# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1157 data_4 _publ_author_name ; H. Werner, M. Bosch, M.E. Schneider, C. Hahn, F. Kukla, M. Manger, B. Windmueller, B. Weberndoerfer, M. Laubender ; _publ_author_address ; Prof. Dr. Helmut Werner Institut f\"ur Anorganische Chemie Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Deutschland ; _publ_contact_author ; Prof. Dr. Helmut Werner Institut f\"ur Anorganische Chemie Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Deutschland ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4605' _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_requested_journal 'J. Chem. Soc.,Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "J. Chem. Soc.,Dalton Trans." ; _publ_section_title ; "Preparation, molecular structure and reactivity of mono- and dinuclear sulfonato rhodium(I) complexes" ; _publ_section_abstract ; The reaction of [Rh(C3H3)(PPri3)2] 1 or [Rh(CH2C6H5)(PPri3)2] 2 with an equimolar amount of RSO3H (R = Me, p-Tol, CF3, F, Camph) led to the formation of the monomeric sulfonato rhodium(I) complexes [Rh{h2-O2S(O)R}(PPri3)3] 3-7 in excellent yield. An alternative route for the preparation of 4 (R = p-Tol) and 5 (R = CF3) is based on the reaction of PPri3 with the dinuclear compounds [{Rh(C8H14)2(m-O2S(O)R)}2] 11,12, which were obtained either from [{Rh(C8H14)2(m-Cl)}2] 8 or [{Rh(C8H14)2(m-OH)}2] 9 as starting materials. Compounds 3-7 react smoothly with hydrogen by oxidative addition to give the dihydrido rhodium(III) complexes [RhH2{h2-O2S(O)R}(PPri3)2] 13-17. Moreover, on treatment of 3-6 with CO and C2H4 the chelating bond of the sulfonato ligand is partially opened and the carbonyl and ethene complexes trans-[Rh{(1- OS(O)2R}(L)(PPri3)2] (L = CO 18-21; C2H4 22-25) are formed. The bis(stibine) rhodium(I) derivative trans-[Rh{(1-OS(O)2CF3}(C2H4)(SbPri3)2] 28 is obtained from [{Rh(C2H4)2((-O2S(O)CF3)}2] 27 and SbPri3. Reaction of the compounds [Rh{(2-O2S(O)CF3}(olefin)(PPri3)] (olefin = C8H14 29; C2H4 30) with benzene led to the displacement of the sulfonato ligand and to the formation of the halfsandwich-type complexes [{(6-C6H6)Rh(olefin)(PPri3)]CF3SO3 31, 32 containing a rather labile benzene-rhodium bond. The preparation of the vinylidene complex trans-[Rh{(1-OS(O)2p-Tol}(=C=CHPh)(PPri3)2] 33 is also described and the crystal and molecular structures of compounds 4, 29 and 31 have been determined. The four-coordinate sulfonato complexes 3-6 are active catalysts in the C-C coupling reaction of ethene and diphenyldiazomethane. Besides the three isomeric 1:1 adducts of C2H4 and CPh2 (34a-c), quite unexpectedly also the 2:1 adduct 3.3-diphenyl-1-pentene 34d is formed. ; _publ_section_exptl_prep ; Crystals growm from acetone at 8_C. ; _publ_section_exptl_refinement ; "Bemerkungen zur Verfeinerung" ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C25 H49 O3 P2 Rh S' _chemical_formula_weight 594.55 _chemical_melting_point 80_C _chemical_compound_source ? 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' -1.2870 0.9190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 14 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 10.498(4) _cell_length_b 14.104(3) _cell_length_c 20.276(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.89(2) _cell_angle_gamma 90.00 _cell_volume 2998.2(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 10 _cell_measurement_theta_max 14 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.580 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method ? _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.97 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method 'Omega/Theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -0.03 _diffrn_reflns_number 4422 _diffrn_reflns_av_R_equivalents 0.0127 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 22.97 _reflns_number_total 4156 _reflns_number_observed 3517 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CAD4 (Enraf-Nonius)' _computing_data_reduction 'BEGIN (SDP)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor(obs) 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 w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+1.1143P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4156 _refine_ls_number_parameters 302 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_obs 0.0266 _refine_ls_wR_factor_all 0.0717 _refine_ls_wR_factor_obs 0.0666 _refine_ls_goodness_of_fit_all 1.081 _refine_ls_goodness_of_fit_obs 1.099 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.099 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh Rh 0.78444(2) 0.19072(2) 0.132841(10) 0.04076(10) Uani 1 d . . P1 P 0.72933(7) 0.21041(6) 0.02727(4) 0.0457(2) Uani 1 d . . P2 P 0.94494(8) 0.28970(6) 0.15550(4) 0.0465(2) Uani 1 d . . S S 0.66999(8) 0.06867(6) 0.21863(4) 0.0511(2) Uani 1 d . . O1 O 0.6346(2) 0.0832(2) 0.14797(10) 0.0579(6) Uani 1 d . . O2 O 0.7848(2) 0.1268(2) 0.23324(10) 0.0551(5) Uani 1 d . . O3 O 0.6825(2) -0.0283(2) 0.23835(13) 0.0737(7) Uani 1 d . . C1 C 0.5726(3) 0.2706(3) 0.0140(2) 0.0616(9) Uani 1 d . . H1 H 0.5481(3) 0.2668(3) -0.0332(2) 0.074 Uiso 1 calc R . C2 C 0.6918(3) 0.0877(2) -0.0028(2) 0.0626(9) Uani 1 d . . H2 H 0.6229(3) 0.0662(2) 0.0245(2) 0.075 Uiso 1 calc R . C3 C 0.8283(3) 0.2700(3) -0.0336(2) 0.0633(9) Uani 1 d . . H3 H 0.8542(3) 0.3303(3) -0.0131(2) 0.076 Uiso 1 calc R . C4 C 1.0038(3) 0.3843(3) 0.1000(2) 0.0634(9) Uani 1 d . . H4 H 1.0056(3) 0.3545(3) 0.0563(2) 0.076 Uiso 1 calc R . C5 C 1.0944(3) 0.2252(3) 0.1795(2) 0.0673(10) Uani 1 d . . H5 H 1.1586(3) 0.2725(3) 0.1933(2) 0.081 Uiso 1 calc R . C6 C 0.9039(4) 0.3459(3) 0.2348(2) 0.0622(9) Uani 1 d . . H6 H 0.8882(4) 0.2919(3) 0.2636(2) 0.075 Uiso 1 calc R . C7 C 0.4675(4) 0.2236(4) 0.0516(2) 0.0915(14) Uani 1 d . . H7A H 0.4542(22) 0.1601(9) 0.0355(11) 0.137 Uiso 1 calc R . H7B H 0.3900(9) 0.2592(13) 0.0451(13) 0.137 Uiso 1 calc R . H7C H 0.4922(14) 0.2217(21) 0.0978(3) 0.137 Uiso 1 calc R . C8 C 0.5812(4) 0.3755(3) 0.0325(2) 0.0976(15) Uani 1 d . . H8A H 0.6441(23) 0.4059(6) 0.0070(12) 0.146 Uiso 1 calc R . H8B H 0.6051(31) 0.3815(3) 0.0787(4) 0.146 Uiso 1 calc R . H8C H 0.4998(9) 0.4051(6) 0.0235(16) 0.146 Uiso 1 calc R . C9 C 0.8001(4) 0.0176(3) 0.0122(2) 0.0918(13) Uani 1 d . . H9A H 0.8321(21) 0.0257(16) 0.0571(5) 0.138 Uiso 1 calc R . H9B H 0.8675(14) 0.0289(15) -0.0171(11) 0.138 Uiso 1 calc R . H9C H 0.7690(8) -0.0460(3) 0.0062(16) 0.138 Uiso 1 calc R . C10 C 0.6370(5) 0.0779(3) -0.0740(2) 0.0914(14) Uani 1 d . . H10A H 0.5718(22) 0.1247(15) -0.0823(5) 0.137 Uiso 1 calc R . H10B H 0.6012(28) 0.0157(9) -0.0803(5) 0.137 Uiso 1 calc R . H10C H 0.7039(8) 0.0870(23) -0.1040(2) 0.137 Uiso 1 calc R . C11 C 0.7642(5) 0.2964(3) -0.1006(2) 0.0911(14) Uani 1 d . . H11A H 0.6904(19) 0.3347(20) -0.0940(2) 0.137 Uiso 1 calc R . H11B H 0.7390(28) 0.2398(3) -0.1240(7) 0.137 Uiso 1 calc R . H11C H 0.8232(11) 0.3315(21) -0.1259(7) 0.137 Uiso 1 calc R . C12 C 0.9518(4) 0.2165(4) -0.0431(2) 0.0965(15) Uani 1 d . . H12A H 0.9872(17) 0.1956(21) -0.0010(3) 0.145 Uiso 1 calc R . H12B H 1.0114(12) 0.2576(8) -0.0633(15) 0.145 Uiso 1 calc R . H12C H 0.9348(6) 0.1625(14) -0.0711(14) 0.145 Uiso 1 calc R . C13 C 0.9107(4) 0.4661(3) 0.0910(2) 0.0856(12) Uani 1 d . . H13A H 0.8256(5) 0.4418(3) 0.0845(15) 0.128 Uiso 1 calc R . H13B H 0.9318(18) 0.5029(13) 0.0533(9) 0.128 Uiso 1 calc R . H13C H 0.9158(21) 0.5055(12) 0.1297(6) 0.128 Uiso 1 calc R . C14 C 1.1396(4) 0.4222(4) 0.1143(2) 0.099(2) Uani 1 d . . H14A H 1.1991(5) 0.3705(5) 0.1144(17) 0.148 Uiso 1 calc R . H14B H 1.1445(9) 0.4528(21) 0.1566(8) 0.148 Uiso 1 calc R . H14C H 1.1600(13) 0.4670(19) 0.0808(10) 0.148 Uiso 1 calc R . C15 C 1.1443(4) 0.1719(4) 0.1205(3) 0.115(2) Uani 1 d . . H15A H 1.1569(37) 0.2156(6) 0.0852(8) 0.173 Uiso 1 calc R . H15B H 1.0835(19) 0.1245(19) 0.1060(13) 0.173 Uiso 1 calc R . H15C H 1.2239(20) 0.1420(25) 0.1333(6) 0.173 Uiso 1 calc R . C16 C 1.0794(4) 0.1578(3) 0.2372(2) 0.0931(15) Uani 1 d . . H16A H 1.0538(29) 0.1929(4) 0.2749(5) 0.140 Uiso 1 calc R . H16B H 1.1593(9) 0.1268(17) 0.2478(10) 0.140 Uiso 1 calc R . H16C H 1.0157(22) 0.1111(14) 0.2254(6) 0.140 Uiso 1 calc R . C17 C 0.7773(4) 0.3984(3) 0.2307(2) 0.0716(10) Uani 1 d . . H17A H 0.7149(7) 0.3612(9) 0.2059(11) 0.107 Uiso 1 calc R . H17B H 0.7877(7) 0.4583(8) 0.2091(12) 0.107 Uiso 1 calc R . H17C H 0.7491(13) 0.4089(17) 0.2744(2) 0.107 Uiso 1 calc R . C18 C 1.0085(4) 0.4005(3) 0.2720(2) 0.0853(12) Uani 1 d . . H18A H 1.0819(11) 0.3605(7) 0.2792(13) 0.128 Uiso 1 calc R . H18B H 0.9789(11) 0.4207(19) 0.3138(7) 0.128 Uiso 1 calc R . H18C H 1.0311(21) 0.4550(12) 0.2467(7) 0.128 Uiso 1 calc R . C19 C 0.5490(3) 0.1189(2) 0.26455(14) 0.0488(7) Uani 1 d . . C20 C 0.5120(4) 0.2112(2) 0.2538(2) 0.0646(9) Uani 1 d . . H20 H 0.5460(4) 0.2458(2) 0.2198(2) 0.077 Uiso 1 calc R . C21 C 0.4248(4) 0.2525(3) 0.2931(2) 0.0780(11) Uani 1 d . . H21 H 0.4004(4) 0.3151(3) 0.2855(2) 0.094 Uiso 1 calc R . C22 C 0.3727(3) 0.2028(4) 0.3438(2) 0.0777(12) Uani 1 d . . C23 C 0.4095(4) 0.1103(4) 0.3535(2) 0.0789(11) Uani 1 d . . H23 H 0.3747(4) 0.0756(4) 0.3872(2) 0.095 Uiso 1 calc R . C24 C 0.4968(3) 0.0675(3) 0.3145(2) 0.0636(9) Uani 1 d . . H24 H 0.5204(3) 0.0046(3) 0.3218(2) 0.076 Uiso 1 calc R . C25 C 0.2780(4) 0.2496(5) 0.3870(2) 0.121(2) Uani 1 d . . H25A H 0.1933(5) 0.2293(22) 0.3736(13) 0.181 Uiso 1 calc R . H25B H 0.2839(26) 0.3172(5) 0.3826(15) 0.181 Uiso 1 calc R . H25C H 0.2965(24) 0.2321(23) 0.4322(3) 0.181 Uiso 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 Rh 0.04180(15) 0.04743(15) 0.03306(14) -0.00322(10) 0.00205(9) -0.00455(11) P1 0.0475(4) 0.0549(5) 0.0347(4) -0.0045(3) 0.0023(3) -0.0024(4) P2 0.0481(4) 0.0491(5) 0.0420(4) -0.0045(3) 0.0001(3) -0.0055(4) S 0.0555(5) 0.0527(5) 0.0452(4) 0.0039(4) 0.0030(3) -0.0061(4) O1 0.0618(13) 0.0713(15) 0.0405(12) -0.0037(11) 0.0007(10) -0.0203(11) O2 0.0516(12) 0.0723(15) 0.0410(11) 0.0053(10) -0.0018(9) -0.0102(11) O3 0.087(2) 0.0522(14) 0.082(2) 0.0090(12) 0.0091(14) 0.0042(12) C1 0.058(2) 0.079(2) 0.048(2) 0.002(2) -0.004(2) 0.009(2) C2 0.078(2) 0.062(2) 0.048(2) -0.014(2) 0.001(2) -0.009(2) C3 0.072(2) 0.079(2) 0.039(2) -0.001(2) 0.009(2) -0.017(2) C4 0.072(2) 0.068(2) 0.050(2) -0.003(2) 0.006(2) -0.023(2) C5 0.049(2) 0.067(2) 0.085(3) -0.012(2) -0.010(2) -0.004(2) C6 0.083(2) 0.059(2) 0.044(2) -0.008(2) -0.001(2) -0.009(2) C7 0.052(2) 0.146(4) 0.076(3) 0.018(3) 0.008(2) 0.015(2) C8 0.103(3) 0.083(3) 0.105(3) -0.015(3) -0.018(3) 0.032(3) C9 0.118(4) 0.069(3) 0.088(3) -0.025(2) -0.002(3) 0.016(3) C10 0.130(4) 0.089(3) 0.053(2) -0.018(2) -0.010(2) -0.029(3) C11 0.112(3) 0.116(4) 0.045(2) 0.017(2) 0.001(2) -0.030(3) C12 0.074(3) 0.140(4) 0.078(3) -0.018(3) 0.034(2) -0.014(3) C13 0.125(4) 0.063(2) 0.070(3) 0.012(2) 0.014(2) -0.012(2) C14 0.097(3) 0.121(4) 0.078(3) 0.010(3) 0.002(2) -0.056(3) C15 0.063(3) 0.137(4) 0.144(5) -0.050(4) -0.001(3) 0.031(3) C16 0.069(3) 0.065(2) 0.142(4) 0.023(3) -0.026(3) 0.001(2) C17 0.084(3) 0.068(2) 0.064(2) -0.017(2) 0.017(2) -0.002(2) C18 0.113(3) 0.073(3) 0.068(2) -0.020(2) -0.016(2) -0.012(2) C19 0.050(2) 0.054(2) 0.042(2) 0.0040(14) -0.0025(14) -0.0087(15) C20 0.074(2) 0.062(2) 0.058(2) 0.009(2) 0.005(2) 0.004(2) C21 0.077(3) 0.077(3) 0.078(3) -0.009(2) -0.013(2) 0.021(2) C22 0.047(2) 0.127(4) 0.058(2) -0.018(2) -0.006(2) 0.008(2) C23 0.061(2) 0.116(4) 0.061(2) 0.006(2) 0.015(2) -0.011(2) C24 0.062(2) 0.069(2) 0.060(2) 0.012(2) 0.007(2) -0.011(2) C25 0.072(3) 0.208(6) 0.081(3) -0.044(4) -0.004(2) 0.044(4) _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 Rh P1 2.2065(11) . ? Rh O1 2.217(2) . ? Rh P2 2.2183(10) . ? Rh O2 2.227(2) . ? Rh S 2.7647(10) . ? P1 C3 1.854(3) . ? P1 C1 1.859(3) . ? P1 C2 1.870(3) . ? P2 C5 1.857(4) . ? P2 C6 1.862(3) . ? P2 C4 1.870(3) . ? S O3 1.429(2) . ? S O2 1.475(2) . ? S O1 1.476(2) . ? S C19 1.761(3) . ? C1 C7 1.523(5) . ? C1 C8 1.528(5) . ? C2 C9 1.526(5) . ? C2 C10 1.533(4) . ? C3 C12 1.521(5) . ? C3 C11 1.532(5) . ? C4 C13 1.518(5) . ? C4 C14 1.537(5) . ? C5 C16 1.523(6) . ? C5 C15 1.527(6) . ? C6 C18 1.512(5) . ? C6 C17 1.521(5) . ? C19 C20 1.373(5) . ? C19 C24 1.382(4) . ? C20 C21 1.374(5) . ? C21 C22 1.379(6) . ? C22 C23 1.372(6) . ? C22 C25 1.510(5) . ? C23 C24 1.379(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 Rh O1 93.85(6) . . ? P1 Rh P2 106.32(3) . . ? O1 Rh P2 159.79(6) . . ? P1 Rh O2 157.86(6) . . ? O1 Rh O2 64.21(7) . . ? P2 Rh O2 95.70(6) . . ? P1 Rh S 126.00(3) . . ? O1 Rh S 32.15(5) . . ? P2 Rh S 127.67(3) . . ? O2 Rh S 32.14(5) . . ? C3 P1 C1 102.6(2) . . ? C3 P1 C2 108.6(2) . . ? C1 P1 C2 101.9(2) . . ? C3 P1 Rh 125.05(11) . . ? C1 P1 Rh 112.60(11) . . ? C2 P1 Rh 103.91(11) . . ? C5 P2 C6 102.2(2) . . ? C5 P2 C4 101.9(2) . . ? C6 P2 C4 108.3(2) . . ? C5 P2 Rh 111.64(12) . . ? C6 P2 Rh 103.92(12) . . ? C4 P2 Rh 126.46(11) . . ? O3 S O2 114.38(15) . . ? O3 S O1 114.82(14) . . ? O2 S O1 106.31(12) . . ? O3 S C19 107.2(2) . . ? O2 S C19 105.91(14) . . ? O1 S C19 107.70(14) . . ? O3 S Rh 137.33(12) . . ? O2 S Rh 53.41(8) . . ? O1 S Rh 53.05(8) . . ? C19 S Rh 115.46(11) . . ? S O1 Rh 94.80(10) . . ? S O2 Rh 94.46(10) . . ? C7 C1 C8 109.6(3) . . ? C7 C1 P1 112.7(3) . . ? C8 C1 P1 111.5(3) . . ? C9 C2 C10 111.7(3) . . ? C9 C2 P1 113.1(2) . . ? C10 C2 P1 117.0(3) . . ? C12 C3 C11 110.3(3) . . ? C12 C3 P1 111.7(3) . . ? C11 C3 P1 117.7(3) . . ? C13 C4 C14 110.1(3) . . ? C13 C4 P2 112.6(3) . . ? C14 C4 P2 117.7(3) . . ? C16 C5 C15 110.3(4) . . ? C16 C5 P2 112.9(3) . . ? C15 C5 P2 110.8(3) . . ? C18 C6 C17 113.0(3) . . ? C18 C6 P2 117.1(3) . . ? C17 C6 P2 113.6(2) . . ? C20 C19 C24 119.7(3) . . ? C20 C19 S 120.2(3) . . ? C24 C19 S 119.9(3) . . ? C19 C20 C21 120.1(4) . . ? C20 C21 C22 121.2(4) . . ? C23 C22 C21 118.1(4) . . ? C23 C22 C25 121.4(5) . . ? C21 C22 C25 120.5(5) . . ? C22 C23 C24 121.7(4) . . ? C23 C24 C19 119.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Rh P1 C3 -164.9(2) . . . . ? P2 Rh P1 C3 16.3(2) . . . . ? O2 Rh P1 C3 -157.5(2) . . . . ? S Rh P1 C3 -164.8(2) . . . . ? O1 Rh P1 C1 69.51(15) . . . . ? P2 Rh P1 C1 -109.24(13) . . . . ? O2 Rh P1 C1 77.0(2) . . . . ? S Rh P1 C1 69.62(14) . . . . ? O1 Rh P1 C2 -39.89(14) . . . . ? P2 Rh P1 C2 141.36(12) . . . . ? O2 Rh P1 C2 -32.4(2) . . . . ? S Rh P1 C2 -39.79(13) . . . . ? P1 Rh P2 C5 -115.84(13) . . . . ? O1 Rh P2 C5 67.8(2) . . . . ? O2 Rh P2 C5 61.80(15) . . . . ? S Rh P2 C5 65.34(14) . . . . ? P1 Rh P2 C6 134.72(13) . . . . ? O1 Rh P2 C6 -41.7(2) . . . . ? O2 Rh P2 C6 -47.65(14) . . . . ? S Rh P2 C6 -44.11(13) . . . . ? P1 Rh P2 C4 8.9(2) . . . . ? O1 Rh P2 C4 -167.5(2) . . . . ? O2 Rh P2 C4 -173.5(2) . . . . ? S Rh P2 C4 -169.92(15) . . . . ? P1 Rh S O3 87.5(2) . . . . ? O1 Rh S O3 87.6(2) . . . . ? P2 Rh S O3 -93.9(2) . . . . ? O2 Rh S O3 -87.3(2) . . . . ? P1 Rh S O2 174.77(11) . . . . ? O1 Rh S O2 175.0(2) . . . . ? P2 Rh S O2 -6.62(12) . . . . ? O2 Rh S O2 0.0 . . . . ? P1 Rh S O1 -0.20(12) . . . . ? O1 Rh S O1 0.0 . . . . ? P2 Rh S O1 178.41(12) . . . . ? O2 Rh S O1 -175.0(2) . . . . ? P1 Rh S C19 -93.82(11) . . . . ? O1 Rh S C19 -93.6(2) . . . . ? P2 Rh S C19 84.78(12) . . . . ? O2 Rh S C19 91.4(2) . . . . ? O3 S O1 Rh -131.75(14) . . . . ? O2 S O1 Rh -4.21(14) . . . . ? C19 S O1 Rh 108.94(13) . . . . ? Rh S O1 Rh 0.0 . . . . ? P1 Rh O1 S 179.84(10) . . . . ? P2 Rh O1 S -3.6(3) . . . . ? O2 Rh O1 S 2.97(10) . . . . ? S Rh O1 S 0.0 . . . . ? O3 S O2 Rh 131.99(13) . . . . ? O1 S O2 Rh 4.19(14) . . . . ? C19 S O2 Rh -110.19(12) . . . . ? Rh S O2 Rh 0.0 . . . . ? P1 Rh O2 S -11.3(2) . . . . ? O1 Rh O2 S -2.97(10) . . . . ? P2 Rh O2 S 174.73(10) . . . . ? S Rh O2 S 0.0 . . . . ? C3 P1 C1 C7 171.3(3) . . . . ? C2 P1 C1 C7 58.9(3) . . . . ? Rh P1 C1 C7 -51.8(3) . . . . ? C3 P1 C1 C8 -65.0(3) . . . . ? C2 P1 C1 C8 -177.3(3) . . . . ? Rh P1 C1 C8 72.0(3) . . . . ? C3 P1 C2 C9 81.1(3) . . . . ? C1 P1 C2 C9 -171.1(3) . . . . ? Rh P1 C2 C9 -53.9(3) . . . . ? C3 P1 C2 C10 -50.8(3) . . . . ? C1 P1 C2 C10 57.0(3) . . . . ? Rh P1 C2 C10 174.2(3) . . . . ? C1 P1 C3 C12 -166.5(3) . . . . ? C2 P1 C3 C12 -59.2(3) . . . . ? Rh P1 C3 C12 63.9(3) . . . . ? C1 P1 C3 C11 -37.3(3) . . . . ? C2 P1 C3 C11 69.9(3) . . . . ? Rh P1 C3 C11 -167.0(3) . . . . ? C5 P2 C4 C13 -161.2(3) . . . . ? C6 P2 C4 C13 -53.8(3) . . . . ? Rh P2 C4 C13 70.2(3) . . . . ? C5 P2 C4 C14 -31.4(3) . . . . ? C6 P2 C4 C14 75.9(3) . . . . ? Rh P2 C4 C14 -160.1(3) . . . . ? C6 P2 C5 C16 54.9(3) . . . . ? C4 P2 C5 C16 166.9(3) . . . . ? Rh P2 C5 C16 -55.6(3) . . . . ? C6 P2 C5 C15 179.2(3) . . . . ? C4 P2 C5 C15 -68.8(3) . . . . ? Rh P2 C5 C15 68.7(3) . . . . ? C5 P2 C6 C18 49.9(3) . . . . ? C4 P2 C6 C18 -57.2(3) . . . . ? Rh P2 C6 C18 166.2(3) . . . . ? C5 P2 C6 C17 -175.6(3) . . . . ? C4 P2 C6 C17 77.3(3) . . . . ? Rh P2 C6 C17 -59.3(3) . . . . ? O3 S C19 C20 -177.1(3) . . . . ? O2 S C19 C20 60.4(3) . . . . ? O1 S C19 C20 -53.0(3) . . . . ? Rh S C19 C20 3.8(3) . . . . ? O3 S C19 C24 7.1(3) . . . . ? O2 S C19 C24 -115.4(3) . . . . ? O1 S C19 C24 131.2(3) . . . . ? Rh S C19 C24 -172.0(2) . . . . ? C24 C19 C20 C21 0.9(5) . . . . ? S C19 C20 C21 -174.9(3) . . . . ? C19 C20 C21 C22 -0.1(6) . . . . ? C20 C21 C22 C23 -0.7(6) . . . . ? C20 C21 C22 C25 179.4(4) . . . . ? C21 C22 C23 C24 0.6(6) . . . . ? C25 C22 C23 C24 -179.4(3) . . . . ? C22 C23 C24 C19 0.2(6) . . . . ? C20 C19 C24 C23 -0.9(5) . . . . ? S C19 C24 C23 174.9(3) . . . . ? _refine_diff_density_max 0.576 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.051 #===END data_29 _publ_section_exptl_prep ; "crystals grown from pentane at room temperature" ; _publ_section_exptl_refinement ; Two independent molecules, A and B, were found in the asymmetric unit. Due to mesurement on an area detector system no standards were reported. ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H35 F3 O3 P Rh S' _chemical_formula_weight 522.40 _chemical_melting_point 36_C _chemical_compound_source ? 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' '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' 'Rh' 'Rh' -1.2870 0.9190 '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' _symmetry_Int_Tables_number 14 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 14.177(3) _cell_length_b 17.626(6) _cell_length_c 19.038(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.61(3) _cell_angle_gamma 90.00 _cell_volume 4623.8(24) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 25.97 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method ? _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.928 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'IPDS (STOE)' _diffrn_measurement_method 'Psi scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36543 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.97 _reflns_number_total 8695 _reflns_number_observed 5141 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'IPDS (STOE)' _computing_cell_refinement 'IPDS (STOE)' _computing_data_reduction 'IPDS (STOE)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor(obs) 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 w=1/[\s^2^(Fo^2^)+(0.0289P)^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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8695 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0720 _refine_ls_R_factor_obs 0.0334 _refine_ls_wR_factor_all 0.0683 _refine_ls_wR_factor_obs 0.0619 _refine_ls_goodness_of_fit_all 0.813 _refine_ls_goodness_of_fit_obs 0.977 _refine_ls_restrained_S_all 0.813 _refine_ls_restrained_S_obs 0.977 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 0.49581(2) 0.28147(2) 0.246240(15) 0.02349(8) Uani 1 d . . P1 P 0.56144(7) 0.30187(5) 0.36094(5) 0.0239(2) Uani 1 d . . S1 S 0.46815(8) 0.14641(6) 0.16797(5) 0.0319(2) Uani 1 d . . O1 O 0.5140(2) 0.15643(14) 0.24552(13) 0.0325(7) Uani 1 d . . O2 O 0.4535(2) 0.2206(2) 0.13329(13) 0.0373(7) Uani 1 d . . O3 O 0.5067(2) 0.0880(2) 0.1315(2) 0.0502(8) Uani 1 d . . F1 F 0.2981(2) 0.16468(14) 0.19766(14) 0.0531(7) Uani 1 d . . F2 F 0.3476(2) 0.05012(15) 0.2033(2) 0.0700(9) Uani 1 d . . F3 F 0.2959(2) 0.1027(2) 0.10009(15) 0.0725(9) Uani 1 d . . C1 C 0.3456(3) 0.1148(2) 0.1669(2) 0.0399(11) Uani 1 d . . C10 C 0.6955(3) 0.3034(2) 0.3774(2) 0.0274(9) Uani 1 d . . H10 H 0.7220(3) 0.3147(2) 0.4298(2) 0.033 Uiso 1 calc R . C11 C 0.5376(3) 0.2177(2) 0.4125(2) 0.0309(9) Uani 1 d . . H11 H 0.5670(3) 0.1740(2) 0.3918(2) 0.037 Uiso 1 calc R . C12 C 0.5300(3) 0.3904(2) 0.4028(2) 0.0282(9) Uani 1 d . . H12 H 0.5255(3) 0.4309(2) 0.3653(2) 0.034 Uiso 1 calc R . C13 C 0.7296(3) 0.3669(2) 0.3338(2) 0.0404(11) Uani 1 d . . H13A H 0.7016(15) 0.4153(3) 0.3441(11) 0.061 Uiso 1 calc R . H13B H 0.7083(16) 0.3556(8) 0.2821(2) 0.061 Uiso 1 calc R . H13C H 0.8005(3) 0.3702(10) 0.3475(10) 0.061 Uiso 1 calc R . C14 C 0.7368(3) 0.2267(2) 0.3618(2) 0.0333(9) Uani 1 d . . H14A H 0.7031(12) 0.2094(7) 0.3134(5) 0.050 Uiso 1 calc R . H14B H 0.7274(16) 0.1895(4) 0.3978(8) 0.050 Uiso 1 calc R . H14C H 0.8063(4) 0.2320(4) 0.3640(12) 0.050 Uiso 1 calc R . C15 C 0.6052(3) 0.4191(2) 0.4700(2) 0.0442(12) Uani 1 d . . H15A H 0.6681(6) 0.4260(14) 0.4579(4) 0.066 Uiso 1 calc R . H15B H 0.6118(14) 0.3818(7) 0.5091(5) 0.066 Uiso 1 calc R . H15C H 0.5834(10) 0.4676(7) 0.4858(9) 0.066 Uiso 1 calc R . C16 C 0.4299(3) 0.3863(2) 0.4194(2) 0.0400(11) Uani 1 d . . H16A H 0.3849(5) 0.3602(13) 0.3799(7) 0.060 Uiso 1 calc R . H16B H 0.4062(8) 0.4378(2) 0.4244(14) 0.060 Uiso 1 calc R . H16C H 0.4345(4) 0.3584(12) 0.4646(7) 0.060 Uiso 1 calc R . C17 C 0.5889(3) 0.2188(3) 0.4934(2) 0.0448(11) Uani 1 d . . H17A H 0.6572(6) 0.2324(15) 0.4990(2) 0.067 Uiso 1 calc R . H17B H 0.5845(18) 0.1684(5) 0.5142(4) 0.067 Uiso 1 calc R . H17C H 0.5574(13) 0.2562(11) 0.5185(3) 0.067 Uiso 1 calc R . C18 C 0.4300(3) 0.1977(2) 0.4015(2) 0.0427(11) Uani 1 d . . H18A H 0.3980(5) 0.2015(14) 0.3500(3) 0.064 Uiso 1 calc R . H18B H 0.3994(5) 0.2330(9) 0.4291(11) 0.064 Uiso 1 calc R . H18C H 0.4238(3) 0.1457(5) 0.4182(13) 0.064 Uiso 1 calc R . C20 C 0.4997(3) 0.3952(2) 0.2159(2) 0.0302(9) Uani 1 d . . C21 C 0.4083(3) 0.3772(2) 0.2292(2) 0.0276(9) Uani 1 d . . C22 C 0.3185(3) 0.3646(2) 0.1706(2) 0.0326(9) Uani 1 d . . H22A H 0.2771(3) 0.3265(2) 0.1869(2) 0.039 Uiso 1 calc R . H22B H 0.3370(3) 0.3442(2) 0.1272(2) 0.039 Uiso 1 calc R . C23 C 0.2601(3) 0.4386(2) 0.1503(2) 0.0385(11) Uani 1 d . . H23A H 0.2075(3) 0.4289(2) 0.1068(2) 0.046 Uiso 1 calc R . H23B H 0.2293(3) 0.4520(2) 0.1902(2) 0.046 Uiso 1 calc R . C24 C 0.3202(3) 0.5068(2) 0.1352(2) 0.0433(11) Uani 1 d . . H24A H 0.2755(3) 0.5500(2) 0.1198(2) 0.052 Uiso 1 calc R . H24B H 0.3657(3) 0.5215(2) 0.1811(2) 0.052 Uiso 1 calc R . C25 C 0.3786(3) 0.4946(2) 0.0783(2) 0.0457(12) Uani 1 d . . H25A H 0.3699(3) 0.5397(2) 0.0464(2) 0.055 Uiso 1 calc R . H25B H 0.3504(3) 0.4507(2) 0.0481(2) 0.055 Uiso 1 calc R . C26 C 0.4881(3) 0.4804(2) 0.1061(2) 0.0418(11) Uani 1 d . . H26A H 0.5192(3) 0.4865(2) 0.0650(2) 0.050 Uiso 1 calc R . H26B H 0.5147(3) 0.5204(2) 0.1418(2) 0.050 Uiso 1 calc R . C27 C 0.5176(3) 0.4032(2) 0.1410(2) 0.0337(10) Uani 1 d . . H27A H 0.4810(3) 0.3631(2) 0.1097(2) 0.040 Uiso 1 calc R . H27B H 0.5875(3) 0.3950(2) 0.1439(2) 0.040 Uiso 1 calc R . Rh2 Rh -0.00276(2) 0.67563(2) 0.221646(15) 0.02401(8) Uani 1 d . . P2 P 0.06367(7) 0.65880(5) 0.33686(5) 0.0238(2) Uani 1 d . . S2 S -0.03180(8) 0.80921(6) 0.14190(5) 0.0303(2) Uani 1 d . . O4 O 0.0164(2) 0.79962(15) 0.21871(13) 0.0355(7) Uani 1 d . . O5 O -0.0486(2) 0.73451(14) 0.10860(12) 0.0332(7) Uani 1 d . . O6 O 0.0063(2) 0.86662(15) 0.10374(14) 0.0399(7) Uani 1 d . . F4 F -0.1480(2) 0.9079(2) 0.1791(2) 0.0709(9) Uani 1 d . . F5 F -0.2003(2) 0.79359(14) 0.17474(14) 0.0513(7) Uani 1 d . . F6 F -0.2044(2) 0.8546(2) 0.0763(2) 0.0728(9) Uani 1 d . . C2 C -0.1528(3) 0.8426(2) 0.1434(2) 0.0423(11) Uani 1 d . . C30 C 0.1972(3) 0.6612(2) 0.3525(2) 0.0286(9) Uani 1 d . . H30 H 0.2251(3) 0.6528(2) 0.4052(2) 0.034 Uiso 1 calc R . C31 C 0.0378(3) 0.5700(2) 0.3814(2) 0.0275(9) Uani 1 d . . H31 H 0.0350(3) 0.5289(2) 0.3448(2) 0.033 Uiso 1 calc R . C32 C 0.0338(3) 0.7425(2) 0.3859(2) 0.0269(9) Uani 1 d . . H32 H 0.0609(3) 0.7869(2) 0.3646(2) 0.032 Uiso 1 calc R . C33 C 0.2340(3) 0.7380(2) 0.3320(2) 0.0348(10) Uani 1 d . . H33A H 0.2223(16) 0.7770(3) 0.3657(8) 0.052 Uiso 1 calc R . H33B H 0.1995(12) 0.7514(7) 0.2827(5) 0.052 Uiso 1 calc R . H33C H 0.3037(4) 0.7346(4) 0.3346(12) 0.052 Uiso 1 calc R . C34 C 0.2333(3) 0.5970(2) 0.3109(2) 0.0378(10) Uani 1 d . . H34A H 0.2082(15) 0.5484(3) 0.3236(11) 0.057 Uiso 1 calc R . H34B H 0.3044(3) 0.5960(9) 0.3238(10) 0.057 Uiso 1 calc R . H34C H 0.2103(15) 0.6058(8) 0.2589(2) 0.057 Uiso 1 calc R . C35 C 0.1157(3) 0.5450(2) 0.4484(2) 0.0395(11) Uani 1 d . . H35A H 0.1226(13) 0.5840(7) 0.4860(5) 0.059 Uiso 1 calc R . H35B H 0.1778(5) 0.5382(14) 0.4351(4) 0.059 Uiso 1 calc R . H35C H 0.0961(9) 0.4970(7) 0.4667(8) 0.059 Uiso 1 calc R . C36 C -0.0624(3) 0.5709(2) 0.3990(2) 0.0371(11) Uani 1 d . . H36A H -0.0819(9) 0.5189(2) 0.4069(13) 0.056 Uiso 1 calc R . H36B H -0.1099(5) 0.5935(13) 0.3585(6) 0.056 Uiso 1 calc R . H36C H -0.0593(5) 0.6010(12) 0.4427(8) 0.056 Uiso 1 calc R . C37 C 0.0828(3) 0.7446(2) 0.4672(2) 0.0392(11) Uani 1 d . . H37A H 0.1532(4) 0.7403(15) 0.4738(2) 0.059 Uiso 1 calc R . H37B H 0.0590(14) 0.7023(9) 0.4916(3) 0.059 Uiso 1 calc R . H37C H 0.0673(16) 0.7927(6) 0.4878(3) 0.059 Uiso 1 calc R . C38 C -0.0755(3) 0.7582(2) 0.3729(2) 0.0406(11) Uani 1 d . . H38A H -0.1064(4) 0.7508(14) 0.3216(3) 0.061 Uiso 1 calc R . H38B H -0.0857(3) 0.8106(5) 0.3867(13) 0.061 Uiso 1 calc R . H38C H -0.1043(4) 0.7233(9) 0.4021(10) 0.061 Uiso 1 calc R . C40 C -0.0898(3) 0.5797(2) 0.2091(2) 0.0279(9) Uani 1 d . . C41 C -0.0004(3) 0.5609(2) 0.1939(2) 0.0284(9) Uani 1 d . . C42 C 0.0144(3) 0.5483(2) 0.1187(2) 0.0356(10) Uani 1 d . . H42A H 0.0842(3) 0.5543(2) 0.1198(2) 0.043 Uiso 1 calc R . H42B H -0.0217(3) 0.5876(2) 0.0860(2) 0.043 Uiso 1 calc R . C43 C -0.0192(3) 0.4700(3) 0.0885(2) 0.0472(12) Uani 1 d . . H43A H 0.0119(3) 0.4590(3) 0.0482(2) 0.057 Uiso 1 calc R . H43B H 0.0051(3) 0.4319(3) 0.1268(2) 0.057 Uiso 1 calc R . C44 C -0.1284(4) 0.4589(2) 0.0613(2) 0.0491(12) Uani 1 d . . H44A H -0.1395(4) 0.4133(2) 0.0301(2) 0.059 Uiso 1 calc R . H44B H -0.1548(4) 0.5029(2) 0.0307(2) 0.059 Uiso 1 calc R . C45 C -0.1865(4) 0.4499(2) 0.1195(3) 0.0499(13) Uani 1 d . . H45A H -0.2333(4) 0.4078(2) 0.1050(3) 0.060 Uiso 1 calc R . H45B H -0.1411(4) 0.4349(2) 0.1652(3) 0.060 Uiso 1 calc R . C46 C -0.2424(3) 0.5199(2) 0.1340(2) 0.0423(11) Uani 1 d . . H46A H -0.2717(3) 0.5089(2) 0.1753(2) 0.051 Uiso 1 calc R . H46B H -0.2962(3) 0.5293(2) 0.0912(2) 0.051 Uiso 1 calc R . C47 C -0.1814(3) 0.5921(2) 0.1507(2) 0.0328(10) Uani 1 d . . H47A H -0.1636(3) 0.6097(2) 0.1061(2) 0.039 Uiso 1 calc R . H47B H -0.2207(3) 0.6324(2) 0.1663(2) 0.039 Uiso 1 calc R . H20 H 0.5430(3) 0.4355(2) 0.2548(2) 0.049 Uiso 1 d R . H41 H 0.0428(3) 0.5235(2) 0.2289(2) 0.049 Uiso 1 d R . H21 H 0.3978(3) 0.4094(2) 0.2707(2) 0.049 Uiso 1 d R . H40 H -0.1022(3) 0.5608(2) 0.2625(2) 0.049 Uiso 1 d 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 0.0218(2) 0.0257(2) 0.0223(2) -0.00238(13) 0.00371(12) -0.00086(14) P1 0.0211(6) 0.0275(6) 0.0232(5) -0.0028(4) 0.0053(4) 0.0007(4) S1 0.0258(7) 0.0336(6) 0.0352(6) -0.0101(4) 0.0054(5) 0.0000(4) O1 0.031(2) 0.0275(15) 0.0341(15) -0.0068(11) -0.0022(12) 0.0033(12) O2 0.040(2) 0.042(2) 0.0286(14) -0.0027(13) 0.0058(12) -0.0055(14) O3 0.043(2) 0.047(2) 0.062(2) -0.0315(15) 0.016(2) 0.0060(15) F1 0.035(2) 0.050(2) 0.080(2) -0.0104(13) 0.0230(14) 0.0003(12) F2 0.067(2) 0.036(2) 0.111(2) 0.0127(14) 0.029(2) -0.0082(14) F3 0.041(2) 0.107(3) 0.062(2) -0.027(2) -0.0036(15) -0.023(2) C1 0.035(3) 0.033(3) 0.050(3) -0.005(2) 0.007(2) 0.001(2) C10 0.025(3) 0.029(2) 0.025(2) -0.0039(14) 0.001(2) 0.003(2) C11 0.028(3) 0.036(2) 0.029(2) 0.003(2) 0.007(2) 0.000(2) C12 0.025(3) 0.030(2) 0.028(2) -0.011(2) 0.004(2) 0.004(2) C13 0.024(3) 0.040(3) 0.057(3) 0.004(2) 0.010(2) -0.005(2) C14 0.028(3) 0.037(2) 0.034(2) -0.001(2) 0.007(2) 0.007(2) C15 0.039(3) 0.044(3) 0.046(3) -0.024(2) 0.002(2) 0.003(2) C16 0.034(3) 0.048(3) 0.040(2) -0.012(2) 0.012(2) 0.011(2) C17 0.053(3) 0.054(3) 0.029(2) 0.004(2) 0.011(2) -0.001(2) C18 0.042(3) 0.039(3) 0.051(3) 0.005(2) 0.019(2) -0.008(2) C20 0.023(3) 0.031(2) 0.034(2) 0.002(2) 0.001(2) 0.003(2) C21 0.028(3) 0.028(2) 0.027(2) -0.001(2) 0.007(2) 0.000(2) C22 0.022(3) 0.036(2) 0.039(2) 0.008(2) 0.006(2) 0.001(2) C23 0.028(3) 0.039(3) 0.044(3) 0.007(2) 0.000(2) 0.000(2) C24 0.039(3) 0.032(3) 0.055(3) 0.010(2) 0.002(2) 0.006(2) C25 0.048(4) 0.037(3) 0.046(3) 0.014(2) -0.003(2) -0.005(2) C26 0.045(3) 0.047(3) 0.032(2) 0.013(2) 0.007(2) -0.009(2) C27 0.033(3) 0.037(2) 0.033(2) -0.001(2) 0.012(2) -0.006(2) Rh2 0.0221(2) 0.0279(2) 0.0214(2) 0.00300(13) 0.00388(13) 0.00116(14) P2 0.0211(6) 0.0287(6) 0.0215(5) 0.0028(4) 0.0050(4) -0.0012(4) S2 0.0260(7) 0.0331(6) 0.0319(5) 0.0089(4) 0.0073(4) 0.0012(4) O4 0.035(2) 0.042(2) 0.0275(14) 0.0053(11) 0.0025(13) -0.0018(13) O5 0.040(2) 0.032(2) 0.0269(14) 0.0042(11) 0.0072(12) 0.0026(13) O6 0.038(2) 0.036(2) 0.048(2) 0.0198(13) 0.0162(14) -0.0011(13) F4 0.069(2) 0.040(2) 0.117(2) -0.007(2) 0.048(2) 0.0104(15) F5 0.031(2) 0.052(2) 0.077(2) 0.0188(13) 0.0252(14) 0.0005(12) F6 0.037(2) 0.106(3) 0.072(2) 0.039(2) 0.0051(15) 0.022(2) C2 0.037(3) 0.038(3) 0.056(3) 0.012(2) 0.019(2) 0.007(2) C30 0.023(3) 0.035(2) 0.026(2) 0.005(2) 0.003(2) 0.000(2) C31 0.028(3) 0.029(2) 0.024(2) 0.0048(15) 0.004(2) -0.002(2) C32 0.028(3) 0.029(2) 0.024(2) -0.0026(15) 0.006(2) -0.003(2) C33 0.024(3) 0.043(3) 0.037(2) 0.000(2) 0.007(2) -0.008(2) C34 0.027(3) 0.034(2) 0.053(3) -0.001(2) 0.011(2) 0.002(2) C35 0.051(3) 0.036(3) 0.029(2) 0.011(2) 0.005(2) -0.002(2) C36 0.042(3) 0.039(3) 0.035(2) 0.002(2) 0.018(2) -0.011(2) C37 0.043(3) 0.041(3) 0.034(2) -0.005(2) 0.011(2) -0.003(2) C38 0.036(3) 0.038(3) 0.052(3) -0.005(2) 0.017(2) 0.004(2) C40 0.028(3) 0.030(2) 0.024(2) -0.0039(15) 0.003(2) 0.001(2) C41 0.027(3) 0.029(2) 0.027(2) 0.001(2) 0.002(2) 0.005(2) C42 0.031(3) 0.039(3) 0.036(2) 0.000(2) 0.006(2) 0.007(2) C43 0.051(4) 0.048(3) 0.041(3) -0.004(2) 0.009(2) 0.018(2) C44 0.053(4) 0.038(3) 0.049(3) -0.020(2) -0.004(2) 0.007(2) C45 0.044(4) 0.034(3) 0.064(3) -0.004(2) -0.004(3) -0.007(2) C46 0.031(3) 0.046(3) 0.047(3) -0.006(2) 0.003(2) -0.007(2) C47 0.028(3) 0.034(2) 0.035(2) -0.002(2) 0.003(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C21 2.074(4) . ? Rh1 C20 2.091(4) . ? Rh1 P1 2.1925(12) . ? Rh1 O1 2.219(3) . ? Rh1 O2 2.351(2) . ? Rh1 C22 2.973(4) . ? Rh1 C27 3.000(4) . ? P1 C10 1.852(4) . ? P1 C11 1.853(4) . ? P1 C12 1.854(3) . ? S1 O3 1.422(3) . ? S1 O2 1.458(3) . ? S1 O1 1.477(3) . ? S1 C1 1.820(5) . ? F1 C1 1.325(4) . ? F2 C1 1.331(5) . ? F3 C1 1.319(5) . ? C10 C14 1.530(5) . ? C10 C13 1.538(5) . ? C11 C18 1.531(6) . ? C11 C17 1.541(5) . ? C12 C16 1.527(5) . ? C12 C15 1.545(5) . ? C20 C21 1.413(5) . ? C20 C27 1.512(5) . ? C21 C22 1.499(5) . ? C22 C23 1.543(5) . ? C23 C24 1.539(6) . ? C24 C25 1.527(6) . ? C25 C26 1.538(6) . ? C26 C27 1.530(5) . ? Rh2 C40 2.073(4) . ? Rh2 C41 2.091(4) . ? Rh2 P2 2.1941(12) . ? Rh2 O4 2.205(3) . ? Rh2 O5 2.339(2) . ? Rh2 C47 2.966(4) . ? Rh2 C42 3.027(4) . ? P2 C30 1.846(4) . ? P2 C32 1.848(4) . ? P2 C31 1.857(3) . ? S2 O6 1.424(3) . ? S2 O5 1.456(3) . ? S2 O4 1.471(3) . ? S2 C2 1.820(4) . ? F4 C2 1.331(5) . ? F5 C2 1.321(4) . ? F6 C2 1.331(5) . ? C30 C33 1.533(5) . ? C30 C34 1.536(5) . ? C31 C36 1.534(5) . ? C31 C35 1.542(5) . ? C32 C38 1.536(5) . ? C32 C37 1.540(5) . ? C40 C41 1.404(5) . ? C40 C47 1.513(5) . ? C41 C42 1.512(5) . ? C42 C43 1.528(6) . ? C43 C44 1.526(6) . ? C44 C45 1.536(6) . ? C45 C46 1.526(6) . ? C46 C47 1.531(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 C21 Rh1 C20 39.65(15) . . ? C21 Rh1 P1 96.94(10) . . ? C20 Rh1 P1 94.88(11) . . ? C21 Rh1 O1 150.80(13) . . ? C20 Rh1 O1 160.05(12) . . ? P1 Rh1 O1 98.41(7) . . ? C21 Rh1 O2 102.31(12) . . ? C20 Rh1 O2 101.69(12) . . ? P1 Rh1 O2 160.55(7) . . ? O1 Rh1 O2 63.02(9) . . ? C21 Rh1 C22 27.95(13) . . ? C20 Rh1 C22 57.83(14) . . ? P1 Rh1 C22 120.94(8) . . ? O1 Rh1 C22 124.94(10) . . ? O2 Rh1 C22 77.11(11) . . ? C21 Rh1 C27 57.67(13) . . ? C20 Rh1 C27 27.92(12) . . ? P1 Rh1 C27 117.48(8) . . ? O1 Rh1 C27 132.51(10) . . ? O2 Rh1 C27 76.10(10) . . ? C22 Rh1 C27 62.10(11) . . ? C10 P1 C11 103.3(2) . . ? C10 P1 C12 104.8(2) . . ? C11 P1 C12 110.7(2) . . ? C10 P1 Rh1 110.42(12) . . ? C11 P1 Rh1 107.99(12) . . ? C12 P1 Rh1 118.55(13) . . ? O3 S1 O2 117.3(2) . . ? O3 S1 O1 116.5(2) . . ? O2 S1 O1 109.13(15) . . ? O3 S1 C1 104.4(2) . . ? O2 S1 C1 103.6(2) . . ? O1 S1 C1 104.0(2) . . ? S1 O1 Rh1 95.77(13) . . ? S1 O2 Rh1 90.95(12) . . ? F3 C1 F1 108.8(4) . . ? F3 C1 F2 107.7(4) . . ? F1 C1 F2 106.7(4) . . ? F3 C1 S1 110.7(3) . . ? F1 C1 S1 112.0(3) . . ? F2 C1 S1 110.7(3) . . ? C14 C10 C13 110.8(3) . . ? C14 C10 P1 112.3(3) . . ? C13 C10 P1 111.0(3) . . ? C18 C11 C17 111.1(3) . . ? C18 C11 P1 114.3(3) . . ? C17 C11 P1 114.7(3) . . ? C16 C12 C15 109.7(3) . . ? C16 C12 P1 112.2(3) . . ? C15 C12 P1 116.3(3) . . ? C21 C20 C27 123.6(3) . . ? C21 C20 Rh1 69.5(2) . . ? C27 C20 Rh1 111.7(2) . . ? C20 C21 C22 123.7(3) . . ? C20 C21 Rh1 70.8(2) . . ? C22 C21 Rh1 111.6(2) . . ? C21 C22 C23 111.9(3) . . ? C21 C22 Rh1 40.4(2) . . ? C23 C22 Rh1 151.6(3) . . ? C24 C23 C22 114.8(4) . . ? C25 C24 C23 116.0(4) . . ? C24 C25 C26 116.8(4) . . ? C27 C26 C25 116.4(3) . . ? C20 C27 C26 113.8(3) . . ? C20 C27 Rh1 40.3(2) . . ? C26 C27 Rh1 150.0(3) . . ? C40 Rh2 C41 39.41(15) . . ? C40 Rh2 P2 96.26(10) . . ? C41 Rh2 P2 95.34(10) . . ? C40 Rh2 O4 151.48(13) . . ? C41 Rh2 O4 160.46(12) . . ? P2 Rh2 O4 97.64(7) . . ? C40 Rh2 O5 103.09(12) . . ? C41 Rh2 O5 102.36(12) . . ? P2 Rh2 O5 160.16(7) . . ? O4 Rh2 O5 63.00(9) . . ? C40 Rh2 C47 28.53(13) . . ? C41 Rh2 C47 57.84(14) . . ? P2 Rh2 C47 120.53(8) . . ? O4 Rh2 C47 125.27(11) . . ? O5 Rh2 C47 77.20(10) . . ? C40 Rh2 C42 57.15(13) . . ? C41 Rh2 C42 27.32(12) . . ? P2 Rh2 C42 117.78(8) . . ? O4 Rh2 C42 133.58(10) . . ? O5 Rh2 C42 77.32(10) . . ? C47 Rh2 C42 61.79(11) . . ? C30 P2 C32 104.4(2) . . ? C30 P2 C31 104.5(2) . . ? C32 P2 C31 110.4(2) . . ? C30 P2 Rh2 109.89(12) . . ? C32 P2 Rh2 107.57(12) . . ? C31 P2 Rh2 119.08(13) . . ? O6 S2 O5 117.6(2) . . ? O6 S2 O4 116.5(2) . . ? O5 S2 O4 108.61(15) . . ? O6 S2 C2 104.5(2) . . ? O5 S2 C2 103.9(2) . . ? O4 S2 C2 103.9(2) . . ? S2 O4 Rh2 96.20(13) . . ? S2 O5 Rh2 91.09(12) . . ? F5 C2 F4 107.7(3) . . ? F5 C2 F6 108.3(4) . . ? F4 C2 F6 107.6(4) . . ? F5 C2 S2 112.3(3) . . ? F4 C2 S2 110.7(3) . . ? F6 C2 S2 110.1(3) . . ? C33 C30 C34 110.2(3) . . ? C33 C30 P2 112.2(3) . . ? C34 C30 P2 110.7(3) . . ? C36 C31 C35 110.0(3) . . ? C36 C31 P2 112.5(3) . . ? C35 C31 P2 116.0(3) . . ? C38 C32 C37 110.9(3) . . ? C38 C32 P2 113.9(3) . . ? C37 C32 P2 115.1(3) . . ? C41 C40 C47 122.8(3) . . ? C41 C40 Rh2 71.0(2) . . ? C47 C40 Rh2 110.6(2) . . ? C40 C41 C42 124.3(3) . . ? C40 C41 Rh2 69.6(2) . . ? C42 C41 Rh2 113.3(2) . . ? C41 C42 C43 112.8(3) . . ? C41 C42 Rh2 39.4(2) . . ? C43 C42 Rh2 148.0(3) . . ? C44 C43 C42 116.4(4) . . ? C43 C44 C45 116.2(4) . . ? C46 C45 C44 115.9(4) . . ? C45 C46 C47 114.7(4) . . ? C40 C47 C46 112.2(3) . . ? C40 C47 Rh2 40.9(2) . . ? C46 C47 Rh2 152.6(3) . . ? 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 C21 Rh1 P1 C10 -124.3(2) . . . . ? C20 Rh1 P1 C10 -84.5(2) . . . . ? O1 Rh1 P1 C10 80.57(14) . . . . ? O2 Rh1 P1 C10 64.0(2) . . . . ? C22 Rh1 P1 C10 -139.65(15) . . . . ? C27 Rh1 P1 C10 -67.3(2) . . . . ? C21 Rh1 P1 C11 123.4(2) . . . . ? C20 Rh1 P1 C11 163.3(2) . . . . ? O1 Rh1 P1 C11 -31.7(2) . . . . ? O2 Rh1 P1 C11 -48.2(3) . . . . ? C22 Rh1 P1 C11 108.1(2) . . . . ? C27 Rh1 P1 C11 -179.5(2) . . . . ? C21 Rh1 P1 C12 -3.4(2) . . . . ? C20 Rh1 P1 C12 36.4(2) . . . . ? O1 Rh1 P1 C12 -158.5(2) . . . . ? O2 Rh1 P1 C12 -175.1(2) . . . . ? C22 Rh1 P1 C12 -18.7(2) . . . . ? C27 Rh1 P1 C12 53.6(2) . . . . ? O3 S1 O1 Rh1 145.8(2) . . . . ? O2 S1 O1 Rh1 10.1(2) . . . . ? C1 S1 O1 Rh1 -100.0(2) . . . . ? C21 Rh1 O1 S1 58.5(3) . . . . ? C20 Rh1 O1 S1 -49.2(4) . . . . ? P1 Rh1 O1 S1 179.53(11) . . . . ? O2 Rh1 O1 S1 -6.60(11) . . . . ? C22 Rh1 O1 S1 42.0(2) . . . . ? C27 Rh1 O1 S1 -40.3(2) . . . . ? O3 S1 O2 Rh1 -144.7(2) . . . . ? O1 S1 O2 Rh1 -9.4(2) . . . . ? C1 S1 O2 Rh1 100.9(2) . . . . ? C21 Rh1 O2 S1 -146.41(15) . . . . ? C20 Rh1 O2 S1 173.0(2) . . . . ? P1 Rh1 O2 S1 25.1(3) . . . . ? O1 Rh1 O2 S1 6.65(12) . . . . ? C22 Rh1 O2 S1 -134.22(15) . . . . ? C27 Rh1 O2 S1 161.7(2) . . . . ? O3 S1 C1 F3 -56.8(3) . . . . ? O2 S1 C1 F3 66.6(3) . . . . ? O1 S1 C1 F3 -179.4(3) . . . . ? O3 S1 C1 F1 -178.4(3) . . . . ? O2 S1 C1 F1 -55.0(3) . . . . ? O1 S1 C1 F1 59.1(3) . . . . ? O3 S1 C1 F2 62.6(3) . . . . ? O2 S1 C1 F2 -174.0(3) . . . . ? O1 S1 C1 F2 -60.0(3) . . . . ? C11 P1 C10 C14 51.1(3) . . . . ? C12 P1 C10 C14 167.2(3) . . . . ? Rh1 P1 C10 C14 -64.1(3) . . . . ? C11 P1 C10 C13 175.8(3) . . . . ? C12 P1 C10 C13 -68.2(3) . . . . ? Rh1 P1 C10 C13 60.6(3) . . . . ? C10 P1 C11 C18 -173.6(3) . . . . ? C12 P1 C11 C18 74.7(3) . . . . ? Rh1 P1 C11 C18 -56.6(3) . . . . ? C10 P1 C11 C17 56.4(3) . . . . ? C12 P1 C11 C17 -55.3(3) . . . . ? Rh1 P1 C11 C17 173.4(3) . . . . ? C10 P1 C12 C16 -159.1(3) . . . . ? C11 P1 C12 C16 -48.3(3) . . . . ? Rh1 P1 C12 C16 77.2(3) . . . . ? C10 P1 C12 C15 -31.6(3) . . . . ? C11 P1 C12 C15 79.2(3) . . . . ? Rh1 P1 C12 C15 -155.3(3) . . . . ? C21 Rh1 C20 C21 0.0 . . . . ? P1 Rh1 C20 C21 -95.0(2) . . . . ? O1 Rh1 C20 C21 133.3(4) . . . . ? O2 Rh1 C20 C21 95.3(2) . . . . ? C22 Rh1 C20 C21 28.8(2) . . . . ? C27 Rh1 C20 C21 119.2(4) . . . . ? C21 Rh1 C20 C27 -119.2(4) . . . . ? P1 Rh1 C20 C27 145.9(3) . . . . ? O1 Rh1 C20 C27 14.1(6) . . . . ? O2 Rh1 C20 C27 -23.9(3) . . . . ? C22 Rh1 C20 C27 -90.4(3) . . . . ? C27 Rh1 C20 C27 0.0 . . . . ? C27 C20 C21 C22 -0.6(6) . . . . ? Rh1 C20 C21 C22 -103.7(3) . . . . ? C27 C20 C21 Rh1 103.1(3) . . . . ? Rh1 C20 C21 Rh1 0.0 . . . . ? C20 Rh1 C21 C20 0.0 . . . . ? P1 Rh1 C21 C20 89.3(2) . . . . ? O1 Rh1 C21 C20 -149.4(2) . . . . ? O2 Rh1 C21 C20 -93.5(2) . . . . ? C22 Rh1 C21 C20 -119.6(3) . . . . ? C27 Rh1 C21 C20 -28.9(2) . . . . ? C20 Rh1 C21 C22 119.6(3) . . . . ? P1 Rh1 C21 C22 -151.1(2) . . . . ? O1 Rh1 C21 C22 -29.8(4) . . . . ? O2 Rh1 C21 C22 26.0(3) . . . . ? C22 Rh1 C21 C22 0.0 . . . . ? C27 Rh1 C21 C22 90.6(3) . . . . ? C20 C21 C22 C23 -91.4(4) . . . . ? Rh1 C21 C22 C23 -172.2(2) . . . . ? C20 C21 C22 Rh1 80.7(4) . . . . ? Rh1 C21 C22 Rh1 0.0 . . . . ? C21 Rh1 C22 C21 0.000(1) . . . . ? C20 Rh1 C22 C21 -41.0(3) . . . . ? P1 Rh1 C22 C21 34.0(3) . . . . ? O1 Rh1 C22 C21 162.8(2) . . . . ? O2 Rh1 C22 C21 -153.9(3) . . . . ? C27 Rh1 C22 C21 -73.0(3) . . . . ? C21 Rh1 C22 C23 15.5(5) . . . . ? C20 Rh1 C22 C23 -25.5(5) . . . . ? P1 Rh1 C22 C23 49.4(6) . . . . ? O1 Rh1 C22 C23 178.2(5) . . . . ? O2 Rh1 C22 C23 -138.4(6) . . . . ? C27 Rh1 C22 C23 -57.5(5) . . . . ? C21 C22 C23 C24 49.9(5) . . . . ? Rh1 C22 C23 C24 39.1(7) . . . . ? C22 C23 C24 C25 54.5(5) . . . . ? C23 C24 C25 C26 -102.2(5) . . . . ? C24 C25 C26 C27 72.2(5) . . . . ? C21 C20 C27 C26 81.4(5) . . . . ? Rh1 C20 C27 C26 160.6(3) . . . . ? C21 C20 C27 Rh1 -79.2(4) . . . . ? Rh1 C20 C27 Rh1 0.0 . . . . ? C25 C26 C27 C20 -74.5(5) . . . . ? C25 C26 C27 Rh1 -49.0(7) . . . . ? C21 Rh1 C27 C20 41.3(3) . . . . ? C20 Rh1 C27 C20 0.000(2) . . . . ? P1 Rh1 C27 C20 -39.1(3) . . . . ? O1 Rh1 C27 C20 -173.5(3) . . . . ? O2 Rh1 C27 C20 155.9(3) . . . . ? C22 Rh1 C27 C20 73.3(3) . . . . ? C21 Rh1 C27 C26 3.9(5) . . . . ? C20 Rh1 C27 C26 -37.4(5) . . . . ? P1 Rh1 C27 C26 -76.5(6) . . . . ? O1 Rh1 C27 C26 149.1(5) . . . . ? O2 Rh1 C27 C26 118.5(6) . . . . ? C22 Rh1 C27 C26 35.9(6) . . . . ? C40 Rh2 P2 C30 126.8(2) . . . . ? C41 Rh2 P2 C30 87.2(2) . . . . ? O4 Rh2 P2 C30 -78.13(15) . . . . ? O5 Rh2 P2 C30 -66.0(2) . . . . ? C47 Rh2 P2 C30 142.8(2) . . . . ? C42 Rh2 P2 C30 70.8(2) . . . . ? C40 Rh2 P2 C32 -120.1(2) . . . . ? C41 Rh2 P2 C32 -159.7(2) . . . . ? O4 Rh2 P2 C32 35.0(2) . . . . ? O5 Rh2 P2 C32 47.1(2) . . . . ? C47 Rh2 P2 C32 -104.1(2) . . . . ? C42 Rh2 P2 C32 -176.1(2) . . . . ? C40 Rh2 P2 C31 6.4(2) . . . . ? C41 Rh2 P2 C31 -33.2(2) . . . . ? O4 Rh2 P2 C31 161.4(2) . . . . ? O5 Rh2 P2 C31 173.6(2) . . . . ? C47 Rh2 P2 C31 22.4(2) . . . . ? C42 Rh2 P2 C31 -49.6(2) . . . . ? O6 S2 O4 Rh2 -145.45(15) . . . . ? O5 S2 O4 Rh2 -9.9(2) . . . . ? C2 S2 O4 Rh2 100.3(2) . . . . ? C40 Rh2 O4 S2 -59.5(3) . . . . ? C41 Rh2 O4 S2 50.7(4) . . . . ? P2 Rh2 O4 S2 -178.05(12) . . . . ? O5 Rh2 O4 S2 6.55(11) . . . . ? C47 Rh2 O4 S2 -41.8(2) . . . . ? C42 Rh2 O4 S2 41.0(2) . . . . ? O6 S2 O5 Rh2 144.26(15) . . . . ? O4 S2 O5 Rh2 9.3(2) . . . . ? C2 S2 O5 Rh2 -100.9(2) . . . . ? C40 Rh2 O5 S2 146.8(2) . . . . ? C41 Rh2 O5 S2 -172.8(2) . . . . ? P2 Rh2 O5 S2 -20.1(3) . . . . ? O4 Rh2 O5 S2 -6.58(12) . . . . ? C47 Rh2 O5 S2 134.71(15) . . . . ? C42 Rh2 O5 S2 -161.8(2) . . . . ? O6 S2 C2 F5 177.4(3) . . . . ? O5 S2 C2 F5 53.5(4) . . . . ? O4 S2 C2 F5 -60.1(4) . . . . ? O6 S2 C2 F4 -62.2(3) . . . . ? O5 S2 C2 F4 173.9(3) . . . . ? O4 S2 C2 F4 60.4(3) . . . . ? O6 S2 C2 F6 56.6(3) . . . . ? O5 S2 C2 F6 -67.2(3) . . . . ? O4 S2 C2 F6 179.2(3) . . . . ? C32 P2 C30 C33 -53.2(3) . . . . ? C31 P2 C30 C33 -169.2(3) . . . . ? Rh2 P2 C30 C33 61.9(3) . . . . ? C32 P2 C30 C34 -176.7(3) . . . . ? C31 P2 C30 C34 67.3(3) . . . . ? Rh2 P2 C30 C34 -61.6(3) . . . . ? C30 P2 C31 C36 159.1(3) . . . . ? C32 P2 C31 C36 47.4(3) . . . . ? Rh2 P2 C31 C36 -77.8(3) . . . . ? C30 P2 C31 C35 31.2(3) . . . . ? C32 P2 C31 C35 -80.5(3) . . . . ? Rh2 P2 C31 C35 154.4(2) . . . . ? C30 P2 C32 C38 172.7(3) . . . . ? C31 P2 C32 C38 -75.4(3) . . . . ? Rh2 P2 C32 C38 56.0(3) . . . . ? C30 P2 C32 C37 -57.5(3) . . . . ? C31 P2 C32 C37 54.3(3) . . . . ? Rh2 P2 C32 C37 -174.3(3) . . . . ? C41 Rh2 C40 C41 0.0 . . . . ? P2 Rh2 C40 C41 -90.8(2) . . . . ? O4 Rh2 C40 C41 150.4(2) . . . . ? O5 Rh2 C40 C41 93.6(2) . . . . ? C47 Rh2 C40 C41 118.9(3) . . . . ? C42 Rh2 C40 C41 28.4(2) . . . . ? C41 Rh2 C40 C47 -118.9(3) . . . . ? P2 Rh2 C40 C47 150.3(2) . . . . ? O4 Rh2 C40 C47 31.5(4) . . . . ? O5 Rh2 C40 C47 -25.3(3) . . . . ? C47 Rh2 C40 C47 0.0 . . . . ? C42 Rh2 C40 C47 -90.6(3) . . . . ? C47 C40 C41 C42 -2.2(6) . . . . ? Rh2 C40 C41 C42 -104.9(3) . . . . ? C47 C40 C41 Rh2 102.7(3) . . . . ? Rh2 C40 C41 Rh2 0.0 . . . . ? C40 Rh2 C41 C40 0.0 . . . . ? P2 Rh2 C41 C40 93.4(2) . . . . ? O4 Rh2 C41 C40 -135.1(4) . . . . ? O5 Rh2 C41 C40 -95.7(2) . . . . ? C47 Rh2 C41 C40 -29.6(2) . . . . ? C42 Rh2 C41 C40 -119.6(4) . . . . ? C40 Rh2 C41 C42 119.6(4) . . . . ? P2 Rh2 C41 C42 -147.0(3) . . . . ? O4 Rh2 C41 C42 -15.5(6) . . . . ? O5 Rh2 C41 C42 24.0(3) . . . . ? C47 Rh2 C41 C42 90.0(3) . . . . ? C42 Rh2 C41 C42 0.000(1) . . . . ? C40 C41 C42 C43 -79.0(5) . . . . ? Rh2 C41 C42 C43 -159.5(3) . . . . ? C40 C41 C42 Rh2 80.5(4) . . . . ? Rh2 C41 C42 Rh2 0.000(1) . . . . ? C40 Rh2 C42 C41 -41.1(3) . . . . ? C41 Rh2 C42 C41 0.000(2) . . . . ? P2 Rh2 C42 C41 37.8(3) . . . . ? O4 Rh2 C42 C41 172.9(3) . . . . ? O5 Rh2 C42 C41 -156.0(3) . . . . ? C47 Rh2 C42 C41 -73.9(3) . . . . ? C40 Rh2 C42 C43 -3.6(5) . . . . ? C41 Rh2 C42 C43 37.5(5) . . . . ? P2 Rh2 C42 C43 75.3(6) . . . . ? O4 Rh2 C42 C43 -149.6(5) . . . . ? O5 Rh2 C42 C43 -118.5(6) . . . . ? C47 Rh2 C42 C43 -36.4(5) . . . . ? C41 C42 C43 C44 76.8(5) . . . . ? Rh2 C42 C43 C44 52.0(7) . . . . ? C42 C43 C44 C45 -75.5(5) . . . . ? C43 C44 C45 C46 102.2(5) . . . . ? C44 C45 C46 C47 -53.0(5) . . . . ? C41 C40 C47 C46 93.7(4) . . . . ? Rh2 C40 C47 C46 173.8(3) . . . . ? C41 C40 C47 Rh2 -80.1(4) . . . . ? Rh2 C40 C47 Rh2 0.0 . . . . ? C45 C46 C47 C40 -50.7(5) . . . . ? C45 C46 C47 Rh2 -41.8(7) . . . . ? C40 Rh2 C47 C40 0.0 . . . . ? C41 Rh2 C47 C40 41.0(3) . . . . ? P2 Rh2 C47 C40 -34.9(3) . . . . ? O4 Rh2 C47 C40 -162.2(2) . . . . ? O5 Rh2 C47 C40 154.7(3) . . . . ? C42 Rh2 C47 C40 72.4(3) . . . . ? C40 Rh2 C47 C46 -12.6(5) . . . . ? C41 Rh2 C47 C46 28.4(5) . . . . ? P2 Rh2 C47 C46 -47.5(6) . . . . ? O4 Rh2 C47 C46 -174.8(5) . . . . ? O5 Rh2 C47 C46 142.1(6) . . . . ? C42 Rh2 C47 C46 59.8(6) . . . . ? _refine_diff_density_max 0.719 _refine_diff_density_min -0.766 _refine_diff_density_rms 0.091 #===END data_31 _publ_section_exptl_prep ; "Crystals grown from benzene at romm temperature" ; _publ_section_exptl_refinement ; Two independent molecules in the asymetric unit ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C48 H82 F6 O6 P2 Rh2 S2' _chemical_formula_weight 1201.02 _chemical_melting_point 67_C _chemical_compound_source ? 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' 'F' 'F' 0.0171 0.0103 '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' -1.2870 0.9190 '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_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.042(4) _cell_length_b 15.347(4) _cell_length_c 15.532(2) _cell_angle_alpha 63.12(2) _cell_angle_beta 73.03(2) _cell_angle_gamma 70.98(2) _cell_volume 2780.8(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method ? _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; empirical absorption correction by psi-scans from 5 reflections with chi-angles near 90 degrees ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'CAD4 (Enraf-Nonius)' _diffrn_measurement_method 'Omega/Theta scans' _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 16.9 _diffrn_reflns_number 9104 _diffrn_reflns_av_R_equivalents 0.0096 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 23.98 _reflns_number_total 8703 _reflns_number_observed 7718 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius)' _computing_cell_refinement 'CAD4 (Enraf-Nonius)' _computing_data_reduction 'BEGIN (SDP)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R- factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R-factor(obs) 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 w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+2.5370P] 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 refxyz _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0060(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8701 _refine_ls_number_parameters 624 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_obs 0.0294 _refine_ls_wR_factor_all 0.0751 _refine_ls_wR_factor_obs 0.0704 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.055 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Rh1 Rh 0.01783(2) 0.40262(2) 0.78189(2) 0.03392(8) Uani 1 d . . Rh2 Rh 0.38485(2) 0.75402(2) 0.49050(2) 0.04035(8) Uani 1 d . . S1 S -0.13662(8) 0.80217(7) 0.49241(7) 0.0655(3) Uani 1 d . . S2 S 0.42184(6) 0.37289(7) 0.84406(6) 0.0573(2) Uani 1 d . . P1 P -0.15269(5) 0.45275(5) 0.83748(5) 0.0374(2) Uani 1 d . . P2 P 0.40175(6) 0.89795(5) 0.35400(5) 0.0373(2) Uani 1 d . . O1 O -0.1248(3) 0.7612(2) 0.5930(2) 0.0971(10) Uani 1 d . . O2 O -0.2050(3) 0.8977(2) 0.4622(2) 0.0985(10) Uani 1 d . . O3 O -0.1454(3) 0.7296(3) 0.4653(3) 0.1227(13) Uani 1 d . . O4 O 0.3353(2) 0.4508(2) 0.8508(2) 0.0939(9) Uani 1 d . . O5 O 0.4023(2) 0.3074(3) 0.8109(2) 0.0912(9) Uani 1 d . . O6 O 0.5180(2) 0.3986(3) 0.7996(2) 0.1047(12) Uani 1 d . . F1 F 0.0099(3) 0.8892(4) 0.4490(3) 0.166(2) Uani 1 d . . F2 F -0.0073(3) 0.8684(3) 0.3323(2) 0.1339(12) Uani 1 d . . F3 F 0.0606(3) 0.7438(3) 0.4497(3) 0.169(2) Uani 1 d . . F4 F 0.4455(2) 0.3416(3) 1.0166(2) 0.1174(10) Uani 1 d . . F5 F 0.3530(2) 0.2570(3) 1.0194(2) 0.1182(11) Uani 1 d . . F6 F 0.5157(2) 0.2175(2) 0.9776(2) 0.1064(9) Uani 1 d . . C1 C -0.0126(4) 0.8254(4) 0.4275(4) 0.0939(14) Uani 1 d . . C2 C 0.4345(3) 0.2918(3) 0.9697(3) 0.0662(10) Uani 1 d . . C10 C -0.2214(2) 0.5408(2) 0.7334(2) 0.0506(8) Uani 1 d . . H10 H -0.1842(2) 0.5946(2) 0.6964(2) 0.061 Uiso 1 calc R . C11 C -0.2236(2) 0.3531(3) 0.9196(3) 0.0560(9) Uani 1 d . . H11 H -0.1787(2) 0.3022(3) 0.9658(3) 0.067 Uiso 1 calc R . C12 C -0.1754(2) 0.5279(2) 0.9104(2) 0.0483(7) Uani 1 d . . H12 H -0.2496(2) 0.5462(2) 0.9308(2) 0.058 Uiso 1 calc R . C13 C -0.2155(3) 0.4970(3) 0.6606(3) 0.0716(11) Uani 1 d . . H13A H -0.1507(9) 0.4507(17) 0.6565(16) 0.107 Uiso 1 calc R . H13B H -0.2224(22) 0.5502(4) 0.5973(5) 0.107 Uiso 1 calc R . H13C H -0.2696(14) 0.4625(18) 0.6824(11) 0.107 Uiso 1 calc R . C14 C -0.3323(3) 0.5940(3) 0.7603(3) 0.0783(12) Uani 1 d . . H14A H -0.3351(5) 0.6220(20) 0.8054(18) 0.117 Uiso 1 calc R . H14B H -0.3750(5) 0.5465(6) 0.7902(20) 0.117 Uiso 1 calc R . H14C H -0.3560(8) 0.6467(15) 0.7021(4) 0.117 Uiso 1 calc R . C15 C -0.2430(3) 0.2996(3) 0.8657(3) 0.0759(12) Uani 1 d . . H15A H -0.2579(23) 0.2362(10) 0.9120(4) 0.114 Uiso 1 calc R . H15B H -0.1832(9) 0.2889(20) 0.8189(16) 0.114 Uiso 1 calc R . H15C H -0.2999(15) 0.3403(11) 0.8323(18) 0.114 Uiso 1 calc R . C16 C -0.3240(3) 0.3851(3) 0.9825(3) 0.0798(13) Uani 1 d . . H16A H -0.3106(4) 0.4119(22) 1.0218(17) 0.120 Uiso 1 calc R . H16B H -0.3531(12) 0.3280(6) 1.0244(17) 0.120 Uiso 1 calc R . H16C H -0.3712(9) 0.4354(17) 0.9407(3) 0.120 Uiso 1 calc R . C17 C -0.1286(3) 0.4677(3) 1.0039(2) 0.0616(9) Uani 1 d . . H17A H -0.1539(15) 0.4077(10) 1.0416(9) 0.092 Uiso 1 calc R . H17B H -0.1469(17) 0.5075(8) 1.0419(9) 0.092 Uiso 1 calc R . H17C H -0.0555(3) 0.4501(17) 0.9868(2) 0.092 Uiso 1 calc R . C18 C -0.1393(3) 0.6252(3) 0.8529(3) 0.0694(10) Uani 1 d . . H18A H -0.1634(18) 0.6599(10) 0.7914(9) 0.104 Uiso 1 calc R . H18B H -0.0659(3) 0.6105(3) 0.8411(18) 0.104 Uiso 1 calc R . H18C H -0.1656(18) 0.6666(9) 0.8897(9) 0.104 Uiso 1 calc R . C20 C 0.4039(3) 0.8816(3) 0.2426(2) 0.0599(9) Uani 1 d . . H20 H 0.4597(3) 0.8231(3) 0.2427(2) 0.072 Uiso 1 calc R . C21 C 0.3094(3) 1.0163(2) 0.3540(2) 0.0504(8) Uani 1 d . . H21 H 0.2965(3) 1.0120(2) 0.4212(2) 0.060 Uiso 1 calc R . C22 C 0.5278(3) 0.9262(3) 0.3314(3) 0.0587(9) Uani 1 d . . H22 H 0.5274(3) 0.9913(3) 0.2760(3) 0.070 Uiso 1 calc R . C23 C 0.4308(4) 0.9674(3) 0.1457(3) 0.094(2) Uani 1 d . . H23A H 0.4949(14) 0.9787(18) 0.1436(12) 0.141 Uiso 1 calc R . H23B H 0.3783(14) 1.0273(8) 0.1406(12) 0.141 Uiso 1 calc R . H23C H 0.4361(28) 0.9500(12) 0.0921(3) 0.141 Uiso 1 calc R . C24 C 0.3079(4) 0.8540(3) 0.2438(3) 0.0883(14) Uani 1 d . . H24A H 0.2816(15) 0.8139(21) 0.3098(5) 0.132 Uiso 1 calc R . H24B H 0.3248(6) 0.8166(22) 0.2037(20) 0.132 Uiso 1 calc R . H24C H 0.2570(10) 0.9141(4) 0.2187(23) 0.132 Uiso 1 calc R . C25 C 0.3469(4) 1.1137(3) 0.2881(3) 0.0876(15) Uani 1 d . . H25A H 0.3573(25) 1.1237(14) 0.2206(3) 0.131 Uiso 1 calc R . H25B H 0.4101(14) 1.1086(10) 0.3040(17) 0.131 Uiso 1 calc R . H25C H 0.2966(12) 1.1695(4) 0.2985(19) 0.131 Uiso 1 calc R . C26 C 0.2054(3) 1.0268(3) 0.3329(3) 0.0745(11) Uani 1 d . . H26A H 0.1544(5) 1.0741(17) 0.3565(20) 0.112 Uiso 1 calc R . H26B H 0.1874(11) 0.9629(6) 0.3654(18) 0.112 Uiso 1 calc R . H26C H 0.2091(7) 1.0502(22) 0.2636(3) 0.112 Uiso 1 calc R . C27 C 0.6192(3) 0.8516(3) 0.3036(4) 0.0861(13) Uani 1 d . . H27A H 0.6099(12) 0.8450(19) 0.2482(16) 0.129 Uiso 1 calc R . H27B H 0.6252(15) 0.7876(7) 0.3579(9) 0.129 Uiso 1 calc R . H27C H 0.6803(4) 0.8752(13) 0.2871(24) 0.129 Uiso 1 calc R . C28 C 0.5420(3) 0.9379(4) 0.4193(3) 0.0854(13) Uani 1 d . . H28A H 0.4863(14) 0.9885(18) 0.4336(16) 0.128 Uiso 1 calc R . H28B H 0.6052(13) 0.9574(25) 0.4043(10) 0.128 Uiso 1 calc R . H28C H 0.5433(26) 0.8753(7) 0.4752(7) 0.128 Uiso 1 calc R . C30 C 0.0221(2) 0.2459(2) 0.8631(2) 0.0425(7) Uani 1 d . . C31 C 0.0358(2) 0.2854(2) 0.9231(2) 0.0368(6) Uani 1 d . . C32 C 0.1352(2) 0.2583(2) 0.9574(2) 0.0493(8) Uani 1 d . . H32A H 0.1432(2) 0.3146(2) 0.9653(2) 0.059 Uiso 1 calc R . H32B H 0.1917(2) 0.2431(2) 0.9089(2) 0.059 Uiso 1 calc R . C33 C 0.1371(3) 0.1670(3) 1.0552(3) 0.0725(11) Uani 1 d . . H33A H 0.2056(3) 0.1444(3) 1.0704(3) 0.087 Uiso 1 calc R . H33B H 0.0914(3) 0.1882(3) 1.1060(3) 0.087 Uiso 1 calc R . C34 C 0.1069(4) 0.0785(3) 1.0594(3) 0.0853(13) Uani 1 d . . H34A H 0.1121(4) 0.0252(3) 1.1239(3) 0.102 Uiso 1 calc R . H34B H 0.0357(4) 0.0990(3) 1.0520(3) 0.102 Uiso 1 calc R . C35 C 0.1683(4) 0.0366(3) 0.9846(4) 0.108(2) Uani 1 d . . H35A H 0.1843(4) -0.0360(3) 1.0172(4) 0.130 Uiso 1 calc R . H35B H 0.2326(4) 0.0576(3) 0.9603(4) 0.130 Uiso 1 calc R . C36 C 0.1189(4) 0.0659(3) 0.8954(4) 0.0905(15) Uani 1 d . . H36A H 0.1600(4) 0.0243(3) 0.8597(4) 0.109 Uiso 1 calc R . H36B H 0.0518(4) 0.0506(3) 0.9194(4) 0.109 Uiso 1 calc R . C37 C 0.1069(3) 0.1765(2) 0.8234(3) 0.0619(9) Uani 1 d . . H37A H 0.1707(3) 0.1962(2) 0.8088(3) 0.074 Uiso 1 calc R . H37B H 0.0932(3) 0.1835(2) 0.7626(3) 0.074 Uiso 1 calc R . C40 C 0.2518(2) 0.8272(2) 0.5635(2) 0.0456(7) Uani 1 d . . C41 C 0.3388(3) 0.8341(2) 0.5841(2) 0.0481(8) Uani 1 d . . C42 C 0.3735(3) 0.7779(3) 0.6828(3) 0.0716(11) Uani 1 d . . H42A H 0.4464(3) 0.7718(3) 0.6738(3) 0.086 Uiso 1 calc R . H42B H 0.3613(3) 0.7109(3) 0.7124(3) 0.086 Uiso 1 calc R . C43 C 0.3152(5) 0.8334(4) 0.7525(3) 0.110(2) Uani 1 d . . H43A H 0.3140(5) 0.9043(4) 0.7163(3) 0.132 Uiso 1 calc R . H43B H 0.3529(5) 0.8087(4) 0.8054(3) 0.132 Uiso 1 calc R . C44 C 0.2025(6) 0.8208(4) 0.7978(3) 0.123(2) Uani 1 d . . H44A H 0.2024(6) 0.7505(4) 0.8218(3) 0.148 Uiso 1 calc R . H44B H 0.1799(6) 0.8393(4) 0.8538(3) 0.148 Uiso 1 calc R . C45 C 0.1268(5) 0.8808(4) 0.7300(4) 0.126(2) Uani 1 d . . H45A H 0.0662(5) 0.9130(4) 0.7637(4) 0.151 Uiso 1 calc R . H45B H 0.1558(5) 0.9334(4) 0.6744(4) 0.151 Uiso 1 calc R . C46 C 0.0958(4) 0.8220(4) 0.6933(4) 0.103(2) Uani 1 d . . H46A H 0.0477(4) 0.8678(4) 0.6495(4) 0.124 Uiso 1 calc R . H46B H 0.0596(4) 0.7750(4) 0.7486(4) 0.124 Uiso 1 calc R . C47 C 0.1800(3) 0.7636(3) 0.6399(3) 0.0671(10) Uani 1 d . . H47A H 0.2183(3) 0.7058(3) 0.6869(3) 0.080 Uiso 1 calc R . H47B H 0.1497(3) 0.7394(3) 0.6087(3) 0.080 Uiso 1 calc R . C50 C 0.1387(4) 0.4969(4) 0.7344(3) 0.090(2) Uani 1 d . . H50 H 0.1599(4) 0.5145(4) 0.7746(3) 0.108 Uiso 1 calc R . C51 C 0.1883(2) 0.4050(3) 0.7187(3) 0.0671(11) Uani 1 d . . H51 H 0.2424(2) 0.3602(3) 0.7504(3) 0.080 Uiso 1 calc R . C52 C 0.1552(3) 0.3853(3) 0.6577(3) 0.0686(10) Uani 1 d . . H52 H 0.1893(3) 0.3272(3) 0.6467(3) 0.082 Uiso 1 calc R . C53 C 0.0760(3) 0.4445(3) 0.6123(3) 0.0697(10) Uani 1 d . . H53 H 0.0556(3) 0.4270(3) 0.5716(3) 0.084 Uiso 1 calc R . C54 C 0.0270(3) 0.5281(3) 0.6253(2) 0.0607(9) Uani 1 d . . H54 H -0.0287(3) 0.5677(3) 0.5937(2) 0.073 Uiso 1 calc R . C55 C 0.0532(3) 0.5598(3) 0.6824(3) 0.0654(10) Uani 1 d . . H55 H 0.0174(3) 0.6202(3) 0.6882(3) 0.078 Uiso 1 calc R . C60 C 0.4080(5) 0.6351(3) 0.4275(3) 0.090(2) Uani 1 d . . H60 H 0.3874(5) 0.6451(3) 0.3713(3) 0.108 Uiso 1 calc R . C61 C 0.3424(4) 0.6060(3) 0.5202(4) 0.0884(14) Uani 1 d . . H61 H 0.2777(4) 0.5976(3) 0.5263(4) 0.106 Uiso 1 calc R . C62 C 0.3791(4) 0.5906(2) 0.6009(3) 0.0743(12) Uani 1 d . . H62 H 0.3371(4) 0.5736(2) 0.6620(3) 0.089 Uiso 1 calc R . C63 C 0.4756(4) 0.5996(3) 0.5935(3) 0.0801(13) Uani 1 d . . H63 H 0.4987(4) 0.5857(3) 0.6497(3) 0.096 Uiso 1 calc R . C64 C 0.5384(4) 0.6289(3) 0.5042(3) 0.0870(14) Uani 1 d . . H64 H 0.6036(4) 0.6354(3) 0.4993(3) 0.104 Uiso 1 calc R . C65 C 0.5029(4) 0.6484(3) 0.4223(3) 0.0829(14) Uani 1 d . . H65 H 0.5439(4) 0.6713(3) 0.3613(3) 0.100 Uiso 1 calc R . H30 H -0.0419(24) 0.2368(22) 0.8700(21) 0.045(8) Uiso 1 d . . H40 H 0.2206(22) 0.8827(22) 0.5163(21) 0.038(8) Uiso 1 d . . H41 H 0.3609(23) 0.8957(24) 0.5476(22) 0.046(8) Uiso 1 d . . H31 H -0.0245(21) 0.2995(20) 0.9717(20) 0.035(7) Uiso 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 0.03205(13) 0.03221(13) 0.03493(13) -0.01032(9) -0.00849(9) -0.00600(9) Rh2 0.04713(15) 0.02709(12) 0.03782(14) -0.01064(10) -0.00387(10) -0.00349(10) S1 0.0841(7) 0.0431(5) 0.0663(6) -0.0206(4) -0.0171(5) -0.0084(4) S2 0.0414(4) 0.0720(6) 0.0494(5) -0.0211(4) -0.0086(4) -0.0052(4) P1 0.0310(4) 0.0378(4) 0.0424(4) -0.0127(3) -0.0115(3) -0.0064(3) P2 0.0406(4) 0.0290(4) 0.0352(4) -0.0119(3) -0.0027(3) -0.0036(3) O1 0.132(3) 0.071(2) 0.061(2) -0.0175(15) -0.018(2) 0.000(2) O2 0.097(2) 0.062(2) 0.105(2) -0.013(2) -0.031(2) 0.004(2) O3 0.167(4) 0.106(3) 0.134(3) -0.074(2) -0.006(3) -0.056(3) O4 0.079(2) 0.089(2) 0.097(2) -0.042(2) -0.025(2) 0.019(2) O5 0.082(2) 0.124(3) 0.092(2) -0.072(2) -0.026(2) 0.000(2) O6 0.061(2) 0.140(3) 0.072(2) 0.005(2) -0.0100(15) -0.043(2) F1 0.171(4) 0.191(4) 0.170(4) -0.045(3) -0.048(3) -0.107(3) F2 0.144(3) 0.147(3) 0.072(2) -0.013(2) 0.000(2) -0.046(2) F3 0.092(2) 0.143(3) 0.159(3) -0.005(3) 0.000(2) 0.016(2) F4 0.117(2) 0.179(3) 0.092(2) -0.076(2) -0.029(2) -0.035(2) F5 0.088(2) 0.164(3) 0.073(2) -0.003(2) 0.0003(14) -0.070(2) F6 0.088(2) 0.097(2) 0.089(2) -0.0092(15) -0.0318(15) 0.009(2) C1 0.089(3) 0.089(3) 0.080(3) -0.010(3) -0.024(3) -0.018(3) C2 0.048(2) 0.087(3) 0.057(2) -0.024(2) -0.004(2) -0.018(2) C10 0.045(2) 0.049(2) 0.052(2) -0.0097(15) -0.0235(15) -0.0055(14) C11 0.042(2) 0.053(2) 0.064(2) -0.007(2) -0.015(2) -0.019(2) C12 0.039(2) 0.054(2) 0.051(2) -0.027(2) -0.0043(14) -0.0024(14) C13 0.075(3) 0.079(3) 0.069(2) -0.022(2) -0.036(2) -0.016(2) C14 0.051(2) 0.078(3) 0.086(3) -0.018(2) -0.033(2) 0.008(2) C15 0.065(2) 0.062(2) 0.109(3) -0.019(2) -0.039(2) -0.026(2) C16 0.040(2) 0.085(3) 0.083(3) -0.005(2) -0.001(2) -0.024(2) C17 0.067(2) 0.072(2) 0.054(2) -0.038(2) -0.012(2) -0.007(2) C18 0.090(3) 0.055(2) 0.071(2) -0.037(2) -0.005(2) -0.018(2) C20 0.079(2) 0.051(2) 0.046(2) -0.024(2) -0.015(2) 0.001(2) C21 0.060(2) 0.031(2) 0.041(2) -0.0115(13) -0.0009(14) 0.0022(14) C22 0.048(2) 0.058(2) 0.066(2) -0.026(2) 0.009(2) -0.022(2) C23 0.140(4) 0.076(3) 0.040(2) -0.016(2) -0.014(2) -0.006(3) C24 0.106(4) 0.090(3) 0.095(3) -0.052(3) -0.051(3) -0.003(3) C25 0.109(3) 0.031(2) 0.080(3) -0.011(2) 0.016(2) -0.009(2) C26 0.062(2) 0.072(3) 0.065(2) -0.024(2) -0.021(2) 0.019(2) C27 0.044(2) 0.092(3) 0.115(4) -0.051(3) 0.007(2) -0.011(2) C28 0.069(3) 0.123(4) 0.093(3) -0.056(3) 0.003(2) -0.052(3) C30 0.044(2) 0.036(2) 0.046(2) -0.0125(13) -0.0107(14) -0.0107(13) C31 0.036(2) 0.0335(14) 0.0353(15) -0.0089(12) -0.0076(12) -0.0062(12) C32 0.047(2) 0.052(2) 0.045(2) -0.0090(14) -0.0180(14) -0.0125(15) C33 0.065(2) 0.075(3) 0.057(2) 0.005(2) -0.031(2) -0.018(2) C34 0.081(3) 0.059(2) 0.069(3) 0.010(2) -0.014(2) -0.009(2) C35 0.116(4) 0.042(2) 0.101(4) -0.001(2) -0.010(3) 0.015(2) C36 0.114(4) 0.041(2) 0.100(3) -0.034(2) 0.006(3) -0.009(2) C37 0.082(3) 0.044(2) 0.060(2) -0.027(2) -0.005(2) -0.012(2) C40 0.050(2) 0.034(2) 0.040(2) -0.0119(14) 0.0025(14) -0.0064(14) C41 0.065(2) 0.039(2) 0.037(2) -0.0131(14) -0.0009(15) -0.017(2) C42 0.095(3) 0.072(2) 0.048(2) -0.016(2) -0.019(2) -0.024(2) C43 0.216(7) 0.095(3) 0.040(2) -0.021(2) -0.013(3) -0.078(4) C44 0.209(7) 0.075(3) 0.045(2) -0.022(2) 0.021(3) -0.023(4) C45 0.158(6) 0.068(3) 0.091(4) -0.031(3) 0.058(4) -0.020(3) C46 0.085(3) 0.082(3) 0.096(3) -0.029(3) 0.044(3) -0.022(3) C47 0.063(2) 0.059(2) 0.066(2) -0.020(2) 0.011(2) -0.025(2) C50 0.114(4) 0.143(4) 0.049(2) -0.030(3) 0.013(2) -0.110(4) C51 0.033(2) 0.078(3) 0.055(2) 0.004(2) -0.003(2) -0.018(2) C52 0.063(2) 0.068(2) 0.057(2) -0.024(2) 0.013(2) -0.016(2) C53 0.082(3) 0.073(3) 0.042(2) -0.016(2) -0.002(2) -0.020(2) C54 0.064(2) 0.056(2) 0.043(2) 0.001(2) -0.013(2) -0.015(2) C55 0.079(3) 0.040(2) 0.060(2) -0.013(2) 0.012(2) -0.023(2) C60 0.156(5) 0.037(2) 0.080(3) -0.031(2) -0.033(3) -0.003(3) C61 0.129(4) 0.037(2) 0.103(4) -0.024(2) -0.022(3) -0.027(2) C62 0.103(3) 0.026(2) 0.065(2) -0.007(2) 0.001(2) -0.006(2) C63 0.092(3) 0.041(2) 0.070(3) -0.008(2) -0.021(2) 0.016(2) C64 0.075(3) 0.055(2) 0.082(3) -0.012(2) -0.012(2) 0.022(2) C65 0.109(4) 0.039(2) 0.069(3) -0.026(2) 0.008(3) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C31 2.138(3) . ? Rh1 C30 2.141(3) . ? Rh1 P1 2.2942(10) . ? Rh1 C51 2.313(3) . ? Rh1 C54 2.320(3) . ? Rh1 C55 2.328(3) . ? Rh1 C50 2.330(3) . ? Rh1 C52 2.338(4) . ? Rh1 C53 2.361(4) . ? Rh2 C40 2.141(3) . ? Rh2 C41 2.143(3) . ? Rh2 P2 2.2901(10) . ? Rh2 C65 2.296(4) . ? Rh2 C62 2.324(3) . ? Rh2 C60 2.332(4) . ? Rh2 C61 2.346(4) . ? Rh2 C64 2.362(4) . ? Rh2 C63 2.365(4) . ? S1 O3 1.405(3) . ? S1 O2 1.420(3) . ? S1 O1 1.435(3) . ? S1 C1 1.798(5) . ? S2 O4 1.417(3) . ? S2 O6 1.419(3) . ? S2 O5 1.443(3) . ? S2 C2 1.804(4) . ? P1 C12 1.856(3) . ? P1 C11 1.856(3) . ? P1 C10 1.859(3) . ? P2 C20 1.849(3) . ? P2 C22 1.856(3) . ? P2 C21 1.857(3) . ? F1 C1 1.316(6) . ? F2 C1 1.309(5) . ? F3 C1 1.312(6) . ? F4 C2 1.334(5) . ? F5 C2 1.305(4) . ? F6 C2 1.313(4) . ? C10 C13 1.527(5) . ? C10 C14 1.538(5) . ? C11 C15 1.534(5) . ? C11 C16 1.537(5) . ? C12 C18 1.519(5) . ? C12 C17 1.531(5) . ? C20 C23 1.530(5) . ? C20 C24 1.532(6) . ? C21 C26 1.531(5) . ? C21 C25 1.541(5) . ? C22 C27 1.519(5) . ? C22 C28 1.530(5) . ? C30 C31 1.403(4) . ? C30 C37 1.506(4) . ? C31 C32 1.504(4) . ? C32 C33 1.531(4) . ? C33 C34 1.521(6) . ? C34 C35 1.495(6) . ? C35 C36 1.548(7) . ? C36 C37 1.539(5) . ? C40 C41 1.396(5) . ? C40 C47 1.507(4) . ? C41 C42 1.516(5) . ? C42 C43 1.558(6) . ? C43 C44 1.570(8) . ? C44 C45 1.492(9) . ? C45 C46 1.481(8) . ? C46 C47 1.516(5) . ? C50 C51 1.452(6) . ? C50 C55 1.459(6) . ? C51 C52 1.347(6) . ? C52 C53 1.333(6) . ? C53 C54 1.318(5) . ? C54 C55 1.363(5) . ? C60 C65 1.388(7) . ? C60 C61 1.426(7) . ? C61 C62 1.387(6) . ? C62 C63 1.373(6) . ? C63 C64 1.372(6) . ? C64 C65 1.373(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 C31 Rh1 C30 38.27(11) . . ? C31 Rh1 P1 90.43(8) . . ? C30 Rh1 P1 94.43(9) . . ? C31 Rh1 C51 98.38(12) . . ? C30 Rh1 C51 102.90(14) . . ? P1 Rh1 C51 161.03(12) . . ? C31 Rh1 C54 170.49(12) . . ? C30 Rh1 C54 143.74(13) . . ? P1 Rh1 C54 98.19(10) . . ? C51 Rh1 C54 72.21(13) . . ? C31 Rh1 C55 140.54(14) . . ? C30 Rh1 C55 166.76(13) . . ? P1 Rh1 C55 98.80(10) . . ? C51 Rh1 C55 63.93(14) . . ? C54 Rh1 C55 34.11(14) . . ? C31 Rh1 C50 108.75(14) . . ? C30 Rh1 C50 132.5(2) . . ? P1 Rh1 C50 124.7(2) . . ? C51 Rh1 C50 36.4(2) . . ? C54 Rh1 C50 62.93(15) . . ? C55 Rh1 C50 36.5(2) . . ? C31 Rh1 C52 113.84(13) . . ? C30 Rh1 C52 96.55(13) . . ? P1 Rh1 C52 151.99(11) . . ? C51 Rh1 C52 33.65(14) . . ? C54 Rh1 C52 58.96(14) . . ? C55 Rh1 C52 71.78(14) . . ? C50 Rh1 C52 62.3(2) . . ? C31 Rh1 C53 143.28(13) . . ? C30 Rh1 C53 112.83(13) . . ? P1 Rh1 C53 119.31(11) . . ? C51 Rh1 C53 60.67(15) . . ? C54 Rh1 C53 32.70(13) . . ? C55 Rh1 C53 60.56(14) . . ? C50 Rh1 C53 73.26(14) . . ? C52 Rh1 C53 32.96(14) . . ? C40 Rh2 C41 38.05(13) . . ? C40 Rh2 P2 93.92(9) . . ? C41 Rh2 P2 91.35(9) . . ? C40 Rh2 C65 165.8(2) . . ? C41 Rh2 C65 152.1(2) . . ? P2 Rh2 C65 95.21(11) . . ? C40 Rh2 C62 96.92(13) . . ? C41 Rh2 C62 102.70(14) . . ? P2 Rh2 C62 165.95(11) . . ? C65 Rh2 C62 72.53(15) . . ? C40 Rh2 C60 131.8(2) . . ? C41 Rh2 C60 163.2(2) . . ? P2 Rh2 C60 103.90(12) . . ? C65 Rh2 C60 34.9(2) . . ? C62 Rh2 C60 62.1(2) . . ? C40 Rh2 C61 103.0(2) . . ? C41 Rh2 C61 127.7(2) . . ? P2 Rh2 C61 133.59(13) . . ? C65 Rh2 C61 62.9(2) . . ? C62 Rh2 C61 34.6(2) . . ? C60 Rh2 C61 35.5(2) . . ? C40 Rh2 C64 147.42(15) . . ? C41 Rh2 C64 118.9(2) . . ? P2 Rh2 C64 112.20(12) . . ? C65 Rh2 C64 34.3(2) . . ? C62 Rh2 C64 61.3(2) . . ? C60 Rh2 C64 62.0(2) . . ? C61 Rh2 C64 73.4(2) . . ? C40 Rh2 C63 115.38(14) . . ? C41 Rh2 C63 99.42(14) . . ? P2 Rh2 C63 144.31(13) . . ? C65 Rh2 C63 60.8(2) . . ? C62 Rh2 C63 34.0(2) . . ? C60 Rh2 C63 72.3(2) . . ? C61 Rh2 C63 61.7(2) . . ? C64 Rh2 C63 33.75(15) . . ? O3 S1 O2 118.0(2) . . ? O3 S1 O1 112.0(2) . . ? O2 S1 O1 114.0(2) . . ? O3 S1 C1 103.1(3) . . ? O2 S1 C1 104.9(2) . . ? O1 S1 C1 102.7(2) . . ? O4 S2 O6 117.9(2) . . ? O4 S2 O5 112.5(2) . . ? O6 S2 O5 113.5(2) . . ? O4 S2 C2 104.2(2) . . ? O6 S2 C2 104.8(2) . . ? O5 S2 C2 101.8(2) . . ? C12 P1 C11 103.1(2) . . ? C12 P1 C10 103.16(15) . . ? C11 P1 C10 108.9(2) . . ? C12 P1 Rh1 112.38(10) . . ? C11 P1 Rh1 117.38(12) . . ? C10 P1 Rh1 110.73(11) . . ? C20 P2 C22 103.2(2) . . ? C20 P2 C21 109.4(2) . . ? C22 P2 C21 103.4(2) . . ? C20 P2 Rh2 110.70(12) . . ? C22 P2 Rh2 111.30(12) . . ? C21 P2 Rh2 117.65(10) . . ? F2 C1 F3 109.2(5) . . ? F2 C1 F1 104.0(5) . . ? F3 C1 F1 106.6(5) . . ? F2 C1 S1 113.2(4) . . ? F3 C1 S1 112.5(4) . . ? F1 C1 S1 110.8(4) . . ? F5 C2 F6 110.0(4) . . ? F5 C2 F4 105.1(3) . . ? F6 C2 F4 105.4(3) . . ? F5 C2 S2 112.0(3) . . ? F6 C2 S2 112.6(3) . . ? F4 C2 S2 111.2(3) . . ? C13 C10 C14 110.1(3) . . ? C13 C10 P1 114.2(2) . . ? C14 C10 P1 116.2(2) . . ? C15 C11 C16 109.5(3) . . ? C15 C11 P1 112.9(3) . . ? C16 C11 P1 115.8(3) . . ? C18 C12 C17 109.6(3) . . ? C18 C12 P1 113.7(2) . . ? C17 C12 P1 112.3(2) . . ? C23 C20 C24 110.8(3) . . ? C23 C20 P2 115.1(3) . . ? C24 C20 P2 113.9(3) . . ? C26 C21 C25 109.5(3) . . ? C26 C21 P2 113.0(2) . . ? C25 C21 P2 116.1(2) . . ? C27 C22 C28 110.0(4) . . ? C27 C22 P2 115.0(3) . . ? C28 C22 P2 110.7(2) . . ? C31 C30 C37 123.0(3) . . ? C31 C30 Rh1 70.7(2) . . ? C37 C30 Rh1 115.5(2) . . ? C30 C31 C32 122.8(3) . . ? C30 C31 Rh1 71.0(2) . . ? C32 C31 Rh1 117.9(2) . . ? C31 C32 C33 110.0(3) . . ? C34 C33 C32 115.7(3) . . ? C35 C34 C33 115.9(4) . . ? C34 C35 C36 116.8(4) . . ? C37 C36 C35 115.5(4) . . ? C30 C37 C36 112.7(3) . . ? C41 C40 C47 122.6(3) . . ? C41 C40 Rh2 71.0(2) . . ? C47 C40 Rh2 117.3(2) . . ? C40 C41 C42 124.8(3) . . ? C40 C41 Rh2 70.9(2) . . ? C42 C41 Rh2 116.2(2) . . ? C41 C42 C43 111.0(3) . . ? C42 C43 C44 114.5(4) . . ? C45 C44 C43 115.5(4) . . ? C46 C45 C44 114.5(5) . . ? C45 C46 C47 117.2(4) . . ? C40 C47 C46 111.7(3) . . ? C51 C50 C55 115.1(3) . . ? C51 C50 Rh1 71.1(2) . . ? C55 C50 Rh1 71.7(2) . . ? C52 C51 C50 119.4(4) . . ? C52 C51 Rh1 74.2(2) . . ? C50 C51 Rh1 72.4(2) . . ? C53 C52 C51 123.5(4) . . ? C53 C52 Rh1 74.5(2) . . ? C51 C52 Rh1 72.1(2) . . ? C54 C53 C52 119.7(4) . . ? C54 C53 Rh1 72.0(2) . . ? C52 C53 Rh1 72.6(2) . . ? C53 C54 C55 123.7(4) . . ? C53 C54 Rh1 75.4(2) . . ? C55 C54 Rh1 73.2(2) . . ? C54 C55 C50 118.6(4) . . ? C54 C55 Rh1 72.7(2) . . ? C50 C55 Rh1 71.8(2) . . ? C65 C60 C61 118.9(5) . . ? C65 C60 Rh2 71.1(2) . . ? C61 C60 Rh2 72.8(2) . . ? C62 C61 C60 117.3(5) . . ? C62 C61 Rh2 71.9(2) . . ? C60 C61 Rh2 71.7(2) . . ? C63 C62 C61 122.0(4) . . ? C63 C62 Rh2 74.6(2) . . ? C61 C62 Rh2 73.6(2) . . ? C64 C63 C62 120.9(5) . . ? C64 C63 Rh2 73.0(2) . . ? C62 C63 Rh2 71.4(2) . . ? C63 C64 C65 118.5(5) . . ? C63 C64 Rh2 73.2(2) . . ? C65 C64 Rh2 70.2(2) . . ? C64 C65 C60 122.3(4) . . ? C64 C65 Rh2 75.5(2) . . ? C60 C65 Rh2 74.0(2) . . ? 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 C31 Rh1 P1 C12 78.62(14) . . . . ? C30 Rh1 P1 C12 116.73(14) . . . . ? C51 Rh1 P1 C12 -39.4(3) . . . . ? C54 Rh1 P1 C12 -97.3(2) . . . . ? C55 Rh1 P1 C12 -62.9(2) . . . . ? C50 Rh1 P1 C12 -34.7(2) . . . . ? C52 Rh1 P1 C12 -130.4(2) . . . . ? C53 Rh1 P1 C12 -123.9(2) . . . . ? C31 Rh1 P1 C11 -40.7(2) . . . . ? C30 Rh1 P1 C11 -2.6(2) . . . . ? C51 Rh1 P1 C11 -158.7(3) . . . . ? C54 Rh1 P1 C11 143.3(2) . . . . ? C55 Rh1 P1 C11 177.8(2) . . . . ? C50 Rh1 P1 C11 -154.0(2) . . . . ? C52 Rh1 P1 C11 110.3(3) . . . . ? C53 Rh1 P1 C11 116.7(2) . . . . ? C31 Rh1 P1 C10 -166.60(14) . . . . ? C30 Rh1 P1 C10 -128.50(14) . . . . ? C51 Rh1 P1 C10 75.4(3) . . . . ? C54 Rh1 P1 C10 17.4(2) . . . . ? C55 Rh1 P1 C10 51.9(2) . . . . ? C50 Rh1 P1 C10 80.1(2) . . . . ? C52 Rh1 P1 C10 -15.6(3) . . . . ? C53 Rh1 P1 C10 -9.2(2) . . . . ? C40 Rh2 P2 C20 -124.6(2) . . . . ? C41 Rh2 P2 C20 -162.6(2) . . . . ? C65 Rh2 P2 C20 44.6(2) . . . . ? C62 Rh2 P2 C20 15.9(6) . . . . ? C60 Rh2 P2 C20 10.3(2) . . . . ? C61 Rh2 P2 C20 -12.5(2) . . . . ? C64 Rh2 P2 C20 75.4(2) . . . . ? C63 Rh2 P2 C20 89.2(2) . . . . ? C40 Rh2 P2 C22 121.2(2) . . . . ? C41 Rh2 P2 C22 83.2(2) . . . . ? C65 Rh2 P2 C22 -69.6(2) . . . . ? C62 Rh2 P2 C22 -98.3(5) . . . . ? C60 Rh2 P2 C22 -103.9(2) . . . . ? C61 Rh2 P2 C22 -126.7(2) . . . . ? C64 Rh2 P2 C22 -38.8(2) . . . . ? C63 Rh2 P2 C22 -25.0(2) . . . . ? C40 Rh2 P2 C21 2.2(2) . . . . ? C41 Rh2 P2 C21 -35.8(2) . . . . ? C65 Rh2 P2 C21 171.3(2) . . . . ? C62 Rh2 P2 C21 142.6(5) . . . . ? C60 Rh2 P2 C21 137.0(2) . . . . ? C61 Rh2 P2 C21 114.3(2) . . . . ? C64 Rh2 P2 C21 -157.9(2) . . . . ? C63 Rh2 P2 C21 -144.1(2) . . . . ? O3 S1 C1 F2 66.7(5) . . . . ? O2 S1 C1 F2 -57.3(5) . . . . ? O1 S1 C1 F2 -176.7(4) . . . . ? O3 S1 C1 F3 -57.7(5) . . . . ? O2 S1 C1 F3 178.3(4) . . . . ? O1 S1 C1 F3 58.8(5) . . . . ? O3 S1 C1 F1 -176.9(4) . . . . ? O2 S1 C1 F1 59.1(4) . . . . ? O1 S1 C1 F1 -60.4(4) . . . . ? O4 S2 C2 F5 59.2(4) . . . . ? O6 S2 C2 F5 -176.4(3) . . . . ? O5 S2 C2 F5 -58.0(4) . . . . ? O4 S2 C2 F6 -176.2(3) . . . . ? O6 S2 C2 F6 -51.7(4) . . . . ? O5 S2 C2 F6 66.7(3) . . . . ? O4 S2 C2 F4 -58.1(3) . . . . ? O6 S2 C2 F4 66.3(3) . . . . ? O5 S2 C2 F4 -175.2(3) . . . . ? C12 P1 C10 C13 -179.7(3) . . . . ? C11 P1 C10 C13 -70.7(3) . . . . ? Rh1 P1 C10 C13 59.8(3) . . . . ? C12 P1 C10 C14 -49.8(3) . . . . ? C11 P1 C10 C14 59.3(3) . . . . ? Rh1 P1 C10 C14 -170.2(2) . . . . ? C12 P1 C11 C15 163.2(2) . . . . ? C10 P1 C11 C15 54.1(3) . . . . ? Rh1 P1 C11 C15 -72.7(3) . . . . ? C12 P1 C11 C16 35.8(3) . . . . ? C10 P1 C11 C16 -73.2(3) . . . . ? Rh1 P1 C11 C16 160.0(2) . . . . ? C11 P1 C12 C18 -170.7(3) . . . . ? C10 P1 C12 C18 -57.3(3) . . . . ? Rh1 P1 C12 C18 62.0(3) . . . . ? C11 P1 C12 C17 64.2(3) . . . . ? C10 P1 C12 C17 177.6(2) . . . . ? Rh1 P1 C12 C17 -63.1(3) . . . . ? C22 P2 C20 C23 -52.1(3) . . . . ? C21 P2 C20 C23 57.5(3) . . . . ? Rh2 P2 C20 C23 -171.3(3) . . . . ? C22 P2 C20 C24 178.3(3) . . . . ? C21 P2 C20 C24 -72.1(3) . . . . ? Rh2 P2 C20 C24 59.1(3) . . . . ? C20 P2 C21 C26 48.9(3) . . . . ? C22 P2 C21 C26 158.3(2) . . . . ? Rh2 P2 C21 C26 -78.5(3) . . . . ? C20 P2 C21 C25 -78.8(3) . . . . ? C22 P2 C21 C25 30.7(3) . . . . ? Rh2 P2 C21 C25 153.9(3) . . . . ? C20 P2 C22 C27 -52.1(3) . . . . ? C21 P2 C22 C27 -166.1(3) . . . . ? Rh2 P2 C22 C27 66.6(3) . . . . ? C20 P2 C22 C28 -177.6(3) . . . . ? C21 P2 C22 C28 68.4(3) . . . . ? Rh2 P2 C22 C28 -58.8(3) . . . . ? C31 Rh1 C30 C31 0.0 . . . . ? P1 Rh1 C30 C31 -85.1(2) . . . . ? C51 Rh1 C30 C31 87.2(2) . . . . ? C54 Rh1 C30 C31 164.6(2) . . . . ? C55 Rh1 C30 C31 93.1(6) . . . . ? C50 Rh1 C30 C31 62.7(2) . . . . ? C52 Rh1 C30 C31 120.8(2) . . . . ? C53 Rh1 C30 C31 150.5(2) . . . . ? C31 Rh1 C30 C37 -118.2(3) . . . . ? P1 Rh1 C30 C37 156.8(2) . . . . ? C51 Rh1 C30 C37 -31.0(3) . . . . ? C54 Rh1 C30 C37 46.5(4) . . . . ? C55 Rh1 C30 C37 -25.0(7) . . . . ? C50 Rh1 C30 C37 -55.5(3) . . . . ? C52 Rh1 C30 C37 2.6(3) . . . . ? C53 Rh1 C30 C37 32.4(3) . . . . ? C37 C30 C31 C32 -3.0(4) . . . . ? Rh1 C30 C31 C32 -111.6(3) . . . . ? C37 C30 C31 Rh1 108.5(3) . . . . ? Rh1 C30 C31 Rh1 0.0 . . . . ? C30 Rh1 C31 C30 0.0 . . . . ? P1 Rh1 C31 C30 96.6(2) . . . . ? C51 Rh1 C31 C30 -100.2(2) . . . . ? C54 Rh1 C31 C30 -108.3(8) . . . . ? C55 Rh1 C31 C30 -158.9(2) . . . . ? C50 Rh1 C31 C30 -136.3(2) . . . . ? C52 Rh1 C31 C30 -69.0(2) . . . . ? C53 Rh1 C31 C30 -49.3(3) . . . . ? C30 Rh1 C31 C32 117.8(3) . . . . ? P1 Rh1 C31 C32 -145.6(2) . . . . ? C51 Rh1 C31 C32 17.6(3) . . . . ? C54 Rh1 C31 C32 9.5(9) . . . . ? C55 Rh1 C31 C32 -41.1(3) . . . . ? C50 Rh1 C31 C32 -18.5(3) . . . . ? C52 Rh1 C31 C32 48.8(3) . . . . ? C53 Rh1 C31 C32 68.5(3) . . . . ? C30 C31 C32 C33 -90.3(4) . . . . ? Rh1 C31 C32 C33 -174.8(2) . . . . ? C31 C32 C33 C34 48.9(5) . . . . ? C32 C33 C34 C35 57.1(5) . . . . ? C33 C34 C35 C36 -102.1(5) . . . . ? C34 C35 C36 C37 69.0(6) . . . . ? C31 C30 C37 C36 85.7(4) . . . . ? Rh1 C30 C37 C36 168.5(3) . . . . ? C35 C36 C37 C30 -74.0(5) . . . . ? C41 Rh2 C40 C41 0.0 . . . . ? P2 Rh2 C40 C41 -87.2(2) . . . . ? C65 Rh2 C40 C41 142.8(6) . . . . ? C62 Rh2 C40 C41 101.8(2) . . . . ? C60 Rh2 C40 C41 160.2(2) . . . . ? C61 Rh2 C40 C41 136.3(2) . . . . ? C64 Rh2 C40 C41 57.0(3) . . . . ? C63 Rh2 C40 C41 71.8(2) . . . . ? C41 Rh2 C40 C47 -117.7(4) . . . . ? P2 Rh2 C40 C47 155.1(3) . . . . ? C65 Rh2 C40 C47 25.2(8) . . . . ? C62 Rh2 C40 C47 -15.9(3) . . . . ? C60 Rh2 C40 C47 42.5(4) . . . . ? C61 Rh2 C40 C47 18.7(3) . . . . ? C64 Rh2 C40 C47 -60.7(4) . . . . ? C63 Rh2 C40 C47 -45.9(3) . . . . ? C47 C40 C41 C42 1.7(5) . . . . ? Rh2 C40 C41 C42 -109.2(3) . . . . ? C47 C40 C41 Rh2 110.9(3) . . . . ? Rh2 C40 C41 Rh2 0.0 . . . . ? C40 Rh2 C41 C40 0.0 . . . . ? P2 Rh2 C41 C40 94.6(2) . . . . ? C65 Rh2 C41 C40 -161.6(3) . . . . ? C62 Rh2 C41 C40 -85.0(2) . . . . ? C60 Rh2 C41 C40 -60.6(6) . . . . ? C61 Rh2 C41 C40 -58.2(3) . . . . ? C64 Rh2 C41 C40 -149.0(2) . . . . ? C63 Rh2 C41 C40 -119.5(2) . . . . ? C40 Rh2 C41 C42 120.2(3) . . . . ? P2 Rh2 C41 C42 -145.2(3) . . . . ? C65 Rh2 C41 C42 -41.4(4) . . . . ? C62 Rh2 C41 C42 35.2(3) . . . . ? C60 Rh2 C41 C42 59.5(7) . . . . ? C61 Rh2 C41 C42 62.0(3) . . . . ? C64 Rh2 C41 C42 -28.8(3) . . . . ? C63 Rh2 C41 C42 0.6(3) . . . . ? C40 C41 C42 C43 -82.7(5) . . . . ? Rh2 C41 C42 C43 -166.8(3) . . . . ? C41 C42 C43 C44 76.2(5) . . . . ? C42 C43 C44 C45 -75.4(6) . . . . ? C43 C44 C45 C46 104.4(5) . . . . ? C44 C45 C46 C47 -57.1(6) . . . . ? C41 C40 C47 C46 89.7(5) . . . . ? Rh2 C40 C47 C46 173.8(3) . . . . ? C45 C46 C47 C40 -47.9(6) . . . . ? C31 Rh1 C50 C51 78.4(2) . . . . ? C30 Rh1 C50 C51 42.9(3) . . . . ? P1 Rh1 C50 C51 -177.4(2) . . . . ? C51 Rh1 C50 C51 0.0 . . . . ? C54 Rh1 C50 C51 -96.6(2) . . . . ? C55 Rh1 C50 C51 -125.9(3) . . . . ? C52 Rh1 C50 C51 -29.3(2) . . . . ? C53 Rh1 C50 C51 -63.0(2) . . . . ? C31 Rh1 C50 C55 -155.7(2) . . . . ? C30 Rh1 C50 C55 168.7(2) . . . . ? P1 Rh1 C50 C55 -51.6(2) . . . . ? C51 Rh1 C50 C55 125.9(3) . . . . ? C54 Rh1 C50 C55 29.3(2) . . . . ? C55 Rh1 C50 C55 0.0 . . . . ? C52 Rh1 C50 C55 96.6(2) . . . . ? C53 Rh1 C50 C55 62.8(2) . . . . ? C55 C50 C51 C52 1.5(5) . . . . ? Rh1 C50 C51 C52 59.6(3) . . . . ? C55 C50 C51 Rh1 -58.2(3) . . . . ? Rh1 C50 C51 Rh1 0.0 . . . . ? C31 Rh1 C51 C52 121.1(2) . . . . ? C30 Rh1 C51 C52 82.4(2) . . . . ? P1 Rh1 C51 C52 -122.1(4) . . . . ? C54 Rh1 C51 C52 -60.3(2) . . . . ? C55 Rh1 C51 C52 -96.1(3) . . . . ? C50 Rh1 C51 C52 -128.6(3) . . . . ? C52 Rh1 C51 C52 0.0 . . . . ? C53 Rh1 C51 C52 -26.8(2) . . . . ? C31 Rh1 C51 C50 -110.3(2) . . . . ? C30 Rh1 C51 C50 -149.0(2) . . . . ? P1 Rh1 C51 C50 6.5(5) . . . . ? C54 Rh1 C51 C50 68.3(2) . . . . ? C55 Rh1 C51 C50 32.5(2) . . . . ? C50 Rh1 C51 C50 0.0 . . . . ? C52 Rh1 C51 C50 128.6(3) . . . . ? C53 Rh1 C51 C50 101.8(3) . . . . ? C50 C51 C52 C53 -2.2(5) . . . . ? Rh1 C51 C52 C53 56.5(3) . . . . ? C50 C51 C52 Rh1 -58.7(3) . . . . ? Rh1 C51 C52 Rh1 0.0 . . . . ? C31 Rh1 C52 C53 158.3(2) . . . . ? C30 Rh1 C52 C53 122.7(3) . . . . ? P1 Rh1 C52 C53 10.3(4) . . . . ? C51 Rh1 C52 C53 -133.8(4) . . . . ? C54 Rh1 C52 C53 -28.7(2) . . . . ? C55 Rh1 C52 C53 -63.7(3) . . . . ? C50 Rh1 C52 C53 -102.2(3) . . . . ? C53 Rh1 C52 C53 0.0 . . . . ? C31 Rh1 C52 C51 -67.9(3) . . . . ? C30 Rh1 C52 C51 -103.5(2) . . . . ? P1 Rh1 C52 C51 144.1(2) . . . . ? C51 Rh1 C52 C51 0.0 . . . . ? C54 Rh1 C52 C51 105.1(3) . . . . ? C55 Rh1 C52 C51 70.1(3) . . . . ? C50 Rh1 C52 C51 31.6(2) . . . . ? C53 Rh1 C52 C51 133.8(4) . . . . ? C51 C52 C53 C54 0.9(6) . . . . ? Rh1 C52 C53 C54 56.4(3) . . . . ? C51 C52 C53 Rh1 -55.5(3) . . . . ? Rh1 C52 C53 Rh1 0.0 . . . . ? C31 Rh1 C53 C54 -164.8(2) . . . . ? C30 Rh1 C53 C54 164.5(2) . . . . ? P1 Rh1 C53 C54 55.1(3) . . . . ? C51 Rh1 C53 C54 -103.1(3) . . . . ? C54 Rh1 C53 C54 0.000(1) . . . . ? C55 Rh1 C53 C54 -28.3(2) . . . . ? C50 Rh1 C53 C54 -65.7(3) . . . . ? C52 Rh1 C53 C54 -130.4(4) . . . . ? C31 Rh1 C53 C52 -34.4(4) . . . . ? C30 Rh1 C53 C52 -65.1(3) . . . . ? P1 Rh1 C53 C52 -174.5(2) . . . . ? C51 Rh1 C53 C52 27.3(3) . . . . ? C54 Rh1 C53 C52 130.4(4) . . . . ? C55 Rh1 C53 C52 102.2(3) . . . . ? C50 Rh1 C53 C52 64.7(3) . . . . ? C52 Rh1 C53 C52 0.0 . . . . ? C52 C53 C54 C55 1.1(6) . . . . ? Rh1 C53 C54 C55 57.8(3) . . . . ? C52 C53 C54 Rh1 -56.8(3) . . . . ? Rh1 C53 C54 Rh1 0.0 . . . . ? C31 Rh1 C54 C53 71.4(8) . . . . ? C30 Rh1 C54 C53 -24.6(4) . . . . ? P1 Rh1 C54 C53 -133.7(2) . . . . ? C51 Rh1 C54 C53 63.1(3) . . . . ? C55 Rh1 C54 C53 132.7(4) . . . . ? C50 Rh1 C54 C53 101.4(3) . . . . ? C52 Rh1 C54 C53 28.9(3) . . . . ? C53 Rh1 C54 C53 0.0 . . . . ? C31 Rh1 C54 C55 -61.2(8) . . . . ? C30 Rh1 C54 C55 -157.2(2) . . . . ? P1 Rh1 C54 C55 93.6(2) . . . . ? C51 Rh1 C54 C55 -69.6(3) . . . . ? C55 Rh1 C54 C55 0.0 . . . . ? C50 Rh1 C54 C55 -31.3(2) . . . . ? C52 Rh1 C54 C55 -103.8(3) . . . . ? C53 Rh1 C54 C55 -132.7(4) . . . . ? C53 C54 C55 C50 -1.6(5) . . . . ? Rh1 C54 C55 C50 57.2(3) . . . . ? C53 C54 C55 Rh1 -58.8(3) . . . . ? Rh1 C54 C55 Rh1 0.0 . . . . ? C51 C50 C55 C54 0.3(5) . . . . ? Rh1 C50 C55 C54 -57.6(3) . . . . ? C51 C50 C55 Rh1 57.9(3) . . . . ? Rh1 C50 C55 Rh1 0.0 . . . . ? C31 Rh1 C55 C54 166.8(2) . . . . ? C30 Rh1 C55 C54 90.2(6) . . . . ? P1 Rh1 C55 C54 -91.6(2) . . . . ? C51 Rh1 C55 C54 96.6(3) . . . . ? C54 Rh1 C55 C54 0.0 . . . . ? C50 Rh1 C55 C54 129.1(3) . . . . ? C52 Rh1 C55 C54 61.2(2) . . . . ? C53 Rh1 C55 C54 27.1(2) . . . . ? C31 Rh1 C55 C50 37.8(3) . . . . ? C30 Rh1 C55 C50 -38.9(7) . . . . ? P1 Rh1 C55 C50 139.3(2) . . . . ? C51 Rh1 C55 C50 -32.4(2) . . . . ? C54 Rh1 C55 C50 -129.1(3) . . . . ? C50 Rh1 C55 C50 0.0 . . . . ? C52 Rh1 C55 C50 -67.9(3) . . . . ? C53 Rh1 C55 C50 -101.9(3) . . . . ? C40 Rh2 C60 C65 -172.6(2) . . . . ? C41 Rh2 C60 C65 -126.6(6) . . . . ? P2 Rh2 C60 C65 79.0(3) . . . . ? C65 Rh2 C60 C65 0.0 . . . . ? C62 Rh2 C60 C65 -99.5(3) . . . . ? C61 Rh2 C60 C65 -129.9(4) . . . . ? C64 Rh2 C60 C65 -29.1(3) . . . . ? C63 Rh2 C60 C65 -64.1(3) . . . . ? C40 Rh2 C60 C61 -42.8(4) . . . . ? C41 Rh2 C60 C61 3.3(8) . . . . ? P2 Rh2 C60 C61 -151.2(3) . . . . ? C65 Rh2 C60 C61 129.9(4) . . . . ? C62 Rh2 C60 C61 30.4(3) . . . . ? C61 Rh2 C60 C61 0.0 . . . . ? C64 Rh2 C60 C61 100.8(3) . . . . ? C63 Rh2 C60 C61 65.8(3) . . . . ? C65 C60 C61 C62 -1.3(5) . . . . ? Rh2 C60 C61 C62 -57.4(3) . . . . ? C65 C60 C61 Rh2 56.1(3) . . . . ? Rh2 C60 C61 Rh2 0.0 . . . . ? C40 Rh2 C61 C62 -83.3(3) . . . . ? C41 Rh2 C61 C62 -50.8(4) . . . . ? P2 Rh2 C61 C62 168.3(2) . . . . ? C65 Rh2 C61 C62 98.5(3) . . . . ? C62 Rh2 C61 C62 0.000(1) . . . . ? C60 Rh2 C61 C62 128.0(5) . . . . ? C64 Rh2 C61 C62 63.2(3) . . . . ? C63 Rh2 C61 C62 28.8(3) . . . . ? C40 Rh2 C61 C60 148.7(3) . . . . ? C41 Rh2 C61 C60 -178.8(3) . . . . ? P2 Rh2 C61 C60 40.2(4) . . . . ? C65 Rh2 C61 C60 -29.5(3) . . . . ? C62 Rh2 C61 C60 -128.0(5) . . . . ? C60 Rh2 C61 C60 0.0 . . . . ? C64 Rh2 C61 C60 -64.8(3) . . . . ? C63 Rh2 C61 C60 -99.3(3) . . . . ? C60 C61 C62 C63 -2.0(5) . . . . ? Rh2 C61 C62 C63 -59.3(3) . . . . ? C60 C61 C62 Rh2 57.3(3) . . . . ? Rh2 C61 C62 Rh2 0.0 . . . . ? C40 Rh2 C62 C63 -126.3(3) . . . . ? C41 Rh2 C62 C63 -88.1(3) . . . . ? P2 Rh2 C62 C63 93.5(6) . . . . ? C65 Rh2 C62 C63 63.4(3) . . . . ? C60 Rh2 C62 C63 99.7(3) . . . . ? C61 Rh2 C62 C63 130.9(4) . . . . ? C64 Rh2 C62 C63 28.1(3) . . . . ? C63 Rh2 C62 C63 0.0 . . . . ? C40 Rh2 C62 C61 102.9(3) . . . . ? C41 Rh2 C62 C61 141.1(3) . . . . ? P2 Rh2 C62 C61 -37.3(7) . . . . ? C65 Rh2 C62 C61 -67.4(3) . . . . ? C60 Rh2 C62 C61 -31.2(3) . . . . ? C61 Rh2 C62 C61 0.000(1) . . . . ? C64 Rh2 C62 C61 -102.8(3) . . . . ? C63 Rh2 C62 C61 -130.9(4) . . . . ? C61 C62 C63 C64 2.9(6) . . . . ? Rh2 C62 C63 C64 -55.9(3) . . . . ? C61 C62 C63 Rh2 58.8(3) . . . . ? Rh2 C62 C63 Rh2 0.0 . . . . ? C40 Rh2 C63 C64 -165.6(3) . . . . ? C41 Rh2 C63 C64 -129.2(3) . . . . ? P2 Rh2 C63 C64 -23.4(4) . . . . ? C65 Rh2 C63 C64 29.8(3) . . . . ? C62 Rh2 C63 C64 132.0(5) . . . . ? C60 Rh2 C63 C64 65.9(3) . . . . ? C61 Rh2 C63 C64 102.9(4) . . . . ? C64 Rh2 C63 C64 0.0 . . . . ? C40 Rh2 C63 C62 62.4(3) . . . . ? C41 Rh2 C63 C62 98.8(3) . . . . ? P2 Rh2 C63 C62 -155.5(2) . . . . ? C65 Rh2 C63 C62 -102.3(3) . . . . ? C62 Rh2 C63 C62 0.0 . . . . ? C60 Rh2 C63 C62 -66.2(3) . . . . ? C61 Rh2 C63 C62 -29.2(3) . . . . ? C64 Rh2 C63 C62 -132.0(5) . . . . ? C62 C63 C64 C65 -0.4(6) . . . . ? Rh2 C63 C64 C65 -55.5(3) . . . . ? C62 C63 C64 Rh2 55.1(3) . . . . ? Rh2 C63 C64 Rh2 0.0 . . . . ? C40 Rh2 C64 C63 24.6(5) . . . . ? C41 Rh2 C64 C63 60.8(4) . . . . ? P2 Rh2 C64 C63 165.5(3) . . . . ? C65 Rh2 C64 C63 -129.7(5) . . . . ? C62 Rh2 C64 C63 -28.3(3) . . . . ? C60 Rh2 C64 C63 -100.1(4) . . . . ? C61 Rh2 C64 C63 -63.6(3) . . . . ? C63 Rh2 C64 C63 0.0 . . . . ? C40 Rh2 C64 C65 154.3(3) . . . . ? C41 Rh2 C64 C65 -169.6(3) . . . . ? P2 Rh2 C64 C65 -64.8(3) . . . . ? C65 Rh2 C64 C65 0.000(1) . . . . ? C62 Rh2 C64 C65 101.3(3) . . . . ? C60 Rh2 C64 C65 29.6(3) . . . . ? C61 Rh2 C64 C65 66.1(3) . . . . ? C63 Rh2 C64 C65 129.7(5) . . . . ? C63 C64 C65 C60 -3.0(6) . . . . ? Rh2 C64 C65 C60 -60.0(3) . . . . ? C63 C64 C65 Rh2 57.0(3) . . . . ? Rh2 C64 C65 Rh2 0.0 . . . . ? C61 C60 C65 C64 3.8(6) . . . . ? Rh2 C60 C65 C64 60.7(3) . . . . ? C61 C60 C65 Rh2 -56.9(3) . . . . ? Rh2 C60 C65 Rh2 0.0 . . . . ? C40 Rh2 C65 C64 -107.4(7) . . . . ? C41 Rh2 C65 C64 19.8(5) . . . . ? P2 Rh2 C65 C64 122.7(3) . . . . ? C62 Rh2 C65 C64 -64.3(3) . . . . ? C60 Rh2 C65 C64 -130.4(4) . . . . ? C61 Rh2 C65 C64 -100.3(3) . . . . ? C64 Rh2 C65 C64 0.000(1) . . . . ? C63 Rh2 C65 C64 -29.3(3) . . . . ? C40 Rh2 C65 C60 22.9(8) . . . . ? C41 Rh2 C65 C60 150.2(3) . . . . ? P2 Rh2 C65 C60 -106.9(3) . . . . ? C62 Rh2 C65 C60 66.1(3) . . . . ? C60 Rh2 C65 C60 0.0 . . . . ? C61 Rh2 C65 C60 30.0(3) . . . . ? C64 Rh2 C65 C60 130.4(4) . . . . ? C63 Rh2 C65 C60 101.0(3) . . . . ? _refine_diff_density_max 0.593 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.051