# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lever, Susan' _publ_contact_author_email levers@missouri.edu _publ_section_title ; The Complexation of Rhodium(III) with Acyclic Diaminedithioether (DADTE) Ligands ; loop_ _publ_author_name Z.Akgun H.Engelbrecht K.-H.Fan C.Barnes C.Cutler S.Jurisson ; S.Lever ; data_232-N2S2-2P-Rh _database_code_depnum_ccdc_archive 'CCDC 781961' #TrackingRef '232N2S2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H42 N2 O2 S2 Cl2 Rh . P F6 . 0.5(C2H6O)' _chemical_formula_weight 835.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2~1~/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8256(11) _cell_length_b 10.4632(6) _cell_length_c 18.7671(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.3150(10) _cell_angle_gamma 90.00 _cell_volume 3490.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5708 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.1 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.871 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 24240 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0305 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.14 _reflns_number_total 7684 _reflns_number_gt 6278 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+3.2087P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7684 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.006 _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 0.721597(10) 0.198658(19) 0.333267(10) 0.02246(7) Uani 1 1 d . . . Cl1 Cl 0.78349(3) 0.06489(6) 0.25627(3) 0.02910(14) Uani 1 1 d . . . S1 S 0.73997(3) 0.03909(6) 0.41909(3) 0.02675(14) Uani 1 1 d . . . P1 P 0.60893(4) -0.18053(8) 0.67078(4) 0.03710(18) Uani 1 1 d . . . F1 F 0.62800(14) -0.1081(3) 0.74320(13) 0.0937(9) Uani 1 1 d . . . O1 O 1.02132(11) 0.2341(2) 0.65056(11) 0.0397(5) Uani 1 1 d . . . N1 N 0.62058(12) 0.1022(2) 0.30416(11) 0.0267(5) Uani 1 1 d . . . C1 C 0.64780(15) -0.0467(3) 0.40751(15) 0.0317(6) Uani 1 1 d . . . Cl2 Cl 0.65313(4) 0.33154(7) 0.40450(4) 0.03347(15) Uani 1 1 d . . . S2 S 0.82999(3) 0.31423(6) 0.37088(3) 0.02568(14) Uani 1 1 d . . . F2 F 0.66483(18) -0.2900(3) 0.69216(17) 0.1114(13) Uani 1 1 d . . . O2 O 1.18787(10) 0.4149(2) 0.47452(11) 0.0432(5) Uani 1 1 d . . . N2 N 0.70725(13) 0.3359(2) 0.25180(12) 0.0269(5) Uani 1 1 d . . . C2 C 0.62428(15) -0.0326(3) 0.32816(14) 0.0308(6) Uani 1 1 d . . . H2A H 0.6606 -0.0792 0.3003 0.037 Uiso 1 1 calc R . . H2B H 0.5743 -0.0726 0.3180 0.037 Uiso 1 1 calc R . . F3 F 0.59115(17) -0.2435(4) 0.59523(16) 0.1136(12) Uani 1 1 d . . . C3 C 0.59117(15) 0.1067(3) 0.22748(14) 0.0321(6) Uani 1 1 d . . . H3A H 0.5397 0.0705 0.2231 0.039 Uiso 1 1 calc R . . H3B H 0.6233 0.0524 0.1991 0.039 Uiso 1 1 calc R . . F4 F 0.55354(15) -0.0665(3) 0.64950(16) 0.1007(10) Uani 1 1 d . . . C4 C 0.58898(16) 0.2399(3) 0.19671(15) 0.0350(6) Uani 1 1 d . . . H4A H 0.5643 0.2973 0.2298 0.042 Uiso 1 1 calc R . . H4B H 0.5577 0.2390 0.1508 0.042 Uiso 1 1 calc R . . F5 F 0.67567(12) -0.1067(2) 0.63569(13) 0.0659(6) Uani 1 1 d . . . C5 C 0.66569(16) 0.2944(3) 0.18384(14) 0.0331(6) Uani 1 1 d . . . H5A H 0.6955 0.2287 0.1606 0.040 Uiso 1 1 calc R . . H5B H 0.6594 0.3683 0.1510 0.040 Uiso 1 1 calc R . . F6 F 0.54252(16) -0.2518(3) 0.70358(18) 0.1028(11) Uani 1 1 d . . . C6 C 0.78102(15) 0.3922(3) 0.23601(14) 0.0323(6) Uani 1 1 d . . . H6A H 0.7723 0.4623 0.2009 0.039 Uiso 1 1 calc R . . H6B H 0.8116 0.3260 0.2141 0.039 Uiso 1 1 calc R . . C7 C 0.82440(15) 0.4439(3) 0.30244(14) 0.0290(6) Uani 1 1 d . . . C8 C 0.66308(19) -0.1869(3) 0.4252(2) 0.0470(8) Uani 1 1 d . . . H8A H 0.6829 -0.1947 0.4751 0.071 Uiso 1 1 calc R . . H8B H 0.7000 -0.2207 0.3939 0.071 Uiso 1 1 calc R . . H8C H 0.6162 -0.2356 0.4179 0.071 Uiso 1 1 calc R . . C9 C 0.58873(16) 0.0088(3) 0.45392(16) 0.0410(7) Uani 1 1 d . . . H9A H 0.5854 0.1014 0.4467 0.062 Uiso 1 1 calc R . . H9B H 0.6033 -0.0092 0.5043 0.062 Uiso 1 1 calc R . . H9C H 0.5397 -0.0303 0.4405 0.062 Uiso 1 1 calc R . . C10 C 0.90217(17) 0.4875(3) 0.28306(17) 0.0392(7) Uani 1 1 d . . . H10A H 0.9274 0.4169 0.2603 0.059 Uiso 1 1 calc R . . H10B H 0.9322 0.5137 0.3265 0.059 Uiso 1 1 calc R . . H10C H 0.8967 0.5599 0.2500 0.059 Uiso 1 1 calc R . . C11 C 0.78398(17) 0.5549(3) 0.33652(16) 0.0379(7) Uani 1 1 d . . . H11A H 0.7744 0.6231 0.3012 0.057 Uiso 1 1 calc R . . H11B H 0.8156 0.5879 0.3774 0.057 Uiso 1 1 calc R . . H11C H 0.7361 0.5247 0.3528 0.057 Uiso 1 1 calc R . . C12 C 0.74023(15) 0.0967(3) 0.51107(14) 0.0346(6) Uani 1 1 d . . . H12A H 0.7071 0.1725 0.5123 0.042 Uiso 1 1 calc R . . H12B H 0.7194 0.0295 0.5410 0.042 Uiso 1 1 calc R . . C13 C 0.81783(15) 0.1321(3) 0.54212(13) 0.0299(6) Uani 1 1 d . . . C14 C 0.83169(16) 0.2550(3) 0.56851(14) 0.0325(6) Uani 1 1 d . . . H14 H 0.7939 0.3186 0.5614 0.039 Uiso 1 1 calc R . . C15 C 0.89966(16) 0.2858(3) 0.60492(14) 0.0308(6) Uani 1 1 d . . . H15 H 0.9079 0.3695 0.6235 0.037 Uiso 1 1 calc R . . C16 C 0.95569(16) 0.1939(3) 0.61417(14) 0.0312(6) Uani 1 1 d . . . C17 C 0.94364(17) 0.0720(3) 0.58701(16) 0.0371(7) Uani 1 1 d . . . H17 H 0.9823 0.0096 0.5924 0.045 Uiso 1 1 calc R . . C18 C 0.87471(16) 0.0415(3) 0.55183(15) 0.0355(6) Uani 1 1 d . . . H18 H 0.8663 -0.0427 0.5341 0.043 Uiso 1 1 calc R . . C19 C 1.08206(18) 0.1445(3) 0.6577(2) 0.0517(9) Uani 1 1 d . . . H19A H 1.0668 0.0698 0.6847 0.078 Uiso 1 1 calc R . . H19B H 1.1259 0.1848 0.6832 0.078 Uiso 1 1 calc R . . H19C H 1.0951 0.1174 0.6102 0.078 Uiso 1 1 calc R . . C20 C 0.91151(15) 0.2182(3) 0.35106(17) 0.0353(6) Uani 1 1 d . . . H20A H 0.9054 0.1308 0.3699 0.042 Uiso 1 1 calc R . . H20B H 0.9131 0.2117 0.2986 0.042 Uiso 1 1 calc R . . C21 C 0.98541(15) 0.2726(3) 0.38250(15) 0.0301(6) Uani 1 1 d . . . C22 C 1.04759(16) 0.2766(3) 0.34267(16) 0.0355(6) Uani 1 1 d . . . H22 H 1.0429 0.2477 0.2945 0.043 Uiso 1 1 calc R . . C23 C 1.11695(15) 0.3218(3) 0.37134(15) 0.0331(6) Uani 1 1 d . . . H23 H 1.1591 0.3226 0.3432 0.040 Uiso 1 1 calc R . . C24 C 1.12388(15) 0.3654(3) 0.44071(15) 0.0325(6) Uani 1 1 d . . . C25 C 1.06132(17) 0.3623(4) 0.48118(16) 0.0554(10) Uani 1 1 d . . . H25 H 1.0656 0.3919 0.5292 0.066 Uiso 1 1 calc R . . C26 C 0.99367(17) 0.3168(4) 0.45207(16) 0.0482(9) Uani 1 1 d . . . H26 H 0.9516 0.3156 0.4803 0.058 Uiso 1 1 calc R . . C27 C 1.25420(15) 0.4159(3) 0.43660(17) 0.0409(7) Uani 1 1 d . . . H27A H 1.2662 0.3284 0.4227 0.061 Uiso 1 1 calc R . . H27B H 1.2961 0.4509 0.4673 0.061 Uiso 1 1 calc R . . H27C H 1.2458 0.4690 0.3937 0.061 Uiso 1 1 calc R . . C1S C 0.4911(4) -0.4630(5) 0.4683(4) 0.098(2) Uani 1 1 d . . . H2N H 0.6845(18) 0.395(3) 0.2707(18) 0.043(10) Uiso 1 1 d . . . H1N H 0.5898(16) 0.141(3) 0.3270(16) 0.026(8) Uiso 1 1 d . . . O1S O 0.4854(9) -0.3562(17) 0.4695(6) 0.204(6) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02558(10) 0.02541(11) 0.01666(10) -0.00170(7) 0.00332(7) -0.00030(8) Cl1 0.0338(3) 0.0303(3) 0.0240(3) -0.0066(2) 0.0073(2) -0.0005(3) S1 0.0282(3) 0.0320(3) 0.0203(3) 0.0021(3) 0.0039(2) 0.0011(3) P1 0.0356(4) 0.0398(4) 0.0360(4) 0.0015(3) 0.0034(3) 0.0012(3) F1 0.0765(16) 0.151(3) 0.0529(14) -0.0385(16) -0.0022(12) 0.0016(17) O1 0.0416(11) 0.0353(11) 0.0407(12) -0.0064(9) -0.0062(9) 0.0013(9) N1 0.0278(11) 0.0318(12) 0.0207(11) -0.0005(9) 0.0036(9) -0.0008(9) C1 0.0301(13) 0.0341(15) 0.0311(14) 0.0064(12) 0.0044(11) -0.0037(11) Cl2 0.0352(3) 0.0369(4) 0.0292(3) -0.0061(3) 0.0083(3) 0.0051(3) S2 0.0282(3) 0.0266(3) 0.0221(3) -0.0014(2) 0.0017(2) -0.0007(2) F2 0.129(2) 0.095(2) 0.121(2) 0.0744(18) 0.082(2) 0.0728(18) O2 0.0268(9) 0.0685(15) 0.0342(11) -0.0089(11) 0.0013(8) -0.0004(10) N2 0.0330(11) 0.0282(12) 0.0196(11) -0.0015(9) 0.0028(9) -0.0011(10) C2 0.0335(13) 0.0295(14) 0.0293(14) 0.0020(11) 0.0013(11) -0.0032(11) F3 0.092(2) 0.172(3) 0.0784(19) -0.067(2) 0.0191(16) -0.043(2) C3 0.0335(13) 0.0384(16) 0.0238(13) -0.0011(11) -0.0026(11) -0.0070(12) F4 0.0738(16) 0.126(2) 0.102(2) 0.0374(18) 0.0065(15) 0.0560(17) C4 0.0355(14) 0.0432(17) 0.0252(14) 0.0024(12) -0.0067(11) -0.0027(13) F5 0.0655(13) 0.0521(13) 0.0833(16) 0.0098(11) 0.0261(12) -0.0068(10) C5 0.0413(15) 0.0384(16) 0.0191(13) 0.0021(11) -0.0012(11) -0.0041(12) F6 0.0906(19) 0.0770(18) 0.151(3) -0.0093(19) 0.080(2) -0.0206(15) C6 0.0383(14) 0.0343(15) 0.0246(13) 0.0015(11) 0.0048(11) -0.0051(12) C7 0.0351(13) 0.0268(14) 0.0250(13) 0.0013(11) 0.0018(11) -0.0034(11) C8 0.0488(18) 0.0359(17) 0.056(2) 0.0168(15) -0.0002(15) -0.0046(14) C9 0.0346(15) 0.058(2) 0.0311(15) 0.0075(14) 0.0067(12) -0.0034(14) C10 0.0415(16) 0.0368(16) 0.0395(17) 0.0029(13) 0.0035(13) -0.0089(13) C11 0.0480(17) 0.0303(15) 0.0348(16) -0.0041(12) -0.0013(13) 0.0005(13) C12 0.0367(14) 0.0482(18) 0.0196(13) 0.0029(12) 0.0057(11) 0.0012(13) C13 0.0370(14) 0.0360(15) 0.0171(12) 0.0037(11) 0.0044(10) 0.0017(12) C14 0.0403(15) 0.0331(15) 0.0252(14) 0.0046(11) 0.0094(11) 0.0090(12) C15 0.0429(15) 0.0263(14) 0.0242(13) 0.0011(11) 0.0101(11) 0.0020(12) C16 0.0396(14) 0.0321(15) 0.0220(13) -0.0003(11) 0.0027(11) 0.0015(12) C17 0.0428(15) 0.0319(15) 0.0355(16) -0.0027(12) -0.0051(12) 0.0100(13) C18 0.0433(15) 0.0315(15) 0.0311(15) -0.0025(12) -0.0019(12) 0.0029(12) C19 0.0399(17) 0.051(2) 0.062(2) -0.0112(18) -0.0091(15) 0.0045(15) C20 0.0304(13) 0.0312(15) 0.0448(17) 0.0004(13) 0.0061(12) 0.0021(12) C21 0.0297(13) 0.0296(14) 0.0312(14) 0.0047(11) 0.0031(11) -0.0003(11) C22 0.0356(14) 0.0392(16) 0.0326(15) -0.0104(12) 0.0080(12) 0.0031(12) C23 0.0300(13) 0.0370(16) 0.0335(15) -0.0032(12) 0.0112(11) 0.0011(12) C24 0.0300(13) 0.0400(16) 0.0278(14) 0.0027(12) 0.0032(11) 0.0016(12) C25 0.0352(15) 0.112(3) 0.0190(14) -0.0067(17) 0.0046(12) -0.0021(18) C26 0.0301(14) 0.090(3) 0.0252(15) 0.0097(16) 0.0074(12) -0.0052(16) C27 0.0278(13) 0.0518(19) 0.0433(17) 0.0051(15) 0.0035(12) -0.0002(13) C1S 0.136(5) 0.058(3) 0.103(5) 0.020(3) 0.025(4) 0.023(3) O1S 0.261(15) 0.278(17) 0.076(7) 0.011(10) 0.033(8) 0.035(15) _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 N2 2.099(2) . ? Rh1 N1 2.101(2) . ? Rh1 S1 2.3259(7) . ? Rh1 Cl2 2.3358(7) . ? Rh1 S2 2.3427(7) . ? Rh1 Cl1 2.3461(6) . ? S1 C12 1.828(3) . ? S1 C1 1.871(3) . ? P1 F2 1.551(2) . ? P1 F6 1.564(2) . ? P1 F1 1.571(2) . ? P1 F3 1.574(3) . ? P1 F4 1.580(2) . ? P1 F5 1.601(2) . ? O1 C16 1.376(3) . ? O1 C19 1.431(4) . ? N1 C2 1.480(3) . ? N1 C3 1.495(3) . ? C1 C2 1.524(4) . ? C1 C8 1.524(4) . ? C1 C9 1.530(4) . ? S2 C20 1.828(3) . ? S2 C7 1.866(3) . ? O2 C24 1.365(3) . ? O2 C27 1.425(3) . ? N2 C5 1.491(3) . ? N2 C6 1.491(3) . ? C3 C4 1.508(4) . ? C4 C5 1.517(4) . ? C6 C7 1.517(4) . ? C7 C10 1.529(4) . ? C7 C11 1.532(4) . ? C12 C13 1.506(4) . ? C13 C18 1.390(4) . ? C13 C14 1.393(4) . ? C14 C15 1.384(4) . ? C15 C16 1.388(4) . ? C16 C17 1.384(4) . ? C17 C18 1.388(4) . ? C20 C21 1.513(4) . ? C21 C26 1.382(4) . ? C21 C22 1.383(4) . ? C22 C23 1.394(4) . ? C23 C24 1.376(4) . ? C24 C25 1.396(4) . ? C25 C26 1.371(4) . ? C1S O1S 1.123(17) . ? C1S C1S 1.436(12) 3_646 ? 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 N2 Rh1 N1 94.83(9) . . ? N2 Rh1 S1 176.93(7) . . ? N1 Rh1 S1 84.75(6) . . ? N2 Rh1 Cl2 88.24(7) . . ? N1 Rh1 Cl2 87.72(7) . . ? S1 Rh1 Cl2 94.78(2) . . ? N2 Rh1 S2 85.35(6) . . ? N1 Rh1 S2 176.27(7) . . ? S1 Rh1 S2 95.27(2) . . ? Cl2 Rh1 S2 88.56(2) . . ? N2 Rh1 Cl1 89.81(7) . . ? N1 Rh1 Cl1 89.24(7) . . ? S1 Rh1 Cl1 87.14(2) . . ? Cl2 Rh1 Cl1 176.24(2) . . ? S2 Rh1 Cl1 94.48(2) . . ? C12 S1 C1 102.00(13) . . ? C12 S1 Rh1 114.03(10) . . ? C1 S1 Rh1 100.80(9) . . ? F2 P1 F6 92.09(17) . . ? F2 P1 F1 92.25(19) . . ? F6 P1 F1 90.60(17) . . ? F2 P1 F3 90.3(2) . . ? F6 P1 F3 92.74(17) . . ? F1 P1 F3 175.7(2) . . ? F2 P1 F4 178.6(2) . . ? F6 P1 F4 89.00(17) . . ? F1 P1 F4 86.85(17) . . ? F3 P1 F4 90.51(19) . . ? F2 P1 F5 88.83(14) . . ? F6 P1 F5 178.72(17) . . ? F1 P1 F5 90.24(15) . . ? F3 P1 F5 86.38(15) . . ? F4 P1 F5 90.08(14) . . ? C16 O1 C19 117.1(2) . . ? C2 N1 C3 109.1(2) . . ? C2 N1 Rh1 111.16(16) . . ? C3 N1 Rh1 117.83(16) . . ? C2 C1 C8 109.7(3) . . ? C2 C1 C9 111.7(2) . . ? C8 C1 C9 111.1(3) . . ? C2 C1 S1 103.99(18) . . ? C8 C1 S1 107.2(2) . . ? C9 C1 S1 112.8(2) . . ? C20 S2 C7 105.17(13) . . ? C20 S2 Rh1 107.78(10) . . ? C7 S2 Rh1 99.67(8) . . ? C24 O2 C27 117.8(2) . . ? C5 N2 C6 109.5(2) . . ? C5 N2 Rh1 116.69(17) . . ? C6 N2 Rh1 110.74(17) . . ? N1 C2 C1 113.1(2) . . ? N1 C3 C4 113.3(2) . . ? C3 C4 C5 114.2(2) . . ? N2 C5 C4 111.7(2) . . ? N2 C6 C7 112.4(2) . . ? C6 C7 C10 109.0(2) . . ? C6 C7 C11 112.8(2) . . ? C10 C7 C11 109.7(2) . . ? C6 C7 S2 107.69(18) . . ? C10 C7 S2 112.23(19) . . ? C11 C7 S2 105.45(19) . . ? C13 C12 S1 112.54(18) . . ? C18 C13 C14 118.3(3) . . ? C18 C13 C12 121.5(3) . . ? C14 C13 C12 119.8(3) . . ? C15 C14 C13 121.1(3) . . ? C14 C15 C16 119.7(3) . . ? O1 C16 C17 124.6(3) . . ? O1 C16 C15 115.3(2) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 C18 119.6(3) . . ? C17 C18 C13 121.1(3) . . ? C21 C20 S2 113.3(2) . . ? C26 C21 C22 117.9(3) . . ? C26 C21 C20 121.4(2) . . ? C22 C21 C20 120.6(3) . . ? C21 C22 C23 121.7(3) . . ? C24 C23 C22 119.5(2) . . ? O2 C24 C23 125.3(2) . . ? O2 C24 C25 115.5(3) . . ? C23 C24 C25 119.2(3) . . ? C26 C25 C24 120.4(3) . . ? C25 C26 C21 121.4(3) . . ? O1S C1S C1S 122.2(11) . 3_646 ? 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 N2 Rh1 S1 C12 162.9(12) . . . . ? N1 Rh1 S1 C12 -114.88(12) . . . . ? Cl2 Rh1 S1 C12 -27.62(10) . . . . ? S2 Rh1 S1 C12 61.38(10) . . . . ? Cl1 Rh1 S1 C12 155.62(10) . . . . ? N2 Rh1 S1 C1 -88.7(12) . . . . ? N1 Rh1 S1 C1 -6.41(11) . . . . ? Cl2 Rh1 S1 C1 80.85(9) . . . . ? S2 Rh1 S1 C1 169.85(9) . . . . ? Cl1 Rh1 S1 C1 -95.91(9) . . . . ? N2 Rh1 N1 C2 155.13(17) . . . . ? S1 Rh1 N1 C2 -21.81(16) . . . . ? Cl2 Rh1 N1 C2 -116.82(17) . . . . ? S2 Rh1 N1 C2 -112.3(10) . . . . ? Cl1 Rh1 N1 C2 65.39(17) . . . . ? N2 Rh1 N1 C3 28.2(2) . . . . ? S1 Rh1 N1 C3 -148.8(2) . . . . ? Cl2 Rh1 N1 C3 116.20(19) . . . . ? S2 Rh1 N1 C3 120.8(9) . . . . ? Cl1 Rh1 N1 C3 -61.59(19) . . . . ? C12 S1 C1 C2 149.95(19) . . . . ? Rh1 S1 C1 C2 32.28(19) . . . . ? C12 S1 C1 C8 -93.9(2) . . . . ? Rh1 S1 C1 C8 148.5(2) . . . . ? C12 S1 C1 C9 28.8(2) . . . . ? Rh1 S1 C1 C9 -88.9(2) . . . . ? N2 Rh1 S2 C20 -108.92(13) . . . . ? N1 Rh1 S2 C20 158.2(10) . . . . ? S1 Rh1 S2 C20 68.06(11) . . . . ? Cl2 Rh1 S2 C20 162.73(11) . . . . ? Cl1 Rh1 S2 C20 -19.47(11) . . . . ? N2 Rh1 S2 C7 0.56(11) . . . . ? N1 Rh1 S2 C7 -92.4(10) . . . . ? S1 Rh1 S2 C7 177.53(9) . . . . ? Cl2 Rh1 S2 C7 -87.80(9) . . . . ? Cl1 Rh1 S2 C7 90.00(9) . . . . ? N1 Rh1 N2 C5 -31.2(2) . . . . ? S1 Rh1 N2 C5 50.8(13) . . . . ? Cl2 Rh1 N2 C5 -118.76(19) . . . . ? S2 Rh1 N2 C5 152.54(19) . . . . ? Cl1 Rh1 N2 C5 58.03(19) . . . . ? N1 Rh1 N2 C6 -157.37(18) . . . . ? S1 Rh1 N2 C6 -75.4(12) . . . . ? Cl2 Rh1 N2 C6 115.07(17) . . . . ? S2 Rh1 N2 C6 26.37(17) . . . . ? Cl1 Rh1 N2 C6 -68.14(17) . . . . ? C3 N1 C2 C1 -175.4(2) . . . . ? Rh1 N1 C2 C1 53.0(3) . . . . ? C8 C1 C2 N1 -170.5(2) . . . . ? C9 C1 C2 N1 65.8(3) . . . . ? S1 C1 C2 N1 -56.1(3) . . . . ? C2 N1 C3 C4 -177.0(2) . . . . ? Rh1 N1 C3 C4 -49.1(3) . . . . ? N1 C3 C4 C5 72.5(3) . . . . ? C6 N2 C5 C4 -178.2(2) . . . . ? Rh1 N2 C5 C4 55.0(3) . . . . ? C3 C4 C5 N2 -75.9(3) . . . . ? C5 N2 C6 C7 176.6(2) . . . . ? Rh1 N2 C6 C7 -53.4(3) . . . . ? N2 C6 C7 C10 174.4(2) . . . . ? N2 C6 C7 C11 -63.5(3) . . . . ? N2 C6 C7 S2 52.4(3) . . . . ? C20 S2 C7 C6 85.1(2) . . . . ? Rh1 S2 C7 C6 -26.45(19) . . . . ? C20 S2 C7 C10 -34.9(2) . . . . ? Rh1 S2 C7 C10 -146.47(19) . . . . ? C20 S2 C7 C11 -154.28(19) . . . . ? Rh1 S2 C7 C11 94.18(17) . . . . ? C1 S1 C12 C13 161.4(2) . . . . ? Rh1 S1 C12 C13 -90.9(2) . . . . ? S1 C12 C13 C18 -63.5(3) . . . . ? S1 C12 C13 C14 123.1(2) . . . . ? C18 C13 C14 C15 -1.4(4) . . . . ? C12 C13 C14 C15 172.2(2) . . . . ? C13 C14 C15 C16 1.3(4) . . . . ? C19 O1 C16 C17 2.9(4) . . . . ? C19 O1 C16 C15 -176.6(3) . . . . ? C14 C15 C16 O1 179.5(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? O1 C16 C17 C18 179.3(3) . . . . ? C15 C16 C17 C18 -1.4(4) . . . . ? C16 C17 C18 C13 1.3(5) . . . . ? C14 C13 C18 C17 0.1(4) . . . . ? C12 C13 C18 C17 -173.4(3) . . . . ? C7 S2 C20 C21 82.9(2) . . . . ? Rh1 S2 C20 C21 -171.42(18) . . . . ? S2 C20 C21 C26 45.1(4) . . . . ? S2 C20 C21 C22 -136.5(3) . . . . ? C26 C21 C22 C23 0.8(5) . . . . ? C20 C21 C22 C23 -177.6(3) . . . . ? C21 C22 C23 C24 -0.9(5) . . . . ? C27 O2 C24 C23 -3.5(4) . . . . ? C27 O2 C24 C25 177.6(3) . . . . ? C22 C23 C24 O2 -178.3(3) . . . . ? C22 C23 C24 C25 0.6(5) . . . . ? O2 C24 C25 C26 178.7(3) . . . . ? C23 C24 C25 C26 -0.2(6) . . . . ? C24 C25 C26 C21 0.2(6) . . . . ? C22 C21 C26 C25 -0.5(5) . . . . ? C20 C21 C26 C25 177.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.985 _refine_diff_density_min -0.639 _refine_diff_density_rms 0.077 data_323N2S2-Rh _database_code_depnum_ccdc_archive 'CCDC 781962' #TrackingRef '323N2S2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H24 Cl2 F6 N2 P Rh S2' _chemical_formula_weight 555.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.4677(12) _cell_length_b 9.5972(9) _cell_length_c 16.3961(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.783(2) _cell_angle_gamma 90.00 _cell_volume 1905.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11170 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 27.1 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.935 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 1.532 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.70 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of G\"ottingen, Germany). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 12833 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.11 _reflns_number_total 4168 _reflns_number_gt 3984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Burnett & Johnson, 1996)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.1375P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4168 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0507 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _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 Rh1 Rh 0.235143(10) 0.208113(13) 0.266796(8) 0.01965(5) Uani 1 1 d . . . Cl1 Cl 0.11094(4) 0.17688(5) 0.35281(3) 0.02800(9) Uani 1 1 d . . . S1 S 0.26461(4) 0.43306(5) 0.32165(3) 0.02775(10) Uani 1 1 d . . . P1 P 0.71538(4) 0.21107(5) 0.43402(3) 0.02816(11) Uani 1 1 d . . . F1 F 0.79322(12) 0.34565(13) 0.45175(9) 0.0478(3) Uani 1 1 d . . . N1 N 0.37376(12) 0.12991(16) 0.35468(9) 0.0266(3) Uani 1 1 d . . . H1 H 0.4349 0.1737 0.3429 0.032 Uiso 1 1 calc R . . C1 C 0.30461(17) 0.4087(2) 0.43470(12) 0.0344(4) Uani 1 1 d . . . H1A H 0.3244 0.5008 0.4612 0.041 Uiso 1 1 calc R . . H1B H 0.2394 0.3745 0.4533 0.041 Uiso 1 1 calc R . . Cl2 Cl 0.35760(4) 0.22709(5) 0.17950(3) 0.03089(10) Uani 1 1 d . . . S2 S 0.08256(4) 0.29837(5) 0.17019(3) 0.02625(10) Uani 1 1 d . . . F2 F 0.66041(11) 0.25462(14) 0.50935(8) 0.0433(3) Uani 1 1 d . . . N2 N 0.21031(12) -0.00017(15) 0.22863(9) 0.0242(3) Uani 1 1 d . . . H2 H 0.2468 -0.0133 0.1859 0.029 Uiso 1 1 calc R . . C2 C 0.39975(17) 0.3095(2) 0.46768(12) 0.0333(4) Uani 1 1 d . . . H2A H 0.4639 0.3413 0.4469 0.040 Uiso 1 1 calc R . . H2B H 0.4204 0.3170 0.5297 0.040 Uiso 1 1 calc R . . F3 F 0.62431(13) 0.30050(16) 0.36946(9) 0.0567(4) Uani 1 1 d . . . C3 C 0.37996(16) 0.1575(2) 0.44492(11) 0.0315(4) Uani 1 1 d . . . H3A H 0.4405 0.1012 0.4796 0.038 Uiso 1 1 calc R . . H3B H 0.3100 0.1275 0.4582 0.038 Uiso 1 1 calc R . . F4 F 0.63557(12) 0.07870(15) 0.41526(8) 0.0506(3) Uani 1 1 d . . . C4 C 0.38361(16) -0.0211(2) 0.33429(13) 0.0322(4) Uani 1 1 d . . . H4A H 0.4231 -0.0716 0.3853 0.039 Uiso 1 1 calc R . . H4B H 0.4269 -0.0306 0.2912 0.039 Uiso 1 1 calc R . . F5 F 0.76951(11) 0.16758(14) 0.35874(8) 0.0424(3) Uani 1 1 d . . . C5 C 0.27091(16) -0.08363(19) 0.30209(12) 0.0307(4) Uani 1 1 d . . . H5A H 0.2778 -0.1815 0.2849 0.037 Uiso 1 1 calc R . . H5B H 0.2298 -0.0827 0.3469 0.037 Uiso 1 1 calc R . . F6 F 0.80544(11) 0.12294(14) 0.49840(8) 0.0452(3) Uani 1 1 d . . . C6 C 0.09660(15) -0.05658(19) 0.19766(12) 0.0294(4) Uani 1 1 d . . . H6A H 0.0580 -0.0526 0.2439 0.035 Uiso 1 1 calc R . . H6B H 0.1018 -0.1557 0.1824 0.035 Uiso 1 1 calc R . . C7 C 0.02812(16) 0.0207(2) 0.12235(12) 0.0327(4) Uani 1 1 d . . . H7A H -0.0344 -0.0394 0.0944 0.039 Uiso 1 1 calc R . . H7B H 0.0743 0.0372 0.0818 0.039 Uiso 1 1 calc R . . C8 C -0.01768(15) 0.1598(2) 0.14306(13) 0.0331(4) Uani 1 1 d . . . H8A H -0.0529 0.1458 0.1905 0.040 Uiso 1 1 calc R . . H8B H -0.0760 0.1899 0.0940 0.040 Uiso 1 1 calc R . . C9 C 0.38957(16) 0.5071(2) 0.30330(13) 0.0338(4) Uani 1 1 d . . . H9A H 0.4071 0.5935 0.3356 0.051 Uiso 1 1 calc R . . H9B H 0.3792 0.5275 0.2434 0.051 Uiso 1 1 calc R . . H9C H 0.4504 0.4407 0.3209 0.051 Uiso 1 1 calc R . . C10 C 0.11362(19) 0.3275(3) 0.06972(12) 0.0402(5) Uani 1 1 d . . . H10A H 0.1441 0.2421 0.0514 0.060 Uiso 1 1 calc R . . H10B H 0.1678 0.4029 0.0746 0.060 Uiso 1 1 calc R . . H10C H 0.0459 0.3533 0.0284 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02155(8) 0.02103(8) 0.01676(7) 0.00062(4) 0.00532(5) 0.00233(5) Cl1 0.0287(2) 0.0350(2) 0.0229(2) 0.00181(17) 0.01124(16) 0.00254(17) S1 0.0273(2) 0.0237(2) 0.0317(2) -0.00384(17) 0.00600(18) 0.00262(17) P1 0.0320(2) 0.0260(2) 0.0254(2) 0.00046(17) 0.00463(19) -0.00076(18) F1 0.0638(9) 0.0334(6) 0.0504(8) -0.0104(6) 0.0222(7) -0.0178(6) N1 0.0266(7) 0.0288(8) 0.0234(7) -0.0005(6) 0.0035(6) 0.0043(6) C1 0.0377(10) 0.0389(11) 0.0285(9) -0.0117(8) 0.0113(8) -0.0019(8) Cl2 0.0321(2) 0.0359(2) 0.0289(2) 0.00072(18) 0.01559(18) 0.00050(18) S2 0.0277(2) 0.0280(2) 0.0221(2) 0.00359(16) 0.00396(17) 0.00463(16) F2 0.0523(8) 0.0421(7) 0.0399(7) -0.0008(6) 0.0197(6) 0.0037(6) N2 0.0269(7) 0.0233(7) 0.0226(7) 0.0000(6) 0.0063(6) 0.0008(6) C2 0.0371(10) 0.0428(11) 0.0189(9) -0.0041(8) 0.0048(7) -0.0030(8) F3 0.0529(8) 0.0684(10) 0.0459(8) 0.0213(7) 0.0062(7) 0.0214(7) C3 0.0338(10) 0.0376(10) 0.0217(9) 0.0033(7) 0.0038(7) 0.0037(8) F4 0.0588(8) 0.0507(8) 0.0420(7) -0.0076(6) 0.0112(6) -0.0261(7) C4 0.0330(10) 0.0293(9) 0.0315(10) -0.0001(8) 0.0019(8) 0.0101(8) F5 0.0494(7) 0.0468(7) 0.0334(6) -0.0098(5) 0.0145(5) -0.0051(6) C5 0.0390(10) 0.0239(9) 0.0278(9) 0.0039(7) 0.0049(8) 0.0046(8) F6 0.0504(7) 0.0434(7) 0.0362(6) 0.0017(5) -0.0004(6) 0.0146(6) C6 0.0312(9) 0.0271(9) 0.0300(9) 0.0002(7) 0.0075(7) -0.0061(7) C7 0.0311(9) 0.0349(10) 0.0292(9) -0.0020(8) 0.0013(8) -0.0067(8) C8 0.0244(9) 0.0410(11) 0.0314(10) 0.0037(8) 0.0018(7) -0.0014(8) C9 0.0323(10) 0.0293(10) 0.0381(11) 0.0044(8) 0.0049(8) -0.0037(8) C10 0.0474(12) 0.0478(12) 0.0244(9) 0.0136(9) 0.0065(9) -0.0026(10) _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 N2 2.0955(15) . ? Rh1 N1 2.1071(15) . ? Rh1 S2 2.3329(5) . ? Rh1 S1 2.3339(5) . ? Rh1 Cl2 2.3353(5) . ? Rh1 Cl1 2.3489(5) . ? S1 C9 1.802(2) . ? S1 C1 1.816(2) . ? P1 F6 1.5892(13) . ? P1 F5 1.5968(13) . ? P1 F4 1.5978(13) . ? P1 F1 1.6000(13) . ? P1 F2 1.6042(14) . ? P1 F3 1.6043(14) . ? N1 C3 1.487(2) . ? N1 C4 1.499(2) . ? N1 H1 0.9300 . ? C1 C2 1.517(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? S2 C10 1.801(2) . ? S2 C8 1.806(2) . ? N2 C6 1.489(2) . ? N2 C5 1.493(2) . ? N2 H2 0.9300 . ? C2 C3 1.512(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.503(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.517(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.522(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 N2 Rh1 N1 84.44(6) . . ? N2 Rh1 S2 96.48(4) . . ? N1 Rh1 S2 179.07(4) . . ? N2 Rh1 S1 174.86(4) . . ? N1 Rh1 S1 92.17(4) . . ? S2 Rh1 S1 86.918(17) . . ? N2 Rh1 Cl2 87.88(4) . . ? N1 Rh1 Cl2 84.12(4) . . ? S2 Rh1 Cl2 95.815(19) . . ? S1 Rh1 Cl2 95.633(17) . . ? N2 Rh1 Cl1 89.19(4) . . ? N1 Rh1 Cl1 95.43(5) . . ? S2 Rh1 Cl1 84.689(18) . . ? S1 Rh1 Cl1 87.275(17) . . ? Cl2 Rh1 Cl1 177.069(17) . . ? C9 S1 C1 100.55(10) . . ? C9 S1 Rh1 111.32(7) . . ? C1 S1 Rh1 104.70(7) . . ? F6 P1 F5 90.71(7) . . ? F6 P1 F4 90.79(8) . . ? F5 P1 F4 90.11(7) . . ? F6 P1 F1 90.40(8) . . ? F5 P1 F1 90.10(7) . . ? F4 P1 F1 178.79(9) . . ? F6 P1 F2 89.49(7) . . ? F5 P1 F2 179.72(8) . . ? F4 P1 F2 89.69(8) . . ? F1 P1 F2 90.09(7) . . ? F6 P1 F3 179.68(9) . . ? F5 P1 F3 89.59(8) . . ? F4 P1 F3 89.31(8) . . ? F1 P1 F3 89.50(8) . . ? F2 P1 F3 90.21(8) . . ? C3 N1 C4 113.97(15) . . ? C3 N1 Rh1 117.19(11) . . ? C4 N1 Rh1 106.82(11) . . ? C3 N1 H1 106.0 . . ? C4 N1 H1 106.0 . . ? Rh1 N1 H1 106.0 . . ? C2 C1 S1 116.49(13) . . ? C2 C1 H1A 108.2 . . ? S1 C1 H1A 108.2 . . ? C2 C1 H1B 108.2 . . ? S1 C1 H1B 108.2 . . ? H1A C1 H1B 107.3 . . ? C10 S2 C8 100.12(10) . . ? C10 S2 Rh1 111.12(8) . . ? C8 S2 Rh1 107.36(7) . . ? C6 N2 C5 109.73(14) . . ? C6 N2 Rh1 120.63(11) . . ? C5 N2 Rh1 105.10(11) . . ? C6 N2 H2 106.9 . . ? C5 N2 H2 106.9 . . ? Rh1 N2 H2 106.9 . . ? C3 C2 C1 116.74(17) . . ? C3 C2 H2A 108.1 . . ? C1 C2 H2A 108.1 . . ? C3 C2 H2B 108.1 . . ? C1 C2 H2B 108.1 . . ? H2A C2 H2B 107.3 . . ? N1 C3 C2 112.58(16) . . ? N1 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N1 C4 C5 110.18(15) . . ? N1 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? N1 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N2 C5 C4 108.67(15) . . ? N2 C5 H5A 110.0 . . ? C4 C5 H5A 110.0 . . ? N2 C5 H5B 110.0 . . ? C4 C5 H5B 110.0 . . ? H5A C5 H5B 108.3 . . ? N2 C6 C7 113.90(15) . . ? N2 C6 H6A 108.8 . . ? C7 C6 H6A 108.8 . . ? N2 C6 H6B 108.8 . . ? C7 C6 H6B 108.8 . . ? H6A C6 H6B 107.7 . . ? C6 C7 C8 114.57(16) . . ? C6 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 S2 115.23(13) . . ? C7 C8 H8A 108.5 . . ? S2 C8 H8A 108.5 . . ? C7 C8 H8B 108.5 . . ? S2 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? S1 C9 H9A 109.5 . . ? S1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Rh1 S1 C9 115.9(5) . . . . ? N1 Rh1 S1 C9 67.25(8) . . . . ? S2 Rh1 S1 C9 -112.59(7) . . . . ? Cl2 Rh1 S1 C9 -17.05(7) . . . . ? Cl1 Rh1 S1 C9 162.58(7) . . . . ? N2 Rh1 S1 C1 8.1(5) . . . . ? N1 Rh1 S1 C1 -40.55(8) . . . . ? S2 Rh1 S1 C1 139.61(7) . . . . ? Cl2 Rh1 S1 C1 -124.85(7) . . . . ? Cl1 Rh1 S1 C1 54.78(7) . . . . ? N2 Rh1 N1 C3 -122.83(14) . . . . ? S2 Rh1 N1 C3 63(3) . . . . ? S1 Rh1 N1 C3 53.29(13) . . . . ? Cl2 Rh1 N1 C3 148.74(13) . . . . ? Cl1 Rh1 N1 C3 -34.17(13) . . . . ? N2 Rh1 N1 C4 6.40(12) . . . . ? S2 Rh1 N1 C4 -168(3) . . . . ? S1 Rh1 N1 C4 -177.48(12) . . . . ? Cl2 Rh1 N1 C4 -82.04(12) . . . . ? Cl1 Rh1 N1 C4 95.06(12) . . . . ? C9 S1 C1 C2 -62.33(17) . . . . ? Rh1 S1 C1 C2 53.21(16) . . . . ? N2 Rh1 S2 C10 -82.74(9) . . . . ? N1 Rh1 S2 C10 91(3) . . . . ? S1 Rh1 S2 C10 101.13(9) . . . . ? Cl2 Rh1 S2 C10 5.78(9) . . . . ? Cl1 Rh1 S2 C10 -171.32(9) . . . . ? N2 Rh1 S2 C8 25.81(8) . . . . ? N1 Rh1 S2 C8 -160(3) . . . . ? S1 Rh1 S2 C8 -150.31(7) . . . . ? Cl2 Rh1 S2 C8 114.33(7) . . . . ? Cl1 Rh1 S2 C8 -62.77(7) . . . . ? N1 Rh1 N2 C6 146.25(13) . . . . ? S2 Rh1 N2 C6 -33.85(13) . . . . ? S1 Rh1 N2 C6 97.3(5) . . . . ? Cl2 Rh1 N2 C6 -129.46(12) . . . . ? Cl1 Rh1 N2 C6 50.71(12) . . . . ? N1 Rh1 N2 C5 21.76(12) . . . . ? S2 Rh1 N2 C5 -158.33(11) . . . . ? S1 Rh1 N2 C5 -27.1(5) . . . . ? Cl2 Rh1 N2 C5 106.05(11) . . . . ? Cl1 Rh1 N2 C5 -73.77(11) . . . . ? S1 C1 C2 C3 -66.6(2) . . . . ? C4 N1 C3 C2 165.02(16) . . . . ? Rh1 N1 C3 C2 -69.22(18) . . . . ? C1 C2 C3 N1 71.1(2) . . . . ? C3 N1 C4 C5 96.90(18) . . . . ? Rh1 N1 C4 C5 -34.16(18) . . . . ? C6 N2 C5 C4 -177.72(15) . . . . ? Rh1 N2 C5 C4 -46.61(16) . . . . ? N1 C4 C5 N2 55.7(2) . . . . ? C5 N2 C6 C7 -179.60(16) . . . . ? Rh1 N2 C6 C7 58.12(19) . . . . ? N2 C6 C7 C8 -77.1(2) . . . . ? C6 C7 C8 S2 73.0(2) . . . . ? C10 S2 C8 C7 69.17(16) . . . . ? Rh1 S2 C8 C7 -46.89(16) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.745 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.068