# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name M.Block C.Wagner S.Gomez-Ruiz D.Steinborn _publ_contact_author_name 'Dirk Steinborn' _publ_contact_author_email DIRK.STEINBORN@CHEMIE.UNI-HALLE.DE # Attachment 'pub_block_9c_I2T0017.CIF' data_i2t0017 _database_code_depnum_ccdc_archive 'CCDC 759014' #TrackingRef 'pub_block_9c_I2T0017.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H40 N O2 P2 Rh S, C4 H8 O' _chemical_formula_sum 'C41 H48 N O3 P2 Rh S' _chemical_formula_weight 799.71 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Fdd2 _symmetry_space_group_name_Hall 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 30.109(3) _cell_length_b 41.095(4) _cell_length_c 12.580(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 15565(4) _cell_formula_units_Z 16 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 6757 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 30.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6656 _exptl_absorpt_coefficient_mu 0.613 _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 200(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 IPDS2T _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33320 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7652 _reflns_number_gt 7229 _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^)+(0.0325P)^2^+40.2898P] 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 -0.01(3) _refine_ls_number_reflns 7652 _refine_ls_number_parameters 444 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0854 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _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 0.26548(13) 0.16849(9) 0.4380(3) 0.0364(8) Uani 1 1 d . . . C2 C 0.30236(14) 0.15668(11) 0.4932(4) 0.0449(10) Uani 1 1 d . . . H1 H 0.3021 0.1354 0.5185 0.054 Uiso 1 1 calc R . . C3 C 0.33919(15) 0.17598(12) 0.5109(4) 0.0517(11) Uani 1 1 d . . . H2 H 0.3632 0.1678 0.5491 0.062 Uiso 1 1 calc R . . C4 C 0.34043(16) 0.20731(12) 0.4720(4) 0.0546(12) Uani 1 1 d . . . H3 H 0.3654 0.2202 0.4826 0.066 Uiso 1 1 calc R . . C5 C 0.30453(18) 0.21940(11) 0.4173(4) 0.0594(13) Uani 1 1 d . . . H4 H 0.3054 0.2405 0.3905 0.071 Uiso 1 1 calc R . . C6 C 0.26698(15) 0.20029(10) 0.4018(4) 0.0497(11) Uani 1 1 d . . . H6A H 0.2425 0.2090 0.3666 0.060 Uiso 1 1 calc R . . C7 C 0.24013(13) 0.11124(10) 0.3269(3) 0.0374(8) Uani 1 1 d . . . C8 C 0.27624(14) 0.11688(11) 0.2589(3) 0.0437(9) Uani 1 1 d . . . H5 H 0.2908 0.1368 0.2605 0.052 Uiso 1 1 calc R . . C9 C 0.29019(17) 0.09300(12) 0.1898(4) 0.0527(11) Uani 1 1 d . . . H6 H 0.3144 0.0970 0.1459 0.063 Uiso 1 1 calc R . . C10 C 0.26906(19) 0.06330(12) 0.1843(4) 0.0588(13) Uani 1 1 d . . . H7 H 0.2787 0.0475 0.1367 0.071 Uiso 1 1 calc R . . C11 C 0.23319(18) 0.05735(11) 0.2508(4) 0.0559(12) Uani 1 1 d . . . H8 H 0.2188 0.0374 0.2483 0.067 Uiso 1 1 calc R . . C12 C 0.21897(15) 0.08092(10) 0.3203(4) 0.0459(10) Uani 1 1 d . . . H9 H 0.1948 0.0767 0.3641 0.055 Uiso 1 1 calc R . . C13 C 0.21137(13) 0.12125(10) 0.5421(3) 0.0412(9) Uani 1 1 d . . . H10 H 0.2259 0.1002 0.5377 0.049 Uiso 1 1 calc R . . H11 H 0.2258 0.1338 0.5975 0.049 Uiso 1 1 calc R . . C14 C 0.16278(14) 0.11663(10) 0.5694(3) 0.0418(9) Uani 1 1 d . . . H12 H 0.1594 0.1131 0.6452 0.050 Uiso 1 1 calc R . . H13 H 0.1510 0.0979 0.5322 0.050 Uiso 1 1 calc R . . C15 C 0.15034(12) 0.18210(10) 0.6337(3) 0.0410(9) Uani 1 1 d . . . C16 C 0.14602(15) 0.17505(13) 0.7419(3) 0.0486(10) Uani 1 1 d . . . H14 H 0.1322 0.1559 0.7632 0.058 Uiso 1 1 calc R . . C17 C 0.16206(17) 0.19624(15) 0.8166(4) 0.0615(13) Uani 1 1 d . . . H15 H 0.1587 0.1914 0.8883 0.074 Uiso 1 1 calc R . . C18 C 0.18305(18) 0.22463(14) 0.7870(5) 0.0646(14) Uani 1 1 d . . . H16 H 0.1940 0.2388 0.8384 0.077 Uiso 1 1 calc R . . C19 C 0.18769(17) 0.23195(13) 0.6809(4) 0.0596(13) Uani 1 1 d . . . H17 H 0.2018 0.2511 0.6603 0.071 Uiso 1 1 calc R . . C20 C 0.17136(14) 0.21076(10) 0.6047(4) 0.0478(10) Uani 1 1 d . . . H18 H 0.1745 0.2158 0.5331 0.057 Uiso 1 1 calc R . . C21 C 0.07546(14) 0.14312(10) 0.5650(3) 0.0401(9) Uani 1 1 d . . . C22 C 0.05673(15) 0.11518(12) 0.5208(4) 0.0498(10) Uani 1 1 d . . . H19 H 0.0736 0.1026 0.4744 0.060 Uiso 1 1 calc R . . C23 C 0.01354(17) 0.10571(14) 0.5444(4) 0.0588(13) Uani 1 1 d . . . H20 H 0.0018 0.0868 0.5153 0.071 Uiso 1 1 calc R . . C24 C -0.01197(14) 0.12490(14) 0.6120(5) 0.0623(13) Uani 1 1 d . . . H21 H -0.0408 0.1188 0.6289 0.075 Uiso 1 1 calc R . . C25 C 0.00573(16) 0.15298(14) 0.6537(4) 0.0593(13) Uani 1 1 d . . . H22 H -0.0118 0.1661 0.6971 0.071 Uiso 1 1 calc R . . C26 C 0.04918(14) 0.16222(11) 0.6324(4) 0.0482(10) Uani 1 1 d . . . H23 H 0.0608 0.1810 0.6628 0.058 Uiso 1 1 calc R . . C27 C 0.20461(15) 0.18744(14) 0.1610(4) 0.0590(13) Uani 1 1 d . . . H24 H 0.2293 0.1752 0.1881 0.071 Uiso 1 1 calc R . . H26 H 0.2054 0.2091 0.1898 0.071 Uiso 1 1 calc R . . H25 H 0.2065 0.1885 0.0849 0.071 Uiso 1 1 calc R . . C28 C 0.16146(17) 0.13902(12) 0.1389(4) 0.0563(12) Uani 1 1 d . . . H28 H 0.1867 0.1264 0.1604 0.068 Uiso 1 1 calc R . . H27 H 0.1619 0.1418 0.0631 0.068 Uiso 1 1 calc R . . H29 H 0.1347 0.1279 0.1592 0.068 Uiso 1 1 calc R . . C29 C 0.12572(14) 0.19199(12) 0.1504(4) 0.0484(10) Uani 1 1 d . . . H30 H 0.1237 0.1897 0.0738 0.058 Uiso 1 1 calc R . . H31 H 0.1313 0.2147 0.1666 0.058 Uiso 1 1 calc R . . C30 C 0.08269(14) 0.18149(11) 0.2008(3) 0.0413(9) Uani 1 1 d . . . H33 H 0.0754 0.1597 0.1770 0.050 Uiso 1 1 calc R . . H32 H 0.0591 0.1960 0.1781 0.050 Uiso 1 1 calc R . . C31 C 0.08560(13) 0.18184(9) 0.3217(3) 0.0353(8) Uani 1 1 d . . . H34 H 0.0635 0.1667 0.3504 0.042 Uiso 1 1 calc R . . C32 C 0.01911(15) 0.22880(10) 0.3355(3) 0.0470(11) Uani 1 1 d . . . C33 C 0.0102(2) 0.24590(13) 0.2434(4) 0.0708(17) Uani 1 1 d . . . H35 H 0.0333 0.2546 0.2033 0.085 Uiso 1 1 calc R . . C34 C -0.0336(3) 0.24993(18) 0.2113(6) 0.110(4) Uani 1 1 d . . . H36 H -0.0396 0.2611 0.1487 0.132 Uiso 1 1 calc R . . C35 C -0.0673(3) 0.2381(2) 0.2686(9) 0.126(5) Uani 1 1 d . . . H37 H -0.0964 0.2412 0.2463 0.151 Uiso 1 1 calc R . . C36 C -0.05874(18) 0.22113(17) 0.3611(8) 0.098(3) Uani 1 1 d . . . H38 H -0.0823 0.2130 0.4010 0.118 Uiso 1 1 calc R . . C37 C -0.01528(16) 0.21605(13) 0.3956(5) 0.0649(15) Uani 1 1 d . . . H39 H -0.0095 0.2044 0.4574 0.078 Uiso 1 1 calc R . . C38 C 0.1209(4) 0.3195(4) 0.1645(12) 0.173(6) Uani 1 1 d . . . H40 H 0.0889 0.3176 0.1587 0.207 Uiso 1 1 calc R . . H41 H 0.1285 0.3249 0.2373 0.207 Uiso 1 1 calc R . . C39 C 0.1426(7) 0.2900(4) 0.1311(14) 0.248(10) Uani 1 1 d . . . H42 H 0.1563 0.2796 0.1922 0.298 Uiso 1 1 calc R . . H43 H 0.1207 0.2751 0.1022 0.298 Uiso 1 1 calc R . . C40 C 0.1752(4) 0.2962(3) 0.0541(15) 0.193(7) Uani 1 1 d . . . H44 H 0.1691 0.2842 -0.0107 0.231 Uiso 1 1 calc R . . H45 H 0.2044 0.2903 0.0799 0.231 Uiso 1 1 calc R . . C41 C 0.1722(3) 0.3307(2) 0.0361(7) 0.107(3) Uani 1 1 d . . . H46 H 0.1996 0.3412 0.0576 0.129 Uiso 1 1 calc R . . H47 H 0.1674 0.3350 -0.0388 0.129 Uiso 1 1 calc R . . N1 N 0.16299(11) 0.17157(9) 0.1917(3) 0.0394(8) Uani 1 1 d . . . O1 O 0.07594(10) 0.22042(8) 0.4874(2) 0.0498(7) Uani 1 1 d . . . O2 O 0.10238(12) 0.24434(8) 0.3188(3) 0.0608(9) Uani 1 1 d . . . O3 O 0.1369(2) 0.34268(18) 0.0953(8) 0.155(3) Uani 1 1 d . . . P1 P 0.21683(3) 0.14287(2) 0.41272(8) 0.0341(2) Uani 1 1 d . . . P2 P 0.13262(3) 0.15373(3) 0.52916(8) 0.0355(2) Uani 1 1 d . . . S1 S 0.07524(3) 0.22042(2) 0.37255(9) 0.0389(2) Uani 1 1 d . . . Rh Rh 0.151075(9) 0.164807(7) 0.36461(2) 0.03266(7) 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 0.036(2) 0.039(2) 0.0339(19) -0.0004(16) 0.0051(16) 0.0016(16) C2 0.034(2) 0.044(2) 0.056(3) 0.0047(19) -0.0031(19) 0.0007(17) C3 0.034(2) 0.063(3) 0.058(3) 0.001(2) -0.003(2) -0.004(2) C4 0.045(3) 0.052(3) 0.066(3) -0.003(2) -0.005(2) -0.014(2) C5 0.064(3) 0.043(2) 0.072(3) 0.005(2) -0.010(3) -0.010(2) C6 0.045(2) 0.040(2) 0.064(3) 0.0041(19) -0.008(2) -0.0004(18) C7 0.037(2) 0.040(2) 0.0344(19) 0.0013(16) -0.0047(16) 0.0017(17) C8 0.043(2) 0.047(2) 0.041(2) 0.0036(18) 0.0018(18) 0.0013(18) C9 0.050(3) 0.066(3) 0.042(2) -0.004(2) 0.008(2) 0.011(2) C10 0.075(3) 0.052(3) 0.050(3) -0.013(2) -0.003(3) 0.012(2) C11 0.067(3) 0.042(2) 0.058(3) -0.010(2) -0.012(3) -0.001(2) C12 0.044(2) 0.046(2) 0.048(2) -0.0002(19) -0.0044(19) -0.0006(18) C13 0.038(2) 0.045(2) 0.041(2) 0.0072(18) -0.0008(18) 0.0044(17) C14 0.039(2) 0.046(2) 0.040(2) 0.0065(18) 0.0020(18) 0.0011(18) C15 0.0311(18) 0.050(2) 0.042(2) 0.0003(18) 0.0008(17) 0.0061(16) C16 0.042(2) 0.069(3) 0.035(2) 0.003(2) 0.0026(18) 0.006(2) C17 0.058(3) 0.091(4) 0.036(2) -0.008(2) -0.004(2) 0.017(3) C18 0.059(3) 0.071(3) 0.063(3) -0.025(3) -0.013(3) 0.012(3) C19 0.054(3) 0.059(3) 0.066(3) -0.017(2) -0.004(2) -0.004(2) C20 0.043(2) 0.054(2) 0.047(2) -0.001(2) 0.000(2) -0.0019(18) C21 0.039(2) 0.051(2) 0.0304(19) 0.0058(17) -0.0023(17) -0.0026(18) C22 0.043(2) 0.065(3) 0.042(2) 0.002(2) 0.002(2) -0.010(2) C23 0.054(3) 0.080(3) 0.043(3) 0.003(2) 0.000(2) -0.022(3) C24 0.039(2) 0.099(4) 0.049(2) 0.005(3) 0.004(3) -0.019(2) C25 0.037(2) 0.091(4) 0.050(3) -0.003(3) 0.010(2) 0.002(2) C26 0.038(2) 0.061(3) 0.046(3) 0.000(2) 0.0038(19) 0.0014(18) C27 0.042(2) 0.089(4) 0.046(2) 0.014(2) 0.007(2) -0.004(2) C28 0.056(3) 0.067(3) 0.046(3) -0.005(2) 0.004(2) 0.015(2) C29 0.045(2) 0.062(3) 0.038(2) 0.0035(19) -0.0048(18) 0.009(2) C30 0.036(2) 0.049(2) 0.038(2) -0.0017(17) -0.0054(17) 0.0032(18) C31 0.0293(17) 0.041(2) 0.0354(18) -0.0007(16) -0.0025(15) -0.0011(15) C32 0.048(2) 0.042(2) 0.051(3) -0.0114(18) -0.013(2) 0.0130(18) C33 0.104(5) 0.053(3) 0.055(3) -0.014(2) -0.028(3) 0.028(3) C34 0.147(8) 0.087(5) 0.095(5) -0.044(4) -0.085(6) 0.080(6) C35 0.077(5) 0.125(7) 0.176(10) -0.092(7) -0.078(6) 0.069(5) C36 0.042(3) 0.096(4) 0.156(7) -0.061(5) -0.020(5) 0.015(3) C37 0.041(2) 0.067(3) 0.087(4) -0.017(3) -0.007(2) 0.007(2) C38 0.125(9) 0.177(12) 0.216(15) 0.065(11) 0.053(9) -0.019(9) C39 0.37(3) 0.148(12) 0.232(18) 0.089(13) 0.094(19) -0.053(15) C40 0.114(8) 0.133(10) 0.33(2) -0.017(12) 0.027(11) -0.008(7) C41 0.094(6) 0.126(7) 0.101(6) 0.045(5) 0.010(5) 0.005(5) N1 0.0337(17) 0.052(2) 0.0320(17) 0.0032(15) 0.0052(14) 0.0035(15) O1 0.0439(16) 0.0618(19) 0.0436(16) -0.0089(14) -0.0068(14) 0.0127(15) O2 0.069(2) 0.0453(17) 0.068(2) -0.0043(15) 0.0056(18) -0.0187(16) O3 0.118(5) 0.131(5) 0.214(9) 0.049(6) 0.023(6) 0.022(4) P1 0.0280(4) 0.0389(5) 0.0354(5) 0.0020(4) 0.0004(4) 0.0023(4) P2 0.0311(5) 0.0439(5) 0.0313(5) 0.0036(4) 0.0031(4) -0.0001(4) S1 0.0380(4) 0.0399(4) 0.0387(5) -0.0030(4) -0.0027(5) 0.0002(4) Rh 0.02837(12) 0.03876(13) 0.03086(12) 0.00132(13) 0.00099(13) 0.00116(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 C6 1.385(6) . ? C1 C2 1.397(6) . ? C1 P1 1.832(4) . ? C2 C3 1.381(6) . ? C2 H1 0.9300 . ? C3 C4 1.378(7) . ? C3 H2 0.9300 . ? C4 C5 1.374(7) . ? C4 H3 0.9300 . ? C5 C6 1.391(6) . ? C5 H4 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.402(6) . ? C7 C8 1.402(6) . ? C7 P1 1.830(4) . ? C8 C9 1.376(6) . ? C8 H5 0.9300 . ? C9 C10 1.378(7) . ? C9 H6 0.9300 . ? C10 C11 1.388(7) . ? C10 H7 0.9300 . ? C11 C12 1.373(7) . ? C11 H8 0.9300 . ? C12 H9 0.9300 . ? C13 C14 1.515(5) . ? C13 P1 1.861(4) . ? C13 H10 0.9700 . ? C13 H11 0.9700 . ? C14 P2 1.845(4) . ? C14 H12 0.9700 . ? C14 H13 0.9700 . ? C15 C20 1.386(6) . ? C15 C16 1.398(6) . ? C15 P2 1.836(4) . ? C16 C17 1.369(7) . ? C16 H14 0.9300 . ? C17 C18 1.378(8) . ? C17 H15 0.9300 . ? C18 C19 1.375(8) . ? C18 H16 0.9300 . ? C19 C20 1.385(7) . ? C19 H17 0.9300 . ? C20 H18 0.9300 . ? C21 C22 1.395(6) . ? C21 C26 1.400(6) . ? C21 P2 1.832(4) . ? C22 C23 1.390(7) . ? C22 H19 0.9300 . ? C23 C24 1.391(8) . ? C23 H20 0.9300 . ? C24 C25 1.375(8) . ? C24 H21 0.9300 . ? C25 C26 1.388(6) . ? C25 H22 0.9300 . ? C26 H23 0.9300 . ? C27 N1 1.465(6) . ? C27 H24 0.9600 . ? C27 H26 0.9600 . ? C27 H25 0.9600 . ? C28 N1 1.494(6) . ? C28 H28 0.9600 . ? C28 H27 0.9600 . ? C28 H29 0.9600 . ? C29 N1 1.494(5) . ? C29 C30 1.505(6) . ? C29 H30 0.9700 . ? C29 H31 0.9700 . ? C30 C31 1.524(5) . ? C30 H33 0.9700 . ? C30 H32 0.9700 . ? C31 S1 1.738(4) . ? C31 Rh 2.160(4) . ? C31 H34 0.9800 . ? C32 C33 1.382(7) . ? C32 C37 1.384(7) . ? C32 S1 1.786(4) . ? C33 C34 1.390(10) . ? C33 H35 0.9300 . ? C34 C35 1.335(14) . ? C34 H36 0.9300 . ? C35 C36 1.380(14) . ? C35 H37 0.9300 . ? C36 C37 1.394(7) . ? C36 H38 0.9300 . ? C37 H39 0.9300 . ? C38 O3 1.376(13) . ? C38 C39 1.442(19) . ? C38 H40 0.9700 . ? C38 H41 0.9700 . ? C39 C40 1.401(18) . ? C39 H42 0.9700 . ? C39 H43 0.9700 . ? C40 C41 1.435(14) . ? C40 H44 0.9700 . ? C40 H45 0.9700 . ? C41 O3 1.387(10) . ? C41 H46 0.9700 . ? C41 H47 0.9700 . ? N1 Rh 2.222(3) . ? O1 S1 1.444(3) . ? O2 S1 1.446(3) . ? P1 Rh 2.2579(10) . ? P2 Rh 2.1911(11) . ? 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 C6 C1 C2 117.7(4) . . ? C6 C1 P1 120.8(3) . . ? C2 C1 P1 121.5(3) . . ? C3 C2 C1 121.2(4) . . ? C3 C2 H1 119.4 . . ? C1 C2 H1 119.4 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H2 120.0 . . ? C2 C3 H2 120.0 . . ? C5 C4 C3 119.6(4) . . ? C5 C4 H3 120.2 . . ? C3 C4 H3 120.2 . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H4 119.8 . . ? C6 C5 H4 119.8 . . ? C1 C6 C5 120.9(4) . . ? C1 C6 H6A 119.6 . . ? C5 C6 H6A 119.6 . . ? C12 C7 C8 117.6(4) . . ? C12 C7 P1 119.5(3) . . ? C8 C7 P1 122.7(3) . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H5 119.9 . . ? C7 C8 H5 119.9 . . ? C8 C9 C10 121.5(5) . . ? C8 C9 H6 119.3 . . ? C10 C9 H6 119.3 . . ? C9 C10 C11 119.0(4) . . ? C9 C10 H7 120.5 . . ? C11 C10 H7 120.5 . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H8 119.9 . . ? C10 C11 H8 119.9 . . ? C11 C12 C7 121.5(4) . . ? C11 C12 H9 119.3 . . ? C7 C12 H9 119.3 . . ? C14 C13 P1 110.1(3) . . ? C14 C13 H10 109.6 . . ? P1 C13 H10 109.6 . . ? C14 C13 H11 109.6 . . ? P1 C13 H11 109.6 . . ? H10 C13 H11 108.2 . . ? C13 C14 P2 108.0(3) . . ? C13 C14 H12 110.1 . . ? P2 C14 H12 110.1 . . ? C13 C14 H13 110.1 . . ? P2 C14 H13 110.1 . . ? H12 C14 H13 108.4 . . ? C20 C15 C16 118.3(4) . . ? C20 C15 P2 119.0(3) . . ? C16 C15 P2 122.6(3) . . ? C17 C16 C15 120.2(5) . . ? C17 C16 H14 119.9 . . ? C15 C16 H14 119.9 . . ? C16 C17 C18 121.0(5) . . ? C16 C17 H15 119.5 . . ? C18 C17 H15 119.5 . . ? C19 C18 C17 119.6(5) . . ? C19 C18 H16 120.2 . . ? C17 C18 H16 120.2 . . ? C18 C19 C20 119.8(5) . . ? C18 C19 H17 120.1 . . ? C20 C19 H17 120.1 . . ? C19 C20 C15 121.0(5) . . ? C19 C20 H18 119.5 . . ? C15 C20 H18 119.5 . . ? C22 C21 C26 118.3(4) . . ? C22 C21 P2 118.5(3) . . ? C26 C21 P2 123.1(3) . . ? C23 C22 C21 121.6(5) . . ? C23 C22 H19 119.2 . . ? C21 C22 H19 119.2 . . ? C22 C23 C24 119.3(5) . . ? C22 C23 H20 120.4 . . ? C24 C23 H20 120.4 . . ? C25 C24 C23 119.7(4) . . ? C25 C24 H21 120.2 . . ? C23 C24 H21 120.2 . . ? C24 C25 C26 121.4(5) . . ? C24 C25 H22 119.3 . . ? C26 C25 H22 119.3 . . ? C25 C26 C21 119.7(5) . . ? C25 C26 H23 120.1 . . ? C21 C26 H23 120.1 . . ? N1 C27 H24 109.5 . . ? N1 C27 H26 109.5 . . ? H24 C27 H26 109.5 . . ? N1 C27 H25 109.5 . . ? H24 C27 H25 109.5 . . ? H26 C27 H25 109.5 . . ? N1 C28 H28 109.5 . . ? N1 C28 H27 109.5 . . ? H28 C28 H27 109.5 . . ? N1 C28 H29 109.5 . . ? H28 C28 H29 109.5 . . ? H27 C28 H29 109.5 . . ? N1 C29 C30 109.8(4) . . ? N1 C29 H30 109.7 . . ? C30 C29 H30 109.7 . . ? N1 C29 H31 109.7 . . ? C30 C29 H31 109.7 . . ? H30 C29 H31 108.2 . . ? C29 C30 C31 111.6(4) . . ? C29 C30 H33 109.3 . . ? C31 C30 H33 109.3 . . ? C29 C30 H32 109.3 . . ? C31 C30 H32 109.3 . . ? H33 C30 H32 108.0 . . ? C30 C31 S1 111.4(3) . . ? C30 C31 Rh 107.4(3) . . ? S1 C31 Rh 111.57(19) . . ? C30 C31 H34 108.8 . . ? S1 C31 H34 108.8 . . ? Rh C31 H34 108.8 . . ? C33 C32 C37 120.4(5) . . ? C33 C32 S1 120.0(4) . . ? C37 C32 S1 119.5(4) . . ? C32 C33 C34 119.2(7) . . ? C32 C33 H35 120.4 . . ? C34 C33 H35 120.4 . . ? C35 C34 C33 121.4(7) . . ? C35 C34 H36 119.3 . . ? C33 C34 H36 119.3 . . ? C34 C35 C36 119.9(6) . . ? C34 C35 H37 120.1 . . ? C36 C35 H37 120.1 . . ? C35 C36 C37 120.8(8) . . ? C35 C36 H38 119.6 . . ? C37 C36 H38 119.6 . . ? C32 C37 C36 118.4(7) . . ? C32 C37 H39 120.8 . . ? C36 C37 H39 120.8 . . ? O3 C38 C39 103.8(11) . . ? O3 C38 H40 111.0 . . ? C39 C38 H40 111.0 . . ? O3 C38 H41 111.0 . . ? C39 C38 H41 111.0 . . ? H40 C38 H41 109.0 . . ? C40 C39 C38 111.4(11) . . ? C40 C39 H42 109.4 . . ? C38 C39 H42 109.4 . . ? C40 C39 H43 109.4 . . ? C38 C39 H43 109.4 . . ? H42 C39 H43 108.0 . . ? C39 C40 C41 104.2(12) . . ? C39 C40 H44 110.9 . . ? C41 C40 H44 110.9 . . ? C39 C40 H45 110.9 . . ? C41 C40 H45 110.9 . . ? H44 C40 H45 108.9 . . ? O3 C41 C40 108.3(8) . . ? O3 C41 H46 110.0 . . ? C40 C41 H46 110.0 . . ? O3 C41 H47 110.0 . . ? C40 C41 H47 110.0 . . ? H46 C41 H47 108.4 . . ? C27 N1 C28 107.9(4) . . ? C27 N1 C29 107.5(3) . . ? C28 N1 C29 109.0(4) . . ? C27 N1 Rh 116.9(3) . . ? C28 N1 Rh 108.6(3) . . ? C29 N1 Rh 106.8(2) . . ? C38 O3 C41 111.2(9) . . ? C7 P1 C1 101.77(18) . . ? C7 P1 C13 102.17(18) . . ? C1 P1 C13 101.15(19) . . ? C7 P1 Rh 117.48(13) . . ? C1 P1 Rh 121.21(13) . . ? C13 P1 Rh 110.34(13) . . ? C21 P2 C15 104.35(18) . . ? C21 P2 C14 101.42(19) . . ? C15 P2 C14 100.65(19) . . ? C21 P2 Rh 121.35(13) . . ? C15 P2 Rh 118.09(14) . . ? C14 P2 Rh 107.83(14) . . ? O1 S1 O2 117.3(2) . . ? O1 S1 C31 111.43(19) . . ? O2 S1 C31 110.3(2) . . ? O1 S1 C32 105.9(2) . . ? O2 S1 C32 106.4(2) . . ? C31 S1 C32 104.46(19) . . ? C31 Rh P2 94.11(11) . . ? C31 Rh N1 82.09(14) . . ? P2 Rh N1 172.63(10) . . ? C31 Rh P1 175.11(11) . . ? P2 Rh P1 83.46(4) . . ? N1 Rh P1 99.84(9) . . ? 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 C6 C1 C2 C3 -0.2(7) . . . . ? P1 C1 C2 C3 179.2(4) . . . . ? C1 C2 C3 C4 -1.3(7) . . . . ? C2 C3 C4 C5 1.2(8) . . . . ? C3 C4 C5 C6 0.4(8) . . . . ? C2 C1 C6 C5 1.9(7) . . . . ? P1 C1 C6 C5 -177.5(4) . . . . ? C4 C5 C6 C1 -2.0(8) . . . . ? C12 C7 C8 C9 -0.8(6) . . . . ? P1 C7 C8 C9 -174.8(4) . . . . ? C7 C8 C9 C10 0.8(7) . . . . ? C8 C9 C10 C11 -0.6(8) . . . . ? C9 C10 C11 C12 0.5(8) . . . . ? C10 C11 C12 C7 -0.5(7) . . . . ? C8 C7 C12 C11 0.6(6) . . . . ? P1 C7 C12 C11 174.8(4) . . . . ? P1 C13 C14 P2 -38.7(4) . . . . ? C20 C15 C16 C17 0.4(6) . . . . ? P2 C15 C16 C17 176.3(4) . . . . ? C15 C16 C17 C18 -0.6(7) . . . . ? C16 C17 C18 C19 0.5(8) . . . . ? C17 C18 C19 C20 -0.1(8) . . . . ? C18 C19 C20 C15 -0.1(7) . . . . ? C16 C15 C20 C19 0.0(6) . . . . ? P2 C15 C20 C19 -176.1(4) . . . . ? C26 C21 C22 C23 -1.7(7) . . . . ? P2 C21 C22 C23 -179.9(4) . . . . ? C21 C22 C23 C24 1.4(7) . . . . ? C22 C23 C24 C25 0.5(8) . . . . ? C23 C24 C25 C26 -2.0(8) . . . . ? C24 C25 C26 C21 1.6(8) . . . . ? C22 C21 C26 C25 0.2(7) . . . . ? P2 C21 C26 C25 178.4(4) . . . . ? N1 C29 C30 C31 54.4(5) . . . . ? C29 C30 C31 S1 84.2(4) . . . . ? C29 C30 C31 Rh -38.2(4) . . . . ? C37 C32 C33 C34 -0.5(7) . . . . ? S1 C32 C33 C34 174.9(4) . . . . ? C32 C33 C34 C35 1.1(9) . . . . ? C33 C34 C35 C36 -0.7(11) . . . . ? C34 C35 C36 C37 -0.3(11) . . . . ? C33 C32 C37 C36 -0.5(7) . . . . ? S1 C32 C37 C36 -175.8(4) . . . . ? C35 C36 C37 C32 0.9(9) . . . . ? O3 C38 C39 C40 8(2) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 O3 -4.3(17) . . . . ? C30 C29 N1 C27 -166.7(4) . . . . ? C30 C29 N1 C28 76.6(4) . . . . ? C30 C29 N1 Rh -40.5(4) . . . . ? C39 C38 O3 C41 -10.8(17) . . . . ? C40 C41 O3 C38 9.9(14) . . . . ? C12 C7 P1 C1 156.9(3) . . . . ? C8 C7 P1 C1 -29.2(4) . . . . ? C12 C7 P1 C13 52.6(4) . . . . ? C8 C7 P1 C13 -133.5(3) . . . . ? C12 C7 P1 Rh -68.3(3) . . . . ? C8 C7 P1 Rh 105.6(3) . . . . ? C6 C1 P1 C7 115.3(4) . . . . ? C2 C1 P1 C7 -64.1(4) . . . . ? C6 C1 P1 C13 -139.6(4) . . . . ? C2 C1 P1 C13 41.0(4) . . . . ? C6 C1 P1 Rh -17.3(4) . . . . ? C2 C1 P1 Rh 163.2(3) . . . . ? C14 C13 P1 C7 -111.9(3) . . . . ? C14 C13 P1 C1 143.3(3) . . . . ? C14 C13 P1 Rh 13.8(3) . . . . ? C22 C21 P2 C15 -161.5(3) . . . . ? C26 C21 P2 C15 20.4(4) . . . . ? C22 C21 P2 C14 -57.2(4) . . . . ? C26 C21 P2 C14 124.6(4) . . . . ? C22 C21 P2 Rh 62.1(4) . . . . ? C26 C21 P2 Rh -116.1(3) . . . . ? C20 C15 P2 C21 -132.8(3) . . . . ? C16 C15 P2 C21 51.3(4) . . . . ? C20 C15 P2 C14 122.4(3) . . . . ? C16 C15 P2 C14 -53.5(4) . . . . ? C20 C15 P2 Rh 5.4(4) . . . . ? C16 C15 P2 Rh -170.5(3) . . . . ? C13 C14 P2 C21 178.6(3) . . . . ? C13 C14 P2 C15 -74.2(3) . . . . ? C13 C14 P2 Rh 50.1(3) . . . . ? C30 C31 S1 O1 177.3(3) . . . . ? Rh C31 S1 O1 -62.7(2) . . . . ? C30 C31 S1 O2 -50.6(3) . . . . ? Rh C31 S1 O2 69.4(3) . . . . ? C30 C31 S1 C32 63.4(3) . . . . ? Rh C31 S1 C32 -176.6(2) . . . . ? C33 C32 S1 O1 147.8(4) . . . . ? C37 C32 S1 O1 -36.9(4) . . . . ? C33 C32 S1 O2 22.2(4) . . . . ? C37 C32 S1 O2 -162.4(4) . . . . ? C33 C32 S1 C31 -94.5(4) . . . . ? C37 C32 S1 C31 80.9(4) . . . . ? C30 C31 Rh P2 -162.0(3) . . . . ? S1 C31 Rh P2 75.64(19) . . . . ? C30 C31 Rh N1 11.7(3) . . . . ? S1 C31 Rh N1 -110.7(2) . . . . ? C21 P2 Rh C31 27.42(19) . . . . ? C15 P2 Rh C31 -103.44(17) . . . . ? C14 P2 Rh C31 143.50(18) . . . . ? C21 P2 Rh P1 -148.31(17) . . . . ? C15 P2 Rh P1 80.83(14) . . . . ? C14 P2 Rh P1 -32.24(15) . . . . ? C27 N1 Rh C31 135.7(3) . . . . ? C28 N1 Rh C31 -102.0(3) . . . . ? C29 N1 Rh C31 15.4(3) . . . . ? C27 N1 Rh P1 -48.8(3) . . . . ? C28 N1 Rh P1 73.5(3) . . . . ? C29 N1 Rh P1 -169.1(3) . . . . ? C7 P1 Rh P2 129.44(15) . . . . ? C1 P1 Rh P2 -104.82(15) . . . . ? C13 P1 Rh P2 12.93(15) . . . . ? C7 P1 Rh N1 -43.91(18) . . . . ? C1 P1 Rh N1 81.83(18) . . . . ? C13 P1 Rh N1 -160.41(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.597 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.058 # Attachment 'pub_block_10c_archive.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-08-07 at 14:34:09 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\xray\wingx\files\archive.dat # CIF files read : p21c x0562 data_p21c _database_code_depnum_ccdc_archive 'CCDC 759015' #TrackingRef 'pub_block_10c_archive.cif' _audit_creation_date 2008-08-07T14:34:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C47 H45 Cl O2 P3 Rh S' _chemical_formula_weight 905.16 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 21.349(5) _cell_length_b 16.099(5) _cell_length_c 12.008(5) _cell_angle_alpha 90 _cell_angle_beta 94.237(5) _cell_angle_gamma 90 _cell_volume 4116(2) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 5211 _cell_measurement_theta_min 2.6377 _cell_measurement_theta_max 32.4602 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plates _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.686 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0411302467 _diffrn_orient_matrix_ub_12 0.0035726887 _diffrn_orient_matrix_ub_13 0.025399392 _diffrn_orient_matrix_ub_21 -0.0068800231 _diffrn_orient_matrix_ub_22 -0.0425494667 _diffrn_orient_matrix_ub_23 0.0072393825 _diffrn_orient_matrix_ub_31 0.0418505568 _diffrn_orient_matrix_ub_32 -0.0105202911 _diffrn_orient_matrix_ub_33 -0.0202283711 _diffrn_measurement_device_type 'ccd xcalibur s' _diffrn_measurement_method '\w scans and \f scans' _diffrn_reflns_av_R_equivalents 0.1424 _diffrn_reflns_av_unetI/netI 0.1555 _diffrn_reflns_number 65301 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 25.19 _diffrn_reflns_theta_full 25.19 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 7399 _reflns_number_gt 3462 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0090P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7399 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0403 _refine_ls_wR_factor_gt 0.0353 _refine_ls_goodness_of_fit_ref 0.7 _refine_ls_restrained_S_all 0.7 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.409 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 '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' 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.220253(14) 0.022426(17) 0.73275(2) 0.02507(8) Uani 1 1 d . . . Cl1 Cl 0.21801(4) 0.12263(5) 0.58556(7) 0.0350(3) Uani 1 1 d . . . P1 P 0.22058(4) -0.07858(6) 0.85354(7) 0.0245(3) Uani 1 1 d . . . P2 P 0.22244(5) -0.07961(6) 0.60344(8) 0.0280(3) Uani 1 1 d . . . P3 P 0.21187(4) 0.12847(6) 0.86164(7) 0.0248(3) Uani 1 1 d . . . S1 S 0.43535(5) 0.13827(7) 0.73713(9) 0.0482(3) Uani 1 1 d . . . O1 O 0.44597(11) 0.09228(16) 0.6370(2) 0.0715(9) Uani 1 1 d . . . O2 O 0.46254(11) 0.10711(15) 0.8429(2) 0.0601(8) Uani 1 1 d . . . C1 C 0.14480(15) -0.1048(2) 0.9052(2) 0.0228(9) Uani 1 1 d . . . C2 C 0.13444(16) -0.1771(2) 0.9630(2) 0.0278(9) Uani 1 1 d . . . H2 H 0.1679 -0.2153 0.9782 0.033 Uiso 1 1 calc R . . C3 C 0.07581(17) -0.1946(2) 0.9991(3) 0.0347(10) Uani 1 1 d . . . H3 H 0.0696 -0.2443 1.0393 0.042 Uiso 1 1 calc R . . C4 C 0.02672(16) -0.1411(2) 0.9775(3) 0.0339(10) Uani 1 1 d . . . H4 H -0.0132 -0.1528 1.004 0.041 Uiso 1 1 calc R . . C5 C 0.03576(16) -0.0704(2) 0.9170(3) 0.0353(10) Uani 1 1 d . . . H5 H 0.0016 -0.0338 0.8991 0.042 Uiso 1 1 calc R . . C6 C 0.09429(16) -0.05223(19) 0.8820(2) 0.0281(9) Uani 1 1 d . . . H6 H 0.1 -0.0026 0.8412 0.034 Uiso 1 1 calc R . . C7 C 0.27799(16) -0.08235(19) 0.9747(3) 0.0213(9) Uani 1 1 d . . . C8 C 0.26454(16) -0.09724(19) 1.0825(3) 0.0273(10) Uani 1 1 d . . . H8 H 0.2222 -0.1042 1.1001 0.033 Uiso 1 1 calc R . . C9 C 0.31254(18) -0.1022(2) 1.1657(3) 0.0390(11) Uani 1 1 d . . . H9 H 0.3029 -0.1122 1.2405 0.047 Uiso 1 1 calc R . . C10 C 0.37355(18) -0.0930(2) 1.1419(3) 0.0474(12) Uani 1 1 d . . . H10 H 0.4062 -0.098 1.1998 0.057 Uiso 1 1 calc R . . C11 C 0.38805(17) -0.0766(2) 1.0353(3) 0.0482(12) Uani 1 1 d . . . H11 H 0.4305 -0.0691 1.0189 0.058 Uiso 1 1 calc R . . C12 C 0.34041(17) -0.0710(2) 0.9516(3) 0.0321(10) Uani 1 1 d . . . H12 H 0.3503 -0.0592 0.8774 0.039 Uiso 1 1 calc R . . C13 C 0.24069(14) -0.17626(18) 0.7860(2) 0.0278(9) Uani 1 1 d . . . H13A H 0.2865 -0.1791 0.7786 0.033 Uiso 1 1 calc R . . H13B H 0.2284 -0.2242 0.8312 0.033 Uiso 1 1 calc R . . C14 C 0.20555(15) -0.17845(19) 0.6719(3) 0.0328(10) Uani 1 1 d . . . H14A H 0.1599 -0.1844 0.6791 0.039 Uiso 1 1 calc R . . H14B H 0.2199 -0.2258 0.6278 0.039 Uiso 1 1 calc R . . C15 C 0.29596(16) -0.0977(2) 0.5398(3) 0.0304(10) Uani 1 1 d . . . C16 C 0.33008(16) -0.0294(2) 0.5086(2) 0.0386(9) Uani 1 1 d . . . H16 H 0.315 0.0249 0.5224 0.046 Uiso 1 1 calc R . . C17 C 0.38601(17) -0.0388(3) 0.4573(3) 0.0447(11) Uani 1 1 d . . . H17 H 0.4089 0.0086 0.4361 0.054 Uiso 1 1 calc R . . C18 C 0.40776(18) -0.1174(3) 0.4376(3) 0.0459(12) Uani 1 1 d . . . H18 H 0.4459 -0.1244 0.4028 0.055 Uiso 1 1 calc R . . C19 C 0.37463(18) -0.1856(3) 0.4680(3) 0.0495(12) Uani 1 1 d . . . H19 H 0.39 -0.2397 0.4542 0.059 Uiso 1 1 calc R . . C20 C 0.31930(17) -0.1762(2) 0.5184(3) 0.0404(11) Uani 1 1 d . . . H20 H 0.2967 -0.224 0.5388 0.048 Uiso 1 1 calc R . . C21 C 0.16438(17) -0.0778(2) 0.4853(3) 0.0263(10) Uani 1 1 d . . . C22 C 0.17560(17) -0.1080(2) 0.3817(3) 0.0352(11) Uani 1 1 d . . . H22 H 0.2165 -0.1274 0.3688 0.042 Uiso 1 1 calc R . . C23 C 0.12868(19) -0.1111(2) 0.2954(3) 0.0389(11) Uani 1 1 d . . . H23 H 0.1374 -0.1332 0.2249 0.047 Uiso 1 1 calc R . . C24 C 0.07074(18) -0.0825(2) 0.3119(3) 0.0423(11) Uani 1 1 d . . . H24 H 0.0387 -0.0838 0.2526 0.051 Uiso 1 1 calc R . . C25 C 0.05816(17) -0.0519(3) 0.4136(3) 0.0694(15) Uani 1 1 d . . . H25 H 0.0173 -0.032 0.4257 0.083 Uiso 1 1 calc R . . C26 C 0.10513(18) -0.0498(2) 0.4990(3) 0.0608(13) Uani 1 1 d . . . H26 H 0.0959 -0.0281 0.5696 0.073 Uiso 1 1 calc R . . C27 C 0.26598(14) 0.21458(18) 0.8460(2) 0.0295(9) Uani 1 1 d . . . H27A H 0.2519 0.2439 0.7762 0.035 Uiso 1 1 calc R . . H27B H 0.2605 0.2537 0.9082 0.035 Uiso 1 1 calc R . . C28 C 0.33649(14) 0.1990(2) 0.8428(2) 0.0381(10) Uani 1 1 d . . . H28A H 0.3583 0.2531 0.8406 0.046 Uiso 1 1 calc R . . H28B H 0.3519 0.1705 0.9126 0.046 Uiso 1 1 calc R . . C29 C 0.35363(14) 0.1475(2) 0.7446(3) 0.0393(10) Uani 1 1 d . . . H29A H 0.3351 0.1732 0.6749 0.047 Uiso 1 1 calc R . . H29B H 0.3352 0.0913 0.7504 0.047 Uiso 1 1 calc R . . C30 C 0.21709(16) 0.11045(18) 1.0125(3) 0.0243(9) Uani 1 1 d . . . C31 C 0.16398(17) 0.09419(18) 1.0677(3) 0.0341(10) Uani 1 1 d . . . H31 H 0.1244 0.0911 1.0263 0.041 Uiso 1 1 calc R . . C32 C 0.1673(2) 0.0824(2) 1.1811(3) 0.0459(12) Uani 1 1 d . . . H32 H 0.13 0.0724 1.2175 0.055 Uiso 1 1 calc R . . C33 C 0.2235(2) 0.08495(19) 1.2417(3) 0.0502(11) Uani 1 1 d . . . H33 H 0.2254 0.0773 1.3203 0.06 Uiso 1 1 calc R . . C34 C 0.2772(2) 0.0984(2) 1.1901(3) 0.0479(11) Uani 1 1 d . . . H34 H 0.3166 0.0992 1.2321 0.058 Uiso 1 1 calc R . . C35 C 0.27374(17) 0.11096(19) 1.0754(3) 0.0333(10) Uani 1 1 d . . . H35 H 0.3113 0.1201 1.0395 0.04 Uiso 1 1 calc R . . C36 C 0.13823(14) 0.18732(19) 0.8424(3) 0.0229(8) Uani 1 1 d . . . C37 C 0.09737(16) 0.1756(2) 0.7479(3) 0.0315(10) Uani 1 1 d . . . H37 H 0.1051 0.1326 0.6964 0.038 Uiso 1 1 calc R . . C38 C 0.04566(16) 0.2265(2) 0.7289(3) 0.0380(10) Uani 1 1 d . . . H38 H 0.0182 0.2184 0.6639 0.046 Uiso 1 1 calc R . . C39 C 0.03327(16) 0.2880(2) 0.8015(3) 0.0406(10) Uani 1 1 d . . . H39 H -0.0028 0.3221 0.7877 0.049 Uiso 1 1 calc R . . C40 C 0.07335(16) 0.3007(2) 0.8955(3) 0.0370(10) Uani 1 1 d . . . H40 H 0.0652 0.3438 0.9465 0.044 Uiso 1 1 calc R . . C41 C 0.12506(15) 0.2507(2) 0.9146(3) 0.0306(10) Uani 1 1 d . . . H41 H 0.1525 0.2598 0.9794 0.037 Uiso 1 1 calc R . . C42 C 0.46063(16) 0.2411(2) 0.7204(3) 0.0374(10) Uani 1 1 d . . . C43 C 0.49271(18) 0.2815(3) 0.8063(3) 0.0601(13) Uani 1 1 d . . . H43 H 0.5032 0.2538 0.875 0.072 Uiso 1 1 calc R . . C44 C 0.50977(19) 0.3632(3) 0.7922(3) 0.0730(14) Uani 1 1 d . . . H44 H 0.5325 0.3919 0.8514 0.088 Uiso 1 1 calc R . . C45 C 0.49432(19) 0.4032(3) 0.6941(4) 0.0622(13) Uani 1 1 d . . . H45 H 0.5054 0.4599 0.6851 0.075 Uiso 1 1 calc R . . C46 C 0.46311(18) 0.3614(3) 0.6095(3) 0.0631(14) Uani 1 1 d . . . H46 H 0.4526 0.3888 0.5406 0.076 Uiso 1 1 calc R . . C47 C 0.44658(17) 0.2806(3) 0.6220(3) 0.0556(13) Uani 1 1 d . . . H47 H 0.4251 0.2517 0.5616 0.067 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 0.03074(18) 0.02240(16) 0.02126(15) -0.00076(18) -0.00341(12) -0.0009(2) Cl1 0.0429(7) 0.0326(7) 0.0284(6) 0.0075(5) -0.0039(5) -0.0006(5) P1 0.0289(7) 0.0219(7) 0.0222(6) -0.0017(5) -0.0021(5) 0.0000(5) P2 0.0320(7) 0.0291(7) 0.0221(6) -0.0039(5) -0.0024(5) -0.0030(5) P3 0.0258(6) 0.0227(7) 0.0251(6) -0.0004(5) -0.0039(5) -0.0009(5) S1 0.0276(7) 0.0566(8) 0.0601(8) -0.0076(7) 0.0018(6) -0.0023(6) O1 0.0445(19) 0.087(2) 0.085(2) -0.0478(17) 0.0202(16) -0.0059(16) O2 0.0397(18) 0.060(2) 0.077(2) 0.0164(16) -0.0203(15) 0.0026(14) C1 0.026(2) 0.022(2) 0.020(2) -0.0023(17) -0.0032(17) 0.0012(18) C2 0.026(2) 0.029(3) 0.027(2) 0.0006(18) -0.0055(18) -0.0010(19) C3 0.042(3) 0.030(3) 0.030(2) 0.0041(19) -0.008(2) -0.004(2) C4 0.028(2) 0.035(3) 0.038(2) -0.001(2) 0.0016(19) -0.007(2) C5 0.031(3) 0.031(3) 0.042(2) -0.0046(19) -0.006(2) 0.007(2) C6 0.033(2) 0.024(2) 0.027(2) -0.0036(16) -0.0016(19) -0.0038(19) C7 0.024(2) 0.020(2) 0.019(2) 0.0005(17) 0.0028(18) 0.0028(18) C8 0.027(2) 0.023(2) 0.030(2) 0.0007(18) -0.002(2) 0.0016(18) C9 0.039(3) 0.054(3) 0.022(2) 0.0030(19) -0.006(2) 0.005(2) C10 0.034(3) 0.080(4) 0.027(3) -0.002(2) -0.008(2) 0.012(2) C11 0.024(3) 0.072(3) 0.048(3) -0.008(2) -0.001(2) 0.004(2) C12 0.028(3) 0.043(3) 0.026(2) 0.0011(19) 0.006(2) 0.003(2) C13 0.035(2) 0.024(2) 0.025(2) -0.0012(18) 0.0024(19) 0.0022(18) C14 0.037(3) 0.030(3) 0.031(2) -0.0083(19) 0.002(2) -0.0094(19) C15 0.029(3) 0.040(3) 0.021(2) -0.003(2) -0.0115(18) 0.005(2) C16 0.035(2) 0.054(3) 0.027(2) -0.006(2) 0.0033(18) -0.005(2) C17 0.044(3) 0.058(3) 0.032(2) -0.005(2) 0.002(2) -0.014(2) C18 0.029(3) 0.079(4) 0.029(2) -0.009(2) -0.002(2) 0.001(3) C19 0.033(3) 0.063(4) 0.050(3) -0.013(2) -0.007(2) 0.018(3) C20 0.030(3) 0.046(3) 0.044(3) -0.004(2) 0.000(2) 0.003(2) C21 0.030(3) 0.025(2) 0.025(2) -0.0043(18) -0.001(2) -0.006(2) C22 0.035(3) 0.046(3) 0.024(2) -0.002(2) 0.001(2) 0.002(2) C23 0.048(3) 0.047(3) 0.021(2) -0.0067(19) -0.002(2) -0.005(2) C24 0.040(3) 0.050(3) 0.035(3) 0.003(2) -0.013(2) -0.012(2) C25 0.027(3) 0.114(5) 0.064(3) -0.040(3) -0.014(2) 0.020(3) C26 0.037(3) 0.102(4) 0.042(3) -0.037(2) -0.003(2) 0.010(3) C27 0.034(2) 0.028(2) 0.026(2) -0.0002(17) -0.0014(17) -0.0046(19) C28 0.030(2) 0.049(3) 0.036(2) -0.005(2) 0.0052(19) -0.007(2) C29 0.025(2) 0.043(3) 0.049(3) -0.005(2) -0.001(2) -0.006(2) C30 0.031(2) 0.016(2) 0.026(2) -0.0028(16) 0.0025(19) 0.0026(17) C31 0.044(3) 0.027(2) 0.032(2) 0.0022(18) 0.003(2) 0.0066(19) C32 0.068(4) 0.035(3) 0.037(3) 0.005(2) 0.023(3) 0.007(2) C33 0.104(4) 0.026(2) 0.021(3) 0.000(2) 0.006(3) 0.000(3) C34 0.078(4) 0.035(3) 0.027(3) 0.001(2) -0.017(2) -0.007(2) C35 0.042(3) 0.025(2) 0.032(2) 0.0028(18) -0.001(2) -0.0097(19) C36 0.025(2) 0.023(2) 0.020(2) 0.0022(17) 0.0016(17) -0.0031(18) C37 0.032(2) 0.032(3) 0.030(2) 0.0000(18) -0.0023(19) -0.002(2) C38 0.030(3) 0.043(3) 0.040(3) 0.012(2) -0.006(2) -0.004(2) C39 0.027(2) 0.044(3) 0.050(3) 0.017(2) 0.002(2) 0.013(2) C40 0.043(3) 0.030(3) 0.040(3) 0.0030(19) 0.013(2) 0.011(2) C41 0.027(2) 0.034(3) 0.031(2) -0.0010(19) 0.0048(19) -0.004(2) C42 0.022(2) 0.051(3) 0.039(3) -0.003(2) -0.002(2) -0.006(2) C43 0.060(3) 0.073(4) 0.044(3) 0.014(3) -0.021(2) -0.031(3) C44 0.087(4) 0.074(4) 0.053(3) 0.005(3) -0.025(3) -0.039(3) C45 0.053(3) 0.057(3) 0.076(4) 0.012(3) -0.002(3) -0.024(3) C46 0.045(3) 0.086(4) 0.056(3) 0.028(3) -0.009(2) -0.021(3) C47 0.040(3) 0.089(4) 0.037(3) 0.007(3) -0.005(2) -0.019(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 P1 2.1787(12) . ? Rh1 P2 2.2632(12) . ? Rh1 P3 2.3201(11) . ? Rh1 Cl1 2.3909(11) . ? P1 C1 1.825(3) . ? P1 C7 1.832(3) . ? P1 C13 1.835(3) . ? P2 C21 1.814(3) . ? P2 C15 1.819(4) . ? P2 C14 1.839(3) . ? P3 C27 1.823(3) . ? P3 C30 1.830(3) . ? P3 C36 1.835(3) . ? S1 O1 1.444(2) . ? S1 O2 1.446(2) . ? S1 C29 1.760(3) . ? S1 C42 1.757(4) . ? C1 C2 1.382(4) . ? C1 C6 1.383(4) . ? C2 C3 1.383(4) . ? C3 C4 1.366(4) . ? C4 C5 1.372(4) . ? C5 C6 1.378(4) . ? C7 C8 1.368(4) . ? C7 C12 1.393(4) . ? C8 C9 1.380(4) . ? C9 C10 1.362(4) . ? C10 C11 1.366(4) . ? C11 C12 1.379(4) . ? C13 C14 1.513(3) . ? C15 C16 1.386(4) . ? C15 C20 1.390(4) . ? C16 C17 1.392(4) . ? C17 C18 1.374(4) . ? C18 C19 1.370(4) . ? C19 C20 1.375(4) . ? C21 C26 1.364(4) . ? C21 C22 1.374(4) . ? C22 C23 1.388(4) . ? C23 C24 1.348(4) . ? C24 C25 1.363(4) . ? C25 C26 1.381(4) . ? C27 C28 1.529(4) . ? C28 C29 1.508(4) . ? C30 C31 1.380(4) . ? C30 C35 1.378(4) . ? C31 C32 1.371(4) . ? C32 C33 1.357(5) . ? C33 C34 1.359(5) . ? C34 C35 1.388(4) . ? C36 C41 1.381(4) . ? C36 C37 1.392(4) . ? C37 C38 1.380(4) . ? C38 C39 1.358(4) . ? C39 C40 1.380(4) . ? C40 C41 1.373(4) . ? C42 C43 1.361(4) . ? C42 C47 1.356(4) . ? C43 C44 1.379(5) . ? C44 C45 1.362(5) . ? C45 C46 1.352(5) . ? C46 C47 1.359(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Rh1 P2 85.17(4) . . ? P1 Rh1 P3 95.84(4) . . ? P2 Rh1 P3 176.61(4) . . ? P1 Rh1 Cl1 174.09(4) . . ? P2 Rh1 Cl1 89.02(4) . . ? P3 Rh1 Cl1 89.90(4) . . ? C1 P1 C7 106.29(15) . . ? C1 P1 C13 101.19(15) . . ? C7 P1 C13 99.09(15) . . ? C1 P1 Rh1 116.09(12) . . ? C7 P1 Rh1 121.48(12) . . ? C13 P1 Rh1 109.54(10) . . ? C21 P2 C15 103.59(16) . . ? C21 P2 C14 102.60(15) . . ? C15 P2 C14 104.67(17) . . ? C21 P2 Rh1 118.52(13) . . ? C15 P2 Rh1 117.80(13) . . ? C14 P2 Rh1 107.86(11) . . ? C27 P3 C30 103.27(14) . . ? C27 P3 C36 97.92(14) . . ? C30 P3 C36 101.29(14) . . ? C27 P3 Rh1 114.23(10) . . ? C30 P3 Rh1 122.80(10) . . ? C36 P3 Rh1 113.78(11) . . ? O1 S1 O2 118.39(17) . . ? O1 S1 C29 107.64(16) . . ? O2 S1 C29 108.61(15) . . ? O1 S1 C42 108.62(17) . . ? O2 S1 C42 108.70(18) . . ? C29 S1 C42 103.93(17) . . ? C2 C1 C6 117.7(3) . . ? C2 C1 P1 123.0(3) . . ? C6 C1 P1 119.2(3) . . ? C1 C2 C3 120.7(3) . . ? C4 C3 C2 120.8(3) . . ? C3 C4 C5 119.2(3) . . ? C4 C5 C6 120.2(3) . . ? C5 C6 C1 121.3(3) . . ? C8 C7 C12 118.8(3) . . ? C8 C7 P1 125.6(3) . . ? C12 C7 P1 115.6(3) . . ? C7 C8 C9 119.9(3) . . ? C10 C9 C8 120.8(3) . . ? C9 C10 C11 120.3(4) . . ? C10 C11 C12 119.3(4) . . ? C11 C12 C7 120.8(3) . . ? C14 C13 P1 107.7(2) . . ? C13 C14 P2 106.5(2) . . ? C16 C15 C20 117.9(3) . . ? C16 C15 P2 118.3(3) . . ? C20 C15 P2 123.7(3) . . ? C15 C16 C17 121.2(4) . . ? C18 C17 C16 119.2(4) . . ? C19 C18 C17 120.3(4) . . ? C18 C19 C20 120.4(4) . . ? C19 C20 C15 120.9(4) . . ? C26 C21 C22 116.8(3) . . ? C26 C21 P2 119.8(3) . . ? C22 C21 P2 123.2(3) . . ? C21 C22 C23 121.6(3) . . ? C24 C23 C22 119.9(3) . . ? C23 C24 C25 119.9(4) . . ? C24 C25 C26 119.6(4) . . ? C21 C26 C25 122.1(4) . . ? C28 C27 P3 120.7(2) . . ? C29 C28 C27 114.0(3) . . ? C28 C29 S1 112.6(2) . . ? C31 C30 C35 117.2(3) . . ? C31 C30 P3 120.9(3) . . ? C35 C30 P3 121.9(3) . . ? C32 C31 C30 121.2(3) . . ? C33 C32 C31 120.5(4) . . ? C32 C33 C34 120.1(4) . . ? C33 C34 C35 119.4(4) . . ? C30 C35 C34 121.5(3) . . ? C41 C36 C37 117.9(3) . . ? C41 C36 P3 120.9(3) . . ? C37 C36 P3 120.8(3) . . ? C38 C37 C36 120.0(3) . . ? C39 C38 C37 121.2(3) . . ? C38 C39 C40 119.6(4) . . ? C41 C40 C39 119.5(3) . . ? C40 C41 C36 121.8(3) . . ? C43 C42 C47 120.2(4) . . ? C43 C42 S1 120.3(3) . . ? C47 C42 S1 119.5(3) . . ? C42 C43 C44 119.0(4) . . ? C45 C44 C43 120.5(4) . . ? C46 C45 C44 119.3(4) . . ? C45 C46 C47 120.7(4) . . ? C46 C47 C42 120.2(4) . . ? # Attachment 'pub_block_11_i2t0073.cif' data_z:\i2t0073 _database_code_depnum_ccdc_archive 'CCDC 759016' #TrackingRef 'pub_block_11_i2t0073.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H32 O2 P Rh S' _chemical_formula_sum 'C29 H32 O2 P Rh S' _chemical_formula_weight 578.49 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' 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3705(9) _cell_length_b 12.1565(11) _cell_length_c 12.6514(13) _cell_angle_alpha 63.954(7) _cell_angle_beta 78.562(8) _cell_angle_gamma 77.146(7) _cell_volume 1254.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 11836 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 29.62 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8957 _exptl_absorpt_correction_T_max 0.9339 _exptl_absorpt_process_details '(IPDS Software; Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealedX-ray tube,12x0.4mmlong-fine focus' _diffrn_source_voltage 5 _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_reflns_number 17184 _diffrn_reflns_av_R_equivalents 0.0322 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 29.17 _reflns_number_total 6724 _reflns_number_gt 6075 _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^)+(0.0815P)^2^+0.4546P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.042(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6724 _refine_ls_number_parameters 436 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _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 0.6400(3) -0.0436(2) 0.3581(2) 0.0270(5) Uani 1 1 d . . . H1 H 0.585(5) -0.071(4) 0.437(4) 0.045(11) Uiso 1 1 d . . . C2 C 0.7767(3) 0.0044(3) 0.3615(3) 0.0294(5) Uani 1 1 d . . . H2 H 0.825(5) -0.056(4) 0.434(4) 0.042(10) Uiso 1 1 d . . . H3 H 0.849(4) 0.010(3) 0.288(3) 0.031(9) Uiso 1 1 d . . . C3 C 0.7334(3) 0.1324(3) 0.3622(2) 0.0296(5) Uani 1 1 d . . . H5 H 0.671(4) 0.127(3) 0.435(3) 0.033(9) Uiso 1 1 d . . . H4 H 0.823(4) 0.173(3) 0.352(3) 0.031(9) Uiso 1 1 d . . . C4 C 0.7599(3) 0.2610(3) 0.1079(2) 0.0289(5) Uani 1 1 d . . . C5 C 0.8112(3) 0.1724(3) 0.0607(3) 0.0325(6) Uani 1 1 d . . . H6 H 0.769(4) 0.102(3) 0.091(3) 0.030(8) Uiso 1 1 d . . . C6 C 0.9215(4) 0.1941(3) -0.0350(3) 0.0376(6) Uani 1 1 d . . . H7 H 0.954(5) 0.127(4) -0.067(4) 0.043(10) Uiso 1 1 d . . . C7 C 0.9780(4) 0.3044(3) -0.0858(3) 0.0391(6) Uani 1 1 d . . . H8 H 1.046(6) 0.325(5) -0.150(5) 0.065(14) Uiso 1 1 d . . . C8 C 0.9252(4) 0.3936(3) -0.0412(3) 0.0399(7) Uani 1 1 d . . . H9 H 0.960(5) 0.467(4) -0.080(4) 0.048(11) Uiso 1 1 d . . . C9 C 0.8175(3) 0.3717(3) 0.0561(3) 0.0346(6) Uani 1 1 d . . . H10 H 0.783(4) 0.438(4) 0.089(3) 0.038(10) Uiso 1 1 d . . . C10 C 0.5554(3) 0.3716(2) 0.2489(2) 0.0275(5) Uani 1 1 d . . . C11 C 0.5996(3) 0.3965(3) 0.3346(3) 0.0331(6) Uani 1 1 d . . . H11 H 0.656(5) 0.340(4) 0.384(4) 0.039(10) Uiso 1 1 d . . . C12 C 0.5516(4) 0.5104(3) 0.3401(3) 0.0370(6) Uani 1 1 d . . . H12 H 0.580(5) 0.528(4) 0.398(4) 0.050(12) Uiso 1 1 d . . . C13 C 0.4570(4) 0.6000(3) 0.2624(3) 0.0370(6) Uani 1 1 d . . . H13 H 0.420(4) 0.665(4) 0.265(3) 0.036(9) Uiso 1 1 d . . . C14 C 0.4111(4) 0.5758(3) 0.1779(3) 0.0359(6) Uani 1 1 d . . . H14 H 0.355(5) 0.631(4) 0.128(4) 0.042(10) Uiso 1 1 d . . . C15 C 0.4609(3) 0.4629(3) 0.1708(3) 0.0317(5) Uani 1 1 d . . . H15 H 0.423(4) 0.449(3) 0.115(3) 0.022(8) Uiso 1 1 d . . . C16 C 0.8381(3) -0.2714(3) 0.4291(3) 0.0309(5) Uani 1 1 d . . . C17 C 0.9857(4) -0.2665(3) 0.3863(3) 0.0391(6) Uani 1 1 d . . . H16 H 1.011(5) -0.217(4) 0.302(4) 0.047(11) Uiso 1 1 d . . . C18 C 1.0913(4) -0.3383(4) 0.4633(3) 0.0458(7) Uani 1 1 d . . . H17 H 1.190(6) -0.340(5) 0.440(4) 0.062(14) Uiso 1 1 d . . . C19 C 1.0497(4) -0.4130(3) 0.5802(3) 0.0441(7) Uani 1 1 d . . . H18 H 1.114(5) -0.468(4) 0.630(4) 0.055(12) Uiso 1 1 d . . . C20 C 0.9017(4) -0.4160(3) 0.6213(3) 0.0435(7) Uani 1 1 d . . . H19 H 0.873(6) -0.468(5) 0.693(4) 0.062(13) Uiso 1 1 d . . . C21 C 0.7954(4) -0.3460(3) 0.5464(3) 0.0376(6) Uani 1 1 d . . . H20 H 0.695(5) -0.349(4) 0.574(4) 0.045(11) Uiso 1 1 d . . . C22 C 0.3836(3) -0.0274(3) 0.1898(3) 0.0310(5) Uani 1 1 d . . . H21 H 0.467(5) -0.086(4) 0.183(4) 0.045(11) Uiso 1 1 d . . . C23 C 0.3171(3) -0.0377(3) 0.2992(3) 0.0330(6) Uani 1 1 d . . . H22 H 0.355(5) -0.103(4) 0.367(4) 0.043(10) Uiso 1 1 d . . . C24 C 0.1677(3) 0.0303(4) 0.3229(3) 0.0416(7) Uani 1 1 d . . . H23 H 0.153(5) 0.023(4) 0.398(4) 0.053(12) Uiso 1 1 d . . . H24 H 0.088(6) -0.014(5) 0.319(4) 0.063(14) Uiso 1 1 d . . . C25 C 0.1412(3) 0.1682(3) 0.2381(3) 0.0397(7) Uani 1 1 d . . . H25 H 0.091(5) 0.178(4) 0.175(4) 0.054(12) Uiso 1 1 d . . . H26 H 0.069(5) 0.210(4) 0.275(4) 0.053(12) Uiso 1 1 d . . . C26 C 0.2806(3) 0.2268(3) 0.1946(3) 0.0329(5) Uani 1 1 d . . . H27 H 0.274(4) 0.300(3) 0.209(3) 0.028(8) Uiso 1 1 d . . . C27 C 0.3737(3) 0.2338(3) 0.0920(3) 0.0320(5) Uani 1 1 d . . . H28 H 0.432(4) 0.303(3) 0.050(3) 0.030(8) Uiso 1 1 d . . . C28 C 0.3600(4) 0.1778(3) 0.0099(3) 0.0374(6) Uani 1 1 d . . . H30 H 0.293(5) 0.234(4) -0.048(4) 0.047(11) Uiso 1 1 d . . . H29 H 0.455(5) 0.169(4) -0.034(4) 0.043(10) Uiso 1 1 d . . . C29 C 0.3138(4) 0.0491(3) 0.0755(3) 0.0376(6) Uani 1 1 d . . . H31 H 0.210(5) 0.052(4) 0.094(4) 0.038(10) Uiso 1 1 d . . . H32 H 0.344(5) 0.006(4) 0.030(4) 0.043(10) Uiso 1 1 d . . . O1 O 0.5791(3) -0.2503(2) 0.3728(2) 0.0446(5) Uani 1 1 d . . . O2 O 0.7711(3) -0.1475(2) 0.2141(2) 0.0437(5) Uani 1 1 d . . . P P 0.62197(7) 0.22321(6) 0.23879(6) 0.02503(15) Uani 1 1 d . . . S S 0.69869(8) -0.17916(6) 0.33427(6) 0.03162(16) Uani 1 1 d . . . Rh Rh 0.47908(2) 0.092880(18) 0.243950(17) 0.02520(10) 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 0.0233(11) 0.0275(11) 0.0306(12) -0.0125(10) -0.0052(9) -0.0018(9) C2 0.0257(12) 0.0287(12) 0.0353(13) -0.0136(10) -0.0067(10) -0.0032(10) C3 0.0297(13) 0.0305(12) 0.0313(12) -0.0140(10) -0.0071(10) -0.0045(10) C4 0.0254(12) 0.0330(12) 0.0293(12) -0.0142(10) -0.0032(9) -0.0034(10) C5 0.0348(14) 0.0306(13) 0.0305(12) -0.0128(10) -0.0037(11) -0.0016(11) C6 0.0358(15) 0.0412(15) 0.0334(13) -0.0180(12) -0.0032(11) 0.0037(12) C7 0.0307(14) 0.0493(17) 0.0311(13) -0.0143(12) 0.0006(11) -0.0031(13) C8 0.0357(15) 0.0481(17) 0.0359(14) -0.0143(13) -0.0004(12) -0.0160(13) C9 0.0322(14) 0.0380(14) 0.0350(13) -0.0156(11) -0.0024(11) -0.0083(11) C10 0.0258(11) 0.0268(11) 0.0326(12) -0.0143(10) -0.0018(9) -0.0064(9) C11 0.0319(14) 0.0350(14) 0.0363(13) -0.0166(11) -0.0095(11) -0.0035(11) C12 0.0392(16) 0.0380(15) 0.0416(15) -0.0230(13) -0.0049(12) -0.0068(12) C13 0.0367(15) 0.0322(14) 0.0452(16) -0.0207(13) 0.0012(12) -0.0061(12) C14 0.0331(14) 0.0312(13) 0.0398(14) -0.0115(12) -0.0065(12) -0.0024(11) C15 0.0322(13) 0.0313(13) 0.0329(12) -0.0137(11) -0.0063(10) -0.0040(11) C16 0.0302(13) 0.0276(12) 0.0353(13) -0.0142(10) -0.0054(10) -0.0015(10) C17 0.0347(15) 0.0399(15) 0.0391(15) -0.0156(13) -0.0005(12) -0.0038(12) C18 0.0271(14) 0.0527(19) 0.0558(19) -0.0231(16) -0.0041(13) -0.0016(13) C19 0.0366(16) 0.0425(17) 0.0502(18) -0.0165(14) -0.0140(14) 0.0022(13) C20 0.0419(17) 0.0407(16) 0.0389(16) -0.0083(13) -0.0088(13) -0.0026(14) C21 0.0320(14) 0.0367(14) 0.0375(14) -0.0096(12) -0.0050(11) -0.0040(12) C22 0.0308(13) 0.0322(13) 0.0360(13) -0.0167(11) -0.0088(11) -0.0064(11) C23 0.0292(13) 0.0374(14) 0.0358(13) -0.0139(11) -0.0057(11) -0.0127(11) C24 0.0265(14) 0.0556(19) 0.0415(16) -0.0174(14) -0.0005(12) -0.0128(13) C25 0.0246(13) 0.0490(17) 0.0462(17) -0.0214(14) -0.0039(12) -0.0029(12) C26 0.0234(12) 0.0356(14) 0.0413(14) -0.0190(12) -0.0073(10) 0.0020(10) C27 0.0309(13) 0.0315(13) 0.0312(12) -0.0097(10) -0.0105(10) -0.0009(10) C28 0.0427(17) 0.0388(15) 0.0313(13) -0.0138(12) -0.0096(12) -0.0039(13) C29 0.0414(17) 0.0404(15) 0.0388(14) -0.0203(13) -0.0115(12) -0.0066(13) O1 0.0438(13) 0.0319(10) 0.0632(15) -0.0177(10) -0.0208(11) -0.0066(9) O2 0.0522(14) 0.0451(12) 0.0341(11) -0.0213(10) -0.0088(10) 0.0060(11) P 0.0230(3) 0.0266(3) 0.0279(3) -0.0130(2) -0.0043(2) -0.0035(2) S 0.0340(3) 0.0291(3) 0.0358(3) -0.0162(3) -0.0099(3) -0.0015(3) Rh 0.02164(13) 0.02803(13) 0.02852(13) -0.01332(9) -0.00453(8) -0.00387(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.536(4) . ? C1 S 1.754(3) . ? C1 Rh 2.182(3) . ? C1 H1 0.98(4) . ? C2 C3 1.521(4) . ? C2 H2 1.00(4) . ? C2 H3 1.02(4) . ? C3 P 1.835(3) . ? C3 H5 0.97(4) . ? C3 H4 1.03(4) . ? C4 C9 1.393(4) . ? C4 C5 1.403(4) . ? C4 P 1.836(3) . ? C5 C6 1.396(4) . ? C5 H6 0.91(4) . ? C6 C7 1.384(5) . ? C6 H7 1.02(4) . ? C7 C8 1.388(5) . ? C7 H8 0.91(5) . ? C8 C9 1.394(4) . ? C8 H9 0.91(4) . ? C9 H10 1.03(4) . ? C10 C15 1.393(4) . ? C10 C11 1.400(4) . ? C10 P 1.825(3) . ? C11 C12 1.385(4) . ? C11 H11 0.85(4) . ? C12 C13 1.383(5) . ? C12 H12 0.95(5) . ? C13 C14 1.390(5) . ? C13 H13 0.80(4) . ? C14 C15 1.384(4) . ? C14 H14 0.85(4) . ? C15 H15 0.93(3) . ? C16 C17 1.386(4) . ? C16 C21 1.389(4) . ? C16 S 1.786(3) . ? C17 C18 1.393(5) . ? C17 H16 0.98(4) . ? C18 C19 1.383(5) . ? C18 H17 0.92(5) . ? C19 C20 1.384(5) . ? C19 H18 0.90(5) . ? C20 C21 1.380(5) . ? C20 H19 0.88(5) . ? C21 H20 0.94(4) . ? C22 C23 1.365(4) . ? C22 C29 1.519(4) . ? C22 Rh 2.261(3) . ? C22 H21 0.95(4) . ? C23 C24 1.506(5) . ? C23 Rh 2.234(3) . ? C23 H22 0.95(4) . ? C24 C25 1.537(5) . ? C24 H23 0.90(5) . ? C24 H24 1.03(5) . ? C25 C26 1.517(4) . ? C25 H25 0.96(5) . ? C25 H26 0.94(5) . ? C26 C27 1.393(4) . ? C26 Rh 2.173(3) . ? C26 H27 0.98(4) . ? C27 C28 1.508(4) . ? C27 Rh 2.171(3) . ? C27 H28 0.99(4) . ? C28 C29 1.531(5) . ? C28 H30 0.97(4) . ? C28 H29 0.96(4) . ? C29 H31 0.95(4) . ? C29 H32 0.91(4) . ? O1 S 1.444(2) . ? O2 S 1.454(2) . ? P Rh 2.2640(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 C2 C1 S 108.37(18) . . ? C2 C1 Rh 115.97(18) . . ? S C1 Rh 114.92(13) . . ? C2 C1 H1 109(3) . . ? S C1 H1 104(3) . . ? Rh C1 H1 104(3) . . ? C3 C2 C1 110.3(2) . . ? C3 C2 H2 111(2) . . ? C1 C2 H2 109(2) . . ? C3 C2 H3 109(2) . . ? C1 C2 H3 109(2) . . ? H2 C2 H3 109(3) . . ? C2 C3 P 105.15(18) . . ? C2 C3 H5 110(2) . . ? P C3 H5 108(2) . . ? C2 C3 H4 112(2) . . ? P C3 H4 111(2) . . ? H5 C3 H4 111(3) . . ? C9 C4 C5 119.2(3) . . ? C9 C4 P 122.9(2) . . ? C5 C4 P 117.9(2) . . ? C6 C5 C4 120.1(3) . . ? C6 C5 H6 121(2) . . ? C4 C5 H6 119(2) . . ? C7 C6 C5 120.2(3) . . ? C7 C6 H7 123(2) . . ? C5 C6 H7 117(2) . . ? C6 C7 C8 120.0(3) . . ? C6 C7 H8 124(3) . . ? C8 C7 H8 116(3) . . ? C7 C8 C9 120.3(3) . . ? C7 C8 H9 117(3) . . ? C9 C8 H9 122(3) . . ? C4 C9 C8 120.2(3) . . ? C4 C9 H10 121(2) . . ? C8 C9 H10 119(2) . . ? C15 C10 C11 118.6(3) . . ? C15 C10 P 120.7(2) . . ? C11 C10 P 120.7(2) . . ? C12 C11 C10 120.4(3) . . ? C12 C11 H11 121(3) . . ? C10 C11 H11 119(3) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 118(3) . . ? C11 C12 H12 121(3) . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13 125(3) . . ? C14 C13 H13 115(3) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 119(3) . . ? C13 C14 H14 120(3) . . ? C14 C15 C10 120.8(3) . . ? C14 C15 H15 117(2) . . ? C10 C15 H15 122(2) . . ? C17 C16 C21 121.0(3) . . ? C17 C16 S 120.3(2) . . ? C21 C16 S 118.7(2) . . ? C16 C17 C18 118.7(3) . . ? C16 C17 H16 118(3) . . ? C18 C17 H16 123(3) . . ? C19 C18 C17 120.7(3) . . ? C19 C18 H17 117(3) . . ? C17 C18 H17 123(3) . . ? C18 C19 C20 119.7(3) . . ? C18 C19 H18 123(3) . . ? C20 C19 H18 117(3) . . ? C21 C20 C19 120.6(3) . . ? C21 C20 H19 118(3) . . ? C19 C20 H19 121(3) . . ? C20 C21 C16 119.4(3) . . ? C20 C21 H20 120(3) . . ? C16 C21 H20 120(3) . . ? C23 C22 C29 124.6(3) . . ? C23 C22 Rh 71.24(16) . . ? C29 C22 Rh 111.17(19) . . ? C23 C22 H21 120(3) . . ? C29 C22 H21 114(3) . . ? Rh C22 H21 102(3) . . ? C22 C23 C24 124.8(3) . . ? C22 C23 Rh 73.43(17) . . ? C24 C23 Rh 107.3(2) . . ? C22 C23 H22 119(3) . . ? C24 C23 H22 115(3) . . ? Rh C23 H22 101(3) . . ? C23 C24 C25 114.4(3) . . ? C23 C24 H23 110(3) . . ? C25 C24 H23 109(3) . . ? C23 C24 H24 109(3) . . ? C25 C24 H24 110(3) . . ? H23 C24 H24 104(4) . . ? C26 C25 C24 113.1(3) . . ? C26 C25 H25 113(3) . . ? C24 C25 H25 110(3) . . ? C26 C25 H26 112(3) . . ? C24 C25 H26 109(3) . . ? H25 C25 H26 100(4) . . ? C27 C26 C25 125.3(3) . . ? C27 C26 Rh 71.22(16) . . ? C25 C26 Rh 113.1(2) . . ? C27 C26 H27 111(2) . . ? C25 C26 H27 114(2) . . ? Rh C26 H27 115(2) . . ? C26 C27 C28 126.4(3) . . ? C26 C27 Rh 71.37(16) . . ? C28 C27 Rh 109.7(2) . . ? C26 C27 H28 120(2) . . ? C28 C27 H28 110(2) . . ? Rh C27 H28 110(2) . . ? C27 C28 C29 113.0(3) . . ? C27 C28 H30 110(3) . . ? C29 C28 H30 111(3) . . ? C27 C28 H29 108(3) . . ? C29 C28 H29 108(2) . . ? H30 C28 H29 107(3) . . ? C22 C29 C28 112.3(2) . . ? C22 C29 H31 108(2) . . ? C28 C29 H31 113(2) . . ? C22 C29 H32 106(3) . . ? C28 C29 H32 110(3) . . ? H31 C29 H32 107(4) . . ? C10 P C3 104.93(12) . . ? C10 P C4 103.52(12) . . ? C3 P C4 103.35(13) . . ? C10 P Rh 125.72(9) . . ? C3 P Rh 105.41(9) . . ? C4 P Rh 111.71(9) . . ? O1 S O2 118.33(16) . . ? O1 S C1 109.60(14) . . ? O2 S C1 109.21(14) . . ? O1 S C16 106.14(14) . . ? O2 S C16 105.82(14) . . ? C1 S C16 107.11(13) . . ? C27 Rh C26 37.42(11) . . ? C27 Rh C1 163.42(11) . . ? C26 Rh C1 158.40(11) . . ? C27 Rh C23 95.76(11) . . ? C26 Rh C23 80.81(12) . . ? C1 Rh C23 94.24(11) . . ? C27 Rh C22 79.79(11) . . ? C26 Rh C22 86.89(11) . . ? C1 Rh C22 101.27(10) . . ? C23 Rh C22 35.34(11) . . ? C27 Rh P 92.37(8) . . ? C26 Rh P 97.75(8) . . ? C1 Rh P 81.26(7) . . ? C23 Rh P 164.11(8) . . ? C22 Rh P 160.49(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S C1 C2 C3 170.94(19) . . . . ? Rh C1 C2 C3 40.0(3) . . . . ? C1 C2 C3 P -50.6(3) . . . . ? C9 C4 C5 C6 1.7(4) . . . . ? P C4 C5 C6 -176.8(2) . . . . ? C4 C5 C6 C7 -1.7(5) . . . . ? C5 C6 C7 C8 0.1(5) . . . . ? C6 C7 C8 C9 1.4(5) . . . . ? C5 C4 C9 C8 -0.3(4) . . . . ? P C4 C9 C8 178.2(2) . . . . ? C7 C8 C9 C4 -1.3(5) . . . . ? C15 C10 C11 C12 -0.9(4) . . . . ? P C10 C11 C12 178.4(2) . . . . ? C10 C11 C12 C13 1.3(5) . . . . ? C11 C12 C13 C14 -0.5(5) . . . . ? C12 C13 C14 C15 -0.7(5) . . . . ? C13 C14 C15 C10 1.1(5) . . . . ? C11 C10 C15 C14 -0.3(4) . . . . ? P C10 C15 C14 -179.6(2) . . . . ? C21 C16 C17 C18 0.2(5) . . . . ? S C16 C17 C18 179.0(3) . . . . ? C16 C17 C18 C19 -0.1(5) . . . . ? C17 C18 C19 C20 -0.3(6) . . . . ? C18 C19 C20 C21 0.6(6) . . . . ? C19 C20 C21 C16 -0.5(5) . . . . ? C17 C16 C21 C20 0.1(5) . . . . ? S C16 C21 C20 -178.7(3) . . . . ? C29 C22 C23 C24 -3.4(5) . . . . ? Rh C22 C23 C24 99.8(3) . . . . ? C29 C22 C23 Rh -103.2(3) . . . . ? C22 C23 C24 C25 -44.5(4) . . . . ? Rh C23 C24 C25 37.0(3) . . . . ? C23 C24 C25 C26 -31.4(4) . . . . ? C24 C25 C26 C27 91.3(4) . . . . ? C24 C25 C26 Rh 8.6(3) . . . . ? C25 C26 C27 C28 -4.4(5) . . . . ? Rh C26 C27 C28 101.2(3) . . . . ? C25 C26 C27 Rh -105.5(3) . . . . ? C26 C27 C28 C29 -39.6(4) . . . . ? Rh C27 C28 C29 41.4(3) . . . . ? C23 C22 C29 C28 96.3(4) . . . . ? Rh C22 C29 C28 15.1(3) . . . . ? C27 C28 C29 C22 -37.5(4) . . . . ? C15 C10 P C3 -177.3(2) . . . . ? C11 C10 P C3 3.4(3) . . . . ? C15 C10 P C4 74.6(2) . . . . ? C11 C10 P C4 -104.6(2) . . . . ? C15 C10 P Rh -55.3(3) . . . . ? C11 C10 P Rh 125.5(2) . . . . ? C2 C3 P C10 174.62(18) . . . . ? C2 C3 P C4 -77.2(2) . . . . ? C2 C3 P Rh 40.2(2) . . . . ? C9 C4 P C10 14.4(3) . . . . ? C5 C4 P C10 -167.1(2) . . . . ? C9 C4 P C3 -94.8(3) . . . . ? C5 C4 P C3 83.6(2) . . . . ? C9 C4 P Rh 152.3(2) . . . . ? C5 C4 P Rh -29.2(2) . . . . ? C2 C1 S O1 159.19(19) . . . . ? Rh C1 S O1 -69.27(18) . . . . ? C2 C1 S O2 -69.7(2) . . . . ? Rh C1 S O2 61.83(18) . . . . ? C2 C1 S C16 44.5(2) . . . . ? Rh C1 S C16 175.99(14) . . . . ? C17 C16 S O1 147.1(3) . . . . ? C21 C16 S O1 -34.1(3) . . . . ? C17 C16 S O2 20.5(3) . . . . ? C21 C16 S O2 -160.6(2) . . . . ? C17 C16 S C1 -95.9(3) . . . . ? C21 C16 S C1 82.9(3) . . . . ? C28 C27 Rh C26 -123.0(3) . . . . ? C26 C27 Rh C1 -166.5(3) . . . . ? C28 C27 Rh C1 70.6(4) . . . . ? C26 C27 Rh C23 66.67(19) . . . . ? C28 C27 Rh C23 -56.3(2) . . . . ? C26 C27 Rh C22 98.32(19) . . . . ? C28 C27 Rh C22 -24.7(2) . . . . ? C26 C27 Rh P -99.67(17) . . . . ? C28 C27 Rh P 137.3(2) . . . . ? C25 C26 Rh C27 121.2(3) . . . . ? C27 C26 Rh C1 169.6(2) . . . . ? C25 C26 Rh C1 -69.3(4) . . . . ? C27 C26 Rh C23 -112.26(19) . . . . ? C25 C26 Rh C23 8.9(2) . . . . ? C27 C26 Rh C22 -77.23(18) . . . . ? C25 C26 Rh C22 44.0(2) . . . . ? C27 C26 Rh P 83.73(17) . . . . ? C25 C26 Rh P -155.1(2) . . . . ? C2 C1 Rh C27 57.8(4) . . . . ? S C1 Rh C27 -70.0(4) . . . . ? C2 C1 Rh C26 -99.5(3) . . . . ? S C1 Rh C26 132.7(3) . . . . ? C2 C1 Rh C23 -175.1(2) . . . . ? S C1 Rh C23 57.06(16) . . . . ? C2 C1 Rh C22 149.87(19) . . . . ? S C1 Rh C22 22.08(17) . . . . ? C2 C1 Rh P -10.48(18) . . . . ? S C1 Rh P -138.28(14) . . . . ? C22 C23 Rh C27 63.24(19) . . . . ? C24 C23 Rh C27 -58.9(2) . . . . ? C22 C23 Rh C26 97.65(19) . . . . ? C24 C23 Rh C26 -24.4(2) . . . . ? C22 C23 Rh C1 -103.53(19) . . . . ? C24 C23 Rh C1 134.4(2) . . . . ? C24 C23 Rh C22 -122.1(3) . . . . ? C22 C23 Rh P -176.3(2) . . . . ? C24 C23 Rh P 61.6(4) . . . . ? C23 C22 Rh C27 -115.5(2) . . . . ? C29 C22 Rh C27 5.3(2) . . . . ? C23 C22 Rh C26 -78.47(19) . . . . ? C29 C22 Rh C26 42.3(2) . . . . ? C23 C22 Rh C1 81.35(19) . . . . ? C29 C22 Rh C1 -157.9(2) . . . . ? C29 C22 Rh C23 120.8(3) . . . . ? C23 C22 Rh P 176.98(19) . . . . ? C29 C22 Rh P -62.2(4) . . . . ? C10 P Rh C27 57.91(14) . . . . ? C3 P Rh C27 179.73(12) . . . . ? C4 P Rh C27 -68.70(13) . . . . ? C10 P Rh C26 20.71(14) . . . . ? C3 P Rh C26 142.54(13) . . . . ? C4 P Rh C26 -105.89(13) . . . . ? C10 P Rh C1 -137.48(13) . . . . ? C3 P Rh C1 -15.65(12) . . . . ? C4 P Rh C1 95.92(12) . . . . ? C10 P Rh C23 -63.0(3) . . . . ? C3 P Rh C23 58.9(3) . . . . ? C4 P Rh C23 170.4(3) . . . . ? C10 P Rh C22 123.4(3) . . . . ? C3 P Rh C22 -114.7(2) . . . . ? C4 P Rh C22 -3.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.17 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.825 _refine_diff_density_min -1.112 _refine_diff_density_rms 0.112 data_z:\i2t0070 _database_code_depnum_ccdc_archive 'CCDC 759017' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H28 N O2 Rh S' _chemical_formula_sum 'C19 H28 N O2 Rh S' _chemical_formula_weight 437.39 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2943(9) _cell_length_b 17.1678(16) _cell_length_c 17.2075(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3631.9(5) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7793 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 29.61 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 1.067 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8441 _exptl_absorpt_correction_T_max 0.9531 _exptl_absorpt_process_details '(IPDS Software; Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 35 _diffrn_source_power 1.75 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_reflns_number 32256 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4144 _reflns_number_gt 3330 _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^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens refall _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4144 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1000 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.8821(3) -0.04212(17) 0.81604(18) 0.0286(6) Uani 1 1 d . . . H1 H 0.951(4) -0.016(2) 0.837(2) 0.046(11) Uiso 1 1 d . . . C2 C 0.9089(4) -0.1177(2) 0.7727(2) 0.0412(9) Uani 1 1 d . . . H3 H 0.830(3) -0.146(2) 0.763(2) 0.030(10) Uiso 1 1 d . . . H2 H 0.958(4) -0.145(2) 0.798(2) 0.038(10) Uiso 1 1 d . . . C3 C 0.9560(4) -0.0959(2) 0.6942(2) 0.0401(8) Uani 1 1 d . . . H4 H 1.024(4) -0.064(2) 0.701(2) 0.035(10) Uiso 1 1 d . . . H5 H 0.969(4) -0.144(2) 0.663(2) 0.042(10) Uiso 1 1 d . . . C4 C 0.9334(3) -0.0169(2) 0.58102(19) 0.0383(8) Uani 1 1 d . . . H7 H 0.879(3) 0.013(2) 0.550(2) 0.033(9) Uiso 1 1 d . . . H8 H 0.963(3) -0.063(2) 0.549(2) 0.040(10) Uiso 1 1 d . . . H6 H 1.001(4) 0.015(3) 0.594(3) 0.065(14) Uiso 1 1 d . . . C5 C 0.7813(4) -0.0910(2) 0.6281(2) 0.0418(8) Uani 1 1 d . . . H10 H 0.807(4) -0.140(3) 0.606(3) 0.056(13) Uiso 1 1 d . . . H9 H 0.744(4) -0.060(3) 0.587(3) 0.047(11) Uiso 1 1 d . . . H11 H 0.735(4) -0.104(3) 0.671(3) 0.062(14) Uiso 1 1 d . . . C6 C 0.8925(3) -0.14009(17) 0.94590(17) 0.0295(6) Uani 1 1 d . . . C7 C 0.9962(3) -0.12333(19) 0.97195(18) 0.0340(7) Uani 1 1 d . . . H12 H 1.030(3) -0.069(2) 0.973(2) 0.040(10) Uiso 1 1 d . . . C8 C 1.0615(3) -0.1841(2) 0.9988(2) 0.0400(8) Uani 1 1 d . . . H13 H 1.132(4) -0.175(3) 1.018(3) 0.059(14) Uiso 1 1 d . . . C9 C 1.0233(4) -0.2603(2) 0.9991(2) 0.0416(9) Uani 1 1 d . . . H14 H 1.073(4) -0.300(3) 1.017(3) 0.059(13) Uiso 1 1 d . . . C10 C 0.9191(4) -0.2761(2) 0.9726(2) 0.0453(9) Uani 1 1 d . . . H15 H 0.893(4) -0.333(3) 0.973(3) 0.057(13) Uiso 1 1 d . . . C11 C 0.8533(3) -0.2162(2) 0.9458(2) 0.0382(8) Uani 1 1 d . . . H16 H 0.782(4) -0.226(2) 0.927(3) 0.049(12) Uiso 1 1 d . . . C12 C 0.8240(3) 0.14171(17) 0.65670(19) 0.0312(7) Uani 1 1 d . . . H17 H 0.884(4) 0.131(2) 0.622(3) 0.049(12) Uiso 1 1 d . . . C13 C 0.7289(3) 0.10088(19) 0.64431(19) 0.0324(7) Uani 1 1 d . . . H18 H 0.723(3) 0.063(2) 0.603(2) 0.036(10) Uiso 1 1 d . . . C14 C 0.6192(3) 0.1241(3) 0.6750(2) 0.0435(9) Uani 1 1 d . . . H20 H 0.593(4) 0.170(3) 0.647(3) 0.069(15) Uiso 1 1 d . . . H19 H 0.564(5) 0.076(4) 0.670(3) 0.088(18) Uiso 1 1 d . . . C15 C 0.6182(3) 0.1421(2) 0.7626(2) 0.0406(8) Uani 1 1 d . . . H22 H 0.627(4) 0.201(3) 0.771(2) 0.044(11) Uiso 1 1 d . . . H21 H 0.549(4) 0.130(2) 0.785(2) 0.040(10) Uiso 1 1 d . . . C16 C 0.7085(3) 0.10162(19) 0.80733(19) 0.0316(7) Uani 1 1 d . . . H23 H 0.683(3) 0.063(3) 0.843(3) 0.047(12) Uiso 1 1 d . . . C17 C 0.8120(3) 0.13290(18) 0.81855(19) 0.0326(7) Uani 1 1 d . . . H24 H 0.852(4) 0.117(3) 0.869(3) 0.053(12) Uiso 1 1 d . . . C18 C 0.8505(3) 0.2101(2) 0.7859(2) 0.0364(7) Uani 1 1 d . . . H26 H 0.820(3) 0.250(2) 0.812(2) 0.035(10) Uiso 1 1 d . . . H25 H 0.928(4) 0.215(3) 0.797(3) 0.064(14) Uiso 1 1 d . . . C19 C 0.8268(3) 0.21882(19) 0.6990(2) 0.0389(8) Uani 1 1 d . . . H27 H 0.755(4) 0.246(2) 0.691(2) 0.042(11) Uiso 1 1 d . . . H28 H 0.881(3) 0.249(2) 0.674(2) 0.032(9) Uiso 1 1 d . . . N N 0.8775(3) -0.04500(14) 0.65195(15) 0.0306(6) Uani 1 1 d . . . O1 O 0.7074(2) -0.09779(15) 0.88611(15) 0.0406(6) Uani 1 1 d . . . O2 O 0.8165(2) 0.00236(13) 0.95399(13) 0.0388(6) Uani 1 1 d . . . S S 0.81301(7) -0.06394(5) 0.90227(4) 0.02882(18) Uani 1 1 d . . . Rh Rh 0.82029(2) 0.041740(12) 0.734545(13) 0.02486(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0310(18) 0.0285(14) 0.0264(14) 0.0052(11) -0.0002(12) 0.0051(12) C2 0.062(3) 0.0303(16) 0.0316(16) 0.0046(13) 0.0049(16) 0.0162(17) C3 0.049(2) 0.0378(17) 0.0332(16) 0.0038(13) 0.0086(16) 0.0167(17) C4 0.050(2) 0.0385(17) 0.0260(14) 0.0001(13) 0.0126(15) -0.0004(16) C5 0.055(2) 0.0311(16) 0.0391(19) -0.0070(15) 0.0021(17) -0.0123(16) C6 0.0310(18) 0.0334(15) 0.0240(14) 0.0013(11) -0.0008(12) 0.0005(12) C7 0.0367(19) 0.0377(15) 0.0275(15) -0.0004(13) -0.0019(13) 0.0000(14) C8 0.035(2) 0.055(2) 0.0296(15) -0.0034(14) -0.0044(14) 0.0100(16) C9 0.051(3) 0.0429(19) 0.0304(16) 0.0049(14) -0.0024(15) 0.0145(17) C10 0.063(3) 0.0338(17) 0.0392(18) 0.0086(14) -0.0001(18) 0.0013(16) C11 0.041(2) 0.0379(17) 0.0353(17) 0.0085(13) -0.0040(15) -0.0062(15) C12 0.0374(19) 0.0274(14) 0.0287(15) 0.0105(11) 0.0007(14) 0.0014(13) C13 0.0355(19) 0.0350(16) 0.0266(15) 0.0075(12) -0.0071(13) 0.0059(13) C14 0.033(2) 0.054(2) 0.044(2) 0.0076(17) -0.0065(15) 0.0053(16) C15 0.030(2) 0.047(2) 0.0443(19) 0.0061(15) 0.0051(15) 0.0104(15) C16 0.0322(18) 0.0327(15) 0.0298(15) 0.0008(12) 0.0099(13) 0.0091(13) C17 0.0382(19) 0.0292(14) 0.0303(15) -0.0072(12) 0.0006(13) 0.0062(13) C18 0.037(2) 0.0289(15) 0.0430(18) -0.0078(14) 0.0004(15) 0.0005(14) C19 0.042(2) 0.0279(15) 0.046(2) 0.0041(14) 0.0030(17) -0.0016(15) N 0.0396(17) 0.0307(13) 0.0215(12) -0.0018(9) 0.0036(11) 0.0011(11) O1 0.0281(13) 0.0452(13) 0.0486(15) 0.0102(11) -0.0030(10) -0.0049(10) O2 0.0535(17) 0.0357(12) 0.0273(11) -0.0019(9) 0.0037(10) 0.0067(11) S 0.0281(4) 0.0315(4) 0.0269(4) 0.0028(3) 0.0009(3) 0.0004(3) Rh 0.02588(16) 0.02463(14) 0.02406(15) 0.00088(8) 0.00073(9) 0.00091(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.531(4) . ? C1 S 1.751(3) . ? C1 Rh 2.149(3) . ? C1 H1 1.03(5) . ? C2 C3 1.518(5) . ? C2 H3 1.10(4) . ? C2 H2 0.88(4) . ? C3 N 1.491(4) . ? C3 H4 1.00(4) . ? C3 H5 1.00(4) . ? C4 N 1.481(4) . ? C4 H7 1.00(4) . ? C4 H8 1.03(4) . ? C4 H6 1.03(5) . ? C5 N 1.480(5) . ? C5 H10 0.97(5) . ? C5 H9 1.00(5) . ? C5 H11 0.96(5) . ? C6 C7 1.381(5) . ? C6 C11 1.392(5) . ? C6 S 1.797(3) . ? C7 C8 1.396(5) . ? C7 H12 1.02(4) . ? C8 C9 1.390(6) . ? C8 H13 0.94(5) . ? C9 C10 1.386(6) . ? C9 H14 0.96(5) . ? C10 C11 1.387(5) . ? C10 H15 1.02(4) . ? C11 H16 0.95(5) . ? C12 C13 1.380(5) . ? C12 C19 1.511(5) . ? C12 Rh 2.178(3) . ? C12 H17 0.96(5) . ? C13 C14 1.503(5) . ? C13 Rh 2.169(3) . ? C13 H18 0.97(4) . ? C14 C15 1.538(6) . ? C14 H20 0.98(5) . ? C14 H19 1.08(6) . ? C15 C16 1.520(5) . ? C15 H22 1.02(5) . ? C15 H21 0.96(5) . ? C16 C17 1.394(5) . ? C16 Rh 2.124(3) . ? C16 H23 0.95(5) . ? C17 C18 1.514(5) . ? C17 Rh 2.133(3) . ? C17 H24 1.04(5) . ? C18 C19 1.532(5) . ? C18 H26 0.90(4) . ? C18 H25 0.97(5) . ? C19 H27 1.01(4) . ? C19 H28 0.95(4) . ? N Rh 2.176(2) . ? O1 S 1.449(3) . ? O2 S 1.445(2) . ? 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 S 109.6(2) . . ? C2 C1 Rh 109.0(2) . . ? S C1 Rh 121.66(17) . . ? C2 C1 H1 112(2) . . ? S C1 H1 102(2) . . ? Rh C1 H1 103(2) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 H3 108.4(19) . . ? C1 C2 H3 105(2) . . ? C3 C2 H2 108(3) . . ? C1 C2 H2 111(3) . . ? H3 C2 H2 116(3) . . ? N C3 C2 109.3(3) . . ? N C3 H4 106(2) . . ? C2 C3 H4 110(2) . . ? N C3 H5 109(2) . . ? C2 C3 H5 110(2) . . ? H4 C3 H5 113(3) . . ? N C4 H7 107(2) . . ? N C4 H8 110(2) . . ? H7 C4 H8 110(3) . . ? N C4 H6 112(3) . . ? H7 C4 H6 113(3) . . ? H8 C4 H6 104(4) . . ? N C5 H10 108(3) . . ? N C5 H9 106(3) . . ? H10 C5 H9 109(4) . . ? N C5 H11 112(3) . . ? H10 C5 H11 108(4) . . ? H9 C5 H11 113(4) . . ? C7 C6 C11 121.0(3) . . ? C7 C6 S 119.1(2) . . ? C11 C6 S 119.6(3) . . ? C6 C7 C8 118.9(3) . . ? C6 C7 H12 125(2) . . ? C8 C7 H12 116(2) . . ? C9 C8 C7 120.7(4) . . ? C9 C8 H13 118(3) . . ? C7 C8 H13 121(3) . . ? C10 C9 C8 119.7(3) . . ? C10 C9 H14 124(3) . . ? C8 C9 H14 117(3) . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H15 118(3) . . ? C11 C10 H15 122(3) . . ? C10 C11 C6 119.5(4) . . ? C10 C11 H16 121(3) . . ? C6 C11 H16 119(3) . . ? C13 C12 C19 122.6(3) . . ? C13 C12 Rh 71.15(17) . . ? C19 C12 Rh 113.3(2) . . ? C13 C12 H17 117(3) . . ? C19 C12 H17 117(3) . . ? Rh C12 H17 104(3) . . ? C12 C13 C14 124.8(3) . . ? C12 C13 Rh 71.83(18) . . ? C14 C13 Rh 109.7(2) . . ? C12 C13 H18 121(3) . . ? C14 C13 H18 112(2) . . ? Rh C13 H18 104(2) . . ? C13 C14 C15 113.9(3) . . ? C13 C14 H20 109(3) . . ? C15 C14 H20 109(3) . . ? C13 C14 H19 109(3) . . ? C15 C14 H19 104(3) . . ? H20 C14 H19 112(4) . . ? C16 C15 C14 113.5(3) . . ? C16 C15 H22 107(3) . . ? C14 C15 H22 110(2) . . ? C16 C15 H21 111(2) . . ? C14 C15 H21 111(2) . . ? H22 C15 H21 104(3) . . ? C17 C16 C15 124.1(3) . . ? C17 C16 Rh 71.21(18) . . ? C15 C16 Rh 113.3(2) . . ? C17 C16 H23 119(3) . . ? C15 C16 H23 114(3) . . ? Rh C16 H23 105(3) . . ? C16 C17 C18 124.8(3) . . ? C16 C17 Rh 70.55(18) . . ? C18 C17 Rh 112.1(2) . . ? C16 C17 H24 116(3) . . ? C18 C17 H24 113(3) . . ? Rh C17 H24 111(2) . . ? C17 C18 C19 112.8(3) . . ? C17 C18 H26 111(3) . . ? C19 C18 H26 109(3) . . ? C17 C18 H25 108(3) . . ? C19 C18 H25 111(3) . . ? H26 C18 H25 104(4) . . ? C12 C19 C18 112.8(3) . . ? C12 C19 H27 109(2) . . ? C18 C19 H27 110(2) . . ? C12 C19 H28 106(2) . . ? C18 C19 H28 111(2) . . ? H27 C19 H28 108(3) . . ? C5 N C4 108.4(3) . . ? C5 N C3 109.8(3) . . ? C4 N C3 107.0(3) . . ? C5 N Rh 106.7(2) . . ? C4 N Rh 117.7(2) . . ? C3 N Rh 107.00(19) . . ? O2 S O1 117.43(16) . . ? O2 S C1 109.81(15) . . ? O1 S C1 110.98(16) . . ? O2 S C6 107.42(14) . . ? O1 S C6 106.00(15) . . ? C1 S C6 104.24(15) . . ? C16 Rh C17 38.24(14) . . ? C16 Rh C1 99.69(12) . . ? C17 Rh C1 93.80(12) . . ? C16 Rh C13 81.98(13) . . ? C17 Rh C13 96.72(13) . . ? C1 Rh C13 164.61(13) . . ? C16 Rh N 157.76(13) . . ? C17 Rh N 163.83(13) . . ? C1 Rh N 81.56(11) . . ? C13 Rh N 91.17(12) . . ? C16 Rh C12 89.70(13) . . ? C17 Rh C12 80.77(13) . . ? C1 Rh C12 157.24(13) . . ? C13 Rh C12 37.02(13) . . ? N Rh C12 97.52(11) . . ? 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 S C1 C2 C3 173.2(3) . . . . ? Rh C1 C2 C3 37.8(4) . . . . ? C1 C2 C3 N -56.2(4) . . . . ? C11 C6 C7 C8 -0.4(5) . . . . ? S C6 C7 C8 -173.8(3) . . . . ? C6 C7 C8 C9 0.2(5) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C9 C10 C11 0.0(5) . . . . ? C9 C10 C11 C6 -0.1(6) . . . . ? C7 C6 C11 C10 0.3(5) . . . . ? S C6 C11 C10 173.7(3) . . . . ? C19 C12 C13 C14 -4.3(5) . . . . ? Rh C12 C13 C14 101.8(3) . . . . ? C19 C12 C13 Rh -106.1(3) . . . . ? C12 C13 C14 C15 -50.4(5) . . . . ? Rh C13 C14 C15 30.8(4) . . . . ? C13 C14 C15 C16 -24.9(5) . . . . ? C14 C15 C16 C17 88.7(4) . . . . ? C14 C15 C16 Rh 6.3(4) . . . . ? C15 C16 C17 C18 -2.0(5) . . . . ? Rh C16 C17 C18 103.9(3) . . . . ? C15 C16 C17 Rh -105.9(3) . . . . ? C16 C17 C18 C19 -49.3(5) . . . . ? Rh C17 C18 C19 31.7(4) . . . . ? C13 C12 C19 C18 93.9(4) . . . . ? Rh C12 C19 C18 12.1(4) . . . . ? C17 C18 C19 C12 -28.6(4) . . . . ? C2 C3 N C5 -70.1(4) . . . . ? C2 C3 N C4 172.4(3) . . . . ? C2 C3 N Rh 45.4(3) . . . . ? C2 C1 S O2 162.7(3) . . . . ? Rh C1 S O2 -68.5(2) . . . . ? C2 C1 S O1 -65.8(3) . . . . ? Rh C1 S O1 63.0(2) . . . . ? C2 C1 S C6 47.9(3) . . . . ? Rh C1 S C6 176.65(18) . . . . ? C7 C6 S O2 -49.9(3) . . . . ? C11 C6 S O2 136.5(3) . . . . ? C7 C6 S O1 -176.2(3) . . . . ? C11 C6 S O1 10.2(3) . . . . ? C7 C6 S C1 66.6(3) . . . . ? C11 C6 S C1 -107.0(3) . . . . ? C15 C16 Rh C17 119.9(3) . . . . ? C17 C16 Rh C1 83.8(2) . . . . ? C15 C16 Rh C1 -156.3(3) . . . . ? C17 C16 Rh C13 -111.7(2) . . . . ? C15 C16 Rh C13 8.2(3) . . . . ? C17 C16 Rh N 175.2(3) . . . . ? C15 C16 Rh N -65.0(4) . . . . ? C17 C16 Rh C12 -75.4(2) . . . . ? C15 C16 Rh C12 44.5(3) . . . . ? C18 C17 Rh C16 -120.7(3) . . . . ? C16 C17 Rh C1 -100.9(2) . . . . ? C18 C17 Rh C1 138.5(3) . . . . ? C16 C17 Rh C13 67.9(2) . . . . ? C18 C17 Rh C13 -52.8(3) . . . . ? C16 C17 Rh N -173.4(3) . . . . ? C18 C17 Rh N 65.9(5) . . . . ? C16 C17 Rh C12 101.4(2) . . . . ? C18 C17 Rh C12 -19.3(3) . . . . ? C2 C1 Rh C16 146.9(3) . . . . ? S C1 Rh C16 17.9(2) . . . . ? C2 C1 Rh C17 -175.0(3) . . . . ? S C1 Rh C17 56.0(2) . . . . ? C2 C1 Rh C13 51.9(6) . . . . ? S C1 Rh C13 -77.1(5) . . . . ? C2 C1 Rh N -10.6(3) . . . . ? S C1 Rh N -139.6(2) . . . . ? C2 C1 Rh C12 -100.0(4) . . . . ? S C1 Rh C12 131.1(3) . . . . ? C12 C13 Rh C16 100.3(2) . . . . ? C14 C13 Rh C16 -21.1(3) . . . . ? C12 C13 Rh C17 64.9(2) . . . . ? C14 C13 Rh C17 -56.5(3) . . . . ? C12 C13 Rh C1 -162.4(4) . . . . ? C14 C13 Rh C1 76.2(6) . . . . ? C12 C13 Rh N -101.0(2) . . . . ? C14 C13 Rh N 137.6(3) . . . . ? C14 C13 Rh C12 -121.4(3) . . . . ? C5 N Rh C16 4.0(4) . . . . ? C4 N Rh C16 126.1(3) . . . . ? C3 N Rh C16 -113.5(3) . . . . ? C5 N Rh C17 173.2(4) . . . . ? C4 N Rh C17 -64.7(5) . . . . ? C3 N Rh C17 55.7(5) . . . . ? C5 N Rh C1 99.0(2) . . . . ? C4 N Rh C1 -139.0(3) . . . . ? C3 N Rh C1 -18.5(2) . . . . ? C5 N Rh C13 -67.4(2) . . . . ? C4 N Rh C13 54.7(3) . . . . ? C3 N Rh C13 175.1(2) . . . . ? C5 N Rh C12 -104.0(2) . . . . ? C4 N Rh C12 18.1(3) . . . . ? C3 N Rh C12 138.5(2) . . . . ? C13 C12 Rh C16 -77.0(2) . . . . ? C19 C12 Rh C16 41.2(3) . . . . ? C13 C12 Rh C17 -114.4(2) . . . . ? C19 C12 Rh C17 3.9(3) . . . . ? C13 C12 Rh C1 168.0(3) . . . . ? C19 C12 Rh C1 -73.8(4) . . . . ? C19 C12 Rh C13 118.2(4) . . . . ? C13 C12 Rh N 81.9(2) . . . . ? C19 C12 Rh N -159.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.709 _refine_diff_density_min -0.830 _refine_diff_density_rms 0.107 #END===================================================================== #Prof. Dr. Dirk Steinborn #Martin-Luther-Universit\"at Halle-Wittenberg #Institut f\"ur Chemie -- Anorganische Chemie #Kurt-Mothes-Stra\&se 2 #06120 Halle #Deutschland