2 C21 C22 175.8(6) . . . . ? C22 Rh2 C21 C28 -117.1(6) . . . . ? C26 Rh2 C21 C28 -3.2(4) . . . . ? C25 Rh2 C21 C28 -41.3(5) . . . . ? O21 Rh2 C21 C28 151.0(4) . . . . ? O22 Rh2 C21 C28 58.7(10) . . . . ? C28 C21 C22 C23 0.1(7) . . . . ? Rh2 C21 C22 C23 -104.5(5) . . . . ? C28 C21 C22 Rh2 104.6(4) . . . . ? C26 Rh2 C22 C21 -66.6(4) . . . . ? C25 Rh2 C22 C21 -102.3(3) . . . . ? O21 Rh2 C22 C21 92.3(3) . . . . ? O22 Rh2 C22 C21 -177.1(4) . . . . ? C26 Rh2 C22 C23 55.5(4) . . . . ? C25 Rh2 C22 C23 19.7(4) . . . . ? O21 Rh2 C22 C23 -145.7(4) . . . . ? C21 Rh2 C22 C23 122.0(6) . . . . ? O22 Rh2 C22 C23 -55.1(7) . . . . ? C21 C22 C23 C24 52.9(7) . . . . ? Rh2 C22 C23 C24 -30.1(6) . . . . ? C22 C23 C24 C25 25.3(7) . . . . ? C23 C24 C25 C26 -90.0(6) . . . . ? C23 C24 C25 Rh2 -9.0(6) . . . . ? C22 Rh2 C25 C26 113.9(3) . . . . ? O21 Rh2 C25 C26 -161.4(6) . . . . ? C21 Rh2 C25 C26 76.0(3) . . . . ? O22 Rh2 C25 C26 -88.5(3) . . . . ? C22 Rh2 C25 C24 -5.8(4) . . . . ? C26 Rh2 C25 C24 -119.7(5) . . . . ? O21 Rh2 C25 C24 78.9(8) . . . . ? C21 Rh2 C25 C24 -43.8(4) . . . . ? O22 Rh2 C25 C24 151.8(4) . . . . ? C24 C25 C26 C27 2.8(8) . . . . ? Rh2 C25 C26 C27 -102.3(5) . . . . ? C24 C25 C26 Rh2 105.1(5) . . . . ? C22 Rh2 C26 C25 -66.6(3) . . . . ? O21 Rh2 C26 C25 169.3(3) . . . . ? C21 Rh2 C26 C25 -102.2(3) . . . . ? O22 Rh2 C26 C25 91.7(3) . . . . ? C22 Rh2 C26 C27 54.4(4) . . . . ? C25 Rh2 C26 C27 121.0(5) . . . . ? O21 Rh2 C26 C27 -69.7(5) . . . . ? C21 Rh2 C26 C27 18.8(4) . . . . ? O22 Rh2 C26 C27 -147.3(4) . . . . ? C25 C26 C27 C28 48.5(7) . . . . ? Rh2 C26 C27 C28 -31.9(6) . . . . ? C26 C27 C28 C21 29.6(7) . . . . ? C22 C21 C28 C27 -92.4(6) . . . . ? Rh2 C21 C28 C27 -13.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.603 _refine_diff_density_min -1.205 _refine_diff_density_rms 0.114 data_m275 _database_code_CSD 177301 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H24 F6 O4 P Rh S4' _chemical_formula_weight 560.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 8.8580(18) _cell_length_b 5.9930(12) _cell_length_c 19.061(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.50(3) _cell_angle_gamma 90.00 _cell_volume 1010.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 28.28 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.841 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 1.400 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3089 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 30.51 _reflns_number_total 3089 _reflns_number_gt 2984 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0394P)^2^+0.4578P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(2) _refine_ls_number_reflns 3089 _refine_ls_number_parameters 225 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.07649(2) 0.51994(4) 0.058619(16) 0.01712(7) Uani 1 1 d . . . S2 S -0.08360(10) 0.72064(15) 0.19254(5) 0.01985(16) Uani 1 1 d . . . O20 O 0.0530(3) 0.5916(5) 0.16606(14) 0.0232(5) Uani 1 1 d . . . C21 C 0.0016(5) 0.9381(7) 0.2451(2) 0.0300(8) Uani 1 1 d . . . H21A H 0.0792 0.8759 0.2759 0.045 Uiso 1 1 calc R . . H21B H -0.0738 1.0076 0.2724 0.045 Uiso 1 1 calc R . . H21C H 0.0450 1.0472 0.2151 0.045 Uiso 1 1 calc R . . C22 C -0.1533(5) 0.5506(7) 0.2604(2) 0.0255(7) Uani 1 1 d . . . H22A H -0.2043 0.4233 0.2401 0.038 Uiso 1 1 calc R . . H22B H -0.2227 0.6352 0.2871 0.038 Uiso 1 1 calc R . . H22C H -0.0704 0.5014 0.2907 0.038 Uiso 1 1 calc R . . S3 S -0.13911(9) 0.35122(14) 0.04794(5) 0.01741(15) Uani 1 1 d . . . O30 O -0.2337(3) 0.3596(5) 0.11091(14) 0.0304(6) Uani 1 1 d . . . C31 C -0.1222(6) 0.0651(7) 0.0248(2) 0.0320(9) Uani 1 1 d . . . H31A H -0.0633 -0.0115 0.0608 0.048 Uiso 1 1 calc R . . H31B H -0.0734 0.0532 -0.0190 0.048 Uiso 1 1 calc R . . H31C H -0.2210 -0.0008 0.0202 0.048 Uiso 1 1 calc R . . C32 C -0.2573(4) 0.4429(7) -0.0239(2) 0.0288(8) Uani 1 1 d . . . H32A H -0.3509 0.3621 -0.0245 0.043 Uiso 1 1 calc R . . H32B H -0.2078 0.4167 -0.0670 0.043 Uiso 1 1 calc R . . H32C H -0.2771 0.5995 -0.0191 0.043 Uiso 1 1 calc R . . S4 S 0.13534(9) 0.46293(14) -0.04893(4) 0.01625(15) Uani 1 1 d . . . O40 O 0.0477(3) 0.3067(4) -0.09557(14) 0.0225(5) Uani 1 1 d . . . C41 C 0.1424(5) 0.7235(7) -0.0940(2) 0.0291(8) Uani 1 1 d . . . H41A H 0.1904 0.7032 -0.1378 0.044 Uiso 1 1 calc R . . H41B H 0.1990 0.8291 -0.0656 0.044 Uiso 1 1 calc R . . H41C H 0.0416 0.7784 -0.1030 0.044 Uiso 1 1 calc R . . C42 C 0.3280(4) 0.3811(8) -0.0517(2) 0.0294(8) Uani 1 1 d . . . H42A H 0.3390 0.2304 -0.0352 0.044 Uiso 1 1 calc R . . H42B H 0.3892 0.4783 -0.0223 0.044 Uiso 1 1 calc R . . H42C H 0.3598 0.3904 -0.0991 0.044 Uiso 1 1 calc R . . S5 S 0.34194(10) 0.80371(19) 0.13794(5) 0.0278(2) Uani 1 1 d . . . O50 O 0.2857(3) 0.6829(7) 0.07108(16) 0.0448(10) Uani 1 1 d . . . C51 C 0.5112(6) 0.9280(12) 0.1095(3) 0.0513(15) Uani 1 1 d . . . H51A H 0.5782 0.8136 0.0942 0.077 Uiso 1 1 calc R . . H51B H 0.5593 1.0094 0.1476 0.077 Uiso 1 1 calc R . . H51C H 0.4875 1.0280 0.0712 0.077 Uiso 1 1 calc R . . C52 C 0.4229(6) 0.5950(9) 0.1942(3) 0.0407(10) Uani 1 1 d . . . H52A H 0.3441 0.5039 0.2120 0.061 Uiso 1 1 calc R . . H52B H 0.4783 0.6648 0.2327 0.061 Uiso 1 1 calc R . . H52C H 0.4900 0.5037 0.1683 0.061 Uiso 1 1 calc R . . P1 P 0.56975(10) -0.09308(15) -0.15676(5) 0.01843(17) Uani 1 1 d . . . F1 F 0.5159(3) -0.1025(5) -0.07722(12) 0.0329(5) Uani 1 1 d . . . F2 F 0.6254(3) -0.0814(4) -0.23562(13) 0.0330(5) Uani 1 1 d . . . F3 F 0.5466(4) -0.3540(4) -0.16295(16) 0.0441(7) Uani 1 1 d . . . F4 F 0.5913(3) 0.1687(4) -0.15049(15) 0.0390(6) Uani 1 1 d . . . F5 F 0.7412(3) -0.1307(6) -0.12921(14) 0.0406(7) Uani 1 1 d . . . F6 F 0.3992(3) -0.0508(6) -0.18436(18) 0.0463(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 Rh1 0.01348(10) 0.02488(12) 0.01312(11) -0.00230(11) 0.00177(7) -0.00266(11) S2 0.0206(4) 0.0229(4) 0.0161(4) 0.0006(3) 0.0018(3) -0.0004(3) O20 0.0197(12) 0.0325(15) 0.0176(12) -0.0069(11) 0.0030(9) -0.0005(11) C21 0.035(2) 0.0295(19) 0.0262(19) -0.0058(16) 0.0066(16) -0.0073(16) C22 0.0295(19) 0.0295(18) 0.0181(17) 0.0011(14) 0.0072(14) -0.0015(15) S3 0.0161(3) 0.0193(4) 0.0171(4) -0.0028(3) 0.0038(3) -0.0039(3) O30 0.0249(13) 0.0440(17) 0.0235(13) -0.0133(12) 0.0131(11) -0.0137(12) C31 0.044(2) 0.0191(17) 0.034(2) 0.0001(15) 0.0104(18) -0.0069(16) C32 0.0175(16) 0.037(2) 0.031(2) -0.0018(17) -0.0038(14) 0.0002(15) S4 0.0138(4) 0.0217(4) 0.0134(4) -0.0011(3) 0.0021(3) -0.0009(3) O40 0.0228(12) 0.0264(13) 0.0180(11) -0.0054(10) 0.0001(9) -0.0048(10) C41 0.035(2) 0.0267(18) 0.0264(18) 0.0016(15) 0.0076(16) -0.0028(15) C42 0.0151(15) 0.042(2) 0.031(2) -0.0062(17) 0.0029(13) 0.0051(15) S5 0.0225(4) 0.0415(5) 0.0194(4) -0.0057(4) 0.0011(3) -0.0110(4) O50 0.0263(15) 0.089(3) 0.0193(14) -0.0192(16) 0.0058(11) -0.0311(17) C51 0.034(2) 0.089(4) 0.031(2) -0.004(3) -0.0002(19) -0.040(3) C52 0.036(2) 0.038(2) 0.048(3) -0.005(2) -0.0049(19) -0.0019(19) P1 0.0214(4) 0.0159(4) 0.0183(4) 0.0001(3) 0.0042(3) -0.0001(3) F1 0.0425(14) 0.0341(13) 0.0231(11) 0.0011(10) 0.0144(10) 0.0034(11) F2 0.0436(15) 0.0361(12) 0.0198(12) 0.0023(10) 0.0072(10) 0.0028(12) F3 0.071(2) 0.0175(11) 0.0447(16) -0.0040(11) 0.0138(14) -0.0088(12) F4 0.0532(17) 0.0195(11) 0.0456(15) -0.0015(11) 0.0179(13) -0.0039(11) F5 0.0257(12) 0.066(2) 0.0303(13) 0.0122(13) 0.0014(9) 0.0060(12) F6 0.0219(12) 0.066(2) 0.0504(18) 0.0213(16) -0.0012(12) -0.0008(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 Rh1 O50 2.099(3) . ? Rh1 O20 2.112(3) . ? Rh1 S3 2.1627(9) . ? Rh1 S4 2.1643(10) . ? S2 O20 1.539(3) . ? S2 C22 1.779(4) . ? S2 C21 1.790(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? S3 O30 1.494(3) . ? S3 C32 1.774(4) . ? S3 C31 1.778(4) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? S4 O40 1.486(3) . ? S4 C42 1.779(4) . ? S4 C41 1.785(4) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? S5 O50 1.530(3) . ? S5 C52 1.778(5) . ? S5 C51 1.780(5) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? P1 F3 1.581(3) . ? P1 F4 1.584(3) . ? P1 F6 1.598(3) . ? P1 F5 1.601(3) . ? P1 F2 1.604(3) . ? P1 F1 1.610(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O50 Rh1 O20 85.39(11) . . ? O50 Rh1 S3 178.90(10) . . ? O20 Rh1 S3 93.57(8) . . ? O50 Rh1 S4 86.14(9) . . ? O20 Rh1 S4 171.39(8) . . ? S3 Rh1 S4 94.89(4) . . ? O20 S2 C22 104.67(18) . . ? O20 S2 C21 103.36(19) . . ? C22 S2 C21 99.3(2) . . ? S2 O20 Rh1 122.16(16) . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O30 S3 C32 106.07(19) . . ? O30 S3 C31 106.72(19) . . ? C32 S3 C31 99.2(2) . . ? O30 S3 Rh1 115.64(11) . . ? C32 S3 Rh1 114.62(15) . . ? C31 S3 Rh1 113.00(16) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O40 S4 C42 106.57(18) . . ? O40 S4 C41 106.95(18) . . ? C42 S4 C41 100.0(2) . . ? O40 S4 Rh1 121.66(11) . . ? C42 S4 Rh1 110.04(14) . . ? C41 S4 Rh1 109.44(14) . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O50 S5 C52 106.1(2) . . ? O50 S5 C51 101.1(2) . . ? C52 S5 C51 98.9(3) . . ? S5 O50 Rh1 124.64(17) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? F3 P1 F4 179.46(18) . . ? F3 P1 F6 90.83(19) . . ? F4 P1 F6 88.68(17) . . ? F3 P1 F5 90.20(18) . . ? F4 P1 F5 90.29(17) . . ? F6 P1 F5 178.96(19) . . ? F3 P1 F2 91.01(15) . . ? F4 P1 F2 89.23(14) . . ? F6 P1 F2 90.56(16) . . ? F5 P1 F2 89.27(15) . . ? F3 P1 F1 89.59(15) . . ? F4 P1 F1 90.19(15) . . ? F6 P1 F1 90.04(17) . . ? F5 P1 F1 90.12(15) . . ? F2 P1 F1 179.15(16) . . ? 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 C22 S2 O20 Rh1 128.2(2) . . . . ? C21 S2 O20 Rh1 -128.3(2) . . . . ? O50 Rh1 O20 S2 124.2(2) . . . . ? S3 Rh1 O20 S2 -56.14(19) . . . . ? S4 Rh1 O20 S2 134.5(5) . . . . ? O50 Rh1 S3 O30 24(7) . . . . ? O20 Rh1 S3 O30 5.83(18) . . . . ? S4 Rh1 S3 O30 -175.75(16) . . . . ? O50 Rh1 S3 C32 148(7) . . . . ? O20 Rh1 S3 C32 129.73(18) . . . . ? S4 Rh1 S3 C32 -51.85(16) . . . . ? O50 Rh1 S3 C31 -99(7) . . . . ? O20 Rh1 S3 C31 -117.56(19) . . . . ? S4 Rh1 S3 C31 60.86(17) . . . . ? O50 Rh1 S4 O40 168.27(19) . . . . ? O20 Rh1 S4 O40 158.0(6) . . . . ? S3 Rh1 S4 O40 -11.35(14) . . . . ? O50 Rh1 S4 C42 42.7(2) . . . . ? O20 Rh1 S4 C42 32.5(6) . . . . ? S3 Rh1 S4 C42 -136.91(17) . . . . ? O50 Rh1 S4 C41 -66.22(19) . . . . ? O20 Rh1 S4 C41 -76.5(6) . . . . ? S3 Rh1 S4 C41 114.17(16) . . . . ? C52 S5 O50 Rh1 83.7(3) . . . . ? C51 S5 O50 Rh1 -173.5(3) . . . . ? O20 Rh1 O50 S5 -5.8(3) . . . . ? S3 Rh1 O50 S5 -24(7) . . . . ? S4 Rh1 O50 S5 175.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.772 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.093