# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 # Attachment '- cif-revised.cif' data_I #TrackingRef '- cif-revised.cif' _audit_update_record ; 2010-08-15 # Formatted by publCIF ; #-------------------------------------------------------------- # SUBMISSION DETAILS _publ_contact_author ; Alireza Abbasi School of Chemistry College of Science University of Tehran Tehran Iran ; _publ_contact_author_email aabbasi@khayam.ut.ac.ir _publ_contact_author_fax '+98 21 66495291' _publ_contact_author_phone '+98 21 61112499' _publ_requested_journal 'Dalton Transactions' _publ_requested_category EI #-------------------------------------------------------------- # TITLE AND AUTHOR LIST _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address _publ_author_footnote A.Abbasi ; School of Chemistry College of Science University of Tehran Tehran Iran ; . M.Skripkin ; Department of General and Inorganic Chemistry Saint-Petersburg State University Universitetsky pr. 26 198504, Saint-Petersburg Russia ; . L.Eriksson ; Materials and Environmental Chemistry Arrhenius Laboratory Stockhom University Stockhom Sweden ; . #-------------------------------------------------------------- data_Rh-6dmso_I _database_code_depnum_ccdc_archive 'CCDC 789614' #TrackingRef '- cif-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 O6 Rh S6, 3(C F3 O3 S)' _chemical_formula_sum 'C15 H36 F9 O15 Rh S9' _chemical_formula_weight 1018.89 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 28.715(5) _cell_length_b 12.243(2) _cell_length_c 11.097(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3901.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 19457 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 25.02 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8548 _exptl_absorpt_correction_T_max 0.9117 _exptl_absorpt_process_details 'X-red (STOE, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'X-calibur 2 with Sapphire-III CCD detector' _diffrn_measurement_method '\w-scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 19457 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.1915 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6798 _reflns_number_gt 2716 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg, 2001)' _computing_publication_material 'Platon (Spek, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In total 159 restraints: 1 floating origin restraint 36 distance restraints for fixing the geometry of the 3 different triflate molecules. The geometrical restraints were used to stabilize and fix the geometry of the triflate counter ions 122 DELU restraints for all anisotropic displacement parameters, used for stabilizing the anisotropic displacement ellipsoids for all atoms, some were very little affected. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.36(5) _refine_ls_number_reflns 6798 _refine_ls_number_parameters 447 _refine_ls_number_restraints 159 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0854 _refine_ls_goodness_of_fit_ref 0.754 _refine_ls_restrained_S_all 0.777 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.65018(2) 0.14617(6) 0.79964(10) 0.0506(2) Uani 1 1 d U . . S1 S 0.53946(8) 0.1664(2) 0.7923(4) 0.0896(9) Uani 1 1 d U . . O1 O 0.5795(2) 0.0972(5) 0.7701(6) 0.077(2) Uani 1 1 d U . . C12 C 0.5152(4) 0.1195(10) 0.9287(11) 0.088(4) Uani 1 1 d U . . H12A H 0.5347 0.1416 0.9947 0.131 Uiso 1 1 calc R . . H12B H 0.5131 0.0413 0.9270 0.131 Uiso 1 1 calc R . . H12C H 0.4847 0.1501 0.9387 0.131 Uiso 1 1 calc R . . C11 C 0.4985(4) 0.1104(11) 0.6907(11) 0.097(4) Uani 1 1 d U . . H11A H 0.5066 0.1307 0.6099 0.145 Uiso 1 1 calc R . . H11B H 0.4680 0.1377 0.7095 0.145 Uiso 1 1 calc R . . H11C H 0.4986 0.0322 0.6977 0.145 Uiso 1 1 calc R . . S2 S 0.61662(10) 0.2940(3) 0.5933(3) 0.0669(8) Uani 1 1 d U . . O2 O 0.6452(2) 0.2903(6) 0.7114(6) 0.0643(18) Uani 1 1 d U . . C22 C 0.6584(4) 0.3467(10) 0.4884(12) 0.098(5) Uani 1 1 d U . . H22A H 0.6808 0.2909 0.4694 0.147 Uiso 1 1 calc R . . H22B H 0.6741 0.4082 0.5235 0.147 Uiso 1 1 calc R . . H22C H 0.6428 0.3693 0.4160 0.147 Uiso 1 1 calc R . . C21 C 0.5806(4) 0.4074(9) 0.6080(13) 0.094(4) Uani 1 1 d U . . H21A H 0.5562 0.3914 0.6644 0.140 Uiso 1 1 calc R . . H21B H 0.5673 0.4250 0.5312 0.140 Uiso 1 1 calc R . . H21C H 0.5985 0.4683 0.6367 0.140 Uiso 1 1 calc R . . S3 S 0.64762(11) 0.3364(3) 0.9807(3) 0.0818(9) Uani 1 1 d U . . O3 O 0.6295(2) 0.2213(6) 0.9532(6) 0.0683(18) Uani 1 1 d U . . C31 C 0.5974(4) 0.4165(10) 0.9839(13) 0.107(4) Uani 1 1 d U . . H31A H 0.5872 0.4303 0.9030 0.161 Uiso 1 1 calc R . . H31B H 0.6041 0.4845 1.0233 0.161 Uiso 1 1 calc R . . H31C H 0.5734 0.3787 1.0273 0.161 Uiso 1 1 calc R . . C32 C 0.6592(5) 0.3277(11) 1.1352(12) 0.099(4) Uani 1 1 d U . . H32A H 0.6853 0.2801 1.1483 0.148 Uiso 1 1 calc R . . H32B H 0.6324 0.2992 1.1761 0.148 Uiso 1 1 calc R . . H32C H 0.6663 0.3991 1.1659 0.148 Uiso 1 1 calc R . . S4 S 0.62736(11) -0.0220(3) 0.9957(3) 0.0742(10) Uani 1 1 d U . . O4 O 0.6587(2) 0.0029(5) 0.8864(6) 0.0673(18) Uani 1 1 d U . . C41 C 0.6176(4) -0.1595(9) 0.9817(11) 0.121(4) Uani 1 1 d U . . H41A H 0.5959 -0.1723 0.9175 0.182 Uiso 1 1 calc R . . H41B H 0.6051 -0.1874 1.0558 0.182 Uiso 1 1 calc R . . H41C H 0.6465 -0.1959 0.9641 0.182 Uiso 1 1 calc R . . C42 C 0.6660(6) -0.0231(13) 1.1175(13) 0.172(7) Uani 1 1 d U . . H42A H 0.6750 0.0504 1.1364 0.257 Uiso 1 1 calc R . . H42B H 0.6931 -0.0650 1.0968 0.257 Uiso 1 1 calc R . . H42C H 0.6510 -0.0554 1.1862 0.257 Uiso 1 1 calc R . . S5 S 0.64281(11) -0.0323(3) 0.6053(3) 0.0812(11) Uani 1 1 d U . . O5 O 0.6670(2) 0.0757(5) 0.6418(6) 0.0663(18) Uani 1 1 d U . . C51 C 0.6167(4) 0.0058(9) 0.4657(12) 0.114(4) Uani 1 1 d U . . H51A H 0.5901 0.0513 0.4809 0.171 Uiso 1 1 calc R . . H51B H 0.6071 -0.0586 0.4231 0.171 Uiso 1 1 calc R . . H51C H 0.6389 0.0453 0.4179 0.171 Uiso 1 1 calc R . . C52 C 0.6874(4) -0.1097(9) 0.5492(12) 0.111(5) Uani 1 1 d U . . H52A H 0.7058 -0.1375 0.6146 0.166 Uiso 1 1 calc R . . H52B H 0.7066 -0.0655 0.4978 0.166 Uiso 1 1 calc R . . H52C H 0.6749 -0.1696 0.5037 0.166 Uiso 1 1 calc R . . S6 S 0.72549(8) 0.1721(2) 0.8358(2) 0.0636(9) Uani 1 1 d U . . O6 O 0.7352(2) 0.2049(7) 0.9580(7) 0.101(3) Uani 1 1 d U . . C62 C 0.7556(3) 0.0493(6) 0.8027(17) 0.098(3) Uani 1 1 d U . . H62A H 0.7431 -0.0091 0.8505 0.147 Uiso 1 1 calc R . . H62B H 0.7881 0.0582 0.8210 0.147 Uiso 1 1 calc R . . H62C H 0.7521 0.0322 0.7188 0.147 Uiso 1 1 calc R . . C61 C 0.7502(4) 0.2636(8) 0.7368(10) 0.086(4) Uani 1 1 d U . . H61A H 0.7373 0.3349 0.7502 0.129 Uiso 1 1 calc R . . H61B H 0.7439 0.2411 0.6556 0.129 Uiso 1 1 calc R . . H61C H 0.7833 0.2659 0.7494 0.129 Uiso 1 1 calc R . . S10 S 0.73926(15) 0.6433(5) 0.8796(4) 0.1434(19) Uani 1 1 d DU . . O11 O 0.7164(6) 0.5858(15) 0.9752(13) 0.306(9) Uani 1 1 d DU . . O12 O 0.7369(4) 0.7551(10) 0.8931(17) 0.323(10) Uani 1 1 d DU . . O13 O 0.7805(3) 0.6038(10) 0.8414(10) 0.212(6) Uani 1 1 d DU . . C10 C 0.6982(5) 0.6111(10) 0.7735(16) 0.134(5) Uani 1 1 d DU . . F11 F 0.6575(3) 0.6484(10) 0.7854(16) 0.255(6) Uani 1 1 d DU . . F12 F 0.6955(4) 0.5128(8) 0.7482(11) 0.276(7) Uani 1 1 d DU . . F13 F 0.7141(5) 0.6525(14) 0.6692(11) 0.306(8) Uani 1 1 d DU . . S20 S 0.53008(12) 0.2105(3) 0.3118(4) 0.0959(10) Uani 1 1 d DU . . O21 O 0.5065(4) 0.1388(8) 0.3906(10) 0.168(4) Uani 1 1 d DU . . O22 O 0.5632(3) 0.2789(7) 0.3601(9) 0.161(5) Uani 1 1 d DU . . O23 O 0.5469(4) 0.1509(10) 0.2113(10) 0.201(5) Uani 1 1 d DU . . C20 C 0.4819(5) 0.2889(12) 0.2552(13) 0.125(4) Uani 1 1 d DU . . F21 F 0.4644(4) 0.3527(8) 0.3341(11) 0.208(5) Uani 1 1 d DU . . F22 F 0.4496(3) 0.2345(8) 0.2055(9) 0.209(5) Uani 1 1 d DU . . F23 F 0.4982(3) 0.3570(8) 0.1698(9) 0.208(5) Uani 1 1 d DU . . S30 S 0.38960(11) 0.3205(3) 0.8218(6) 0.1238(16) Uani 1 1 d DU . . O31 O 0.3670(5) 0.3680(9) 0.9247(12) 0.176(5) Uani 1 1 d DU . . O32 O 0.3993(3) 0.2155(6) 0.8086(14) 0.182(4) Uani 1 1 d DU . . O33 O 0.3606(5) 0.3615(13) 0.7091(15) 0.259(8) Uani 1 1 d DU . . C30 C 0.4381(5) 0.3980(10) 0.7879(15) 0.131(4) Uani 1 1 d DU . . F31 F 0.4634(5) 0.3714(11) 0.8846(14) 0.289(8) Uani 1 1 d DU . . F32 F 0.4265(3) 0.5024(5) 0.7879(12) 0.214(4) Uani 1 1 d DU . . F33 F 0.4566(5) 0.3780(9) 0.6865(12) 0.216(5) Uani 1 1 d DU . . 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 0.0491(3) 0.0547(4) 0.0481(4) 0.0035(6) -0.0007(7) -0.0001(4) S1 0.0667(15) 0.121(2) 0.081(2) -0.007(3) -0.005(2) 0.0062(17) O1 0.095(4) 0.089(5) 0.047(6) -0.029(4) -0.014(3) 0.041(3) C12 0.065(8) 0.122(11) 0.076(6) -0.004(8) 0.013(6) -0.011(7) C11 0.082(8) 0.126(11) 0.082(8) 0.001(8) -0.016(7) 0.024(8) S2 0.0738(19) 0.064(2) 0.063(2) 0.0074(17) -0.0125(16) 0.0028(17) O2 0.081(5) 0.057(4) 0.055(4) 0.002(3) -0.014(4) 0.010(4) C22 0.102(10) 0.121(11) 0.071(8) 0.000(8) 0.025(7) 0.018(8) C21 0.096(9) 0.080(8) 0.105(11) 0.030(8) 0.004(7) 0.030(7) S3 0.096(2) 0.074(2) 0.075(2) -0.015(2) 0.004(2) -0.007(2) O3 0.073(4) 0.080(5) 0.051(4) -0.006(4) 0.001(3) -0.007(4) C31 0.116(9) 0.107(9) 0.100(11) -0.012(9) -0.008(9) 0.014(8) C32 0.115(11) 0.111(11) 0.070(7) -0.034(7) -0.008(7) -0.009(8) S4 0.083(2) 0.077(2) 0.062(2) 0.018(2) 0.0060(18) 0.0041(19) O4 0.060(4) 0.064(4) 0.078(5) 0.020(3) 0.011(3) 0.009(3) C41 0.155(11) 0.089(7) 0.120(11) 0.021(8) 0.025(9) -0.042(8) C42 0.218(17) 0.194(16) 0.103(10) 0.065(11) -0.070(11) -0.081(14) S5 0.086(2) 0.073(2) 0.085(3) -0.021(2) 0.019(2) -0.019(2) O5 0.073(4) 0.060(4) 0.066(4) -0.012(3) -0.002(3) -0.013(4) C51 0.121(9) 0.094(9) 0.127(11) -0.031(8) -0.051(9) -0.015(8) C52 0.105(9) 0.076(9) 0.151(13) -0.046(8) -0.009(8) 0.007(6) S6 0.0500(13) 0.0729(19) 0.068(3) 0.0059(16) -0.0022(13) -0.0042(13) O6 0.066(5) 0.166(8) 0.071(5) -0.019(5) -0.019(4) -0.010(5) C62 0.053(5) 0.057(6) 0.184(11) -0.002(9) 0.007(11) 0.011(5) C61 0.072(7) 0.072(7) 0.115(9) 0.028(6) 0.012(6) -0.017(6) S10 0.098(3) 0.194(5) 0.139(4) -0.066(4) -0.029(3) 0.036(4) O11 0.302(17) 0.50(2) 0.116(9) -0.044(12) 0.048(9) -0.015(17) O12 0.191(11) 0.214(9) 0.56(3) -0.231(13) -0.118(14) 0.008(9) O13 0.142(7) 0.332(15) 0.164(13) -0.043(10) -0.014(7) 0.098(9) C10 0.149(9) 0.088(9) 0.166(12) -0.009(11) -0.047(11) 0.001(9) F11 0.120(6) 0.362(12) 0.283(13) -0.151(14) -0.087(8) 0.039(8) F12 0.341(14) 0.158(8) 0.329(19) -0.113(9) -0.134(14) -0.022(8) F13 0.296(16) 0.47(2) 0.155(10) 0.119(14) -0.048(9) 0.004(17) S20 0.124(3) 0.090(2) 0.074(2) 0.013(3) -0.023(3) -0.025(2) O21 0.217(11) 0.138(9) 0.150(9) 0.072(7) 0.021(7) -0.018(7) O22 0.176(8) 0.101(7) 0.207(13) 0.013(6) -0.095(8) -0.023(6) O23 0.231(13) 0.266(15) 0.107(8) -0.045(8) 0.013(8) 0.039(10) C20 0.144(11) 0.122(13) 0.109(13) 0.035(7) -0.036(8) -0.026(7) F21 0.252(11) 0.158(8) 0.213(13) 0.026(7) 0.015(8) 0.090(7) F22 0.160(8) 0.207(10) 0.258(12) 0.041(8) -0.095(7) -0.057(7) F23 0.178(9) 0.240(10) 0.206(11) 0.146(8) -0.037(7) -0.033(7) S30 0.087(2) 0.080(3) 0.204(5) -0.011(4) 0.044(3) 0.0055(18) O31 0.180(11) 0.159(11) 0.188(9) -0.034(9) 0.089(9) -0.016(8) O32 0.226(9) 0.079(5) 0.242(11) 0.017(10) 0.113(11) -0.008(6) O33 0.196(12) 0.34(2) 0.244(10) -0.055(12) -0.081(11) 0.109(12) C30 0.164(9) 0.081(7) 0.148(11) 0.077(12) 0.035(8) 0.003(7) F31 0.289(13) 0.290(15) 0.289(11) -0.048(11) -0.213(12) 0.021(11) F32 0.265(9) 0.076(5) 0.303(12) 0.054(8) 0.102(11) 0.008(5) F33 0.265(13) 0.167(9) 0.215(9) 0.056(8) 0.134(9) 0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh O5 2.011(6) . ? Rh O4 2.016(6) . ? Rh O2 2.023(7) . ? Rh O3 2.026(7) . ? Rh O1 2.143(6) . ? Rh S6 2.222(2) . ? S1 O1 1.449(6) . ? S1 C12 1.763(12) . ? S1 C11 1.768(12) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? S2 O2 1.547(6) . ? S2 C21 1.739(11) . ? S2 C22 1.793(12) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? S3 O3 1.533(7) . ? S3 C31 1.743(11) . ? S3 C32 1.749(14) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? S4 O4 1.540(7) . ? S4 C41 1.713(11) . ? S4 C42 1.748(13) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? S5 O5 1.548(7) . ? S5 C52 1.711(11) . ? S5 C51 1.783(12) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? S6 O6 1.441(8) . ? S6 C61 1.723(9) . ? S6 C62 1.773(9) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? S10 O13 1.346(9) . ? S10 O12 1.379(11) . ? S10 O11 1.431(12) . ? S10 C10 1.712(16) . ? C10 F12 1.239(12) . ? C10 F11 1.261(13) . ? C10 F13 1.344(15) . ? S20 O22 1.377(7) . ? S20 O21 1.413(8) . ? S20 O23 1.416(9) . ? S20 C20 1.798(15) . ? C20 F22 1.267(12) . ? C20 F21 1.277(13) . ? C20 F23 1.346(13) . ? S30 O32 1.324(7) . ? S30 O31 1.436(10) . ? S30 O33 1.584(12) . ? S30 C30 1.726(13) . ? C30 F33 1.268(13) . ? C30 F32 1.322(11) . ? C30 F31 1.335(13) . ? 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 O5 Rh O4 90.8(3) . . ? O5 Rh O2 88.3(3) . . ? O4 Rh O2 177.1(3) . . ? O5 Rh O3 176.2(3) . . ? O4 Rh O3 91.7(3) . . ? O2 Rh O3 89.4(3) . . ? O5 Rh O1 88.6(2) . . ? O4 Rh O1 86.8(2) . . ? O2 Rh O1 95.9(3) . . ? O3 Rh O1 88.7(2) . . ? O5 Rh S6 89.10(18) . . ? O4 Rh S6 85.43(19) . . ? O2 Rh S6 91.8(2) . . ? O3 Rh S6 93.97(19) . . ? O1 Rh S6 171.84(19) . . ? O1 S1 C12 105.6(5) . . ? O1 S1 C11 101.1(5) . . ? C12 S1 C11 99.1(5) . . ? S1 O1 Rh 124.2(4) . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 S2 C21 105.0(6) . . ? O2 S2 C22 101.9(6) . . ? C21 S2 C22 99.9(6) . . ? S2 O2 Rh 118.2(4) . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O3 S3 C31 103.9(5) . . ? O3 S3 C32 101.8(5) . . ? C31 S3 C32 99.8(6) . . ? S3 O3 Rh 119.0(4) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O4 S4 C41 102.6(5) . . ? O4 S4 C42 103.9(6) . . ? C41 S4 C42 99.5(7) . . ? S4 O4 Rh 118.5(4) . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O5 S5 C52 103.4(5) . . ? O5 S5 C51 101.1(5) . . ? C52 S5 C51 98.2(6) . . ? S5 O5 Rh 119.1(4) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O6 S6 C61 109.8(6) . . ? O6 S6 C62 109.7(6) . . ? C61 S6 C62 102.6(6) . . ? O6 S6 Rh 113.4(3) . . ? C61 S6 Rh 112.3(4) . . ? C62 S6 Rh 108.5(3) . . ? S6 C62 H62A 109.5 . . ? S6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? S6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? S6 C61 H61A 109.5 . . ? S6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? S6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O13 S10 O12 115.7(9) . . ? O13 S10 O11 117.4(10) . . ? O12 S10 O11 112.6(9) . . ? O13 S10 C10 107.9(8) . . ? O12 S10 C10 105.6(8) . . ? O11 S10 C10 94.7(10) . . ? F12 C10 F11 108.5(13) . . ? F12 C10 F13 101.0(15) . . ? F11 C10 F13 105.7(15) . . ? F12 C10 S10 115.0(12) . . ? F11 C10 S10 118.9(13) . . ? F13 C10 S10 105.7(12) . . ? O22 S20 O21 117.9(7) . . ? O22 S20 O23 112.6(7) . . ? O21 S20 O23 109.3(6) . . ? O22 S20 C20 110.1(6) . . ? O21 S20 C20 100.3(6) . . ? O23 S20 C20 105.2(8) . . ? F22 C20 F21 109.4(14) . . ? F22 C20 F23 105.8(11) . . ? F21 C20 F23 103.9(13) . . ? F22 C20 S20 115.7(12) . . ? F21 C20 S20 113.0(10) . . ? F23 C20 S20 108.0(10) . . ? O32 S30 O31 125.2(8) . . ? O32 S30 O33 109.3(9) . . ? O31 S30 O33 105.2(5) . . ? O32 S30 C30 109.8(6) . . ? O31 S30 C30 108.4(8) . . ? O33 S30 C30 94.5(9) . . ? F33 C30 F32 107.0(11) . . ? F33 C30 F31 116.0(12) . . ? F32 C30 F31 111.8(14) . . ? F33 C30 S30 115.2(13) . . ? F32 C30 S30 109.1(10) . . ? F31 C30 S30 97.4(10) . . ? 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 C12 S1 O1 Rh -103.3(6) . . . . ? C11 S1 O1 Rh 153.9(5) . . . . ? O5 Rh O1 S1 -136.9(5) . . . . ? O4 Rh O1 S1 132.2(5) . . . . ? O2 Rh O1 S1 -48.8(5) . . . . ? O3 Rh O1 S1 40.5(5) . . . . ? S6 Rh O1 S1 149.8(11) . . . . ? C21 S2 O2 Rh 132.1(5) . . . . ? C22 S2 O2 Rh -124.1(5) . . . . ? O5 Rh O2 S2 48.5(4) . . . . ? O4 Rh O2 S2 119(6) . . . . ? O3 Rh O2 S2 -128.5(4) . . . . ? O1 Rh O2 S2 -39.8(4) . . . . ? S6 Rh O2 S2 137.6(4) . . . . ? C31 S3 O3 Rh 118.0(6) . . . . ? C32 S3 O3 Rh -138.6(6) . . . . ? O5 Rh O3 S3 -92(4) . . . . ? O4 Rh O3 S3 138.0(4) . . . . ? O2 Rh O3 S3 -39.3(4) . . . . ? O1 Rh O3 S3 -135.3(4) . . . . ? S6 Rh O3 S3 52.5(4) . . . . ? C41 S4 O4 Rh 143.3(6) . . . . ? C42 S4 O4 Rh -113.4(7) . . . . ? O5 Rh O4 S4 -146.8(4) . . . . ? O2 Rh O4 S4 143(6) . . . . ? O3 Rh O4 S4 30.3(4) . . . . ? O1 Rh O4 S4 -58.3(4) . . . . ? S6 Rh O4 S4 124.2(4) . . . . ? C52 S5 O5 Rh -137.0(6) . . . . ? C51 S5 O5 Rh 121.6(6) . . . . ? O4 Rh O5 S5 49.3(4) . . . . ? O2 Rh O5 S5 -133.5(4) . . . . ? O3 Rh O5 S5 -81(4) . . . . ? O1 Rh O5 S5 -37.5(4) . . . . ? S6 Rh O5 S5 134.7(4) . . . . ? O5 Rh S6 O6 -168.3(5) . . . . ? O4 Rh S6 O6 -77.5(5) . . . . ? O2 Rh S6 O6 103.4(5) . . . . ? O3 Rh S6 O6 13.9(5) . . . . ? O1 Rh S6 O6 -95.1(14) . . . . ? O5 Rh S6 C61 66.5(5) . . . . ? O4 Rh S6 C61 157.3(5) . . . . ? O2 Rh S6 C61 -21.8(5) . . . . ? O3 Rh S6 C61 -111.3(5) . . . . ? O1 Rh S6 C61 139.8(14) . . . . ? O5 Rh S6 C62 -46.2(6) . . . . ? O4 Rh S6 C62 44.6(6) . . . . ? O2 Rh S6 C62 -134.4(7) . . . . ? O3 Rh S6 C62 136.0(7) . . . . ? O1 Rh S6 C62 27.1(16) . . . . ? O13 S10 C10 F12 55.0(15) . . . . ? O12 S10 C10 F12 179.2(15) . . . . ? O11 S10 C10 F12 -65.7(16) . . . . ? O13 S10 C10 F11 -173.9(14) . . . . ? O12 S10 C10 F11 -49.7(18) . . . . ? O11 S10 C10 F11 65.4(16) . . . . ? O13 S10 C10 F13 -55.5(13) . . . . ? O12 S10 C10 F13 68.7(15) . . . . ? O11 S10 C10 F13 -176.2(13) . . . . ? O22 S20 C20 F22 178.2(11) . . . . ? O21 S20 C20 F22 -56.8(13) . . . . ? O23 S20 C20 F22 56.6(13) . . . . ? O22 S20 C20 F21 -54.6(13) . . . . ? O21 S20 C20 F21 70.4(13) . . . . ? O23 S20 C20 F21 -176.1(12) . . . . ? O22 S20 C20 F23 59.8(12) . . . . ? O21 S20 C20 F23 -175.2(11) . . . . ? O23 S20 C20 F23 -61.7(12) . . . . ? O32 S30 C30 F33 52.5(14) . . . . ? O31 S30 C30 F33 -167.6(12) . . . . ? O33 S30 C30 F33 -59.9(12) . . . . ? O32 S30 C30 F32 172.9(13) . . . . ? O31 S30 C30 F32 -47.2(14) . . . . ? O33 S30 C30 F32 60.5(13) . . . . ? O32 S30 C30 F31 -70.9(13) . . . . ? O31 S30 C30 F31 69.0(12) . . . . ? O33 S30 C30 F31 176.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.331 _refine_diff_density_min -0.582 _refine_diff_density_rms 0.071 #end data_rh-6dmso_I data_rh-6dmso_Istar _database_code_depnum_ccdc_archive 'CCDC 789615' #TrackingRef '- cif-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H36 O6 Rh S6, 3(C F3 O3 S)' _chemical_formula_sum 'C15 H36 F9 O15 Rh S9' _chemical_formula_weight 1018.89 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 28.1746(19) _cell_length_b 12.1626(8) _cell_length_c 11.0466(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3785.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 15080 _cell_measurement_theta_min 3.65 _cell_measurement_theta_max 25.03 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7959 _exptl_absorpt_correction_T_max 0.9343 _exptl_absorpt_process_details 'X-red (STOE, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'X-calibur 2 with Sapphire-III CCD detector' _diffrn_measurement_method '\w-scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 15080 _diffrn_reflns_av_R_equivalents 0.0947 _diffrn_reflns_av_sigmaI/netI 0.1163 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4895 _reflns_number_gt 3254 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg, 2001)' _computing_publication_material 'Platon (Spek, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In total 37 restraints: 1 floating origin restraint 36 distance restraints for fixing the geometry of the 3 different triflate molecules. The geometrical restraints were used to stabilize and fix the geometry of the triflate counter ions ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0007(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(6) _refine_ls_number_reflns 4895 _refine_ls_number_parameters 448 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.65027(2) 0.13990(5) 0.79880(11) 0.0323(2) Uani 1 1 d . . . S1 S 0.53798(8) 0.17049(17) 0.7921(4) 0.0437(7) Uani 1 1 d . . . O1 O 0.5796(2) 0.0948(5) 0.7641(7) 0.040(2) Uani 1 1 d . . . C11 C 0.4938(4) 0.1149(10) 0.6936(14) 0.059(4) Uani 1 1 d . . . H11A H 0.5013 0.1346 0.6097 0.088 Uiso 1 1 calc R . . H11B H 0.4627 0.1449 0.7153 0.088 Uiso 1 1 calc R . . H11C H 0.4932 0.0347 0.7017 0.088 Uiso 1 1 calc R . . C12 C 0.5151(4) 0.1222(8) 0.9332(11) 0.041(3) Uani 1 1 d . . . H12A H 0.5360 0.1464 0.9991 0.062 Uiso 1 1 calc R . . H12B H 0.5137 0.0417 0.9322 0.062 Uiso 1 1 calc R . . H12C H 0.4832 0.1519 0.9458 0.062 Uiso 1 1 calc R . . S2 S 0.61671(8) 0.29321(18) 0.5923(3) 0.0323(6) Uani 1 1 d . . . O2 O 0.6438(2) 0.2905(5) 0.7166(7) 0.0353(18) Uani 1 1 d . . . C21 C 0.5821(4) 0.4132(8) 0.6059(11) 0.039(3) Uani 1 1 d . . . H21A H 0.5563 0.4003 0.6636 0.059 Uiso 1 1 calc R . . H21B H 0.5687 0.4324 0.5267 0.059 Uiso 1 1 calc R . . H21C H 0.6020 0.4738 0.6348 0.059 Uiso 1 1 calc R . . C22 C 0.6591(4) 0.3401(9) 0.4833(11) 0.039(3) Uani 1 1 d . . . H22A H 0.6817 0.2809 0.4654 0.059 Uiso 1 1 calc R . . H22B H 0.6763 0.4036 0.5159 0.059 Uiso 1 1 calc R . . H22C H 0.6427 0.3616 0.4088 0.059 Uiso 1 1 calc R . . S3 S 0.65057(10) 0.3285(2) 0.9823(3) 0.0471(8) Uani 1 1 d . . . O3 O 0.6277(2) 0.2142(5) 0.9536(7) 0.0428(19) Uani 1 1 d . . . C31 C 0.6007(4) 0.4214(9) 0.9732(14) 0.066(4) Uani 1 1 d . . . H31A H 0.5920 0.4324 0.8882 0.099 Uiso 1 1 calc R . . H31B H 0.6094 0.4921 1.0095 0.099 Uiso 1 1 calc R . . H31C H 0.5737 0.3900 1.0170 0.099 Uiso 1 1 calc R . . C32 C 0.6604(5) 0.3208(12) 1.1384(13) 0.066(4) Uani 1 1 d . . . H32A H 0.6873 0.2719 1.1545 0.099 Uiso 1 1 calc R . . H32B H 0.6319 0.2918 1.1783 0.099 Uiso 1 1 calc R . . H32C H 0.6674 0.3944 1.1700 0.099 Uiso 1 1 calc R . . S4 S 0.62496(8) -0.0305(2) 0.9945(3) 0.0393(7) Uani 1 1 d . . . O4 O 0.6579(2) -0.0069(5) 0.8848(7) 0.0400(19) Uani 1 1 d . . . C41 C 0.6153(4) -0.1726(8) 0.9821(13) 0.060(4) Uani 1 1 d . . . H41A H 0.5929 -0.1870 0.9161 0.090 Uiso 1 1 calc R . . H41B H 0.6021 -0.2006 1.0583 0.090 Uiso 1 1 calc R . . H41C H 0.6454 -0.2097 0.9651 0.090 Uiso 1 1 calc R . . C42 C 0.6641(4) -0.0300(11) 1.1176(14) 0.077(5) Uani 1 1 d . . . H42A H 0.6732 0.0459 1.1364 0.115 Uiso 1 1 calc R . . H42B H 0.6925 -0.0727 1.0973 0.115 Uiso 1 1 calc R . . H42C H 0.6484 -0.0628 1.1882 0.115 Uiso 1 1 calc R . . S5 S 0.64153(9) -0.0373(2) 0.5999(3) 0.0413(8) Uani 1 1 d . . . O5 O 0.6698(2) 0.0696(5) 0.6377(7) 0.0345(17) Uani 1 1 d . . . C51 C 0.6107(3) 0.0073(7) 0.4701(12) 0.052(3) Uani 1 1 d . . . H51A H 0.5838 0.0535 0.4945 0.078 Uiso 1 1 calc R . . H51B H 0.5989 -0.0566 0.4253 0.078 Uiso 1 1 calc R . . H51C H 0.6321 0.0499 0.4183 0.078 Uiso 1 1 calc R . . C52 C 0.6872(4) -0.1181(8) 0.5285(13) 0.056(4) Uani 1 1 d . . . H52A H 0.7079 -0.1498 0.5907 0.084 Uiso 1 1 calc R . . H52B H 0.7060 -0.0711 0.4747 0.084 Uiso 1 1 calc R . . H52C H 0.6725 -0.1772 0.4813 0.084 Uiso 1 1 calc R . . S6 S 0.72728(8) 0.16291(19) 0.8414(3) 0.0365(7) Uani 1 1 d . . . O6 O 0.7362(2) 0.1883(6) 0.9688(8) 0.049(2) Uani 1 1 d . . . C62 C 0.7580(3) 0.0432(7) 0.7958(15) 0.049(3) Uani 1 1 d . . . H62A H 0.7466 -0.0199 0.8425 0.073 Uiso 1 1 calc R . . H62B H 0.7921 0.0531 0.8102 0.073 Uiso 1 1 calc R . . H62C H 0.7525 0.0302 0.7094 0.073 Uiso 1 1 calc R . . C61 C 0.7532(3) 0.2643(7) 0.7463(10) 0.041(3) Uani 1 1 d . . . H61A H 0.7388 0.3360 0.7635 0.061 Uiso 1 1 calc R . . H61B H 0.7476 0.2449 0.6614 0.061 Uiso 1 1 calc R . . H61C H 0.7874 0.2679 0.7617 0.061 Uiso 1 1 calc R . . S10 S 0.73716(10) 0.6243(3) 0.9033(4) 0.0616(10) Uani 1 1 d D . . O11 O 0.7184(3) 0.5363(7) 0.9837(9) 0.084(3) Uani 1 1 d D . . O12 O 0.7299(3) 0.7288(6) 0.9489(9) 0.074(3) Uani 1 1 d D . . O13 O 0.7823(2) 0.6003(6) 0.8465(8) 0.062(3) Uani 1 1 d D . . C10 C 0.6968(3) 0.6116(7) 0.7722(12) 0.045(4) Uani 1 1 d D . . F11 F 0.6514(2) 0.6254(5) 0.8014(12) 0.087(2) Uani 1 1 d D . . F12 F 0.6997(3) 0.5185(6) 0.7216(10) 0.125(4) Uani 1 1 d D . . F13 F 0.7051(4) 0.6912(8) 0.6942(9) 0.126(4) Uani 1 1 d D . . S20 S 0.52894(9) 0.2055(2) 0.3120(4) 0.0516(8) Uani 1 1 d D . . O21 O 0.5013(3) 0.1415(5) 0.3970(9) 0.073(3) Uani 1 1 d D . . O22 O 0.5608(3) 0.2822(6) 0.3674(8) 0.076(3) Uani 1 1 d D . . O23 O 0.5486(4) 0.1424(9) 0.2142(10) 0.108(4) Uani 1 1 d D . . C20 C 0.4837(4) 0.2895(10) 0.2429(11) 0.053(3) Uani 1 1 d D . . F21 F 0.4623(3) 0.3559(5) 0.3207(9) 0.077(2) Uani 1 1 d D . . F22 F 0.4495(2) 0.2291(6) 0.1920(7) 0.080(2) Uani 1 1 d D . . F23 F 0.5006(2) 0.3537(7) 0.1541(8) 0.096(3) Uani 1 1 d D . . S30 S 0.39056(10) 0.3305(2) 0.8257(5) 0.0852(17) Uani 1 1 d D . . O31 O 0.3645(3) 0.3798(6) 0.9254(8) 0.048(2) Uani 1 1 d D . . O32 O 0.3971(3) 0.2203(5) 0.8113(12) 0.089(3) Uani 1 1 d D . . O33 O 0.3627(4) 0.3767(9) 0.6933(10) 0.105(5) Uani 1 1 d D . . C30 C 0.4388(5) 0.4084(9) 0.7827(14) 0.104(7) Uani 1 1 d D . . F31 F 0.4689(5) 0.3837(11) 0.8783(12) 0.169(6) Uani 1 1 d D . . F32 F 0.4279(3) 0.5116(5) 0.7708(10) 0.126(4) Uani 1 1 d D . . F33 F 0.4600(4) 0.3745(5) 0.6836(8) 0.098(4) Uani 1 1 d 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 Rh 0.0157(3) 0.0300(3) 0.0510(5) 0.0176(5) -0.0021(5) -0.0009(3) S1 0.0230(11) 0.0318(12) 0.076(2) 0.011(2) -0.0048(18) 0.0039(8) O1 0.022(3) 0.038(4) 0.061(6) 0.007(3) -0.001(3) 0.000(3) C11 0.020(6) 0.064(8) 0.093(11) -0.005(7) -0.014(7) 0.013(5) C12 0.023(5) 0.034(6) 0.066(9) 0.012(5) 0.004(6) 0.007(4) S2 0.0283(13) 0.0219(12) 0.0468(18) 0.0090(12) -0.0117(13) -0.0009(10) O2 0.029(4) 0.024(3) 0.053(5) 0.004(3) -0.006(4) 0.001(3) C21 0.035(6) 0.031(5) 0.052(8) 0.017(5) -0.002(6) -0.005(5) C22 0.035(6) 0.041(6) 0.041(7) 0.007(6) -0.005(6) -0.001(5) S3 0.0371(15) 0.0440(16) 0.060(2) 0.0116(15) -0.0031(17) -0.0033(12) O3 0.020(3) 0.054(4) 0.054(5) 0.026(4) -0.002(4) 0.001(3) C31 0.050(7) 0.052(7) 0.095(11) 0.020(8) -0.014(8) 0.004(6) C32 0.036(7) 0.087(10) 0.074(10) -0.004(9) 0.000(7) -0.003(7) S4 0.0205(13) 0.0396(15) 0.058(2) 0.0225(15) -0.0002(14) 0.0024(11) O4 0.014(3) 0.038(4) 0.068(5) 0.025(4) 0.000(3) 0.000(3) C41 0.052(7) 0.042(6) 0.085(10) 0.034(7) 0.001(7) -0.006(5) C42 0.054(8) 0.072(9) 0.105(13) 0.036(9) -0.012(9) -0.008(6) S5 0.0238(13) 0.0280(14) 0.072(2) 0.0058(14) 0.0073(15) -0.0059(11) O5 0.014(3) 0.029(4) 0.061(5) 0.007(3) 0.011(3) -0.005(2) C51 0.030(6) 0.029(6) 0.098(11) 0.004(6) -0.021(7) -0.003(4) C52 0.049(7) 0.037(7) 0.081(11) -0.005(6) 0.008(7) -0.002(5) S6 0.0159(11) 0.0395(14) 0.054(2) 0.0165(13) -0.0010(11) -0.0033(9) O6 0.023(4) 0.067(5) 0.057(6) 0.010(4) -0.001(4) -0.002(3) C62 0.013(4) 0.035(5) 0.099(9) 0.025(8) -0.001(7) 0.003(3) C61 0.022(5) 0.036(6) 0.065(8) 0.007(5) 0.007(5) -0.002(4) S10 0.0332(16) 0.061(2) 0.091(3) -0.009(2) -0.0136(18) 0.0067(14) O11 0.083(6) 0.074(6) 0.095(8) 0.031(6) -0.025(6) -0.029(5) O12 0.049(5) 0.053(5) 0.122(9) -0.021(5) -0.027(5) 0.010(4) O13 0.020(4) 0.071(5) 0.096(7) 0.002(5) -0.006(4) 0.016(3) C10 0.028(5) 0.028(5) 0.079(12) 0.012(6) -0.004(6) 0.002(4) F11 0.036(3) 0.100(5) 0.124(6) -0.044(6) -0.033(5) 0.008(3) F12 0.124(7) 0.067(6) 0.186(10) -0.061(6) -0.074(8) 0.045(5) F13 0.151(9) 0.127(8) 0.100(8) 0.071(7) -0.024(7) -0.017(7) S20 0.0446(15) 0.0454(14) 0.065(2) -0.0139(19) -0.0110(19) -0.0116(11) O21 0.054(5) 0.048(5) 0.116(8) 0.012(5) 0.014(5) 0.011(4) O22 0.079(6) 0.046(5) 0.104(8) 0.002(5) -0.043(6) -0.016(4) O23 0.094(8) 0.134(9) 0.098(9) -0.048(8) -0.005(7) 0.027(7) C20 0.049(7) 0.066(8) 0.045(8) 0.014(7) -0.017(7) -0.013(7) F21 0.080(5) 0.046(3) 0.106(8) 0.004(5) -0.011(5) 0.018(3) F22 0.041(4) 0.095(5) 0.104(7) -0.011(5) -0.022(4) -0.020(4) F23 0.048(5) 0.115(6) 0.124(8) 0.051(6) -0.037(5) -0.017(4) S30 0.0436(17) 0.0282(14) 0.184(5) -0.025(2) 0.067(3) -0.0071(11) O31 0.032(4) 0.060(5) 0.052(6) -0.005(4) -0.001(4) 0.009(3) O32 0.104(7) 0.040(4) 0.121(9) -0.009(7) 0.035(8) 0.004(4) O33 0.059(7) 0.146(10) 0.110(10) -0.073(8) -0.054(7) 0.032(6) C30 0.146(15) 0.049(7) 0.118(15) 0.026(10) 0.123(14) 0.024(8) F31 0.116(9) 0.252(14) 0.141(12) -0.064(10) -0.076(9) 0.069(9) F32 0.164(8) 0.029(4) 0.185(11) 0.027(5) 0.080(9) 0.005(4) F33 0.164(9) 0.049(4) 0.082(7) 0.019(4) 0.077(7) 0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh O4 2.034(6) . ? Rh O3 2.035(8) . ? Rh O5 2.050(7) . ? Rh O2 2.052(6) . ? Rh O1 2.100(6) . ? Rh S6 2.238(2) . ? S1 O1 1.523(6) . ? S1 C11 1.786(12) . ? S1 C12 1.786(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? S2 O2 1.571(7) . ? S2 C21 1.762(10) . ? S2 C22 1.790(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? S3 O3 1.565(7) . ? S3 C32 1.750(15) . ? S3 C31 1.805(11) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? S4 O4 1.553(8) . ? S4 C42 1.750(14) . ? S4 C41 1.755(11) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? S5 O5 1.581(6) . ? S5 C51 1.763(11) . ? S5 C52 1.801(11) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? S6 O6 1.463(9) . ? S6 C62 1.767(10) . ? S6 C61 1.776(9) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? S10 O12 1.383(7) . ? S10 O13 1.447(7) . ? S10 O11 1.487(8) . ? S10 C10 1.847(12) . ? C10 F12 1.266(10) . ? C10 F13 1.317(11) . ? C10 F11 1.331(10) . ? S20 O22 1.433(7) . ? S20 O23 1.436(9) . ? S20 O21 1.448(8) . ? S20 C20 1.803(12) . ? C20 F21 1.325(12) . ? C20 F22 1.336(11) . ? C20 F23 1.340(11) . ? S30 O32 1.362(6) . ? S30 O31 1.453(8) . ? S30 C30 1.723(13) . ? S30 O33 1.753(11) . ? C30 F32 1.300(11) . ? C30 F33 1.313(12) . ? C30 F31 1.388(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Rh O3 91.7(3) . . ? O4 Rh O5 90.6(3) . . ? O3 Rh O5 176.7(3) . . ? O4 Rh O2 178.1(3) . . ? O3 Rh O2 87.0(3) . . ? O5 Rh O2 90.7(3) . . ? O4 Rh O1 87.5(2) . . ? O3 Rh O1 88.5(3) . . ? O5 Rh O1 89.3(3) . . ? O2 Rh O1 93.9(2) . . ? O4 Rh S6 84.79(18) . . ? O3 Rh S6 94.04(19) . . ? O5 Rh S6 88.51(18) . . ? O2 Rh S6 93.88(18) . . ? O1 Rh S6 171.93(18) . . ? O1 S1 C11 100.6(5) . . ? O1 S1 C12 104.8(4) . . ? C11 S1 C12 99.0(6) . . ? S1 O1 Rh 122.3(4) . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 S2 C21 102.2(5) . . ? O2 S2 C22 105.7(5) . . ? C21 S2 C22 99.4(5) . . ? S2 O2 Rh 116.7(4) . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O3 S3 C32 102.5(6) . . ? O3 S3 C31 103.0(5) . . ? C32 S3 C31 102.2(7) . . ? S3 O3 Rh 115.9(4) . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O4 S4 C42 103.3(5) . . ? O4 S4 C41 102.4(5) . . ? C42 S4 C41 99.3(6) . . ? S4 O4 Rh 117.6(4) . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O5 S5 C51 102.2(4) . . ? O5 S5 C52 101.8(4) . . ? C51 S5 C52 99.4(6) . . ? S5 O5 Rh 115.9(3) . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O6 S6 C62 111.3(6) . . ? O6 S6 C61 110.6(5) . . ? C62 S6 C61 101.7(5) . . ? O6 S6 Rh 113.3(3) . . ? C62 S6 Rh 108.2(3) . . ? C61 S6 Rh 111.1(3) . . ? S6 C62 H62A 109.5 . . ? S6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? S6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? S6 C61 H61A 109.5 . . ? S6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? S6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O12 S10 O13 118.2(5) . . ? O12 S10 O11 113.0(6) . . ? O13 S10 O11 115.2(5) . . ? O12 S10 C10 105.8(5) . . ? O13 S10 C10 100.6(5) . . ? O11 S10 C10 101.0(5) . . ? F12 C10 F13 110.9(11) . . ? F12 C10 F11 106.3(8) . . ? F13 C10 F11 103.6(9) . . ? F12 C10 S10 112.4(7) . . ? F13 C10 S10 110.1(7) . . ? F11 C10 S10 113.1(10) . . ? O22 S20 O23 115.3(6) . . ? O22 S20 O21 114.3(6) . . ? O23 S20 O21 114.0(6) . . ? O22 S20 C20 104.8(5) . . ? O23 S20 C20 104.9(7) . . ? O21 S20 C20 101.5(5) . . ? F21 C20 F22 106.3(9) . . ? F21 C20 F23 106.3(10) . . ? F22 C20 F23 105.6(9) . . ? F21 C20 S20 113.1(8) . . ? F22 C20 S20 112.1(8) . . ? F23 C20 S20 112.9(8) . . ? O32 S30 O31 124.3(6) . . ? O32 S30 C30 113.7(5) . . ? O31 S30 C30 112.4(6) . . ? O32 S30 O33 106.2(7) . . ? O31 S30 O33 105.8(4) . . ? C30 S30 O33 87.0(7) . . ? F32 C30 F33 109.1(10) . . ? F32 C30 F31 115.5(14) . . ? F33 C30 F31 106.7(10) . . ? F32 C30 S30 111.9(9) . . ? F33 C30 S30 114.6(11) . . ? F31 C30 S30 98.8(10) . . ? 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 C11 S1 O1 Rh 158.4(6) . . . . ? C12 S1 O1 Rh -99.2(5) . . . . ? O4 Rh O1 S1 129.8(5) . . . . ? O3 Rh O1 S1 38.0(5) . . . . ? O5 Rh O1 S1 -139.5(5) . . . . ? O2 Rh O1 S1 -48.9(5) . . . . ? S6 Rh O1 S1 146.6(13) . . . . ? C21 S2 O2 Rh 138.7(5) . . . . ? C22 S2 O2 Rh -117.8(5) . . . . ? O4 Rh O2 S2 180(100) . . . . ? O3 Rh O2 S2 -132.0(4) . . . . ? O5 Rh O2 S2 45.6(4) . . . . ? O1 Rh O2 S2 -43.7(4) . . . . ? S6 Rh O2 S2 134.2(4) . . . . ? C32 S3 O3 Rh -138.8(5) . . . . ? C31 S3 O3 Rh 115.4(6) . . . . ? O4 Rh O3 S3 134.4(4) . . . . ? O5 Rh O3 S3 -90(4) . . . . ? O2 Rh O3 S3 -44.2(4) . . . . ? O1 Rh O3 S3 -138.2(4) . . . . ? S6 Rh O3 S3 49.5(4) . . . . ? C42 S4 O4 Rh -111.7(6) . . . . ? C41 S4 O4 Rh 145.4(5) . . . . ? O3 Rh O4 S4 29.1(4) . . . . ? O5 Rh O4 S4 -148.6(4) . . . . ? O2 Rh O4 S4 77(9) . . . . ? O1 Rh O4 S4 -59.3(4) . . . . ? S6 Rh O4 S4 123.0(4) . . . . ? C51 S5 O5 Rh 113.7(5) . . . . ? C52 S5 O5 Rh -143.8(5) . . . . ? O4 Rh O5 S5 52.3(4) . . . . ? O3 Rh O5 S5 -83(4) . . . . ? O2 Rh O5 S5 -129.0(4) . . . . ? O1 Rh O5 S5 -35.2(4) . . . . ? S6 Rh O5 S5 137.1(4) . . . . ? O4 Rh S6 O6 -74.3(4) . . . . ? O3 Rh S6 O6 17.0(4) . . . . ? O5 Rh S6 O6 -165.1(4) . . . . ? O2 Rh S6 O6 104.3(4) . . . . ? O1 Rh S6 O6 -91.1(16) . . . . ? O4 Rh S6 C62 49.6(6) . . . . ? O3 Rh S6 C62 140.9(6) . . . . ? O5 Rh S6 C62 -41.2(6) . . . . ? O2 Rh S6 C62 -131.8(6) . . . . ? O1 Rh S6 C62 32.8(17) . . . . ? O4 Rh S6 C61 160.4(4) . . . . ? O3 Rh S6 C61 -108.2(4) . . . . ? O5 Rh S6 C61 69.6(4) . . . . ? O2 Rh S6 C61 -21.0(4) . . . . ? O1 Rh S6 C61 143.6(16) . . . . ? O12 S10 C10 F12 -179.7(9) . . . . ? O13 S10 C10 F12 56.8(9) . . . . ? O11 S10 C10 F12 -61.7(9) . . . . ? O12 S10 C10 F13 56.1(9) . . . . ? O13 S10 C10 F13 -67.5(9) . . . . ? O11 S10 C10 F13 174.0(9) . . . . ? O12 S10 C10 F11 -59.3(8) . . . . ? O13 S10 C10 F11 177.2(7) . . . . ? O11 S10 C10 F11 58.7(8) . . . . ? O22 S20 C20 F21 -56.7(9) . . . . ? O23 S20 C20 F21 -178.5(8) . . . . ? O21 S20 C20 F21 62.5(9) . . . . ? O22 S20 C20 F22 -176.8(8) . . . . ? O23 S20 C20 F22 61.4(10) . . . . ? O21 S20 C20 F22 -57.6(10) . . . . ? O22 S20 C20 F23 64.1(10) . . . . ? O23 S20 C20 F23 -57.7(10) . . . . ? O21 S20 C20 F23 -176.7(8) . . . . ? O32 S30 C30 F32 165.1(12) . . . . ? O31 S30 C30 F32 -47.1(14) . . . . ? O33 S30 C30 F32 58.8(12) . . . . ? O32 S30 C30 F33 40.3(14) . . . . ? O31 S30 C30 F33 -171.9(9) . . . . ? O33 S30 C30 F33 -66.0(11) . . . . ? O32 S30 C30 F31 -72.8(11) . . . . ? O31 S30 C30 F31 75.0(9) . . . . ? O33 S30 C30 F31 -179.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.037 _refine_diff_density_min -0.604 _refine_diff_density_rms 0.105 #end data_rh-6dmso_Istar data_rh-5dmso_II _database_code_depnum_ccdc_archive 'CCDC 789616' #TrackingRef '- cif-revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H30 Cl O5 Rh S5, 2(C F3 O3 S)' _chemical_formula_sum 'C12 H30 Cl F6 O11 Rh S7' _chemical_formula_weight 827.14 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' Rh Rh -1.1178 0.9187 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 27.987(8) _cell_length_b 11.065(3) _cell_length_c 10.176(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3151.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 22003 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 26.01 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.744 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8101 _exptl_absorpt_correction_T_max 0.8955 _exptl_absorpt_process_details 'X-red (STOE, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'X-calibur 2 with Sapphire-III CCD detector' _diffrn_measurement_method '\w-scans at different \f' _diffrn_detector_area_resol_mean 12 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% . _diffrn_reflns_number 22003 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5829 _reflns_number_gt 3053 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2003)' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg, 2001)' _computing_publication_material 'Platon (Spek, 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. In total 209 restraints: 1 floating origin restraint 14 dfix restraints for stabilizing the triflate geometry, not as strict as the dfix used in 1 or 1* 98 DELU restraints for all atoms and 96 ISOR restraints for the atoms of the triflate ions. CF3SO3, 2 molecules, 8 atoms / molecule and 6 ADP per atoms which give 2*6*8 = 96 restraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00078(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(4) _refine_ls_number_reflns 5829 _refine_ls_number_parameters 347 _refine_ls_number_restraints 209 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0882 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.391427(17) 0.99579(7) 0.26168(5) 0.03377(14) Uani 1 1 d U . . S1 S 0.40047(8) 1.1826(2) 0.1778(3) 0.0549(6) Uani 1 1 d U . . O1 O 0.3891(3) 1.2748(5) 0.2777(8) 0.090(2) Uani 1 1 d U . . C12 C 0.4572(4) 1.2107(9) 0.1101(11) 0.085(4) Uani 1 1 d U . . H12A H 0.4811 1.2018 0.1770 0.128 Uiso 1 1 calc R . . H12B H 0.4582 1.2915 0.0757 0.128 Uiso 1 1 calc R . . H12C H 0.4633 1.1541 0.0405 0.128 Uiso 1 1 calc R . . C11 C 0.3623(3) 1.2046(9) 0.0416(10) 0.067(3) Uani 1 1 d U . . H11A H 0.3299 1.1896 0.0674 0.101 Uiso 1 1 calc R . . H11B H 0.3711 1.1499 -0.0275 0.101 Uiso 1 1 calc R . . H11C H 0.3653 1.2863 0.0109 0.101 Uiso 1 1 calc R . . S2 S 0.40788(8) 0.9003(2) 0.0709(2) 0.0492(6) Uani 1 1 d U . . O2 O 0.4217(2) 0.9804(6) -0.0419(6) 0.084(2) Uani 1 1 d U . . C21 C 0.3583(3) 0.8106(8) 0.0291(10) 0.061(3) Uani 1 1 d U . . H21A H 0.3312 0.8616 0.0130 0.092 Uiso 1 1 calc R . . H21B H 0.3513 0.7564 0.1002 0.092 Uiso 1 1 calc R . . H21C H 0.3655 0.7648 -0.0485 0.092 Uiso 1 1 calc R . . C22 C 0.4524(3) 0.7881(9) 0.0962(11) 0.082(4) Uani 1 1 d U . . H22A H 0.4820 0.8263 0.1198 0.123 Uiso 1 1 calc R . . H22B H 0.4567 0.7426 0.0168 0.123 Uiso 1 1 calc R . . H22C H 0.4425 0.7349 0.1656 0.123 Uiso 1 1 calc R . . O3 O 0.32042(15) 1.0056(5) 0.2067(4) 0.0423(11) Uani 1 1 d U . . S3 S 0.28102(6) 0.9938(2) 0.31275(16) 0.0409(4) Uani 1 1 d U . . C32 C 0.2413(3) 0.8868(9) 0.2418(13) 0.082(4) Uani 1 1 d U . . H32A H 0.2547 0.8073 0.2493 0.123 Uiso 1 1 calc R . . H32B H 0.2364 0.9059 0.1508 0.123 Uiso 1 1 calc R . . H32C H 0.2112 0.8895 0.2871 0.123 Uiso 1 1 calc R . . C31 C 0.2468(4) 1.1254(9) 0.2812(14) 0.091(4) Uani 1 1 d U . . H31A H 0.2636 1.1950 0.3131 0.137 Uiso 1 1 calc R . . H31B H 0.2165 1.1191 0.3250 0.137 Uiso 1 1 calc R . . H31C H 0.2417 1.1333 0.1883 0.137 Uiso 1 1 calc R . . O4 O 0.37547(19) 0.8239(5) 0.3367(6) 0.0484(13) Uani 1 1 d U . . S4 S 0.39256(8) 0.7858(2) 0.4767(3) 0.0610(7) Uani 1 1 d U . . C42 C 0.3966(5) 0.6260(10) 0.4548(14) 0.129(5) Uani 1 1 d U . . H42A H 0.4239 0.6073 0.4014 0.193 Uiso 1 1 calc R . . H42B H 0.3681 0.5971 0.4124 0.193 Uiso 1 1 calc R . . H42C H 0.3999 0.5875 0.5389 0.193 Uiso 1 1 calc R . . C41 C 0.3413(3) 0.7878(9) 0.5747(11) 0.076(3) Uani 1 1 d U . . H41A H 0.3336 0.8697 0.5974 0.114 Uiso 1 1 calc R . . H41B H 0.3469 0.7422 0.6534 0.114 Uiso 1 1 calc R . . H41C H 0.3151 0.7525 0.5272 0.114 Uiso 1 1 calc R . . O5 O 0.37136(18) 1.0593(5) 0.4445(5) 0.0462(14) Uani 1 1 d U . . S5 S 0.39934(8) 1.1588(2) 0.5223(2) 0.0545(6) Uani 1 1 d U . . C52 C 0.4107(4) 1.0833(10) 0.6768(12) 0.086(3) Uani 1 1 d U . . H52A H 0.4360 1.0256 0.6655 0.128 Uiso 1 1 calc R . . H52B H 0.3823 1.0425 0.7052 0.128 Uiso 1 1 calc R . . H52C H 0.4200 1.1419 0.7416 0.128 Uiso 1 1 calc R . . C51 C 0.3523(4) 1.2565(9) 0.5713(12) 0.088(4) Uani 1 1 d U . . H51A H 0.3418 1.3032 0.4971 0.132 Uiso 1 1 calc R . . H51B H 0.3635 1.3098 0.6390 0.132 Uiso 1 1 calc R . . H51C H 0.3261 1.2094 0.6041 0.132 Uiso 1 1 calc R . . Cl1 Cl 0.47013(6) 0.9893(2) 0.3293(2) 0.0527(5) Uani 1 1 d U . . S10 S 0.24560(8) 0.5141(3) 0.3419(2) 0.0590(6) Uani 1 1 d DU . . O11 O 0.1983(2) 0.5184(11) 0.2973(9) 0.133(3) Uani 1 1 d DU . . O12 O 0.2625(3) 0.6196(7) 0.4065(9) 0.112(3) Uani 1 1 d DU . . O13 O 0.2563(4) 0.4040(8) 0.4063(9) 0.126(4) Uani 1 1 d DU . . C10 C 0.2801(3) 0.5041(11) 0.1930(10) 0.070(2) Uani 1 1 d DU . . F11 F 0.2711(3) 0.4104(7) 0.1203(7) 0.107(3) Uani 1 1 d DU . . F12 F 0.2715(3) 0.5974(8) 0.1165(8) 0.135(3) Uani 1 1 d DU . . F13 F 0.3255(2) 0.5059(9) 0.2129(7) 0.141(3) Uani 1 1 d DU . . S20 S 0.41470(9) 0.5141(3) 0.8506(3) 0.0723(7) Uani 1 1 d DU . . O21 O 0.4150(5) 0.6402(8) 0.8000(9) 0.167(4) Uani 1 1 d DU . . O22 O 0.4211(3) 0.5138(7) 0.9906(7) 0.101(2) Uani 1 1 d DU . . O23 O 0.3806(4) 0.4498(12) 0.7965(12) 0.198(6) Uani 1 1 d DU . . C20 C 0.4704(5) 0.4654(12) 0.7828(14) 0.123(4) Uani 1 1 d DU . . F21 F 0.4705(4) 0.4750(11) 0.6553(10) 0.211(5) Uani 1 1 d DU . . F22 F 0.5062(3) 0.5303(13) 0.8241(12) 0.216(5) Uani 1 1 d DU . . F23 F 0.4754(5) 0.3522(10) 0.8225(11) 0.212(5) Uani 1 1 d DU . . 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 0.0286(2) 0.0456(3) 0.0271(3) 0.0002(4) -0.0004(3) 0.0009(4) S1 0.0653(15) 0.0527(13) 0.0466(16) 0.0063(11) 0.0037(12) -0.0030(11) O1 0.155(6) 0.046(3) 0.068(5) -0.014(4) 0.011(5) 0.016(4) C12 0.068(6) 0.075(7) 0.112(11) 0.026(6) 0.024(6) -0.018(5) C11 0.075(6) 0.080(7) 0.046(6) 0.023(5) 0.005(5) 0.018(5) S2 0.0427(12) 0.0628(14) 0.0422(14) -0.0069(11) 0.0043(9) 0.0047(10) O2 0.101(5) 0.104(5) 0.047(4) 0.007(4) 0.036(3) -0.005(4) C21 0.057(5) 0.078(6) 0.049(7) -0.026(5) -0.015(5) -0.010(4) C22 0.063(6) 0.089(7) 0.094(10) -0.044(6) -0.028(6) 0.038(5) O3 0.031(2) 0.067(3) 0.029(3) 0.000(3) -0.0009(17) 0.007(3) S3 0.0293(8) 0.0549(11) 0.0384(11) 0.0018(13) -0.0002(6) 0.0025(11) C32 0.065(7) 0.091(6) 0.089(10) -0.020(7) 0.010(6) -0.033(5) C31 0.087(8) 0.073(5) 0.114(11) 0.009(7) 0.030(7) 0.038(5) O4 0.051(3) 0.054(3) 0.040(3) 0.014(3) -0.010(3) -0.001(3) S4 0.0452(13) 0.0833(16) 0.0543(16) 0.0264(13) -0.0037(12) 0.0078(13) C42 0.200(15) 0.082(7) 0.104(11) 0.034(7) 0.001(9) 0.069(9) C41 0.079(7) 0.101(8) 0.048(7) 0.027(6) 0.010(5) 0.005(6) O5 0.036(3) 0.068(3) 0.035(3) -0.013(3) 0.000(2) -0.003(2) S5 0.0475(14) 0.0749(15) 0.0412(15) -0.0183(11) 0.0022(10) -0.0101(11) C52 0.077(7) 0.128(9) 0.051(7) 0.000(6) -0.029(6) -0.021(6) C51 0.072(7) 0.096(7) 0.097(9) -0.061(7) -0.018(6) 0.016(5) Cl1 0.0290(9) 0.0782(14) 0.0508(12) -0.0037(15) -0.0056(8) 0.0005(12) S10 0.0521(13) 0.0653(15) 0.0595(16) -0.0005(16) -0.0009(10) -0.0012(13) O11 0.050(3) 0.230(9) 0.118(8) -0.030(7) -0.016(4) 0.011(5) O12 0.134(7) 0.107(6) 0.093(7) -0.039(5) 0.012(5) -0.042(5) O13 0.198(9) 0.099(6) 0.080(7) 0.032(5) 0.038(6) 0.039(6) C10 0.061(5) 0.072(5) 0.077(5) 0.001(5) 0.006(4) -0.002(7) F11 0.124(6) 0.107(5) 0.090(6) -0.034(4) 0.024(4) 0.000(4) F12 0.192(8) 0.115(5) 0.099(7) 0.036(5) 0.047(5) 0.017(6) F13 0.068(4) 0.223(7) 0.131(7) -0.019(7) 0.019(3) -0.009(5) S20 0.0701(15) 0.0911(19) 0.0557(18) -0.0149(18) -0.0058(11) 0.0011(15) O21 0.268(12) 0.130(6) 0.103(8) 0.013(6) -0.015(7) 0.093(6) O22 0.151(6) 0.093(5) 0.060(4) -0.010(4) 0.004(4) -0.009(5) O23 0.136(7) 0.296(12) 0.162(11) -0.130(9) -0.001(6) -0.086(8) C20 0.127(7) 0.136(9) 0.107(9) 0.021(8) 0.029(8) 0.037(6) F21 0.218(9) 0.312(12) 0.102(7) 0.048(7) 0.065(5) 0.133(8) F22 0.083(5) 0.295(10) 0.269(12) 0.078(9) -0.003(6) -0.043(7) F23 0.276(11) 0.159(6) 0.201(11) 0.067(6) 0.063(8) 0.109(6) _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 O5 2.067(5) . ? Rh1 O3 2.067(4) . ? Rh1 O4 2.098(5) . ? Rh1 S1 2.251(2) . ? Rh1 S2 2.258(2) . ? Rh1 Cl1 2.3087(18) . ? S1 O1 1.475(7) . ? S1 C12 1.758(10) . ? S1 C11 1.766(10) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? S2 O2 1.500(6) . ? S2 C21 1.757(8) . ? S2 C22 1.777(9) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? O3 S3 1.549(5) . ? S3 C31 1.772(9) . ? S3 C32 1.777(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? O4 S4 1.561(6) . ? S4 C41 1.748(10) . ? S4 C42 1.786(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? O5 S5 1.566(5) . ? S5 C51 1.775(9) . ? S5 C52 1.808(12) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? S10 O11 1.401(7) . ? S10 O13 1.415(8) . ? S10 O12 1.421(8) . ? S10 C10 1.799(10) . ? C10 F13 1.287(10) . ? C10 F11 1.298(10) . ? C10 F12 1.315(10) . ? S20 O23 1.311(8) . ? S20 O22 1.436(7) . ? S20 O21 1.487(9) . ? S20 C20 1.788(13) . ? C20 F22 1.301(13) . ? C20 F21 1.303(14) . ? C20 F23 1.323(12) . ? 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 O5 Rh1 O3 87.98(19) . . ? O5 Rh1 O4 85.6(2) . . ? O3 Rh1 O4 86.6(2) . . ? O5 Rh1 S1 93.42(16) . . ? O3 Rh1 S1 87.55(17) . . ? O4 Rh1 S1 174.14(17) . . ? O5 Rh1 S2 171.38(16) . . ? O3 Rh1 S2 89.29(14) . . ? O4 Rh1 S2 86.10(18) . . ? S1 Rh1 S2 94.63(9) . . ? O5 Rh1 Cl1 90.09(15) . . ? O3 Rh1 Cl1 177.98(16) . . ? O4 Rh1 Cl1 93.81(16) . . ? S1 Rh1 Cl1 91.96(9) . . ? S2 Rh1 Cl1 92.71(8) . . ? O1 S1 C12 110.0(5) . . ? O1 S1 C11 108.4(5) . . ? C12 S1 C11 102.3(5) . . ? O1 S1 Rh1 110.5(3) . . ? C12 S1 Rh1 114.4(4) . . ? C11 S1 Rh1 110.9(3) . . ? S1 C12 H12A 109.5 . . ? S1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? S1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? S1 C11 H11A 109.5 . . ? S1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? S1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 S2 C21 110.6(5) . . ? O2 S2 C22 110.1(5) . . ? C21 S2 C22 101.2(5) . . ? O2 S2 Rh1 115.7(3) . . ? C21 S2 Rh1 108.1(3) . . ? C22 S2 Rh1 110.2(4) . . ? S2 C21 H21A 109.5 . . ? S2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S2 C22 H22A 109.5 . . ? S2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S3 O3 Rh1 119.4(2) . . ? O3 S3 C31 100.9(5) . . ? O3 S3 C32 102.6(4) . . ? C31 S3 C32 97.8(5) . . ? S3 C32 H32A 109.5 . . ? S3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? S3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? S3 C31 H31A 109.5 . . ? S3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? S3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? S4 O4 Rh1 120.8(3) . . ? O4 S4 C41 105.4(4) . . ? O4 S4 C42 99.9(5) . . ? C41 S4 C42 97.8(6) . . ? S4 C42 H42A 109.5 . . ? S4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? S4 C41 H41A 109.5 . . ? S4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? S5 O5 Rh1 123.9(3) . . ? O5 S5 C51 101.5(4) . . ? O5 S5 C52 101.7(4) . . ? C51 S5 C52 99.7(6) . . ? S5 C52 H52A 109.5 . . ? S5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? S5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? S5 C51 H51A 109.5 . . ? S5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? S5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O11 S10 O13 112.3(7) . . ? O11 S10 O12 115.9(6) . . ? O13 S10 O12 115.0(6) . . ? O11 S10 C10 103.6(5) . . ? O13 S10 C10 103.0(5) . . ? O12 S10 C10 105.2(5) . . ? F13 C10 F11 107.0(9) . . ? F13 C10 F12 105.1(9) . . ? F11 C10 F12 104.7(9) . . ? F13 C10 S10 113.3(7) . . ? F11 C10 S10 115.2(7) . . ? F12 C10 S10 110.7(7) . . ? O23 S20 O22 120.4(7) . . ? O23 S20 O21 111.6(9) . . ? O22 S20 O21 110.2(6) . . ? O23 S20 C20 108.0(7) . . ? O22 S20 C20 105.8(6) . . ? O21 S20 C20 98.3(6) . . ? F22 C20 F21 105.9(13) . . ? F22 C20 F23 110.1(14) . . ? F21 C20 F23 112.4(13) . . ? F22 C20 S20 112.3(10) . . ? F21 C20 S20 111.3(10) . . ? F23 C20 S20 105.1(10) . . ? 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 O5 Rh1 S1 O1 -0.4(4) . . . . ? O3 Rh1 S1 O1 87.4(4) . . . . ? O4 Rh1 S1 O1 80(2) . . . . ? S2 Rh1 S1 O1 176.5(4) . . . . ? Cl1 Rh1 S1 O1 -90.6(4) . . . . ? O5 Rh1 S1 C12 124.4(5) . . . . ? O3 Rh1 S1 C12 -147.8(5) . . . . ? O4 Rh1 S1 C12 -155.6(19) . . . . ? S2 Rh1 S1 C12 -58.7(4) . . . . ? Cl1 Rh1 S1 C12 34.2(4) . . . . ? O5 Rh1 S1 C11 -120.6(4) . . . . ? O3 Rh1 S1 C11 -32.7(4) . . . . ? O4 Rh1 S1 C11 -41(2) . . . . ? S2 Rh1 S1 C11 56.4(4) . . . . ? Cl1 Rh1 S1 C11 149.2(4) . . . . ? O5 Rh1 S2 O2 162.5(11) . . . . ? O3 Rh1 S2 O2 90.9(4) . . . . ? O4 Rh1 S2 O2 177.6(3) . . . . ? S1 Rh1 S2 O2 3.4(3) . . . . ? Cl1 Rh1 S2 O2 -88.8(3) . . . . ? O5 Rh1 S2 C21 37.8(12) . . . . ? O3 Rh1 S2 C21 -33.7(4) . . . . ? O4 Rh1 S2 C21 53.0(4) . . . . ? S1 Rh1 S2 C21 -121.2(4) . . . . ? Cl1 Rh1 S2 C21 146.6(4) . . . . ? O5 Rh1 S2 C22 -71.9(12) . . . . ? O3 Rh1 S2 C22 -143.4(4) . . . . ? O4 Rh1 S2 C22 -56.8(4) . . . . ? S1 Rh1 S2 C22 129.1(4) . . . . ? Cl1 Rh1 S2 C22 36.9(4) . . . . ? O5 Rh1 O3 S3 -27.1(4) . . . . ? O4 Rh1 O3 S3 58.6(4) . . . . ? S1 Rh1 O3 S3 -120.6(3) . . . . ? S2 Rh1 O3 S3 144.7(3) . . . . ? Cl1 Rh1 O3 S3 -45(5) . . . . ? Rh1 O3 S3 C31 127.3(5) . . . . ? Rh1 O3 S3 C32 -132.0(5) . . . . ? O5 Rh1 O4 S4 -44.8(4) . . . . ? O3 Rh1 O4 S4 -133.1(4) . . . . ? S1 Rh1 O4 S4 -125.3(17) . . . . ? S2 Rh1 O4 S4 137.4(4) . . . . ? Cl1 Rh1 O4 S4 45.0(4) . . . . ? Rh1 O4 S4 C41 106.5(5) . . . . ? Rh1 O4 S4 C42 -152.5(6) . . . . ? O3 Rh1 O5 S5 -136.4(4) . . . . ? O4 Rh1 O5 S5 136.8(4) . . . . ? S1 Rh1 O5 S5 -49.0(4) . . . . ? S2 Rh1 O5 S5 152.0(8) . . . . ? Cl1 Rh1 O5 S5 43.0(4) . . . . ? Rh1 O5 S5 C51 132.6(5) . . . . ? Rh1 O5 S5 C52 -124.9(5) . . . . ? O11 S10 C10 F13 176.4(9) . . . . ? O13 S10 C10 F13 -66.5(10) . . . . ? O12 S10 C10 F13 54.3(10) . . . . ? O11 S10 C10 F11 -59.9(10) . . . . ? O13 S10 C10 F11 57.2(9) . . . . ? O12 S10 C10 F11 178.0(8) . . . . ? O11 S10 C10 F12 58.6(9) . . . . ? O13 S10 C10 F12 175.8(9) . . . . ? O12 S10 C10 F12 -63.4(9) . . . . ? O23 S20 C20 F22 175.4(11) . . . . ? O22 S20 C20 F22 -54.4(11) . . . . ? O21 S20 C20 F22 59.5(11) . . . . ? O23 S20 C20 F21 56.9(13) . . . . ? O22 S20 C20 F21 -172.9(11) . . . . ? O21 S20 C20 F21 -59.1(12) . . . . ? O23 S20 C20 F23 -64.9(13) . . . . ? O22 S20 C20 F23 65.2(11) . . . . ? O21 S20 C20 F23 179.1(11) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.576 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.082 #end data_rh-5dmso_II #========================================================================= # END of CIF #=========================================================================