# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Connelly, Neil' _publ_contact_author_name 'Connelly, Neil' _publ_contact_author_email neil.connelly@bristol.ac.uk _publ_section_title ; The oxidative conversion of the N,S-bridged complexes [{RhLL'(-X)}2] to [(RhLL')3(-X)2]+ (X = mt or taz): a comparison with the oxidation of N,N-bridged analogues+ ; # Attachment '- all.cif' data_ml27sad _database_code_depnum_ccdc_archive 'CCDC 826255' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H34 N4 Rh2 S2' _chemical_formula_sum 'C24 H34 N4 Rh2 S2' _chemical_formula_weight 648.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -P2ybc 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 11.1408(17) _cell_length_b 17.344(2) _cell_length_c 12.795(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.784(11) _cell_angle_gamma 90.00 _cell_volume 2449.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10821 _cell_measurement_theta_min 2.188 _cell_measurement_theta_max 27.484 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.530596 _exptl_absorpt_correction_T_max 0.670000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker 2003)' _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15353 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5616 _reflns_number_gt 5122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.41A (Bruker, 2002)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 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. ; _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^)+(0.0294P)^2^+1.2896P] 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_number_reflns 5616 _refine_ls_number_parameters 328 _refine_ls_number_restraints 217 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0223 _refine_ls_wR_factor_ref 0.0567 _refine_ls_wR_factor_gt 0.0554 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.054 _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 0.170623(14) 0.184864(9) 0.176431(11) 0.01587(5) Uani 1 1 d . C . Rh2 Rh 0.495709(14) 0.105111(9) 0.220797(12) 0.01748(5) Uani 1 1 d . . . S1 S 0.21105(5) 0.08933(3) 0.05408(4) 0.02234(11) Uani 1 1 d . . . S2 S 0.41302(5) 0.12635(3) 0.37866(4) 0.02163(11) Uani 1 1 d . C . N1 N 0.38266(15) 0.00954(10) 0.18586(13) 0.0196(3) Uani 1 1 d . C . N2 N 0.22098(15) -0.05949(10) 0.12981(14) 0.0204(3) Uani 1 1 d . . . N3 N 0.17463(15) 0.10323(9) 0.29761(13) 0.0181(3) Uani 1 1 d . . . N4 N 0.24100(16) 0.02300(10) 0.42586(13) 0.0205(3) Uani 1 1 d . . . C1 C 0.27430(18) 0.01130(11) 0.12680(15) 0.0179(4) Uani 1 1 d . C . C2 C 0.39809(19) -0.06377(12) 0.22735(17) 0.0226(4) Uani 1 1 d . . . H2 H 0.4672 -0.0814 0.2727 0.027 Uiso 1 1 calc R C . C3 C 0.2988(2) -0.10670(12) 0.19307(17) 0.0235(4) Uani 1 1 d . C . H3 H 0.2856 -0.1592 0.2096 0.028 Uiso 1 1 calc R . . C4 C 0.0994(2) -0.07963(14) 0.08138(19) 0.0284(5) Uani 1 1 d . C . H4A H 0.0400 -0.0500 0.1147 0.043 Uiso 1 1 calc R . . H4B H 0.0857 -0.1349 0.0909 0.043 Uiso 1 1 calc R . . H4C H 0.0904 -0.0676 0.0059 0.043 Uiso 1 1 calc R . . C5 C 0.27185(18) 0.08251(11) 0.36501(15) 0.0176(4) Uani 1 1 d . C . C6 C 0.08070(19) 0.05584(12) 0.31724(17) 0.0227(4) Uani 1 1 d . C . H6 H 0.0004 0.0577 0.2812 0.027 Uiso 1 1 calc R . . C7 C 0.1213(2) 0.00626(12) 0.39608(17) 0.0249(4) Uani 1 1 d . C . H7 H 0.0754 -0.0326 0.4250 0.030 Uiso 1 1 calc R . . C8 C 0.3237(2) -0.02185(14) 0.50112(18) 0.0305(5) Uani 1 1 d . C . H8A H 0.3479 -0.0688 0.4668 0.046 Uiso 1 1 calc R . . H8B H 0.2829 -0.0358 0.5616 0.046 Uiso 1 1 calc R . . H8C H 0.3958 0.0091 0.5253 0.046 Uiso 1 1 calc R . . C9 C 0.06413(19) 0.26094(12) 0.25575(16) 0.0225(4) Uani 1 1 d . . . H9 H 0.0194 0.2352 0.3088 0.027 Uiso 1 1 calc R C . C10 C 0.1874(2) 0.27414(12) 0.29099(15) 0.0216(4) Uani 1 1 d . C . H10 H 0.2141 0.2557 0.3645 0.026 Uiso 1 1 calc R . . C11 C 0.2599(2) 0.34134(13) 0.25836(17) 0.0271(5) Uani 1 1 d . . . H11A H 0.3467 0.3330 0.2845 0.033 Uiso 1 1 calc R C . H11B H 0.2339 0.3890 0.2914 0.033 Uiso 1 1 calc R . . C12 C 0.2444(2) 0.35206(13) 0.13778(17) 0.0286(5) Uani 1 1 d . C . H12A H 0.1789 0.3898 0.1171 0.034 Uiso 1 1 calc R . . H12B H 0.3203 0.3735 0.1174 0.034 Uiso 1 1 calc R . . C13 C 0.2143(2) 0.27716(12) 0.07800(15) 0.0225(4) Uani 1 1 d . . . H13 H 0.2744 0.2628 0.0300 0.027 Uiso 1 1 calc R C . C14 C 0.0969(2) 0.25114(12) 0.04347(15) 0.0218(4) Uani 1 1 d . C . H14 H 0.0887 0.2223 -0.0248 0.026 Uiso 1 1 calc R . . C15 C -0.0184(2) 0.29037(14) 0.06536(17) 0.0282(5) Uani 1 1 d . . . H15A H -0.0873 0.2546 0.0476 0.034 Uiso 1 1 calc R C . H15B H -0.0331 0.3362 0.0193 0.034 Uiso 1 1 calc R . . C16 C -0.0132(2) 0.31564(13) 0.18129(17) 0.0281(5) Uani 1 1 d . C . H16A H 0.0209 0.3683 0.1896 0.034 Uiso 1 1 calc R . . H16B H -0.0964 0.3171 0.2004 0.034 Uiso 1 1 calc R . . C17 C 0.64724(19) 0.17348(12) 0.28392(17) 0.0233(4) Uani 1 1 d U C . H17A H 0.6520 0.1842 0.3612 0.028 Uiso 1 1 calc R A 1 C18 C 0.5632(2) 0.21946(12) 0.21991(17) 0.0247(4) Uani 1 1 d U C . H18A H 0.5189 0.2569 0.2602 0.030 Uiso 1 1 calc R B 1 C19A C 0.5769(3) 0.24594(15) 0.1094(2) 0.0372(6) Uani 0.331(10) 1 d PU C 1 H19A H 0.6629 0.2598 0.1082 0.045 Uiso 0.331(10) 1 calc PR C 1 H19B H 0.5286 0.2936 0.0947 0.045 Uiso 0.331(10) 1 calc PR C 1 C20A C 0.5385(11) 0.1872(5) 0.0162(7) 0.0261(19) Uani 0.331(10) 1 d PU C 1 H20A H 0.4604 0.2040 -0.0236 0.031 Uiso 0.331(10) 1 calc PR C 1 H20B H 0.6001 0.1880 -0.0327 0.031 Uiso 0.331(10) 1 calc PR C 1 C21A C 0.5254(19) 0.1061(17) 0.055(2) 0.024(3) Uani 0.331(10) 1 d PU C 1 H21A H 0.4675 0.0734 0.0075 0.029 Uiso 0.331(10) 1 calc PR C 1 C22A C 0.616(3) 0.0655(13) 0.116(2) 0.021(3) Uani 0.331(10) 1 d PU C 1 H22A H 0.6128 0.0085 0.1037 0.025 Uiso 0.331(10) 1 calc PR C 1 C23A C 0.7465(7) 0.0984(6) 0.1500(8) 0.030(2) Uani 0.331(10) 1 d PU C 1 H23A H 0.8041 0.0546 0.1579 0.035 Uiso 0.331(10) 1 calc PR C 1 H23B H 0.7681 0.1314 0.0922 0.035 Uiso 0.331(10) 1 calc PR C 1 C24A C 0.7638(2) 0.14448(15) 0.2502(2) 0.0342(5) Uani 0.331(10) 1 d PU C 1 H24A H 0.8165 0.1892 0.2406 0.041 Uiso 0.331(10) 1 calc PR C 1 H24B H 0.8063 0.1121 0.3073 0.041 Uiso 0.331(10) 1 calc PR C 1 C19B C 0.5769(3) 0.24594(15) 0.1094(2) 0.0372(6) Uani 0.669(10) 1 d PU C 2 H19C H 0.5020 0.2731 0.0791 0.045 Uiso 0.669(10) 1 calc PR C 2 H19D H 0.6445 0.2834 0.1134 0.045 Uiso 0.669(10) 1 calc PR C 2 C20B C 0.6003(6) 0.1831(3) 0.0387(3) 0.0339(11) Uani 0.669(10) 1 d PU C 2 H20C H 0.6886 0.1800 0.0364 0.041 Uiso 0.669(10) 1 calc PR C 2 H20D H 0.5608 0.1956 -0.0334 0.041 Uiso 0.669(10) 1 calc PR C 2 C21B C 0.5553(9) 0.1037(8) 0.0701(11) 0.0245(17) Uani 0.669(10) 1 d PU C 2 H21B H 0.4984 0.0777 0.0138 0.029 Uiso 0.669(10) 1 calc PR C 2 C22B C 0.6265(13) 0.0530(7) 0.1383(10) 0.0233(17) Uani 0.669(10) 1 d PU C 2 H22B H 0.6102 -0.0026 0.1216 0.028 Uiso 0.669(10) 1 calc PR C 2 C23B C 0.7524(3) 0.0685(3) 0.1921(4) 0.0316(11) Uani 0.669(10) 1 d PU C 2 H23C H 0.8089 0.0682 0.1387 0.038 Uiso 0.669(10) 1 calc PR C 2 H23D H 0.7767 0.0263 0.2428 0.038 Uiso 0.669(10) 1 calc PR C 2 C24B C 0.7638(2) 0.14448(15) 0.2502(2) 0.0342(5) Uani 0.669(10) 1 d PU C 2 H24C H 0.8248 0.1389 0.3136 0.041 Uiso 0.669(10) 1 calc PR C 2 H24D H 0.7943 0.1837 0.2041 0.041 Uiso 0.669(10) 1 calc PR C 2 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 0.01733(8) 0.01629(8) 0.01386(8) 0.00187(5) 0.00167(6) 0.00128(5) Rh2 0.01454(8) 0.01760(8) 0.02031(8) -0.00237(6) 0.00244(6) -0.00218(5) S1 0.0268(3) 0.0202(2) 0.0188(2) -0.00100(18) -0.0011(2) 0.00492(19) S2 0.0159(2) 0.0287(3) 0.0200(2) -0.0022(2) 0.00142(18) -0.00334(19) N1 0.0177(8) 0.0170(8) 0.0234(8) -0.0015(7) 0.0005(7) 0.0000(6) N2 0.0170(8) 0.0187(8) 0.0249(8) -0.0026(7) 0.0011(7) -0.0011(6) N3 0.0155(8) 0.0197(8) 0.0188(8) 0.0025(6) 0.0013(6) -0.0006(6) N4 0.0225(9) 0.0192(8) 0.0195(8) 0.0051(7) 0.0020(7) 0.0026(7) C1 0.0181(9) 0.0171(9) 0.0189(9) -0.0026(7) 0.0034(7) 0.0004(7) C2 0.0197(10) 0.0198(10) 0.0275(10) 0.0004(8) 0.0005(8) 0.0031(8) C3 0.0233(11) 0.0176(10) 0.0295(11) 0.0013(8) 0.0032(9) 0.0009(8) C4 0.0207(11) 0.0290(11) 0.0339(12) -0.0010(9) -0.0019(9) -0.0076(9) C5 0.0172(9) 0.0189(9) 0.0170(9) 0.0007(7) 0.0029(7) 0.0013(7) C6 0.0167(10) 0.0254(10) 0.0259(10) 0.0000(8) 0.0023(8) -0.0029(8) C7 0.0271(11) 0.0219(10) 0.0263(10) 0.0021(8) 0.0054(9) -0.0070(8) C8 0.0352(13) 0.0279(11) 0.0270(11) 0.0098(9) -0.0014(9) 0.0089(10) C9 0.0257(11) 0.0242(10) 0.0182(9) 0.0002(8) 0.0055(8) 0.0027(8) C10 0.0280(11) 0.0225(10) 0.0148(9) -0.0020(8) 0.0044(8) 0.0016(8) C11 0.0315(12) 0.0259(11) 0.0235(10) -0.0042(9) 0.0022(9) -0.0048(9) C12 0.0367(13) 0.0230(11) 0.0267(11) 0.0029(9) 0.0063(9) -0.0061(9) C13 0.0310(11) 0.0213(10) 0.0164(9) 0.0050(8) 0.0072(8) -0.0003(8) C14 0.0291(11) 0.0212(10) 0.0148(9) 0.0035(7) 0.0018(8) 0.0045(8) C15 0.0290(12) 0.0297(12) 0.0242(10) 0.0003(9) -0.0026(9) 0.0095(9) C16 0.0286(12) 0.0298(12) 0.0263(11) -0.0006(9) 0.0054(9) 0.0096(9) C17 0.0203(10) 0.0245(10) 0.0245(10) -0.0043(8) 0.0008(8) -0.0074(8) C18 0.0235(11) 0.0191(10) 0.0309(11) -0.0023(8) 0.0019(9) -0.0056(8) C19A 0.0445(15) 0.0317(13) 0.0332(12) 0.0068(10) -0.0032(11) -0.0094(11) C20A 0.026(5) 0.033(4) 0.021(3) 0.002(3) 0.006(3) 0.005(3) C21A 0.031(8) 0.028(4) 0.014(7) -0.002(4) 0.007(6) 0.007(6) C22A 0.023(7) 0.022(7) 0.019(8) -0.002(4) 0.005(5) -0.002(5) C23A 0.016(3) 0.036(5) 0.038(5) 0.004(3) 0.009(3) 0.007(3) C24A 0.0178(11) 0.0425(14) 0.0408(13) -0.0066(11) -0.0017(9) -0.0022(9) C19B 0.0445(15) 0.0317(13) 0.0332(12) 0.0068(10) -0.0032(11) -0.0094(11) C20B 0.038(3) 0.042(2) 0.0228(19) 0.0042(15) 0.007(2) -0.006(2) C21B 0.023(4) 0.031(3) 0.019(4) -0.005(3) 0.002(3) -0.005(3) C22B 0.018(3) 0.028(4) 0.024(5) -0.006(3) 0.004(3) 0.004(2) C23B 0.0198(18) 0.036(3) 0.040(3) -0.006(2) 0.0064(17) 0.0026(16) C24B 0.0178(11) 0.0425(14) 0.0408(13) -0.0066(11) -0.0017(9) -0.0022(9) _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 N3 2.0958(16) . ? Rh1 C9 2.122(2) . ? Rh1 C10 2.123(2) . ? Rh1 C14 2.1241(19) . ? Rh1 C13 2.133(2) . ? Rh1 S1 2.3643(6) . ? Rh1 Rh2 3.8465(6) . ? Rh2 N1 2.0931(17) . ? Rh2 C22B 2.114(15) . ? Rh2 C21B 2.123(16) . ? Rh2 C18 2.121(2) . ? Rh2 C17 2.130(2) . ? Rh2 C22A 2.13(3) . ? Rh2 C21A 2.19(3) . ? Rh2 S2 2.3598(7) . ? S1 C1 1.737(2) . ? S2 C5 1.734(2) . ? N1 C1 1.335(3) . ? N1 C2 1.380(3) . ? N2 C1 1.367(3) . ? N2 C3 1.374(3) . ? N2 C4 1.454(3) . ? N3 C5 1.339(2) . ? N3 C6 1.380(3) . ? N4 C5 1.365(3) . ? N4 C7 1.368(3) . ? N4 C8 1.463(3) . ? C2 C3 1.356(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.356(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.405(3) . ? C9 C16 1.526(3) . ? C9 H9 1.0000 . ? C10 C11 1.509(3) . ? C10 H10 1.0000 . ? C11 C12 1.540(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.522(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.398(3) . ? C13 H13 1.0000 . ? C14 C15 1.513(3) . ? C14 H14 1.0000 . ? C15 C16 1.540(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.406(3) . ? C17 C24A 1.509(3) . ? C17 H17A 1.0000 . ? C18 C19A 1.514(3) . ? C18 H18A 1.0000 . ? C19A C20A 1.583(9) . ? C19A H19A 0.9900 . ? C19A H19B 0.9900 . ? C20A C21A 1.50(3) . ? C20A H20A 0.9900 . ? C20A H20B 0.9900 . ? C21A C22A 1.381(19) . ? C21A H21A 1.0000 . ? C22A C23A 1.57(3) . ? C22A H22A 1.0000 . ? C23A C24A 1.501(9) . ? C23A H23A 0.9900 . ? C23A H23B 0.9900 . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C20B C21B 1.537(15) . ? C20B H20C 0.9900 . ? C20B H20D 0.9900 . ? C21B C22B 1.406(10) . ? C21B H21B 1.0000 . ? C22B C23B 1.501(14) . ? C22B H22B 1.0000 . ? C23B H23C 0.9900 . ? C23B H23D 0.9900 . ? 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 N3 Rh1 C9 91.35(7) . . ? N3 Rh1 C10 89.47(7) . . ? C9 Rh1 C10 38.64(8) . . ? N3 Rh1 C14 157.72(8) . . ? C9 Rh1 C14 82.30(8) . . ? C10 Rh1 C14 98.43(8) . . ? N3 Rh1 C13 163.73(7) . . ? C9 Rh1 C13 90.16(8) . . ? C10 Rh1 C13 81.64(8) . . ? C14 Rh1 C13 38.33(8) . . ? N3 Rh1 S1 91.69(5) . . ? C9 Rh1 S1 157.11(6) . . ? C10 Rh1 S1 164.06(6) . . ? C14 Rh1 S1 86.37(6) . . ? C13 Rh1 S1 93.20(6) . . ? N3 Rh1 Rh2 73.89(5) . . ? C9 Rh1 Rh2 136.81(6) . . ? C10 Rh1 Rh2 99.64(6) . . ? C14 Rh1 Rh2 124.55(6) . . ? C13 Rh1 Rh2 94.09(6) . . ? S1 Rh1 Rh2 65.527(16) . . ? N1 Rh2 C22B 89.5(4) . . ? N1 Rh2 C21B 92.9(3) . . ? C22B Rh2 C21B 38.7(3) . . ? N1 Rh2 C18 160.48(7) . . ? C22B Rh2 C18 97.4(4) . . ? C21B Rh2 C18 81.4(4) . . ? N1 Rh2 C17 160.86(8) . . ? C22B Rh2 C17 82.1(4) . . ? C21B Rh2 C17 91.2(3) . . ? C18 Rh2 C17 38.61(8) . . ? N1 Rh2 C22A 91.2(7) . . ? C22B Rh2 C22A 9.8(6) . . ? C21B Rh2 C22A 29.0(6) . . ? C18 Rh2 C22A 92.6(7) . . ? C17 Rh2 C22A 83.4(8) . . ? N1 Rh2 C21A 88.0(7) . . ? C22B Rh2 C21A 46.8(6) . . ? C21B Rh2 C21A 9.5(6) . . ? C18 Rh2 C21A 83.5(8) . . ? C17 Rh2 C21A 98.4(6) . . ? C22A Rh2 C21A 37.3(6) . . ? N1 Rh2 S2 90.75(5) . . ? C22B Rh2 S2 150.4(2) . . ? C21B Rh2 S2 170.3(4) . . ? C18 Rh2 S2 92.19(6) . . ? C17 Rh2 S2 88.27(6) . . ? C22A Rh2 S2 160.0(5) . . ? C21A Rh2 S2 162.8(5) . . ? N1 Rh2 Rh1 74.09(5) . . ? C22B Rh2 Rh1 141.1(3) . . ? C21B Rh2 Rh1 105.9(2) . . ? C18 Rh2 Rh1 89.43(6) . . ? C17 Rh2 Rh1 122.53(6) . . ? C22A Rh2 Rh1 133.0(6) . . ? C21A Rh2 Rh1 96.7(5) . . ? S2 Rh2 Rh1 66.502(16) . . ? C1 S1 Rh1 106.93(7) . . ? C5 S2 Rh2 107.41(7) . . ? C1 N1 C2 107.15(16) . . ? C1 N1 Rh2 125.07(14) . . ? C2 N1 Rh2 127.42(13) . . ? C1 N2 C3 108.06(17) . . ? C1 N2 C4 125.96(18) . . ? C3 N2 C4 125.82(18) . . ? C5 N3 C6 106.86(16) . . ? C5 N3 Rh1 126.31(13) . . ? C6 N3 Rh1 126.60(13) . . ? C5 N4 C7 108.24(16) . . ? C5 N4 C8 126.35(18) . . ? C7 N4 C8 125.03(19) . . ? N1 C1 N2 109.06(17) . . ? N1 C1 S1 126.25(15) . . ? N2 C1 S1 124.67(15) . . ? C3 C2 N1 109.14(18) . . ? C3 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C2 C3 N2 106.58(18) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N4 109.03(17) . . ? N3 C5 S2 126.20(15) . . ? N4 C5 S2 124.69(15) . . ? C7 C6 N3 109.18(18) . . ? C7 C6 H6 125.4 . . ? N3 C6 H6 125.4 . . ? C6 C7 N4 106.67(18) . . ? C6 C7 H7 126.7 . . ? N4 C7 H7 126.7 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C16 122.9(2) . . ? C10 C9 Rh1 70.70(12) . . ? C16 C9 Rh1 113.14(14) . . ? C10 C9 H9 114.2 . . ? C16 C9 H9 114.2 . . ? Rh1 C9 H9 114.2 . . ? C9 C10 C11 125.01(19) . . ? C9 C10 Rh1 70.66(12) . . ? C11 C10 Rh1 111.87(14) . . ? C9 C10 H10 113.8 . . ? C11 C10 H10 113.8 . . ? Rh1 C10 H10 113.8 . . ? C10 C11 C12 112.27(17) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C11 112.80(17) . . ? C13 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C14 C13 C12 124.6(2) . . ? C14 C13 Rh1 70.47(11) . . ? C12 C13 Rh1 113.34(13) . . ? C14 C13 H13 113.7 . . ? C12 C13 H13 113.7 . . ? Rh1 C13 H13 113.7 . . ? C13 C14 C15 125.31(19) . . ? C13 C14 Rh1 71.19(11) . . ? C15 C14 Rh1 109.94(14) . . ? C13 C14 H14 114.1 . . ? C15 C14 H14 114.1 . . ? Rh1 C14 H14 114.1 . . ? C14 C15 C16 112.59(18) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C9 C16 C15 111.64(18) . . ? C9 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C9 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C18 C17 C24A 123.6(2) . . ? C18 C17 Rh2 70.34(12) . . ? C24A C17 Rh2 111.98(15) . . ? C18 C17 H17A 114.3 . . ? C24A C17 H17A 114.3 . . ? Rh2 C17 H17A 114.3 . . ? C17 C18 C19A 124.9(2) . . ? C17 C18 Rh2 71.05(12) . . ? C19A C18 Rh2 111.68(15) . . ? C17 C18 H18A 113.8 . . ? C19A C18 H18A 113.8 . . ? Rh2 C18 H18A 113.8 . . ? C18 C19A C20A 117.2(3) . . ? C18 C19A H19A 108.0 . . ? C20A C19A H19A 108.0 . . ? C18 C19A H19B 108.0 . . ? C20A C19A H19B 108.0 . . ? H19A C19A H19B 107.2 . . ? C21A C20A C19A 112.4(11) . . ? C21A C20A H20A 109.1 . . ? C19A C20A H20A 109.1 . . ? C21A C20A H20B 109.1 . . ? C19A C20A H20B 109.1 . . ? H20A C20A H20B 107.8 . . ? C22A C21A C20A 124.6(19) . . ? C22A C21A Rh2 68.9(17) . . ? C20A C21A Rh2 111.1(15) . . ? C22A C21A H21A 114.4 . . ? C20A C21A H21A 114.4 . . ? Rh2 C21A H21A 114.4 . . ? C21A C22A C23A 123.2(19) . . ? C21A C22A Rh2 73.8(18) . . ? C23A C22A Rh2 110.3(15) . . ? C21A C22A H22A 114.2 . . ? C23A C22A H22A 114.2 . . ? Rh2 C22A H22A 114.2 . . ? C24A C23A C22A 115.8(12) . . ? C24A C23A H23A 108.3 . . ? C22A C23A H23A 108.3 . . ? C24A C23A H23B 108.3 . . ? C22A C23A H23B 108.3 . . ? H23A C23A H23B 107.4 . . ? C23A C24A C17 114.0(3) . . ? C23A C24A H24A 108.8 . . ? C17 C24A H24A 108.8 . . ? C23A C24A H24B 108.8 . . ? C17 C24A H24B 108.8 . . ? H24A C24A H24B 107.7 . . ? C21B C20B H20C 108.7 . . ? C21B C20B H20D 108.7 . . ? H20C C20B H20D 107.6 . . ? C22B C21B C20B 123.1(8) . . ? C22B C21B Rh2 70.3(9) . . ? C20B C21B Rh2 112.4(8) . . ? C22B C21B H21B 114.4 . . ? C20B C21B H21B 114.4 . . ? Rh2 C21B H21B 114.4 . . ? C21B C22B C23B 126.0(11) . . ? C21B C22B Rh2 70.9(8) . . ? C23B C22B Rh2 111.0(8) . . ? C21B C22B H22B 113.7 . . ? C23B C22B H22B 113.7 . . ? Rh2 C22B H22B 113.7 . . ? C22B C23B H23C 109.0 . . ? C22B C23B H23D 109.0 . . ? H23C C23B H23D 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Rh1 Rh2 N1 57.16(7) . . . . ? C9 Rh1 Rh2 N1 131.38(10) . . . . ? C10 Rh1 Rh2 N1 143.79(7) . . . . ? C14 Rh1 Rh2 N1 -108.90(9) . . . . ? C13 Rh1 Rh2 N1 -134.01(7) . . . . ? S1 Rh1 Rh2 N1 -42.35(5) . . . . ? N3 Rh1 Rh2 C22B 125.5(5) . . . . ? C9 Rh1 Rh2 C22B -160.3(6) . . . . ? C10 Rh1 Rh2 C22B -147.9(5) . . . . ? C14 Rh1 Rh2 C22B -40.6(5) . . . . ? C13 Rh1 Rh2 C22B -65.7(5) . . . . ? S1 Rh1 Rh2 C22B 26.0(5) . . . . ? N3 Rh1 Rh2 C21B 145.6(4) . . . . ? C9 Rh1 Rh2 C21B -140.2(4) . . . . ? C10 Rh1 Rh2 C21B -127.8(4) . . . . ? C14 Rh1 Rh2 C21B -20.4(4) . . . . ? C13 Rh1 Rh2 C21B -45.6(4) . . . . ? S1 Rh1 Rh2 C21B 46.1(4) . . . . ? N3 Rh1 Rh2 C18 -133.45(8) . . . . ? C9 Rh1 Rh2 C18 -59.23(10) . . . . ? C10 Rh1 Rh2 C18 -46.82(8) . . . . ? C14 Rh1 Rh2 C18 60.49(9) . . . . ? C13 Rh1 Rh2 C18 35.38(8) . . . . ? S1 Rh1 Rh2 C18 127.04(6) . . . . ? N3 Rh1 Rh2 C17 -112.37(9) . . . . ? C9 Rh1 Rh2 C17 -38.15(11) . . . . ? C10 Rh1 Rh2 C17 -25.74(9) . . . . ? C14 Rh1 Rh2 C17 81.57(10) . . . . ? C13 Rh1 Rh2 C17 56.46(9) . . . . ? S1 Rh1 Rh2 C17 148.12(7) . . . . ? N3 Rh1 Rh2 C22A 133.5(9) . . . . ? C9 Rh1 Rh2 C22A -152.3(9) . . . . ? C10 Rh1 Rh2 C22A -139.9(9) . . . . ? C14 Rh1 Rh2 C22A -32.6(9) . . . . ? C13 Rh1 Rh2 C22A -57.7(9) . . . . ? S1 Rh1 Rh2 C22A 34.0(9) . . . . ? N3 Rh1 Rh2 C21A 143.1(8) . . . . ? C9 Rh1 Rh2 C21A -142.6(8) . . . . ? C10 Rh1 Rh2 C21A -130.2(8) . . . . ? C14 Rh1 Rh2 C21A -22.9(8) . . . . ? C13 Rh1 Rh2 C21A -48.0(8) . . . . ? S1 Rh1 Rh2 C21A 43.6(8) . . . . ? N3 Rh1 Rh2 S2 -40.82(5) . . . . ? C9 Rh1 Rh2 S2 33.41(9) . . . . ? C10 Rh1 Rh2 S2 45.82(6) . . . . ? C14 Rh1 Rh2 S2 153.12(7) . . . . ? C13 Rh1 Rh2 S2 128.02(6) . . . . ? S1 Rh1 Rh2 S2 -140.33(2) . . . . ? N3 Rh1 S1 C1 -20.12(9) . . . . ? C9 Rh1 S1 C1 -117.62(17) . . . . ? C10 Rh1 S1 C1 73.9(2) . . . . ? C14 Rh1 S1 C1 -177.90(9) . . . . ? C13 Rh1 S1 C1 144.36(9) . . . . ? Rh2 Rh1 S1 C1 51.31(7) . . . . ? N1 Rh2 S2 C5 -22.13(8) . . . . ? C22B Rh2 S2 C5 -112.3(8) . . . . ? C21B Rh2 S2 C5 89.8(16) . . . . ? C18 Rh2 S2 C5 138.57(9) . . . . ? C17 Rh2 S2 C5 176.99(9) . . . . ? C22A Rh2 S2 C5 -118(2) . . . . ? C21A Rh2 S2 C5 63(2) . . . . ? Rh1 Rh2 S2 C5 50.14(7) . . . . ? C22B Rh2 N1 C1 -116.4(3) . . . . ? C21B Rh2 N1 C1 -77.8(3) . . . . ? C18 Rh2 N1 C1 -5.5(3) . . . . ? C17 Rh2 N1 C1 -179.9(2) . . . . ? C22A Rh2 N1 C1 -106.7(5) . . . . ? C21A Rh2 N1 C1 -69.6(6) . . . . ? S2 Rh2 N1 C1 93.19(16) . . . . ? Rh1 Rh2 N1 C1 27.92(15) . . . . ? C22B Rh2 N1 C2 71.4(3) . . . . ? C21B Rh2 N1 C2 110.0(3) . . . . ? C18 Rh2 N1 C2 -177.8(2) . . . . ? C17 Rh2 N1 C2 7.8(3) . . . . ? C22A Rh2 N1 C2 81.0(5) . . . . ? C21A Rh2 N1 C2 118.1(6) . . . . ? S2 Rh2 N1 C2 -79.05(17) . . . . ? Rh1 Rh2 N1 C2 -144.32(18) . . . . ? C9 Rh1 N3 C5 -111.92(17) . . . . ? C10 Rh1 N3 C5 -73.32(17) . . . . ? C14 Rh1 N3 C5 175.32(18) . . . . ? C13 Rh1 N3 C5 -16.7(4) . . . . ? S1 Rh1 N3 C5 90.77(16) . . . . ? Rh2 Rh1 N3 C5 26.87(15) . . . . ? C9 Rh1 N3 C6 74.27(17) . . . . ? C10 Rh1 N3 C6 112.87(17) . . . . ? C14 Rh1 N3 C6 1.5(3) . . . . ? C13 Rh1 N3 C6 169.5(2) . . . . ? S1 Rh1 N3 C6 -83.03(16) . . . . ? Rh2 Rh1 N3 C6 -146.93(17) . . . . ? C2 N1 C1 N2 -0.2(2) . . . . ? Rh2 N1 C1 N2 -173.75(13) . . . . ? C2 N1 C1 S1 -178.48(15) . . . . ? Rh2 N1 C1 S1 8.0(3) . . . . ? C3 N2 C1 N1 0.1(2) . . . . ? C4 N2 C1 N1 175.73(19) . . . . ? C3 N2 C1 S1 178.46(16) . . . . ? C4 N2 C1 S1 -5.9(3) . . . . ? Rh1 S1 C1 N1 -67.75(19) . . . . ? Rh1 S1 C1 N2 114.22(16) . . . . ? C1 N1 C2 C3 0.2(2) . . . . ? Rh2 N1 C2 C3 173.53(15) . . . . ? N1 C2 C3 N2 -0.1(2) . . . . ? C1 N2 C3 C2 0.0(2) . . . . ? C4 N2 C3 C2 -175.6(2) . . . . ? C6 N3 C5 N4 0.3(2) . . . . ? Rh1 N3 C5 N4 -174.46(13) . . . . ? C6 N3 C5 S2 -176.75(15) . . . . ? Rh1 N3 C5 S2 8.4(3) . . . . ? C7 N4 C5 N3 -0.3(2) . . . . ? C8 N4 C5 N3 172.92(19) . . . . ? C7 N4 C5 S2 176.89(16) . . . . ? C8 N4 C5 S2 -9.9(3) . . . . ? Rh2 S2 C5 N3 -66.21(19) . . . . ? Rh2 S2 C5 N4 117.13(16) . . . . ? C5 N3 C6 C7 -0.3(2) . . . . ? Rh1 N3 C6 C7 174.48(14) . . . . ? N3 C6 C7 N4 0.1(2) . . . . ? C5 N4 C7 C6 0.1(2) . . . . ? C8 N4 C7 C6 -173.2(2) . . . . ? N3 Rh1 C9 C10 87.47(12) . . . . ? C14 Rh1 C9 C10 -113.96(13) . . . . ? C13 Rh1 C9 C10 -76.33(13) . . . . ? S1 Rh1 C9 C10 -174.96(11) . . . . ? Rh2 Rh1 C9 C10 19.83(16) . . . . ? N3 Rh1 C9 C16 -154.04(16) . . . . ? C10 Rh1 C9 C16 118.5(2) . . . . ? C14 Rh1 C9 C16 4.53(16) . . . . ? C13 Rh1 C9 C16 42.16(17) . . . . ? S1 Rh1 C9 C16 -56.5(3) . . . . ? Rh2 Rh1 C9 C16 138.32(13) . . . . ? C16 C9 C10 C11 -1.9(3) . . . . ? Rh1 C9 C10 C11 103.7(2) . . . . ? C16 C9 C10 Rh1 -105.61(19) . . . . ? N3 Rh1 C10 C9 -92.82(12) . . . . ? C14 Rh1 C10 C9 66.27(13) . . . . ? C13 Rh1 C10 C9 100.86(13) . . . . ? S1 Rh1 C10 C9 172.86(16) . . . . ? Rh2 Rh1 C10 C9 -166.38(11) . . . . ? N3 Rh1 C10 C11 146.23(15) . . . . ? C9 Rh1 C10 C11 -120.9(2) . . . . ? C14 Rh1 C10 C11 -54.68(16) . . . . ? C13 Rh1 C10 C11 -20.09(15) . . . . ? S1 Rh1 C10 C11 51.9(3) . . . . ? Rh2 Rh1 C10 C11 72.67(15) . . . . ? C9 C10 C11 C12 -49.6(3) . . . . ? Rh1 C10 C11 C12 31.5(2) . . . . ? C10 C11 C12 C13 -27.4(3) . . . . ? C11 C12 C13 C14 92.3(3) . . . . ? C11 C12 C13 Rh1 10.6(2) . . . . ? N3 Rh1 C13 C14 -172.7(2) . . . . ? C9 Rh1 C13 C14 -77.31(13) . . . . ? C10 Rh1 C13 C14 -115.13(13) . . . . ? S1 Rh1 C13 C14 80.04(12) . . . . ? Rh2 Rh1 C13 C14 145.71(11) . . . . ? N3 Rh1 C13 C12 -52.5(3) . . . . ? C9 Rh1 C13 C12 42.89(17) . . . . ? C10 Rh1 C13 C12 5.06(16) . . . . ? C14 Rh1 C13 C12 120.2(2) . . . . ? S1 Rh1 C13 C12 -159.77(16) . . . . ? Rh2 Rh1 C13 C12 -94.10(16) . . . . ? C12 C13 C14 C15 -3.9(3) . . . . ? Rh1 C13 C14 C15 101.6(2) . . . . ? C12 C13 C14 Rh1 -105.43(19) . . . . ? N3 Rh1 C14 C13 174.60(16) . . . . ? C9 Rh1 C14 C13 100.12(13) . . . . ? C10 Rh1 C14 C13 64.89(13) . . . . ? S1 Rh1 C14 C13 -99.81(12) . . . . ? Rh2 Rh1 C14 C13 -43.02(14) . . . . ? N3 Rh1 C14 C15 52.9(3) . . . . ? C9 Rh1 C14 C15 -21.61(15) . . . . ? C10 Rh1 C14 C15 -56.84(16) . . . . ? C13 Rh1 C14 C15 -121.7(2) . . . . ? S1 Rh1 C14 C15 138.45(15) . . . . ? Rh2 Rh1 C14 C15 -164.76(12) . . . . ? C13 C14 C15 C16 -45.3(3) . . . . ? Rh1 C14 C15 C16 35.3(2) . . . . ? C10 C9 C16 C15 94.6(3) . . . . ? Rh1 C9 C16 C15 13.3(2) . . . . ? C14 C15 C16 C9 -32.0(3) . . . . ? N1 Rh2 C17 C18 177.0(2) . . . . ? C22B Rh2 C17 C18 112.4(3) . . . . ? C21B Rh2 C17 C18 74.6(4) . . . . ? C22A Rh2 C17 C18 102.6(5) . . . . ? C21A Rh2 C17 C18 68.4(7) . . . . ? S2 Rh2 C17 C18 -95.69(13) . . . . ? Rh1 Rh2 C17 C18 -35.19(15) . . . . ? N1 Rh2 C17 C24A 57.7(3) . . . . ? C22B Rh2 C17 C24A -7.0(3) . . . . ? C21B Rh2 C17 C24A -44.7(4) . . . . ? C18 Rh2 C17 C24A -119.3(2) . . . . ? C22A Rh2 C17 C24A -16.8(5) . . . . ? C21A Rh2 C17 C24A -51.0(7) . . . . ? S2 Rh2 C17 C24A 144.98(16) . . . . ? Rh1 Rh2 C17 C24A -154.52(14) . . . . ? C24A C17 C18 C19A 0.2(3) . . . . ? Rh2 C17 C18 C19A -103.7(2) . . . . ? C24A C17 C18 Rh2 103.9(2) . . . . ? N1 Rh2 C18 C17 -177.1(2) . . . . ? C22B Rh2 C18 C17 -67.5(3) . . . . ? C21B Rh2 C18 C17 -102.9(3) . . . . ? C22A Rh2 C18 C17 -76.1(6) . . . . ? C21A Rh2 C18 C17 -112.3(5) . . . . ? S2 Rh2 C18 C17 84.47(12) . . . . ? Rh1 Rh2 C18 C17 150.93(12) . . . . ? N1 Rh2 C18 C19A -56.1(3) . . . . ? C22B Rh2 C18 C19A 53.5(3) . . . . ? C21B Rh2 C18 C19A 18.1(3) . . . . ? C17 Rh2 C18 C19A 121.0(2) . . . . ? C22A Rh2 C18 C19A 44.9(6) . . . . ? C21A Rh2 C18 C19A 8.7(5) . . . . ? S2 Rh2 C18 C19A -154.57(16) . . . . ? Rh1 Rh2 C18 C19A -88.11(17) . . . . ? C17 C18 C19A C20A 82.4(5) . . . . ? Rh2 C18 C19A C20A 1.0(5) . . . . ? C18 C19A C20A C21A -15.5(12) . . . . ? C19A C20A C21A C22A -57(3) . . . . ? C19A C20A C21A Rh2 21.7(13) . . . . ? N1 Rh2 C21A C22A -94.6(15) . . . . ? C22B Rh2 C21A C22A -3.5(17) . . . . ? C21B Rh2 C21A C22A 26(6) . . . . ? C18 Rh2 C21A C22A 103.0(15) . . . . ? C17 Rh2 C21A C22A 67.3(16) . . . . ? S2 Rh2 C21A C22A 179.4(18) . . . . ? Rh1 Rh2 C21A C22A -168.3(15) . . . . ? N1 Rh2 C21A C20A 145.1(10) . . . . ? C22B Rh2 C21A C20A -123.7(15) . . . . ? C21B Rh2 C21A C20A -94(7) . . . . ? C18 Rh2 C21A C20A -17.3(9) . . . . ? C17 Rh2 C21A C20A -53.0(10) . . . . ? C22A Rh2 C21A C20A -120.3(19) . . . . ? S2 Rh2 C21A C20A 59(3) . . . . ? Rh1 Rh2 C21A C20A 71.4(10) . . . . ? C20A C21A C22A C23A -2(4) . . . . ? Rh2 C21A C22A C23A -104(2) . . . . ? C20A C21A C22A Rh2 102(2) . . . . ? N1 Rh2 C22A C21A 85.1(15) . . . . ? C22B Rh2 C22A C21A 165(8) . . . . ? C21B Rh2 C22A C21A -8.7(18) . . . . ? C18 Rh2 C22A C21A -75.7(16) . . . . ? C17 Rh2 C22A C21A -113.3(15) . . . . ? S2 Rh2 C22A C21A -179.5(15) . . . . ? Rh1 Rh2 C22A C21A 16(2) . . . . ? N1 Rh2 C22A C23A -154.8(9) . . . . ? C22B Rh2 C22A C23A -75(6) . . . . ? C21B Rh2 C22A C23A 111(2) . . . . ? C18 Rh2 C22A C23A 44.3(9) . . . . ? C17 Rh2 C22A C23A 6.8(8) . . . . ? C21A Rh2 C22A C23A 120.0(18) . . . . ? S2 Rh2 C22A C23A -59(2) . . . . ? Rh1 Rh2 C22A C23A 136.0(8) . . . . ? C21A C22A C23A C24A 88(3) . . . . ? Rh2 C22A C23A C24A 4.4(12) . . . . ? C22A C23A C24A C17 -18.6(11) . . . . ? C18 C17 C24A C23A -56.6(6) . . . . ? Rh2 C17 C24A C23A 23.7(6) . . . . ? N1 Rh2 C21B C22B -85.5(8) . . . . ? C18 Rh2 C21B C22B 113.2(8) . . . . ? C17 Rh2 C21B C22B 75.8(8) . . . . ? C22A Rh2 C21B C22B 2(2) . . . . ? C21A Rh2 C21B C22B -145(7) . . . . ? S2 Rh2 C21B C22B 162.7(13) . . . . ? Rh1 Rh2 C21B C22B -159.8(7) . . . . ? N1 Rh2 C21B C20B 155.8(4) . . . . ? C22B Rh2 C21B C20B -118.7(8) . . . . ? C18 Rh2 C21B C20B -5.4(4) . . . . ? C17 Rh2 C21B C20B -42.9(5) . . . . ? C22A Rh2 C21B C20B -116.9(17) . . . . ? C21A Rh2 C21B C20B 97(7) . . . . ? S2 Rh2 C21B C20B 44.1(17) . . . . ? Rh1 Rh2 C21B C20B 81.5(4) . . . . ? C20B C21B C22B C23B 2(2) . . . . ? Rh2 C21B C22B C23B -102.6(12) . . . . ? C20B C21B C22B Rh2 104.5(12) . . . . ? N1 Rh2 C22B C21B 95.3(7) . . . . ? C18 Rh2 C22B C21B -66.4(8) . . . . ? C17 Rh2 C22B C21B -102.0(7) . . . . ? C22A Rh2 C22B C21B -5(6) . . . . ? C21A Rh2 C22B C21B 7.5(15) . . . . ? S2 Rh2 C22B C21B -174.2(5) . . . . ? Rh1 Rh2 C22B C21B 31.9(11) . . . . ? N1 Rh2 C22B C23B -142.5(5) . . . . ? C21B Rh2 C22B C23B 122.2(11) . . . . ? C18 Rh2 C22B C23B 55.8(5) . . . . ? C17 Rh2 C22B C23B 20.2(5) . . . . ? C22A Rh2 C22B C23B 117(7) . . . . ? C21A Rh2 C22B C23B 129.7(13) . . . . ? S2 Rh2 C22B C23B -52.0(11) . . . . ? Rh1 Rh2 C22B C23B 154.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.356 _refine_diff_density_min -0.825 _refine_diff_density_rms 0.109 data_2squeeze _database_code_depnum_ccdc_archive 'CCDC 826256' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 N6 Rh2 S2' _chemical_formula_sum 'C26 H40 N6 Rh2 S2' _chemical_formula_weight 706.58 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 18.847(4) _cell_length_b 11.036(2) _cell_length_c 30.704(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.28(3) _cell_angle_gamma 90.00 _cell_volume 6303(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6216 _cell_measurement_theta_min 2.195 _cell_measurement_theta_max 24.790 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.204 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.779671 _exptl_absorpt_correction_T_max 0.950000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS 2003)' _exptl_special_details ; ? ; # SQUEEZE RESULTS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 -0.016 0.000 551.5 130.7 2 0.000 -0.026 0.500 551.6 131.1 3 0.566 0.176 0.511 25.7 0.5 4 0.566 0.324 0.011 25.7 0.7 5 0.434 0.676 0.989 25.7 0.8 6 0.434 0.824 0.489 25.7 0.2 _platon_squeeze_details ; Void count and molecular volume equate well with three molecules of dichloromethane (electron count 42, molecular volume \~ 112 cubic Angstroms) - i.e. 6 in total in the cell. ; _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_reflns_number 70590 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 27.48 _reflns_number_total 14455 _reflns_number_gt 11160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART V5.625 (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT V7.06A (Bruker, 2001)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 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. ; _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^)+(0.0544P)^2^+13.1924P] 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_number_reflns 14455 _refine_ls_number_parameters 657 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1407 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 0.76818(3) 0.27302(4) 0.146178(15) 0.02433(11) Uani 1 1 d . . . Rh2 Rh 0.86102(3) -0.03375(4) 0.139465(17) 0.02681(12) Uani 1 1 d . . . S1 S 0.71162(8) 0.10950(12) 0.17649(5) 0.0271(3) Uani 1 1 d . . . S2 S 0.94132(9) 0.13068(13) 0.15425(6) 0.0378(4) Uani 1 1 d . . . N1 N 0.8331(2) -0.0219(4) 0.20240(17) 0.0246(11) Uani 1 1 d . . . N2 N 0.8725(3) -0.0713(4) 0.24036(18) 0.0318(12) Uani 1 1 d . . . N3 N 0.7797(3) 0.0284(4) 0.25778(17) 0.0282(11) Uani 1 1 d . . . N4 N 0.8550(3) 0.2683(4) 0.19776(16) 0.0240(10) Uani 1 1 d . . . N5 N 0.8567(3) 0.3245(4) 0.23817(16) 0.0267(11) Uani 1 1 d . . . N6 N 0.9575(3) 0.2257(4) 0.23839(19) 0.0333(13) Uani 1 1 d . . . C1 C 0.7776(3) 0.0372(5) 0.2127(2) 0.0240(12) Uani 1 1 d . . . C2 C 0.8383(4) -0.0403(5) 0.2726(2) 0.0332(15) Uani 1 1 d . . . C3 C 0.8604(5) -0.0793(7) 0.3196(2) 0.054(2) Uani 1 1 d . . . H3A H 0.8211 -0.1251 0.3292 0.082 Uiso 1 1 calc R . . H3B H 0.8713 -0.0078 0.3383 0.082 Uiso 1 1 calc R . . H3C H 0.9032 -0.1308 0.3218 0.082 Uiso 1 1 calc R . . C4 C 0.7297(4) 0.0811(6) 0.2841(2) 0.0367(16) Uani 1 1 d . . . H4A H 0.7153 0.0176 0.3038 0.044 Uiso 1 1 calc R . . H4B H 0.6859 0.1073 0.2641 0.044 Uiso 1 1 calc R . . C5 C 0.7594(4) 0.1873(6) 0.3119(2) 0.0412(17) Uani 1 1 d . . . H5A H 0.8006 0.1609 0.3334 0.062 Uiso 1 1 calc R . . H5B H 0.7221 0.2200 0.3274 0.062 Uiso 1 1 calc R . . H5C H 0.7748 0.2501 0.2929 0.062 Uiso 1 1 calc R . . C6 C 0.9162(3) 0.2093(5) 0.1982(2) 0.0273(13) Uani 1 1 d . . . C7 C 0.9186(3) 0.2973(5) 0.2617(2) 0.0335(15) Uani 1 1 d . . . C8 C 0.9440(5) 0.3409(6) 0.3077(3) 0.055(2) Uani 1 1 d . . . H8A H 0.9940 0.3681 0.3104 0.082 Uiso 1 1 calc R . . H8B H 0.9408 0.2746 0.3286 0.082 Uiso 1 1 calc R . . H8C H 0.9137 0.4085 0.3144 0.082 Uiso 1 1 calc R . . C9 C 1.0296(4) 0.1749(6) 0.2539(3) 0.052(2) Uani 1 1 d . . . H9A H 1.0612 0.2402 0.2680 0.063 Uiso 1 1 calc R . . H9B H 1.0500 0.1455 0.2281 0.063 Uiso 1 1 calc R . . C10 C 1.0293(4) 0.0731(6) 0.2860(3) 0.053(2) Uani 1 1 d . . . H10A H 1.0098 0.1018 0.3118 0.080 Uiso 1 1 calc R . . H10B H 1.0786 0.0441 0.2952 0.080 Uiso 1 1 calc R . . H10C H 0.9994 0.0069 0.2719 0.080 Uiso 1 1 calc R . . C11 C 0.7808(4) 0.4595(5) 0.1346(2) 0.0349(15) Uani 1 1 d . . . H11 H 0.8039 0.5053 0.1613 0.042 Uiso 1 1 calc R . . C12 C 0.8291(4) 0.3951(5) 0.1139(2) 0.0387(17) Uani 1 1 d . . . H12 H 0.8803 0.4033 0.1286 0.046 Uiso 1 1 calc R . . C13 C 0.8206(6) 0.3680(7) 0.0650(3) 0.067(3) Uani 1 1 d . . . H13A H 0.8286 0.4434 0.0490 0.080 Uiso 1 1 calc R . . H13B H 0.8578 0.3088 0.0597 0.080 Uiso 1 1 calc R . . C14 C 0.7478(5) 0.3181(7) 0.0468(2) 0.063(3) Uani 1 1 d . . . H14A H 0.7524 0.2633 0.0219 0.076 Uiso 1 1 calc R . . H14B H 0.7160 0.3859 0.0350 0.076 Uiso 1 1 calc R . . C15 C 0.7123(4) 0.2484(6) 0.0808(2) 0.047(2) Uani 1 1 d . . . H15 H 0.7003 0.1622 0.0727 0.057 Uiso 1 1 calc R . . C16 C 0.6665(4) 0.3027(6) 0.1063(2) 0.0438(19) Uani 1 1 d . . . H16 H 0.6274 0.2483 0.1134 0.053 Uiso 1 1 calc R . . C17 C 0.6470(4) 0.4370(6) 0.1045(3) 0.054(2) Uani 1 1 d . . . H17A H 0.6182 0.4551 0.1280 0.065 Uiso 1 1 calc R . . H17B H 0.6168 0.4548 0.0758 0.065 Uiso 1 1 calc R . . C18 C 0.7132(4) 0.5194(6) 0.1103(3) 0.052(2) Uani 1 1 d . . . H18A H 0.7221 0.5456 0.0809 0.062 Uiso 1 1 calc R . . H18B H 0.7029 0.5927 0.1268 0.062 Uiso 1 1 calc R . . C19 C 0.9165(4) -0.0727(6) 0.0862(2) 0.0381(16) Uani 1 1 d . . . H19 H 0.9603 -0.0219 0.0856 0.046 Uiso 1 1 calc R . . C20 C 0.8518(4) -0.0152(6) 0.0699(2) 0.0403(16) Uani 1 1 d . . . H20 H 0.8575 0.0699 0.0598 0.048 Uiso 1 1 calc R . . C21 C 0.7880(4) -0.0808(6) 0.0446(2) 0.0456(18) Uani 1 1 d . . . H21A H 0.8050 -0.1517 0.0295 0.055 Uiso 1 1 calc R . . H21B H 0.7625 -0.0261 0.0218 0.055 Uiso 1 1 calc R . . C22 C 0.7354(4) -0.1236(6) 0.0747(2) 0.0428(17) Uani 1 1 d . . . H22A H 0.6985 -0.0603 0.0756 0.051 Uiso 1 1 calc R . . H22B H 0.7106 -0.1977 0.0619 0.051 Uiso 1 1 calc R . . C23 C 0.7718(4) -0.1504(5) 0.1210(2) 0.0333(14) Uani 1 1 d . . . H23 H 0.7382 -0.1542 0.1430 0.040 Uiso 1 1 calc R . . C24 C 0.8332(4) -0.2192(5) 0.1322(2) 0.0325(14) Uani 1 1 d . . . H24 H 0.8357 -0.2641 0.1607 0.039 Uiso 1 1 calc R . . C25 C 0.8697(4) -0.2844(5) 0.0975(2) 0.0382(16) Uani 1 1 d . . . H25A H 0.8905 -0.3618 0.1100 0.046 Uiso 1 1 calc R . . H25B H 0.8332 -0.3037 0.0715 0.046 Uiso 1 1 calc R . . C26 C 0.9290(4) -0.2082(5) 0.0828(2) 0.0411(17) Uani 1 1 d . . . H26A H 0.9755 -0.2293 0.1012 0.049 Uiso 1 1 calc R . . H26B H 0.9325 -0.2285 0.0518 0.049 Uiso 1 1 calc R . . Rh3 Rh 0.33258(3) 0.30412(4) 0.111961(15) 0.02541(12) Uani 1 1 d . . . Rh4 Rh 0.43459(3) -0.00389(4) 0.120529(14) 0.02457(11) Uani 1 1 d . . . S3 S 0.25843(9) 0.13994(14) 0.12367(6) 0.0378(4) Uani 1 1 d . . . S4 S 0.50213(8) 0.15833(12) 0.15494(5) 0.0249(3) Uani 1 1 d . . . N7 N 0.3660(3) -0.0024(4) 0.16675(17) 0.0283(11) Uani 1 1 d . . . N8 N 0.3842(3) -0.0641(4) 0.20641(17) 0.0283(11) Uani 1 1 d . . . N9 N 0.2815(3) 0.0320(4) 0.20576(19) 0.0323(12) Uani 1 1 d . . . N10 N 0.3894(2) 0.2890(4) 0.17568(15) 0.0206(10) Uani 1 1 d . . . N11 N 0.3659(2) 0.3382(4) 0.21249(15) 0.0219(10) Uani 1 1 d . . . N12 N 0.4669(2) 0.2395(4) 0.23354(14) 0.0172(9) Uani 1 1 d . . . C27 C 0.3046(3) 0.0547(5) 0.1669(2) 0.0300(14) Uani 1 1 d . . . C28 C 0.3328(3) -0.0415(5) 0.2291(2) 0.0303(14) Uani 1 1 d . . . C29 C 0.3295(4) -0.0888(6) 0.2741(2) 0.0437(18) Uani 1 1 d . . . H29A H 0.3638 -0.1555 0.2808 0.066 Uiso 1 1 calc R . . H29B H 0.2808 -0.1183 0.2754 0.066 Uiso 1 1 calc R . . H29C H 0.3416 -0.0238 0.2958 0.066 Uiso 1 1 calc R . . C30 C 0.2171(3) 0.0784(6) 0.2208(3) 0.0427(18) Uani 1 1 d . . . H30A H 0.1930 0.0115 0.2341 0.051 Uiso 1 1 calc R . . H30B H 0.1834 0.1094 0.1951 0.051 Uiso 1 1 calc R . . C31 C 0.2348(4) 0.1795(6) 0.2545(3) 0.050(2) Uani 1 1 d . . . H31A H 0.2675 0.1486 0.2802 0.076 Uiso 1 1 calc R . . H31B H 0.1905 0.2085 0.2638 0.076 Uiso 1 1 calc R . . H31C H 0.2580 0.2464 0.2412 0.076 Uiso 1 1 calc R . . C32 C 0.4500(3) 0.2302(4) 0.18878(17) 0.0181(11) Uani 1 1 d . . . C33 C 0.4131(3) 0.3065(5) 0.24684(18) 0.0211(11) Uani 1 1 d . . . C34 C 0.4110(3) 0.3440(5) 0.29286(18) 0.0291(13) Uani 1 1 d . . . H34A H 0.3735 0.4054 0.2932 0.044 Uiso 1 1 calc R . . H34B H 0.4577 0.3778 0.3058 0.044 Uiso 1 1 calc R . . H34C H 0.4003 0.2734 0.3101 0.044 Uiso 1 1 calc R . . C35 C 0.5276(3) 0.1818(5) 0.26188(19) 0.0274(13) Uani 1 1 d . . . H35A H 0.5502 0.2412 0.2841 0.033 Uiso 1 1 calc R . . H35B H 0.5641 0.1577 0.2437 0.033 Uiso 1 1 calc R . . C36 C 0.5049(4) 0.0712(5) 0.28542(19) 0.0311(14) Uani 1 1 d . . . H36A H 0.4685 0.0945 0.3033 0.047 Uiso 1 1 calc R . . H36B H 0.5468 0.0371 0.3046 0.047 Uiso 1 1 calc R . . H36C H 0.4847 0.0105 0.2636 0.047 Uiso 1 1 calc R . . C37 C 0.4140(3) 0.4210(5) 0.09720(19) 0.0281(13) Uani 1 1 d . . . H37 H 0.4582 0.4221 0.1201 0.034 Uiso 1 1 calc R . . C38 C 0.3572(3) 0.4910(5) 0.10793(19) 0.0270(13) Uani 1 1 d . . . H38 H 0.3681 0.5327 0.1372 0.032 Uiso 1 1 calc R . . C39 C 0.3038(4) 0.5583(6) 0.0738(2) 0.0368(16) Uani 1 1 d . . . H39A H 0.2903 0.6358 0.0865 0.044 Uiso 1 1 calc R . . H39B H 0.3268 0.5772 0.0478 0.044 Uiso 1 1 calc R . . C40 C 0.2368(4) 0.4836(6) 0.0593(2) 0.0444(18) Uani 1 1 d . . . H40A H 0.2021 0.4996 0.0796 0.053 Uiso 1 1 calc R . . H40B H 0.2143 0.5100 0.0294 0.053 Uiso 1 1 calc R . . C41 C 0.2510(4) 0.3489(6) 0.0584(2) 0.0437(19) Uani 1 1 d . . . H41 H 0.2069 0.2974 0.0561 0.052 Uiso 1 1 calc R . . C42 C 0.3071(4) 0.2958(6) 0.0422(2) 0.0439(19) Uani 1 1 d . . . H42 H 0.2961 0.2119 0.0308 0.053 Uiso 1 1 calc R . . C43 C 0.3602(5) 0.3622(6) 0.0186(2) 0.052(2) Uani 1 1 d . . . H43A H 0.3369 0.4357 0.0043 0.062 Uiso 1 1 calc R . . H43B H 0.3736 0.3094 -0.0048 0.062 Uiso 1 1 calc R . . C44 C 0.4287(4) 0.3992(6) 0.0503(2) 0.0422(18) Uani 1 1 d . . . H44A H 0.4652 0.3345 0.0508 0.051 Uiso 1 1 calc R . . H44B H 0.4485 0.4741 0.0392 0.051 Uiso 1 1 calc R . . C45 C 0.5201(4) -0.0417(6) 0.0852(2) 0.0359(15) Uani 1 1 d . . . H45 H 0.5663 0.0001 0.0970 0.043 Uiso 1 1 calc R . . C46 C 0.4695(5) 0.0319(6) 0.0597(2) 0.048(2) Uani 1 1 d . . . H46 H 0.4867 0.1170 0.0574 0.058 Uiso 1 1 calc R . . C47 C 0.4154(6) -0.0036(9) 0.0216(3) 0.069(3) Uani 1 1 d . . . H47A H 0.4404 -0.0252 -0.0033 0.083 Uiso 1 1 calc R . . H47B H 0.3841 0.0668 0.0124 0.083 Uiso 1 1 calc R . . C48 C 0.3701(6) -0.1070(7) 0.0308(3) 0.083(4) Uani 1 1 d . . . H48A H 0.3903 -0.1825 0.0204 0.100 Uiso 1 1 calc R . . H48B H 0.3212 -0.0963 0.0137 0.100 Uiso 1 1 calc R . . C49 C 0.3641(4) -0.1213(6) 0.0795(2) 0.0458(19) Uani 1 1 d . . . H49 H 0.3137 -0.1219 0.0859 0.055 Uiso 1 1 calc R . . C50 C 0.4118(4) -0.1888(5) 0.1085(2) 0.0307(14) Uani 1 1 d . . . H50 H 0.3900 -0.2304 0.1321 0.037 Uiso 1 1 calc R . . C51 C 0.4753(4) -0.2545(6) 0.0951(2) 0.0433(18) Uani 1 1 d . . . H51A H 0.5014 -0.2972 0.1212 0.052 Uiso 1 1 calc R . . H51B H 0.4569 -0.3168 0.0729 0.052 Uiso 1 1 calc R . . C52 C 0.5279(5) -0.1754(6) 0.0762(3) 0.0490(19) Uani 1 1 d . . . H52A H 0.5215 -0.1881 0.0439 0.059 Uiso 1 1 calc R . . H52B H 0.5773 -0.2010 0.0887 0.059 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 0.0293(3) 0.0151(2) 0.0278(2) 0.00022(18) 0.00203(19) -0.00593(18) Rh2 0.0269(3) 0.0140(2) 0.0415(3) -0.00145(19) 0.0113(2) -0.00282(18) S1 0.0206(7) 0.0164(6) 0.0433(9) 0.0024(6) 0.0029(6) -0.0025(5) S2 0.0331(9) 0.0173(7) 0.0700(12) -0.0082(7) 0.0293(8) -0.0062(6) N1 0.019(2) 0.012(2) 0.044(3) 0.002(2) 0.007(2) 0.0002(18) N2 0.031(3) 0.014(2) 0.047(3) 0.003(2) -0.003(2) -0.002(2) N3 0.031(3) 0.015(2) 0.039(3) -0.002(2) 0.010(2) -0.008(2) N4 0.027(3) 0.014(2) 0.031(3) -0.0012(19) 0.005(2) -0.0040(19) N5 0.031(3) 0.015(2) 0.034(3) -0.002(2) 0.005(2) -0.003(2) N6 0.021(3) 0.015(2) 0.061(4) -0.004(2) -0.003(2) -0.003(2) C1 0.020(3) 0.015(3) 0.037(3) 0.002(2) 0.003(2) -0.007(2) C2 0.039(4) 0.018(3) 0.041(4) 0.000(3) 0.002(3) -0.011(3) C3 0.082(6) 0.029(4) 0.045(4) 0.003(3) -0.010(4) -0.009(4) C4 0.039(4) 0.029(3) 0.047(4) -0.008(3) 0.023(3) -0.014(3) C5 0.058(5) 0.035(4) 0.034(4) -0.006(3) 0.018(3) -0.020(3) C6 0.017(3) 0.015(3) 0.051(4) -0.004(3) 0.013(3) -0.006(2) C7 0.032(4) 0.010(3) 0.054(4) -0.005(3) -0.004(3) -0.006(2) C8 0.065(5) 0.029(4) 0.060(5) -0.006(3) -0.023(4) 0.005(4) C9 0.022(3) 0.022(3) 0.107(7) 0.001(4) -0.008(4) -0.003(3) C10 0.037(4) 0.027(4) 0.086(6) 0.002(4) -0.020(4) 0.007(3) C11 0.042(4) 0.014(3) 0.046(4) 0.000(3) -0.003(3) -0.009(3) C12 0.062(5) 0.021(3) 0.033(4) 0.001(3) 0.008(3) -0.020(3) C13 0.127(9) 0.037(4) 0.041(5) 0.001(3) 0.029(5) -0.028(5) C14 0.110(8) 0.045(5) 0.031(4) 0.006(3) 0.002(4) -0.027(5) C15 0.072(6) 0.026(3) 0.038(4) 0.004(3) -0.008(4) -0.013(3) C16 0.035(4) 0.035(4) 0.054(4) 0.013(3) -0.015(3) -0.016(3) C17 0.056(5) 0.035(4) 0.061(5) 0.012(4) -0.020(4) -0.005(4) C18 0.055(5) 0.025(4) 0.067(5) 0.012(3) -0.015(4) -0.002(3) C19 0.044(4) 0.027(3) 0.048(4) -0.001(3) 0.021(3) -0.003(3) C20 0.050(4) 0.027(3) 0.047(4) 0.001(3) 0.014(3) -0.005(3) C21 0.057(5) 0.032(4) 0.047(4) 0.001(3) 0.004(4) 0.004(3) C22 0.042(4) 0.026(3) 0.059(5) -0.007(3) 0.005(4) -0.002(3) C23 0.036(4) 0.025(3) 0.041(4) -0.002(3) 0.012(3) -0.010(3) C24 0.044(4) 0.019(3) 0.037(4) 0.003(3) 0.011(3) -0.003(3) C25 0.049(4) 0.016(3) 0.050(4) -0.003(3) 0.011(3) 0.003(3) C26 0.049(4) 0.022(3) 0.053(4) -0.008(3) 0.010(3) 0.001(3) Rh3 0.0327(3) 0.0157(2) 0.0240(2) 0.00360(17) -0.00698(19) -0.00395(18) Rh4 0.0372(3) 0.0147(2) 0.0207(2) -0.00166(17) 0.00124(18) -0.00258(19) S3 0.0310(9) 0.0214(7) 0.0540(11) 0.0081(7) -0.0142(8) -0.0063(6) S4 0.0266(8) 0.0199(7) 0.0295(8) -0.0058(6) 0.0089(6) -0.0030(6) N7 0.029(3) 0.016(2) 0.037(3) 0.004(2) -0.001(2) -0.002(2) N8 0.027(3) 0.016(2) 0.043(3) 0.009(2) 0.010(2) 0.000(2) N9 0.025(3) 0.018(2) 0.057(4) 0.014(2) 0.014(2) 0.001(2) N10 0.020(2) 0.015(2) 0.028(2) 0.0023(18) 0.0069(19) -0.0020(18) N11 0.023(3) 0.013(2) 0.030(3) 0.0008(19) 0.006(2) 0.0021(18) N12 0.016(2) 0.011(2) 0.023(2) -0.0004(17) -0.0017(18) 0.0008(17) C27 0.032(3) 0.007(2) 0.047(4) 0.006(2) -0.005(3) -0.008(2) C28 0.022(3) 0.015(3) 0.057(4) 0.012(3) 0.015(3) 0.004(2) C29 0.042(4) 0.039(4) 0.059(5) 0.024(3) 0.031(4) 0.015(3) C30 0.026(3) 0.026(3) 0.083(5) 0.021(3) 0.026(4) 0.002(3) C31 0.042(4) 0.029(4) 0.089(6) 0.017(4) 0.037(4) 0.016(3) C32 0.020(3) 0.011(2) 0.023(3) -0.001(2) 0.001(2) -0.003(2) C33 0.024(3) 0.015(2) 0.024(3) 0.001(2) 0.003(2) 0.002(2) C34 0.040(4) 0.025(3) 0.023(3) -0.001(2) 0.010(3) 0.007(3) C35 0.026(3) 0.021(3) 0.031(3) -0.006(2) -0.008(2) 0.003(2) C36 0.040(4) 0.027(3) 0.025(3) 0.002(2) -0.001(3) 0.010(3) C37 0.042(4) 0.017(3) 0.025(3) -0.001(2) 0.003(3) -0.009(3) C38 0.041(4) 0.016(3) 0.023(3) 0.002(2) 0.002(3) -0.003(2) C39 0.045(4) 0.028(3) 0.035(4) 0.005(3) -0.001(3) -0.002(3) C40 0.050(4) 0.035(4) 0.042(4) 0.016(3) -0.010(3) 0.003(3) C41 0.056(5) 0.030(3) 0.037(4) 0.009(3) -0.020(3) -0.011(3) C42 0.066(5) 0.029(3) 0.030(4) 0.006(3) -0.014(3) -0.010(3) C43 0.098(7) 0.035(4) 0.020(3) -0.001(3) 0.001(4) 0.009(4) C44 0.075(5) 0.026(3) 0.027(3) 0.001(3) 0.014(3) 0.001(3) C45 0.055(4) 0.026(3) 0.031(3) -0.002(3) 0.018(3) -0.008(3) C46 0.095(6) 0.028(3) 0.022(3) -0.002(3) 0.015(4) 0.006(4) C47 0.100(8) 0.077(7) 0.031(4) -0.008(4) 0.010(4) 0.023(6) C48 0.154(10) 0.034(4) 0.043(5) 0.000(4) -0.043(6) 0.012(5) C49 0.052(5) 0.023(3) 0.057(5) -0.011(3) -0.008(4) -0.009(3) C50 0.044(4) 0.015(3) 0.030(3) -0.002(2) -0.004(3) -0.008(3) C51 0.065(5) 0.020(3) 0.044(4) -0.008(3) 0.009(4) -0.001(3) C52 0.069(6) 0.031(4) 0.051(5) 0.002(3) 0.021(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N4 2.086(5) . ? Rh1 C11 2.108(6) . ? Rh1 C12 2.117(6) . ? Rh1 C16 2.126(7) . ? Rh1 C15 2.129(7) . ? Rh1 S1 2.3619(15) . ? Rh1 Rh2 3.8318(9) . ? Rh2 N1 2.087(5) . ? Rh2 C24 2.116(6) . ? Rh2 C19 2.122(7) . ? Rh2 C23 2.121(6) . ? Rh2 C20 2.124(7) . ? Rh2 S2 2.3596(16) . ? S1 C1 1.724(6) . ? S2 C6 1.732(6) . ? N1 C1 1.314(7) . ? N1 N2 1.389(7) . ? N2 C2 1.312(8) . ? N3 C2 1.355(8) . ? N3 C1 1.382(8) . ? N3 C4 1.459(8) . ? N4 C6 1.323(7) . ? N4 N5 1.383(7) . ? N5 C7 1.305(8) . ? N6 C7 1.359(8) . ? N6 C6 1.362(8) . ? N6 C9 1.475(8) . ? C2 C3 1.498(9) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.502(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.496(10) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.494(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.387(10) . ? C11 C18 1.520(9) . ? C11 H11 1.0000 . ? C12 C13 1.515(10) . ? C12 H12 1.0000 . ? C13 C14 1.500(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.534(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.393(11) . ? C15 H15 1.0000 . ? C16 C17 1.526(10) . ? C16 H16 1.0000 . ? C17 C18 1.531(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.394(10) . ? C19 C26 1.520(9) . ? C19 H19 1.0000 . ? C20 C21 1.508(10) . ? C20 H20 1.0000 . ? C21 C22 1.533(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.505(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.379(9) . ? C23 H23 1.0000 . ? C24 C25 1.537(9) . ? C24 H24 1.0000 . ? C25 C26 1.524(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? Rh3 N10 2.080(5) . ? Rh3 C37 2.110(6) . ? Rh3 C42 2.119(7) . ? Rh3 C41 2.120(6) . ? Rh3 C38 2.122(5) . ? Rh3 S3 2.3511(17) . ? Rh3 Rh4 3.8932(9) . ? Rh4 N7 2.069(5) . ? Rh4 C50 2.106(5) . ? Rh4 C46 2.116(7) . ? Rh4 C49 2.119(6) . ? Rh4 C45 2.124(7) . ? Rh4 S4 2.3469(15) . ? S3 C27 1.741(6) . ? S4 C32 1.733(6) . ? N7 C27 1.318(8) . ? N7 N8 1.389(7) . ? N8 C28 1.304(8) . ? N9 C27 1.357(8) . ? N9 C28 1.372(7) . ? N9 C30 1.460(8) . ? N10 C32 1.319(7) . ? N10 N11 1.389(6) . ? N11 C33 1.313(7) . ? N12 C32 1.364(7) . ? N12 C33 1.370(7) . ? N12 C35 1.466(7) . ? C28 C29 1.488(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.521(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C33 C34 1.479(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.516(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.403(9) . ? C37 C44 1.529(8) . ? C37 H37 1.0000 . ? C38 C39 1.524(8) . ? C38 H38 1.0000 . ? C39 C40 1.513(9) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.512(9) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.371(11) . ? C41 H41 1.0000 . ? C42 C43 1.516(11) . ? C42 H42 1.0000 . ? C43 C44 1.541(10) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.394(10) . ? C45 C52 1.512(9) . ? C45 H45 1.0000 . ? C46 C47 1.474(11) . ? C46 H46 1.0000 . ? C47 C48 1.481(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.527(12) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.378(9) . ? C49 H49 1.0000 . ? C50 C51 1.513(10) . ? C50 H50 1.0000 . ? C51 C52 1.506(10) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? 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 N4 Rh1 C11 93.2(2) . . ? N4 Rh1 C12 87.3(2) . . ? C11 Rh1 C12 38.3(3) . . ? N4 Rh1 C16 164.7(3) . . ? C11 Rh1 C16 82.5(3) . . ? C12 Rh1 C16 98.0(3) . . ? N4 Rh1 C15 157.1(3) . . ? C11 Rh1 C15 91.0(3) . . ? C12 Rh1 C15 82.1(3) . . ? C16 Rh1 C15 38.2(3) . . ? N4 Rh1 S1 91.73(13) . . ? C11 Rh1 S1 151.9(2) . . ? C12 Rh1 S1 169.7(2) . . ? C16 Rh1 S1 85.53(19) . . ? C15 Rh1 S1 95.1(2) . . ? N4 Rh1 Rh2 73.13(12) . . ? C11 Rh1 Rh2 142.0(2) . . ? C12 Rh1 Rh2 104.5(2) . . ? C16 Rh1 Rh2 118.8(2) . . ? C15 Rh1 Rh2 89.8(2) . . ? S1 Rh1 Rh2 65.50(4) . . ? N1 Rh2 C24 93.6(2) . . ? N1 Rh2 C19 162.8(2) . . ? C24 Rh2 C19 82.4(2) . . ? N1 Rh2 C23 88.7(2) . . ? C24 Rh2 C23 38.0(2) . . ? C19 Rh2 C23 98.0(3) . . ? N1 Rh2 C20 158.9(2) . . ? C24 Rh2 C20 90.5(2) . . ? C19 Rh2 C20 38.3(3) . . ? C23 Rh2 C20 81.8(3) . . ? N1 Rh2 S2 91.36(13) . . ? C24 Rh2 S2 154.79(19) . . ? C19 Rh2 S2 85.60(19) . . ? C23 Rh2 S2 167.02(18) . . ? C20 Rh2 S2 93.73(19) . . ? N1 Rh2 Rh1 73.10(12) . . ? C24 Rh2 Rh1 138.82(18) . . ? C19 Rh2 Rh1 120.44(18) . . ? C23 Rh2 Rh1 101.63(18) . . ? C20 Rh2 Rh1 90.29(19) . . ? S2 Rh2 Rh1 66.08(4) . . ? C1 S1 Rh1 106.45(19) . . ? C6 S2 Rh2 106.71(19) . . ? C1 N1 N2 109.4(5) . . ? C1 N1 Rh2 125.7(4) . . ? N2 N1 Rh2 124.9(4) . . ? C2 N2 N1 105.6(5) . . ? C2 N3 C1 105.5(5) . . ? C2 N3 C4 126.9(6) . . ? C1 N3 C4 127.6(5) . . ? C6 N4 N5 108.6(5) . . ? C6 N4 Rh1 126.5(4) . . ? N5 N4 Rh1 124.9(4) . . ? C7 N5 N4 106.5(5) . . ? C7 N6 C6 106.1(5) . . ? C7 N6 C9 126.8(6) . . ? C6 N6 C9 127.2(6) . . ? N1 C1 N3 108.1(5) . . ? N1 C1 S1 126.4(5) . . ? N3 C1 S1 125.5(4) . . ? N2 C2 N3 111.4(6) . . ? N2 C2 C3 123.9(6) . . ? N3 C2 C3 124.7(7) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 114.3(5) . . ? N3 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? N3 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N6 108.3(5) . . ? N4 C6 S2 125.9(5) . . ? N6 C6 S2 125.8(5) . . ? N5 C7 N6 110.6(6) . . ? N5 C7 C8 124.8(6) . . ? N6 C7 C8 124.5(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C10 113.4(6) . . ? N6 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N6 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C18 123.9(7) . . ? C12 C11 Rh1 71.2(3) . . ? C18 C11 Rh1 113.5(4) . . ? C12 C11 H11 113.7 . . ? C18 C11 H11 113.7 . . ? Rh1 C11 H11 113.7 . . ? C11 C12 C13 125.7(7) . . ? C11 C12 Rh1 70.5(4) . . ? C13 C12 Rh1 111.1(4) . . ? C11 C12 H12 113.8 . . ? C13 C12 H12 113.8 . . ? Rh1 C12 H12 113.8 . . ? C14 C13 C12 112.7(7) . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? C12 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 C15 113.8(6) . . ? C13 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? C16 C15 C14 123.1(7) . . ? C16 C15 Rh1 70.8(4) . . ? C14 C15 Rh1 112.0(5) . . ? C16 C15 H15 114.4 . . ? C14 C15 H15 114.4 . . ? Rh1 C15 H15 114.4 . . ? C15 C16 C17 124.4(7) . . ? C15 C16 Rh1 71.0(4) . . ? C17 C16 Rh1 111.1(4) . . ? C15 C16 H16 114.2 . . ? C17 C16 H16 114.2 . . ? Rh1 C16 H16 114.2 . . ? C16 C17 C18 112.7(6) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C11 C18 C17 113.7(5) . . ? C11 C18 H18A 108.8 . . ? C17 C18 H18A 108.8 . . ? C11 C18 H18B 108.8 . . ? C17 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C20 C19 C26 124.0(6) . . ? C20 C19 Rh2 70.9(4) . . ? C26 C19 Rh2 110.7(5) . . ? C20 C19 H19 114.4 . . ? C26 C19 H19 114.4 . . ? Rh2 C19 H19 114.4 . . ? C19 C20 C21 123.1(6) . . ? C19 C20 Rh2 70.7(4) . . ? C21 C20 Rh2 113.6(5) . . ? C19 C20 H20 114.0 . . ? C21 C20 H20 114.0 . . ? Rh2 C20 H20 114.0 . . ? C20 C21 C22 112.2(6) . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C23 C22 C21 112.9(6) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C24 C23 C22 125.4(6) . . ? C24 C23 Rh2 70.8(4) . . ? C22 C23 Rh2 110.7(4) . . ? C24 C23 H23 113.9 . . ? C22 C23 H23 113.9 . . ? Rh2 C23 H23 113.9 . . ? C23 C24 C25 122.5(6) . . ? C23 C24 Rh2 71.2(3) . . ? C25 C24 Rh2 113.3(4) . . ? C23 C24 H24 114.2 . . ? C25 C24 H24 114.2 . . ? Rh2 C24 H24 114.2 . . ? C26 C25 C24 112.2(5) . . ? C26 C25 H25A 109.2 . . ? C24 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C24 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C19 C26 C25 113.2(6) . . ? C19 C26 H26A 108.9 . . ? C25 C26 H26A 108.9 . . ? C19 C26 H26B 108.9 . . ? C25 C26 H26B 108.9 . . ? H26A C26 H26B 107.8 . . ? N10 Rh3 C37 88.2(2) . . ? N10 Rh3 C42 160.9(3) . . ? C37 Rh3 C42 82.1(3) . . ? N10 Rh3 C41 161.2(3) . . ? C37 Rh3 C41 98.8(3) . . ? C42 Rh3 C41 37.7(3) . . ? N10 Rh3 C38 92.80(19) . . ? C37 Rh3 C38 38.7(2) . . ? C42 Rh3 C38 89.9(2) . . ? C41 Rh3 C38 82.3(2) . . ? N10 Rh3 S3 91.30(13) . . ? C37 Rh3 S3 167.21(17) . . ? C42 Rh3 S3 94.5(2) . . ? C41 Rh3 S3 85.61(19) . . ? C38 Rh3 S3 154.00(18) . . ? N10 Rh3 Rh4 72.11(12) . . ? C37 Rh3 Rh4 100.35(17) . . ? C42 Rh3 Rh4 93.4(2) . . ? C41 Rh3 Rh4 123.0(2) . . ? C38 Rh3 Rh4 137.94(17) . . ? S3 Rh3 Rh4 67.42(5) . . ? N7 Rh4 C50 89.7(2) . . ? N7 Rh4 C46 157.2(3) . . ? C50 Rh4 C46 96.3(3) . . ? N7 Rh4 C49 90.6(3) . . ? C50 Rh4 C49 38.1(2) . . ? C46 Rh4 C49 81.0(3) . . ? N7 Rh4 C45 164.1(2) . . ? C50 Rh4 C45 82.6(3) . . ? C46 Rh4 C45 38.4(3) . . ? C49 Rh4 C45 91.8(3) . . ? N7 Rh4 S4 92.22(14) . . ? C50 Rh4 S4 153.96(17) . . ? C46 Rh4 S4 91.8(2) . . ? C49 Rh4 S4 167.6(2) . . ? C45 Rh4 S4 88.78(18) . . ? N7 Rh4 Rh3 71.50(13) . . ? C50 Rh4 Rh3 138.58(18) . . ? C46 Rh4 Rh3 89.88(19) . . ? C49 Rh4 Rh3 103.8(2) . . ? C45 Rh4 Rh3 122.98(17) . . ? S4 Rh4 Rh3 65.83(4) . . ? C27 S3 Rh3 107.3(2) . . ? C32 S4 Rh4 107.48(18) . . ? C27 N7 N8 108.9(5) . . ? C27 N7 Rh4 130.8(4) . . ? N8 N7 Rh4 120.3(4) . . ? C28 N8 N7 106.0(5) . . ? C27 N9 C28 105.6(5) . . ? C27 N9 C30 127.8(5) . . ? C28 N9 C30 126.5(6) . . ? C32 N10 N11 108.5(4) . . ? C32 N10 Rh3 128.0(4) . . ? N11 N10 Rh3 123.4(3) . . ? C33 N11 N10 106.6(4) . . ? C32 N12 C33 106.1(4) . . ? C32 N12 C35 126.8(5) . . ? C33 N12 C35 127.0(5) . . ? N7 C27 N9 108.7(5) . . ? N7 C27 S3 125.8(5) . . ? N9 C27 S3 125.4(5) . . ? N8 C28 N9 110.8(6) . . ? N8 C28 C29 125.2(5) . . ? N9 C28 C29 124.0(5) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N9 C30 C31 111.7(6) . . ? N9 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? N9 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N10 C32 N12 108.7(5) . . ? N10 C32 S4 126.1(4) . . ? N12 C32 S4 125.1(4) . . ? N11 C33 N12 110.0(5) . . ? N11 C33 C34 125.0(5) . . ? N12 C33 C34 124.8(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N12 C35 C36 112.2(5) . . ? N12 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? N12 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C44 124.7(6) . . ? C38 C37 Rh3 71.1(3) . . ? C44 C37 Rh3 110.8(4) . . ? C38 C37 H37 114.1 . . ? C44 C37 H37 114.1 . . ? Rh3 C37 H37 114.1 . . ? C37 C38 C39 123.4(5) . . ? C37 C38 Rh3 70.2(3) . . ? C39 C38 Rh3 112.8(4) . . ? C37 C38 H38 114.2 . . ? C39 C38 H38 114.2 . . ? Rh3 C38 H38 114.2 . . ? C40 C39 C38 111.3(5) . . ? C40 C39 H39A 109.4 . . ? C38 C39 H39A 109.4 . . ? C40 C39 H39B 109.4 . . ? C38 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C41 C40 C39 113.5(6) . . ? C41 C40 H40A 108.9 . . ? C39 C40 H40A 108.9 . . ? C41 C40 H40B 108.9 . . ? C39 C40 H40B 108.9 . . ? H40A C40 H40B 107.7 . . ? C42 C41 C40 125.2(7) . . ? C42 C41 Rh3 71.1(4) . . ? C40 C41 Rh3 108.9(4) . . ? C42 C41 H41 114.4 . . ? C40 C41 H41 114.4 . . ? Rh3 C41 H41 114.4 . . ? C41 C42 C43 125.1(6) . . ? C41 C42 Rh3 71.2(4) . . ? C43 C42 Rh3 113.8(5) . . ? C41 C42 H42 113.3 . . ? C43 C42 H42 113.3 . . ? Rh3 C42 H42 113.3 . . ? C42 C43 C44 112.1(5) . . ? C42 C43 H43A 109.2 . . ? C44 C43 H43A 109.2 . . ? C42 C43 H43B 109.2 . . ? C44 C43 H43B 109.2 . . ? H43A C43 H43B 107.9 . . ? C37 C44 C43 112.1(6) . . ? C37 C44 H44A 109.2 . . ? C43 C44 H44A 109.2 . . ? C37 C44 H44B 109.2 . . ? C43 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C46 C45 C52 122.9(7) . . ? C46 C45 Rh4 70.5(4) . . ? C52 C45 Rh4 112.9(5) . . ? C46 C45 H45 114.3 . . ? C52 C45 H45 114.3 . . ? Rh4 C45 H45 114.3 . . ? C45 C46 C47 127.9(7) . . ? C45 C46 Rh4 71.1(4) . . ? C47 C46 Rh4 112.2(6) . . ? C45 C46 H46 112.7 . . ? C47 C46 H46 112.7 . . ? Rh4 C46 H46 112.7 . . ? C46 C47 C48 113.6(7) . . ? C46 C47 H47A 108.9 . . ? C48 C47 H47A 108.9 . . ? C46 C47 H47B 108.9 . . ? C48 C47 H47B 108.9 . . ? H47A C47 H47B 107.7 . . ? C47 C48 C49 113.8(6) . . ? C47 C48 H48A 108.8 . . ? C49 C48 H48A 108.8 . . ? C47 C48 H48B 108.8 . . ? C49 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C50 C49 C48 123.1(8) . . ? C50 C49 Rh4 70.4(4) . . ? C48 C49 Rh4 112.4(6) . . ? C50 C49 H49 114.4 . . ? C48 C49 H49 114.4 . . ? Rh4 C49 H49 114.4 . . ? C49 C50 C51 123.0(6) . . ? C49 C50 Rh4 71.5(3) . . ? C51 C50 Rh4 111.4(4) . . ? C49 C50 H50 114.5 . . ? C51 C50 H50 114.5 . . ? Rh4 C50 H50 114.5 . . ? C52 C51 C50 115.2(5) . . ? C52 C51 H51A 108.5 . . ? C50 C51 H51A 108.5 . . ? C52 C51 H51B 108.5 . . ? C50 C51 H51B 108.5 . . ? H51A C51 H51B 107.5 . . ? C51 C52 C45 113.9(6) . . ? C51 C52 H52A 108.8 . . ? C45 C52 H52A 108.8 . . ? C51 C52 H52B 108.8 . . ? C45 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? 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 N4 Rh1 Rh2 N1 56.78(19) . . . . ? C11 Rh1 Rh2 N1 129.7(3) . . . . ? C12 Rh1 Rh2 N1 139.4(2) . . . . ? C16 Rh1 Rh2 N1 -112.8(3) . . . . ? C15 Rh1 Rh2 N1 -138.8(3) . . . . ? S1 Rh1 Rh2 N1 -43.17(14) . . . . ? N4 Rh1 Rh2 C24 132.5(3) . . . . ? C11 Rh1 Rh2 C24 -154.6(4) . . . . ? C12 Rh1 Rh2 C24 -144.9(3) . . . . ? C16 Rh1 Rh2 C24 -37.1(4) . . . . ? C15 Rh1 Rh2 C24 -63.1(3) . . . . ? S1 Rh1 Rh2 C24 32.5(3) . . . . ? N4 Rh1 Rh2 C19 -111.6(3) . . . . ? C11 Rh1 Rh2 C19 -38.6(4) . . . . ? C12 Rh1 Rh2 C19 -29.0(3) . . . . ? C16 Rh1 Rh2 C19 78.9(3) . . . . ? C15 Rh1 Rh2 C19 52.9(3) . . . . ? S1 Rh1 Rh2 C19 148.5(2) . . . . ? N4 Rh1 Rh2 C23 141.9(2) . . . . ? C11 Rh1 Rh2 C23 -145.2(3) . . . . ? C12 Rh1 Rh2 C23 -135.6(3) . . . . ? C16 Rh1 Rh2 C23 -27.7(3) . . . . ? C15 Rh1 Rh2 C23 -53.7(3) . . . . ? S1 Rh1 Rh2 C23 41.89(19) . . . . ? N4 Rh1 Rh2 C20 -136.5(2) . . . . ? C11 Rh1 Rh2 C20 -63.5(4) . . . . ? C12 Rh1 Rh2 C20 -53.9(3) . . . . ? C16 Rh1 Rh2 C20 54.0(3) . . . . ? C15 Rh1 Rh2 C20 27.9(3) . . . . ? S1 Rh1 Rh2 C20 123.6(2) . . . . ? N4 Rh1 Rh2 S2 -42.53(15) . . . . ? C11 Rh1 Rh2 S2 30.4(3) . . . . ? C12 Rh1 Rh2 S2 40.0(2) . . . . ? C16 Rh1 Rh2 S2 147.9(2) . . . . ? C15 Rh1 Rh2 S2 121.9(2) . . . . ? S1 Rh1 Rh2 S2 -142.49(7) . . . . ? N4 Rh1 S1 C1 -19.2(3) . . . . ? C11 Rh1 S1 C1 -119.3(4) . . . . ? C12 Rh1 S1 C1 65.3(11) . . . . ? C16 Rh1 S1 C1 175.9(3) . . . . ? C15 Rh1 S1 C1 138.9(3) . . . . ? Rh2 Rh1 S1 C1 51.4(2) . . . . ? N1 Rh2 S2 C6 -19.9(3) . . . . ? C24 Rh2 S2 C6 -121.4(5) . . . . ? C19 Rh2 S2 C6 177.0(3) . . . . ? C23 Rh2 S2 C6 70.4(9) . . . . ? C20 Rh2 S2 C6 139.5(3) . . . . ? Rh1 Rh2 S2 C6 50.9(2) . . . . ? C24 Rh2 N1 C1 -109.9(5) . . . . ? C19 Rh2 N1 C1 174.3(7) . . . . ? C23 Rh2 N1 C1 -72.2(5) . . . . ? C20 Rh2 N1 C1 -9.2(9) . . . . ? S2 Rh2 N1 C1 94.8(4) . . . . ? Rh1 Rh2 N1 C1 30.4(4) . . . . ? C24 Rh2 N1 N2 73.2(4) . . . . ? C19 Rh2 N1 N2 -2.6(9) . . . . ? C23 Rh2 N1 N2 110.9(4) . . . . ? C20 Rh2 N1 N2 173.9(6) . . . . ? S2 Rh2 N1 N2 -82.1(4) . . . . ? Rh1 Rh2 N1 N2 -146.5(4) . . . . ? C1 N1 N2 C2 0.5(6) . . . . ? Rh2 N1 N2 C2 177.9(4) . . . . ? C11 Rh1 N4 C6 -114.0(5) . . . . ? C12 Rh1 N4 C6 -76.1(5) . . . . ? C16 Rh1 N4 C6 173.0(7) . . . . ? C15 Rh1 N4 C6 -13.7(8) . . . . ? S1 Rh1 N4 C6 93.6(5) . . . . ? Rh2 Rh1 N4 C6 29.9(4) . . . . ? C11 Rh1 N4 N5 68.1(4) . . . . ? C12 Rh1 N4 N5 106.0(4) . . . . ? C16 Rh1 N4 N5 -4.9(10) . . . . ? C15 Rh1 N4 N5 168.4(5) . . . . ? S1 Rh1 N4 N5 -84.3(4) . . . . ? Rh2 Rh1 N4 N5 -148.0(4) . . . . ? C6 N4 N5 C7 -0.2(6) . . . . ? Rh1 N4 N5 C7 178.0(4) . . . . ? N2 N1 C1 N3 0.3(6) . . . . ? Rh2 N1 C1 N3 -177.0(3) . . . . ? N2 N1 C1 S1 -177.8(4) . . . . ? Rh2 N1 C1 S1 5.0(7) . . . . ? C2 N3 C1 N1 -1.0(6) . . . . ? C4 N3 C1 N1 179.2(5) . . . . ? C2 N3 C1 S1 177.1(4) . . . . ? C4 N3 C1 S1 -2.8(8) . . . . ? Rh1 S1 C1 N1 -66.3(5) . . . . ? Rh1 S1 C1 N3 116.0(4) . . . . ? N1 N2 C2 N3 -1.2(6) . . . . ? N1 N2 C2 C3 177.1(5) . . . . ? C1 N3 C2 N2 1.4(6) . . . . ? C4 N3 C2 N2 -178.8(5) . . . . ? C1 N3 C2 C3 -176.9(6) . . . . ? C4 N3 C2 C3 2.9(9) . . . . ? C2 N3 C4 C5 73.3(8) . . . . ? C1 N3 C4 C5 -106.9(7) . . . . ? N5 N4 C6 N6 0.4(6) . . . . ? Rh1 N4 C6 N6 -177.8(4) . . . . ? N5 N4 C6 S2 -176.8(4) . . . . ? Rh1 N4 C6 S2 5.0(7) . . . . ? C7 N6 C6 N4 -0.4(6) . . . . ? C9 N6 C6 N4 178.9(5) . . . . ? C7 N6 C6 S2 176.8(4) . . . . ? C9 N6 C6 S2 -3.9(9) . . . . ? Rh2 S2 C6 N4 -65.3(5) . . . . ? Rh2 S2 C6 N6 117.9(5) . . . . ? N4 N5 C7 N6 0.0(6) . . . . ? N4 N5 C7 C8 178.9(6) . . . . ? C6 N6 C7 N5 0.2(7) . . . . ? C9 N6 C7 N5 -179.0(6) . . . . ? C6 N6 C7 C8 -178.7(6) . . . . ? C9 N6 C7 C8 2.0(10) . . . . ? C7 N6 C9 C10 73.6(8) . . . . ? C6 N6 C9 C10 -105.5(8) . . . . ? N4 Rh1 C11 C12 81.5(4) . . . . ? C16 Rh1 C11 C12 -113.2(5) . . . . ? C15 Rh1 C11 C12 -75.9(5) . . . . ? S1 Rh1 C11 C12 -178.7(3) . . . . ? Rh2 Rh1 C11 C12 15.2(6) . . . . ? N4 Rh1 C11 C18 -158.8(6) . . . . ? C12 Rh1 C11 C18 119.7(7) . . . . ? C16 Rh1 C11 C18 6.4(6) . . . . ? C15 Rh1 C11 C18 43.8(6) . . . . ? S1 Rh1 C11 C18 -59.0(7) . . . . ? Rh2 Rh1 C11 C18 134.8(5) . . . . ? C18 C11 C12 C13 -3.8(10) . . . . ? Rh1 C11 C12 C13 102.4(6) . . . . ? C18 C11 C12 Rh1 -106.2(6) . . . . ? N4 Rh1 C12 C11 -98.6(4) . . . . ? C16 Rh1 C12 C11 66.9(4) . . . . ? C15 Rh1 C12 C11 101.8(4) . . . . ? S1 Rh1 C12 C11 176.5(9) . . . . ? Rh2 Rh1 C12 C11 -170.4(4) . . . . ? N4 Rh1 C12 C13 139.6(6) . . . . ? C11 Rh1 C12 C13 -121.8(8) . . . . ? C16 Rh1 C12 C13 -54.9(6) . . . . ? C15 Rh1 C12 C13 -20.0(6) . . . . ? S1 Rh1 C12 C13 54.8(14) . . . . ? Rh2 Rh1 C12 C13 67.8(6) . . . . ? C11 C12 C13 C14 -48.6(10) . . . . ? Rh1 C12 C13 C14 31.9(9) . . . . ? C12 C13 C14 C15 -28.3(11) . . . . ? C13 C14 C15 C16 91.9(10) . . . . ? C13 C14 C15 Rh1 11.1(10) . . . . ? N4 Rh1 C15 C16 -177.1(5) . . . . ? C11 Rh1 C15 C16 -76.4(4) . . . . ? C12 Rh1 C15 C16 -113.8(4) . . . . ? S1 Rh1 C15 C16 76.2(4) . . . . ? Rh2 Rh1 C15 C16 141.5(4) . . . . ? N4 Rh1 C15 C14 -58.3(9) . . . . ? C11 Rh1 C15 C14 42.5(6) . . . . ? C12 Rh1 C15 C14 5.1(6) . . . . ? C16 Rh1 C15 C14 118.9(7) . . . . ? S1 Rh1 C15 C14 -165.0(6) . . . . ? Rh2 Rh1 C15 C14 -99.6(6) . . . . ? C14 C15 C16 C17 -1.2(11) . . . . ? Rh1 C15 C16 C17 103.1(6) . . . . ? C14 C15 C16 Rh1 -104.2(7) . . . . ? N4 Rh1 C16 C15 175.8(7) . . . . ? C11 Rh1 C16 C15 101.4(4) . . . . ? C12 Rh1 C16 C15 66.2(4) . . . . ? S1 Rh1 C16 C15 -104.0(4) . . . . ? Rh2 Rh1 C16 C15 -45.2(4) . . . . ? N4 Rh1 C16 C17 55.3(11) . . . . ? C11 Rh1 C16 C17 -19.1(6) . . . . ? C12 Rh1 C16 C17 -54.2(6) . . . . ? C15 Rh1 C16 C17 -120.5(7) . . . . ? S1 Rh1 C16 C17 135.5(6) . . . . ? Rh2 Rh1 C16 C17 -165.7(5) . . . . ? C15 C16 C17 C18 -52.4(10) . . . . ? Rh1 C16 C17 C18 28.5(9) . . . . ? C12 C11 C18 C17 90.1(9) . . . . ? Rh1 C11 C18 C17 7.6(9) . . . . ? C16 C17 C18 C11 -23.7(10) . . . . ? N1 Rh2 C19 C20 178.0(6) . . . . ? C24 Rh2 C19 C20 100.5(4) . . . . ? C23 Rh2 C19 C20 65.8(4) . . . . ? S2 Rh2 C19 C20 -101.7(4) . . . . ? Rh1 Rh2 C19 C20 -42.8(4) . . . . ? N1 Rh2 C19 C26 57.9(10) . . . . ? C24 Rh2 C19 C26 -19.6(5) . . . . ? C23 Rh2 C19 C26 -54.3(5) . . . . ? C20 Rh2 C19 C26 -120.1(7) . . . . ? S2 Rh2 C19 C26 138.2(5) . . . . ? Rh1 Rh2 C19 C26 -162.9(4) . . . . ? C26 C19 C20 C21 -3.5(11) . . . . ? Rh2 C19 C20 C21 -106.2(7) . . . . ? C26 C19 C20 Rh2 102.6(7) . . . . ? N1 Rh2 C20 C19 -178.3(5) . . . . ? C24 Rh2 C20 C19 -77.0(4) . . . . ? C23 Rh2 C20 C19 -114.2(4) . . . . ? S2 Rh2 C20 C19 78.1(4) . . . . ? Rh1 Rh2 C20 C19 144.1(4) . . . . ? N1 Rh2 C20 C21 -59.7(8) . . . . ? C24 Rh2 C20 C21 41.5(5) . . . . ? C19 Rh2 C20 C21 118.6(7) . . . . ? C23 Rh2 C20 C21 4.4(5) . . . . ? S2 Rh2 C20 C21 -163.3(5) . . . . ? Rh1 Rh2 C20 C21 -97.3(5) . . . . ? C19 C20 C21 C22 93.7(8) . . . . ? Rh2 C20 C21 C22 12.0(7) . . . . ? C20 C21 C22 C23 -29.4(8) . . . . ? C21 C22 C23 C24 -48.0(9) . . . . ? C21 C22 C23 Rh2 32.7(7) . . . . ? N1 Rh2 C23 C24 -97.5(4) . . . . ? C19 Rh2 C23 C24 66.6(4) . . . . ? C20 Rh2 C23 C24 101.4(4) . . . . ? S2 Rh2 C23 C24 171.9(7) . . . . ? Rh1 Rh2 C23 C24 -170.0(3) . . . . ? N1 Rh2 C23 C22 140.9(5) . . . . ? C24 Rh2 C23 C22 -121.6(6) . . . . ? C19 Rh2 C23 C22 -55.0(5) . . . . ? C20 Rh2 C23 C22 -20.2(5) . . . . ? S2 Rh2 C23 C22 50.3(11) . . . . ? Rh1 Rh2 C23 C22 68.4(5) . . . . ? C22 C23 C24 C25 -3.9(10) . . . . ? Rh2 C23 C24 C25 -106.1(6) . . . . ? C22 C23 C24 Rh2 102.3(6) . . . . ? N1 Rh2 C24 C23 83.3(4) . . . . ? C19 Rh2 C24 C23 -113.5(4) . . . . ? C20 Rh2 C24 C23 -75.9(4) . . . . ? S2 Rh2 C24 C23 -175.7(3) . . . . ? Rh1 Rh2 C24 C23 15.0(5) . . . . ? N1 Rh2 C24 C25 -158.6(5) . . . . ? C19 Rh2 C24 C25 4.5(5) . . . . ? C23 Rh2 C24 C25 118.1(7) . . . . ? C20 Rh2 C24 C25 42.1(5) . . . . ? S2 Rh2 C24 C25 -57.7(7) . . . . ? Rh1 Rh2 C24 C25 133.1(4) . . . . ? C23 C24 C25 C26 93.3(8) . . . . ? Rh2 C24 C25 C26 11.5(7) . . . . ? C20 C19 C26 C25 -48.7(9) . . . . ? Rh2 C19 C26 C25 31.7(7) . . . . ? C24 C25 C26 C19 -28.3(9) . . . . ? N10 Rh3 Rh4 N7 59.48(19) . . . . ? C37 Rh3 Rh4 N7 144.2(2) . . . . ? C42 Rh3 Rh4 N7 -133.2(3) . . . . ? C41 Rh3 Rh4 N7 -108.1(3) . . . . ? C38 Rh3 Rh4 N7 133.1(3) . . . . ? S3 Rh3 Rh4 N7 -39.73(15) . . . . ? N10 Rh3 Rh4 C50 126.7(3) . . . . ? C37 Rh3 Rh4 C50 -148.6(3) . . . . ? C42 Rh3 Rh4 C50 -65.9(3) . . . . ? C41 Rh3 Rh4 C50 -40.9(4) . . . . ? C38 Rh3 Rh4 C50 -159.6(3) . . . . ? S3 Rh3 Rh4 C50 27.5(3) . . . . ? N10 Rh3 Rh4 C46 -133.8(3) . . . . ? C37 Rh3 Rh4 C46 -49.1(3) . . . . ? C42 Rh3 Rh4 C46 33.5(3) . . . . ? C41 Rh3 Rh4 C46 58.6(3) . . . . ? C38 Rh3 Rh4 C46 -60.2(3) . . . . ? S3 Rh3 Rh4 C46 127.0(2) . . . . ? N10 Rh3 Rh4 C49 145.4(3) . . . . ? C37 Rh3 Rh4 C49 -129.8(3) . . . . ? C42 Rh3 Rh4 C49 -47.2(3) . . . . ? C41 Rh3 Rh4 C49 -22.2(3) . . . . ? C38 Rh3 Rh4 C49 -140.9(3) . . . . ? S3 Rh3 Rh4 C49 46.2(2) . . . . ? N10 Rh3 Rh4 C45 -113.2(3) . . . . ? C37 Rh3 Rh4 C45 -28.4(3) . . . . ? C42 Rh3 Rh4 C45 54.2(3) . . . . ? C41 Rh3 Rh4 C45 79.3(3) . . . . ? C38 Rh3 Rh4 C45 -39.5(3) . . . . ? S3 Rh3 Rh4 C45 147.6(2) . . . . ? N10 Rh3 Rh4 S4 -41.77(13) . . . . ? C37 Rh3 Rh4 S4 42.97(16) . . . . ? C42 Rh3 Rh4 S4 125.6(2) . . . . ? C41 Rh3 Rh4 S4 150.6(3) . . . . ? C38 Rh3 Rh4 S4 31.9(2) . . . . ? S3 Rh3 Rh4 S4 -140.97(6) . . . . ? N10 Rh3 S3 C27 -22.0(3) . . . . ? C37 Rh3 S3 C27 65.8(8) . . . . ? C42 Rh3 S3 C27 139.9(3) . . . . ? C41 Rh3 S3 C27 176.6(3) . . . . ? C38 Rh3 S3 C27 -121.0(4) . . . . ? Rh4 Rh3 S3 C27 48.0(2) . . . . ? N7 Rh4 S4 C32 -18.4(2) . . . . ? C50 Rh4 S4 C32 -112.3(5) . . . . ? C46 Rh4 S4 C32 139.2(3) . . . . ? C49 Rh4 S4 C32 84.6(11) . . . . ? C45 Rh4 S4 C32 177.5(3) . . . . ? Rh3 Rh4 S4 C32 50.14(19) . . . . ? C50 Rh4 N7 C27 -114.4(5) . . . . ? C46 Rh4 N7 C27 -8.5(9) . . . . ? C49 Rh4 N7 C27 -76.3(5) . . . . ? C45 Rh4 N7 C27 -175.0(7) . . . . ? S4 Rh4 N7 C27 91.6(5) . . . . ? Rh3 Rh4 N7 C27 28.0(5) . . . . ? C50 Rh4 N7 N8 69.3(4) . . . . ? C46 Rh4 N7 N8 175.2(6) . . . . ? C49 Rh4 N7 N8 107.4(4) . . . . ? C45 Rh4 N7 N8 8.7(10) . . . . ? S4 Rh4 N7 N8 -84.7(4) . . . . ? Rh3 Rh4 N7 N8 -148.3(4) . . . . ? C27 N7 N8 C28 -0.1(6) . . . . ? Rh4 N7 N8 C28 177.0(4) . . . . ? C37 Rh3 N10 C32 -72.3(5) . . . . ? C42 Rh3 N10 C32 -12.8(9) . . . . ? C41 Rh3 N10 C32 175.1(6) . . . . ? C38 Rh3 N10 C32 -110.7(5) . . . . ? S3 Rh3 N10 C32 94.9(4) . . . . ? Rh4 Rh3 N10 C32 29.2(4) . . . . ? C37 Rh3 N10 N11 110.4(4) . . . . ? C42 Rh3 N10 N11 169.9(6) . . . . ? C41 Rh3 N10 N11 -2.2(9) . . . . ? C38 Rh3 N10 N11 72.0(4) . . . . ? S3 Rh3 N10 N11 -82.4(4) . . . . ? Rh4 Rh3 N10 N11 -148.1(4) . . . . ? C32 N10 N11 C33 -0.5(6) . . . . ? Rh3 N10 N11 C33 177.3(3) . . . . ? N8 N7 C27 N9 -0.2(6) . . . . ? Rh4 N7 C27 N9 -176.8(4) . . . . ? N8 N7 C27 S3 -177.7(4) . . . . ? Rh4 N7 C27 S3 5.7(8) . . . . ? C28 N9 C27 N7 0.4(6) . . . . ? C30 N9 C27 N7 178.5(6) . . . . ? C28 N9 C27 S3 177.8(4) . . . . ? C30 N9 C27 S3 -4.0(9) . . . . ? Rh3 S3 C27 N7 -63.1(5) . . . . ? Rh3 S3 C27 N9 119.8(5) . . . . ? N7 N8 C28 N9 0.3(7) . . . . ? N7 N8 C28 C29 -179.9(6) . . . . ? C27 N9 C28 N8 -0.4(7) . . . . ? C30 N9 C28 N8 -178.6(6) . . . . ? C27 N9 C28 C29 179.8(6) . . . . ? C30 N9 C28 C29 1.6(10) . . . . ? C27 N9 C30 C31 -103.3(8) . . . . ? C28 N9 C30 C31 74.4(8) . . . . ? N11 N10 C32 N12 0.1(6) . . . . ? Rh3 N10 C32 N12 -177.5(3) . . . . ? N11 N10 C32 S4 -177.3(4) . . . . ? Rh3 N10 C32 S4 5.1(7) . . . . ? C33 N12 C32 N10 0.2(6) . . . . ? C35 N12 C32 N10 176.3(5) . . . . ? C33 N12 C32 S4 177.7(4) . . . . ? C35 N12 C32 S4 -6.2(7) . . . . ? Rh4 S4 C32 N10 -65.5(5) . . . . ? Rh4 S4 C32 N12 117.5(4) . . . . ? N10 N11 C33 N12 0.6(6) . . . . ? N10 N11 C33 C34 177.2(5) . . . . ? C32 N12 C33 N11 -0.5(6) . . . . ? C35 N12 C33 N11 -176.6(5) . . . . ? C32 N12 C33 C34 -177.1(5) . . . . ? C35 N12 C33 C34 6.8(8) . . . . ? C32 N12 C35 C36 -102.1(6) . . . . ? C33 N12 C35 C36 73.1(7) . . . . ? N10 Rh3 C37 C38 -96.7(3) . . . . ? C42 Rh3 C37 C38 99.8(4) . . . . ? C41 Rh3 C37 C38 65.8(4) . . . . ? S3 Rh3 C37 C38 175.2(6) . . . . ? Rh4 Rh3 C37 C38 -168.1(3) . . . . ? N10 Rh3 C37 C44 142.4(5) . . . . ? C42 Rh3 C37 C44 -21.1(5) . . . . ? C41 Rh3 C37 C44 -55.0(5) . . . . ? C38 Rh3 C37 C44 -120.9(6) . . . . ? S3 Rh3 C37 C44 54.3(10) . . . . ? Rh4 Rh3 C37 C44 71.0(4) . . . . ? C44 C37 C38 C39 -2.1(9) . . . . ? Rh3 C37 C38 C39 -104.8(6) . . . . ? C44 C37 C38 Rh3 102.7(6) . . . . ? N10 Rh3 C38 C37 83.7(3) . . . . ? C42 Rh3 C38 C37 -77.5(4) . . . . ? C41 Rh3 C38 C37 -114.5(4) . . . . ? S3 Rh3 C38 C37 -177.6(3) . . . . ? Rh4 Rh3 C38 C37 17.6(4) . . . . ? N10 Rh3 C38 C39 -157.4(5) . . . . ? C37 Rh3 C38 C39 118.9(6) . . . . ? C42 Rh3 C38 C39 41.5(5) . . . . ? C41 Rh3 C38 C39 4.4(5) . . . . ? S3 Rh3 C38 C39 -58.6(6) . . . . ? Rh4 Rh3 C38 C39 136.5(4) . . . . ? C37 C38 C39 C40 94.7(7) . . . . ? Rh3 C38 C39 C40 14.1(7) . . . . ? C38 C39 C40 C41 -33.7(9) . . . . ? C39 C40 C41 C42 -43.1(9) . . . . ? C39 C40 C41 Rh3 36.6(8) . . . . ? N10 Rh3 C41 C42 175.8(6) . . . . ? C37 Rh3 C41 C42 64.8(4) . . . . ? C38 Rh3 C41 C42 100.0(4) . . . . ? S3 Rh3 C41 C42 -103.1(4) . . . . ? Rh4 Rh3 C41 C42 -43.7(5) . . . . ? N10 Rh3 C41 C40 54.1(10) . . . . ? C37 Rh3 C41 C40 -57.0(6) . . . . ? C42 Rh3 C41 C40 -121.8(7) . . . . ? C38 Rh3 C41 C40 -21.8(5) . . . . ? S3 Rh3 C41 C40 135.1(6) . . . . ? Rh4 Rh3 C41 C40 -165.5(4) . . . . ? C40 C41 C42 C43 -6.2(11) . . . . ? Rh3 C41 C42 C43 -106.4(6) . . . . ? C40 C41 C42 Rh3 100.2(6) . . . . ? N10 Rh3 C42 C41 -175.9(5) . . . . ? C37 Rh3 C42 C41 -115.5(4) . . . . ? C38 Rh3 C42 C41 -77.4(4) . . . . ? S3 Rh3 C42 C41 76.9(4) . . . . ? Rh4 Rh3 C42 C41 144.5(4) . . . . ? N10 Rh3 C42 C43 -55.0(9) . . . . ? C37 Rh3 C42 C43 5.4(5) . . . . ? C41 Rh3 C42 C43 120.9(7) . . . . ? C38 Rh3 C42 C43 43.4(6) . . . . ? S3 Rh3 C42 C43 -162.2(5) . . . . ? Rh4 Rh3 C42 C43 -94.6(5) . . . . ? C41 C42 C43 C44 94.5(8) . . . . ? Rh3 C42 C43 C44 11.4(8) . . . . ? C38 C37 C44 C43 -47.6(8) . . . . ? Rh3 C37 C44 C43 33.3(6) . . . . ? C42 C43 C44 C37 -29.1(8) . . . . ? N7 Rh4 C45 C46 171.7(7) . . . . ? C50 Rh4 C45 C46 110.1(4) . . . . ? C49 Rh4 C45 C46 73.1(4) . . . . ? S4 Rh4 C45 C46 -94.5(4) . . . . ? Rh3 Rh4 C45 C46 -34.6(5) . . . . ? N7 Rh4 C45 C52 53.2(11) . . . . ? C50 Rh4 C45 C52 -8.3(5) . . . . ? C46 Rh4 C45 C52 -118.4(7) . . . . ? C49 Rh4 C45 C52 -45.3(5) . . . . ? S4 Rh4 C45 C52 147.1(5) . . . . ? Rh3 Rh4 C45 C52 -153.1(4) . . . . ? C52 C45 C46 C47 1.4(12) . . . . ? Rh4 C45 C46 C47 -103.8(9) . . . . ? C52 C45 C46 Rh4 105.2(6) . . . . ? N7 Rh4 C46 C45 -174.1(5) . . . . ? C50 Rh4 C46 C45 -69.5(4) . . . . ? C49 Rh4 C46 C45 -104.5(4) . . . . ? S4 Rh4 C46 C45 85.7(4) . . . . ? Rh3 Rh4 C46 C45 151.5(4) . . . . ? N7 Rh4 C46 C47 -49.9(9) . . . . ? C50 Rh4 C46 C47 54.6(6) . . . . ? C49 Rh4 C46 C47 19.7(6) . . . . ? C45 Rh4 C46 C47 124.2(7) . . . . ? S4 Rh4 C46 C47 -150.1(5) . . . . ? Rh3 Rh4 C46 C47 -84.3(5) . . . . ? C45 C46 C47 C48 52.7(12) . . . . ? Rh4 C46 C47 C48 -30.1(9) . . . . ? C46 C47 C48 C49 25.0(12) . . . . ? C47 C48 C49 C50 -88.8(9) . . . . ? C47 C48 C49 Rh4 -8.2(10) . . . . ? N7 Rh4 C49 C50 -88.8(5) . . . . ? C46 Rh4 C49 C50 112.5(5) . . . . ? C45 Rh4 C49 C50 75.5(5) . . . . ? S4 Rh4 C49 C50 168.0(8) . . . . ? Rh3 Rh4 C49 C50 -159.9(4) . . . . ? N7 Rh4 C49 C48 152.5(6) . . . . ? C50 Rh4 C49 C48 -118.7(8) . . . . ? C46 Rh4 C49 C48 -6.2(6) . . . . ? C45 Rh4 C49 C48 -43.2(6) . . . . ? S4 Rh4 C49 C48 49.3(14) . . . . ? Rh3 Rh4 C49 C48 81.5(6) . . . . ? C48 C49 C50 C51 0.6(10) . . . . ? Rh4 C49 C50 C51 -103.9(6) . . . . ? C48 C49 C50 Rh4 104.5(7) . . . . ? N7 Rh4 C50 C49 91.3(5) . . . . ? C46 Rh4 C50 C49 -66.7(5) . . . . ? C45 Rh4 C50 C49 -102.6(5) . . . . ? S4 Rh4 C50 C49 -174.2(4) . . . . ? Rh3 Rh4 C50 C49 30.4(6) . . . . ? N7 Rh4 C50 C51 -149.6(5) . . . . ? C46 Rh4 C50 C51 52.4(5) . . . . ? C49 Rh4 C50 C51 119.1(7) . . . . ? C45 Rh4 C50 C51 16.5(5) . . . . ? S4 Rh4 C50 C51 -55.1(7) . . . . ? Rh3 Rh4 C50 C51 149.5(4) . . . . ? C49 C50 C51 C52 58.8(9) . . . . ? Rh4 C50 C51 C52 -22.4(7) . . . . ? C50 C51 C52 C45 15.9(9) . . . . ? C46 C45 C52 C51 -82.6(9) . . . . ? Rh4 C45 C52 C51 -1.7(8) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.362 _refine_diff_density_min -0.871 _refine_diff_density_rms 0.144 data_3 _database_code_depnum_ccdc_archive 'CCDC 826257' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H10 N4 O4 Rh2 S2, C7 H8' _chemical_formula_sum 'C19 H18 N4 O4 Rh2 S2' _chemical_formula_weight 636.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 6.7420(4) _cell_length_b 24.9787(15) _cell_length_c 14.0857(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.7430(10) _cell_angle_gamma 90.00 _cell_volume 2330.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3967 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.75 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 1.627 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_reflns_number 24595 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5341 _reflns_number_gt 3428 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0308P)^2^+6.3962P] 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_number_reflns 5341 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.17367(6) 0.367359(16) 0.44242(3) 0.02257(11) Uani 1 1 d . . . Rh2 Rh 0.60329(6) 0.369814(17) 0.40326(3) 0.02358(11) Uani 1 1 d . . . S1 S 0.1176(2) 0.31763(5) 0.29560(10) 0.0273(3) Uani 1 1 d . . . S2 S 0.6808(2) 0.32649(6) 0.55625(10) 0.0303(3) Uani 1 1 d . . . O1 O 0.2076(8) 0.42826(17) 0.6286(3) 0.0532(12) Uani 1 1 d . . . O2 O 0.0249(6) 0.46366(16) 0.3246(3) 0.0421(10) Uani 1 1 d . . . O3 O 0.7132(7) 0.47316(17) 0.5065(3) 0.0532(12) Uani 1 1 d . . . O4 O 0.5107(8) 0.42272(18) 0.2089(3) 0.0559(13) Uani 1 1 d . . . N1 N 0.5245(6) 0.29531(17) 0.3405(3) 0.0238(9) Uani 1 1 d . . . N2 N 0.3337(7) 0.22569(16) 0.2884(3) 0.0265(10) Uani 1 1 d . . . N3 N 0.2796(6) 0.29699(17) 0.5160(3) 0.0243(9) Uani 1 1 d . . . N4 N 0.4867(6) 0.23195(17) 0.5744(3) 0.0251(10) Uani 1 1 d . . . C1 C 0.3325(8) 0.2784(2) 0.3091(4) 0.0233(11) Uani 1 1 d . . . C2 C 0.6474(8) 0.2511(2) 0.3391(4) 0.0283(12) Uani 1 1 d . . . H2 H 0.7902 0.2508 0.3580 0.034 Uiso 1 1 calc R . . C3 C 0.5312(9) 0.2083(2) 0.3065(4) 0.0322(13) Uani 1 1 d . . . H3 H 0.5771 0.1730 0.2978 0.039 Uiso 1 1 calc R . . C4 C 0.1571(9) 0.1922(2) 0.2579(4) 0.0356(14) Uani 1 1 d . . . H4A H 0.0523 0.2019 0.2945 0.053 Uiso 1 1 calc R . . H4B H 0.1942 0.1545 0.2698 0.053 Uiso 1 1 calc R . . H4C H 0.1057 0.1976 0.1888 0.053 Uiso 1 1 calc R . . C5 C 0.4734(8) 0.2842(2) 0.5469(3) 0.0228(11) Uani 1 1 d . . . C6 C 0.1680(8) 0.2517(2) 0.5234(4) 0.0278(12) Uani 1 1 d . . . H6 H 0.0253 0.2492 0.5059 0.033 Uiso 1 1 calc R . . C7 C 0.2921(8) 0.2112(2) 0.5592(4) 0.0328(13) Uani 1 1 d . . . H7 H 0.2541 0.1756 0.5715 0.039 Uiso 1 1 calc R . . C8 C 0.6734(8) 0.2016(2) 0.6045(4) 0.0355(14) Uani 1 1 d . . . H8A H 0.7141 0.1855 0.5476 0.053 Uiso 1 1 calc R . . H8B H 0.6511 0.1733 0.6495 0.053 Uiso 1 1 calc R . . H8C H 0.7802 0.2256 0.6364 0.053 Uiso 1 1 calc R . . C9 C 0.1967(8) 0.4047(2) 0.5575(4) 0.0326(13) Uani 1 1 d . . . C10 C 0.0802(8) 0.4273(2) 0.3694(4) 0.0297(12) Uani 1 1 d . . . C11 C 0.6718(8) 0.4342(2) 0.4655(4) 0.0318(13) Uani 1 1 d . . . C12 C 0.5477(9) 0.4034(2) 0.2822(4) 0.0326(13) Uani 1 1 d . . . C13 C 0.8577(12) 0.0689(3) 0.4820(5) 0.0525(18) Uani 1 1 d . . . C14 C 0.6560(12) 0.0574(3) 0.4584(6) 0.059(2) Uani 1 1 d . . . H14 H 0.5810 0.0522 0.5085 0.070 Uiso 1 1 calc R . . C15 C 0.5579(13) 0.0533(3) 0.3619(6) 0.063(2) Uani 1 1 d . . . H15 H 0.4174 0.0459 0.3464 0.076 Uiso 1 1 calc R . . C16 C 0.6685(14) 0.0602(3) 0.2895(6) 0.063(2) Uani 1 1 d . . . H16 H 0.6057 0.0562 0.2237 0.076 Uiso 1 1 calc R . . C17 C 0.8670(14) 0.0728(3) 0.3130(7) 0.071(2) Uani 1 1 d . . . H17 H 0.9410 0.0790 0.2629 0.085 Uiso 1 1 calc R . . C18 C 0.9642(13) 0.0767(3) 0.4080(6) 0.065(2) Uani 1 1 d . . . H18 H 1.1043 0.0848 0.4226 0.078 Uiso 1 1 calc R . . C19 C 0.9658(15) 0.0719(3) 0.5859(6) 0.080(3) Uani 1 1 d . . . H19A H 0.9610 0.1088 0.6094 0.120 Uiso 1 1 calc R . . H19B H 1.1068 0.0610 0.5902 0.120 Uiso 1 1 calc R . . H19C H 0.8997 0.0480 0.6256 0.120 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 0.0211(2) 0.0226(2) 0.0240(2) 0.00012(18) 0.00400(16) 0.00289(18) Rh2 0.0222(2) 0.0217(2) 0.0271(2) -0.00089(18) 0.00535(17) -0.00443(18) S1 0.0217(7) 0.0297(7) 0.0280(7) -0.0048(6) -0.0017(5) 0.0004(5) S2 0.0252(7) 0.0336(8) 0.0289(7) 0.0018(6) -0.0035(6) -0.0057(6) O1 0.083(4) 0.045(3) 0.032(2) -0.004(2) 0.012(2) 0.013(2) O2 0.048(3) 0.031(2) 0.045(3) 0.010(2) 0.004(2) 0.0068(19) O3 0.060(3) 0.034(2) 0.063(3) -0.019(2) 0.005(2) -0.011(2) O4 0.075(4) 0.053(3) 0.041(3) 0.021(2) 0.013(2) 0.005(3) N1 0.023(2) 0.026(2) 0.024(2) 0.0001(18) 0.0068(18) -0.0040(18) N2 0.028(3) 0.022(2) 0.030(2) -0.0045(19) 0.008(2) -0.0019(18) N3 0.021(2) 0.026(2) 0.025(2) 0.0032(19) 0.0039(18) 0.0011(18) N4 0.023(2) 0.027(2) 0.026(2) 0.0051(19) 0.0042(19) 0.0056(18) C1 0.023(3) 0.027(3) 0.021(3) -0.005(2) 0.008(2) -0.004(2) C2 0.020(3) 0.031(3) 0.032(3) 0.001(2) 0.003(2) 0.003(2) C3 0.035(3) 0.025(3) 0.038(3) -0.004(2) 0.010(3) 0.003(2) C4 0.037(3) 0.028(3) 0.042(3) -0.008(3) 0.005(3) -0.010(3) C5 0.024(3) 0.025(3) 0.019(3) -0.001(2) 0.002(2) -0.003(2) C6 0.025(3) 0.032(3) 0.026(3) 0.007(2) 0.005(2) -0.004(2) C7 0.034(3) 0.033(3) 0.033(3) 0.007(2) 0.008(3) -0.007(3) C8 0.030(3) 0.034(3) 0.044(3) 0.015(3) 0.010(3) 0.012(3) C9 0.028(3) 0.040(3) 0.030(3) 0.004(3) 0.004(2) 0.003(3) C10 0.032(3) 0.033(3) 0.024(3) -0.008(2) 0.005(2) 0.000(2) C11 0.026(3) 0.031(3) 0.038(3) 0.001(3) 0.005(3) -0.003(2) C12 0.039(3) 0.021(3) 0.040(3) -0.005(3) 0.013(3) -0.004(2) C13 0.069(5) 0.032(4) 0.055(5) -0.006(3) 0.008(4) -0.001(3) C14 0.069(5) 0.049(4) 0.066(5) -0.003(4) 0.031(4) -0.003(4) C15 0.069(5) 0.055(5) 0.065(5) -0.007(4) 0.012(4) 0.002(4) C16 0.093(7) 0.041(4) 0.052(5) -0.003(3) 0.005(5) 0.000(4) C17 0.085(7) 0.061(5) 0.073(6) -0.009(4) 0.032(5) -0.009(5) C18 0.076(6) 0.046(4) 0.079(6) -0.011(4) 0.032(5) -0.010(4) C19 0.107(7) 0.058(5) 0.072(6) -0.009(4) 0.010(5) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C9 1.851(6) . ? Rh1 C10 1.858(6) . ? Rh1 N3 2.097(4) . ? Rh1 S1 2.3815(14) . ? Rh1 Rh2 3.0485(6) . ? Rh2 C11 1.848(6) . ? Rh2 C12 1.874(6) . ? Rh2 N1 2.086(4) . ? Rh2 S2 2.3808(14) . ? S1 C1 1.730(5) . ? S2 C5 1.738(5) . ? O1 C9 1.152(7) . ? O2 C10 1.129(6) . ? O3 C11 1.140(6) . ? O4 C12 1.125(7) . ? N1 C1 1.355(6) . ? N1 C2 1.384(6) . ? N2 C1 1.349(6) . ? N2 C3 1.378(7) . ? N2 C4 1.453(6) . ? N3 C5 1.336(6) . ? N3 C6 1.373(6) . ? N4 C5 1.360(6) . ? N4 C7 1.389(7) . ? N4 C8 1.464(6) . ? C2 C3 1.353(7) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.349(7) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C13 C14 1.369(10) . ? C13 C18 1.386(10) . ? C13 C19 1.510(10) . ? C14 C15 1.400(10) . ? C14 H14 0.9500 . ? C15 C16 1.382(10) . ? C15 H15 0.9500 . ? C16 C17 1.354(11) . ? C16 H16 0.9500 . ? C17 C18 1.379(11) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 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 C9 Rh1 C10 92.5(2) . . ? C9 Rh1 N3 91.4(2) . . ? C10 Rh1 N3 176.1(2) . . ? C9 Rh1 S1 175.50(18) . . ? C10 Rh1 S1 87.52(16) . . ? N3 Rh1 S1 88.65(12) . . ? C9 Rh1 Rh2 102.76(17) . . ? C10 Rh1 Rh2 96.84(17) . . ? N3 Rh1 Rh2 81.89(11) . . ? S1 Rh1 Rh2 81.70(3) . . ? C11 Rh2 C12 91.8(2) . . ? C11 Rh2 N1 176.8(2) . . ? C12 Rh2 N1 91.3(2) . . ? C11 Rh2 S2 88.43(18) . . ? C12 Rh2 S2 178.73(18) . . ? N1 Rh2 S2 88.49(12) . . ? C11 Rh2 Rh1 95.38(17) . . ? C12 Rh2 Rh1 97.94(18) . . ? N1 Rh2 Rh1 83.30(11) . . ? S2 Rh2 Rh1 83.27(4) . . ? C1 S1 Rh1 101.90(17) . . ? C5 S2 Rh2 99.77(17) . . ? C1 N1 C2 106.5(4) . . ? C1 N1 Rh2 124.7(3) . . ? C2 N1 Rh2 127.8(3) . . ? C1 N2 C3 108.2(4) . . ? C1 N2 C4 126.0(5) . . ? C3 N2 C4 125.7(4) . . ? C5 N3 C6 107.2(4) . . ? C5 N3 Rh1 125.6(3) . . ? C6 N3 Rh1 126.0(3) . . ? C5 N4 C7 107.7(4) . . ? C5 N4 C8 126.0(5) . . ? C7 N4 C8 126.0(5) . . ? N2 C1 N1 109.3(4) . . ? N2 C1 S1 124.6(4) . . ? N1 C1 S1 126.1(4) . . ? C3 C2 N1 109.0(5) . . ? C3 C2 H2 125.5 . . ? N1 C2 H2 125.5 . . ? C2 C3 N2 107.0(5) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N4 109.3(4) . . ? N3 C5 S2 127.2(4) . . ? N4 C5 S2 123.5(4) . . ? C7 C6 N3 109.6(5) . . ? C7 C6 H6 125.2 . . ? N3 C6 H6 125.2 . . ? C6 C7 N4 106.2(5) . . ? C6 C7 H7 126.9 . . ? N4 C7 H7 126.9 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 Rh1 178.8(5) . . ? O2 C10 Rh1 179.4(5) . . ? O3 C11 Rh2 177.9(5) . . ? O4 C12 Rh2 178.4(6) . . ? C14 C13 C18 118.5(8) . . ? C14 C13 C19 121.6(8) . . ? C18 C13 C19 119.9(8) . . ? C13 C14 C15 121.3(7) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.0(8) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 119.5(8) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 121.6(8) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C13 120.0(8) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 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 C9 Rh1 Rh2 C11 -29.3(3) . . . . ? C10 Rh1 Rh2 C11 64.9(2) . . . . ? N3 Rh1 Rh2 C11 -118.9(2) . . . . ? S1 Rh1 Rh2 C11 151.32(18) . . . . ? C9 Rh1 Rh2 C12 -121.9(2) . . . . ? C10 Rh1 Rh2 C12 -27.8(2) . . . . ? N3 Rh1 Rh2 C12 148.5(2) . . . . ? S1 Rh1 Rh2 C12 58.71(17) . . . . ? C9 Rh1 Rh2 N1 147.7(2) . . . . ? C10 Rh1 Rh2 N1 -118.1(2) . . . . ? N3 Rh1 Rh2 N1 58.18(16) . . . . ? S1 Rh1 Rh2 N1 -31.63(12) . . . . ? C9 Rh1 Rh2 S2 58.48(18) . . . . ? C10 Rh1 Rh2 S2 152.63(16) . . . . ? N3 Rh1 Rh2 S2 -31.09(12) . . . . ? S1 Rh1 Rh2 S2 -120.90(5) . . . . ? C9 Rh1 S1 C1 -132(2) . . . . ? C10 Rh1 S1 C1 137.1(2) . . . . ? N3 Rh1 S1 C1 -42.2(2) . . . . ? Rh2 Rh1 S1 C1 39.83(18) . . . . ? C11 Rh2 S2 C5 134.9(2) . . . . ? C12 Rh2 S2 C5 -123(8) . . . . ? N1 Rh2 S2 C5 -44.1(2) . . . . ? Rh1 Rh2 S2 C5 39.30(18) . . . . ? C11 Rh2 N1 C1 87(4) . . . . ? C12 Rh2 N1 C1 -76.9(4) . . . . ? S2 Rh2 N1 C1 104.4(4) . . . . ? Rh1 Rh2 N1 C1 21.0(4) . . . . ? C11 Rh2 N1 C2 -80(4) . . . . ? C12 Rh2 N1 C2 116.3(4) . . . . ? S2 Rh2 N1 C2 -62.5(4) . . . . ? Rh1 Rh2 N1 C2 -145.9(4) . . . . ? C9 Rh1 N3 C5 -83.2(4) . . . . ? C10 Rh1 N3 C5 91(3) . . . . ? S1 Rh1 N3 C5 101.3(4) . . . . ? Rh2 Rh1 N3 C5 19.5(4) . . . . ? C9 Rh1 N3 C6 111.2(5) . . . . ? C10 Rh1 N3 C6 -75(3) . . . . ? S1 Rh1 N3 C6 -64.3(4) . . . . ? Rh2 Rh1 N3 C6 -146.1(4) . . . . ? C3 N2 C1 N1 -0.3(6) . . . . ? C4 N2 C1 N1 176.4(5) . . . . ? C3 N2 C1 S1 179.0(4) . . . . ? C4 N2 C1 S1 -4.3(8) . . . . ? C2 N1 C1 N2 -0.1(6) . . . . ? Rh2 N1 C1 N2 -169.3(3) . . . . ? C2 N1 C1 S1 -179.4(4) . . . . ? Rh2 N1 C1 S1 11.4(6) . . . . ? Rh1 S1 C1 N2 135.3(4) . . . . ? Rh1 S1 C1 N1 -45.4(5) . . . . ? C1 N1 C2 C3 0.5(6) . . . . ? Rh2 N1 C2 C3 169.3(4) . . . . ? N1 C2 C3 N2 -0.7(6) . . . . ? C1 N2 C3 C2 0.6(6) . . . . ? C4 N2 C3 C2 -176.1(5) . . . . ? C6 N3 C5 N4 -0.5(6) . . . . ? Rh1 N3 C5 N4 -168.3(3) . . . . ? C6 N3 C5 S2 -178.4(4) . . . . ? Rh1 N3 C5 S2 13.8(7) . . . . ? C7 N4 C5 N3 0.4(6) . . . . ? C8 N4 C5 N3 174.3(5) . . . . ? C7 N4 C5 S2 178.4(4) . . . . ? C8 N4 C5 S2 -7.7(7) . . . . ? Rh2 S2 C5 N3 -46.3(5) . . . . ? Rh2 S2 C5 N4 136.1(4) . . . . ? C5 N3 C6 C7 0.3(6) . . . . ? Rh1 N3 C6 C7 168.2(4) . . . . ? N3 C6 C7 N4 -0.1(6) . . . . ? C5 N4 C7 C6 -0.2(6) . . . . ? C8 N4 C7 C6 -174.1(5) . . . . ? C10 Rh1 C9 O1 47(27) . . . . ? N3 Rh1 C9 O1 -133(27) . . . . ? S1 Rh1 C9 O1 -43(28) . . . . ? Rh2 Rh1 C9 O1 145(27) . . . . ? C9 Rh1 C10 O2 116(51) . . . . ? N3 Rh1 C10 O2 -58(53) . . . . ? S1 Rh1 C10 O2 -68(51) . . . . ? Rh2 Rh1 C10 O2 13(51) . . . . ? C12 Rh2 C11 O3 160(14) . . . . ? N1 Rh2 C11 O3 -3(17) . . . . ? S2 Rh2 C11 O3 -21(14) . . . . ? Rh1 Rh2 C11 O3 62(14) . . . . ? C11 Rh2 C12 O4 -144(20) . . . . ? N1 Rh2 C12 O4 35(20) . . . . ? S2 Rh2 C12 O4 114(19) . . . . ? Rh1 Rh2 C12 O4 -48(20) . . . . ? C18 C13 C14 C15 0.3(11) . . . . ? C19 C13 C14 C15 -178.3(7) . . . . ? C13 C14 C15 C16 1.0(11) . . . . ? C14 C15 C16 C17 -2.4(11) . . . . ? C15 C16 C17 C18 2.7(12) . . . . ? C16 C17 C18 C13 -1.4(12) . . . . ? C14 C13 C18 C17 -0.1(11) . . . . ? C19 C13 C18 C17 178.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.381 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.133 data_5squeeze _database_code_depnum_ccdc_archive 'CCDC 826258' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H40 N4 O2 P2 Rh2 S2, C7 H8' _chemical_formula_sum 'C53 H48 N4 O2 P2 Rh2 S2' _chemical_formula_weight 1104.83 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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_space_group_name_Hall '-P 2ybc' 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 18.748(4) _cell_length_b 13.648(3) _cell_length_c 21.383(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.10(3) _cell_angle_gamma 90.00 _cell_volume 5169.9(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17205 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_reflns_number 58139 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.51 _reflns_number_total 11852 _reflns_number_gt 9512 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 225 53 ' ' 2 0.500 0.500 0.500 225 53 ' ' _platon_squeeze_details ; ; _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^)+(0.0366P)^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_number_reflns 11852 _refine_ls_number_parameters 589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0658 _refine_ls_wR_factor_gt 0.0639 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.900 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.172288(9) 0.087149(12) 0.332352(8) 0.01469(4) Uani 1 1 d . . . Rh2 Rh 0.251459(9) 0.264904(12) 0.462074(8) 0.01505(5) Uani 1 1 d . . . P1 P 0.22820(3) -0.06140(4) 0.36152(3) 0.01529(11) Uani 1 1 d . . . P2 P 0.16355(3) 0.35710(4) 0.48647(3) 0.01547(11) Uani 1 1 d . . . S1 S 0.11004(3) 0.24050(4) 0.30127(3) 0.02175(12) Uani 1 1 d . . . S2 S 0.35022(3) 0.17152(4) 0.44435(3) 0.02092(12) Uani 1 1 d . . . N1 N 0.23764(9) 0.33916(12) 0.37347(9) 0.0167(4) Uani 1 1 d . . . N2 N 0.19364(11) 0.38425(14) 0.26931(9) 0.0250(4) Uani 1 1 d . . . N3 N 0.26637(10) 0.14513(12) 0.31365(9) 0.0173(4) Uani 1 1 d . . . N4 N 0.38031(11) 0.20106(14) 0.32923(10) 0.0268(4) Uani 1 1 d . . . O1 O 0.03192(9) 0.01238(12) 0.35077(8) 0.0272(4) Uani 1 1 d . . . O2 O 0.27802(11) 0.16266(13) 0.59007(8) 0.0404(5) Uani 1 1 d . . . C1 C 0.18264(12) 0.32442(15) 0.31589(10) 0.0183(4) Uani 1 1 d . . . C2 C 0.28529(12) 0.40912(15) 0.36197(12) 0.0235(5) Uani 1 1 d . . . H2 H 0.3300 0.4333 0.3940 0.028 Uiso 1 1 calc R . . C3 C 0.25822(13) 0.43763(17) 0.29806(13) 0.0286(5) Uani 1 1 d . . . H3 H 0.2796 0.4852 0.2771 0.034 Uiso 1 1 calc R . . C4 C 0.14729(16) 0.3872(2) 0.19958(12) 0.0416(7) Uani 1 1 d . . . H4A H 0.1327 0.3204 0.1837 0.062 Uiso 1 1 calc R . . H4B H 0.1762 0.4169 0.1737 0.062 Uiso 1 1 calc R . . H4C H 0.1019 0.4262 0.1945 0.062 Uiso 1 1 calc R . . C5 C 0.33055(12) 0.17255(15) 0.35964(11) 0.0189(4) Uani 1 1 d . . . C6 C 0.27544(13) 0.15815(16) 0.25290(11) 0.0246(5) Uani 1 1 d . . . H6 H 0.2382 0.1456 0.2112 0.029 Uiso 1 1 calc R . . C7 C 0.34589(14) 0.19162(18) 0.26222(13) 0.0317(6) Uani 1 1 d . . . H7 H 0.3675 0.2059 0.2288 0.038 Uiso 1 1 calc R . . C8 C 0.45736(15) 0.2344(2) 0.36322(15) 0.0451(7) Uani 1 1 d . . . H8A H 0.4568 0.2850 0.3956 0.068 Uiso 1 1 calc R . . H8B H 0.4788 0.2616 0.3308 0.068 Uiso 1 1 calc R . . H8C H 0.4882 0.1789 0.3861 0.068 Uiso 1 1 calc R . . C9 C 0.08684(12) 0.04003(15) 0.34401(11) 0.0198(4) Uani 1 1 d . . . C10 C 0.26750(13) 0.20175(17) 0.54027(11) 0.0248(5) Uani 1 1 d . . . C11 C 0.19477(12) -0.16165(14) 0.30161(10) 0.0161(4) Uani 1 1 d . . . C12 C 0.11799(12) -0.17017(16) 0.26659(10) 0.0190(4) Uani 1 1 d . . . H12 H 0.0835 -0.1246 0.2744 0.023 Uiso 1 1 calc R . . C13 C 0.09115(13) -0.24414(16) 0.22046(10) 0.0212(5) Uani 1 1 d . . . H13 H 0.0386 -0.2493 0.1972 0.025 Uiso 1 1 calc R . . C14 C 0.14071(13) -0.31032(16) 0.20825(11) 0.0221(5) Uani 1 1 d . . . H14 H 0.1223 -0.3603 0.1761 0.027 Uiso 1 1 calc R . . C15 C 0.21689(13) -0.30391(15) 0.24277(11) 0.0229(5) Uani 1 1 d . . . H15 H 0.2509 -0.3499 0.2346 0.027 Uiso 1 1 calc R . . C16 C 0.24397(12) -0.23045(15) 0.28937(10) 0.0200(5) Uani 1 1 d . . . H16 H 0.2965 -0.2268 0.3132 0.024 Uiso 1 1 calc R . . C17 C 0.33063(11) -0.06824(15) 0.38043(11) 0.0180(4) Uani 1 1 d . . . C18 C 0.37924(12) -0.09802(16) 0.44193(11) 0.0246(5) Uani 1 1 d . . . H18 H 0.3594 -0.1177 0.4756 0.030 Uiso 1 1 calc R . . C19 C 0.45710(13) -0.09896(18) 0.45411(13) 0.0324(6) Uani 1 1 d . . . H19 H 0.4900 -0.1194 0.4961 0.039 Uiso 1 1 calc R . . C20 C 0.48650(13) -0.07055(17) 0.40585(13) 0.0319(6) Uani 1 1 d . . . H20 H 0.5395 -0.0718 0.4145 0.038 Uiso 1 1 calc R . . C21 C 0.43901(13) -0.04013(17) 0.34477(13) 0.0278(5) Uani 1 1 d . . . H21 H 0.4593 -0.0192 0.3117 0.033 Uiso 1 1 calc R . . C22 C 0.36147(12) -0.04041(15) 0.33206(11) 0.0207(5) Uani 1 1 d . . . H22 H 0.3289 -0.0213 0.2896 0.025 Uiso 1 1 calc R . . C23 C 0.21529(12) -0.11042(16) 0.43663(10) 0.0188(4) Uani 1 1 d . . . C24 C 0.20896(12) -0.04485(17) 0.48414(11) 0.0241(5) Uani 1 1 d . . . H24 H 0.2083 0.0236 0.4760 0.029 Uiso 1 1 calc R . . C25 C 0.20350(15) -0.07902(18) 0.54369(12) 0.0318(6) Uani 1 1 d . . . H25 H 0.2000 -0.0340 0.5764 0.038 Uiso 1 1 calc R . . C26 C 0.20317(15) -0.17865(18) 0.55509(12) 0.0331(6) Uani 1 1 d . . . H26 H 0.1987 -0.2021 0.5955 0.040 Uiso 1 1 calc R . . C27 C 0.20927(15) -0.24404(18) 0.50805(12) 0.0316(6) Uani 1 1 d . . . H27 H 0.2094 -0.3125 0.5163 0.038 Uiso 1 1 calc R . . C28 C 0.21517(13) -0.21049(17) 0.44877(11) 0.0253(5) Uani 1 1 d . . . H28 H 0.2191 -0.2559 0.4164 0.030 Uiso 1 1 calc R . . C29 C 0.10745(11) 0.44051(15) 0.42272(10) 0.0160(4) Uani 1 1 d . . . C30 C 0.14600(12) 0.51478(15) 0.40195(10) 0.0192(4) Uani 1 1 d . . . H30 H 0.1991 0.5212 0.4221 0.023 Uiso 1 1 calc R . . C31 C 0.10791(12) 0.57856(15) 0.35265(11) 0.0208(5) Uani 1 1 d . . . H31 H 0.1348 0.6278 0.3382 0.025 Uiso 1 1 calc R . . C32 C 0.02980(13) 0.57105(15) 0.32383(11) 0.0224(5) Uani 1 1 d . . . H32 H 0.0034 0.6154 0.2899 0.027 Uiso 1 1 calc R . . C33 C -0.00899(12) 0.49934(16) 0.34462(11) 0.0222(5) Uani 1 1 d . . . H33 H -0.0623 0.4950 0.3254 0.027 Uiso 1 1 calc R . . C34 C 0.02938(12) 0.43332(15) 0.39349(11) 0.0200(5) Uani 1 1 d . . . H34 H 0.0024 0.3832 0.4070 0.024 Uiso 1 1 calc R . . C35 C 0.20145(12) 0.44354(15) 0.55481(10) 0.0184(4) Uani 1 1 d . . . C36 C 0.15574(13) 0.51451(15) 0.56941(11) 0.0227(5) Uani 1 1 d . . . H36 H 0.1035 0.5171 0.5445 0.027 Uiso 1 1 calc R . . C37 C 0.18610(15) 0.58128(16) 0.61996(11) 0.0272(5) Uani 1 1 d . . . H37 H 0.1543 0.6278 0.6307 0.033 Uiso 1 1 calc R . . C38 C 0.26259(15) 0.58040(16) 0.65480(11) 0.0295(6) Uani 1 1 d . . . H38 H 0.2834 0.6273 0.6887 0.035 Uiso 1 1 calc R . . C39 C 0.30883(14) 0.51139(17) 0.64038(11) 0.0280(5) Uani 1 1 d . . . H39 H 0.3614 0.5111 0.6641 0.034 Uiso 1 1 calc R . . C40 C 0.27825(13) 0.44239(16) 0.59113(11) 0.0229(5) Uani 1 1 d . . . H40 H 0.3100 0.3940 0.5821 0.028 Uiso 1 1 calc R . . C41 C 0.09395(12) 0.28359(15) 0.50873(10) 0.0182(4) Uani 1 1 d . . . C42 C 0.06416(14) 0.30539(17) 0.55864(12) 0.0282(5) Uani 1 1 d . . . H42 H 0.0798 0.3632 0.5842 0.034 Uiso 1 1 calc R . . C43 C 0.01196(15) 0.24388(18) 0.57144(13) 0.0342(6) Uani 1 1 d . . . H43 H -0.0076 0.2597 0.6060 0.041 Uiso 1 1 calc R . . C44 C -0.01190(13) 0.16056(17) 0.53510(12) 0.0286(5) Uani 1 1 d . . . H44 H -0.0477 0.1187 0.5443 0.034 Uiso 1 1 calc R . . C45 C 0.01650(14) 0.13777(17) 0.48498(12) 0.0307(6) Uani 1 1 d . . . H45 H -0.0003 0.0804 0.4592 0.037 Uiso 1 1 calc R . . C46 C 0.06969(13) 0.19859(16) 0.47192(12) 0.0267(5) Uani 1 1 d . . . H46 H 0.0895 0.1819 0.4377 0.032 Uiso 1 1 calc R . . C47 C 0.41614(17) 0.9709(3) 0.73867(19) 0.0539(9) Uani 1 1 d . . . C48 C 0.38292(16) 0.9160(3) 0.68141(16) 0.0528(9) Uani 1 1 d . . . H48 H 0.3600 0.9487 0.6405 0.063 Uiso 1 1 calc R . . C49 C 0.38290(17) 0.8157(3) 0.68345(18) 0.0559(9) Uani 1 1 d . . . H49 H 0.3599 0.7792 0.6442 0.067 Uiso 1 1 calc R . . C50 C 0.41637(18) 0.7679(3) 0.74256(19) 0.0618(10) Uani 1 1 d . . . H50 H 0.4161 0.6984 0.7438 0.074 Uiso 1 1 calc R . . C51 C 0.4503(2) 0.8200(4) 0.7999(2) 0.0775(12) Uani 1 1 d . . . H51 H 0.4739 0.7868 0.8405 0.093 Uiso 1 1 calc R . . C52 C 0.44955(19) 0.9200(3) 0.79742(17) 0.0679(11) Uani 1 1 d . . . H52 H 0.4725 0.9560 0.8370 0.081 Uiso 1 1 calc R . . C53 C 0.4169(2) 1.0756(3) 0.7372(2) 0.0694(11) Uani 1 1 d . . . H53A H 0.3819 1.1013 0.7586 0.104 Uiso 1 1 calc R . . H53B H 0.4013 1.0981 0.6911 0.104 Uiso 1 1 calc R . . H53C H 0.4680 1.0993 0.7607 0.104 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 0.01462(8) 0.01550(8) 0.01435(8) -0.00010(6) 0.00531(6) 0.00050(6) Rh2 0.01683(8) 0.01578(8) 0.01211(8) -0.00025(6) 0.00416(6) 0.00166(6) P1 0.0170(3) 0.0161(3) 0.0134(3) 0.0006(2) 0.0057(2) -0.0001(2) P2 0.0197(3) 0.0145(3) 0.0132(3) -0.0005(2) 0.0069(2) 0.0001(2) S1 0.0178(3) 0.0186(3) 0.0244(3) -0.0028(2) 0.0008(2) 0.0025(2) S2 0.0166(3) 0.0237(3) 0.0212(3) -0.0015(2) 0.0044(2) 0.0040(2) N1 0.0192(9) 0.0134(8) 0.0188(9) 0.0007(7) 0.0079(7) 0.0005(7) N2 0.0354(11) 0.0233(10) 0.0200(10) 0.0085(8) 0.0139(9) 0.0091(9) N3 0.0218(9) 0.0159(9) 0.0170(9) 0.0009(7) 0.0101(7) 0.0026(7) N4 0.0253(10) 0.0280(10) 0.0349(12) -0.0013(9) 0.0202(9) -0.0034(8) O1 0.0220(8) 0.0329(9) 0.0309(9) -0.0046(7) 0.0143(7) -0.0057(7) O2 0.0621(13) 0.0388(10) 0.0182(9) 0.0087(8) 0.0101(9) 0.0111(9) C1 0.0232(11) 0.0155(10) 0.0180(11) 0.0008(8) 0.0090(9) 0.0047(9) C2 0.0222(11) 0.0174(11) 0.0350(14) -0.0005(10) 0.0150(10) -0.0005(9) C3 0.0323(13) 0.0218(12) 0.0409(15) 0.0115(11) 0.0244(12) 0.0057(10) C4 0.0542(17) 0.0501(17) 0.0199(13) 0.0149(12) 0.0114(12) 0.0156(14) C5 0.0200(11) 0.0151(10) 0.0250(12) 0.0000(9) 0.0120(9) 0.0014(9) C6 0.0364(13) 0.0215(11) 0.0203(12) 0.0010(9) 0.0154(10) 0.0022(10) C7 0.0419(15) 0.0298(13) 0.0345(15) 0.0017(11) 0.0276(12) -0.0008(11) C8 0.0287(14) 0.0578(19) 0.0534(19) -0.0003(15) 0.0198(13) -0.0148(13) C9 0.0223(11) 0.0184(11) 0.0175(11) -0.0026(9) 0.0047(9) 0.0017(9) C10 0.0292(12) 0.0221(11) 0.0209(12) -0.0025(9) 0.0053(10) 0.0052(10) C11 0.0227(11) 0.0153(10) 0.0119(10) 0.0034(8) 0.0079(8) -0.0006(8) C12 0.0228(11) 0.0208(11) 0.0155(11) 0.0024(8) 0.0091(9) 0.0008(9) C13 0.0246(11) 0.0229(11) 0.0150(11) 0.0026(9) 0.0051(9) -0.0039(9) C14 0.0332(13) 0.0191(11) 0.0159(11) -0.0015(9) 0.0105(10) -0.0074(10) C15 0.0332(13) 0.0164(10) 0.0240(12) 0.0000(9) 0.0161(10) 0.0008(9) C16 0.0219(11) 0.0205(11) 0.0192(11) 0.0023(9) 0.0087(9) -0.0004(9) C17 0.0174(10) 0.0139(10) 0.0212(11) -0.0018(8) 0.0043(9) 0.0011(8) C18 0.0239(11) 0.0231(12) 0.0244(12) 0.0021(9) 0.0046(10) 0.0030(9) C19 0.0228(12) 0.0327(14) 0.0327(14) 0.0002(11) -0.0031(10) 0.0061(11) C20 0.0162(11) 0.0293(13) 0.0474(16) -0.0060(12) 0.0064(11) 0.0015(10) C21 0.0256(12) 0.0233(12) 0.0396(15) -0.0051(11) 0.0176(11) -0.0007(10) C22 0.0213(11) 0.0170(10) 0.0238(12) -0.0018(9) 0.0074(9) 0.0025(9) C23 0.0207(11) 0.0223(11) 0.0136(10) -0.0001(8) 0.0058(8) -0.0011(9) C24 0.0303(12) 0.0238(11) 0.0193(12) -0.0008(9) 0.0098(10) -0.0016(10) C25 0.0463(15) 0.0333(14) 0.0188(12) -0.0057(10) 0.0149(11) -0.0030(12) C26 0.0497(16) 0.0350(14) 0.0189(13) 0.0039(10) 0.0171(12) -0.0039(12) C27 0.0497(16) 0.0250(12) 0.0224(13) 0.0040(10) 0.0150(12) -0.0037(11) C28 0.0354(13) 0.0241(12) 0.0183(12) -0.0005(9) 0.0114(10) -0.0035(10) C29 0.0217(10) 0.0149(10) 0.0130(10) -0.0025(8) 0.0076(8) 0.0026(8) C30 0.0211(11) 0.0195(11) 0.0179(11) -0.0008(9) 0.0077(9) 0.0008(9) C31 0.0279(12) 0.0175(10) 0.0192(11) 0.0002(9) 0.0106(9) 0.0002(9) C32 0.0295(12) 0.0203(11) 0.0142(11) -0.0002(9) 0.0028(9) 0.0057(9) C33 0.0194(11) 0.0231(11) 0.0208(12) -0.0058(9) 0.0022(9) 0.0012(9) C34 0.0233(11) 0.0182(11) 0.0198(11) -0.0023(9) 0.0088(9) -0.0012(9) C35 0.0284(12) 0.0154(10) 0.0136(10) 0.0004(8) 0.0098(9) -0.0038(9) C36 0.0311(12) 0.0192(11) 0.0216(12) 0.0001(9) 0.0141(10) -0.0023(9) C37 0.0494(15) 0.0172(11) 0.0241(12) -0.0013(9) 0.0244(11) -0.0032(11) C38 0.0548(16) 0.0204(11) 0.0149(11) -0.0034(9) 0.0134(11) -0.0116(11) C39 0.0363(13) 0.0275(12) 0.0170(12) -0.0008(10) 0.0045(10) -0.0076(11) C40 0.0318(12) 0.0215(11) 0.0168(11) 0.0004(9) 0.0096(9) -0.0015(10) C41 0.0243(11) 0.0144(10) 0.0170(11) 0.0011(8) 0.0083(9) -0.0003(9) C42 0.0390(14) 0.0222(12) 0.0307(14) -0.0084(10) 0.0212(11) -0.0083(10) C43 0.0443(15) 0.0342(14) 0.0365(15) -0.0064(11) 0.0302(13) -0.0072(12) C44 0.0316(13) 0.0255(12) 0.0329(14) 0.0030(10) 0.0166(11) -0.0064(10) C45 0.0433(15) 0.0242(12) 0.0293(14) -0.0061(10) 0.0182(12) -0.0125(11) C46 0.0381(14) 0.0244(12) 0.0243(13) -0.0064(10) 0.0194(11) -0.0083(10) C47 0.0419(17) 0.060(2) 0.077(3) -0.0055(18) 0.0424(18) -0.0081(16) C48 0.0338(15) 0.089(3) 0.0427(18) 0.0028(17) 0.0219(14) -0.0136(17) C49 0.0416(18) 0.068(2) 0.069(2) -0.0040(19) 0.0319(17) -0.0088(17) C50 0.0430(18) 0.081(3) 0.066(2) 0.004(2) 0.0244(18) 0.0104(18) C51 0.067(3) 0.099(3) 0.070(3) 0.009(3) 0.028(2) 0.032(2) C52 0.0455(19) 0.118(4) 0.039(2) 0.001(2) 0.0114(15) 0.002(2) C53 0.069(2) 0.069(2) 0.083(3) -0.003(2) 0.042(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C9 1.817(2) . ? Rh1 N3 2.0879(17) . ? Rh1 P1 2.2738(7) . ? Rh1 S1 2.3826(7) . ? Rh1 Rh2 3.6177(8) . ? Rh2 C10 1.817(2) . ? Rh2 N1 2.0886(17) . ? Rh2 P2 2.2659(6) . ? Rh2 S2 2.3781(7) . ? P1 C23 1.828(2) . ? P1 C17 1.831(2) . ? P1 C11 1.839(2) . ? P2 C29 1.823(2) . ? P2 C41 1.828(2) . ? P2 C35 1.831(2) . ? S1 C1 1.727(2) . ? S2 C5 1.726(2) . ? N1 C1 1.337(3) . ? N1 C2 1.384(3) . ? N2 C1 1.355(3) . ? N2 C3 1.374(3) . ? N2 C4 1.460(3) . ? N3 C5 1.334(3) . ? N3 C6 1.376(3) . ? N4 C5 1.357(3) . ? N4 C7 1.372(3) . ? N4 C8 1.461(3) . ? O1 C9 1.149(3) . ? O2 C10 1.149(3) . ? C2 C3 1.350(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.349(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C11 C12 1.393(3) . ? C11 C16 1.400(3) . ? C12 C13 1.386(3) . ? C12 H12 0.9500 . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C14 C15 1.379(3) . ? C14 H14 0.9500 . ? C15 C16 1.387(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.393(3) . ? C17 C18 1.393(3) . ? C18 C19 1.396(3) . ? C18 H18 0.9500 . ? C19 C20 1.375(4) . ? C19 H19 0.9500 . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.388(3) . ? C23 C28 1.390(3) . ? C24 C25 1.391(3) . ? C24 H24 0.9500 . ? C25 C26 1.382(3) . ? C25 H25 0.9500 . ? C26 C27 1.377(3) . ? C26 H26 0.9500 . ? C27 C28 1.386(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.394(3) . ? C29 C30 1.399(3) . ? C30 C31 1.373(3) . ? C30 H30 0.9500 . ? C31 C32 1.394(3) . ? C31 H31 0.9500 . ? C32 C33 1.377(3) . ? C32 H32 0.9500 . ? C33 C34 1.389(3) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.394(3) . ? C35 C36 1.395(3) . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 C38 1.383(4) . ? C37 H37 0.9500 . ? C38 C39 1.382(3) . ? C38 H38 0.9500 . ? C39 C40 1.389(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.389(3) . ? C41 C46 1.392(3) . ? C42 C43 1.383(3) . ? C42 H42 0.9500 . ? C43 C44 1.367(3) . ? C43 H43 0.9500 . ? C44 C45 1.379(3) . ? C44 H44 0.9500 . ? C45 C46 1.394(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.392(5) . ? C47 C48 1.396(4) . ? C47 C53 1.430(5) . ? C48 C49 1.370(5) . ? C48 H48 0.9500 . ? C49 C50 1.378(5) . ? C49 H49 0.9500 . ? C50 C51 1.380(5) . ? C50 H50 0.9500 . ? C51 C52 1.366(5) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 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 C9 Rh1 N3 176.55(8) . . ? C9 Rh1 P1 89.70(7) . . ? N3 Rh1 P1 92.75(5) . . ? C9 Rh1 S1 88.62(7) . . ? N3 Rh1 S1 88.91(5) . . ? P1 Rh1 S1 178.24(2) . . ? C9 Rh1 Rh2 106.92(7) . . ? N3 Rh1 Rh2 74.48(5) . . ? P1 Rh1 Rh2 110.55(3) . . ? S1 Rh1 Rh2 70.45(3) . . ? C10 Rh2 N1 177.67(9) . . ? C10 Rh2 P2 88.01(8) . . ? N1 Rh2 P2 93.19(5) . . ? C10 Rh2 S2 89.39(8) . . ? N1 Rh2 S2 89.28(5) . . ? P2 Rh2 S2 175.70(2) . . ? C10 Rh2 Rh1 106.88(7) . . ? N1 Rh2 Rh1 74.45(5) . . ? P2 Rh2 Rh1 113.71(2) . . ? S2 Rh2 Rh1 70.36(3) . . ? C23 P1 C17 102.60(10) . . ? C23 P1 C11 103.11(9) . . ? C17 P1 C11 102.10(10) . . ? C23 P1 Rh1 112.69(7) . . ? C17 P1 Rh1 117.52(7) . . ? C11 P1 Rh1 116.81(7) . . ? C29 P2 C41 104.55(10) . . ? C29 P2 C35 99.94(10) . . ? C41 P2 C35 105.63(10) . . ? C29 P2 Rh2 117.38(7) . . ? C41 P2 Rh2 112.96(7) . . ? C35 P2 Rh2 114.83(7) . . ? C1 S1 Rh1 104.30(7) . . ? C5 S2 Rh2 104.64(8) . . ? C1 N1 C2 106.75(18) . . ? C1 N1 Rh2 126.27(14) . . ? C2 N1 Rh2 126.91(15) . . ? C1 N2 C3 108.33(19) . . ? C1 N2 C4 125.7(2) . . ? C3 N2 C4 125.8(2) . . ? C5 N3 C6 107.43(18) . . ? C5 N3 Rh1 125.43(14) . . ? C6 N3 Rh1 127.09(15) . . ? C5 N4 C7 108.16(19) . . ? C5 N4 C8 125.0(2) . . ? C7 N4 C8 126.8(2) . . ? N1 C1 N2 109.22(19) . . ? N1 C1 S1 126.20(16) . . ? N2 C1 S1 124.55(17) . . ? C3 C2 N1 109.2(2) . . ? C3 C2 H2 125.4 . . ? N1 C2 H2 125.4 . . ? C2 C3 N2 106.5(2) . . ? C2 C3 H3 126.7 . . ? N2 C3 H3 126.7 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N4 108.82(19) . . ? N3 C5 S2 127.05(16) . . ? N4 C5 S2 124.12(17) . . ? C7 C6 N3 108.8(2) . . ? C7 C6 H6 125.6 . . ? N3 C6 H6 125.6 . . ? C6 C7 N4 106.8(2) . . ? C6 C7 H7 126.6 . . ? N4 C7 H7 126.6 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 Rh1 178.3(2) . . ? O2 C10 Rh2 179.3(2) . . ? C12 C11 C16 118.14(19) . . ? C12 C11 P1 119.56(16) . . ? C16 C11 P1 122.30(16) . . ? C13 C12 C11 120.9(2) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.7(2) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? C22 C17 C18 118.6(2) . . ? C22 C17 P1 118.84(16) . . ? C18 C17 P1 122.57(17) . . ? C17 C18 C19 120.0(2) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.6(2) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.1(2) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C17 121.2(2) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? C24 C23 C28 119.4(2) . . ? C24 C23 P1 118.35(17) . . ? C28 C23 P1 122.17(17) . . ? C23 C24 C25 120.2(2) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 119.8(2) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C27 C26 C25 120.2(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C23 120.1(2) . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? C34 C29 C30 118.97(19) . . ? C34 C29 P2 123.74(16) . . ? C30 C29 P2 117.29(16) . . ? C31 C30 C29 120.7(2) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 120.0(2) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 119.9(2) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.4(2) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 120.0(2) . . ? C33 C34 H34 120.0 . . ? C29 C34 H34 120.0 . . ? C40 C35 C36 118.8(2) . . ? C40 C35 P2 119.84(17) . . ? C36 C35 P2 121.31(17) . . ? C37 C36 C35 120.4(2) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.2(2) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 120.1(2) . . ? C39 C38 H38 120.0 . . ? C37 C38 H38 120.0 . . ? C38 C39 C40 119.9(2) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C35 120.6(2) . . ? C39 C40 H40 119.7 . . ? C35 C40 H40 119.7 . . ? C42 C41 C46 118.3(2) . . ? C42 C41 P2 125.67(17) . . ? C46 C41 P2 116.05(16) . . ? C43 C42 C41 120.7(2) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.9(2) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.4(2) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C44 C45 C46 120.3(2) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C41 C46 C45 120.4(2) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C52 C47 C48 117.6(3) . . ? C52 C47 C53 120.9(4) . . ? C48 C47 C53 121.4(4) . . ? C49 C48 C47 120.9(3) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C48 C49 C50 119.9(4) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C51 120.7(4) . . ? C49 C50 H50 119.6 . . ? C51 C50 H50 119.6 . . ? C52 C51 C50 119.0(4) . . ? C52 C51 H51 120.5 . . ? C50 C51 H51 120.5 . . ? C51 C52 C47 122.0(4) . . ? C51 C52 H52 119.0 . . ? C47 C52 H52 119.0 . . ? C47 C53 H53A 109.5 . . ? C47 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C47 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 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 C9 Rh1 Rh2 C10 57.58(10) . . . . ? N3 Rh1 Rh2 C10 -125.71(9) . . . . ? P1 Rh1 Rh2 C10 -38.63(8) . . . . ? S1 Rh1 Rh2 C10 139.83(8) . . . . ? C9 Rh1 Rh2 N1 -124.41(9) . . . . ? N3 Rh1 Rh2 N1 52.30(7) . . . . ? P1 Rh1 Rh2 N1 139.38(5) . . . . ? S1 Rh1 Rh2 N1 -42.16(5) . . . . ? C9 Rh1 Rh2 P2 -37.79(7) . . . . ? N3 Rh1 Rh2 P2 138.92(5) . . . . ? P1 Rh1 Rh2 P2 -134.00(3) . . . . ? S1 Rh1 Rh2 P2 44.46(3) . . . . ? C9 Rh1 Rh2 S2 140.69(7) . . . . ? N3 Rh1 Rh2 S2 -42.60(5) . . . . ? P1 Rh1 Rh2 S2 44.48(2) . . . . ? S1 Rh1 Rh2 S2 -137.06(2) . . . . ? C9 Rh1 P1 C23 -47.42(10) . . . . ? N3 Rh1 P1 C23 135.01(9) . . . . ? S1 Rh1 P1 C23 -63.8(7) . . . . ? Rh2 Rh1 P1 C23 60.56(8) . . . . ? C9 Rh1 P1 C17 -166.41(10) . . . . ? N3 Rh1 P1 C17 16.03(9) . . . . ? S1 Rh1 P1 C17 177(57) . . . . ? Rh2 Rh1 P1 C17 -58.42(8) . . . . ? C9 Rh1 P1 C11 71.71(10) . . . . ? N3 Rh1 P1 C11 -105.86(9) . . . . ? S1 Rh1 P1 C11 55.3(7) . . . . ? Rh2 Rh1 P1 C11 179.69(7) . . . . ? C10 Rh2 P2 C29 -173.56(11) . . . . ? N1 Rh2 P2 C29 8.43(9) . . . . ? S2 Rh2 P2 C29 133.4(3) . . . . ? Rh1 Rh2 P2 C29 -65.98(8) . . . . ? C10 Rh2 P2 C41 -51.78(11) . . . . ? N1 Rh2 P2 C41 130.21(9) . . . . ? S2 Rh2 P2 C41 -104.8(3) . . . . ? Rh1 Rh2 P2 C41 55.80(8) . . . . ? C10 Rh2 P2 C35 69.45(11) . . . . ? N1 Rh2 P2 C35 -108.56(9) . . . . ? S2 Rh2 P2 C35 16.5(3) . . . . ? Rh1 Rh2 P2 C35 177.03(7) . . . . ? C9 Rh1 S1 C1 157.27(10) . . . . ? N3 Rh1 S1 C1 -25.14(9) . . . . ? P1 Rh1 S1 C1 174(11) . . . . ? Rh2 Rh1 S1 C1 48.76(8) . . . . ? C10 Rh2 S2 C5 156.39(10) . . . . ? N1 Rh2 S2 C5 -25.52(9) . . . . ? P2 Rh2 S2 C5 -150.7(3) . . . . ? Rh1 Rh2 S2 C5 48.21(8) . . . . ? C10 Rh2 N1 C1 159(2) . . . . ? P2 Rh2 N1 C1 -80.19(17) . . . . ? S2 Rh2 N1 C1 103.33(16) . . . . ? Rh1 Rh2 N1 C1 33.54(16) . . . . ? C10 Rh2 N1 C2 -18(2) . . . . ? P2 Rh2 N1 C2 103.39(16) . . . . ? S2 Rh2 N1 C2 -73.08(16) . . . . ? Rh1 Rh2 N1 C2 -142.88(17) . . . . ? C9 Rh1 N3 C5 149.3(13) . . . . ? P1 Rh1 N3 C5 -75.53(16) . . . . ? S1 Rh1 N3 C5 105.04(16) . . . . ? Rh2 Rh1 N3 C5 35.05(16) . . . . ? C9 Rh1 N3 C6 -33.8(14) . . . . ? P1 Rh1 N3 C6 101.36(17) . . . . ? S1 Rh1 N3 C6 -78.07(17) . . . . ? Rh2 Rh1 N3 C6 -148.07(18) . . . . ? C2 N1 C1 N2 -1.2(2) . . . . ? Rh2 N1 C1 N2 -178.24(13) . . . . ? C2 N1 C1 S1 177.05(16) . . . . ? Rh2 N1 C1 S1 0.0(3) . . . . ? C3 N2 C1 N1 0.9(2) . . . . ? C4 N2 C1 N1 177.5(2) . . . . ? C3 N2 C1 S1 -177.47(16) . . . . ? C4 N2 C1 S1 -0.9(3) . . . . ? Rh1 S1 C1 N1 -56.62(19) . . . . ? Rh1 S1 C1 N2 121.41(17) . . . . ? C1 N1 C2 C3 1.2(2) . . . . ? Rh2 N1 C2 C3 178.15(15) . . . . ? N1 C2 C3 N2 -0.6(2) . . . . ? C1 N2 C3 C2 -0.1(2) . . . . ? C4 N2 C3 C2 -176.7(2) . . . . ? C6 N3 C5 N4 -1.0(2) . . . . ? Rh1 N3 C5 N4 176.41(13) . . . . ? C6 N3 C5 S2 179.91(16) . . . . ? Rh1 N3 C5 S2 -2.7(3) . . . . ? C7 N4 C5 N3 0.3(2) . . . . ? C8 N4 C5 N3 -178.8(2) . . . . ? C7 N4 C5 S2 179.49(17) . . . . ? C8 N4 C5 S2 0.3(3) . . . . ? Rh2 S2 C5 N3 -54.7(2) . . . . ? Rh2 S2 C5 N4 126.28(18) . . . . ? C5 N3 C6 C7 1.3(2) . . . . ? Rh1 N3 C6 C7 -176.07(15) . . . . ? N3 C6 C7 N4 -1.0(3) . . . . ? C5 N4 C7 C6 0.4(3) . . . . ? C8 N4 C7 C6 179.6(2) . . . . ? N3 Rh1 C9 O1 -39(8) . . . . ? P1 Rh1 C9 O1 -174(100) . . . . ? S1 Rh1 C9 O1 6(7) . . . . ? Rh2 Rh1 C9 O1 75(7) . . . . ? N1 Rh2 C10 O2 48(21) . . . . ? P2 Rh2 C10 O2 -73(19) . . . . ? S2 Rh2 C10 O2 103(19) . . . . ? Rh1 Rh2 C10 O2 173(100) . . . . ? C23 P1 C11 C12 84.53(18) . . . . ? C17 P1 C11 C12 -169.26(16) . . . . ? Rh1 P1 C11 C12 -39.63(18) . . . . ? C23 P1 C11 C16 -95.74(18) . . . . ? C17 P1 C11 C16 10.46(19) . . . . ? Rh1 P1 C11 C16 140.10(15) . . . . ? C16 C11 C12 C13 -0.6(3) . . . . ? P1 C11 C12 C13 179.14(16) . . . . ? C11 C12 C13 C14 -0.5(3) . . . . ? C12 C13 C14 C15 1.1(3) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? C12 C11 C16 C15 1.1(3) . . . . ? P1 C11 C16 C15 -178.62(16) . . . . ? C23 P1 C17 C22 177.10(17) . . . . ? C11 P1 C17 C22 70.50(18) . . . . ? Rh1 P1 C17 C22 -58.69(18) . . . . ? C23 P1 C17 C18 -4.5(2) . . . . ? C11 P1 C17 C18 -111.07(19) . . . . ? Rh1 P1 C17 C18 119.74(17) . . . . ? C22 C17 C18 C19 0.4(3) . . . . ? P1 C17 C18 C19 -178.08(18) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C19 C20 C21 C22 -1.3(4) . . . . ? C20 C21 C22 C17 1.8(3) . . . . ? C18 C17 C22 C21 -1.3(3) . . . . ? P1 C17 C22 C21 177.17(17) . . . . ? C17 P1 C23 C24 96.85(18) . . . . ? C11 P1 C23 C24 -157.33(17) . . . . ? Rh1 P1 C23 C24 -30.50(19) . . . . ? C17 P1 C23 C28 -80.1(2) . . . . ? C11 P1 C23 C28 25.7(2) . . . . ? Rh1 P1 C23 C28 152.54(17) . . . . ? C28 C23 C24 C25 0.8(3) . . . . ? P1 C23 C24 C25 -176.24(18) . . . . ? C23 C24 C25 C26 -1.0(4) . . . . ? C24 C25 C26 C27 0.9(4) . . . . ? C25 C26 C27 C28 -0.5(4) . . . . ? C26 C27 C28 C23 0.3(4) . . . . ? C24 C23 C28 C27 -0.4(4) . . . . ? P1 C23 C28 C27 176.50(19) . . . . ? C41 P2 C29 C34 -8.8(2) . . . . ? C35 P2 C29 C34 -117.91(18) . . . . ? Rh2 P2 C29 C34 117.27(17) . . . . ? C41 P2 C29 C30 172.07(16) . . . . ? C35 P2 C29 C30 62.92(17) . . . . ? Rh2 P2 C29 C30 -61.90(17) . . . . ? C34 C29 C30 C31 -1.3(3) . . . . ? P2 C29 C30 C31 177.96(16) . . . . ? C29 C30 C31 C32 1.5(3) . . . . ? C30 C31 C32 C33 -0.3(3) . . . . ? C31 C32 C33 C34 -1.0(3) . . . . ? C32 C33 C34 C29 1.2(3) . . . . ? C30 C29 C34 C33 -0.1(3) . . . . ? P2 C29 C34 C33 -179.24(16) . . . . ? C29 P2 C35 C40 -132.35(18) . . . . ? C41 P2 C35 C40 119.35(18) . . . . ? Rh2 P2 C35 C40 -5.8(2) . . . . ? C29 P2 C35 C36 44.27(19) . . . . ? C41 P2 C35 C36 -64.02(19) . . . . ? Rh2 P2 C35 C36 170.82(15) . . . . ? C40 C35 C36 C37 -1.2(3) . . . . ? P2 C35 C36 C37 -177.88(16) . . . . ? C35 C36 C37 C38 2.4(3) . . . . ? C36 C37 C38 C39 -1.5(3) . . . . ? C37 C38 C39 C40 -0.5(3) . . . . ? C38 C39 C40 C35 1.6(3) . . . . ? C36 C35 C40 C39 -0.8(3) . . . . ? P2 C35 C40 C39 175.92(17) . . . . ? C29 P2 C41 C42 -91.1(2) . . . . ? C35 P2 C41 C42 13.8(2) . . . . ? Rh2 P2 C41 C42 140.11(19) . . . . ? C29 P2 C41 C46 89.05(18) . . . . ? C35 P2 C41 C46 -166.01(17) . . . . ? Rh2 P2 C41 C46 -39.70(19) . . . . ? C46 C41 C42 C43 0.2(4) . . . . ? P2 C41 C42 C43 -179.58(19) . . . . ? C41 C42 C43 C44 -0.4(4) . . . . ? C42 C43 C44 C45 -0.1(4) . . . . ? C43 C44 C45 C46 0.7(4) . . . . ? C42 C41 C46 C45 0.4(4) . . . . ? P2 C41 C46 C45 -179.79(19) . . . . ? C44 C45 C46 C41 -0.8(4) . . . . ? C52 C47 C48 C49 0.5(4) . . . . ? C53 C47 C48 C49 179.7(3) . . . . ? C47 C48 C49 C50 -0.4(4) . . . . ? C48 C49 C50 C51 -0.3(5) . . . . ? C49 C50 C51 C52 0.8(5) . . . . ? C50 C51 C52 C47 -0.6(6) . . . . ? C48 C47 C52 C51 0.0(5) . . . . ? C53 C47 C52 C51 -179.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.268 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.075 data_6squeeze _database_code_depnum_ccdc_archive 'CCDC 826259' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 N6 O2 P2 Rh2 S2' _chemical_formula_sum 'C48 H46 N6 O2 P2 Rh2 S2' _chemical_formula_weight 1070.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.370(2) _cell_length_b 12.483(3) _cell_length_c 17.364(4) _cell_angle_alpha 94.83(3) _cell_angle_beta 95.12(3) _cell_angle_gamma 102.30(3) _cell_volume 2384.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3642 _cell_measurement_theta_min 2.155 _cell_measurement_theta_max 26.43 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 0.96 _exptl_absorpt_process_details 'SADABS V2008/1' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27239 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10899 _reflns_number_gt 7974 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 159 62 ' ' _platon_squeeze_details ; ; _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^)+(0.0432P)^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_number_reflns 10899 _refine_ls_number_parameters 563 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 0.52083(2) 0.13453(2) 0.232291(15) 0.01247(7) Uani 1 1 d . . . Rh2 Rh 0.55423(2) 0.43166(2) 0.230188(15) 0.01326(7) Uani 1 1 d . . . P1 P 0.35043(8) 0.06041(8) 0.28426(5) 0.01468(19) Uani 1 1 d . . . P2 P 0.74191(8) 0.52542(8) 0.27959(5) 0.0153(2) Uani 1 1 d . . . S1 S 0.70398(8) 0.20736(7) 0.17815(5) 0.01605(19) Uani 1 1 d . . . S2 S 0.35222(8) 0.34305(7) 0.17619(5) 0.01635(19) Uani 1 1 d . . . N1 N 0.6154(3) 0.3791(2) 0.12731(16) 0.0150(6) Uani 1 1 d . . . N2 N 0.5921(3) 0.4259(2) 0.05925(16) 0.0156(6) Uani 1 1 d . . . N3 N 0.6676(3) 0.2805(2) 0.03345(16) 0.0148(6) Uani 1 1 d . . . N4 N 0.4257(3) 0.1563(2) 0.12864(15) 0.0127(6) Uani 1 1 d . . . N5 N 0.4281(3) 0.0884(2) 0.06172(16) 0.0142(6) Uani 1 1 d . . . N6 N 0.3435(3) 0.2256(2) 0.03289(16) 0.0147(6) Uani 1 1 d . . . O1 O 0.6686(3) 0.1079(2) 0.37671(15) 0.0294(7) Uani 1 1 d . . . O2 O 0.4592(2) 0.5128(2) 0.37200(15) 0.0255(6) Uani 1 1 d . . . C1 C 0.6614(3) 0.2917(3) 0.11232(19) 0.0148(7) Uani 1 1 d . . . C2 C 0.6254(3) 0.3648(3) 0.0039(2) 0.0170(8) Uani 1 1 d . . . C3 C 0.6136(4) 0.3827(3) -0.0798(2) 0.0230(9) Uani 1 1 d . . . H3A H 0.5688 0.4406 -0.0873 0.034 Uiso 1 1 calc R . . H3B H 0.5700 0.3141 -0.1106 0.034 Uiso 1 1 calc R . . H3C H 0.6944 0.4052 -0.0967 0.034 Uiso 1 1 calc R . . C4 C 0.7108(3) 0.1928(3) -0.0097(2) 0.0180(8) Uani 1 1 d . . . H4A H 0.6635 0.1732 -0.0616 0.022 Uiso 1 1 calc R . . H4B H 0.6981 0.1263 0.0185 0.022 Uiso 1 1 calc R . . C5 C 0.8438(3) 0.2293(3) -0.0195(2) 0.0239(9) Uani 1 1 d . . . H5A H 0.8563 0.2940 -0.0485 0.036 Uiso 1 1 calc R . . H5B H 0.8705 0.1693 -0.0480 0.036 Uiso 1 1 calc R . . H5C H 0.8908 0.2481 0.0318 0.036 Uiso 1 1 calc R . . C6 C 0.3758(3) 0.2380(3) 0.11190(19) 0.0139(7) Uani 1 1 d . . . C7 C 0.3777(3) 0.1326(3) 0.00525(19) 0.0154(7) Uani 1 1 d . . . C8 C 0.3637(4) 0.0897(3) -0.07866(19) 0.0224(8) Uani 1 1 d . . . H8A H 0.4058 0.0293 -0.0853 0.034 Uiso 1 1 calc R . . H8B H 0.3986 0.1491 -0.1089 0.034 Uiso 1 1 calc R . . H8C H 0.2775 0.0625 -0.0969 0.034 Uiso 1 1 calc R . . C9 C 0.2862(3) 0.2998(3) -0.0120(2) 0.0203(8) Uani 1 1 d . . . H9A H 0.3184 0.3042 -0.0630 0.024 Uiso 1 1 calc R . . H9B H 0.3068 0.3748 0.0162 0.024 Uiso 1 1 calc R . . C10 C 0.1499(4) 0.2595(3) -0.0245(2) 0.0277(9) Uani 1 1 d . . . H10A H 0.1293 0.1856 -0.0530 0.041 Uiso 1 1 calc R . . H10B H 0.1146 0.3101 -0.0547 0.041 Uiso 1 1 calc R . . H10C H 0.1177 0.2568 0.0259 0.041 Uiso 1 1 calc R . . C11 C 0.6104(3) 0.1173(3) 0.3212(2) 0.0199(8) Uani 1 1 d . . . C12 C 0.4965(3) 0.4806(3) 0.3176(2) 0.0182(8) Uani 1 1 d . . . C13 C 0.2064(3) 0.0789(3) 0.2365(2) 0.0179(8) Uani 1 1 d . . . C14 C 0.1269(3) 0.1291(3) 0.2754(2) 0.0213(8) Uani 1 1 d . . . H14 H 0.1466 0.1549 0.3290 0.026 Uiso 1 1 calc R . . C15 C 0.0196(4) 0.1418(3) 0.2367(3) 0.0287(10) Uani 1 1 d . . . H15 H -0.0334 0.1767 0.2638 0.034 Uiso 1 1 calc R . . C16 C -0.0108(4) 0.1040(3) 0.1590(3) 0.0293(10) Uani 1 1 d . . . H16 H -0.0847 0.1122 0.1327 0.035 Uiso 1 1 calc R . . C17 C 0.0668(4) 0.0541(3) 0.1198(2) 0.0283(9) Uani 1 1 d . . . H17 H 0.0459 0.0280 0.0663 0.034 Uiso 1 1 calc R . . C18 C 0.1749(3) 0.0418(3) 0.1574(2) 0.0208(8) Uani 1 1 d . . . H18 H 0.2279 0.0079 0.1295 0.025 Uiso 1 1 calc R . . C19 C 0.3211(3) -0.0891(3) 0.2898(2) 0.0165(7) Uani 1 1 d . . . C20 C 0.4013(4) -0.1322(4) 0.3367(2) 0.0301(10) Uani 1 1 d . . . H20 H 0.4684 -0.0835 0.3668 0.036 Uiso 1 1 calc R . . C21 C 0.3850(4) -0.2447(4) 0.3403(3) 0.0358(11) Uani 1 1 d . . . H21 H 0.4400 -0.2725 0.3734 0.043 Uiso 1 1 calc R . . C22 C 0.2892(4) -0.3165(3) 0.2959(2) 0.0279(9) Uani 1 1 d . . . H22 H 0.2786 -0.3936 0.2987 0.033 Uiso 1 1 calc R . . C23 C 0.2099(4) -0.2783(3) 0.2483(3) 0.0335(10) Uani 1 1 d . . . H23 H 0.1453 -0.3288 0.2173 0.040 Uiso 1 1 calc R . . C24 C 0.2226(4) -0.1643(3) 0.2446(2) 0.0305(10) Uani 1 1 d . . . H24 H 0.1658 -0.1377 0.2121 0.037 Uiso 1 1 calc R . . C25 C 0.3523(3) 0.1197(3) 0.3837(2) 0.0191(8) Uani 1 1 d . . . C26 C 0.3893(4) 0.2329(3) 0.3975(2) 0.0261(9) Uani 1 1 d . . . H26 H 0.4158 0.2747 0.3565 0.031 Uiso 1 1 calc R . . C27 C 0.3884(4) 0.2864(4) 0.4707(2) 0.0327(10) Uani 1 1 d . . . H27 H 0.4165 0.3641 0.4805 0.039 Uiso 1 1 calc R . . C28 C 0.3462(4) 0.2256(4) 0.5289(2) 0.0365(11) Uani 1 1 d . . . H28 H 0.3435 0.2620 0.5788 0.044 Uiso 1 1 calc R . . C29 C 0.3074(4) 0.1121(4) 0.5157(2) 0.0379(11) Uani 1 1 d . . . H29 H 0.2789 0.0708 0.5565 0.046 Uiso 1 1 calc R . . C30 C 0.3105(5) 0.0593(4) 0.4433(2) 0.0371(11) Uani 1 1 d . . . H30 H 0.2840 -0.0186 0.4340 0.045 Uiso 1 1 calc R . . C31 C 0.7675(3) 0.6746(3) 0.27403(19) 0.0177(8) Uani 1 1 d . . . C32 C 0.8836(4) 0.7418(3) 0.2795(2) 0.0304(10) Uani 1 1 d . . . H32 H 0.9524 0.7100 0.2848 0.036 Uiso 1 1 calc R . . C33 C 0.8989(4) 0.8544(4) 0.2773(3) 0.0393(12) Uani 1 1 d . . . H33 H 0.9782 0.8997 0.2806 0.047 Uiso 1 1 calc R . . C34 C 0.7997(4) 0.9009(3) 0.2702(2) 0.0299(10) Uani 1 1 d . . . H34 H 0.8107 0.9784 0.2695 0.036 Uiso 1 1 calc R . . C35 C 0.6849(4) 0.8361(3) 0.2643(2) 0.0244(9) Uani 1 1 d . . . H35 H 0.6166 0.8686 0.2595 0.029 Uiso 1 1 calc R . . C36 C 0.6690(4) 0.7237(3) 0.2654(2) 0.0207(8) Uani 1 1 d . . . H36 H 0.5893 0.6790 0.2601 0.025 Uiso 1 1 calc R . . C37 C 0.7787(3) 0.5095(3) 0.3822(2) 0.0211(8) Uani 1 1 d . . . C38 C 0.8495(4) 0.5918(4) 0.4357(2) 0.0322(10) Uani 1 1 d . . . H38 H 0.8822 0.6620 0.4197 0.039 Uiso 1 1 calc R . . C39 C 0.8725(5) 0.5725(5) 0.5121(2) 0.0441(13) Uani 1 1 d . . . H39 H 0.9205 0.6296 0.5485 0.053 Uiso 1 1 calc R . . C40 C 0.8267(4) 0.4719(5) 0.5355(3) 0.0502(15) Uani 1 1 d . . . H40 H 0.8431 0.4591 0.5881 0.060 Uiso 1 1 calc R . . C41 C 0.7576(5) 0.3896(5) 0.4838(3) 0.0587(17) Uani 1 1 d . . . H41 H 0.7263 0.3193 0.5001 0.070 Uiso 1 1 calc R . . C42 C 0.7332(4) 0.4088(4) 0.4074(3) 0.0440(13) Uani 1 1 d . . . H42 H 0.6841 0.3515 0.3716 0.053 Uiso 1 1 calc R . . C43 C 0.8702(3) 0.4920(3) 0.2338(2) 0.0177(8) Uani 1 1 d . . . C44 C 0.8782(3) 0.5117(3) 0.1565(2) 0.0207(8) Uani 1 1 d . . . H44 H 0.8189 0.5424 0.1296 0.025 Uiso 1 1 calc R . . C45 C 0.9738(4) 0.4863(3) 0.1186(2) 0.0263(9) Uani 1 1 d . . . H45 H 0.9793 0.4997 0.0659 0.032 Uiso 1 1 calc R . . C46 C 1.0598(4) 0.4421(3) 0.1571(3) 0.0291(10) Uani 1 1 d . . . H46 H 1.1243 0.4248 0.1309 0.035 Uiso 1 1 calc R . . C47 C 1.0529(4) 0.4225(3) 0.2344(3) 0.0286(10) Uani 1 1 d . . . H47 H 1.1129 0.3926 0.2612 0.034 Uiso 1 1 calc R . . C48 C 0.9578(3) 0.4469(3) 0.2720(2) 0.0215(8) Uani 1 1 d . . . H48 H 0.9525 0.4327 0.3246 0.026 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 0.01103(14) 0.01389(15) 0.01256(13) 0.00295(10) 0.00161(10) 0.00218(11) Rh2 0.01207(15) 0.01345(15) 0.01434(14) 0.00075(11) 0.00353(10) 0.00242(11) P1 0.0143(5) 0.0144(5) 0.0161(4) 0.0037(4) 0.0039(4) 0.0030(4) P2 0.0147(5) 0.0161(5) 0.0149(4) 0.0019(4) 0.0030(4) 0.0022(4) S1 0.0123(4) 0.0177(5) 0.0194(4) 0.0055(4) 0.0034(3) 0.0040(4) S2 0.0134(4) 0.0150(5) 0.0208(4) 0.0000(4) 0.0028(3) 0.0038(4) N1 0.0135(16) 0.0156(16) 0.0154(14) 0.0029(12) 0.0011(12) 0.0023(13) N2 0.0149(16) 0.0160(16) 0.0164(15) 0.0064(12) 0.0034(12) 0.0022(13) N3 0.0127(15) 0.0162(16) 0.0154(14) 0.0010(12) 0.0032(12) 0.0027(13) N4 0.0124(15) 0.0141(15) 0.0112(13) 0.0008(11) 0.0000(11) 0.0030(12) N5 0.0136(15) 0.0138(15) 0.0144(14) -0.0024(11) 0.0015(12) 0.0028(12) N6 0.0147(16) 0.0140(15) 0.0149(14) 0.0033(12) -0.0002(12) 0.0019(13) O1 0.0266(16) 0.0341(17) 0.0243(15) 0.0118(13) -0.0084(12) 0.0008(13) O2 0.0300(16) 0.0224(15) 0.0254(14) -0.0017(12) 0.0142(12) 0.0057(13) C1 0.0084(17) 0.0174(19) 0.0171(17) 0.0001(14) 0.0029(13) -0.0004(14) C2 0.0134(18) 0.0172(19) 0.0194(18) 0.0052(15) 0.0032(14) -0.0008(15) C3 0.030(2) 0.019(2) 0.0174(18) 0.0061(15) 0.0030(16) -0.0007(17) C4 0.020(2) 0.0137(18) 0.0190(18) -0.0032(14) 0.0037(15) 0.0014(15) C5 0.017(2) 0.026(2) 0.027(2) -0.0030(17) 0.0077(16) 0.0024(17) C6 0.0110(17) 0.0114(17) 0.0171(17) 0.0016(14) 0.0011(13) -0.0025(14) C7 0.0130(18) 0.0159(18) 0.0168(17) 0.0020(14) 0.0020(14) 0.0023(15) C8 0.025(2) 0.026(2) 0.0128(17) -0.0027(15) -0.0018(15) 0.0023(18) C9 0.021(2) 0.0172(19) 0.0222(19) 0.0088(15) -0.0021(15) 0.0024(16) C10 0.019(2) 0.027(2) 0.038(2) 0.0160(19) -0.0037(17) 0.0044(18) C11 0.017(2) 0.0155(19) 0.025(2) 0.0032(15) 0.0049(16) -0.0025(16) C12 0.018(2) 0.0130(18) 0.0232(19) 0.0028(15) 0.0015(15) 0.0027(16) C13 0.0151(19) 0.0142(19) 0.0236(19) 0.0047(15) 0.0042(15) -0.0004(15) C14 0.017(2) 0.0158(19) 0.032(2) 0.0048(16) 0.0052(16) 0.0035(16) C15 0.022(2) 0.012(2) 0.054(3) 0.0095(19) 0.010(2) 0.0031(17) C16 0.012(2) 0.026(2) 0.049(3) 0.016(2) -0.0060(18) -0.0005(17) C17 0.022(2) 0.027(2) 0.029(2) 0.0067(18) -0.0071(17) -0.0081(18) C18 0.0155(19) 0.018(2) 0.027(2) 0.0026(16) 0.0029(16) 0.0003(16) C19 0.0140(18) 0.0179(19) 0.0182(17) 0.0059(14) 0.0036(14) 0.0025(15) C20 0.025(2) 0.028(2) 0.037(2) 0.0051(19) 0.0004(18) 0.0037(19) C21 0.037(3) 0.032(3) 0.042(3) 0.010(2) 0.004(2) 0.016(2) C22 0.029(2) 0.020(2) 0.035(2) 0.0035(18) 0.0009(18) 0.0052(18) C23 0.034(3) 0.022(2) 0.039(2) -0.0022(19) 0.000(2) -0.002(2) C24 0.032(2) 0.027(2) 0.032(2) 0.0042(18) 0.0031(19) 0.004(2) C25 0.023(2) 0.020(2) 0.0154(17) -0.0016(15) 0.0071(15) 0.0074(17) C26 0.031(2) 0.029(2) 0.0149(18) 0.0014(16) 0.0034(16) -0.0025(19) C27 0.042(3) 0.028(2) 0.027(2) -0.0009(18) 0.009(2) 0.003(2) C28 0.053(3) 0.038(3) 0.023(2) 0.0017(19) 0.009(2) 0.019(2) C29 0.052(3) 0.043(3) 0.022(2) 0.009(2) 0.011(2) 0.013(2) C30 0.064(3) 0.024(2) 0.025(2) 0.0030(18) 0.016(2) 0.009(2) C31 0.025(2) 0.0157(19) 0.0114(16) 0.0020(14) 0.0013(14) 0.0021(16) C32 0.019(2) 0.024(2) 0.046(3) 0.0008(19) 0.0090(19) 0.0011(18) C33 0.030(3) 0.022(2) 0.062(3) 0.000(2) 0.017(2) -0.006(2) C34 0.041(3) 0.017(2) 0.031(2) 0.0009(17) 0.014(2) 0.0035(19) C35 0.031(2) 0.023(2) 0.024(2) 0.0064(16) 0.0150(17) 0.0096(18) C36 0.025(2) 0.022(2) 0.0155(18) 0.0024(15) 0.0079(15) 0.0016(17) C37 0.0147(19) 0.032(2) 0.0163(18) 0.0045(16) 0.0027(15) 0.0030(17) C38 0.034(3) 0.038(3) 0.025(2) 0.0025(19) -0.0008(18) 0.011(2) C39 0.045(3) 0.063(4) 0.022(2) -0.006(2) -0.007(2) 0.015(3) C40 0.032(3) 0.096(5) 0.021(2) 0.023(3) 0.001(2) 0.005(3) C41 0.044(3) 0.082(4) 0.039(3) 0.037(3) -0.007(2) -0.016(3) C42 0.043(3) 0.052(3) 0.028(2) 0.017(2) -0.005(2) -0.011(2) C43 0.0131(18) 0.0152(19) 0.0222(18) 0.0005(15) 0.0036(15) -0.0025(15) C44 0.018(2) 0.018(2) 0.0240(19) 0.0007(15) 0.0035(16) 0.0015(16) C45 0.023(2) 0.026(2) 0.027(2) -0.0044(17) 0.0141(17) -0.0029(18) C46 0.018(2) 0.017(2) 0.050(3) -0.0083(19) 0.0124(19) -0.0008(17) C47 0.018(2) 0.020(2) 0.049(3) 0.0046(19) 0.0021(19) 0.0058(18) C48 0.019(2) 0.019(2) 0.027(2) 0.0059(16) 0.0011(16) 0.0024(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C11 1.826(4) . ? Rh1 N4 2.084(3) . ? Rh1 P1 2.2613(12) . ? Rh1 S1 2.3946(12) . ? Rh2 C12 1.817(4) . ? Rh2 N1 2.079(3) . ? Rh2 P2 2.2582(13) . ? Rh2 S2 2.3952(13) . ? P1 C25 1.816(3) . ? P1 C13 1.837(4) . ? P1 C19 1.837(4) . ? P2 C43 1.828(4) . ? P2 C37 1.830(4) . ? P2 C31 1.835(4) . ? S1 C1 1.723(4) . ? S2 C6 1.730(3) . ? N1 C1 1.324(4) . ? N1 N2 1.391(4) . ? N2 C2 1.309(4) . ? N3 C2 1.365(5) . ? N3 C1 1.374(4) . ? N3 C4 1.469(4) . ? N4 C6 1.309(4) . ? N4 N5 1.386(4) . ? N5 C7 1.311(4) . ? N6 C7 1.364(4) . ? N6 C6 1.375(4) . ? N6 C9 1.476(4) . ? O1 C11 1.149(4) . ? O2 C12 1.146(4) . ? C2 C3 1.487(5) . ? C4 C5 1.513(5) . ? C7 C8 1.492(5) . ? C9 C10 1.513(5) . ? C13 C14 1.395(5) . ? C13 C18 1.401(5) . ? C14 C15 1.386(5) . ? C15 C16 1.379(6) . ? C16 C17 1.378(6) . ? C17 C18 1.383(5) . ? C19 C20 1.391(5) . ? C19 C24 1.422(5) . ? C20 C21 1.385(6) . ? C21 C22 1.380(6) . ? C22 C23 1.356(6) . ? C23 C24 1.407(6) . ? C25 C26 1.380(5) . ? C25 C30 1.390(5) . ? C26 C27 1.387(5) . ? C27 C28 1.373(6) . ? C28 C29 1.384(6) . ? C29 C30 1.377(6) . ? C31 C36 1.389(5) . ? C31 C32 1.396(5) . ? C32 C33 1.383(6) . ? C33 C34 1.375(6) . ? C34 C35 1.371(6) . ? C35 C36 1.378(5) . ? C37 C42 1.377(6) . ? C37 C38 1.386(6) . ? C38 C39 1.380(6) . ? C39 C40 1.364(7) . ? C40 C41 1.362(7) . ? C41 C42 1.382(6) . ? C43 C48 1.390(5) . ? C43 C44 1.392(5) . ? C44 C45 1.399(5) . ? C45 C46 1.372(6) . ? C46 C47 1.390(6) . ? C47 C48 1.387(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh1 N4 177.49(14) . . ? C11 Rh1 P1 89.26(12) . . ? N4 Rh1 P1 93.23(8) . . ? C11 Rh1 S1 89.55(12) . . ? N4 Rh1 S1 87.96(8) . . ? P1 Rh1 S1 177.97(4) . . ? C12 Rh2 N1 177.48(14) . . ? C12 Rh2 P2 89.04(12) . . ? N1 Rh2 P2 92.21(9) . . ? C12 Rh2 S2 90.00(12) . . ? N1 Rh2 S2 88.62(9) . . ? P2 Rh2 S2 176.40(4) . . ? C25 P1 C13 103.30(17) . . ? C25 P1 C19 104.66(17) . . ? C13 P1 C19 102.70(17) . . ? C25 P1 Rh1 111.66(13) . . ? C13 P1 Rh1 117.05(12) . . ? C19 P1 Rh1 115.94(12) . . ? C43 P2 C37 103.40(17) . . ? C43 P2 C31 101.60(17) . . ? C37 P2 C31 105.49(17) . . ? C43 P2 Rh2 117.66(12) . . ? C37 P2 Rh2 113.42(13) . . ? C31 P2 Rh2 113.76(13) . . ? C1 S1 Rh1 103.92(12) . . ? C6 S2 Rh2 102.40(12) . . ? C1 N1 N2 110.4(3) . . ? C1 N1 Rh2 128.1(2) . . ? N2 N1 Rh2 120.7(2) . . ? C2 N2 N1 105.6(3) . . ? C2 N3 C1 107.1(3) . . ? C2 N3 C4 127.3(3) . . ? C1 N3 C4 125.6(3) . . ? C6 N4 N5 110.3(3) . . ? C6 N4 Rh1 129.2(2) . . ? N5 N4 Rh1 119.5(2) . . ? C7 N5 N4 105.2(3) . . ? C7 N6 C6 105.8(3) . . ? C7 N6 C9 127.7(3) . . ? C6 N6 C9 126.4(3) . . ? N1 C1 N3 106.4(3) . . ? N1 C1 S1 127.0(3) . . ? N3 C1 S1 126.5(3) . . ? N2 C2 N3 110.5(3) . . ? N2 C2 C3 124.3(3) . . ? N3 C2 C3 125.1(3) . . ? N3 C4 C5 111.1(3) . . ? N4 C6 N6 107.6(3) . . ? N4 C6 S2 127.1(3) . . ? N6 C6 S2 125.3(3) . . ? N5 C7 N6 111.1(3) . . ? N5 C7 C8 124.7(3) . . ? N6 C7 C8 124.2(3) . . ? N6 C9 C10 111.3(3) . . ? O1 C11 Rh1 178.6(3) . . ? O2 C12 Rh2 178.7(3) . . ? C14 C13 C18 118.3(4) . . ? C14 C13 P1 122.9(3) . . ? C18 C13 P1 118.9(3) . . ? C15 C14 C13 120.8(4) . . ? C16 C15 C14 120.3(4) . . ? C17 C16 C15 119.6(4) . . ? C16 C17 C18 120.8(4) . . ? C17 C18 C13 120.3(4) . . ? C20 C19 C24 118.0(4) . . ? C20 C19 P1 119.3(3) . . ? C24 C19 P1 122.6(3) . . ? C21 C20 C19 121.1(4) . . ? C22 C21 C20 120.1(4) . . ? C23 C22 C21 120.8(4) . . ? C22 C23 C24 120.5(4) . . ? C23 C24 C19 119.5(4) . . ? C26 C25 C30 119.4(3) . . ? C26 C25 P1 116.3(3) . . ? C30 C25 P1 124.0(3) . . ? C25 C26 C27 120.6(4) . . ? C28 C27 C26 119.2(4) . . ? C27 C28 C29 120.9(4) . . ? C30 C29 C28 119.6(4) . . ? C29 C30 C25 120.2(4) . . ? C36 C31 C32 118.3(4) . . ? C36 C31 P2 119.6(3) . . ? C32 C31 P2 122.1(3) . . ? C33 C32 C31 120.3(4) . . ? C34 C33 C32 120.1(4) . . ? C35 C34 C33 120.4(4) . . ? C34 C35 C36 119.7(4) . . ? C35 C36 C31 121.2(4) . . ? C42 C37 C38 118.2(4) . . ? C42 C37 P2 117.5(3) . . ? C38 C37 P2 124.3(3) . . ? C39 C38 C37 120.4(4) . . ? C40 C39 C38 120.3(5) . . ? C41 C40 C39 120.3(4) . . ? C40 C41 C42 119.6(5) . . ? C37 C42 C41 121.2(5) . . ? C48 C43 C44 119.1(3) . . ? C48 C43 P2 123.3(3) . . ? C44 C43 P2 117.6(3) . . ? C43 C44 C45 119.8(4) . . ? C46 C45 C44 120.4(4) . . ? C45 C46 C47 120.2(4) . . ? C48 C47 C46 119.5(4) . . ? C47 C48 C43 120.9(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Rh1 P1 C25 46.35(18) . . . . ? N4 Rh1 P1 C25 -133.96(15) . . . . ? S1 Rh1 P1 C25 100.4(10) . . . . ? C11 Rh1 P1 C13 165.08(18) . . . . ? N4 Rh1 P1 C13 -15.22(15) . . . . ? S1 Rh1 P1 C13 -140.8(10) . . . . ? C11 Rh1 P1 C19 -73.39(18) . . . . ? N4 Rh1 P1 C19 106.31(15) . . . . ? S1 Rh1 P1 C19 -19.3(10) . . . . ? C12 Rh2 P2 C43 165.08(18) . . . . ? N1 Rh2 P2 C43 -17.11(16) . . . . ? S2 Rh2 P2 C43 -120.3(5) . . . . ? C12 Rh2 P2 C37 44.27(18) . . . . ? N1 Rh2 P2 C37 -137.93(16) . . . . ? S2 Rh2 P2 C37 118.8(5) . . . . ? C12 Rh2 P2 C31 -76.31(17) . . . . ? N1 Rh2 P2 C31 101.49(15) . . . . ? S2 Rh2 P2 C31 -1.7(6) . . . . ? C11 Rh1 S1 C1 -153.24(17) . . . . ? N4 Rh1 S1 C1 26.99(14) . . . . ? P1 Rh1 S1 C1 152.7(10) . . . . ? C12 Rh2 S2 C6 -154.28(17) . . . . ? N1 Rh2 S2 C6 27.83(15) . . . . ? P2 Rh2 S2 C6 131.2(5) . . . . ? C12 Rh2 N1 C1 -154(3) . . . . ? P2 Rh2 N1 C1 85.9(3) . . . . ? S2 Rh2 N1 C1 -97.6(3) . . . . ? C12 Rh2 N1 N2 14(3) . . . . ? P2 Rh2 N1 N2 -105.3(2) . . . . ? S2 Rh2 N1 N2 71.2(2) . . . . ? C1 N1 N2 C2 -0.2(4) . . . . ? Rh2 N1 N2 C2 -170.7(2) . . . . ? C11 Rh1 N4 C6 -102(3) . . . . ? P1 Rh1 N4 C6 84.9(3) . . . . ? S1 Rh1 N4 C6 -96.7(3) . . . . ? C11 Rh1 N4 N5 66(3) . . . . ? P1 Rh1 N4 N5 -107.2(2) . . . . ? S1 Rh1 N4 N5 71.2(2) . . . . ? C6 N4 N5 C7 -0.2(4) . . . . ? Rh1 N4 N5 C7 -170.2(2) . . . . ? N2 N1 C1 N3 -0.4(4) . . . . ? Rh2 N1 C1 N3 169.2(2) . . . . ? N2 N1 C1 S1 -179.8(3) . . . . ? Rh2 N1 C1 S1 -10.2(5) . . . . ? C2 N3 C1 N1 0.8(4) . . . . ? C4 N3 C1 N1 -178.7(3) . . . . ? C2 N3 C1 S1 -179.7(3) . . . . ? C4 N3 C1 S1 0.7(5) . . . . ? Rh1 S1 C1 N1 60.5(3) . . . . ? Rh1 S1 C1 N3 -118.8(3) . . . . ? N1 N2 C2 N3 0.7(4) . . . . ? N1 N2 C2 C3 178.3(3) . . . . ? C1 N3 C2 N2 -1.0(4) . . . . ? C4 N3 C2 N2 178.6(3) . . . . ? C1 N3 C2 C3 -178.5(3) . . . . ? C4 N3 C2 C3 1.0(6) . . . . ? C2 N3 C4 C5 86.4(4) . . . . ? C1 N3 C4 C5 -94.1(4) . . . . ? N5 N4 C6 N6 0.2(4) . . . . ? Rh1 N4 C6 N6 169.0(2) . . . . ? N5 N4 C6 S2 179.7(3) . . . . ? Rh1 N4 C6 S2 -11.5(5) . . . . ? C7 N6 C6 N4 -0.1(4) . . . . ? C9 N6 C6 N4 -178.9(3) . . . . ? C7 N6 C6 S2 -179.6(3) . . . . ? C9 N6 C6 S2 1.6(5) . . . . ? Rh2 S2 C6 N4 61.5(3) . . . . ? Rh2 S2 C6 N6 -119.1(3) . . . . ? N4 N5 C7 N6 0.2(4) . . . . ? N4 N5 C7 C8 177.9(3) . . . . ? C6 N6 C7 N5 -0.1(4) . . . . ? C9 N6 C7 N5 178.7(3) . . . . ? C6 N6 C7 C8 -177.8(3) . . . . ? C9 N6 C7 C8 1.0(6) . . . . ? C7 N6 C9 C10 86.1(4) . . . . ? C6 N6 C9 C10 -95.4(4) . . . . ? N4 Rh1 C11 O1 22(18) . . . . ? P1 Rh1 C11 O1 -164(15) . . . . ? S1 Rh1 C11 O1 17(15) . . . . ? N1 Rh2 C12 O2 -18(18) . . . . ? P2 Rh2 C12 O2 102(16) . . . . ? S2 Rh2 C12 O2 -74(16) . . . . ? C25 P1 C13 C14 0.3(4) . . . . ? C19 P1 C13 C14 109.0(3) . . . . ? Rh1 P1 C13 C14 -122.8(3) . . . . ? C25 P1 C13 C18 179.9(3) . . . . ? C19 P1 C13 C18 -71.4(3) . . . . ? Rh1 P1 C13 C18 56.8(3) . . . . ? C18 C13 C14 C15 0.0(5) . . . . ? P1 C13 C14 C15 179.6(3) . . . . ? C13 C14 C15 C16 0.5(6) . . . . ? C14 C15 C16 C17 -0.5(6) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? C16 C17 C18 C13 0.6(6) . . . . ? C14 C13 C18 C17 -0.6(6) . . . . ? P1 C13 C18 C17 179.8(3) . . . . ? C25 P1 C19 C20 -59.4(3) . . . . ? C13 P1 C19 C20 -167.0(3) . . . . ? Rh1 P1 C19 C20 64.1(3) . . . . ? C25 P1 C19 C24 124.1(3) . . . . ? C13 P1 C19 C24 16.5(3) . . . . ? Rh1 P1 C19 C24 -112.4(3) . . . . ? C24 C19 C20 C21 -0.9(6) . . . . ? P1 C19 C20 C21 -177.6(3) . . . . ? C19 C20 C21 C22 1.1(6) . . . . ? C20 C21 C22 C23 0.0(7) . . . . ? C21 C22 C23 C24 -1.3(7) . . . . ? C22 C23 C24 C19 1.4(6) . . . . ? C20 C19 C24 C23 -0.3(6) . . . . ? P1 C19 C24 C23 176.2(3) . . . . ? C13 P1 C25 C26 -81.4(3) . . . . ? C19 P1 C25 C26 171.4(3) . . . . ? Rh1 P1 C25 C26 45.2(3) . . . . ? C13 P1 C25 C30 93.4(4) . . . . ? C19 P1 C25 C30 -13.8(4) . . . . ? Rh1 P1 C25 C30 -140.0(3) . . . . ? C30 C25 C26 C27 1.8(6) . . . . ? P1 C25 C26 C27 176.9(3) . . . . ? C25 C26 C27 C28 -2.2(7) . . . . ? C26 C27 C28 C29 1.5(7) . . . . ? C27 C28 C29 C30 -0.4(7) . . . . ? C28 C29 C30 C25 0.0(7) . . . . ? C26 C25 C30 C29 -0.7(7) . . . . ? P1 C25 C30 C29 -175.4(4) . . . . ? C43 P2 C31 C36 147.8(3) . . . . ? C37 P2 C31 C36 -104.6(3) . . . . ? Rh2 P2 C31 C36 20.4(3) . . . . ? C43 P2 C31 C32 -33.2(3) . . . . ? C37 P2 C31 C32 74.4(3) . . . . ? Rh2 P2 C31 C32 -160.7(3) . . . . ? C36 C31 C32 C33 0.8(6) . . . . ? P2 C31 C32 C33 -178.1(3) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C32 C33 C34 C35 -0.9(7) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? C34 C35 C36 C31 1.4(6) . . . . ? C32 C31 C36 C35 -1.8(5) . . . . ? P2 C31 C36 C35 177.2(3) . . . . ? C43 P2 C37 C42 -93.4(4) . . . . ? C31 P2 C37 C42 160.4(4) . . . . ? Rh2 P2 C37 C42 35.2(4) . . . . ? C43 P2 C37 C38 86.4(4) . . . . ? C31 P2 C37 C38 -19.8(4) . . . . ? Rh2 P2 C37 C38 -145.0(3) . . . . ? C42 C37 C38 C39 -0.2(7) . . . . ? P2 C37 C38 C39 179.9(3) . . . . ? C37 C38 C39 C40 0.5(7) . . . . ? C38 C39 C40 C41 -0.1(8) . . . . ? C39 C40 C41 C42 -0.5(9) . . . . ? C38 C37 C42 C41 -0.4(7) . . . . ? P2 C37 C42 C41 179.4(4) . . . . ? C40 C41 C42 C37 0.8(9) . . . . ? C37 P2 C43 C48 9.9(4) . . . . ? C31 P2 C43 C48 119.2(3) . . . . ? Rh2 P2 C43 C48 -115.9(3) . . . . ? C37 P2 C43 C44 -171.0(3) . . . . ? C31 P2 C43 C44 -61.8(3) . . . . ? Rh2 P2 C43 C44 63.1(3) . . . . ? C48 C43 C44 C45 -0.1(5) . . . . ? P2 C43 C44 C45 -179.2(3) . . . . ? C43 C44 C45 C46 0.0(6) . . . . ? C44 C45 C46 C47 -0.2(6) . . . . ? C45 C46 C47 C48 0.6(6) . . . . ? C46 C47 C48 C43 -0.8(6) . . . . ? C44 C43 C48 C47 0.6(6) . . . . ? P2 C43 C48 C47 179.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.065 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.110 data_7 _database_code_depnum_ccdc_archive 'CCDC 826260' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C82 H76 N6 O12 P4 Rh2 S2, C H2 Cl2' _chemical_formula_sum 'C83 H78 Cl2 N6 O12 P4 Rh2 S2' _chemical_formula_weight 1816.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21212 _symmetry_space_group_name_Hall 'P2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 16.991(3) _cell_length_b 19.586(4) _cell_length_c 11.929(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3969.9(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24855 _cell_measurement_theta_min 2.331 _cell_measurement_theta_max 27.468 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.750128 _exptl_absorpt_correction_T_max 0.900000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS 2003)' _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_reflns_number 45315 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9096 _reflns_number_gt 8946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.628 (Bruker, 2005)' _computing_cell_refinement 'Bruker SMART V5.628 (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT V6.41A (Bruker, 2002)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 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. ; _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^)+(0.0414P)^2^+1.3889P] 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 -0.021(14) _refine_ls_number_reflns 9096 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0678 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.122 _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 0.036257(8) 0.122851(7) 0.209199(12) 0.01120(4) Uani 1 1 d . . . P1 P 0.14099(3) 0.18444(3) 0.19057(4) 0.01313(10) Uani 1 1 d . . . P2 P -0.00521(3) 0.18530(3) 0.34661(5) 0.01477(11) Uani 1 1 d . . . S1 S -0.08603(3) 0.06099(2) 0.21916(5) 0.01414(10) Uani 1 1 d . . . N1 N -0.07567(11) -0.05423(9) 0.08768(15) 0.0145(4) Uani 1 1 d . . . N2 N -0.08348(12) -0.07277(10) -0.02433(16) 0.0195(4) Uani 1 1 d . . . N3 N -0.10212(12) 0.03784(9) -0.00772(16) 0.0187(4) Uani 1 1 d . . . O1 O 0.21362(9) 0.15657(8) 0.11448(13) 0.0174(3) Uani 1 1 d . . . O2 O 0.18318(9) 0.20643(8) 0.30610(13) 0.0167(3) Uani 1 1 d . . . O3 O 0.13785(9) 0.25824(8) 0.13052(14) 0.0174(3) Uani 1 1 d . . . O4 O 0.01360(9) 0.15999(9) 0.47330(13) 0.0197(3) Uani 1 1 d . . . O5 O 0.02304(9) 0.26455(8) 0.35016(14) 0.0190(3) Uani 1 1 d . . . O6 O -0.09865(9) 0.19148(8) 0.37146(13) 0.0173(3) Uani 1 1 d . . . C1 C -0.08721(12) 0.01274(11) 0.09779(18) 0.0146(4) Uani 1 1 d . . . C2 C -0.09923(16) -0.01663(12) -0.0783(2) 0.0234(5) Uani 1 1 d . . . C3 C -0.1119(2) -0.01231(14) -0.2022(2) 0.0421(8) Uani 1 1 d . . . H3A H -0.1045 -0.0575 -0.2357 0.063 Uiso 1 1 calc R . . H3B H -0.0741 0.0198 -0.2348 0.063 Uiso 1 1 calc R . . H3C H -0.1656 0.0037 -0.2173 0.063 Uiso 1 1 calc R . . C4 C -0.11455(16) 0.10980(11) -0.0383(2) 0.0223(5) Uani 1 1 d . . . H4A H -0.0899 0.1186 -0.1121 0.027 Uiso 1 1 calc R . . H4B H -0.0881 0.1393 0.0176 0.027 Uiso 1 1 calc R . . C5 C -0.20067(16) 0.12896(14) -0.0442(2) 0.0299(5) Uani 1 1 d . . . H5A H -0.2275 0.0994 -0.0984 0.045 Uiso 1 1 calc R . . H5B H -0.2056 0.1767 -0.0678 0.045 Uiso 1 1 calc R . . H5C H -0.2247 0.1232 0.0299 0.045 Uiso 1 1 calc R . . C6 C 0.25038(13) 0.09342(11) 0.1300(2) 0.0177(4) Uani 1 1 d . . . C7 C 0.25745(14) 0.06274(12) 0.2347(2) 0.0221(5) Uani 1 1 d . . . H7 H 0.2342 0.0829 0.2991 0.026 Uiso 1 1 calc R . . C8 C 0.29959(15) 0.00162(14) 0.2430(2) 0.0280(5) Uani 1 1 d . . . H8 H 0.3041 -0.0204 0.3136 0.034 Uiso 1 1 calc R . . C9 C 0.33486(15) -0.02719(13) 0.1496(3) 0.0291(6) Uani 1 1 d . . . H9 H 0.3645 -0.0681 0.1565 0.035 Uiso 1 1 calc R . . C10 C 0.32663(15) 0.00384(13) 0.0462(2) 0.0287(5) Uani 1 1 d . . . H10 H 0.3503 -0.0162 -0.0180 0.034 Uiso 1 1 calc R . . C11 C 0.28391(14) 0.06433(12) 0.0352(2) 0.0222(5) Uani 1 1 d . . . H11 H 0.2779 0.0853 -0.0361 0.027 Uiso 1 1 calc R . . C12 C 0.24221(13) 0.25569(11) 0.31693(17) 0.0167(4) Uani 1 1 d . . . C13 C 0.22133(15) 0.32415(12) 0.3273(2) 0.0226(5) Uani 1 1 d . . . H13 H 0.1682 0.3382 0.3186 0.027 Uiso 1 1 calc R . . C14 C 0.27992(16) 0.37122(14) 0.3505(2) 0.0282(5) Uani 1 1 d . . . H14 H 0.2665 0.4181 0.3579 0.034 Uiso 1 1 calc R . . C15 C 0.35734(16) 0.35153(14) 0.3629(2) 0.0284(5) Uani 1 1 d . . . H15 H 0.3967 0.3844 0.3799 0.034 Uiso 1 1 calc R . . C16 C 0.37714(15) 0.28304(14) 0.3502(2) 0.0261(5) Uani 1 1 d . . . H16 H 0.4304 0.2691 0.3580 0.031 Uiso 1 1 calc R . . C17 C 0.31963(14) 0.23490(13) 0.3262(2) 0.0226(5) Uani 1 1 d . . . H17 H 0.3333 0.1883 0.3163 0.027 Uiso 1 1 calc R . . C18 C 0.07810(13) 0.28229(11) 0.06099(18) 0.0159(4) Uani 1 1 d . . . C19 C 0.05764(14) 0.35051(12) 0.0760(2) 0.0225(5) Uani 1 1 d . . . H19 H 0.0816 0.3770 0.1333 0.027 Uiso 1 1 calc R . . C20 C 0.00135(16) 0.37920(14) 0.0054(2) 0.0292(5) Uani 1 1 d . . . H20 H -0.0126 0.4259 0.0141 0.035 Uiso 1 1 calc R . . C21 C -0.03433(16) 0.34060(14) -0.0769(2) 0.0287(5) Uani 1 1 d . . . H21 H -0.0724 0.3607 -0.1251 0.034 Uiso 1 1 calc R . . C22 C -0.01426(15) 0.27206(13) -0.0890(2) 0.0252(5) Uani 1 1 d . . . H22 H -0.0394 0.2453 -0.1449 0.030 Uiso 1 1 calc R . . C23 C 0.04251(14) 0.24221(11) -0.01964(19) 0.0202(4) Uani 1 1 d . . . H23 H 0.0563 0.1955 -0.0278 0.024 Uiso 1 1 calc R . . C24 C 0.08195(13) 0.12346(13) 0.49931(18) 0.0190(4) Uani 1 1 d . . . C25 C 0.13591(15) 0.15366(13) 0.5698(2) 0.0252(5) Uani 1 1 d . . . H25 H 0.1264 0.1979 0.5996 0.030 Uiso 1 1 calc R . . C26 C 0.20482(15) 0.11830(15) 0.5967(2) 0.0313(6) Uani 1 1 d . . . H26 H 0.2428 0.1382 0.6451 0.038 Uiso 1 1 calc R . . C27 C 0.21689(15) 0.05426(14) 0.5522(2) 0.0281(5) Uani 1 1 d . . . H27 H 0.2646 0.0309 0.5681 0.034 Uiso 1 1 calc R . . C28 C 0.16232(16) 0.02373(13) 0.4860(2) 0.0282(6) Uani 1 1 d . . . H28 H 0.1710 -0.0214 0.4596 0.034 Uiso 1 1 calc R . . C29 C 0.09389(16) 0.05795(13) 0.4567(2) 0.0234(5) Uani 1 1 d . . . H29 H 0.0561 0.0373 0.4089 0.028 Uiso 1 1 calc R . . C30 C 0.00661(15) 0.30986(11) 0.43793(19) 0.0189(4) Uani 1 1 d . . . C31 C -0.06606(15) 0.34152(12) 0.4457(2) 0.0229(5) Uani 1 1 d . . . H31 H -0.1065 0.3313 0.3934 0.027 Uiso 1 1 calc R . . C32 C -0.07912(16) 0.38871(13) 0.5318(2) 0.0275(5) Uani 1 1 d . . . H32 H -0.1288 0.4106 0.5379 0.033 Uiso 1 1 calc R . . C33 C -0.02059(17) 0.40376(13) 0.6076(2) 0.0292(6) Uani 1 1 d . . . H33 H -0.0300 0.4356 0.6662 0.035 Uiso 1 1 calc R . . C34 C 0.05270(16) 0.37206(14) 0.5981(2) 0.0281(5) Uani 1 1 d . . . H34 H 0.0934 0.3828 0.6497 0.034 Uiso 1 1 calc R . . C35 C 0.06617(15) 0.32512(12) 0.5139(2) 0.0227(5) Uani 1 1 d . . . H35 H 0.1159 0.3033 0.5079 0.027 Uiso 1 1 calc R . . C36 C -0.15210(12) 0.21531(11) 0.2919(2) 0.0183(4) Uani 1 1 d . . . C37 C -0.13066(13) 0.25264(12) 0.1975(2) 0.0224(5) Uani 1 1 d . . . H37 H -0.0768 0.2622 0.1827 0.027 Uiso 1 1 calc R . . C38 C -0.18806(15) 0.27549(13) 0.1261(2) 0.0232(5) Uani 1 1 d . . . H38 H -0.1735 0.3012 0.0619 0.028 Uiso 1 1 calc R . . C39 C -0.26708(15) 0.26187(14) 0.1457(2) 0.0275(5) Uani 1 1 d . . . H39 H -0.3063 0.2787 0.0961 0.033 Uiso 1 1 calc R . . C40 C -0.28789(14) 0.22341(14) 0.2385(2) 0.0264(5) Uani 1 1 d . . . H40 H -0.3417 0.2125 0.2510 0.032 Uiso 1 1 calc R . . C41 C -0.23067(14) 0.20028(12) 0.3144(2) 0.0251(5) Uani 1 1 d . . . H41 H -0.2451 0.1751 0.3793 0.030 Uiso 1 1 calc R . . C43 C 1.0000 0.5000 0.3319(4) 0.074(2) Uani 1 2 d S . . H43A H 1.0080 0.4599 0.3811 0.089 Uiso 0.50 1 calc PR . . H43B H 0.9920 0.5401 0.3811 0.089 Uiso 0.50 1 calc PR . . Cl2 Cl 0.91451(7) 0.48725(6) 0.25492(9) 0.0713(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01188(7) 0.00983(7) 0.01189(7) -0.00015(6) 0.00095(6) -0.00084(5) P1 0.0130(2) 0.0115(2) 0.0149(2) 0.00145(19) 0.00056(19) -0.00119(18) P2 0.0150(2) 0.0140(2) 0.0153(2) 0.0000(2) -0.0002(2) -0.0001(2) S1 0.0138(2) 0.0132(2) 0.0154(2) -0.00214(19) 0.00063(19) -0.00195(17) N1 0.0157(8) 0.0129(8) 0.0150(8) -0.0014(7) -0.0027(7) -0.0011(7) N2 0.0267(10) 0.0156(9) 0.0162(9) -0.0007(7) -0.0065(8) 0.0007(8) N3 0.0285(10) 0.0120(8) 0.0156(9) 0.0010(7) -0.0050(8) 0.0011(8) O1 0.0173(7) 0.0146(7) 0.0203(8) 0.0033(6) 0.0036(6) 0.0007(6) O2 0.0163(7) 0.0170(7) 0.0168(8) 0.0018(6) -0.0008(6) -0.0043(6) O3 0.0178(7) 0.0128(7) 0.0216(8) 0.0038(6) -0.0003(6) -0.0018(6) O4 0.0203(8) 0.0234(8) 0.0153(7) -0.0018(6) -0.0008(6) 0.0028(6) O5 0.0203(8) 0.0161(7) 0.0205(8) -0.0027(6) 0.0013(6) -0.0015(6) O6 0.0166(7) 0.0190(7) 0.0162(7) 0.0004(6) 0.0008(6) 0.0004(6) C1 0.0137(10) 0.0159(10) 0.0142(9) 0.0011(8) -0.0024(7) -0.0007(8) C2 0.0350(13) 0.0176(11) 0.0175(11) -0.0022(9) -0.0082(10) 0.0040(9) C3 0.084(2) 0.0239(12) 0.0184(12) -0.0019(11) -0.0148(15) 0.0127(14) C4 0.0350(13) 0.0118(10) 0.0199(11) 0.0024(8) -0.0043(10) 0.0012(9) C5 0.0380(14) 0.0203(11) 0.0316(13) 0.0003(11) -0.0079(11) 0.0079(11) C6 0.0141(9) 0.0144(10) 0.0245(11) 0.0007(9) 0.0020(9) 0.0003(8) C7 0.0231(11) 0.0170(10) 0.0261(12) 0.0025(9) 0.0018(9) 0.0018(9) C8 0.0295(13) 0.0215(12) 0.0328(13) 0.0055(10) 0.0013(10) 0.0042(10) C9 0.0269(12) 0.0176(11) 0.0429(16) 0.0011(11) 0.0012(11) 0.0058(9) C10 0.0246(12) 0.0232(12) 0.0384(14) -0.0032(11) 0.0104(11) 0.0023(10) C11 0.0213(11) 0.0198(11) 0.0255(12) 0.0013(9) 0.0064(9) -0.0013(9) C12 0.0194(10) 0.0170(10) 0.0138(10) -0.0001(8) -0.0014(8) -0.0056(8) C13 0.0242(11) 0.0206(11) 0.0231(11) -0.0018(9) -0.0027(9) -0.0012(9) C14 0.0374(13) 0.0193(11) 0.0279(12) 0.0017(10) -0.0067(10) -0.0075(11) C15 0.0332(13) 0.0313(13) 0.0208(11) 0.0044(10) -0.0058(10) -0.0177(11) C16 0.0189(11) 0.0388(14) 0.0205(12) 0.0010(10) -0.0034(9) -0.0073(10) C17 0.0213(11) 0.0240(12) 0.0225(11) -0.0002(9) -0.0032(9) -0.0013(9) C18 0.0156(10) 0.0165(10) 0.0155(10) 0.0047(8) 0.0019(8) 0.0005(8) C19 0.0236(12) 0.0161(10) 0.0279(12) 0.0001(9) 0.0030(9) -0.0002(9) C20 0.0282(12) 0.0184(11) 0.0411(14) 0.0071(11) 0.0047(11) 0.0086(11) C21 0.0217(11) 0.0303(13) 0.0341(13) 0.0150(10) -0.0023(11) 0.0016(11) C22 0.0245(12) 0.0261(12) 0.0251(12) 0.0053(10) -0.0049(9) -0.0026(9) C23 0.0218(11) 0.0176(10) 0.0212(10) 0.0010(8) 0.0007(9) -0.0018(9) C24 0.0185(10) 0.0213(10) 0.0172(10) 0.0047(9) -0.0004(8) 0.0016(9) C25 0.0289(12) 0.0198(11) 0.0269(12) 0.0041(10) -0.0037(10) -0.0015(10) C26 0.0234(11) 0.0345(14) 0.0360(14) 0.0162(12) -0.0091(10) -0.0052(11) C27 0.0184(11) 0.0320(13) 0.0340(14) 0.0131(11) 0.0079(10) 0.0049(10) C28 0.0357(14) 0.0255(12) 0.0234(12) 0.0086(10) 0.0066(11) 0.0095(11) C29 0.0300(13) 0.0227(12) 0.0177(11) 0.0005(9) -0.0016(9) 0.0006(10) C30 0.0263(11) 0.0139(10) 0.0164(10) -0.0014(8) 0.0017(9) -0.0022(9) C31 0.0246(11) 0.0174(10) 0.0267(12) -0.0041(10) -0.0015(10) 0.0000(9) C32 0.0296(13) 0.0209(12) 0.0319(13) -0.0046(10) 0.0055(11) 0.0028(10) C33 0.0463(17) 0.0187(11) 0.0227(12) -0.0051(9) 0.0035(11) 0.0002(10) C34 0.0366(14) 0.0253(12) 0.0223(11) -0.0005(10) -0.0072(9) -0.0052(11) C35 0.0217(11) 0.0186(11) 0.0278(12) 0.0017(9) -0.0033(9) -0.0013(9) C36 0.0172(10) 0.0170(10) 0.0205(10) -0.0017(9) -0.0013(9) 0.0033(8) C37 0.0181(10) 0.0268(11) 0.0222(12) -0.0008(10) 0.0035(9) 0.0000(8) C38 0.0245(12) 0.0216(11) 0.0235(12) 0.0020(9) 0.0008(10) 0.0015(9) C39 0.0232(12) 0.0319(13) 0.0273(13) 0.0012(11) -0.0071(10) 0.0048(10) C40 0.0139(10) 0.0321(13) 0.0333(14) -0.0026(11) 0.0008(9) 0.0016(9) C41 0.0193(11) 0.0230(11) 0.0331(14) 0.0005(10) 0.0038(10) -0.0009(9) C43 0.088(4) 0.106(5) 0.028(2) 0.000 0.000 -0.060(4) Cl2 0.0825(7) 0.0740(7) 0.0575(6) 0.0316(5) -0.0123(5) -0.0093(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 N1 2.0872(18) 2 ? Rh1 P1 2.1613(6) . ? Rh1 P2 2.1632(6) . ? Rh1 S1 2.4081(6) . ? Rh1 Rh1 4.9675(10) 2 ? P1 O2 1.6122(17) . ? P1 O3 1.6140(16) . ? P1 O1 1.6262(16) . ? P2 O6 1.6196(17) . ? P2 O4 1.6224(17) . ? P2 O5 1.6254(16) . ? S1 C1 1.729(2) . ? N1 C1 1.332(3) . ? N1 N2 1.391(3) . ? N1 Rh1 2.0872(18) 2 ? N2 C2 1.302(3) . ? N3 C2 1.360(3) . ? N3 C1 1.375(3) . ? N3 C4 1.471(3) . ? O1 C6 1.398(3) . ? O2 C12 1.398(2) . ? O3 C18 1.393(3) . ? O4 C24 1.399(3) . ? O5 C30 1.401(3) . ? O6 C36 1.394(3) . ? C2 C3 1.497(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.512(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.388(3) . ? C6 C7 1.391(3) . ? C7 C8 1.399(3) . ? C7 H7 0.9500 . ? C8 C9 1.386(4) . ? C8 H8 0.9500 . ? C9 C10 1.382(4) . ? C9 H9 0.9500 . ? C10 C11 1.396(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.381(3) . ? C12 C13 1.392(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.379(4) . ? C14 H14 0.9500 . ? C15 C16 1.391(4) . ? C15 H15 0.9500 . ? C16 C17 1.388(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.381(3) . ? C18 C19 1.392(3) . ? C19 C20 1.393(4) . ? C19 H19 0.9500 . ? C20 C21 1.380(4) . ? C20 H20 0.9500 . ? C21 C22 1.392(4) . ? C21 H21 0.9500 . ? C22 C23 1.399(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.377(3) . ? C24 C29 1.395(3) . ? C25 C26 1.398(4) . ? C25 H25 0.9500 . ? C26 C27 1.378(4) . ? C26 H26 0.9500 . ? C27 C28 1.356(4) . ? C27 H27 0.9500 . ? C28 C29 1.387(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.385(3) . ? C30 C35 1.391(3) . ? C31 C32 1.399(3) . ? C31 H31 0.9500 . ? C32 C33 1.376(4) . ? C32 H32 0.9500 . ? C33 C34 1.396(4) . ? C33 H33 0.9500 . ? C34 C35 1.381(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.392(3) . ? C36 C41 1.393(3) . ? C37 C38 1.370(3) . ? C37 H37 0.9500 . ? C38 C39 1.389(4) . ? C38 H38 0.9500 . ? C39 C40 1.386(4) . ? C39 H39 0.9500 . ? C40 C41 1.404(4) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C43 Cl2 1.737(3) . ? C43 Cl2 1.737(3) 2_765 ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? 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 N1 Rh1 P1 91.36(5) 2 . ? N1 Rh1 P2 174.21(5) 2 . ? P1 Rh1 P2 91.75(2) . . ? N1 Rh1 S1 89.26(5) 2 . ? P1 Rh1 S1 175.05(2) . . ? P2 Rh1 S1 88.05(2) . . ? N1 Rh1 Rh1 57.03(5) 2 2 ? P1 Rh1 Rh1 138.151(16) . 2 ? P2 Rh1 Rh1 117.836(17) . 2 ? S1 Rh1 Rh1 45.461(12) . 2 ? O2 P1 O3 98.91(8) . . ? O2 P1 O1 103.26(9) . . ? O3 P1 O1 94.47(8) . . ? O2 P1 Rh1 115.30(6) . . ? O3 P1 Rh1 121.22(6) . . ? O1 P1 Rh1 119.66(6) . . ? O6 P2 O4 92.60(8) . . ? O6 P2 O5 102.31(9) . . ? O4 P2 O5 102.08(9) . . ? O6 P2 Rh1 120.02(6) . . ? O4 P2 Rh1 117.97(7) . . ? O5 P2 Rh1 117.61(6) . . ? C1 S1 Rh1 104.11(7) . . ? C1 N1 N2 109.28(18) . . ? C1 N1 Rh1 128.21(15) . 2 ? N2 N1 Rh1 121.98(14) . 2 ? C2 N2 N1 105.89(18) . . ? C2 N3 C1 106.22(18) . . ? C2 N3 C4 127.10(19) . . ? C1 N3 C4 126.61(18) . . ? C6 O1 P1 124.22(14) . . ? C12 O2 P1 125.63(14) . . ? C18 O3 P1 126.24(14) . . ? C24 O4 P2 121.76(14) . . ? C30 O5 P2 124.45(14) . . ? C36 O6 P2 122.63(14) . . ? N1 C1 N3 107.24(18) . . ? N1 C1 S1 127.78(17) . . ? N3 C1 S1 124.97(16) . . ? N2 C2 N3 111.4(2) . . ? N2 C2 C3 124.5(2) . . ? N3 C2 C3 124.2(2) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 112.8(2) . . ? N3 C4 H4A 109.0 . . ? C5 C4 H4A 109.0 . . ? N3 C4 H4B 109.0 . . ? C5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 121.2(2) . . ? C11 C6 O1 116.0(2) . . ? C7 C6 O1 122.6(2) . . ? C6 C7 C8 118.5(2) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? C9 C8 C7 120.9(2) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C9 C10 C11 120.7(2) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 119.0(2) . . ? C6 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C17 C12 C13 121.3(2) . . ? C17 C12 O2 119.2(2) . . ? C13 C12 O2 119.3(2) . . ? C14 C13 C12 118.4(2) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C15 C14 C13 121.4(2) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 119.3(2) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 120.5(2) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C12 C17 C16 119.1(2) . . ? C12 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C23 C18 C19 121.7(2) . . ? C23 C18 O3 122.8(2) . . ? C19 C18 O3 115.5(2) . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C21 C20 C19 120.7(2) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 120.7(2) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 118.5(2) . . ? C18 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C25 C24 C29 121.4(2) . . ? C25 C24 O4 117.9(2) . . ? C29 C24 O4 120.7(2) . . ? C24 C25 C26 119.0(2) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 119.1(2) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 121.6(2) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 120.4(2) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C24 118.4(2) . . ? C28 C29 H29 120.8 . . ? C24 C29 H29 120.8 . . ? C31 C30 C35 120.6(2) . . ? C31 C30 O5 120.8(2) . . ? C35 C30 O5 118.6(2) . . ? C30 C31 C32 119.1(2) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 120.6(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.7(2) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 120.2(2) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C30 119.8(2) . . ? C34 C35 H35 120.1 . . ? C30 C35 H35 120.1 . . ? C37 C36 C41 121.2(2) . . ? C37 C36 O6 123.80(19) . . ? C41 C36 O6 115.0(2) . . ? C38 C37 C36 119.2(2) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 121.4(2) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C40 C39 C38 119.0(2) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C39 C40 C41 121.0(2) . . ? C39 C40 H40 119.5 . . ? C41 C40 H40 119.5 . . ? C36 C41 C40 118.1(2) . . ? C36 C41 H41 120.9 . . ? C40 C41 H41 120.9 . . ? Cl2 C43 Cl2 116.1(3) . 2_765 ? Cl2 C43 H43A 108.3 . . ? Cl2 C43 H43A 108.3 2_765 . ? Cl2 C43 H43B 108.3 . . ? Cl2 C43 H43B 108.3 2_765 . ? H43A C43 H43B 107.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Rh1 P1 O2 -132.70(8) 2 . . . ? P2 Rh1 P1 O2 42.42(7) . . . . ? S1 Rh1 P1 O2 130.1(2) . . . . ? Rh1 Rh1 P1 O2 -94.83(7) 2 . . . ? N1 Rh1 P1 O3 108.17(9) 2 . . . ? P2 Rh1 P1 O3 -76.71(8) . . . . ? S1 Rh1 P1 O3 11.0(3) . . . . ? Rh1 Rh1 P1 O3 146.04(7) 2 . . . ? N1 Rh1 P1 O1 -8.57(9) 2 . . . ? P2 Rh1 P1 O1 166.55(7) . . . . ? S1 Rh1 P1 O1 -105.8(2) . . . . ? Rh1 Rh1 P1 O1 29.30(8) 2 . . . ? N1 Rh1 P2 O6 -84.8(5) 2 . . . ? P1 Rh1 P2 O6 152.67(7) . . . . ? S1 Rh1 P2 O6 -22.38(7) . . . . ? Rh1 Rh1 P2 O6 -58.13(7) 2 . . . ? N1 Rh1 P2 O4 26.7(5) 2 . . . ? P1 Rh1 P2 O4 -95.84(8) . . . . ? S1 Rh1 P2 O4 89.11(7) . . . . ? Rh1 Rh1 P2 O4 53.36(8) 2 . . . ? N1 Rh1 P2 O5 149.7(5) 2 . . . ? P1 Rh1 P2 O5 27.21(7) . . . . ? S1 Rh1 P2 O5 -147.85(7) . . . . ? Rh1 Rh1 P2 O5 176.40(7) 2 . . . ? N1 Rh1 S1 C1 -17.14(9) 2 . . . ? P1 Rh1 S1 C1 80.2(2) . . . . ? P2 Rh1 S1 C1 167.98(8) . . . . ? Rh1 Rh1 S1 C1 -58.47(7) 2 . . . ? C1 N1 N2 C2 0.2(3) . . . . ? Rh1 N1 N2 C2 -172.13(17) 2 . . . ? O2 P1 O1 C6 75.29(18) . . . . ? O3 P1 O1 C6 175.55(17) . . . . ? Rh1 P1 O1 C6 -54.45(18) . . . . ? O3 P1 O2 C12 -36.72(18) . . . . ? O1 P1 O2 C12 60.06(18) . . . . ? Rh1 P1 O2 C12 -167.59(15) . . . . ? O2 P1 O3 C18 -144.81(17) . . . . ? O1 P1 O3 C18 111.00(18) . . . . ? Rh1 P1 O3 C18 -17.9(2) . . . . ? O6 P2 O4 C24 158.00(17) . . . . ? O5 P2 O4 C24 -98.81(17) . . . . ? Rh1 P2 O4 C24 31.76(19) . . . . ? O6 P2 O5 C30 51.61(19) . . . . ? O4 P2 O5 C30 -43.80(19) . . . . ? Rh1 P2 O5 C30 -174.59(15) . . . . ? O4 P2 O6 C36 177.13(16) . . . . ? O5 P2 O6 C36 74.16(17) . . . . ? Rh1 P2 O6 C36 -58.22(17) . . . . ? N2 N1 C1 N3 -0.3(2) . . . . ? Rh1 N1 C1 N3 171.37(15) 2 . . . ? N2 N1 C1 S1 178.61(16) . . . . ? Rh1 N1 C1 S1 -9.7(3) 2 . . . ? C2 N3 C1 N1 0.3(2) . . . . ? C4 N3 C1 N1 -176.8(2) . . . . ? C2 N3 C1 S1 -178.62(18) . . . . ? C4 N3 C1 S1 4.3(3) . . . . ? Rh1 S1 C1 N1 106.27(19) . . . . ? Rh1 S1 C1 N3 -74.99(19) . . . . ? N1 N2 C2 N3 0.1(3) . . . . ? N1 N2 C2 C3 179.6(3) . . . . ? C1 N3 C2 N2 -0.2(3) . . . . ? C4 N3 C2 N2 176.9(2) . . . . ? C1 N3 C2 C3 -179.8(3) . . . . ? C4 N3 C2 C3 -2.7(4) . . . . ? C2 N3 C4 C5 87.4(3) . . . . ? C1 N3 C4 C5 -96.0(3) . . . . ? P1 O1 C6 C11 152.14(17) . . . . ? P1 O1 C6 C7 -31.5(3) . . . . ? C11 C6 C7 C8 0.2(4) . . . . ? O1 C6 C7 C8 -176.0(2) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C8 C9 C10 C11 0.7(4) . . . . ? C7 C6 C11 C10 -1.2(4) . . . . ? O1 C6 C11 C10 175.3(2) . . . . ? C9 C10 C11 C6 0.7(4) . . . . ? P1 O2 C12 C17 -100.5(2) . . . . ? P1 O2 C12 C13 84.7(2) . . . . ? C17 C12 C13 C14 -1.8(3) . . . . ? O2 C12 C13 C14 172.9(2) . . . . ? C12 C13 C14 C15 0.2(4) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C13 C12 C17 C16 2.3(3) . . . . ? O2 C12 C17 C16 -172.4(2) . . . . ? C15 C16 C17 C12 -1.1(4) . . . . ? P1 O3 C18 C23 -41.8(3) . . . . ? P1 O3 C18 C19 139.82(18) . . . . ? C23 C18 C19 C20 -1.8(4) . . . . ? O3 C18 C19 C20 176.6(2) . . . . ? C18 C19 C20 C21 0.9(4) . . . . ? C19 C20 C21 C22 0.5(4) . . . . ? C20 C21 C22 C23 -0.9(4) . . . . ? C19 C18 C23 C22 1.4(3) . . . . ? O3 C18 C23 C22 -176.9(2) . . . . ? C21 C22 C23 C18 0.0(4) . . . . ? P2 O4 C24 C25 115.4(2) . . . . ? P2 O4 C24 C29 -65.9(3) . . . . ? C29 C24 C25 C26 1.5(4) . . . . ? O4 C24 C25 C26 -179.8(2) . . . . ? C24 C25 C26 C27 0.0(4) . . . . ? C25 C26 C27 C28 -2.4(4) . . . . ? C26 C27 C28 C29 3.2(4) . . . . ? C27 C28 C29 C24 -1.6(4) . . . . ? C25 C24 C29 C28 -0.7(4) . . . . ? O4 C24 C29 C28 -179.4(2) . . . . ? P2 O5 C30 C31 -80.0(3) . . . . ? P2 O5 C30 C35 103.3(2) . . . . ? C35 C30 C31 C32 -0.6(4) . . . . ? O5 C30 C31 C32 -177.2(2) . . . . ? C30 C31 C32 C33 0.2(4) . . . . ? C31 C32 C33 C34 0.5(4) . . . . ? C32 C33 C34 C35 -0.9(4) . . . . ? C33 C34 C35 C30 0.5(4) . . . . ? C31 C30 C35 C34 0.2(4) . . . . ? O5 C30 C35 C34 177.0(2) . . . . ? P2 O6 C36 C37 -18.0(3) . . . . ? P2 O6 C36 C41 163.26(17) . . . . ? C41 C36 C37 C38 0.6(4) . . . . ? O6 C36 C37 C38 -178.0(2) . . . . ? C36 C37 C38 C39 -0.4(4) . . . . ? C37 C38 C39 C40 -1.0(4) . . . . ? C38 C39 C40 C41 2.2(4) . . . . ? C37 C36 C41 C40 0.5(4) . . . . ? O6 C36 C41 C40 179.3(2) . . . . ? C39 C40 C41 C36 -1.9(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.508 _refine_diff_density_min -0.625 _refine_diff_density_rms 0.128 data_9 _database_code_depnum_ccdc_archive 'CCDC 826261' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H52 N6 Rh3 S2, F6 P' _chemical_formula_sum 'C34 H52 F6 N6 P Rh3 S2' _chemical_formula_weight 1062.64 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall 'P 2ybc' 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 8.3024(17) _cell_length_b 21.086(4) _cell_length_c 21.516(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.42(3) _cell_angle_gamma 90.00 _cell_volume 3760.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9792 _cell_measurement_theta_min 2.152 _cell_measurement_theta_max 27.4645 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 1.521 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.666 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details 'SADABS V2.03' _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-AXS D8' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 41346 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8591 _reflns_number_gt 7438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_cell_refinement 'SMART v5.628 (Bruker-AXS, 1997-2002)' _computing_data_reduction 'SAINT v7.06A (Bruker-AXS, 1997-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V6.14' _computing_publication_material 'Bruker SHELXTL V6.14' _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^)+(0.0402P)^2^+4.6215P] 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_number_reflns 8591 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.68814(3) 0.607379(12) 0.345484(12) 0.01024(7) Uani 1 1 d . . . Rh2 Rh 0.29648(3) 0.478795(12) 0.195497(12) 0.01079(7) Uani 1 1 d . . . Rh3 Rh 0.50921(3) 0.468615(12) 0.329232(12) 0.01035(7) Uani 1 1 d . . . S1 S 0.41315(10) 0.57234(4) 0.34452(4) 0.01090(16) Uani 1 1 d . . . S2 S 0.57775(10) 0.48285(4) 0.22580(4) 0.01126(17) Uani 1 1 d . . . N1 N 0.2731(4) 0.57274(13) 0.22358(13) 0.0129(6) Uani 1 1 d . . . N2 N 0.1953(4) 0.61595(14) 0.18296(14) 0.0146(6) Uani 1 1 d . . . N3 N 0.2677(4) 0.66388(13) 0.27149(14) 0.0129(6) Uani 1 1 d . . . N4 N 0.6847(4) 0.60471(14) 0.24855(13) 0.0128(6) Uani 1 1 d . . . N5 N 0.7324(4) 0.65720(14) 0.21399(14) 0.0145(6) Uani 1 1 d . . . N6 N 0.6360(4) 0.58295(13) 0.14955(13) 0.0114(6) Uani 1 1 d . . . C1 C 0.3174(4) 0.60242(16) 0.27642(16) 0.0128(7) Uani 1 1 d . . . C2 C 0.1953(4) 0.67024(16) 0.21266(16) 0.0135(7) Uani 1 1 d . . . C3 C 0.1241(5) 0.73026(17) 0.18705(18) 0.0184(8) Uani 1 1 d . . . H3A H 0.1076 0.7268 0.1417 0.028 Uiso 1 1 calc R . . H3B H 0.1975 0.7656 0.1975 0.028 Uiso 1 1 calc R . . H3C H 0.0203 0.7380 0.2051 0.028 Uiso 1 1 calc R . . C4 C 0.2871(4) 0.71266(16) 0.31996(17) 0.0140(7) Uani 1 1 d . . . H4A H 0.2841 0.6923 0.3613 0.017 Uiso 1 1 calc R . . H4B H 0.1956 0.7427 0.3154 0.017 Uiso 1 1 calc R . . C5 C 0.4435(5) 0.74890(17) 0.31680(18) 0.0176(8) Uani 1 1 d . . . H5A H 0.5347 0.7195 0.3227 0.026 Uiso 1 1 calc R . . H5B H 0.4505 0.7812 0.3496 0.026 Uiso 1 1 calc R . . H5C H 0.4468 0.7694 0.2760 0.026 Uiso 1 1 calc R . . C6 C 0.6299(4) 0.56081(16) 0.20882(15) 0.0114(7) Uani 1 1 d . . . C7 C 0.7026(4) 0.64239(16) 0.15533(16) 0.0138(7) Uani 1 1 d . . . C8 C 0.7416(5) 0.68281(17) 0.10120(17) 0.0174(8) Uani 1 1 d . . . H8A H 0.7819 0.7240 0.1163 0.026 Uiso 1 1 calc R . . H8B H 0.6441 0.6890 0.0739 0.026 Uiso 1 1 calc R . . H8C H 0.8243 0.6619 0.0779 0.026 Uiso 1 1 calc R . . C9 C 0.5742(4) 0.55091(17) 0.09212(16) 0.0140(7) Uani 1 1 d . . . H9A H 0.5536 0.5829 0.0589 0.017 Uiso 1 1 calc R . . H9B H 0.4704 0.5300 0.0997 0.017 Uiso 1 1 calc R . . C10 C 0.6913(5) 0.50181(18) 0.07021(17) 0.0190(8) Uani 1 1 d . . . H10A H 0.7907 0.5228 0.0589 0.028 Uiso 1 1 calc R . . H10B H 0.6424 0.4795 0.0338 0.028 Uiso 1 1 calc R . . H10C H 0.7166 0.4713 0.1037 0.028 Uiso 1 1 calc R . . C11 C 0.9087(4) 0.66023(18) 0.34970(17) 0.0170(7) Uani 1 1 d . . . H11 H 0.9317 0.6820 0.3099 0.020 Uiso 1 1 calc R . . C12 C 0.9426(4) 0.59565(18) 0.35031(17) 0.0168(7) Uani 1 1 d . . . H12 H 0.9867 0.5794 0.3111 0.020 Uiso 1 1 calc R . . C13 C 0.9963(5) 0.55855(19) 0.40807(18) 0.0199(8) Uani 1 1 d . . . H13A H 1.1105 0.5688 0.4197 0.024 Uiso 1 1 calc R . . H13B H 0.9898 0.5127 0.3986 0.024 Uiso 1 1 calc R . . C14 C 0.8931(4) 0.57289(18) 0.46405(17) 0.0173(7) Uani 1 1 d . . . H14A H 0.8920 0.5351 0.4913 0.021 Uiso 1 1 calc R . . H14B H 0.9430 0.6082 0.4886 0.021 Uiso 1 1 calc R . . C15 C 0.7210(4) 0.59049(17) 0.44342(16) 0.0149(7) Uani 1 1 d . . . H15 H 0.6381 0.5617 0.4600 0.018 Uiso 1 1 calc R . . C16 C 0.6675(4) 0.65227(17) 0.43369(16) 0.0139(7) Uani 1 1 d . . . H16 H 0.5536 0.6595 0.4447 0.017 Uiso 1 1 calc R . . C17 C 0.7725(5) 0.71075(17) 0.43910(17) 0.0185(8) Uani 1 1 d . . . H17A H 0.7963 0.7206 0.4837 0.022 Uiso 1 1 calc R . . H17B H 0.7127 0.7471 0.4199 0.022 Uiso 1 1 calc R . . C18 C 0.9315(5) 0.70237(17) 0.40743(17) 0.0183(8) Uani 1 1 d . . . H18A H 0.9723 0.7444 0.3952 0.022 Uiso 1 1 calc R . . H18B H 1.0128 0.6830 0.4372 0.022 Uiso 1 1 calc R . . C19 C 0.0397(4) 0.47210(18) 0.19195(18) 0.0190(8) Uani 1 1 d . . . H19 H -0.0147 0.5080 0.2128 0.023 Uiso 1 1 calc R . . C20 C 0.0877(5) 0.48623(18) 0.13237(18) 0.0176(8) Uani 1 1 d . . . H20 H 0.0625 0.5307 0.1189 0.021 Uiso 1 1 calc R . . C21 C 0.0870(5) 0.43910(17) 0.07851(17) 0.0176(7) Uani 1 1 d . . . H21A H 0.0576 0.4615 0.0390 0.021 Uiso 1 1 calc R . . H21B H 0.0042 0.4062 0.0844 0.021 Uiso 1 1 calc R . . C22 C 0.2519(5) 0.40719(18) 0.07393(17) 0.0174(7) Uani 1 1 d . . . H22A H 0.2362 0.3650 0.0543 0.021 Uiso 1 1 calc R . . H22B H 0.3181 0.4330 0.0467 0.021 Uiso 1 1 calc R . . C23 C 0.3423(4) 0.39917(16) 0.13648(17) 0.0145(7) Uani 1 1 d . . . H23 H 0.4592 0.3887 0.1340 0.017 Uiso 1 1 calc R . . C24 C 0.2747(4) 0.37707(16) 0.19014(17) 0.0148(7) Uani 1 1 d . . . H24 H 0.3526 0.3539 0.2192 0.018 Uiso 1 1 calc R . . C25 C 0.1020(5) 0.35434(18) 0.19221(19) 0.0204(8) Uani 1 1 d . . . H25A H 0.0983 0.3178 0.2210 0.024 Uiso 1 1 calc R . . H25B H 0.0630 0.3398 0.1502 0.024 Uiso 1 1 calc R . . C26 C -0.0093(5) 0.40681(19) 0.2139(2) 0.0224(8) Uani 1 1 d . . . H26A H -0.1212 0.3979 0.1978 0.027 Uiso 1 1 calc R . . H26B H -0.0075 0.4066 0.2599 0.027 Uiso 1 1 calc R . . C27 C 0.5721(4) 0.37028(16) 0.31678(16) 0.0147(7) Uani 1 1 d . . . H27 H 0.5924 0.3588 0.2728 0.018 Uiso 1 1 calc R . . C28 C 0.7001(4) 0.40199(17) 0.34804(17) 0.0154(7) Uani 1 1 d . . . H28 H 0.7951 0.4086 0.3223 0.018 Uiso 1 1 calc R . . C29 C 0.7432(5) 0.39766(18) 0.41696(18) 0.0195(8) Uani 1 1 d . . . H29A H 0.8221 0.4314 0.4289 0.023 Uiso 1 1 calc R . . H29B H 0.7956 0.3563 0.4262 0.023 Uiso 1 1 calc R . . C30 C 0.5960(5) 0.40445(18) 0.45640(17) 0.0181(8) Uani 1 1 d . . . H30A H 0.5480 0.3621 0.4625 0.022 Uiso 1 1 calc R . . H30B H 0.6313 0.4215 0.4979 0.022 Uiso 1 1 calc R . . C31 C 0.4692(5) 0.44814(17) 0.42583(16) 0.0152(7) Uani 1 1 d . . . H31 H 0.4458 0.4865 0.4511 0.018 Uiso 1 1 calc R . . C32 C 0.3381(5) 0.42746(17) 0.38715(16) 0.0151(7) Uani 1 1 d . . . H32 H 0.2380 0.4533 0.3905 0.018 Uiso 1 1 calc R . . C33 C 0.3071(5) 0.35962(17) 0.36835(18) 0.0181(8) Uani 1 1 d . . . H33A H 0.2228 0.3587 0.3338 0.022 Uiso 1 1 calc R . . H33B H 0.2648 0.3365 0.4040 0.022 Uiso 1 1 calc R . . C34 C 0.4572(5) 0.32507(17) 0.34764(18) 0.0183(8) Uani 1 1 d . . . H34A H 0.5144 0.3051 0.3843 0.022 Uiso 1 1 calc R . . H34B H 0.4238 0.2910 0.3179 0.022 Uiso 1 1 calc R . . P1 P 0.72285(12) 0.30620(5) 0.00400(5) 0.0172(2) Uani 1 1 d . . . F1 F 0.8981(3) 0.28587(13) -0.01470(12) 0.0323(6) Uani 1 1 d . . . F2 F 0.7919(3) 0.32009(11) 0.07410(11) 0.0259(5) Uani 1 1 d . . . F3 F 0.6868(3) 0.23440(11) 0.02377(12) 0.0334(6) Uani 1 1 d . . . F4 F 0.7587(4) 0.37743(11) -0.01517(12) 0.0353(6) Uani 1 1 d . . . F5 F 0.6521(3) 0.29173(12) -0.06558(11) 0.0292(6) Uani 1 1 d . . . F6 F 0.5470(3) 0.32661(14) 0.02289(12) 0.0377(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.00764(13) 0.01302(13) 0.01010(13) -0.00011(9) 0.00078(10) -0.00104(10) Rh2 0.00812(13) 0.01078(13) 0.01342(13) -0.00177(10) 0.00025(10) 0.00041(10) Rh3 0.00974(14) 0.01029(13) 0.01120(13) 0.00097(9) 0.00214(10) 0.00096(10) S1 0.0089(4) 0.0116(4) 0.0123(4) 0.0000(3) 0.0010(3) -0.0001(3) S2 0.0101(4) 0.0116(4) 0.0122(4) 0.0004(3) 0.0015(3) 0.0001(3) N1 0.0123(15) 0.0124(14) 0.0140(14) -0.0018(11) -0.0003(12) 0.0017(11) N2 0.0109(15) 0.0153(15) 0.0174(15) 0.0013(12) -0.0019(12) 0.0031(12) N3 0.0104(15) 0.0118(14) 0.0167(15) 0.0007(11) 0.0024(12) -0.0004(11) N4 0.0093(15) 0.0159(14) 0.0130(14) 0.0008(11) 0.0001(11) -0.0022(11) N5 0.0116(15) 0.0163(15) 0.0158(15) 0.0029(12) 0.0025(12) -0.0025(12) N6 0.0107(15) 0.0124(14) 0.0112(14) 0.0003(11) 0.0009(11) -0.0002(11) C1 0.0096(17) 0.0120(16) 0.0173(17) 0.0008(13) 0.0052(13) 0.0005(13) C2 0.0113(17) 0.0163(17) 0.0131(16) 0.0029(13) 0.0017(13) -0.0009(13) C3 0.0176(19) 0.0163(17) 0.0206(19) 0.0034(14) -0.0046(15) 0.0019(14) C4 0.0115(18) 0.0134(16) 0.0171(17) -0.0023(13) 0.0016(14) 0.0007(13) C5 0.0161(19) 0.0155(17) 0.0210(19) 0.0030(14) -0.0012(15) -0.0035(14) C6 0.0074(16) 0.0146(16) 0.0124(16) 0.0013(13) 0.0024(13) 0.0011(13) C7 0.0108(17) 0.0145(17) 0.0164(17) 0.0019(13) 0.0027(14) 0.0008(13) C8 0.019(2) 0.0180(18) 0.0145(17) 0.0051(14) -0.0020(15) -0.0056(14) C9 0.0132(18) 0.0175(17) 0.0110(16) -0.0011(13) -0.0008(13) 0.0007(14) C10 0.020(2) 0.0219(19) 0.0151(18) -0.0006(14) 0.0026(15) 0.0039(15) C11 0.0110(18) 0.0247(19) 0.0154(18) 0.0012(14) 0.0012(14) -0.0070(14) C12 0.0060(16) 0.0260(19) 0.0186(18) -0.0026(15) 0.0037(14) -0.0026(14) C13 0.0122(19) 0.024(2) 0.023(2) 0.0015(15) -0.0008(15) 0.0025(15) C14 0.0137(19) 0.0221(19) 0.0157(18) 0.0055(14) -0.0029(14) 0.0013(14) C15 0.0138(18) 0.0197(18) 0.0113(16) 0.0012(13) 0.0015(13) -0.0011(14) C16 0.0098(17) 0.0189(17) 0.0130(17) -0.0008(13) 0.0006(13) 0.0000(13) C17 0.021(2) 0.0170(18) 0.0174(18) -0.0029(14) -0.0022(15) 0.0005(15) C18 0.020(2) 0.0174(18) 0.0169(18) -0.0001(14) -0.0013(15) -0.0051(15) C19 0.0087(18) 0.025(2) 0.023(2) -0.0063(15) 0.0005(15) 0.0018(14) C20 0.0143(18) 0.0166(18) 0.0211(19) -0.0039(14) -0.0055(15) 0.0034(14) C21 0.0173(19) 0.0164(18) 0.0185(18) -0.0016(14) -0.0028(15) 0.0001(14) C22 0.0168(19) 0.0183(18) 0.0171(18) -0.0026(14) 0.0004(15) 0.0019(15) C23 0.0116(17) 0.0152(17) 0.0166(17) -0.0033(13) -0.0006(14) 0.0007(13) C24 0.0145(18) 0.0103(16) 0.0198(18) -0.0038(13) 0.0021(14) 0.0019(13) C25 0.019(2) 0.0195(19) 0.023(2) -0.0015(15) 0.0029(16) -0.0069(15) C26 0.0138(19) 0.027(2) 0.027(2) -0.0023(16) 0.0066(16) -0.0056(16) C27 0.0173(19) 0.0123(16) 0.0148(17) -0.0008(13) 0.0039(14) 0.0042(14) C28 0.0129(18) 0.0147(17) 0.0188(18) 0.0022(14) 0.0037(14) 0.0087(14) C29 0.0159(19) 0.0207(19) 0.0219(19) 0.0040(15) -0.0002(15) 0.0045(15) C30 0.021(2) 0.0182(18) 0.0147(17) 0.0013(14) 0.0007(15) 0.0040(15) C31 0.0178(19) 0.0143(17) 0.0141(17) -0.0002(13) 0.0067(14) 0.0014(14) C32 0.0155(19) 0.0170(17) 0.0136(17) 0.0037(13) 0.0080(14) 0.0004(14) C33 0.019(2) 0.0136(17) 0.0226(19) -0.0007(14) 0.0065(15) -0.0051(14) C34 0.022(2) 0.0124(17) 0.0208(19) 0.0015(14) 0.0068(16) 0.0029(14) P1 0.0125(5) 0.0190(5) 0.0198(5) -0.0023(4) -0.0020(4) 0.0012(4) F1 0.0157(12) 0.0480(16) 0.0337(14) 0.0077(12) 0.0054(10) 0.0110(11) F2 0.0265(13) 0.0281(12) 0.0221(12) 0.0005(10) -0.0079(10) -0.0021(10) F3 0.0423(16) 0.0228(13) 0.0351(14) 0.0000(10) 0.0031(12) -0.0124(11) F4 0.0526(18) 0.0202(12) 0.0320(14) 0.0033(10) -0.0070(13) -0.0007(12) F5 0.0251(13) 0.0430(15) 0.0190(12) -0.0086(10) -0.0029(10) -0.0020(11) F6 0.0177(13) 0.0673(19) 0.0279(14) -0.0067(13) -0.0002(10) 0.0172(13) _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 N4 2.085(3) . ? Rh1 C12 2.124(4) . ? Rh1 C16 2.137(3) . ? Rh1 C15 2.138(3) . ? Rh1 C11 2.141(4) . ? Rh1 S1 2.3986(10) . ? Rh1 Rh3 3.2907(7) . ? Rh1 Rh2 5.2046(13) . ? Rh2 N1 2.083(3) . ? Rh2 C19 2.134(4) . ? Rh2 C20 2.143(4) . ? Rh2 C23 2.153(3) . ? Rh2 C24 2.155(3) . ? Rh2 S2 2.3883(11) . ? Rh2 Rh3 3.2923(10) . ? Rh3 C32 2.130(3) . ? Rh3 C28 2.138(3) . ? Rh3 C27 2.159(3) . ? Rh3 C31 2.168(3) . ? Rh3 S2 2.3489(10) . ? Rh3 S1 2.3577(9) . ? S1 C1 1.744(4) . ? S2 C6 1.744(3) . ? N1 C1 1.330(4) . ? N1 N2 1.394(4) . ? N2 C2 1.311(5) . ? N3 C1 1.362(4) . ? N3 C2 1.375(5) . ? N3 C4 1.467(4) . ? N4 C6 1.322(4) . ? N4 N5 1.404(4) . ? N5 C7 1.309(5) . ? N6 C6 1.362(4) . ? N6 C7 1.372(4) . ? N6 C9 1.474(4) . ? C2 C3 1.489(5) . ? C4 C5 1.512(5) . ? C7 C8 1.494(5) . ? C9 C10 1.514(5) . ? C11 C12 1.390(5) . ? C11 C18 1.530(5) . ? C12 C13 1.513(5) . ? C13 C14 1.549(5) . ? C14 C15 1.517(5) . ? C15 C16 1.388(5) . ? C16 C17 1.510(5) . ? C17 C18 1.532(5) . ? C19 C20 1.397(5) . ? C19 C26 1.519(5) . ? C20 C21 1.526(5) . ? C21 C22 1.534(5) . ? C22 C23 1.511(5) . ? C23 C24 1.394(5) . ? C24 C25 1.515(5) . ? C25 C26 1.532(5) . ? C27 C28 1.394(5) . ? C27 C34 1.528(5) . ? C28 C29 1.507(5) . ? C29 C30 1.535(5) . ? C30 C31 1.519(5) . ? C31 C32 1.400(5) . ? C32 C33 1.505(5) . ? C33 C34 1.533(5) . ? P1 F4 1.590(3) . ? P1 F1 1.592(3) . ? P1 F6 1.597(3) . ? P1 F5 1.605(2) . ? P1 F3 1.606(3) . ? P1 F2 1.608(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Rh1 C12 89.99(13) . . ? N4 Rh1 C16 154.61(12) . . ? C12 Rh1 C16 98.08(14) . . ? N4 Rh1 C15 167.05(13) . . ? C12 Rh1 C15 82.21(14) . . ? C16 Rh1 C15 37.90(13) . . ? N4 Rh1 C11 90.97(13) . . ? C12 Rh1 C11 38.05(14) . . ? C16 Rh1 C11 81.11(14) . . ? C15 Rh1 C11 89.22(14) . . ? N4 Rh1 S1 91.54(9) . . ? C12 Rh1 S1 155.27(10) . . ? C16 Rh1 S1 91.00(10) . . ? C15 Rh1 S1 91.30(11) . . ? C11 Rh1 S1 166.42(11) . . ? N4 Rh1 Rh3 83.72(8) . . ? C12 Rh1 Rh3 110.07(10) . . ? C16 Rh1 Rh3 115.38(10) . . ? C15 Rh1 Rh3 89.25(10) . . ? C11 Rh1 Rh3 147.87(11) . . ? S1 Rh1 Rh3 45.71(2) . . ? N4 Rh1 Rh2 52.77(8) . . ? C12 Rh1 Rh2 123.55(10) . . ? C16 Rh1 Rh2 134.53(10) . . ? C15 Rh1 Rh2 124.23(10) . . ? C11 Rh1 Rh2 143.00(10) . . ? S1 Rh1 Rh2 43.53(3) . . ? Rh3 Rh1 Rh2 37.768(7) . . ? N1 Rh2 C19 87.89(13) . . ? N1 Rh2 C20 91.63(13) . . ? C19 Rh2 C20 38.14(15) . . ? N1 Rh2 C23 159.30(13) . . ? C19 Rh2 C23 97.97(14) . . ? C20 Rh2 C23 81.25(14) . . ? N1 Rh2 C24 162.34(13) . . ? C19 Rh2 C24 81.47(14) . . ? C20 Rh2 C24 88.67(14) . . ? C23 Rh2 C24 37.75(13) . . ? N1 Rh2 S2 89.61(9) . . ? C19 Rh2 S2 166.13(11) . . ? C20 Rh2 S2 155.65(11) . . ? C23 Rh2 S2 89.12(10) . . ? C24 Rh2 S2 97.34(10) . . ? N1 Rh2 Rh3 82.12(8) . . ? C19 Rh2 Rh3 120.65(11) . . ? C20 Rh2 Rh3 158.46(11) . . ? C23 Rh2 Rh3 111.11(10) . . ? C24 Rh2 Rh3 91.19(10) . . ? S2 Rh2 Rh3 45.48(3) . . ? N1 Rh2 Rh1 52.44(8) . . ? C19 Rh2 Rh1 129.99(10) . . ? C20 Rh2 Rh1 143.77(10) . . ? C23 Rh2 Rh1 130.25(10) . . ? C24 Rh2 Rh1 126.80(10) . . ? S2 Rh2 Rh1 41.19(2) . . ? Rh3 Rh2 Rh1 37.746(13) . . ? C32 Rh3 C28 97.71(14) . . ? C32 Rh3 C27 81.71(14) . . ? C28 Rh3 C27 37.86(14) . . ? C32 Rh3 C31 38.00(14) . . ? C28 Rh3 C31 80.91(14) . . ? C27 Rh3 C31 88.84(13) . . ? C32 Rh3 S2 144.51(10) . . ? C28 Rh3 S2 92.56(10) . . ? C27 Rh3 S2 86.05(10) . . ? C31 Rh3 S2 173.46(10) . . ? C32 Rh3 S1 93.06(10) . . ? C28 Rh3 S1 146.73(10) . . ? C27 Rh3 S1 174.04(10) . . ? C31 Rh3 S1 88.77(10) . . ? S2 Rh3 S1 96.70(3) . . ? C32 Rh3 Rh1 127.80(10) . . ? C28 Rh3 Rh1 103.85(10) . . ? C27 Rh3 Rh1 139.14(10) . . ? C31 Rh3 Rh1 99.75(10) . . ? S2 Rh3 Rh1 81.59(3) . . ? S1 Rh3 Rh1 46.74(2) . . ? C32 Rh3 Rh2 101.31(10) . . ? C28 Rh3 Rh2 124.14(10) . . ? C27 Rh3 Rh2 94.31(10) . . ? C31 Rh3 Rh2 138.25(10) . . ? S2 Rh3 Rh2 46.47(3) . . ? S1 Rh3 Rh2 83.86(2) . . ? Rh1 Rh3 Rh2 104.486(15) . . ? C1 S1 Rh3 111.18(12) . . ? C1 S1 Rh1 106.33(12) . . ? Rh3 S1 Rh1 87.55(3) . . ? C6 S2 Rh3 113.34(12) . . ? C6 S2 Rh2 103.16(12) . . ? Rh3 S2 Rh2 88.05(4) . . ? C1 N1 N2 108.8(3) . . ? C1 N1 Rh2 132.0(2) . . ? N2 N1 Rh2 119.2(2) . . ? C2 N2 N1 106.2(3) . . ? C1 N3 C2 106.2(3) . . ? C1 N3 C4 126.3(3) . . ? C2 N3 C4 127.6(3) . . ? C6 N4 N5 107.9(3) . . ? C6 N4 Rh1 130.5(2) . . ? N5 N4 Rh1 121.4(2) . . ? C7 N5 N4 106.2(3) . . ? C6 N6 C7 105.4(3) . . ? C6 N6 C9 126.7(3) . . ? C7 N6 C9 127.8(3) . . ? N1 C1 N3 108.3(3) . . ? N1 C1 S1 129.5(3) . . ? N3 C1 S1 122.2(3) . . ? N2 C2 N3 110.5(3) . . ? N2 C2 C3 125.0(3) . . ? N3 C2 C3 124.5(3) . . ? N3 C4 C5 112.4(3) . . ? N4 C6 N6 109.6(3) . . ? N4 C6 S2 127.2(3) . . ? N6 C6 S2 122.9(3) . . ? N5 C7 N6 110.9(3) . . ? N5 C7 C8 125.3(3) . . ? N6 C7 C8 123.7(3) . . ? N6 C9 C10 112.1(3) . . ? C12 C11 C18 123.1(3) . . ? C12 C11 Rh1 70.3(2) . . ? C18 C11 Rh1 113.6(2) . . ? C11 C12 C13 124.3(3) . . ? C11 C12 Rh1 71.7(2) . . ? C13 C12 Rh1 110.1(2) . . ? C12 C13 C14 112.9(3) . . ? C15 C14 C13 112.0(3) . . ? C16 C15 C14 124.1(3) . . ? C16 C15 Rh1 71.0(2) . . ? C14 C15 Rh1 113.1(2) . . ? C15 C16 C17 125.2(3) . . ? C15 C16 Rh1 71.1(2) . . ? C17 C16 Rh1 110.7(2) . . ? C16 C17 C18 112.4(3) . . ? C11 C18 C17 111.1(3) . . ? C20 C19 C26 125.1(3) . . ? C20 C19 Rh2 71.3(2) . . ? C26 C19 Rh2 109.5(3) . . ? C19 C20 C21 124.7(3) . . ? C19 C20 Rh2 70.6(2) . . ? C21 C20 Rh2 113.6(2) . . ? C20 C21 C22 111.8(3) . . ? C23 C22 C21 112.9(3) . . ? C24 C23 C22 124.9(3) . . ? C24 C23 Rh2 71.2(2) . . ? C22 C23 Rh2 110.0(2) . . ? C23 C24 C25 124.0(3) . . ? C23 C24 Rh2 71.0(2) . . ? C25 C24 Rh2 113.0(2) . . ? C24 C25 C26 111.7(3) . . ? C19 C26 C25 112.5(3) . . ? C28 C27 C34 124.5(3) . . ? C28 C27 Rh3 70.3(2) . . ? C34 C27 Rh3 112.6(2) . . ? C27 C28 C29 125.1(3) . . ? C27 C28 Rh3 71.9(2) . . ? C29 C28 Rh3 110.8(2) . . ? C28 C29 C30 112.8(3) . . ? C31 C30 C29 111.8(3) . . ? C32 C31 C30 124.3(3) . . ? C32 C31 Rh3 69.5(2) . . ? C30 C31 Rh3 113.2(2) . . ? C31 C32 C33 124.8(3) . . ? C31 C32 Rh3 72.5(2) . . ? C33 C32 Rh3 109.9(2) . . ? C32 C33 C34 113.6(3) . . ? C27 C34 C33 111.7(3) . . ? F4 P1 F1 90.05(15) . . ? F4 P1 F6 89.96(16) . . ? F1 P1 F6 179.91(19) . . ? F4 P1 F5 90.07(14) . . ? F1 P1 F5 90.13(14) . . ? F6 P1 F5 89.96(14) . . ? F4 P1 F3 179.68(15) . . ? F1 P1 F3 90.04(15) . . ? F6 P1 F3 89.95(16) . . ? F5 P1 F3 90.24(14) . . ? F4 P1 F2 90.55(13) . . ? F1 P1 F2 90.34(14) . . ? F6 P1 F2 89.57(14) . . ? F5 P1 F2 179.23(15) . . ? F3 P1 F2 89.14(13) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.346 _refine_diff_density_min -0.837 _refine_diff_density_rms 0.133 data_10 _database_code_depnum_ccdc_archive 'CCDC 826262' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H10 N4 O6 Rh3 S2, BF4' _chemical_formula_sum 'C14 H10 B F4 N4 O6 Rh3 S2' _chemical_formula_weight 789.92 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' B B 0.0013 0.0007 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall -C2yc 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' '-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 16.757(3) _cell_length_b 16.186(3) _cell_length_c 11.502(2) _cell_angle_alpha 90.00 _cell_angle_beta 132.53(3) _cell_angle_gamma 90.00 _cell_volume 2298.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3352 _cell_measurement_theta_min 2.173 _cell_measurement_theta_max 27.433 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 2.382 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.583566 _exptl_absorpt_correction_T_max 0.890000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker AXS 2003)' _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_reflns_number 7769 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2632 _reflns_number_gt 2474 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.628 (Bruker, 2005)' _computing_cell_refinement 'Bruker SMART V5.628 (Bruker, 2005)' _computing_data_reduction 'Bruker SAINT V6.41 (Bruker, 2002)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 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. ; _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^)+(0.0250P)^2^+50.0615P] 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_number_reflns 2632 _refine_ls_number_parameters 171 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1159 _refine_ls_goodness_of_fit_ref 1.316 _refine_ls_restrained_S_all 1.342 _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 0.52022(4) 0.72184(3) 0.48950(6) 0.01262(15) Uani 1 1 d . . . Rh2 Rh 0.5000 0.61676(5) 0.2500 0.01267(19) Uani 1 2 d S . . S1 S 0.37577(13) 0.71508(11) 0.21036(18) 0.0129(3) Uani 1 1 d . . . N1 N 0.4051(4) 0.8091(4) 0.0414(6) 0.0128(11) Uani 1 1 d . . . N2 N 0.3526(5) 0.8814(4) 0.1411(6) 0.0150(12) Uani 1 1 d . . . O1 O 0.3977(5) 0.6110(4) 0.5305(7) 0.0334(14) Uani 1 1 d . . . O2 O 0.7125(5) 0.7252(5) 0.8419(6) 0.0360(15) Uani 1 1 d . . . O3 O 0.6287(5) 0.4850(4) 0.2541(7) 0.0284(13) Uani 1 1 d . . . C1 C 0.3812(5) 0.8053(4) 0.1302(7) 0.0112(12) Uani 1 1 d . . . C2 C 0.3911(5) 0.8908(5) -0.0071(7) 0.0159(14) Uani 1 1 d . . . H2 H 0.4017 0.9117 -0.0731 0.019 Uiso 1 1 calc R . . C3 C 0.3597(6) 0.9353(5) 0.0564(8) 0.0183(14) Uani 1 1 d . . . H3 H 0.3454 0.9929 0.0443 0.022 Uiso 1 1 calc R . . C4 C 0.3177(6) 0.9037(5) 0.2233(9) 0.0225(16) Uani 1 1 d . . . H4A H 0.2397 0.8940 0.1540 0.034 Uiso 1 1 calc R . . H4B H 0.3332 0.9622 0.2526 0.034 Uiso 1 1 calc R . . H4C H 0.3566 0.8699 0.3186 0.034 Uiso 1 1 calc R . . C5 C 0.4442(6) 0.6520(5) 0.5154(8) 0.0207(16) Uani 1 1 d . . . C6 C 0.6395(6) 0.7242(5) 0.7117(8) 0.0209(15) Uani 1 1 d . . . C7 C 0.5813(6) 0.5350(5) 0.2565(8) 0.0172(14) Uani 1 1 d . . . B1 B 0.5000 0.8661(5) 0.7500 0.038(4) Uani 1 2 d SD . . F1 F 0.5000 0.7811(4) 0.7500 0.051(2) Uani 1 2 d SD . . F2 F 0.4221(10) 0.8774(7) 0.5844(9) 0.050(3) Uani 0.50 1 d PD . . F3 F 0.4821(10) 0.9127(6) 0.8279(13) 0.033(2) Uani 0.50 1 d PD . . F4 F 0.5922(10) 0.8948(7) 0.7804(17) 0.049(3) Uani 0.50 1 d PD . . 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 0.0127(3) 0.0172(3) 0.0065(2) 0.0023(2) 0.0059(2) 0.0016(2) Rh2 0.0117(3) 0.0121(4) 0.0100(3) 0.000 0.0056(3) 0.000 S1 0.0102(7) 0.0153(8) 0.0083(7) 0.0017(6) 0.0043(6) -0.0002(6) N1 0.012(3) 0.016(3) 0.006(2) 0.001(2) 0.004(2) 0.000(2) N2 0.015(3) 0.016(3) 0.011(3) -0.001(2) 0.007(2) -0.002(2) O1 0.035(3) 0.037(4) 0.035(3) 0.016(3) 0.026(3) 0.003(3) O2 0.028(3) 0.060(5) 0.006(2) -0.002(3) 0.006(2) 0.004(3) O3 0.026(3) 0.021(3) 0.035(3) -0.007(2) 0.019(3) -0.003(2) C1 0.004(3) 0.014(3) 0.007(3) -0.002(2) 0.000(2) -0.001(2) C2 0.015(3) 0.020(4) 0.007(3) 0.008(3) 0.005(3) 0.002(3) C3 0.017(3) 0.016(3) 0.017(3) 0.003(3) 0.009(3) -0.001(3) C4 0.029(4) 0.022(4) 0.019(3) -0.003(3) 0.017(3) 0.003(3) C5 0.019(3) 0.029(4) 0.014(3) 0.008(3) 0.011(3) 0.008(3) C6 0.021(4) 0.028(4) 0.015(3) 0.002(3) 0.013(3) 0.004(3) C7 0.016(3) 0.020(4) 0.012(3) -0.001(3) 0.008(3) -0.003(3) B1 0.039(8) 0.009(6) 0.032(7) 0.000 0.011(7) 0.000 F1 0.095(7) 0.021(4) 0.097(7) 0.000 0.089(7) 0.000 F2 0.068(8) 0.036(6) 0.023(5) 0.008(5) 0.022(6) 0.016(6) F3 0.056(7) 0.033(6) 0.030(6) -0.004(5) 0.037(6) -0.005(5) F4 0.091(10) 0.031(6) 0.076(9) -0.015(6) 0.077(9) -0.020(7) _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 C5 1.872(8) . ? Rh1 C6 1.903(7) . ? Rh1 N1 2.071(6) 2_655 ? Rh1 S1 2.382(2) . ? Rh1 Rh2 3.0551(8) . ? Rh2 C7 1.864(8) 2_655 ? Rh2 C7 1.864(8) . ? Rh2 S1 2.4064(18) . ? Rh2 S1 2.4065(18) 2_655 ? Rh2 Rh1 3.0551(8) 2_655 ? S1 C1 1.762(7) . ? N1 C1 1.327(8) . ? N1 C2 1.391(9) . ? N1 Rh1 2.071(6) 2_655 ? N2 C1 1.357(9) . ? N2 C3 1.372(9) . ? N2 C4 1.454(9) . ? O1 C5 1.123(10) . ? O2 C6 1.123(9) . ? O3 C7 1.147(9) . ? C2 C3 1.360(10) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? B1 F3 1.351(7) . ? B1 F3 1.351(7) 2_656 ? B1 F1 1.376(7) . ? B1 F4 1.412(8) . ? B1 F4 1.412(8) 2_656 ? B1 F2 1.415(7) . ? B1 F2 1.415(7) 2_656 ? F2 F3 1.316(17) 2_656 ? F2 F4 1.749(16) 2_656 ? F3 F4 1.043(16) 2_656 ? F3 F2 1.316(17) 2_656 ? F4 F3 1.043(16) 2_656 ? F4 F2 1.749(16) 2_656 ? 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 C5 Rh1 C6 90.5(3) . . ? C5 Rh1 N1 174.0(3) . 2_655 ? C6 Rh1 N1 90.5(3) . 2_655 ? C5 Rh1 S1 90.3(2) . . ? C6 Rh1 S1 177.4(2) . . ? N1 Rh1 S1 88.93(15) 2_655 . ? C5 Rh1 Rh2 97.7(2) . . ? C6 Rh1 Rh2 126.7(2) . . ? N1 Rh1 Rh2 86.36(16) 2_655 . ? S1 Rh1 Rh2 50.71(4) . . ? C7 Rh2 C7 89.6(4) 2_655 . ? C7 Rh2 S1 86.9(2) 2_655 . ? C7 Rh2 S1 172.9(2) . . ? C7 Rh2 S1 172.9(2) 2_655 2_655 ? C7 Rh2 S1 86.9(2) . 2_655 ? S1 Rh2 S1 97.20(9) . 2_655 ? C7 Rh2 Rh1 136.6(2) 2_655 2_655 ? C7 Rh2 Rh1 93.6(2) . 2_655 ? S1 Rh2 Rh1 84.64(5) . 2_655 ? S1 Rh2 Rh1 49.99(5) 2_655 2_655 ? C7 Rh2 Rh1 93.6(2) 2_655 . ? C7 Rh2 Rh1 136.6(2) . . ? S1 Rh2 Rh1 49.99(5) . . ? S1 Rh2 Rh1 84.64(5) 2_655 . ? Rh1 Rh2 Rh1 112.34(3) 2_655 . ? C1 S1 Rh1 107.6(2) . . ? C1 S1 Rh2 107.7(2) . . ? Rh1 S1 Rh2 79.30(6) . . ? C1 N1 C2 107.3(6) . . ? C1 N1 Rh1 129.2(5) . 2_655 ? C2 N1 Rh1 122.4(5) . 2_655 ? C1 N2 C3 107.9(6) . . ? C1 N2 C4 127.3(6) . . ? C3 N2 C4 124.8(6) . . ? N1 C1 N2 109.7(6) . . ? N1 C1 S1 126.2(5) . . ? N2 C1 S1 123.9(5) . . ? C3 C2 N1 108.0(6) . . ? C3 C2 H2 126.0 . . ? N1 C2 H2 126.0 . . ? C2 C3 N2 107.2(6) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 Rh1 179.0(7) . . ? O2 C6 Rh1 177.3(7) . . ? O3 C7 Rh2 177.3(6) . . ? F3 B1 F3 112.2(10) . 2_656 ? F3 B1 F1 123.9(5) . . ? F3 B1 F1 123.9(5) 2_656 . ? F3 B1 F4 110.4(8) . . ? F3 B1 F4 44.3(7) 2_656 . ? F1 B1 F4 109.2(6) . . ? F3 B1 F4 44.3(7) . 2_656 ? F3 B1 F4 110.4(7) 2_656 2_656 ? F1 B1 F4 109.2(6) . 2_656 ? F4 B1 F4 141.6(12) . 2_656 ? F3 B1 F2 113.9(8) . . ? F3 B1 F2 56.8(8) 2_656 . ? F1 B1 F2 97.4(6) . . ? F4 B1 F2 98.6(8) . . ? F4 B1 F2 76.4(8) 2_656 . ? F3 B1 F2 56.8(8) . 2_656 ? F3 B1 F2 113.9(8) 2_656 2_656 ? F1 B1 F2 97.4(6) . 2_656 ? F4 B1 F2 76.4(8) . 2_656 ? F4 B1 F2 98.6(8) 2_656 2_656 ? F2 B1 F2 165.2(12) . 2_656 ? F3 F2 B1 59.2(5) 2_656 . ? F3 F2 F4 94.5(7) 2_656 2_656 ? B1 F2 F4 51.7(5) . 2_656 ? F4 F3 F2 130.3(9) 2_656 2_656 ? F4 F3 B1 71.0(5) 2_656 . ? F2 F3 B1 64.1(5) 2_656 . ? F3 F4 B1 64.7(6) 2_656 . ? F3 F4 F2 109.6(8) 2_656 2_656 ? B1 F4 F2 51.9(4) . 2_656 ? 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 C5 Rh1 Rh2 C7 1.2(3) . . . 2_655 ? C6 Rh1 Rh2 C7 97.6(4) . . . 2_655 ? N1 Rh1 Rh2 C7 -174.5(3) 2_655 . . 2_655 ? S1 Rh1 Rh2 C7 -82.9(2) . . . 2_655 ? C5 Rh1 Rh2 C7 -92.1(4) . . . . ? C6 Rh1 Rh2 C7 4.3(4) . . . . ? N1 Rh1 Rh2 C7 92.2(4) 2_655 . . . ? S1 Rh1 Rh2 C7 -176.2(3) . . . . ? C5 Rh1 Rh2 S1 84.1(2) . . . . ? C6 Rh1 Rh2 S1 -179.5(3) . . . . ? N1 Rh1 Rh2 S1 -91.60(16) 2_655 . . . ? C5 Rh1 Rh2 S1 -171.9(2) . . . 2_655 ? C6 Rh1 Rh2 S1 -75.5(3) . . . 2_655 ? N1 Rh1 Rh2 S1 12.47(16) 2_655 . . 2_655 ? S1 Rh1 Rh2 S1 104.07(9) . . . 2_655 ? C5 Rh1 Rh2 Rh1 145.6(2) . . . 2_655 ? C6 Rh1 Rh2 Rh1 -118.0(3) . . . 2_655 ? N1 Rh1 Rh2 Rh1 -30.08(15) 2_655 . . 2_655 ? S1 Rh1 Rh2 Rh1 61.52(5) . . . 2_655 ? C5 Rh1 S1 C1 154.9(3) . . . . ? C6 Rh1 S1 C1 -97(6) . . . . ? N1 Rh1 S1 C1 -19.2(3) 2_655 . . . ? Rh2 Rh1 S1 C1 -105.3(2) . . . . ? C5 Rh1 S1 Rh2 -99.7(2) . . . . ? C6 Rh1 S1 Rh2 8(6) . . . . ? N1 Rh1 S1 Rh2 86.17(16) 2_655 . . . ? C7 Rh2 S1 C1 -157.4(3) 2_655 . . . ? C7 Rh2 S1 C1 -96.4(18) . . . . ? S1 Rh2 S1 C1 28.5(2) 2_655 . . . ? Rh1 Rh2 S1 C1 -20.0(2) 2_655 . . . ? Rh1 Rh2 S1 C1 105.2(2) . . . . ? C7 Rh2 S1 Rh1 97.4(2) 2_655 . . . ? C7 Rh2 S1 Rh1 158.4(18) . . . . ? S1 Rh2 S1 Rh1 -76.76(5) 2_655 . . . ? Rh1 Rh2 S1 Rh1 -125.26(4) 2_655 . . . ? C2 N1 C1 N2 -0.2(7) . . . . ? Rh1 N1 C1 N2 167.8(4) 2_655 . . . ? C2 N1 C1 S1 175.1(5) . . . . ? Rh1 N1 C1 S1 -17.0(8) 2_655 . . . ? C3 N2 C1 N1 -0.4(7) . . . . ? C4 N2 C1 N1 178.1(6) . . . . ? C3 N2 C1 S1 -175.8(5) . . . . ? C4 N2 C1 S1 2.7(9) . . . . ? Rh1 S1 C1 N1 112.7(5) . . . . ? Rh2 S1 C1 N1 28.6(6) . . . . ? Rh1 S1 C1 N2 -72.8(5) . . . . ? Rh2 S1 C1 N2 -156.8(5) . . . . ? C1 N1 C2 C3 0.7(7) . . . . ? Rh1 N1 C2 C3 -168.3(4) 2_655 . . . ? N1 C2 C3 N2 -1.0(7) . . . . ? C1 N2 C3 C2 0.9(7) . . . . ? C4 N2 C3 C2 -177.7(6) . . . . ? C6 Rh1 C5 O1 104(43) . . . . ? N1 Rh1 C5 O1 5(45) 2_655 . . . ? S1 Rh1 C5 O1 -78(43) . . . . ? Rh2 Rh1 C5 O1 -128(43) . . . . ? C5 Rh1 C6 O2 136(17) . . . . ? N1 Rh1 C6 O2 -50(17) 2_655 . . . ? S1 Rh1 C6 O2 28(21) . . . . ? Rh2 Rh1 C6 O2 36(17) . . . . ? C7 Rh2 C7 O3 94(14) 2_655 . . . ? S1 Rh2 C7 O3 33(15) . . . . ? S1 Rh2 C7 O3 -93(14) 2_655 . . . ? Rh1 Rh2 C7 O3 -43(14) 2_655 . . . ? Rh1 Rh2 C7 O3 -172(14) . . . . ? F3 B1 F2 F3 101.8(12) . . . 2_656 ? F1 B1 F2 F3 -126.0(6) . . . 2_656 ? F4 B1 F2 F3 -15.2(9) . . . 2_656 ? F4 B1 F2 F3 126.0(9) 2_656 . . 2_656 ? F2 B1 F2 F3 54.0(6) 2_656 . . 2_656 ? F3 B1 F2 F4 -24.2(8) . . . 2_656 ? F3 B1 F2 F4 -126.0(9) 2_656 . . 2_656 ? F1 B1 F2 F4 108.0(6) . . . 2_656 ? F4 B1 F2 F4 -141.2(12) . . . 2_656 ? F2 B1 F2 F4 -72.0(6) 2_656 . . 2_656 ? F3 B1 F3 F4 97.0(10) 2_656 . . 2_656 ? F1 B1 F3 F4 -83.0(10) . . . 2_656 ? F4 B1 F3 F4 144.7(12) . . . 2_656 ? F2 B1 F3 F4 34.8(12) . . . 2_656 ? F2 B1 F3 F4 -158.2(12) 2_656 . . 2_656 ? F3 B1 F3 F2 -104.8(8) 2_656 . . 2_656 ? F1 B1 F3 F2 75.2(8) . . . 2_656 ? F4 B1 F3 F2 -57.1(10) . . . 2_656 ? F4 B1 F3 F2 158.2(12) 2_656 . . 2_656 ? F2 B1 F3 F2 -167.0(10) . . . 2_656 ? F3 B1 F4 F3 -101.3(12) . . . 2_656 ? F1 B1 F4 F3 119.3(8) . . . 2_656 ? F4 B1 F4 F3 -60.7(8) 2_656 . . 2_656 ? F2 B1 F4 F3 18.3(10) . . . 2_656 ? F2 B1 F4 F3 -147.5(11) 2_656 . . 2_656 ? F3 B1 F4 F2 46.2(7) . . . 2_656 ? F3 B1 F4 F2 147.5(11) 2_656 . . 2_656 ? F1 B1 F4 F2 -93.2(6) . . . 2_656 ? F4 B1 F4 F2 86.8(6) 2_656 . . 2_656 ? F2 B1 F4 F2 165.8(11) . . . 2_656 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.368 _refine_diff_density_min -2.227 _refine_diff_density_rms 0.199 data_12 _database_code_depnum_ccdc_archive 'CCDC 826263' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H55 N4 O3 P3 Rh3 S2, C H2 Cl2, B F4' _chemical_formula_sum 'C66 H57 B Cl2 F4 N4 O3 P3 Rh3 S2' _chemical_formula_weight 1577.63 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' B B 0.0013 0.0007 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9817(8) _cell_length_b 15.4685(11) _cell_length_c 18.5724(13) _cell_angle_alpha 104.309(1) _cell_angle_beta 93.037(1) _cell_angle_gamma 99.896(1) _cell_volume 3269.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.793 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34532 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.1782 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.14 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14840 _reflns_number_gt 7497 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0679P)^2^+0.1793P] 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_number_reflns 14840 _refine_ls_number_parameters 795 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1625 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1622 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _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 0.40675(5) 0.65845(4) 0.31189(3) 0.02140(16) Uani 1 1 d . . . Rh2 Rh 0.42704(5) 0.88780(4) 0.15782(3) 0.02056(15) Uani 1 1 d . . . Rh3 Rh 0.54772(5) 0.82831(4) 0.27975(3) 0.01910(15) Uani 1 1 d . . . P1 P 0.45112(17) 0.51904(13) 0.29778(11) 0.0233(5) Uani 1 1 d . . . P2 P 0.38866(16) 1.02977(13) 0.18571(11) 0.0235(5) Uani 1 1 d . . . P3 P 0.73337(16) 0.83721(13) 0.25727(11) 0.0213(4) Uani 1 1 d . . . S1 S 0.36549(15) 0.80833(13) 0.32654(10) 0.0228(4) Uani 1 1 d . . . S2 S 0.48226(15) 0.74403(12) 0.15325(10) 0.0212(4) Uani 1 1 d . . . N1 N 0.2741(5) 0.8410(4) 0.1988(3) 0.0242(15) Uani 1 1 d . . . N2 N 0.1503(5) 0.7647(4) 0.2553(4) 0.0273(15) Uani 1 1 d . . . N3 N 0.3268(5) 0.6224(4) 0.2033(3) 0.0228(14) Uani 1 1 d . . . N4 N 0.2765(5) 0.6376(4) 0.0914(3) 0.0246(15) Uani 1 1 d . . . O1 O 0.5065(6) 0.7160(4) 0.4698(4) 0.061(2) Uani 1 1 d . . . O2 O 0.6230(5) 0.9269(4) 0.0731(4) 0.0509(18) Uani 1 1 d . . . O3 O 0.6269(5) 0.9661(4) 0.4235(3) 0.0393(15) Uani 1 1 d . . . C1 C 0.4686(7) 0.6931(6) 0.4095(5) 0.036(2) Uani 1 1 d . . . C2 C 0.5494(7) 0.9169(5) 0.1089(5) 0.031(2) Uani 1 1 d . . . C3 C 0.5985(6) 0.9120(5) 0.3689(4) 0.0243(17) Uani 1 1 d . . . C4 C 0.2606(6) 0.8041(5) 0.2564(4) 0.0235(17) Uani 1 1 d . . . C5 C 0.1659(6) 0.8235(5) 0.1602(5) 0.0290(19) Uani 1 1 d . . . H5 H 0.1487 0.8416 0.1174 0.035 Uiso 1 1 calc R . . C6 C 0.0899(6) 0.7762(5) 0.1943(5) 0.031(2) Uani 1 1 d . . . H6 H 0.0125 0.7557 0.1796 0.037 Uiso 1 1 calc R . . C7 C 0.1021(7) 0.7156(6) 0.3076(5) 0.044(2) Uani 1 1 d . . . H7A H 0.1296 0.6597 0.3009 0.065 Uiso 1 1 calc R . . H7B H 0.0206 0.7027 0.2985 0.065 Uiso 1 1 calc R . . H7C H 0.1245 0.7522 0.3578 0.065 Uiso 1 1 calc R . . C8 C 0.3555(6) 0.6664(5) 0.1515(4) 0.0236(17) Uani 1 1 d . . . C9 C 0.2265(6) 0.5639(5) 0.1755(4) 0.0275(18) Uani 1 1 d . . . H9 H 0.1868 0.5240 0.1996 0.033 Uiso 1 1 calc R . . C10 C 0.1940(6) 0.5730(5) 0.1076(4) 0.0286(19) Uani 1 1 d . . . H10 H 0.1281 0.5415 0.0772 0.034 Uiso 1 1 calc R . . C11 C 0.2711(7) 0.6700(6) 0.0243(4) 0.034(2) Uani 1 1 d . . . H11A H 0.3238 0.7265 0.0321 0.052 Uiso 1 1 calc R . . H11B H 0.1954 0.6790 0.0135 0.052 Uiso 1 1 calc R . . H11C H 0.2906 0.6258 -0.0169 0.052 Uiso 1 1 calc R . . C12 C 0.3507(7) 0.4385(5) 0.3319(4) 0.0289(19) Uani 1 1 d . . . C13 C 0.2383(7) 0.4475(6) 0.3312(4) 0.037(2) Uani 1 1 d . . . H13 H 0.2176 0.4989 0.3212 0.044 Uiso 1 1 calc R . . C14 C 0.1544(8) 0.3801(7) 0.3456(5) 0.052(3) Uani 1 1 d . . . H14 H 0.0782 0.3852 0.3427 0.062 Uiso 1 1 calc R . . C15 C 0.1863(8) 0.3065(6) 0.3640(5) 0.048(3) Uani 1 1 d . . . H15 H 0.1315 0.2616 0.3738 0.058 Uiso 1 1 calc R . . C16 C 0.2991(8) 0.2989(6) 0.3678(5) 0.041(2) Uani 1 1 d . . . H16 H 0.3206 0.2497 0.3813 0.049 Uiso 1 1 calc R . . C17 C 0.3803(7) 0.3642(5) 0.3516(4) 0.034(2) Uani 1 1 d . . . H17 H 0.4562 0.3582 0.3540 0.041 Uiso 1 1 calc R . . C18 C 0.4582(6) 0.4624(5) 0.2015(4) 0.0233(17) Uani 1 1 d . . . C19 C 0.4025(6) 0.3731(5) 0.1687(4) 0.0301(19) Uani 1 1 d . . . H19 H 0.3611 0.3401 0.1973 0.036 Uiso 1 1 calc R . . C20 C 0.4084(7) 0.3329(6) 0.0934(5) 0.037(2) Uani 1 1 d . . . H20 H 0.3698 0.2738 0.0715 0.045 Uiso 1 1 calc R . . C21 C 0.4725(7) 0.3819(6) 0.0510(4) 0.034(2) Uani 1 1 d . . . H21 H 0.4778 0.3551 0.0009 0.040 Uiso 1 1 calc R . . C22 C 0.5282(6) 0.4701(6) 0.0833(4) 0.0314(19) Uani 1 1 d . . . H22 H 0.5713 0.5025 0.0550 0.038 Uiso 1 1 calc R . . C23 C 0.5200(6) 0.5099(5) 0.1570(4) 0.0261(18) Uani 1 1 d . . . H23 H 0.5565 0.5698 0.1778 0.031 Uiso 1 1 calc R . . C24 C 0.5897(6) 0.5164(5) 0.3442(4) 0.0242(17) Uani 1 1 d . . . C25 C 0.5997(7) 0.5275(5) 0.4216(5) 0.034(2) Uani 1 1 d . . . H25 H 0.5375 0.5355 0.4487 0.041 Uiso 1 1 calc R . . C26 C 0.7046(8) 0.5266(6) 0.4575(5) 0.043(2) Uani 1 1 d . . . H26 H 0.7119 0.5333 0.5088 0.052 Uiso 1 1 calc R . . C27 C 0.7976(8) 0.5157(6) 0.4179(5) 0.043(2) Uani 1 1 d . . . H27 H 0.8671 0.5157 0.4426 0.051 Uiso 1 1 calc R . . C28 C 0.7877(7) 0.5051(6) 0.3426(5) 0.038(2) Uani 1 1 d . . . H28 H 0.8503 0.4973 0.3158 0.045 Uiso 1 1 calc R . . C29 C 0.6831(6) 0.5059(5) 0.3057(5) 0.0308(19) Uani 1 1 d . . . H29 H 0.6768 0.4992 0.2544 0.037 Uiso 1 1 calc R . . C30 C 0.5036(6) 1.1271(5) 0.1892(5) 0.0269(18) Uani 1 1 d . . . C31 C 0.5522(7) 1.1286(6) 0.1225(5) 0.040(2) Uani 1 1 d . . . H31 H 0.5278 1.0816 0.0796 0.048 Uiso 1 1 calc R . . C32 C 0.6378(8) 1.2016(7) 0.1212(6) 0.052(3) Uani 1 1 d . . . H32 H 0.6707 1.2029 0.0772 0.062 Uiso 1 1 calc R . . C33 C 0.6746(7) 1.2722(6) 0.1850(7) 0.053(3) Uani 1 1 d . . . H33 H 0.7332 1.3197 0.1841 0.064 Uiso 1 1 calc R . . C34 C 0.6239(7) 1.2713(6) 0.2490(6) 0.045(2) Uani 1 1 d . . . H34 H 0.6459 1.3197 0.2913 0.054 Uiso 1 1 calc R . . C35 C 0.5402(6) 1.1989(5) 0.2514(5) 0.033(2) Uani 1 1 d . . . H35 H 0.5079 1.1984 0.2957 0.040 Uiso 1 1 calc R . . C36 C 0.3420(6) 1.0510(5) 0.2789(4) 0.0240(17) Uani 1 1 d . . . C37 C 0.2293(6) 1.0516(5) 0.2927(4) 0.0301(19) Uani 1 1 d . . . H37 H 0.1756 1.0463 0.2531 0.036 Uiso 1 1 calc R . . C38 C 0.1950(7) 1.0597(5) 0.3624(5) 0.035(2) Uani 1 1 d . . . H38 H 0.1191 1.0608 0.3701 0.042 Uiso 1 1 calc R . . C39 C 0.2741(7) 1.0662(5) 0.4217(5) 0.034(2) Uani 1 1 d . . . H39 H 0.2511 1.0712 0.4693 0.041 Uiso 1 1 calc R . . C40 C 0.3858(7) 1.0653(5) 0.4103(4) 0.036(2) Uani 1 1 d . . . H40 H 0.4390 1.0710 0.4503 0.043 Uiso 1 1 calc R . . C41 C 0.4191(6) 1.0559(5) 0.3396(4) 0.0284(18) Uani 1 1 d . . . H41 H 0.4946 1.0528 0.3319 0.034 Uiso 1 1 calc R . . C42 C 0.2782(6) 1.0542(5) 0.1267(4) 0.0298(19) Uani 1 1 d . . . C43 C 0.2378(6) 0.9935(6) 0.0577(5) 0.034(2) Uani 1 1 d . . . H43 H 0.2621 0.9383 0.0440 0.041 Uiso 1 1 calc R . . C44 C 0.1609(7) 1.0156(7) 0.0091(5) 0.045(3) Uani 1 1 d . . . H44 H 0.1343 0.9752 -0.0371 0.055 Uiso 1 1 calc R . . C45 C 0.1244(7) 1.0974(8) 0.0297(7) 0.059(3) Uani 1 1 d . . . H45 H 0.0732 1.1121 -0.0026 0.071 Uiso 1 1 calc R . . C46 C 0.1637(7) 1.1571(7) 0.0980(6) 0.048(3) Uani 1 1 d . . . H46 H 0.1386 1.2120 0.1116 0.058 Uiso 1 1 calc R . . C47 C 0.2397(7) 1.1368(6) 0.1466(5) 0.039(2) Uani 1 1 d . . . H47 H 0.2655 1.1778 0.1927 0.046 Uiso 1 1 calc R . . C48 C 0.8021(6) 0.9410(5) 0.2351(4) 0.0239(17) Uani 1 1 d . . . C49 C 0.9013(6) 0.9460(5) 0.1995(4) 0.0273(18) Uani 1 1 d . . . H49 H 0.9344 0.8949 0.1856 0.033 Uiso 1 1 calc R . . C50 C 0.9511(6) 1.0264(6) 0.1844(4) 0.032(2) Uani 1 1 d . . . H50 H 1.0168 1.0287 0.1599 0.038 Uiso 1 1 calc R . . C51 C 0.9039(7) 1.1036(6) 0.2056(5) 0.037(2) Uani 1 1 d . . . H51 H 0.9385 1.1578 0.1963 0.044 Uiso 1 1 calc R . . C52 C 0.8044(7) 1.0990(6) 0.2408(5) 0.046(2) Uani 1 1 d . . . H52 H 0.7724 1.1505 0.2558 0.055 Uiso 1 1 calc R . . C53 C 0.7531(6) 1.0177(5) 0.2534(5) 0.034(2) Uani 1 1 d . . . H53 H 0.6843 1.0143 0.2746 0.041 Uiso 1 1 calc R . . C54 C 0.7705(6) 0.7444(5) 0.1866(4) 0.0253(18) Uani 1 1 d . . . C55 C 0.8006(6) 0.6689(5) 0.2038(5) 0.0289(19) Uani 1 1 d . . . H55 H 0.7995 0.6645 0.2528 0.035 Uiso 1 1 calc R . . C56 C 0.8324(7) 0.5997(5) 0.1511(5) 0.037(2) Uani 1 1 d . . . H56 H 0.8498 0.5488 0.1640 0.044 Uiso 1 1 calc R . . C57 C 0.8376(7) 0.6076(6) 0.0796(5) 0.047(3) Uani 1 1 d . . . H57 H 0.8631 0.5630 0.0444 0.056 Uiso 1 1 calc R . . C58 C 0.8062(7) 0.6799(7) 0.0585(5) 0.045(2) Uani 1 1 d . . . H58 H 0.8081 0.6831 0.0092 0.054 Uiso 1 1 calc R . . C59 C 0.7715(6) 0.7483(6) 0.1115(4) 0.032(2) Uani 1 1 d . . . H59 H 0.7489 0.7968 0.0974 0.039 Uiso 1 1 calc R . . C60 C 0.8191(6) 0.8356(5) 0.3413(4) 0.0222(17) Uani 1 1 d . . . C61 C 0.7773(6) 0.7741(5) 0.3824(4) 0.0273(18) Uani 1 1 d . . . H61 H 0.7067 0.7359 0.3672 0.033 Uiso 1 1 calc R . . C62 C 0.8409(7) 0.7703(5) 0.4455(4) 0.0318(19) Uani 1 1 d . . . H62 H 0.8133 0.7286 0.4719 0.038 Uiso 1 1 calc R . . C63 C 0.9446(7) 0.8274(6) 0.4697(5) 0.037(2) Uani 1 1 d . . . H63 H 0.9862 0.8246 0.5126 0.045 Uiso 1 1 calc R . . C64 C 0.9870(7) 0.8886(6) 0.4306(5) 0.039(2) Uani 1 1 d . . . H64 H 1.0569 0.9275 0.4470 0.047 Uiso 1 1 calc R . . C65 C 0.9244(6) 0.8919(5) 0.3662(4) 0.0305(19) Uani 1 1 d . . . H65 H 0.9538 0.9326 0.3395 0.037 Uiso 1 1 calc R . . B1 B 0.9793(11) 0.3698(9) 0.1323(11) 0.080(5) Uani 1 1 d . . . F1 F 0.9133(5) 0.2835(5) 0.0999(4) 0.098(2) Uani 1 1 d . . . F2 F 0.9751(6) 0.4171(5) 0.0748(4) 0.103(3) Uani 1 1 d . . . F3 F 1.0882(5) 0.3617(4) 0.1417(4) 0.094(2) Uani 1 1 d . . . F4 F 0.9432(9) 0.4166(6) 0.1889(6) 0.165(5) Uani 1 1 d . . . C66 C 0.2252(11) 0.6991(11) 0.5216(13) 0.203(12) Uani 1 1 d . A 1 H66A H 0.2739 0.6780 0.4836 0.243 Uiso 1 1 calc R A 1 H66B H 0.2469 0.6785 0.5647 0.243 Uiso 1 1 calc R A 1 Cl1 Cl 0.2602(4) 0.8122(3) 0.5468(3) 0.1396(17) Uani 1 1 d . A 1 Cl2 Cl 0.0934(3) 0.6434(3) 0.4897(3) 0.148(2) Uani 1 1 d . A 1 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 0.0273(3) 0.0193(3) 0.0200(3) 0.0086(3) 0.0027(3) 0.0056(3) Rh2 0.0215(3) 0.0212(3) 0.0224(3) 0.0114(3) 0.0034(2) 0.0044(3) Rh3 0.0208(3) 0.0189(3) 0.0192(3) 0.0066(3) 0.0028(2) 0.0052(2) P1 0.0307(11) 0.0208(11) 0.0205(11) 0.0096(9) 0.0049(9) 0.0038(9) P2 0.0256(11) 0.0227(11) 0.0261(12) 0.0127(9) 0.0035(9) 0.0060(9) P3 0.0219(10) 0.0216(11) 0.0229(11) 0.0093(9) 0.0030(8) 0.0053(8) S1 0.0243(10) 0.0232(10) 0.0227(11) 0.0076(9) 0.0061(8) 0.0060(8) S2 0.0241(10) 0.0205(10) 0.0202(10) 0.0061(8) 0.0037(8) 0.0056(8) N1 0.021(3) 0.026(4) 0.028(4) 0.008(3) 0.006(3) 0.010(3) N2 0.017(3) 0.033(4) 0.039(4) 0.020(3) 0.009(3) 0.007(3) N3 0.020(3) 0.024(4) 0.025(4) 0.009(3) 0.001(3) 0.002(3) N4 0.029(4) 0.023(4) 0.023(4) 0.010(3) -0.001(3) 0.003(3) O1 0.107(6) 0.047(4) 0.030(4) 0.001(3) -0.012(4) 0.033(4) O2 0.048(4) 0.064(5) 0.061(5) 0.045(4) 0.031(3) 0.017(3) O3 0.045(4) 0.043(4) 0.025(3) -0.001(3) -0.004(3) 0.013(3) C1 0.052(6) 0.032(5) 0.026(5) 0.007(4) 0.000(4) 0.015(4) C2 0.028(5) 0.034(5) 0.039(5) 0.022(4) -0.001(4) 0.007(4) C3 0.031(4) 0.028(5) 0.022(4) 0.013(4) 0.009(3) 0.019(4) C4 0.027(4) 0.021(4) 0.029(5) 0.014(4) 0.009(3) 0.013(3) C5 0.027(4) 0.025(4) 0.038(5) 0.013(4) 0.005(4) 0.008(4) C6 0.019(4) 0.026(4) 0.054(6) 0.022(4) 0.010(4) 0.007(3) C7 0.034(5) 0.053(6) 0.062(7) 0.041(5) 0.019(4) 0.014(4) C8 0.020(4) 0.023(4) 0.031(5) 0.010(4) 0.001(3) 0.009(3) C9 0.026(4) 0.019(4) 0.035(5) 0.008(4) -0.001(4) -0.002(3) C10 0.030(4) 0.023(4) 0.027(5) 0.000(4) 0.000(4) 0.001(4) C11 0.036(5) 0.038(5) 0.027(5) 0.007(4) -0.004(4) 0.005(4) C12 0.040(5) 0.032(5) 0.013(4) 0.008(4) 0.003(3) -0.002(4) C13 0.042(5) 0.036(5) 0.035(5) 0.022(4) 0.004(4) -0.004(4) C14 0.039(5) 0.077(8) 0.043(6) 0.034(6) 0.002(4) -0.005(5) C15 0.063(7) 0.038(6) 0.042(6) 0.023(5) 0.005(5) -0.013(5) C16 0.064(7) 0.028(5) 0.035(5) 0.016(4) 0.015(5) 0.006(4) C17 0.045(5) 0.022(4) 0.035(5) 0.006(4) 0.014(4) 0.005(4) C18 0.029(4) 0.022(4) 0.024(4) 0.011(4) 0.008(3) 0.010(3) C19 0.034(5) 0.037(5) 0.019(4) 0.010(4) 0.000(3) 0.004(4) C20 0.043(5) 0.026(5) 0.036(5) -0.001(4) -0.002(4) 0.000(4) C21 0.043(5) 0.042(5) 0.016(4) 0.004(4) 0.009(4) 0.011(4) C22 0.034(5) 0.041(5) 0.023(5) 0.015(4) 0.004(4) 0.010(4) C23 0.035(5) 0.020(4) 0.023(4) 0.009(4) -0.002(3) 0.001(3) C24 0.032(4) 0.017(4) 0.025(4) 0.008(3) -0.002(3) 0.008(3) C25 0.048(5) 0.029(5) 0.030(5) 0.010(4) 0.006(4) 0.017(4) C26 0.067(7) 0.041(6) 0.023(5) 0.008(4) -0.010(5) 0.017(5) C27 0.049(6) 0.037(5) 0.039(6) 0.006(5) -0.017(5) 0.011(4) C28 0.030(5) 0.039(5) 0.049(6) 0.021(5) -0.002(4) 0.007(4) C29 0.036(5) 0.022(4) 0.037(5) 0.016(4) 0.002(4) 0.002(4) C30 0.021(4) 0.022(4) 0.043(5) 0.019(4) -0.001(4) 0.004(3) C31 0.055(6) 0.030(5) 0.047(6) 0.026(4) 0.015(5) 0.009(4) C32 0.056(6) 0.051(6) 0.069(7) 0.046(6) 0.027(5) 0.015(5) C33 0.039(6) 0.020(5) 0.108(10) 0.026(6) 0.015(6) 0.009(4) C34 0.042(6) 0.025(5) 0.065(7) 0.010(5) 0.005(5) 0.000(4) C35 0.032(5) 0.020(4) 0.052(6) 0.010(4) 0.012(4) 0.012(4) C36 0.033(4) 0.021(4) 0.025(4) 0.015(3) 0.007(3) 0.007(3) C37 0.031(5) 0.030(5) 0.029(5) 0.011(4) 0.002(4) 0.001(4) C38 0.029(5) 0.040(5) 0.033(5) 0.007(4) 0.010(4) 0.001(4) C39 0.049(5) 0.035(5) 0.024(5) 0.012(4) 0.016(4) 0.011(4) C40 0.058(6) 0.029(5) 0.020(5) 0.000(4) -0.003(4) 0.016(4) C41 0.030(4) 0.028(5) 0.029(5) 0.009(4) 0.001(4) 0.008(4) C42 0.030(5) 0.031(5) 0.034(5) 0.019(4) 0.010(4) 0.004(4) C43 0.037(5) 0.043(5) 0.035(5) 0.027(4) 0.006(4) 0.013(4) C44 0.028(5) 0.079(8) 0.032(5) 0.033(5) -0.006(4) -0.006(5) C45 0.029(5) 0.093(9) 0.086(9) 0.075(8) 0.007(5) 0.018(6) C46 0.036(5) 0.050(6) 0.079(8) 0.049(6) 0.014(5) 0.013(5) C47 0.036(5) 0.032(5) 0.059(6) 0.030(5) 0.011(4) 0.008(4) C48 0.021(4) 0.031(5) 0.025(4) 0.015(4) 0.005(3) 0.008(3) C49 0.031(4) 0.032(5) 0.027(5) 0.018(4) 0.006(3) 0.012(4) C50 0.019(4) 0.051(6) 0.028(5) 0.023(4) -0.002(3) -0.004(4) C51 0.042(5) 0.026(5) 0.049(6) 0.024(4) 0.005(4) 0.002(4) C52 0.048(6) 0.027(5) 0.067(7) 0.019(5) 0.009(5) 0.006(4) C53 0.027(5) 0.037(5) 0.044(6) 0.017(4) 0.013(4) 0.007(4) C54 0.023(4) 0.029(5) 0.023(4) 0.006(4) 0.001(3) 0.005(3) C55 0.029(4) 0.026(5) 0.035(5) 0.011(4) 0.009(4) 0.005(4) C56 0.037(5) 0.026(5) 0.047(6) 0.007(4) 0.009(4) 0.007(4) C57 0.039(5) 0.042(6) 0.052(7) -0.010(5) 0.000(5) 0.019(4) C58 0.034(5) 0.076(7) 0.021(5) 0.003(5) -0.001(4) 0.015(5) C59 0.030(5) 0.036(5) 0.032(5) 0.009(4) -0.002(4) 0.013(4) C60 0.022(4) 0.024(4) 0.022(4) 0.008(3) 0.000(3) 0.004(3) C61 0.035(5) 0.027(4) 0.027(5) 0.014(4) 0.006(4) 0.013(4) C62 0.045(5) 0.036(5) 0.025(5) 0.019(4) 0.008(4) 0.017(4) C63 0.042(5) 0.048(6) 0.029(5) 0.014(4) -0.003(4) 0.023(4) C64 0.036(5) 0.045(6) 0.033(5) 0.008(4) -0.009(4) 0.007(4) C65 0.035(5) 0.034(5) 0.025(5) 0.014(4) -0.002(4) 0.005(4) B1 0.044(8) 0.036(8) 0.161(17) 0.041(10) -0.009(9) -0.004(6) F1 0.072(4) 0.078(5) 0.151(7) 0.057(5) -0.009(4) -0.007(4) F2 0.096(5) 0.078(5) 0.130(7) 0.047(5) -0.023(5) -0.015(4) F3 0.059(4) 0.053(4) 0.161(7) 0.016(4) -0.023(4) 0.013(3) F4 0.228(10) 0.109(7) 0.216(11) 0.078(7) 0.172(9) 0.094(7) C66 0.064(10) 0.140(15) 0.45(3) 0.20(2) -0.037(15) -0.026(10) Cl1 0.119(3) 0.102(3) 0.178(5) 0.002(3) -0.014(3) 0.026(3) Cl2 0.097(3) 0.114(3) 0.266(6) 0.124(4) -0.018(3) 0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.835(9) . ? Rh1 N3 2.087(6) . ? Rh1 P1 2.265(2) . ? Rh1 S1 2.406(2) . ? Rh1 Rh3 3.0773(8) . ? Rh1 Rh2 5.0624(8) . ? Rh2 C2 1.815(8) . ? Rh2 N1 2.103(6) . ? Rh2 P2 2.261(2) . ? Rh2 S2 2.4101(19) . ? Rh2 Rh3 3.0341(8) . ? Rh3 C3 1.830(8) . ? Rh3 P3 2.272(2) . ? Rh3 S1 2.3917(19) . ? Rh3 S2 2.4029(19) . ? P1 C18 1.800(8) . ? P1 C12 1.832(8) . ? P1 C24 1.841(7) . ? P2 C36 1.817(7) . ? P2 C42 1.822(8) . ? P2 C30 1.842(7) . ? P3 C54 1.825(8) . ? P3 C48 1.826(7) . ? P3 C60 1.831(7) . ? S1 C4 1.744(8) . ? S2 C8 1.760(7) . ? N1 C4 1.336(9) . ? N1 C5 1.398(9) . ? N2 C4 1.353(8) . ? N2 C6 1.377(9) . ? N2 C7 1.459(9) . ? N3 C8 1.335(9) . ? N3 C9 1.364(8) . ? N4 C8 1.356(9) . ? N4 C10 1.381(9) . ? N4 C11 1.455(9) . ? O1 C1 1.130(9) . ? O2 C2 1.144(9) . ? O3 C3 1.137(8) . ? C5 C6 1.352(10) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C9 C10 1.347(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.377(11) . ? C12 C17 1.384(11) . ? C13 C14 1.405(11) . ? C13 H13 0.9300 . ? C14 C15 1.373(13) . ? C14 H14 0.9300 . ? C15 C16 1.376(12) . ? C15 H15 0.9300 . ? C16 C17 1.378(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.396(10) . ? C18 C23 1.397(10) . ? C19 C20 1.394(10) . ? C19 H19 0.9300 . ? C20 C21 1.393(11) . ? C20 H20 0.9300 . ? C21 C22 1.381(10) . ? C21 H21 0.9300 . ? C22 C23 1.372(10) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.371(10) . ? C24 C25 1.402(10) . ? C25 C26 1.395(11) . ? C25 H25 0.9300 . ? C26 C27 1.378(12) . ? C26 H26 0.9300 . ? C27 C28 1.365(11) . ? C27 H27 0.9300 . ? C28 C29 1.401(10) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.379(11) . ? C30 C31 1.401(11) . ? C31 C32 1.394(11) . ? C31 H31 0.9300 . ? C32 C33 1.389(13) . ? C32 H32 0.9300 . ? C33 C34 1.366(13) . ? C33 H33 0.9300 . ? C34 C35 1.381(10) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.389(10) . ? C36 C41 1.398(10) . ? C37 C38 1.362(10) . ? C37 H37 0.9300 . ? C38 C39 1.386(11) . ? C38 H38 0.9300 . ? C39 C40 1.368(11) . ? C39 H39 0.9300 . ? C40 C41 1.374(10) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.393(11) . ? C42 C47 1.404(11) . ? C43 C44 1.398(11) . ? C43 H43 0.9300 . ? C44 C45 1.381(14) . ? C44 H44 0.9300 . ? C45 C46 1.376(14) . ? C45 H45 0.9300 . ? C46 C47 1.376(12) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.390(10) . ? C48 C53 1.390(10) . ? C49 C50 1.384(10) . ? C49 H49 0.9300 . ? C50 C51 1.387(11) . ? C50 H50 0.9300 . ? C51 C52 1.390(11) . ? C51 H51 0.9300 . ? C52 C53 1.381(10) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.384(10) . ? C54 C59 1.411(10) . ? C55 C56 1.382(11) . ? C55 H55 0.9300 . ? C56 C57 1.367(12) . ? C56 H56 0.9300 . ? C57 C58 1.376(12) . ? C57 H57 0.9300 . ? C58 C59 1.394(11) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 C65 1.388(9) . ? C60 C61 1.405(10) . ? C61 C62 1.383(10) . ? C61 H61 0.9300 . ? C62 C63 1.376(10) . ? C62 H62 0.9300 . ? C63 C64 1.378(11) . ? C63 H63 0.9300 . ? C64 C65 1.393(10) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? B1 F4 1.264(19) . ? B1 F3 1.339(14) . ? B1 F1 1.400(13) . ? B1 F2 1.439(17) . ? C66 Cl2 1.664(13) . ? C66 Cl1 1.667(16) . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? 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 C1 Rh1 N3 176.2(3) . . ? C1 Rh1 P1 90.7(3) . . ? N3 Rh1 P1 91.84(17) . . ? C1 Rh1 S1 88.9(3) . . ? N3 Rh1 S1 88.61(17) . . ? P1 Rh1 S1 178.28(7) . . ? C1 Rh1 Rh3 91.5(3) . . ? N3 Rh1 Rh3 89.16(16) . . ? P1 Rh1 Rh3 128.44(6) . . ? S1 Rh1 Rh3 49.90(5) . . ? C1 Rh1 Rh2 120.4(3) . . ? N3 Rh1 Rh2 59.09(16) . . ? P1 Rh1 Rh2 135.77(5) . . ? S1 Rh1 Rh2 43.38(5) . . ? Rh3 Rh1 Rh2 33.798(14) . . ? C2 Rh2 N1 171.3(3) . . ? C2 Rh2 P2 94.2(3) . . ? N1 Rh2 P2 89.63(17) . . ? C2 Rh2 S2 88.6(2) . . ? N1 Rh2 S2 89.07(17) . . ? P2 Rh2 S2 168.86(7) . . ? C2 Rh2 Rh3 98.3(2) . . ? N1 Rh2 Rh3 86.69(17) . . ? P2 Rh2 Rh3 118.06(6) . . ? S2 Rh2 Rh3 50.81(5) . . ? C2 Rh2 Rh1 122.9(2) . . ? N1 Rh2 Rh1 58.85(16) . . ? P2 Rh2 Rh1 130.33(5) . . ? S2 Rh2 Rh1 41.11(4) . . ? Rh3 Rh2 Rh1 34.345(14) . . ? C3 Rh3 P3 86.9(2) . . ? C3 Rh3 S1 86.9(2) . . ? P3 Rh3 S1 167.45(7) . . ? C3 Rh3 S2 168.8(2) . . ? P3 Rh3 S2 92.32(7) . . ? S1 Rh3 S2 95.92(6) . . ? C3 Rh3 Rh2 118.7(2) . . ? P3 Rh3 Rh2 107.34(5) . . ? S1 Rh3 Rh2 85.20(5) . . ? S2 Rh3 Rh2 51.03(5) . . ? C3 Rh3 Rh1 108.4(2) . . ? P3 Rh3 Rh1 122.17(5) . . ? S1 Rh3 Rh1 50.31(5) . . ? S2 Rh3 Rh1 81.47(5) . . ? Rh2 Rh3 Rh1 111.86(2) . . ? C18 P1 C12 104.7(3) . . ? C18 P1 C24 103.8(3) . . ? C12 P1 C24 103.4(4) . . ? C18 P1 Rh1 112.4(2) . . ? C12 P1 Rh1 115.3(3) . . ? C24 P1 Rh1 115.9(2) . . ? C36 P2 C42 105.9(4) . . ? C36 P2 C30 105.0(4) . . ? C42 P2 C30 100.1(3) . . ? C36 P2 Rh2 106.8(2) . . ? C42 P2 Rh2 118.3(3) . . ? C30 P2 Rh2 119.3(3) . . ? C54 P3 C48 105.2(3) . . ? C54 P3 C60 102.4(3) . . ? C48 P3 C60 103.6(3) . . ? C54 P3 Rh3 117.9(2) . . ? C48 P3 Rh3 116.3(2) . . ? C60 P3 Rh3 109.7(2) . . ? C4 S1 Rh3 109.1(3) . . ? C4 S1 Rh1 108.7(3) . . ? Rh3 S1 Rh1 79.79(6) . . ? C8 S2 Rh3 109.8(3) . . ? C8 S2 Rh2 106.1(2) . . ? Rh3 S2 Rh2 78.16(6) . . ? C4 N1 C5 105.5(6) . . ? C4 N1 Rh2 128.1(5) . . ? C5 N1 Rh2 125.0(5) . . ? C4 N2 C6 108.3(6) . . ? C4 N2 C7 126.8(6) . . ? C6 N2 C7 124.8(6) . . ? C8 N3 C9 106.6(6) . . ? C8 N3 Rh1 124.3(5) . . ? C9 N3 Rh1 128.1(5) . . ? C8 N4 C10 106.2(6) . . ? C8 N4 C11 128.9(6) . . ? C10 N4 C11 124.8(6) . . ? O1 C1 Rh1 178.8(8) . . ? O2 C2 Rh2 173.2(8) . . ? O3 C3 Rh3 177.0(7) . . ? N1 C4 N2 110.3(6) . . ? N1 C4 S1 126.5(5) . . ? N2 C4 S1 123.2(5) . . ? C6 C5 N1 109.8(7) . . ? C6 C5 H5 125.1 . . ? N1 C5 H5 125.1 . . ? C5 C6 N2 106.0(7) . . ? C5 C6 H6 127.0 . . ? N2 C6 H6 127.0 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 N4 110.5(6) . . ? N3 C8 S2 127.1(6) . . ? N4 C8 S2 122.2(6) . . ? C10 C9 N3 109.2(7) . . ? C10 C9 H9 125.4 . . ? N3 C9 H9 125.4 . . ? C9 C10 N4 107.5(7) . . ? C9 C10 H10 126.2 . . ? N4 C10 H10 126.2 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.4(7) . . ? C13 C12 P1 118.4(6) . . ? C17 C12 P1 122.9(6) . . ? C12 C13 C14 120.9(8) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C15 C14 C13 119.2(9) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 120.2(8) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 120.1(8) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 121.1(8) . . ? C16 C17 H17 119.5 . . ? C12 C17 H17 119.5 . . ? C19 C18 C23 118.2(7) . . ? C19 C18 P1 122.8(5) . . ? C23 C18 P1 118.9(6) . . ? C20 C19 C18 120.7(7) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 119.5(7) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 120.1(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.1(7) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 121.4(7) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? C29 C24 C25 119.4(7) . . ? C29 C24 P1 122.1(6) . . ? C25 C24 P1 118.5(6) . . ? C26 C25 C24 119.0(8) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C27 C26 C25 120.8(8) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 120.1(8) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 119.7(8) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 120.9(8) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C35 C30 C31 118.9(7) . . ? C35 C30 P2 124.6(6) . . ? C31 C30 P2 116.5(6) . . ? C32 C31 C30 119.2(8) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C33 C32 C31 120.7(9) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 119.5(8) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 120.2(9) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C30 C35 C34 121.4(8) . . ? C30 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C37 C36 C41 117.0(7) . . ? C37 C36 P2 123.3(6) . . ? C41 C36 P2 119.2(6) . . ? C38 C37 C36 122.1(8) . . ? C38 C37 H37 118.9 . . ? C36 C37 H37 118.9 . . ? C37 C38 C39 119.4(8) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C40 C39 C38 120.3(8) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 119.8(8) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C40 C41 C36 121.4(7) . . ? C40 C41 H41 119.3 . . ? C36 C41 H41 119.3 . . ? C43 C42 C47 119.0(8) . . ? C43 C42 P2 119.7(6) . . ? C47 C42 P2 121.0(7) . . ? C42 C43 C44 120.1(8) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 119.9(9) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.0(9) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 121.0(9) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C46 C47 C42 119.9(9) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? C49 C48 C53 118.5(7) . . ? C49 C48 P3 122.5(6) . . ? C53 C48 P3 119.1(5) . . ? C50 C49 C48 120.5(7) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 120.6(7) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C50 C51 C52 119.3(7) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? C53 C52 C51 119.8(8) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C48 121.3(8) . . ? C52 C53 H53 119.4 . . ? C48 C53 H53 119.4 . . ? C55 C54 C59 117.2(7) . . ? C55 C54 P3 122.3(6) . . ? C59 C54 P3 120.4(6) . . ? C56 C55 C54 122.7(8) . . ? C56 C55 H55 118.7 . . ? C54 C55 H55 118.7 . . ? C57 C56 C55 118.6(8) . . ? C57 C56 H56 120.7 . . ? C55 C56 H56 120.7 . . ? C56 C57 C58 121.5(8) . . ? C56 C57 H57 119.3 . . ? C58 C57 H57 119.3 . . ? C57 C58 C59 119.5(8) . . ? C57 C58 H58 120.2 . . ? C59 C58 H58 120.2 . . ? C58 C59 C54 120.3(8) . . ? C58 C59 H59 119.8 . . ? C54 C59 H59 119.8 . . ? C65 C60 C61 118.2(7) . . ? C65 C60 P3 123.0(6) . . ? C61 C60 P3 118.8(5) . . ? C62 C61 C60 120.1(7) . . ? C62 C61 H61 119.9 . . ? C60 C61 H61 119.9 . . ? C63 C62 C61 120.8(7) . . ? C63 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C62 C63 C64 120.1(8) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C65 119.5(8) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C60 C65 C64 121.3(7) . . ? C60 C65 H65 119.4 . . ? C64 C65 H65 119.4 . . ? F4 B1 F3 114.8(15) . . ? F4 B1 F1 116.0(13) . . ? F3 B1 F1 108.6(11) . . ? F4 B1 F2 106.9(11) . . ? F3 B1 F2 105.1(12) . . ? F1 B1 F2 104.3(12) . . ? Cl2 C66 Cl1 122.8(9) . . ? Cl2 C66 H66A 106.6 . . ? Cl1 C66 H66A 106.6 . . ? Cl2 C66 H66B 106.6 . . ? Cl1 C66 H66B 106.6 . . ? H66A C66 H66B 106.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 Rh2 C2 84.9(4) . . . . ? N3 Rh1 Rh2 C2 -99.6(4) . . . . ? P1 Rh1 Rh2 C2 -43.7(3) . . . . ? S1 Rh1 Rh2 C2 134.1(3) . . . . ? Rh3 Rh1 Rh2 C2 50.1(3) . . . . ? C1 Rh1 Rh2 N1 -105.2(4) . . . . ? N3 Rh1 Rh2 N1 70.4(3) . . . . ? P1 Rh1 Rh2 N1 126.2(2) . . . . ? S1 Rh1 Rh2 N1 -56.0(2) . . . . ? Rh3 Rh1 Rh2 N1 -139.91(19) . . . . ? C1 Rh1 Rh2 P2 -46.7(3) . . . . ? N3 Rh1 Rh2 P2 128.8(2) . . . . ? P1 Rh1 Rh2 P2 -175.32(10) . . . . ? S1 Rh1 Rh2 P2 2.52(9) . . . . ? Rh3 Rh1 Rh2 P2 -81.44(7) . . . . ? C1 Rh1 Rh2 S2 123.2(3) . . . . ? N3 Rh1 Rh2 S2 -61.23(19) . . . . ? P1 Rh1 Rh2 S2 -5.38(10) . . . . ? S1 Rh1 Rh2 S2 172.45(9) . . . . ? Rh3 Rh1 Rh2 S2 88.49(7) . . . . ? C1 Rh1 Rh2 Rh3 34.7(3) . . . . ? N3 Rh1 Rh2 Rh3 -149.72(19) . . . . ? P1 Rh1 Rh2 Rh3 -93.87(8) . . . . ? S1 Rh1 Rh2 Rh3 83.96(7) . . . . ? C2 Rh2 Rh3 C3 93.3(4) . . . . ? N1 Rh2 Rh3 C3 -93.9(3) . . . . ? P2 Rh2 Rh3 C3 -6.1(3) . . . . ? S2 Rh2 Rh3 C3 174.6(3) . . . . ? Rh1 Rh2 Rh3 C3 -127.4(3) . . . . ? C2 Rh2 Rh3 P3 -2.8(3) . . . . ? N1 Rh2 Rh3 P3 170.08(17) . . . . ? P2 Rh2 Rh3 P3 -102.10(8) . . . . ? S2 Rh2 Rh3 P3 78.58(8) . . . . ? Rh1 Rh2 Rh3 P3 136.57(6) . . . . ? C2 Rh2 Rh3 S1 177.1(3) . . . . ? N1 Rh2 Rh3 S1 -10.09(17) . . . . ? P2 Rh2 Rh3 S1 77.72(8) . . . . ? S2 Rh2 Rh3 S1 -101.59(7) . . . . ? Rh1 Rh2 Rh3 S1 -43.60(5) . . . . ? C2 Rh2 Rh3 S2 -81.4(3) . . . . ? N1 Rh2 Rh3 S2 91.50(17) . . . . ? P2 Rh2 Rh3 S2 179.32(8) . . . . ? Rh1 Rh2 Rh3 S2 58.00(6) . . . . ? C2 Rh2 Rh3 Rh1 -139.3(3) . . . . ? N1 Rh2 Rh3 Rh1 33.51(16) . . . . ? P2 Rh2 Rh3 Rh1 121.32(6) . . . . ? S2 Rh2 Rh3 Rh1 -58.00(6) . . . . ? C1 Rh1 Rh3 C3 -17.9(3) . . . . ? N3 Rh1 Rh3 C3 158.4(3) . . . . ? P1 Rh1 Rh3 C3 -110.0(2) . . . . ? S1 Rh1 Rh3 C3 69.5(2) . . . . ? Rh2 Rh1 Rh3 C3 132.7(2) . . . . ? C1 Rh1 Rh3 P3 80.2(3) . . . . ? N3 Rh1 Rh3 P3 -103.54(17) . . . . ? P1 Rh1 Rh3 P3 -11.87(10) . . . . ? S1 Rh1 Rh3 P3 167.56(9) . . . . ? Rh2 Rh1 Rh3 P3 -129.18(7) . . . . ? C1 Rh1 Rh3 S1 -87.3(3) . . . . ? N3 Rh1 Rh3 S1 88.89(17) . . . . ? P1 Rh1 Rh3 S1 -179.43(10) . . . . ? Rh2 Rh1 Rh3 S1 63.26(6) . . . . ? C1 Rh1 Rh3 S2 167.6(3) . . . . ? N3 Rh1 Rh3 S2 -16.17(17) . . . . ? P1 Rh1 Rh3 S2 75.51(8) . . . . ? S1 Rh1 Rh3 S2 -105.06(8) . . . . ? Rh2 Rh1 Rh3 S2 -41.81(5) . . . . ? C1 Rh1 Rh3 Rh2 -150.6(3) . . . . ? N3 Rh1 Rh3 Rh2 25.64(16) . . . . ? P1 Rh1 Rh3 Rh2 117.32(7) . . . . ? S1 Rh1 Rh3 Rh2 -63.26(6) . . . . ? C1 Rh1 P1 C18 -158.5(4) . . . . ? N3 Rh1 P1 C18 24.4(3) . . . . ? S1 Rh1 P1 C18 -81(3) . . . . ? Rh3 Rh1 P1 C18 -66.0(3) . . . . ? Rh2 Rh1 P1 C18 -20.9(3) . . . . ? C1 Rh1 P1 C12 81.7(4) . . . . ? N3 Rh1 P1 C12 -95.4(3) . . . . ? S1 Rh1 P1 C12 159(2) . . . . ? Rh3 Rh1 P1 C12 174.2(3) . . . . ? Rh2 Rh1 P1 C12 -140.7(3) . . . . ? C1 Rh1 P1 C24 -39.3(4) . . . . ? N3 Rh1 P1 C24 143.6(3) . . . . ? S1 Rh1 P1 C24 39(3) . . . . ? Rh3 Rh1 P1 C24 53.2(3) . . . . ? Rh2 Rh1 P1 C24 98.4(3) . . . . ? C2 Rh2 P2 C36 -142.4(4) . . . . ? N1 Rh2 P2 C36 45.4(3) . . . . ? S2 Rh2 P2 C36 -37.9(5) . . . . ? Rh3 Rh2 P2 C36 -40.7(3) . . . . ? Rh1 Rh2 P2 C36 -1.5(3) . . . . ? C2 Rh2 P2 C42 98.4(4) . . . . ? N1 Rh2 P2 C42 -73.8(3) . . . . ? S2 Rh2 P2 C42 -157.1(4) . . . . ? Rh3 Rh2 P2 C42 -159.8(3) . . . . ? Rh1 Rh2 P2 C42 -120.6(3) . . . . ? C2 Rh2 P2 C30 -23.7(4) . . . . ? N1 Rh2 P2 C30 164.1(3) . . . . ? S2 Rh2 P2 C30 80.8(5) . . . . ? Rh3 Rh2 P2 C30 78.1(3) . . . . ? Rh1 Rh2 P2 C30 117.3(3) . . . . ? C3 Rh3 P3 C54 160.7(4) . . . . ? S1 Rh3 P3 C54 100.7(4) . . . . ? S2 Rh3 P3 C54 -30.4(3) . . . . ? Rh2 Rh3 P3 C54 -80.1(3) . . . . ? Rh1 Rh3 P3 C54 50.9(3) . . . . ? C3 Rh3 P3 C48 -72.9(4) . . . . ? S1 Rh3 P3 C48 -133.0(4) . . . . ? S2 Rh3 P3 C48 95.9(3) . . . . ? Rh2 Rh3 P3 C48 46.2(3) . . . . ? Rh1 Rh3 P3 C48 177.3(3) . . . . ? C3 Rh3 P3 C60 44.2(3) . . . . ? S1 Rh3 P3 C60 -15.9(5) . . . . ? S2 Rh3 P3 C60 -147.0(3) . . . . ? Rh2 Rh3 P3 C60 163.3(2) . . . . ? Rh1 Rh3 P3 C60 -65.6(3) . . . . ? C3 Rh3 S1 C4 136.4(3) . . . . ? P3 Rh3 S1 C4 -163.5(4) . . . . ? S2 Rh3 S1 C4 -32.7(3) . . . . ? Rh2 Rh3 S1 C4 17.3(3) . . . . ? Rh1 Rh3 S1 C4 -106.4(3) . . . . ? C3 Rh3 S1 Rh1 -117.1(2) . . . . ? P3 Rh3 S1 Rh1 -57.0(3) . . . . ? S2 Rh3 S1 Rh1 73.76(6) . . . . ? Rh2 Rh3 S1 Rh1 123.72(4) . . . . ? C1 Rh1 S1 C4 -160.3(4) . . . . ? N3 Rh1 S1 C4 16.8(3) . . . . ? P1 Rh1 S1 C4 122(2) . . . . ? Rh3 Rh1 S1 C4 106.8(3) . . . . ? Rh2 Rh1 S1 C4 60.5(3) . . . . ? C1 Rh1 S1 Rh3 92.9(3) . . . . ? N3 Rh1 S1 Rh3 -90.07(16) . . . . ? P1 Rh1 S1 Rh3 15(3) . . . . ? Rh2 Rh1 S1 Rh3 -46.32(4) . . . . ? C3 Rh3 S2 C8 -128.0(12) . . . . ? P3 Rh3 S2 C8 146.4(3) . . . . ? S1 Rh3 S2 C8 -24.1(3) . . . . ? Rh2 Rh3 S2 C8 -103.0(3) . . . . ? Rh1 Rh3 S2 C8 24.2(3) . . . . ? C3 Rh3 S2 Rh2 -25.0(12) . . . . ? P3 Rh3 S2 Rh2 -110.54(6) . . . . ? S1 Rh3 S2 Rh2 78.93(6) . . . . ? Rh1 Rh3 S2 Rh2 127.26(4) . . . . ? C2 Rh2 S2 C8 -150.7(4) . . . . ? N1 Rh2 S2 C8 20.9(3) . . . . ? P2 Rh2 S2 C8 104.3(4) . . . . ? Rh3 Rh2 S2 C8 107.4(3) . . . . ? Rh1 Rh2 S2 C8 60.7(3) . . . . ? C2 Rh2 S2 Rh3 101.9(3) . . . . ? N1 Rh2 S2 Rh3 -86.49(17) . . . . ? P2 Rh2 S2 Rh3 -3.1(4) . . . . ? Rh1 Rh2 S2 Rh3 -46.69(4) . . . . ? C2 Rh2 N1 C4 126.2(19) . . . . ? P2 Rh2 N1 C4 -117.5(6) . . . . ? S2 Rh2 N1 C4 51.5(6) . . . . ? Rh3 Rh2 N1 C4 0.7(6) . . . . ? Rh1 Rh2 N1 C4 22.0(5) . . . . ? C2 Rh2 N1 C5 -38(2) . . . . ? P2 Rh2 N1 C5 78.2(5) . . . . ? S2 Rh2 N1 C5 -112.8(5) . . . . ? Rh3 Rh2 N1 C5 -163.6(6) . . . . ? Rh1 Rh2 N1 C5 -142.3(6) . . . . ? C1 Rh1 N3 C8 106(5) . . . . ? P1 Rh1 N3 C8 -122.7(6) . . . . ? S1 Rh1 N3 C8 55.7(6) . . . . ? Rh3 Rh1 N3 C8 5.8(6) . . . . ? Rh2 Rh1 N3 C8 22.0(5) . . . . ? C1 Rh1 N3 C9 -61(5) . . . . ? P1 Rh1 N3 C9 70.5(6) . . . . ? S1 Rh1 N3 C9 -111.2(6) . . . . ? Rh3 Rh1 N3 C9 -161.1(6) . . . . ? Rh2 Rh1 N3 C9 -144.8(7) . . . . ? N3 Rh1 C1 O1 -56(46) . . . . ? P1 Rh1 C1 O1 173(100) . . . . ? S1 Rh1 C1 O1 -6(44) . . . . ? Rh3 Rh1 C1 O1 44(44) . . . . ? Rh2 Rh1 C1 O1 26(44) . . . . ? N1 Rh2 C2 O2 -26(7) . . . . ? P2 Rh2 C2 O2 -142(6) . . . . ? S2 Rh2 C2 O2 49(6) . . . . ? Rh3 Rh2 C2 O2 99(6) . . . . ? Rh1 Rh2 C2 O2 73(6) . . . . ? P3 Rh3 C3 O3 128(14) . . . . ? S1 Rh3 C3 O3 -63(14) . . . . ? S2 Rh3 C3 O3 42(15) . . . . ? Rh2 Rh3 C3 O3 20(14) . . . . ? Rh1 Rh3 C3 O3 -109(14) . . . . ? C5 N1 C4 N2 0.2(8) . . . . ? Rh2 N1 C4 N2 -166.5(5) . . . . ? C5 N1 C4 S1 -177.3(5) . . . . ? Rh2 N1 C4 S1 16.0(10) . . . . ? C6 N2 C4 N1 0.2(8) . . . . ? C7 N2 C4 N1 178.5(7) . . . . ? C6 N2 C4 S1 177.8(6) . . . . ? C7 N2 C4 S1 -3.9(11) . . . . ? Rh3 S1 C4 N1 -25.3(7) . . . . ? Rh1 S1 C4 N1 -110.7(6) . . . . ? Rh3 S1 C4 N2 157.5(6) . . . . ? Rh1 S1 C4 N2 72.1(6) . . . . ? C4 N1 C5 C6 -0.5(8) . . . . ? Rh2 N1 C5 C6 166.7(5) . . . . ? N1 C5 C6 N2 0.6(9) . . . . ? C4 N2 C6 C5 -0.5(8) . . . . ? C7 N2 C6 C5 -178.8(7) . . . . ? C9 N3 C8 N4 -0.1(8) . . . . ? Rh1 N3 C8 N4 -169.3(5) . . . . ? C9 N3 C8 S2 -174.7(6) . . . . ? Rh1 N3 C8 S2 16.1(9) . . . . ? C10 N4 C8 N3 0.7(8) . . . . ? C11 N4 C8 N3 176.7(7) . . . . ? C10 N4 C8 S2 175.6(5) . . . . ? C11 N4 C8 S2 -8.3(11) . . . . ? Rh3 S2 C8 N3 -33.3(7) . . . . ? Rh2 S2 C8 N3 -116.2(6) . . . . ? Rh3 S2 C8 N4 152.7(5) . . . . ? Rh2 S2 C8 N4 69.7(6) . . . . ? C8 N3 C9 C10 -0.6(8) . . . . ? Rh1 N3 C9 C10 168.1(5) . . . . ? N3 C9 C10 N4 1.1(9) . . . . ? C8 N4 C10 C9 -1.1(8) . . . . ? C11 N4 C10 C9 -177.3(7) . . . . ? C18 P1 C12 C13 -95.2(7) . . . . ? C24 P1 C12 C13 156.4(6) . . . . ? Rh1 P1 C12 C13 28.9(7) . . . . ? C18 P1 C12 C17 78.6(7) . . . . ? C24 P1 C12 C17 -29.8(7) . . . . ? Rh1 P1 C12 C17 -157.3(6) . . . . ? C17 C12 C13 C14 -4.0(12) . . . . ? P1 C12 C13 C14 170.1(7) . . . . ? C12 C13 C14 C15 3.1(13) . . . . ? C13 C14 C15 C16 -0.4(14) . . . . ? C14 C15 C16 C17 -1.4(14) . . . . ? C15 C16 C17 C12 0.5(13) . . . . ? C13 C12 C17 C16 2.2(12) . . . . ? P1 C12 C17 C16 -171.6(6) . . . . ? C12 P1 C18 C19 -4.9(7) . . . . ? C24 P1 C18 C19 103.2(7) . . . . ? Rh1 P1 C18 C19 -130.7(6) . . . . ? C12 P1 C18 C23 173.9(6) . . . . ? C24 P1 C18 C23 -78.0(6) . . . . ? Rh1 P1 C18 C23 48.1(6) . . . . ? C23 C18 C19 C20 -0.3(11) . . . . ? P1 C18 C19 C20 178.5(6) . . . . ? C18 C19 C20 C21 1.4(12) . . . . ? C19 C20 C21 C22 -1.0(12) . . . . ? C20 C21 C22 C23 -0.4(12) . . . . ? C21 C22 C23 C18 1.5(12) . . . . ? C19 C18 C23 C22 -1.1(11) . . . . ? P1 C18 C23 C22 -180.0(6) . . . . ? C18 P1 C24 C29 22.0(7) . . . . ? C12 P1 C24 C29 131.0(6) . . . . ? Rh1 P1 C24 C29 -101.9(6) . . . . ? C18 P1 C24 C25 -159.5(6) . . . . ? C12 P1 C24 C25 -50.4(7) . . . . ? Rh1 P1 C24 C25 76.7(6) . . . . ? C29 C24 C25 C26 -0.8(11) . . . . ? P1 C24 C25 C26 -179.3(6) . . . . ? C24 C25 C26 C27 0.6(12) . . . . ? C25 C26 C27 C28 -0.5(13) . . . . ? C26 C27 C28 C29 0.5(13) . . . . ? C25 C24 C29 C28 0.8(11) . . . . ? P1 C24 C29 C28 179.3(6) . . . . ? C27 C28 C29 C24 -0.6(12) . . . . ? C36 P2 C30 C35 -0.9(7) . . . . ? C42 P2 C30 C35 108.7(7) . . . . ? Rh2 P2 C30 C35 -120.5(6) . . . . ? C36 P2 C30 C31 -177.9(6) . . . . ? C42 P2 C30 C31 -68.3(7) . . . . ? Rh2 P2 C30 C31 62.4(7) . . . . ? C35 C30 C31 C32 1.4(12) . . . . ? P2 C30 C31 C32 178.6(6) . . . . ? C30 C31 C32 C33 -0.2(13) . . . . ? C31 C32 C33 C34 -1.9(14) . . . . ? C32 C33 C34 C35 2.8(14) . . . . ? C31 C30 C35 C34 -0.5(12) . . . . ? P2 C30 C35 C34 -177.4(6) . . . . ? C33 C34 C35 C30 -1.7(13) . . . . ? C42 P2 C36 C37 21.1(7) . . . . ? C30 P2 C36 C37 126.4(6) . . . . ? Rh2 P2 C36 C37 -105.9(6) . . . . ? C42 P2 C36 C41 -167.2(6) . . . . ? C30 P2 C36 C41 -61.9(7) . . . . ? Rh2 P2 C36 C41 65.8(6) . . . . ? C41 C36 C37 C38 2.2(11) . . . . ? P2 C36 C37 C38 174.0(6) . . . . ? C36 C37 C38 C39 -1.0(12) . . . . ? C37 C38 C39 C40 0.5(12) . . . . ? C38 C39 C40 C41 -1.4(12) . . . . ? C39 C40 C41 C36 2.7(12) . . . . ? C37 C36 C41 C40 -3.0(11) . . . . ? P2 C36 C41 C40 -175.2(6) . . . . ? C36 P2 C42 C43 -133.8(6) . . . . ? C30 P2 C42 C43 117.2(6) . . . . ? Rh2 P2 C42 C43 -14.2(7) . . . . ? C36 P2 C42 C47 51.7(7) . . . . ? C30 P2 C42 C47 -57.3(7) . . . . ? Rh2 P2 C42 C47 171.3(5) . . . . ? C47 C42 C43 C44 0.6(11) . . . . ? P2 C42 C43 C44 -174.1(6) . . . . ? C42 C43 C44 C45 -0.4(12) . . . . ? C43 C44 C45 C46 0.0(13) . . . . ? C44 C45 C46 C47 0.2(14) . . . . ? C45 C46 C47 C42 0.0(13) . . . . ? C43 C42 C47 C46 -0.4(11) . . . . ? P2 C42 C47 C46 174.1(6) . . . . ? C54 P3 C48 C49 -28.3(7) . . . . ? C60 P3 C48 C49 78.9(7) . . . . ? Rh3 P3 C48 C49 -160.8(5) . . . . ? C54 P3 C48 C53 150.8(6) . . . . ? C60 P3 C48 C53 -102.0(7) . . . . ? Rh3 P3 C48 C53 18.3(7) . . . . ? C53 C48 C49 C50 1.6(11) . . . . ? P3 C48 C49 C50 -179.3(6) . . . . ? C48 C49 C50 C51 0.9(12) . . . . ? C49 C50 C51 C52 -1.3(12) . . . . ? C50 C51 C52 C53 -0.8(13) . . . . ? C51 C52 C53 C48 3.4(14) . . . . ? C49 C48 C53 C52 -3.8(12) . . . . ? P3 C48 C53 C52 177.1(7) . . . . ? C48 P3 C54 C55 138.4(6) . . . . ? C60 P3 C54 C55 30.4(7) . . . . ? Rh3 P3 C54 C55 -90.1(6) . . . . ? C48 P3 C54 C59 -40.3(7) . . . . ? C60 P3 C54 C59 -148.3(6) . . . . ? Rh3 P3 C54 C59 91.3(6) . . . . ? C59 C54 C55 C56 0.9(11) . . . . ? P3 C54 C55 C56 -177.8(6) . . . . ? C54 C55 C56 C57 2.1(12) . . . . ? C55 C56 C57 C58 -3.6(12) . . . . ? C56 C57 C58 C59 2.0(13) . . . . ? C57 C58 C59 C54 1.1(12) . . . . ? C55 C54 C59 C58 -2.5(11) . . . . ? P3 C54 C59 C58 176.3(6) . . . . ? C54 P3 C60 C65 96.4(7) . . . . ? C48 P3 C60 C65 -12.9(7) . . . . ? Rh3 P3 C60 C65 -137.6(6) . . . . ? C54 P3 C60 C61 -83.1(6) . . . . ? C48 P3 C60 C61 167.7(6) . . . . ? Rh3 P3 C60 C61 42.9(6) . . . . ? C65 C60 C61 C62 -0.5(11) . . . . ? P3 C60 C61 C62 179.0(6) . . . . ? C60 C61 C62 C63 1.2(12) . . . . ? C61 C62 C63 C64 -0.8(12) . . . . ? C62 C63 C64 C65 -0.4(13) . . . . ? C61 C60 C65 C64 -0.6(11) . . . . ? P3 C60 C65 C64 179.9(6) . . . . ? C63 C64 C65 C60 1.0(13) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.227 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.158 data_13 _database_code_depnum_ccdc_archive 'CCDC 826264' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C67 H61 N6 O3 P3 Rh3 S2, F6 P, 3(C H2 Cl2)' _chemical_formula_sum 'C70 H67 Cl6 F6 N6 O3 P4 Rh3 S2' _chemical_formula_weight 1863.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.673(2) _cell_length_b 16.606(3) _cell_length_c 21.794(4) _cell_angle_alpha 70.04(3) _cell_angle_beta 80.29(3) _cell_angle_gamma 76.75(3) _cell_volume 3846.2(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4328 _cell_measurement_theta_min 2.157 _cell_measurement_theta_max 22.057 _exptl_crystal_description plate _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 1.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686335 _exptl_absorpt_correction_T_max 0.950000 _exptl_absorpt_process_details 'SADABS V2.10 (Bruker 2003)' _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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.5 _diffrn_reflns_number 43773 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.42 _reflns_number_total 17297 _reflns_number_gt 13187 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART V5.054 (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART V5.054 (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT V6.41A (Bruker, 2002)' _computing_structure_solution 'SHELXS V6.12 (Bruker 2001)' _computing_structure_refinement 'SHELXL V6.12 (Bruker 2001)' _computing_molecular_graphics 'Bruker SHELXTL V6.14 (Bruker AXS, 2003)' _computing_publication_material 'Bruker SHELXTL V6.14 (Bruker AXS, 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. ; _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^)+(0.0575P)^2^+2.6362P] 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_number_reflns 17297 _refine_ls_number_parameters 979 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.26480(3) 0.75530(2) 0.168694(15) 0.01277(8) Uani 1 1 d . . . Rh2 Rh -0.09298(3) 0.83525(2) 0.314718(15) 0.01268(8) Uani 1 1 d . . . Rh3 Rh 0.10155(3) 0.91224(2) 0.207794(15) 0.01256(8) Uani 1 1 d . . . P1 P 0.28079(10) 0.73815(7) 0.06808(5) 0.0149(2) Uani 1 1 d . . . P2 P -0.13829(10) 0.82315(7) 0.42339(5) 0.0161(2) Uani 1 1 d . . . P3 P 0.20585(10) 1.00462(7) 0.22194(5) 0.0145(2) Uani 1 1 d . . . S1 S 0.23116(9) 0.78832(7) 0.27150(5) 0.0140(2) Uani 1 1 d . . . S2 S -0.04892(9) 0.83735(7) 0.20101(5) 0.0148(2) Uani 1 1 d . . . N1 N 0.0338(3) 0.7207(2) 0.33987(15) 0.0129(7) Uani 1 1 d . . . N2 N 0.0067(3) 0.6410(2) 0.38134(16) 0.0166(8) Uani 1 1 d . . . N3 N 0.1993(3) 0.6250(2) 0.35009(16) 0.0151(7) Uani 1 1 d . . . N4 N 0.1205(3) 0.6913(2) 0.20020(16) 0.0145(7) Uani 1 1 d . . . N5 N 0.1288(3) 0.6019(2) 0.21611(16) 0.0180(8) Uani 1 1 d . . . N6 N -0.0591(3) 0.6636(2) 0.22915(16) 0.0161(8) Uani 1 1 d . . . O1 O 0.4836(3) 0.8318(2) 0.11941(15) 0.0239(7) Uani 1 1 d . . . O2 O -0.2591(3) 1.0045(2) 0.26987(16) 0.0288(8) Uani 1 1 d . . . O3 O -0.0139(3) 1.0653(2) 0.10397(17) 0.0325(8) Uani 1 1 d . . . C1 C 0.1490(4) 0.7103(3) 0.32195(18) 0.0142(9) Uani 1 1 d . . . C2 C 0.1073(4) 0.5848(3) 0.38683(19) 0.0162(9) Uani 1 1 d . . . C3 C 0.1214(4) 0.4908(3) 0.4255(2) 0.0286(11) Uani 1 1 d . . . H3A H 0.0439 0.4767 0.4460 0.043 Uiso 1 1 calc R . . H3B H 0.1739 0.4778 0.4597 0.043 Uiso 1 1 calc R . . H3C H 0.1556 0.4557 0.3965 0.043 Uiso 1 1 calc R . . C4 C 0.3261(4) 0.5839(3) 0.3408(2) 0.0192(9) Uani 1 1 d . . . H4A H 0.3570 0.6084 0.2944 0.023 Uiso 1 1 calc R . . H4B H 0.3320 0.5204 0.3503 0.023 Uiso 1 1 calc R . . C5 C 0.4016(4) 0.5987(3) 0.3849(2) 0.0298(11) Uani 1 1 d . . . H5A H 0.4018 0.6611 0.3729 0.045 Uiso 1 1 calc R . . H5B H 0.4827 0.5673 0.3794 0.045 Uiso 1 1 calc R . . H5C H 0.3691 0.5771 0.4307 0.045 Uiso 1 1 calc R . . C6 C 0.0078(4) 0.7271(3) 0.20936(18) 0.0129(8) Uani 1 1 d . . . C7 C 0.0191(4) 0.5869(3) 0.2334(2) 0.0160(9) Uani 1 1 d . . . C8 C -0.0140(4) 0.5002(3) 0.2535(2) 0.0266(11) Uani 1 1 d . . . H8A H -0.0559 0.4966 0.2194 0.040 Uiso 1 1 calc R . . H8B H -0.0655 0.4914 0.2948 0.040 Uiso 1 1 calc R . . H8C H 0.0576 0.4550 0.2597 0.040 Uiso 1 1 calc R . . C9 C -0.1896(4) 0.6762(3) 0.2443(2) 0.0227(10) Uani 1 1 d . . . H9A H -0.2164 0.7233 0.2645 0.027 Uiso 1 1 calc R . . H9B H -0.2112 0.6219 0.2765 0.027 Uiso 1 1 calc R . . C10 C -0.2527(4) 0.6995(3) 0.1831(3) 0.0330(12) Uani 1 1 d . . . H10A H -0.2335 0.7542 0.1516 0.049 Uiso 1 1 calc R . . H10B H -0.3383 0.7065 0.1950 0.049 Uiso 1 1 calc R . . H10C H -0.2268 0.6528 0.1631 0.049 Uiso 1 1 calc R . . C11 C 0.3980(4) 0.8039(3) 0.1400(2) 0.0176(9) Uani 1 1 d . . . C12 C -0.1985(4) 0.9384(3) 0.2888(2) 0.0162(9) Uani 1 1 d . . . C13 C 0.0275(4) 1.0080(3) 0.1456(2) 0.0200(10) Uani 1 1 d . . . C14 C 0.1580(4) 0.6983(3) 0.0520(2) 0.0186(9) Uani 1 1 d . . . C15 C 0.1612(5) 0.6093(3) 0.0683(2) 0.0261(11) Uani 1 1 d . . . H15 H 0.2299 0.5691 0.0846 0.031 Uiso 1 1 calc R . . C16 C 0.0654(5) 0.5784(4) 0.0608(2) 0.0350(13) Uani 1 1 d . . . H16 H 0.0686 0.5174 0.0724 0.042 Uiso 1 1 calc R . . C17 C -0.0345(5) 0.6357(4) 0.0368(3) 0.0417(15) Uani 1 1 d . . . H17 H -0.0995 0.6142 0.0313 0.050 Uiso 1 1 calc R . . C18 C -0.0402(5) 0.7250(4) 0.0206(3) 0.0438(15) Uani 1 1 d . . . H18 H -0.1094 0.7644 0.0044 0.053 Uiso 1 1 calc R . . C19 C 0.0554(5) 0.7567(3) 0.0281(2) 0.0312(12) Uani 1 1 d . . . H19 H 0.0514 0.8177 0.0170 0.037 Uiso 1 1 calc R . . C20 C 0.4135(4) 0.6643(3) 0.0478(2) 0.0170(9) Uani 1 1 d . . . C21 C 0.4984(4) 0.6248(3) 0.0933(2) 0.0200(10) Uani 1 1 d . . . H21 H 0.4845 0.6346 0.1346 0.024 Uiso 1 1 calc R . . C22 C 0.6020(4) 0.5718(3) 0.0783(2) 0.0263(11) Uani 1 1 d . . . H22 H 0.6585 0.5452 0.1093 0.032 Uiso 1 1 calc R . . C23 C 0.6235(4) 0.5574(3) 0.0176(2) 0.0288(11) Uani 1 1 d . . . H23 H 0.6960 0.5232 0.0065 0.035 Uiso 1 1 calc R . . C24 C 0.5379(4) 0.5936(3) -0.0270(2) 0.0258(11) Uani 1 1 d . . . H24 H 0.5515 0.5823 -0.0678 0.031 Uiso 1 1 calc R . . C25 C 0.4338(4) 0.6456(3) -0.0120(2) 0.0192(9) Uani 1 1 d . . . H25 H 0.3755 0.6690 -0.0422 0.023 Uiso 1 1 calc R . . C26 C 0.2808(4) 0.8440(3) 0.00402(19) 0.0163(9) Uani 1 1 d . . . C27 C 0.2023(4) 0.9161(3) 0.0172(2) 0.0222(10) Uani 1 1 d . . . H27 H 0.1564 0.9086 0.0584 0.027 Uiso 1 1 calc R . . C28 C 0.1921(4) 0.9979(3) -0.0301(2) 0.0258(11) Uani 1 1 d . . . H28 H 0.1376 1.0458 -0.0216 0.031 Uiso 1 1 calc R . . C29 C 0.2613(4) 1.0095(3) -0.0893(2) 0.0259(11) Uani 1 1 d . . . H29 H 0.2552 1.0657 -0.1211 0.031 Uiso 1 1 calc R . . C30 C 0.3398(4) 0.9394(3) -0.1027(2) 0.0242(11) Uani 1 1 d . . . H30 H 0.3867 0.9479 -0.1438 0.029 Uiso 1 1 calc R . . C31 C 0.3500(4) 0.8566(3) -0.0563(2) 0.0218(10) Uani 1 1 d . . . H31 H 0.4038 0.8088 -0.0657 0.026 Uiso 1 1 calc R . . C32 C -0.2550(4) 0.7584(3) 0.4622(2) 0.0179(9) Uani 1 1 d . . . C33 C -0.2678(4) 0.6948(3) 0.4360(2) 0.0212(10) Uani 1 1 d . . . H33 H -0.2154 0.6852 0.3998 0.025 Uiso 1 1 calc R . . C34 C -0.3571(4) 0.6459(3) 0.4629(2) 0.0244(10) Uani 1 1 d . . . H34 H -0.3655 0.6031 0.4450 0.029 Uiso 1 1 calc R . . C35 C -0.4337(4) 0.6597(3) 0.5161(2) 0.0295(12) Uani 1 1 d . . . H35 H -0.4944 0.6263 0.5344 0.035 Uiso 1 1 calc R . . C36 C -0.4220(4) 0.7225(3) 0.5428(2) 0.0311(12) Uani 1 1 d . . . H36 H -0.4750 0.7317 0.5790 0.037 Uiso 1 1 calc R . . C37 C -0.3324(4) 0.7722(3) 0.5165(2) 0.0254(11) Uani 1 1 d . . . H37 H -0.3240 0.8145 0.5349 0.030 Uiso 1 1 calc R . . C38 C -0.1913(4) 0.9213(3) 0.4491(2) 0.0229(10) Uani 1 1 d . . . C39 C -0.2994(5) 0.9743(3) 0.4308(2) 0.0273(11) Uani 1 1 d . . . H39 H -0.3441 0.9607 0.4043 0.033 Uiso 1 1 calc R . . C40 C -0.3415(5) 1.0472(4) 0.4516(3) 0.0441(15) Uani 1 1 d . . . H40 H -0.4155 1.0830 0.4395 0.053 Uiso 1 1 calc R . . C41 C -0.2764(6) 1.0683(4) 0.4899(3) 0.0443(15) Uani 1 1 d . . . H41 H -0.3047 1.1191 0.5027 0.053 Uiso 1 1 calc R . . C42 C -0.1711(6) 1.0154(4) 0.5092(3) 0.0425(14) Uani 1 1 d . . . H42 H -0.1271 1.0294 0.5358 0.051 Uiso 1 1 calc R . . C43 C -0.1285(5) 0.9414(3) 0.4897(2) 0.0295(12) Uani 1 1 d . . . H43 H -0.0564 0.9044 0.5040 0.035 Uiso 1 1 calc R . . C44 C -0.0104(4) 0.7681(3) 0.4702(2) 0.0191(9) Uani 1 1 d . . . C45 C -0.0182(4) 0.7066(3) 0.5324(2) 0.0232(10) Uani 1 1 d . . . H45 H -0.0930 0.6927 0.5527 0.028 Uiso 1 1 calc R . . C46 C 0.0823(4) 0.6656(3) 0.5650(2) 0.0268(11) Uani 1 1 d . . . H46 H 0.0757 0.6241 0.6074 0.032 Uiso 1 1 calc R . . C47 C 0.1936(4) 0.6851(3) 0.5358(2) 0.0278(11) Uani 1 1 d . . . H47 H 0.2624 0.6560 0.5578 0.033 Uiso 1 1 calc R . . C48 C 0.2019(4) 0.7473(3) 0.4744(2) 0.0235(10) Uani 1 1 d . . . H48 H 0.2765 0.7619 0.4546 0.028 Uiso 1 1 calc R . . C49 C 0.1008(4) 0.7884(3) 0.4418(2) 0.0190(9) Uani 1 1 d . . . H49 H 0.1074 0.8309 0.3997 0.023 Uiso 1 1 calc R . . C50 C 0.1210(4) 1.0686(3) 0.2736(2) 0.0176(9) Uani 1 1 d . . . C51 C 0.0003(4) 1.0680(3) 0.2908(2) 0.0236(10) Uani 1 1 d . . . H51 H -0.0364 1.0334 0.2761 0.028 Uiso 1 1 calc R . . C52 C -0.0672(5) 1.1172(3) 0.3294(2) 0.0326(12) Uani 1 1 d . . . H52 H -0.1488 1.1148 0.3413 0.039 Uiso 1 1 calc R . . C53 C -0.0167(5) 1.1691(3) 0.3502(2) 0.0296(11) Uani 1 1 d . . . H53 H -0.0635 1.2039 0.3754 0.036 Uiso 1 1 calc R . . C54 C 0.1034(5) 1.1705(3) 0.3342(2) 0.0312(12) Uani 1 1 d . . . H54 H 0.1387 1.2058 0.3491 0.037 Uiso 1 1 calc R . . C55 C 0.1725(4) 1.1206(3) 0.2965(2) 0.0255(11) Uani 1 1 d . . . H55 H 0.2546 1.1217 0.2863 0.031 Uiso 1 1 calc R . . C56 C 0.3439(4) 0.9528(3) 0.2616(2) 0.0176(9) Uani 1 1 d . . . C57 C 0.3418(4) 0.9229(3) 0.3301(2) 0.0218(10) Uani 1 1 d . . . H57 H 0.2708 0.9349 0.3567 0.026 Uiso 1 1 calc R . . C58 C 0.4445(4) 0.8755(3) 0.3591(2) 0.0256(11) Uani 1 1 d . . . H58 H 0.4433 0.8553 0.4055 0.031 Uiso 1 1 calc R . . C59 C 0.5486(4) 0.8572(3) 0.3209(2) 0.0273(11) Uani 1 1 d . . . H59 H 0.6178 0.8239 0.3412 0.033 Uiso 1 1 calc R . . C60 C 0.5514(4) 0.8879(3) 0.2530(2) 0.0259(11) Uani 1 1 d . . . H60 H 0.6231 0.8764 0.2268 0.031 Uiso 1 1 calc R . . C61 C 0.4490(4) 0.9356(3) 0.2230(2) 0.0194(10) Uani 1 1 d . . . H61 H 0.4509 0.9562 0.1765 0.023 Uiso 1 1 calc R . . C62 C 0.2553(4) 1.0832(3) 0.1449(2) 0.0165(9) Uani 1 1 d . . . C63 C 0.2542(4) 1.1696(3) 0.1376(2) 0.0231(10) Uani 1 1 d . . . H63 H 0.2227 1.1917 0.1730 0.028 Uiso 1 1 calc R . . C64 C 0.2985(5) 1.2242(3) 0.0789(2) 0.0290(12) Uani 1 1 d . . . H64 H 0.2967 1.2835 0.0743 0.035 Uiso 1 1 calc R . . C65 C 0.3458(4) 1.1925(3) 0.0266(2) 0.0238(11) Uani 1 1 d . . . H65 H 0.3776 1.2296 -0.0133 0.029 Uiso 1 1 calc R . . C66 C 0.3461(4) 1.1063(3) 0.0333(2) 0.0239(10) Uani 1 1 d . . . H66 H 0.3781 1.0843 -0.0021 0.029 Uiso 1 1 calc R . . C67 C 0.3002(4) 1.0525(3) 0.0913(2) 0.0200(10) Uani 1 1 d . . . H67 H 0.2987 0.9941 0.0950 0.024 Uiso 1 1 calc R . . P4 P 0.65074(12) 0.43870(9) 0.28313(6) 0.0302(3) Uani 1 1 d . . . F1A F 0.5532(10) 0.5281(7) 0.2555(5) 0.076(4) Uani 0.65 1 d PU A 1 F2A F 0.7432(9) 0.3579(8) 0.3092(6) 0.065(3) Uani 0.65 1 d PU A 1 F3A F 0.5564(8) 0.4095(5) 0.3437(4) 0.058(2) Uani 0.65 1 d PU A 1 F4A F 0.7413(11) 0.4801(11) 0.2203(8) 0.043(3) Uani 0.65 1 d PU A 1 F5A F 0.5983(10) 0.3952(13) 0.2418(9) 0.057(4) Uani 0.65 1 d PU A 1 F6A F 0.6945(15) 0.4903(12) 0.3231(8) 0.054(4) Uani 0.65 1 d PU A 1 F1B F 0.5286(15) 0.4897(13) 0.2756(9) 0.078(6) Uani 0.35 1 d PU A 2 F2B F 0.7848(13) 0.3734(12) 0.2957(10) 0.032(3) Uani 0.35 1 d PU A 2 F3B F 0.6052(17) 0.3576(12) 0.3444(8) 0.086(6) Uani 0.35 1 d PU A 2 F4B F 0.706(2) 0.4998(19) 0.2270(14) 0.059(7) Uani 0.35 1 d PU A 2 F5B F 0.6371(16) 0.383(2) 0.2346(14) 0.033(4) Uani 0.35 1 d PU A 2 F6B F 0.680(2) 0.4763(19) 0.3362(12) 0.050(7) Uani 0.35 1 d PU A 2 C68 C 0.6776(5) 0.5821(3) 0.7788(3) 0.0338(12) Uani 1 1 d . . . H68A H 0.7031 0.5188 0.7859 0.041 Uiso 1 1 calc R . . H68B H 0.5925 0.5930 0.7944 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.69861(13) 0.64011(9) 0.69337(6) 0.0390(3) Uani 1 1 d . . . Cl2 Cl 0.76011(13) 0.61542(9) 0.82474(7) 0.0409(3) Uani 1 1 d . . . C69 C 0.5535(6) 0.1900(4) 0.2724(3) 0.0491(16) Uani 1 1 d . . . H69A H 0.5512 0.2426 0.2847 0.059 Uiso 1 1 calc R . . H69B H 0.6366 0.1591 0.2701 0.059 Uiso 1 1 calc R . . Cl3 Cl 0.46484(18) 0.12056(13) 0.33235(12) 0.0866(7) Uani 1 1 d . . . Cl4 Cl 0.49919(19) 0.22098(16) 0.19520(10) 0.0883(8) Uani 1 1 d . . . Cl5 Cl 0.8167(2) 0.22988(13) 0.15040(10) 0.0788(6) Uani 1 1 d . . . C70A C 0.8874(12) 0.2918(8) 0.1778(5) 0.055(3) Uani 0.651(9) 1 d P B 3 H70A H 0.8352 0.3091 0.2137 0.066 Uiso 0.651(9) 1 calc PR B 3 H70B H 0.9607 0.2545 0.1963 0.066 Uiso 0.651(9) 1 calc PR B 3 Cl6A Cl 0.9241(5) 0.3853(3) 0.11781(19) 0.090(2) Uani 0.651(9) 1 d P B 3 C70B C 0.837(2) 0.3289(18) 0.140(2) 0.103(12) Uani 0.349(9) 1 d P B 4 H70C H 0.7778 0.3540 0.1704 0.124 Uiso 0.349(9) 1 calc PR B 4 H70D H 0.8231 0.3661 0.0949 0.124 Uiso 0.349(9) 1 calc PR B 4 Cl6B Cl 0.9843(6) 0.3307(6) 0.1559(5) 0.078(3) Uani 0.349(9) 1 d P B 4 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 0.01258(17) 0.01547(16) 0.01029(15) -0.00316(12) -0.00005(12) -0.00487(13) Rh2 0.01232(17) 0.01288(16) 0.01175(16) -0.00194(12) -0.00103(12) -0.00335(13) Rh3 0.01419(17) 0.01309(16) 0.01044(15) -0.00170(12) -0.00212(12) -0.00507(13) P1 0.0173(6) 0.0164(5) 0.0111(5) -0.0029(4) -0.0003(4) -0.0064(5) P2 0.0180(6) 0.0167(5) 0.0138(5) -0.0040(4) 0.0012(4) -0.0066(5) P3 0.0164(6) 0.0159(5) 0.0119(5) -0.0028(4) -0.0010(4) -0.0071(4) S1 0.0148(5) 0.0159(5) 0.0114(5) -0.0023(4) -0.0019(4) -0.0057(4) S2 0.0164(5) 0.0147(5) 0.0135(5) -0.0024(4) -0.0041(4) -0.0045(4) N1 0.0146(19) 0.0136(17) 0.0099(16) -0.0016(13) -0.0019(13) -0.0040(14) N2 0.021(2) 0.0153(18) 0.0131(17) -0.0004(14) -0.0021(15) -0.0090(16) N3 0.0167(19) 0.0155(17) 0.0128(17) -0.0039(14) -0.0016(14) -0.0028(15) N4 0.021(2) 0.0132(17) 0.0109(16) -0.0041(14) -0.0016(14) -0.0056(15) N5 0.024(2) 0.0199(19) 0.0112(17) -0.0036(15) 0.0006(15) -0.0097(16) N6 0.0133(19) 0.0192(18) 0.0163(18) -0.0048(15) -0.0010(14) -0.0057(15) O1 0.0199(18) 0.0300(18) 0.0223(17) -0.0080(14) 0.0050(13) -0.0114(15) O2 0.0257(19) 0.0182(17) 0.036(2) -0.0039(15) -0.0061(15) 0.0027(15) O3 0.034(2) 0.0249(18) 0.034(2) 0.0041(16) -0.0142(16) -0.0090(16) C1 0.019(2) 0.018(2) 0.0078(19) -0.0047(16) -0.0019(16) -0.0054(18) C2 0.020(2) 0.013(2) 0.013(2) 0.0008(16) -0.0041(17) -0.0052(18) C3 0.028(3) 0.018(2) 0.031(3) 0.002(2) -0.002(2) -0.003(2) C4 0.015(2) 0.016(2) 0.023(2) -0.0011(18) -0.0031(18) -0.0019(18) C5 0.024(3) 0.031(3) 0.037(3) -0.013(2) -0.013(2) 0.001(2) C6 0.016(2) 0.018(2) 0.0088(18) -0.0042(16) -0.0031(16) -0.0082(17) C7 0.018(2) 0.017(2) 0.014(2) -0.0066(17) 0.0010(17) -0.0060(18) C8 0.027(3) 0.018(2) 0.036(3) -0.008(2) -0.001(2) -0.010(2) C9 0.018(2) 0.023(2) 0.027(2) -0.007(2) 0.0021(19) -0.0087(19) C10 0.022(3) 0.031(3) 0.051(3) -0.014(3) -0.018(2) -0.003(2) C11 0.024(3) 0.018(2) 0.013(2) -0.0056(17) -0.0051(18) -0.0031(19) C12 0.015(2) 0.020(2) 0.014(2) -0.0058(18) 0.0020(17) -0.0060(18) C13 0.020(2) 0.020(2) 0.022(2) -0.0062(19) -0.0030(19) -0.0093(19) C14 0.022(2) 0.027(2) 0.011(2) -0.0062(18) 0.0011(17) -0.014(2) C15 0.032(3) 0.028(3) 0.023(2) -0.010(2) -0.004(2) -0.011(2) C16 0.043(3) 0.044(3) 0.028(3) -0.012(2) -0.003(2) -0.024(3) C17 0.039(3) 0.058(4) 0.043(3) -0.020(3) -0.008(3) -0.029(3) C18 0.025(3) 0.055(4) 0.053(4) -0.014(3) -0.017(3) -0.006(3) C19 0.029(3) 0.032(3) 0.032(3) -0.005(2) -0.009(2) -0.008(2) C20 0.017(2) 0.015(2) 0.020(2) -0.0038(17) -0.0005(17) -0.0055(18) C21 0.022(2) 0.019(2) 0.020(2) -0.0069(18) 0.0008(18) -0.0061(19) C22 0.027(3) 0.015(2) 0.035(3) -0.005(2) -0.006(2) -0.002(2) C23 0.024(3) 0.022(2) 0.040(3) -0.014(2) 0.010(2) -0.006(2) C24 0.034(3) 0.022(2) 0.027(3) -0.015(2) 0.011(2) -0.016(2) C25 0.024(3) 0.016(2) 0.019(2) -0.0065(18) 0.0008(18) -0.0071(19) C26 0.020(2) 0.018(2) 0.012(2) -0.0027(17) -0.0032(17) -0.0062(18) C27 0.028(3) 0.022(2) 0.019(2) -0.0078(19) -0.0037(19) -0.006(2) C28 0.029(3) 0.023(2) 0.026(2) -0.007(2) -0.010(2) -0.002(2) C29 0.031(3) 0.020(2) 0.024(2) 0.0026(19) -0.016(2) -0.004(2) C30 0.026(3) 0.028(3) 0.016(2) 0.0026(19) -0.0039(19) -0.013(2) C31 0.022(3) 0.024(2) 0.018(2) -0.0048(19) 0.0021(18) -0.009(2) C32 0.016(2) 0.018(2) 0.015(2) 0.0006(17) -0.0022(17) -0.0035(18) C33 0.019(2) 0.021(2) 0.021(2) -0.0030(19) -0.0035(18) -0.0028(19) C34 0.023(3) 0.019(2) 0.029(3) -0.001(2) -0.009(2) -0.006(2) C35 0.022(3) 0.034(3) 0.028(3) 0.001(2) -0.007(2) -0.013(2) C36 0.024(3) 0.041(3) 0.021(2) -0.002(2) 0.005(2) -0.010(2) C37 0.027(3) 0.028(3) 0.017(2) -0.001(2) 0.0060(19) -0.012(2) C38 0.024(3) 0.023(2) 0.020(2) -0.0080(19) 0.0093(19) -0.009(2) C39 0.035(3) 0.025(2) 0.021(2) -0.012(2) 0.005(2) -0.003(2) C40 0.041(4) 0.035(3) 0.049(4) -0.017(3) 0.008(3) 0.004(3) C41 0.061(4) 0.036(3) 0.041(3) -0.024(3) 0.013(3) -0.014(3) C42 0.050(4) 0.042(3) 0.044(3) -0.028(3) 0.007(3) -0.011(3) C43 0.038(3) 0.033(3) 0.023(2) -0.017(2) 0.006(2) -0.012(2) C44 0.025(3) 0.018(2) 0.017(2) -0.0081(18) -0.0055(18) -0.0043(19) C45 0.027(3) 0.022(2) 0.021(2) -0.0030(19) -0.0013(19) -0.011(2) C46 0.032(3) 0.027(3) 0.020(2) -0.001(2) -0.005(2) -0.010(2) C47 0.026(3) 0.033(3) 0.027(3) -0.011(2) -0.011(2) -0.002(2) C48 0.021(3) 0.028(2) 0.024(2) -0.009(2) -0.0003(19) -0.010(2) C49 0.020(2) 0.025(2) 0.016(2) -0.0099(18) 0.0005(18) -0.0088(19) C50 0.025(3) 0.017(2) 0.014(2) -0.0072(17) -0.0044(18) -0.0056(19) C51 0.023(3) 0.027(2) 0.025(2) -0.014(2) 0.002(2) -0.008(2) C52 0.026(3) 0.040(3) 0.036(3) -0.021(2) 0.005(2) -0.009(2) C53 0.036(3) 0.033(3) 0.023(2) -0.016(2) 0.000(2) -0.003(2) C54 0.042(3) 0.030(3) 0.030(3) -0.016(2) -0.004(2) -0.013(2) C55 0.027(3) 0.030(3) 0.024(2) -0.011(2) -0.002(2) -0.011(2) C56 0.022(2) 0.015(2) 0.017(2) -0.0010(17) -0.0036(18) -0.0095(18) C57 0.022(2) 0.025(2) 0.017(2) -0.0006(19) 0.0010(18) -0.011(2) C58 0.028(3) 0.030(3) 0.016(2) 0.0045(19) -0.0063(19) -0.014(2) C59 0.020(3) 0.032(3) 0.026(2) 0.003(2) -0.012(2) -0.010(2) C60 0.017(2) 0.031(3) 0.027(2) -0.006(2) -0.0046(19) -0.001(2) C61 0.019(2) 0.025(2) 0.017(2) -0.0046(18) -0.0033(18) -0.0117(19) C62 0.014(2) 0.022(2) 0.015(2) -0.0043(17) -0.0035(17) -0.0059(18) C63 0.028(3) 0.023(2) 0.019(2) -0.0031(19) -0.0030(19) -0.010(2) C64 0.037(3) 0.021(2) 0.028(3) 0.001(2) -0.005(2) -0.015(2) C65 0.018(2) 0.030(3) 0.019(2) 0.004(2) -0.0045(18) -0.013(2) C66 0.022(3) 0.032(3) 0.016(2) -0.004(2) 0.0000(18) -0.009(2) C67 0.020(2) 0.025(2) 0.018(2) -0.0071(19) -0.0032(18) -0.0080(19) P4 0.0224(7) 0.0405(8) 0.0269(7) -0.0078(6) 0.0035(5) -0.0128(6) F1A 0.055(6) 0.081(7) 0.049(4) 0.002(4) 0.002(4) 0.031(5) F2A 0.081(9) 0.057(6) 0.043(5) -0.010(4) -0.023(6) 0.016(6) F3A 0.064(5) 0.073(5) 0.037(4) -0.011(4) 0.026(3) -0.047(4) F4A 0.018(5) 0.078(8) 0.031(3) -0.015(4) 0.015(4) -0.020(5) F5A 0.040(8) 0.086(9) 0.056(5) -0.030(5) 0.011(6) -0.035(7) F6A 0.052(5) 0.061(5) 0.055(7) -0.025(4) 0.024(4) -0.034(4) F1B 0.022(7) 0.131(18) 0.114(16) -0.100(14) -0.038(10) 0.035(9) F2B 0.014(6) 0.024(6) 0.053(10) -0.007(6) -0.012(5) 0.005(5) F3B 0.105(15) 0.126(14) 0.039(7) 0.003(10) 0.005(9) -0.099(12) F4B 0.045(16) 0.065(14) 0.049(14) 0.026(10) -0.015(10) -0.035(12) F5B 0.019(9) 0.054(7) 0.038(8) -0.029(6) 0.004(8) -0.012(8) F6B 0.041(12) 0.079(16) 0.043(11) -0.046(11) -0.027(10) 0.018(10) C68 0.033(3) 0.030(3) 0.039(3) -0.012(2) -0.002(2) -0.007(2) Cl1 0.0411(8) 0.0396(7) 0.0335(7) -0.0108(6) -0.0058(6) -0.0016(6) Cl2 0.0499(9) 0.0411(8) 0.0346(7) -0.0179(6) -0.0009(6) -0.0072(7) C69 0.062(4) 0.036(3) 0.050(4) -0.015(3) -0.025(3) 0.008(3) Cl3 0.0637(13) 0.0627(12) 0.1253(18) 0.0073(12) -0.0540(13) -0.0202(10) Cl4 0.0794(15) 0.1246(19) 0.0641(12) -0.0613(13) -0.0308(11) 0.0410(13) Cl5 0.1077(17) 0.0683(12) 0.0769(13) -0.0270(11) -0.0237(12) -0.0317(12) C70A 0.068(9) 0.058(7) 0.044(6) -0.012(5) -0.013(5) -0.021(6) Cl6A 0.135(5) 0.090(3) 0.052(2) -0.019(2) 0.029(3) -0.068(3) C70B 0.042(15) 0.073(19) 0.20(4) -0.05(2) -0.018(18) 0.007(13) Cl6B 0.052(4) 0.102(6) 0.091(6) -0.042(6) 0.007(3) -0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C11 1.834(5) . ? Rh1 N4 2.090(3) . ? Rh1 P1 2.2777(12) . ? Rh1 S1 2.4327(12) . ? Rh1 Rh3 3.1370(11) . ? Rh1 Rh2 5.0192(17) . ? Rh2 C12 1.838(4) . ? Rh2 N1 2.093(3) . ? Rh2 P2 2.2871(13) . ? Rh2 S2 2.4344(12) . ? Rh2 Rh3 3.1200(12) . ? Rh3 C13 1.846(5) . ? Rh3 P3 2.2882(12) . ? Rh3 S1 2.4044(15) . ? Rh3 S2 2.4225(12) . ? P1 C26 1.834(4) . ? P1 C20 1.835(5) . ? P1 C14 1.838(4) . ? P2 C44 1.832(5) . ? P2 C32 1.841(4) . ? P2 C38 1.843(5) . ? P3 C50 1.826(5) . ? P3 C62 1.838(4) . ? P3 C56 1.847(5) . ? S1 C1 1.746(4) . ? S2 C6 1.756(4) . ? N1 C1 1.324(5) . ? N1 N2 1.396(4) . ? N2 C2 1.316(5) . ? N3 C1 1.369(5) . ? N3 C2 1.383(5) . ? N3 C4 1.493(5) . ? N4 C6 1.326(5) . ? N4 N5 1.388(5) . ? N5 C7 1.328(5) . ? N6 C6 1.363(5) . ? N6 C7 1.372(5) . ? N6 C9 1.485(5) . ? O1 C11 1.156(5) . ? O2 C12 1.144(5) . ? O3 C13 1.144(5) . ? C2 C3 1.486(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.518(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.476(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.524(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C14 C15 1.391(6) . ? C14 C19 1.407(7) . ? C15 C16 1.386(7) . ? C15 H15 0.9500 . ? C16 C17 1.377(8) . ? C16 H16 0.9500 . ? C17 C18 1.390(8) . ? C17 H17 0.9500 . ? C18 C19 1.392(7) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C25 1.409(6) . ? C20 C21 1.410(6) . ? C21 C22 1.385(6) . ? C21 H21 0.9500 . ? C22 C23 1.395(7) . ? C22 H22 0.9500 . ? C23 C24 1.398(7) . ? C23 H23 0.9500 . ? C24 C25 1.381(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C31 1.399(6) . ? C26 C27 1.413(6) . ? C27 C28 1.390(6) . ? C27 H27 0.9500 . ? C28 C29 1.381(7) . ? C28 H28 0.9500 . ? C29 C30 1.390(7) . ? C29 H29 0.9500 . ? C30 C31 1.394(6) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.406(6) . ? C32 C37 1.413(6) . ? C33 C34 1.396(6) . ? C33 H33 0.9500 . ? C34 C35 1.392(7) . ? C34 H34 0.9500 . ? C35 C36 1.395(7) . ? C35 H35 0.9500 . ? C36 C37 1.405(6) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C38 C39 1.394(7) . ? C38 C43 1.403(7) . ? C39 C40 1.392(7) . ? C39 H39 0.9500 . ? C40 C41 1.389(9) . ? C40 H40 0.9500 . ? C41 C42 1.373(8) . ? C41 H41 0.9500 . ? C42 C43 1.393(7) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.393(6) . ? C44 C49 1.405(6) . ? C45 C46 1.390(7) . ? C45 H45 0.9500 . ? C46 C47 1.403(7) . ? C46 H46 0.9500 . ? C47 C48 1.388(6) . ? C47 H47 0.9500 . ? C48 C49 1.395(6) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C50 C51 1.397(6) . ? C50 C55 1.412(6) . ? C51 C52 1.395(7) . ? C51 H51 0.9500 . ? C52 C53 1.374(7) . ? C52 H52 0.9500 . ? C53 C54 1.389(7) . ? C53 H53 0.9500 . ? C54 C55 1.395(7) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C61 1.395(6) . ? C56 C57 1.402(6) . ? C57 C58 1.392(6) . ? C57 H57 0.9500 . ? C58 C59 1.386(7) . ? C58 H58 0.9500 . ? C59 C60 1.389(6) . ? C59 H59 0.9500 . ? C60 C61 1.400(6) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.385(6) . ? C62 C67 1.407(6) . ? C63 C64 1.388(6) . ? C63 H63 0.9500 . ? C64 C65 1.395(7) . ? C64 H64 0.9500 . ? C65 C66 1.387(7) . ? C65 H65 0.9500 . ? C66 C67 1.379(6) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? P4 F4B 1.46(3) . ? P4 F1B 1.486(17) . ? P4 F2A 1.521(12) . ? P4 F3A 1.584(8) . ? P4 F5A 1.594(19) . ? P4 F6B 1.61(3) . ? P4 F6A 1.618(18) . ? P4 F4A 1.633(14) . ? P4 F1A 1.647(11) . ? P4 F3B 1.656(14) . ? P4 F5B 1.67(3) . ? P4 F2B 1.692(18) . ? C68 Cl1 1.785(5) . ? C68 Cl2 1.784(5) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 Cl4 1.765(6) . ? C69 Cl3 1.781(7) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? Cl5 C70B 1.65(3) . ? Cl5 C70A 1.752(11) . ? C70A Cl6A 1.742(11) . ? C70A H70A 0.9900 . ? C70A H70B 0.9900 . ? C70B Cl6B 1.82(3) . ? C70B H70C 0.9900 . ? C70B H70D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh1 N4 175.69(17) . . ? C11 Rh1 P1 86.90(13) . . ? N4 Rh1 P1 90.97(10) . . ? C11 Rh1 S1 94.07(14) . . ? N4 Rh1 S1 88.47(10) . . ? P1 Rh1 S1 173.53(4) . . ? C11 Rh1 Rh3 97.13(14) . . ? N4 Rh1 Rh3 87.17(10) . . ? P1 Rh1 Rh3 124.36(4) . . ? S1 Rh1 Rh3 49.18(4) . . ? C11 Rh1 Rh2 129.41(14) . . ? N4 Rh1 Rh2 54.55(10) . . ? P1 Rh1 Rh2 130.77(4) . . ? S1 Rh1 Rh2 44.72(3) . . ? Rh3 Rh1 Rh2 36.55(2) . . ? C12 Rh2 N1 176.84(16) . . ? C12 Rh2 P2 92.71(13) . . ? N1 Rh2 P2 89.68(10) . . ? C12 Rh2 S2 89.65(13) . . ? N1 Rh2 S2 88.10(10) . . ? P2 Rh2 S2 175.64(4) . . ? C12 Rh2 Rh3 91.03(13) . . ? N1 Rh2 Rh3 85.82(9) . . ? P2 Rh2 Rh3 133.68(4) . . ? S2 Rh2 Rh3 49.86(3) . . ? C12 Rh2 Rh1 122.45(13) . . ? N1 Rh2 Rh1 54.50(9) . . ? P2 Rh2 Rh1 137.13(4) . . ? S2 Rh2 Rh1 43.05(3) . . ? Rh3 Rh2 Rh1 36.778(17) . . ? C13 Rh3 P3 86.68(14) . . ? C13 Rh3 S1 168.24(14) . . ? P3 Rh3 S1 90.57(4) . . ? C13 Rh3 S2 86.61(14) . . ? P3 Rh3 S2 166.34(4) . . ? S1 Rh3 S2 98.30(4) . . ? C13 Rh3 Rh2 107.89(14) . . ? P3 Rh3 Rh2 121.38(4) . . ? S1 Rh3 Rh2 83.27(4) . . ? S2 Rh3 Rh2 50.20(3) . . ? C13 Rh3 Rh1 121.12(15) . . ? P3 Rh3 Rh1 112.91(4) . . ? S1 Rh3 Rh1 49.96(3) . . ? S2 Rh3 Rh1 80.73(3) . . ? Rh2 Rh3 Rh1 106.68(3) . . ? C26 P1 C20 106.6(2) . . ? C26 P1 C14 103.9(2) . . ? C20 P1 C14 104.1(2) . . ? C26 P1 Rh1 109.76(14) . . ? C20 P1 Rh1 115.96(15) . . ? C14 P1 Rh1 115.48(14) . . ? C44 P2 C32 106.0(2) . . ? C44 P2 C38 102.5(2) . . ? C32 P2 C38 102.6(2) . . ? C44 P2 Rh2 111.71(15) . . ? C32 P2 Rh2 112.15(15) . . ? C38 P2 Rh2 120.49(15) . . ? C50 P3 C62 106.4(2) . . ? C50 P3 C56 103.8(2) . . ? C62 P3 C56 103.07(19) . . ? C50 P3 Rh3 112.51(15) . . ? C62 P3 Rh3 113.86(14) . . ? C56 P3 Rh3 116.08(14) . . ? C1 S1 Rh3 109.70(15) . . ? C1 S1 Rh1 102.30(14) . . ? Rh3 S1 Rh1 80.86(4) . . ? C6 S2 Rh3 111.84(14) . . ? C6 S2 Rh2 102.23(13) . . ? Rh3 S2 Rh2 79.94(4) . . ? C1 N1 N2 108.9(3) . . ? C1 N1 Rh2 128.0(3) . . ? N2 N1 Rh2 123.1(3) . . ? C2 N2 N1 106.2(3) . . ? C1 N3 C2 105.5(3) . . ? C1 N3 C4 126.9(3) . . ? C2 N3 C4 127.6(3) . . ? C6 N4 N5 108.5(3) . . ? C6 N4 Rh1 127.1(3) . . ? N5 N4 Rh1 124.4(3) . . ? C7 N5 N4 106.3(4) . . ? C6 N6 C7 105.9(3) . . ? C6 N6 C9 126.4(4) . . ? C7 N6 C9 127.7(4) . . ? N1 C1 N3 108.9(3) . . ? N1 C1 S1 128.4(3) . . ? N3 C1 S1 122.7(3) . . ? N2 C2 N3 110.5(3) . . ? N2 C2 C3 125.4(4) . . ? N3 C2 C3 124.1(4) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 C5 112.3(4) . . ? N3 C4 H4A 109.2 . . ? C5 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C5 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 N6 109.2(4) . . ? N4 C6 S2 126.5(3) . . ? N6 C6 S2 124.3(3) . . ? N5 C7 N6 110.1(4) . . ? N5 C7 C8 124.9(4) . . ? N6 C7 C8 124.9(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 C10 111.8(4) . . ? N6 C9 H9A 109.3 . . ? C10 C9 H9A 109.3 . . ? N6 C9 H9B 109.3 . . ? C10 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 Rh1 176.1(4) . . ? O2 C12 Rh2 175.9(4) . . ? O3 C13 Rh3 175.6(4) . . ? C15 C14 C19 118.8(4) . . ? C15 C14 P1 120.3(4) . . ? C19 C14 P1 120.7(4) . . ? C16 C15 C14 120.8(5) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.1(5) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 120.1(5) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 120.0(5) . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C25 C20 C21 118.6(4) . . ? C25 C20 P1 122.3(3) . . ? C21 C20 P1 119.1(3) . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.2(5) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C20 120.5(4) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? C31 C26 C27 119.2(4) . . ? C31 C26 P1 124.4(3) . . ? C27 C26 P1 116.4(3) . . ? C28 C27 C26 120.2(4) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 120.0(5) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C31 120.3(4) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 119.8(5) . . ? C30 C31 H31 120.1 . . ? C26 C31 H31 120.1 . . ? C33 C32 C37 119.7(4) . . ? C33 C32 P2 118.5(3) . . ? C37 C32 P2 121.8(4) . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 119.9(5) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 120.4(4) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C35 C36 C37 120.5(5) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C32 119.2(5) . . ? C36 C37 H37 120.4 . . ? C32 C37 H37 120.4 . . ? C39 C38 C43 119.0(5) . . ? C39 C38 P2 119.5(4) . . ? C43 C38 P2 121.4(4) . . ? C40 C39 C38 119.8(5) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.6(6) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 119.9(5) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.2(6) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C42 C43 C38 120.3(5) . . ? C42 C43 H43 119.8 . . ? C38 C43 H43 119.8 . . ? C45 C44 C49 118.6(4) . . ? C45 C44 P2 123.2(4) . . ? C49 C44 P2 118.3(3) . . ? C46 C45 C44 120.6(4) . . ? C46 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? C45 C46 C47 120.6(4) . . ? C45 C46 H46 119.7 . . ? C47 C46 H46 119.7 . . ? C48 C47 C46 119.2(4) . . ? C48 C47 H47 120.4 . . ? C46 C47 H47 120.4 . . ? C47 C48 C49 120.1(4) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C48 C49 C44 120.9(4) . . ? C48 C49 H49 119.5 . . ? C44 C49 H49 119.5 . . ? C51 C50 C55 117.8(4) . . ? C51 C50 P3 119.8(3) . . ? C55 C50 P3 122.4(4) . . ? C52 C51 C50 121.2(4) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.4 . . ? C53 C52 C51 120.5(5) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 119.5(5) . . ? C52 C53 H53 120.2 . . ? C54 C53 H53 120.2 . . ? C53 C54 C55 120.6(5) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C54 C55 C50 120.3(5) . . ? C54 C55 H55 119.8 . . ? C50 C55 H55 119.8 . . ? C61 C56 C57 119.8(4) . . ? C61 C56 P3 119.3(3) . . ? C57 C56 P3 120.6(3) . . ? C58 C57 C56 119.5(4) . . ? C58 C57 H57 120.2 . . ? C56 C57 H57 120.2 . . ? C59 C58 C57 120.8(4) . . ? C59 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C58 C59 C60 119.8(4) . . ? C58 C59 H59 120.1 . . ? C60 C59 H59 120.1 . . ? C59 C60 C61 120.2(5) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C56 C61 C60 119.8(4) . . ? C56 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C63 C62 C67 118.6(4) . . ? C63 C62 P3 123.8(3) . . ? C67 C62 P3 117.6(3) . . ? C62 C63 C64 120.6(4) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C65 120.3(4) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C66 C65 C64 119.5(4) . . ? C66 C65 H65 120.3 . . ? C64 C65 H65 120.3 . . ? C67 C66 C65 120.2(4) . . ? C67 C66 H66 119.9 . . ? C65 C66 H66 119.9 . . ? C66 C67 C62 120.8(4) . . ? C66 C67 H67 119.6 . . ? C62 C67 H67 119.6 . . ? F4B P4 F1B 95.4(13) . . ? F4B P4 F2A 108.7(10) . . ? F1B P4 F2A 155.0(9) . . ? F4B P4 F3A 156.3(10) . . ? F1B P4 F3A 64.6(8) . . ? F2A P4 F3A 93.1(5) . . ? F4B P4 F5A 96.3(16) . . ? F1B P4 F5A 76.8(8) . . ? F2A P4 F5A 93.4(8) . . ? F3A P4 F5A 91.4(6) . . ? F4B P4 F6B 94.7(17) . . ? F1B P4 F6B 96.7(11) . . ? F2A P4 F6B 88.2(11) . . ? F3A P4 F6B 76.3(10) . . ? F5A P4 F6B 167.7(11) . . ? F4B P4 F6A 82.4(15) . . ? F1B P4 F6A 98.3(9) . . ? F2A P4 F6A 91.7(8) . . ? F3A P4 F6A 87.9(6) . . ? F5A P4 F6A 174.9(9) . . ? F6B P4 F6A 12.3(14) . . ? F4B P4 F4A 17.4(13) . . ? F1B P4 F4A 110.6(9) . . ? F2A P4 F4A 92.4(6) . . ? F3A P4 F4A 173.5(6) . . ? F5A P4 F4A 91.7(9) . . ? F6B P4 F4A 100.5(12) . . ? F6A P4 F4A 88.5(9) . . ? F4B P4 F1A 70.5(10) . . ? F1B P4 F1A 26.3(9) . . ? F2A P4 F1A 178.1(7) . . ? F3A P4 F1A 87.4(4) . . ? F5A P4 F1A 88.3(8) . . ? F6B P4 F1A 90.2(11) . . ? F6A P4 F1A 86.5(8) . . ? F4A P4 F1A 86.9(6) . . ? F4B P4 F3B 171.0(12) . . ? F1B P4 F3B 92.5(10) . . ? F2A P4 F3B 63.0(8) . . ? F3A P4 F3B 32.7(7) . . ? F5A P4 F3B 81.3(9) . . ? F6B P4 F3B 88.6(12) . . ? F6A P4 F3B 100.7(8) . . ? F4A P4 F3B 153.7(9) . . ? F1A P4 F3B 117.9(8) . . ? F4B P4 F5B 89.5(17) . . ? F1B P4 F5B 92.4(10) . . ? F2A P4 F5B 81.4(11) . . ? F3A P4 F5B 103.2(9) . . ? F5A P4 F5B 16.5(8) . . ? F6B P4 F5B 169.6(14) . . ? F6A P4 F5B 167.1(9) . . ? F4A P4 F5B 80.9(11) . . ? F1A P4 F5B 100.2(10) . . ? F3B P4 F5B 85.9(12) . . ? F4B P4 F2B 89.2(11) . . ? F1B P4 F2B 175.2(10) . . ? F2A P4 F2B 20.2(6) . . ? F3A P4 F2B 111.3(7) . . ? F5A P4 F2B 101.3(9) . . ? F6B P4 F2B 84.3(12) . . ? F6A P4 F2B 83.7(10) . . ? F4A P4 F2B 73.7(8) . . ? F1A P4 F2B 158.5(6) . . ? F3B P4 F2B 82.8(8) . . ? F5B P4 F2B 86.2(11) . . ? Cl1 C68 Cl2 110.9(3) . . ? Cl1 C68 H68A 109.5 . . ? Cl2 C68 H68A 109.5 . . ? Cl1 C68 H68B 109.5 . . ? Cl2 C68 H68B 109.5 . . ? H68A C68 H68B 108.1 . . ? Cl4 C69 Cl3 109.4(4) . . ? Cl4 C69 H69A 109.8 . . ? Cl3 C69 H69A 109.8 . . ? Cl4 C69 H69B 109.8 . . ? Cl3 C69 H69B 109.8 . . ? H69A C69 H69B 108.2 . . ? C70B Cl5 C70A 34.8(11) . . ? Cl6A C70A Cl5 114.9(6) . . ? Cl6A C70A H70A 108.5 . . ? Cl5 C70A H70A 108.5 . . ? Cl6A C70A H70B 108.5 . . ? Cl5 C70A H70B 108.5 . . ? H70A C70A H70B 107.5 . . ? Cl5 C70B Cl6B 112.9(15) . . ? Cl5 C70B H70C 109.0 . . ? Cl6B C70B H70C 109.0 . . ? Cl5 C70B H70D 109.0 . . ? Cl6B C70B H70D 109.0 . . ? H70C C70B H70D 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Rh1 Rh2 C12 68.4(2) . . . . ? N4 Rh1 Rh2 C12 -113.76(19) . . . . ? P1 Rh1 Rh2 C12 -59.66(16) . . . . ? S1 Rh1 Rh2 C12 113.99(16) . . . . ? Rh3 Rh1 Rh2 C12 35.40(16) . . . . ? C11 Rh1 Rh2 N1 -110.6(2) . . . . ? N4 Rh1 Rh2 N1 67.25(16) . . . . ? P1 Rh1 Rh2 N1 121.35(12) . . . . ? S1 Rh1 Rh2 N1 -65.00(12) . . . . ? Rh3 Rh1 Rh2 N1 -143.59(12) . . . . ? C11 Rh1 Rh2 P2 -71.76(17) . . . . ? N4 Rh1 Rh2 P2 106.11(12) . . . . ? P1 Rh1 Rh2 P2 160.21(6) . . . . ? S1 Rh1 Rh2 P2 -26.14(6) . . . . ? Rh3 Rh1 Rh2 P2 -104.74(5) . . . . ? C11 Rh1 Rh2 S2 114.63(17) . . . . ? N4 Rh1 Rh2 S2 -67.50(12) . . . . ? P1 Rh1 Rh2 S2 -13.40(5) . . . . ? S1 Rh1 Rh2 S2 160.25(5) . . . . ? Rh3 Rh1 Rh2 S2 81.66(5) . . . . ? C11 Rh1 Rh2 Rh3 32.97(17) . . . . ? N4 Rh1 Rh2 Rh3 -149.16(11) . . . . ? P1 Rh1 Rh2 Rh3 -95.06(5) . . . . ? S1 Rh1 Rh2 Rh3 78.59(5) . . . . ? C12 Rh2 Rh3 C13 -19.2(2) . . . . ? N1 Rh2 Rh3 C13 160.56(17) . . . . ? P2 Rh2 Rh3 C13 -113.89(15) . . . . ? S2 Rh2 Rh3 C13 69.52(15) . . . . ? Rh1 Rh2 Rh3 C13 131.58(15) . . . . ? C12 Rh2 Rh3 P3 78.07(14) . . . . ? N1 Rh2 Rh3 P3 -102.22(10) . . . . ? P2 Rh2 Rh3 P3 -16.67(6) . . . . ? S2 Rh2 Rh3 P3 166.74(5) . . . . ? Rh1 Rh2 Rh3 P3 -131.20(4) . . . . ? C12 Rh2 Rh3 S1 164.62(14) . . . . ? N1 Rh2 Rh3 S1 -15.66(10) . . . . ? P2 Rh2 Rh3 S1 69.89(6) . . . . ? S2 Rh2 Rh3 S1 -106.70(5) . . . . ? Rh1 Rh2 Rh3 S1 -44.64(3) . . . . ? C12 Rh2 Rh3 S2 -88.67(14) . . . . ? N1 Rh2 Rh3 S2 91.04(10) . . . . ? P2 Rh2 Rh3 S2 176.59(6) . . . . ? Rh1 Rh2 Rh3 S2 62.06(4) . . . . ? C12 Rh2 Rh3 Rh1 -150.74(13) . . . . ? N1 Rh2 Rh3 Rh1 28.98(9) . . . . ? P2 Rh2 Rh3 Rh1 114.53(5) . . . . ? S2 Rh2 Rh3 Rh1 -62.06(4) . . . . ? C11 Rh1 Rh3 C13 81.3(2) . . . . ? N4 Rh1 Rh3 C13 -99.03(18) . . . . ? P1 Rh1 Rh3 C13 -9.79(16) . . . . ? S1 Rh1 Rh3 C13 170.55(16) . . . . ? Rh2 Rh1 Rh3 C13 -123.75(16) . . . . ? C11 Rh1 Rh3 P3 -19.15(13) . . . . ? N4 Rh1 Rh3 P3 160.50(9) . . . . ? P1 Rh1 Rh3 P3 -110.26(5) . . . . ? S1 Rh1 Rh3 P3 70.07(5) . . . . ? Rh2 Rh1 Rh3 P3 135.78(4) . . . . ? C11 Rh1 Rh3 S1 -89.22(13) . . . . ? N4 Rh1 Rh3 S1 90.43(10) . . . . ? P1 Rh1 Rh3 S1 179.66(5) . . . . ? Rh2 Rh1 Rh3 S1 65.71(4) . . . . ? C11 Rh1 Rh3 S2 161.62(13) . . . . ? N4 Rh1 Rh3 S2 -18.73(9) . . . . ? P1 Rh1 Rh3 S2 70.51(5) . . . . ? S1 Rh1 Rh3 S2 -109.16(5) . . . . ? Rh2 Rh1 Rh3 S2 -43.45(3) . . . . ? C11 Rh1 Rh3 Rh2 -154.93(13) . . . . ? N4 Rh1 Rh3 Rh2 24.72(9) . . . . ? P1 Rh1 Rh3 Rh2 113.96(4) . . . . ? S1 Rh1 Rh3 Rh2 -65.71(4) . . . . ? C11 Rh1 P1 C26 -56.8(2) . . . . ? N4 Rh1 P1 C26 126.94(18) . . . . ? S1 Rh1 P1 C26 42.0(4) . . . . ? Rh3 Rh1 P1 C26 39.71(16) . . . . ? Rh2 Rh1 P1 C26 85.64(16) . . . . ? C11 Rh1 P1 C20 64.0(2) . . . . ? N4 Rh1 P1 C20 -112.28(18) . . . . ? S1 Rh1 P1 C20 162.8(3) . . . . ? Rh3 Rh1 P1 C20 160.49(14) . . . . ? Rh2 Rh1 P1 C20 -153.58(14) . . . . ? C11 Rh1 P1 C14 -173.8(2) . . . . ? N4 Rh1 P1 C14 9.92(19) . . . . ? S1 Rh1 P1 C14 -75.0(4) . . . . ? Rh3 Rh1 P1 C14 -77.31(17) . . . . ? Rh2 Rh1 P1 C14 -31.38(18) . . . . ? C12 Rh2 P2 C44 -148.3(2) . . . . ? N1 Rh2 P2 C44 29.58(18) . . . . ? S2 Rh2 P2 C44 89.0(6) . . . . ? Rh3 Rh2 P2 C44 -54.33(16) . . . . ? Rh1 Rh2 P2 C44 -1.13(16) . . . . ? C12 Rh2 P2 C32 92.8(2) . . . . ? N1 Rh2 P2 C32 -89.23(18) . . . . ? S2 Rh2 P2 C32 -29.9(6) . . . . ? Rh3 Rh2 P2 C32 -173.14(15) . . . . ? Rh1 Rh2 P2 C32 -119.95(15) . . . . ? C12 Rh2 P2 C38 -28.1(2) . . . . ? N1 Rh2 P2 C38 149.8(2) . . . . ? S2 Rh2 P2 C38 -150.8(5) . . . . ? Rh3 Rh2 P2 C38 65.94(19) . . . . ? Rh1 Rh2 P2 C38 119.13(18) . . . . ? C13 Rh3 P3 C50 79.7(2) . . . . ? S1 Rh3 P3 C50 -111.72(15) . . . . ? S2 Rh3 P3 C50 19.0(2) . . . . ? Rh2 Rh3 P3 C50 -29.26(15) . . . . ? Rh1 Rh3 P3 C50 -157.76(15) . . . . ? C13 Rh3 P3 C62 -41.4(2) . . . . ? S1 Rh3 P3 C62 127.14(16) . . . . ? S2 Rh3 P3 C62 -102.1(2) . . . . ? Rh2 Rh3 P3 C62 -150.40(15) . . . . ? Rh1 Rh3 P3 C62 81.10(16) . . . . ? C13 Rh3 P3 C56 -160.9(2) . . . . ? S1 Rh3 P3 C56 7.69(16) . . . . ? S2 Rh3 P3 C56 138.4(2) . . . . ? Rh2 Rh3 P3 C56 90.15(16) . . . . ? Rh1 Rh3 P3 C56 -38.35(16) . . . . ? C13 Rh3 S1 C1 -143.5(7) . . . . ? P3 Rh3 S1 C1 140.12(15) . . . . ? S2 Rh3 S1 C1 -29.47(15) . . . . ? Rh2 Rh3 S1 C1 18.57(15) . . . . ? Rh1 Rh3 S1 C1 -99.88(15) . . . . ? C13 Rh3 S1 Rh1 -43.6(7) . . . . ? P3 Rh3 S1 Rh1 -120.00(4) . . . . ? S2 Rh3 S1 Rh1 70.42(4) . . . . ? Rh2 Rh3 S1 Rh1 118.46(3) . . . . ? C11 Rh1 S1 C1 -155.8(2) . . . . ? N4 Rh1 S1 C1 20.74(18) . . . . ? P1 Rh1 S1 C1 105.9(4) . . . . ? Rh3 Rh1 S1 C1 108.32(15) . . . . ? Rh2 Rh1 S1 C1 57.85(15) . . . . ? C11 Rh1 S1 Rh3 95.91(14) . . . . ? N4 Rh1 S1 Rh3 -87.58(10) . . . . ? P1 Rh1 S1 Rh3 -2.5(4) . . . . ? Rh2 Rh1 S1 Rh3 -50.47(3) . . . . ? C13 Rh3 S2 C6 144.0(2) . . . . ? P3 Rh3 S2 C6 -155.27(19) . . . . ? S1 Rh3 S2 C6 -25.24(14) . . . . ? Rh2 Rh3 S2 C6 -99.24(15) . . . . ? Rh1 Rh3 S2 C6 21.72(14) . . . . ? C13 Rh3 S2 Rh2 -116.74(15) . . . . ? P3 Rh3 S2 Rh2 -56.02(17) . . . . ? S1 Rh3 S2 Rh2 74.00(5) . . . . ? Rh1 Rh3 S2 Rh2 120.96(4) . . . . ? C12 Rh2 S2 C6 -157.98(19) . . . . ? N1 Rh2 S2 C6 24.24(17) . . . . ? P2 Rh2 S2 C6 -35.2(6) . . . . ? Rh3 Rh2 S2 C6 110.37(15) . . . . ? Rh1 Rh2 S2 C6 59.58(14) . . . . ? C12 Rh2 S2 Rh3 91.64(13) . . . . ? N1 Rh2 S2 Rh3 -86.13(10) . . . . ? P2 Rh2 S2 Rh3 -145.6(5) . . . . ? Rh1 Rh2 S2 Rh3 -50.79(3) . . . . ? C12 Rh2 N1 C1 19(3) . . . . ? P2 Rh2 N1 C1 -120.0(3) . . . . ? S2 Rh2 N1 C1 63.7(3) . . . . ? Rh3 Rh2 N1 C1 13.8(3) . . . . ? Rh1 Rh2 N1 C1 34.7(3) . . . . ? C12 Rh2 N1 N2 -163(3) . . . . ? P2 Rh2 N1 N2 58.4(3) . . . . ? S2 Rh2 N1 N2 -117.8(3) . . . . ? Rh3 Rh2 N1 N2 -167.7(3) . . . . ? Rh1 Rh2 N1 N2 -146.8(3) . . . . ? C1 N1 N2 C2 -0.2(4) . . . . ? Rh2 N1 N2 C2 -178.9(3) . . . . ? C11 Rh1 N4 C6 -167(2) . . . . ? P1 Rh1 N4 C6 -106.4(3) . . . . ? S1 Rh1 N4 C6 67.1(3) . . . . ? Rh3 Rh1 N4 C6 17.9(3) . . . . ? Rh2 Rh1 N4 C6 35.7(3) . . . . ? C11 Rh1 N4 N5 14(2) . . . . ? P1 Rh1 N4 N5 74.6(3) . . . . ? S1 Rh1 N4 N5 -111.9(3) . . . . ? Rh3 Rh1 N4 N5 -161.1(3) . . . . ? Rh2 Rh1 N4 N5 -143.3(3) . . . . ? C6 N4 N5 C7 1.2(4) . . . . ? Rh1 N4 N5 C7 -179.7(3) . . . . ? N2 N1 C1 N3 0.6(4) . . . . ? Rh2 N1 C1 N3 179.3(3) . . . . ? N2 N1 C1 S1 -179.1(3) . . . . ? Rh2 N1 C1 S1 -0.4(6) . . . . ? C2 N3 C1 N1 -0.8(4) . . . . ? C4 N3 C1 N1 177.3(4) . . . . ? C2 N3 C1 S1 178.9(3) . . . . ? C4 N3 C1 S1 -3.0(6) . . . . ? Rh3 S1 C1 N1 -18.5(4) . . . . ? Rh1 S1 C1 N1 -103.1(4) . . . . ? Rh3 S1 C1 N3 161.8(3) . . . . ? Rh1 S1 C1 N3 77.3(3) . . . . ? N1 N2 C2 N3 -0.3(5) . . . . ? N1 N2 C2 C3 -178.9(4) . . . . ? C1 N3 C2 N2 0.7(5) . . . . ? C4 N3 C2 N2 -177.3(4) . . . . ? C1 N3 C2 C3 179.3(4) . . . . ? C4 N3 C2 C3 1.3(7) . . . . ? C1 N3 C4 C5 82.7(5) . . . . ? C2 N3 C4 C5 -99.6(5) . . . . ? N5 N4 C6 N6 -1.8(4) . . . . ? Rh1 N4 C6 N6 179.1(2) . . . . ? N5 N4 C6 S2 175.9(3) . . . . ? Rh1 N4 C6 S2 -3.2(5) . . . . ? C7 N6 C6 N4 1.6(4) . . . . ? C9 N6 C6 N4 -179.7(4) . . . . ? C7 N6 C6 S2 -176.1(3) . . . . ? C9 N6 C6 S2 2.6(6) . . . . ? Rh3 S2 C6 N4 -20.2(4) . . . . ? Rh2 S2 C6 N4 -104.1(3) . . . . ? Rh3 S2 C6 N6 157.1(3) . . . . ? Rh2 S2 C6 N6 73.2(3) . . . . ? N4 N5 C7 N6 -0.1(4) . . . . ? N4 N5 C7 C8 179.3(4) . . . . ? C6 N6 C7 N5 -0.9(5) . . . . ? C9 N6 C7 N5 -179.6(4) . . . . ? C6 N6 C7 C8 179.6(4) . . . . ? C9 N6 C7 C8 1.0(7) . . . . ? C6 N6 C9 C10 86.3(5) . . . . ? C7 N6 C9 C10 -95.3(5) . . . . ? N4 Rh1 C11 O1 36(7) . . . . ? P1 Rh1 C11 O1 -24(6) . . . . ? S1 Rh1 C11 O1 162(6) . . . . ? Rh3 Rh1 C11 O1 -148(6) . . . . ? Rh2 Rh1 C11 O1 -167(6) . . . . ? N1 Rh2 C12 O2 -5(8) . . . . ? P2 Rh2 C12 O2 134(6) . . . . ? S2 Rh2 C12 O2 -49(6) . . . . ? Rh3 Rh2 C12 O2 1(6) . . . . ? Rh1 Rh2 C12 O2 -20(6) . . . . ? P3 Rh3 C13 O3 104(5) . . . . ? S1 Rh3 C13 O3 28(6) . . . . ? S2 Rh3 C13 O3 -87(5) . . . . ? Rh2 Rh3 C13 O3 -134(5) . . . . ? Rh1 Rh3 C13 O3 -10(5) . . . . ? C26 P1 C14 C15 150.5(4) . . . . ? C20 P1 C14 C15 39.0(4) . . . . ? Rh1 P1 C14 C15 -89.3(4) . . . . ? C26 P1 C14 C19 -34.5(4) . . . . ? C20 P1 C14 C19 -146.0(4) . . . . ? Rh1 P1 C14 C19 85.7(4) . . . . ? C19 C14 C15 C16 0.2(7) . . . . ? P1 C14 C15 C16 175.2(4) . . . . ? C14 C15 C16 C17 0.4(8) . . . . ? C15 C16 C17 C18 -0.7(8) . . . . ? C16 C17 C18 C19 0.5(9) . . . . ? C17 C18 C19 C14 0.0(8) . . . . ? C15 C14 C19 C18 -0.4(7) . . . . ? P1 C14 C19 C18 -175.4(4) . . . . ? C26 P1 C20 C25 -59.2(4) . . . . ? C14 P1 C20 C25 50.3(4) . . . . ? Rh1 P1 C20 C25 178.3(3) . . . . ? C26 P1 C20 C21 120.7(3) . . . . ? C14 P1 C20 C21 -129.8(3) . . . . ? Rh1 P1 C20 C21 -1.8(4) . . . . ? C25 C20 C21 C22 2.8(6) . . . . ? P1 C20 C21 C22 -177.1(3) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? C21 C22 C23 C24 -2.8(7) . . . . ? C22 C23 C24 C25 2.0(7) . . . . ? C23 C24 C25 C20 1.2(6) . . . . ? C21 C20 C25 C24 -3.6(6) . . . . ? P1 C20 C25 C24 176.3(3) . . . . ? C20 P1 C26 C31 15.9(4) . . . . ? C14 P1 C26 C31 -93.8(4) . . . . ? Rh1 P1 C26 C31 142.2(4) . . . . ? C20 P1 C26 C27 -166.0(3) . . . . ? C14 P1 C26 C27 84.4(4) . . . . ? Rh1 P1 C26 C27 -39.7(4) . . . . ? C31 C26 C27 C28 1.6(7) . . . . ? P1 C26 C27 C28 -176.7(4) . . . . ? C26 C27 C28 C29 -1.9(7) . . . . ? C27 C28 C29 C30 1.3(7) . . . . ? C28 C29 C30 C31 -0.4(7) . . . . ? C29 C30 C31 C26 0.1(7) . . . . ? C27 C26 C31 C30 -0.7(7) . . . . ? P1 C26 C31 C30 177.4(3) . . . . ? C44 P2 C32 C33 -95.0(4) . . . . ? C38 P2 C32 C33 157.9(3) . . . . ? Rh2 P2 C32 C33 27.1(4) . . . . ? C44 P2 C32 C37 86.1(4) . . . . ? C38 P2 C32 C37 -21.0(4) . . . . ? Rh2 P2 C32 C37 -151.8(3) . . . . ? C37 C32 C33 C34 0.5(6) . . . . ? P2 C32 C33 C34 -178.4(3) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C33 C34 C35 C36 0.1(7) . . . . ? C34 C35 C36 C37 -0.3(7) . . . . ? C35 C36 C37 C32 0.6(7) . . . . ? C33 C32 C37 C36 -0.8(7) . . . . ? P2 C32 C37 C36 178.1(4) . . . . ? C44 P2 C38 C39 -170.7(4) . . . . ? C32 P2 C38 C39 -60.9(4) . . . . ? Rh2 P2 C38 C39 64.6(4) . . . . ? C44 P2 C38 C43 5.8(4) . . . . ? C32 P2 C38 C43 115.5(4) . . . . ? Rh2 P2 C38 C43 -119.0(3) . . . . ? C43 C38 C39 C40 1.7(7) . . . . ? P2 C38 C39 C40 178.2(4) . . . . ? C38 C39 C40 C41 0.6(8) . . . . ? C39 C40 C41 C42 -1.9(9) . . . . ? C40 C41 C42 C43 0.9(8) . . . . ? C41 C42 C43 C38 1.4(8) . . . . ? C39 C38 C43 C42 -2.7(7) . . . . ? P2 C38 C43 C42 -179.2(4) . . . . ? C32 P2 C44 C45 -16.6(4) . . . . ? C38 P2 C44 C45 90.7(4) . . . . ? Rh2 P2 C44 C45 -139.0(3) . . . . ? C32 P2 C44 C49 163.0(3) . . . . ? C38 P2 C44 C49 -89.8(4) . . . . ? Rh2 P2 C44 C49 40.6(4) . . . . ? C49 C44 C45 C46 -0.9(7) . . . . ? P2 C44 C45 C46 178.6(4) . . . . ? C44 C45 C46 C47 -0.2(7) . . . . ? C45 C46 C47 C48 1.4(7) . . . . ? C46 C47 C48 C49 -1.4(7) . . . . ? C47 C48 C49 C44 0.2(7) . . . . ? C45 C44 C49 C48 1.0(7) . . . . ? P2 C44 C49 C48 -178.6(3) . . . . ? C62 P3 C50 C51 115.3(4) . . . . ? C56 P3 C50 C51 -136.3(4) . . . . ? Rh3 P3 C50 C51 -10.0(4) . . . . ? C62 P3 C50 C55 -63.8(4) . . . . ? C56 P3 C50 C55 44.6(4) . . . . ? Rh3 P3 C50 C55 170.9(3) . . . . ? C55 C50 C51 C52 0.1(7) . . . . ? P3 C50 C51 C52 -179.0(4) . . . . ? C50 C51 C52 C53 1.3(8) . . . . ? C51 C52 C53 C54 -1.8(8) . . . . ? C52 C53 C54 C55 0.9(8) . . . . ? C53 C54 C55 C50 0.6(7) . . . . ? C51 C50 C55 C54 -1.1(7) . . . . ? P3 C50 C55 C54 178.0(4) . . . . ? C50 P3 C56 C61 -148.7(3) . . . . ? C62 P3 C56 C61 -37.9(4) . . . . ? Rh3 P3 C56 C61 87.3(3) . . . . ? C50 P3 C56 C57 37.7(4) . . . . ? C62 P3 C56 C57 148.5(4) . . . . ? Rh3 P3 C56 C57 -86.3(4) . . . . ? C61 C56 C57 C58 -0.7(7) . . . . ? P3 C56 C57 C58 172.9(3) . . . . ? C56 C57 C58 C59 -0.2(7) . . . . ? C57 C58 C59 C60 1.1(7) . . . . ? C58 C59 C60 C61 -1.2(7) . . . . ? C57 C56 C61 C60 0.6(7) . . . . ? P3 C56 C61 C60 -173.0(3) . . . . ? C59 C60 C61 C56 0.4(7) . . . . ? C50 P3 C62 C63 15.7(4) . . . . ? C56 P3 C62 C63 -93.2(4) . . . . ? Rh3 P3 C62 C63 140.2(3) . . . . ? C50 P3 C62 C67 -166.3(3) . . . . ? C56 P3 C62 C67 84.8(4) . . . . ? Rh3 P3 C62 C67 -41.8(4) . . . . ? C67 C62 C63 C64 -1.3(7) . . . . ? P3 C62 C63 C64 176.7(4) . . . . ? C62 C63 C64 C65 -0.5(7) . . . . ? C63 C64 C65 C66 1.2(7) . . . . ? C64 C65 C66 C67 -0.1(7) . . . . ? C65 C66 C67 C62 -1.7(7) . . . . ? C63 C62 C67 C66 2.4(7) . . . . ? P3 C62 C67 C66 -175.7(3) . . . . ? C70B Cl5 C70A Cl6A -31.1(19) . . . . ? C70A Cl5 C70B Cl6B 33.8(11) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.275 _refine_diff_density_min -1.358 _refine_diff_density_rms 0.125 data_14 _database_code_depnum_ccdc_archive 'CCDC 826265' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 N4 O4 Rh3 S2, 2(C H2 Cl2), B F4' _chemical_formula_sum 'C22 H26 B Cl4 F4 N4 O4 Rh3 S2' _chemical_formula_weight 1011.93 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' B B 0.0013 0.0007 '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' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.979(2) _cell_length_b 13.334(3) _cell_length_c 13.909(3) _cell_angle_alpha 99.01(3) _cell_angle_beta 109.00(3) _cell_angle_gamma 114.02(3) _cell_volume 1657.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7645 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.48 _exptl_crystal_description plates _exptl_crystal_colour violet _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.984 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 5.6 _diffrn_reflns_number 18603 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7519 _reflns_number_gt 6849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0393P)^2^+75.2787P] 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_number_reflns 7519 _refine_ls_number_parameters 419 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_restrained_S_all 1.167 _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 0.14024(10) 0.88830(7) 0.99432(7) 0.0135(2) Uani 1 1 d . . . Rh2 Rh 0.24503(10) 0.56725(7) 0.87534(7) 0.0144(2) Uani 1 1 d . . . Rh3 Rh 0.32776(9) 0.77316(7) 1.06466(7) 0.01049(19) Uani 1 1 d . . . S1 S 0.0673(3) 0.6919(2) 0.9958(2) 0.0150(5) Uani 1 1 d . . . S2 S 0.3429(3) 0.7706(2) 0.8977(2) 0.0149(5) Uani 1 1 d . . . N1 N 0.0322(11) 0.5454(8) 0.8124(8) 0.0167(19) Uani 1 1 d . . . N2 N -0.1535(11) 0.5796(9) 0.7882(9) 0.021(2) Uani 1 1 d . . . N3 N 0.1351(11) 0.8408(8) 0.8443(8) 0.018(2) Uani 1 1 d . . . N4 N 0.1407(11) 0.7445(8) 0.7010(8) 0.0165(19) Uani 1 1 d . . . O1 O 0.2226(11) 1.1330(8) 0.9967(8) 0.029(2) Uani 1 1 d . . . O2 O 0.1111(13) 0.9492(9) 1.1995(9) 0.036(2) Uani 1 1 d . . . O3 O 0.1313(11) 0.3127(8) 0.8470(8) 0.030(2) Uani 1 1 d . . . O4 O 0.5511(10) 0.5993(8) 0.9513(8) 0.027(2) Uani 1 1 d . . . C1 C 0.1966(12) 0.7838(9) 0.8103(9) 0.015(2) Uani 1 1 d . . . C2 C 0.0351(14) 0.8393(11) 0.7492(10) 0.022(3) Uani 1 1 d . . . H2 H -0.0256 0.8741 0.7467 0.026 Uiso 1 1 calc R . . C3 C 0.0381(14) 0.7804(11) 0.6613(10) 0.022(3) Uani 1 1 d . . . H3 H -0.0187 0.7668 0.5877 0.026 Uiso 1 1 calc R . . C4 C 0.1793(16) 0.6766(11) 0.6337(10) 0.024(3) Uani 1 1 d . . . H4A H 0.2592 0.7299 0.6197 0.036 Uiso 1 1 calc R . . H4B H 0.0924 0.6251 0.5652 0.036 Uiso 1 1 calc R . . H4C H 0.2119 0.6297 0.6717 0.036 Uiso 1 1 calc R . . C5 C -0.0190(13) 0.6036(10) 0.8601(9) 0.015(2) Uani 1 1 d . . . C6 C -0.0740(14) 0.4836(10) 0.7047(10) 0.022(3) Uani 1 1 d . . . H6 H -0.0671 0.4355 0.6509 0.027 Uiso 1 1 calc R . . C7 C -0.1889(15) 0.5051(11) 0.6914(11) 0.027(3) Uani 1 1 d . . . H7 H -0.2769 0.4741 0.6270 0.032 Uiso 1 1 calc R . . C8 C -0.2427(15) 0.6281(12) 0.8124(13) 0.030(3) Uani 1 1 d . . . H8A H -0.2388 0.6271 0.8836 0.045 Uiso 1 1 calc R . . H8B H -0.3454 0.5811 0.7576 0.045 Uiso 1 1 calc R . . H8C H -0.2034 0.7085 0.8122 0.045 Uiso 1 1 calc R . . C9 C 0.1932(13) 1.0416(11) 0.9948(9) 0.018(2) Uani 1 1 d . . . C10 C 0.1250(13) 0.9228(11) 1.1243(9) 0.017(2) Uani 1 1 d . . . C11 C 0.1709(14) 0.4082(10) 0.8567(10) 0.022(2) Uani 1 1 d . . . C12 C 0.4368(14) 0.5884(10) 0.9225(10) 0.022(3) Uani 1 1 d . . . C13 C 0.5445(13) 0.9230(11) 1.1504(10) 0.021(2) Uani 1 1 d . . . H13 H 0.5763 0.9700 1.1051 0.025 Uiso 1 1 calc R . . C14 C 0.5615(13) 0.8238(10) 1.1380(10) 0.017(2) Uani 1 1 d . . . H14 H 0.6017 0.8127 1.0846 0.020 Uiso 1 1 calc R . . C15 C 0.6004(14) 0.7740(11) 1.2276(10) 0.021(2) Uani 1 1 d . . . H15A H 0.6581 0.8375 1.2982 0.025 Uiso 1 1 calc R . . H15B H 0.6628 0.7404 1.2179 0.025 Uiso 1 1 calc R . . C16 C 0.4600(13) 0.6788(11) 1.2273(10) 0.020(2) Uani 1 1 d . . . H16A H 0.4322 0.6026 1.1787 0.024 Uiso 1 1 calc R . . H16B H 0.4830 0.6743 1.3009 0.024 Uiso 1 1 calc R . . C17 C 0.3293(13) 0.6997(10) 1.1914(9) 0.017(2) Uani 1 1 d . . . H17 H 0.2329 0.6305 1.1741 0.020 Uiso 1 1 calc R . . C18 C 0.3359(14) 0.8072(10) 1.2271(9) 0.019(2) Uani 1 1 d . . . H18 H 0.2423 0.8001 1.2285 0.022 Uiso 1 1 calc R . . C19 C 0.4733(14) 0.9186(11) 1.3072(9) 0.020(2) Uani 1 1 d . . . H19A H 0.5395 0.8988 1.3582 0.024 Uiso 1 1 calc R . . H19B H 0.4447 0.9645 1.3494 0.024 Uiso 1 1 calc R . . C20 C 0.5580(15) 0.9937(11) 1.2537(10) 0.021(2) Uani 1 1 d . . . H20A H 0.5203 1.0480 1.2374 0.025 Uiso 1 1 calc R . . H20B H 0.6637 1.0410 1.3052 0.025 Uiso 1 1 calc R . . C21 C 0.4393(17) 0.2697(14) 0.4001(12) 0.033(3) Uani 1 1 d . . . H21A H 0.4921 0.3559 0.4239 0.039 Uiso 1 1 calc R . . H21B H 0.3411 0.2439 0.4003 0.039 Uiso 1 1 calc R . . C22 C 0.0474(16) 0.8915(11) 0.4004(11) 0.026(3) Uani 1 1 d . . . H22A H -0.0116 0.8668 0.3216 0.031 Uiso 1 1 calc R . . H22B H -0.0215 0.8599 0.4331 0.031 Uiso 1 1 calc R . . Cl1 Cl 0.5398(4) 0.2236(3) 0.4917(3) 0.0315(7) Uani 1 1 d . . . Cl2 Cl 0.4156(5) 0.2136(3) 0.2676(3) 0.0415(10) Uani 1 1 d . . . Cl3 Cl 0.1457(4) 1.0457(3) 0.4552(3) 0.0271(6) Uani 1 1 d . . . Cl4 Cl 0.1713(5) 0.8352(4) 0.4258(3) 0.0434(9) Uani 1 1 d . . . F1 F 0.6196(11) 0.5283(9) 0.2970(8) 0.051(3) Uani 1 1 d . . . B1A B 0.701(2) 0.5823(18) 0.408(2) 0.022(5) Uani 0.66(2) 1 d PD A 1 F2A F 0.594(3) 0.5460(19) 0.446(2) 0.092(9) Uani 0.66(2) 1 d PD A 1 F3A F 0.805(3) 0.549(2) 0.4492(18) 0.076(9) Uani 0.66(2) 1 d PD A 1 F4A F 0.763(3) 0.7021(15) 0.4361(15) 0.049(6) Uani 0.66(2) 1 d PD A 1 B1B B 0.724(4) 0.587(3) 0.392(4) 0.022(5) Uani 0.34(2) 1 d PD A 2 F2B F 0.860(3) 0.634(3) 0.389(3) 0.059(10) Uani 0.34(2) 1 d PD A 2 F3B F 0.720(6) 0.674(4) 0.456(4) 0.076(9) Uani 0.34(2) 1 d PD A 2 F4B F 0.739(5) 0.520(3) 0.457(3) 0.049(6) Uani 0.34(2) 1 d PD A 2 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 0.0175(4) 0.0108(4) 0.0140(4) 0.0053(3) 0.0060(3) 0.0088(3) Rh2 0.0189(4) 0.0107(4) 0.0163(4) 0.0059(3) 0.0078(3) 0.0088(3) Rh3 0.0120(4) 0.0086(4) 0.0112(4) 0.0051(3) 0.0042(3) 0.0053(3) S1 0.0162(12) 0.0119(12) 0.0178(13) 0.0065(10) 0.0068(11) 0.0075(10) S2 0.0174(13) 0.0122(12) 0.0152(13) 0.0067(10) 0.0055(10) 0.0077(11) N1 0.019(5) 0.011(4) 0.011(4) 0.005(4) 0.002(4) 0.002(4) N2 0.020(5) 0.017(5) 0.027(6) 0.013(4) 0.007(4) 0.011(4) N3 0.020(5) 0.009(4) 0.023(5) 0.008(4) 0.007(4) 0.006(4) N4 0.019(5) 0.014(5) 0.014(5) 0.005(4) 0.004(4) 0.007(4) O1 0.041(6) 0.017(5) 0.041(6) 0.015(4) 0.024(5) 0.017(4) O2 0.061(7) 0.028(5) 0.032(6) 0.014(4) 0.023(5) 0.030(5) O3 0.038(5) 0.020(5) 0.035(5) 0.010(4) 0.015(5) 0.017(4) O4 0.026(5) 0.018(4) 0.037(5) 0.011(4) 0.013(4) 0.011(4) C1 0.016(5) 0.006(5) 0.012(5) 0.002(4) 0.002(4) -0.001(4) C2 0.023(6) 0.019(6) 0.026(6) 0.017(5) 0.005(5) 0.014(5) C3 0.025(6) 0.023(6) 0.013(5) 0.010(5) 0.001(5) 0.011(5) C4 0.038(7) 0.019(6) 0.015(6) 0.005(5) 0.011(5) 0.015(6) C5 0.022(6) 0.014(5) 0.013(5) 0.011(4) 0.009(4) 0.008(5) C6 0.028(6) 0.010(5) 0.018(6) 0.005(5) 0.004(5) 0.003(5) C7 0.028(7) 0.011(6) 0.025(7) 0.008(5) 0.002(5) 0.001(5) C8 0.026(7) 0.026(7) 0.042(8) 0.013(6) 0.012(6) 0.017(6) C9 0.016(5) 0.021(6) 0.012(5) 0.001(4) 0.002(4) 0.010(5) C10 0.023(6) 0.021(6) 0.013(5) 0.009(5) 0.012(5) 0.011(5) C11 0.022(6) 0.011(6) 0.022(6) -0.002(5) 0.005(5) 0.006(5) C12 0.026(6) 0.013(5) 0.024(6) -0.001(5) 0.013(5) 0.008(5) C13 0.021(6) 0.019(6) 0.019(6) 0.011(5) 0.006(5) 0.008(5) C14 0.019(5) 0.014(5) 0.019(6) 0.008(4) 0.009(5) 0.007(5) C15 0.022(6) 0.026(6) 0.024(6) 0.015(5) 0.007(5) 0.020(5) C16 0.016(5) 0.021(6) 0.020(6) 0.016(5) 0.001(5) 0.009(5) C17 0.024(6) 0.016(5) 0.014(5) 0.013(4) 0.007(5) 0.011(5) C18 0.029(6) 0.014(5) 0.016(5) 0.006(4) 0.008(5) 0.013(5) C19 0.028(6) 0.018(6) 0.012(5) 0.003(4) 0.004(5) 0.014(5) C20 0.034(7) 0.017(6) 0.020(6) 0.010(5) 0.013(5) 0.019(5) C21 0.039(8) 0.033(8) 0.035(8) 0.010(6) 0.014(7) 0.027(7) C22 0.033(7) 0.014(6) 0.029(7) 0.007(5) 0.015(6) 0.010(5) Cl1 0.0380(18) 0.0306(17) 0.0291(17) 0.0156(14) 0.0135(14) 0.0184(15) Cl2 0.060(2) 0.037(2) 0.0260(17) 0.0043(15) 0.0031(16) 0.036(2) Cl3 0.0329(16) 0.0203(15) 0.0255(15) 0.0064(12) 0.0115(13) 0.0121(13) Cl4 0.062(3) 0.046(2) 0.046(2) 0.0219(19) 0.027(2) 0.043(2) F1 0.047(6) 0.052(6) 0.033(5) -0.010(4) -0.008(4) 0.035(5) B1A 0.037(11) 0.015(7) 0.028(11) 0.013(7) 0.023(8) 0.016(8) F2A 0.13(2) 0.069(14) 0.115(19) 0.037(13) 0.107(18) 0.044(14) F3A 0.073(14) 0.059(14) 0.055(11) -0.028(10) -0.027(10) 0.056(13) F4A 0.066(12) 0.024(7) 0.033(8) 0.015(6) -0.008(7) 0.021(8) B1B 0.037(11) 0.015(7) 0.028(11) 0.013(7) 0.023(8) 0.016(8) F2B 0.038(17) 0.06(2) 0.049(19) 0.007(16) 0.016(14) -0.001(15) F3B 0.073(14) 0.059(14) 0.055(11) -0.028(10) -0.027(10) 0.056(13) F4B 0.066(12) 0.024(7) 0.033(8) 0.015(6) -0.008(7) 0.021(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 Rh1 C10 1.873(11) . ? Rh1 C9 1.882(13) . ? Rh1 N3 2.058(11) . ? Rh1 S1 2.412(3) . ? Rh1 Rh3 3.0471(14) . ? Rh1 Rh2 5.0417(17) . ? Rh2 C12 1.871(13) . ? Rh2 C11 1.875(12) . ? Rh2 N1 2.084(10) . ? Rh2 S2 2.398(3) . ? Rh2 Rh3 3.0734(19) . ? Rh3 C17 2.145(11) . ? Rh3 C13 2.148(13) . ? Rh3 C14 2.180(12) . ? Rh3 C18 2.198(12) . ? Rh3 S1 2.374(3) . ? Rh3 S2 2.377(3) . ? S1 C5 1.755(12) . ? S2 C1 1.765(12) . ? N1 C5 1.339(15) . ? N1 C6 1.406(15) . ? N2 C5 1.355(15) . ? N2 C7 1.370(18) . ? N2 C8 1.468(16) . ? N3 C1 1.331(15) . ? N3 C2 1.408(15) . ? N4 C1 1.357(15) . ? N4 C3 1.387(15) . ? N4 C4 1.476(15) . ? O1 C9 1.120(15) . ? O2 C10 1.128(15) . ? O3 C11 1.133(15) . ? O4 C12 1.124(16) . ? C2 C3 1.363(19) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C6 C7 1.37(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C13 C14 1.402(17) . ? C13 C20 1.516(17) . ? C13 H13 1.0000 . ? C14 C15 1.523(16) . ? C14 H14 1.0000 . ? C15 C16 1.546(17) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.513(16) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.405(16) . ? C17 H17 1.0000 . ? C18 C19 1.513(17) . ? C18 H18 1.0000 . ? C19 C20 1.532(17) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 Cl1 1.761(14) . ? C21 Cl2 1.766(15) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 Cl3 1.772(13) . ? C22 Cl4 1.773(14) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? F1 B1B 1.28(5) . ? F1 B1A 1.38(3) . ? B1A F3A 1.380(15) . ? B1A F4A 1.382(15) . ? B1A F2A 1.386(15) . ? B1B F4B 1.381(18) . ? B1B F3B 1.382(18) . ? B1B F2B 1.382(18) . ? 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 C10 Rh1 C9 90.6(5) . . ? C10 Rh1 N3 174.5(5) . . ? C9 Rh1 N3 91.2(4) . . ? C10 Rh1 S1 88.1(4) . . ? C9 Rh1 S1 178.3(4) . . ? N3 Rh1 S1 90.0(3) . . ? C10 Rh1 Rh3 95.7(4) . . ? C9 Rh1 Rh3 131.3(4) . . ? N3 Rh1 Rh3 87.1(3) . . ? S1 Rh1 Rh3 49.91(7) . . ? C10 Rh1 Rh2 122.7(4) . . ? C9 Rh1 Rh2 139.3(4) . . ? N3 Rh1 Rh2 58.1(3) . . ? S1 Rh1 Rh2 42.38(7) . . ? Rh3 Rh1 Rh2 34.71(3) . . ? C12 Rh2 C11 89.8(5) . . ? C12 Rh2 N1 175.8(5) . . ? C11 Rh2 N1 91.5(5) . . ? C12 Rh2 S2 89.4(4) . . ? C11 Rh2 S2 178.9(4) . . ? N1 Rh2 S2 89.3(3) . . ? C12 Rh2 Rh3 94.4(4) . . ? C11 Rh2 Rh3 131.2(4) . . ? N1 Rh2 Rh3 87.8(3) . . ? S2 Rh2 Rh3 49.64(7) . . ? C12 Rh2 Rh1 122.5(4) . . ? C11 Rh2 Rh1 138.5(4) . . ? N1 Rh2 Rh1 58.3(3) . . ? S2 Rh2 Rh1 42.51(7) . . ? Rh3 Rh2 Rh1 34.37(3) . . ? C17 Rh3 C13 97.7(5) . . ? C17 Rh3 C14 81.5(4) . . ? C13 Rh3 C14 37.8(4) . . ? C17 Rh3 C18 37.7(4) . . ? C13 Rh3 C18 81.2(5) . . ? C14 Rh3 C18 88.6(5) . . ? C17 Rh3 S1 90.1(3) . . ? C13 Rh3 S1 149.2(4) . . ? C14 Rh3 S1 170.5(3) . . ? C18 Rh3 S1 87.4(3) . . ? C17 Rh3 S2 150.1(3) . . ? C13 Rh3 S2 90.9(3) . . ? C14 Rh3 S2 88.2(3) . . ? C18 Rh3 S2 170.4(3) . . ? S1 Rh3 S2 97.00(11) . . ? C17 Rh3 Rh1 122.2(3) . . ? C13 Rh3 Rh1 100.9(3) . . ? C14 Rh3 Rh1 137.8(3) . . ? C18 Rh3 Rh1 92.6(3) . . ? S1 Rh3 Rh1 51.02(7) . . ? S2 Rh3 Rh1 83.70(7) . . ? C17 Rh3 Rh2 102.5(3) . . ? C13 Rh3 Rh2 123.7(4) . . ? C14 Rh3 Rh2 94.6(3) . . ? C18 Rh3 Rh2 139.1(3) . . ? S1 Rh3 Rh2 82.87(9) . . ? S2 Rh3 Rh2 50.24(7) . . ? Rh1 Rh3 Rh2 110.92(5) . . ? C5 S1 Rh3 110.5(4) . . ? C5 S1 Rh1 105.9(4) . . ? Rh3 S1 Rh1 79.08(10) . . ? C1 S2 Rh3 109.9(4) . . ? C1 S2 Rh2 106.0(4) . . ? Rh3 S2 Rh2 80.13(10) . . ? C5 N1 C6 107.1(10) . . ? C5 N1 Rh2 126.5(8) . . ? C6 N1 Rh2 125.5(9) . . ? C5 N2 C7 108.6(11) . . ? C5 N2 C8 124.4(11) . . ? C7 N2 C8 126.9(11) . . ? C1 N3 C2 104.6(10) . . ? C1 N3 Rh1 129.5(8) . . ? C2 N3 Rh1 124.6(8) . . ? C1 N4 C3 107.3(10) . . ? C1 N4 C4 127.9(10) . . ? C3 N4 C4 124.7(10) . . ? N3 C1 N4 112.0(10) . . ? N3 C1 S2 123.6(9) . . ? N4 C1 S2 124.2(9) . . ? C3 C2 N3 110.0(11) . . ? C3 C2 H2 125.0 . . ? N3 C2 H2 125.0 . . ? C2 C3 N4 106.1(10) . . ? C2 C3 H3 127.0 . . ? N4 C3 H3 127.0 . . ? N4 C4 H4A 109.5 . . ? N4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 N2 109.4(10) . . ? N1 C5 S1 126.3(9) . . ? N2 C5 S1 124.2(9) . . ? C7 C6 N1 107.7(12) . . ? C7 C6 H6 126.2 . . ? N1 C6 H6 126.2 . . ? C6 C7 N2 107.2(11) . . ? C6 C7 H7 126.4 . . ? N2 C7 H7 126.4 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 Rh1 178.0(11) . . ? O2 C10 Rh1 174.3(11) . . ? O3 C11 Rh2 177.4(12) . . ? O4 C12 Rh2 178.7(12) . . ? C14 C13 C20 124.9(11) . . ? C14 C13 Rh3 72.3(7) . . ? C20 C13 Rh3 110.1(9) . . ? C14 C13 H13 114.0 . . ? C20 C13 H13 114.0 . . ? Rh3 C13 H13 114.0 . . ? C13 C14 C15 124.6(11) . . ? C13 C14 Rh3 69.9(7) . . ? C15 C14 Rh3 112.8(8) . . ? C13 C14 H14 113.9 . . ? C15 C14 H14 113.9 . . ? Rh3 C14 H14 113.9 . . ? C14 C15 C16 111.4(9) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 113.7(9) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 124.7(11) . . ? C18 C17 Rh3 73.2(7) . . ? C16 C17 Rh3 109.4(8) . . ? C18 C17 H17 114.0 . . ? C16 C17 H17 114.0 . . ? Rh3 C17 H17 114.0 . . ? C17 C18 C19 125.4(11) . . ? C17 C18 Rh3 69.1(6) . . ? C19 C18 Rh3 112.1(8) . . ? C17 C18 H18 113.9 . . ? C19 C18 H18 113.9 . . ? Rh3 C18 H18 113.9 . . ? C18 C19 C20 113.1(10) . . ? C18 C19 H19A 109.0 . . ? C20 C19 H19A 109.0 . . ? C18 C19 H19B 109.0 . . ? C20 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C13 C20 C19 113.3(10) . . ? C13 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C13 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? Cl1 C21 Cl2 112.0(7) . . ? Cl1 C21 H21A 109.2 . . ? Cl2 C21 H21A 109.2 . . ? Cl1 C21 H21B 109.2 . . ? Cl2 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? Cl3 C22 Cl4 110.5(8) . . ? Cl3 C22 H22A 109.5 . . ? Cl4 C22 H22A 109.5 . . ? Cl3 C22 H22B 109.5 . . ? Cl4 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? B1B F1 B1A 15.6(15) . . ? F3A B1A F4A 112(2) . . ? F3A B1A F1 112.0(17) . . ? F4A B1A F1 111.7(16) . . ? F3A B1A F2A 111(2) . . ? F4A B1A F2A 106.4(19) . . ? F1 B1A F2A 103.2(18) . . ? F1 B1B F4B 114(3) . . ? F1 B1B F3B 119(3) . . ? F4B B1B F3B 103(4) . . ? F1 B1B F2B 111(3) . . ? F4B B1B F2B 101(3) . . ? F3B B1B F2B 107(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Rh1 Rh2 C12 -83.7(7) . . . . ? C9 Rh1 Rh2 C12 56.1(7) . . . . ? N3 Rh1 Rh2 C12 102.8(6) . . . . ? S1 Rh1 Rh2 C12 -124.1(5) . . . . ? Rh3 Rh1 Rh2 C12 -39.6(5) . . . . ? C10 Rh1 Rh2 C11 52.0(7) . . . . ? C9 Rh1 Rh2 C11 -168.2(8) . . . . ? N3 Rh1 Rh2 C11 -121.5(7) . . . . ? S1 Rh1 Rh2 C11 11.6(6) . . . . ? Rh3 Rh1 Rh2 C11 96.1(6) . . . . ? C10 Rh1 Rh2 N1 101.2(5) . . . . ? C9 Rh1 Rh2 N1 -119.0(6) . . . . ? N3 Rh1 Rh2 N1 -72.3(4) . . . . ? S1 Rh1 Rh2 N1 60.7(3) . . . . ? Rh3 Rh1 Rh2 N1 145.2(3) . . . . ? C10 Rh1 Rh2 S2 -128.2(5) . . . . ? C9 Rh1 Rh2 S2 11.6(5) . . . . ? N3 Rh1 Rh2 S2 58.3(3) . . . . ? S1 Rh1 Rh2 S2 -168.61(14) . . . . ? Rh3 Rh1 Rh2 S2 -84.10(11) . . . . ? C10 Rh1 Rh2 Rh3 -44.1(4) . . . . ? C9 Rh1 Rh2 Rh3 95.7(5) . . . . ? N3 Rh1 Rh2 Rh3 142.4(3) . . . . ? S1 Rh1 Rh2 Rh3 -84.50(11) . . . . ? C10 Rh1 Rh3 C17 23.1(5) . . . . ? C9 Rh1 Rh3 C17 118.9(6) . . . . ? N3 Rh1 Rh3 C17 -152.1(5) . . . . ? S1 Rh1 Rh3 C17 -59.6(4) . . . . ? Rh2 Rh1 Rh3 C17 -120.9(4) . . . . ? C10 Rh1 Rh3 C13 -83.3(5) . . . . ? C9 Rh1 Rh3 C13 12.5(6) . . . . ? N3 Rh1 Rh3 C13 101.5(4) . . . . ? S1 Rh1 Rh3 C13 -166.0(4) . . . . ? Rh2 Rh1 Rh3 C13 132.7(3) . . . . ? C10 Rh1 Rh3 C14 -92.7(6) . . . . ? C9 Rh1 Rh3 C14 3.1(7) . . . . ? N3 Rh1 Rh3 C14 92.1(5) . . . . ? S1 Rh1 Rh3 C14 -175.4(5) . . . . ? Rh2 Rh1 Rh3 C14 123.3(5) . . . . ? C10 Rh1 Rh3 C18 -1.9(5) . . . . ? C9 Rh1 Rh3 C18 94.0(6) . . . . ? N3 Rh1 Rh3 C18 -177.0(4) . . . . ? S1 Rh1 Rh3 C18 -84.5(3) . . . . ? Rh2 Rh1 Rh3 C18 -145.8(3) . . . . ? C10 Rh1 Rh3 S1 82.7(4) . . . . ? C9 Rh1 Rh3 S1 178.5(5) . . . . ? N3 Rh1 Rh3 S1 -92.5(3) . . . . ? Rh2 Rh1 Rh3 S1 -61.29(10) . . . . ? C10 Rh1 Rh3 S2 -173.0(4) . . . . ? C9 Rh1 Rh3 S2 -77.2(5) . . . . ? N3 Rh1 Rh3 S2 11.8(3) . . . . ? S1 Rh1 Rh3 S2 104.31(12) . . . . ? Rh2 Rh1 Rh3 S2 43.02(8) . . . . ? C10 Rh1 Rh3 Rh2 144.0(4) . . . . ? C9 Rh1 Rh3 Rh2 -120.2(5) . . . . ? N3 Rh1 Rh3 Rh2 -31.2(3) . . . . ? S1 Rh1 Rh3 Rh2 61.29(10) . . . . ? C12 Rh2 Rh3 C17 -80.7(5) . . . . ? C11 Rh2 Rh3 C17 12.9(6) . . . . ? N1 Rh2 Rh3 C17 102.9(4) . . . . ? S2 Rh2 Rh3 C17 -166.2(3) . . . . ? Rh1 Rh2 Rh3 C17 131.9(3) . . . . ? C12 Rh2 Rh3 C13 27.5(6) . . . . ? C11 Rh2 Rh3 C13 121.1(6) . . . . ? N1 Rh2 Rh3 C13 -148.9(5) . . . . ? S2 Rh2 Rh3 C13 -57.9(4) . . . . ? Rh1 Rh2 Rh3 C13 -119.8(4) . . . . ? C12 Rh2 Rh3 C14 1.6(5) . . . . ? C11 Rh2 Rh3 C14 95.2(6) . . . . ? N1 Rh2 Rh3 C14 -174.8(4) . . . . ? S2 Rh2 Rh3 C14 -83.8(3) . . . . ? Rh1 Rh2 Rh3 C14 -145.8(3) . . . . ? C12 Rh2 Rh3 C18 -91.6(7) . . . . ? C11 Rh2 Rh3 C18 2.0(7) . . . . ? N1 Rh2 Rh3 C18 92.0(6) . . . . ? S2 Rh2 Rh3 C18 -177.1(5) . . . . ? Rh1 Rh2 Rh3 C18 121.0(5) . . . . ? C12 Rh2 Rh3 S1 -169.3(4) . . . . ? C11 Rh2 Rh3 S1 -75.6(5) . . . . ? N1 Rh2 Rh3 S1 14.4(3) . . . . ? S2 Rh2 Rh3 S1 105.30(12) . . . . ? Rh1 Rh2 Rh3 S1 43.40(7) . . . . ? C12 Rh2 Rh3 S2 85.4(4) . . . . ? C11 Rh2 Rh3 S2 179.1(5) . . . . ? N1 Rh2 Rh3 S2 -90.9(3) . . . . ? Rh1 Rh2 Rh3 S2 -61.90(10) . . . . ? C12 Rh2 Rh3 Rh1 147.4(4) . . . . ? C11 Rh2 Rh3 Rh1 -119.0(5) . . . . ? N1 Rh2 Rh3 Rh1 -29.0(3) . . . . ? S2 Rh2 Rh3 Rh1 61.90(10) . . . . ? C17 Rh3 S1 C5 -123.9(5) . . . . ? C13 Rh3 S1 C5 130.7(7) . . . . ? C14 Rh3 S1 C5 -96(2) . . . . ? C18 Rh3 S1 C5 -161.5(5) . . . . ? S2 Rh3 S1 C5 27.0(4) . . . . ? Rh1 Rh3 S1 C5 103.0(4) . . . . ? Rh2 Rh3 S1 C5 -21.4(4) . . . . ? C17 Rh3 S1 Rh1 133.1(3) . . . . ? C13 Rh3 S1 Rh1 27.7(7) . . . . ? C14 Rh3 S1 Rh1 161(2) . . . . ? C18 Rh3 S1 Rh1 95.5(3) . . . . ? S2 Rh3 S1 Rh1 -76.02(10) . . . . ? Rh2 Rh3 S1 Rh1 -124.35(7) . . . . ? C10 Rh1 S1 C5 152.5(6) . . . . ? C9 Rh1 S1 C5 114(13) . . . . ? N3 Rh1 S1 C5 -22.2(5) . . . . ? Rh3 Rh1 S1 C5 -108.4(4) . . . . ? Rh2 Rh1 S1 C5 -60.6(4) . . . . ? C10 Rh1 S1 Rh3 -99.1(4) . . . . ? C9 Rh1 S1 Rh3 -138(13) . . . . ? N3 Rh1 S1 Rh3 86.1(3) . . . . ? Rh2 Rh1 S1 Rh3 47.81(6) . . . . ? C17 Rh3 S2 C1 131.5(8) . . . . ? C13 Rh3 S2 C1 -121.3(5) . . . . ? C14 Rh3 S2 C1 -159.0(5) . . . . ? C18 Rh3 S2 C1 -88(2) . . . . ? S1 Rh3 S2 C1 28.9(4) . . . . ? Rh1 Rh3 S2 C1 -20.5(4) . . . . ? Rh2 Rh3 S2 C1 103.5(4) . . . . ? C17 Rh3 S2 Rh2 27.9(7) . . . . ? C13 Rh3 S2 Rh2 135.2(3) . . . . ? C14 Rh3 S2 Rh2 97.5(3) . . . . ? C18 Rh3 S2 Rh2 168(2) . . . . ? S1 Rh3 S2 Rh2 -74.64(10) . . . . ? Rh1 Rh3 S2 Rh2 -124.00(7) . . . . ? C12 Rh2 S2 C1 155.7(6) . . . . ? C11 Rh2 S2 C1 113(23) . . . . ? N1 Rh2 S2 C1 -20.3(5) . . . . ? Rh3 Rh2 S2 C1 -108.0(4) . . . . ? Rh1 Rh2 S2 C1 -60.5(4) . . . . ? C12 Rh2 S2 Rh3 -96.3(4) . . . . ? C11 Rh2 S2 Rh3 -139(23) . . . . ? N1 Rh2 S2 Rh3 87.7(3) . . . . ? Rh1 Rh2 S2 Rh3 47.48(7) . . . . ? C12 Rh2 N1 C5 -127(6) . . . . ? C11 Rh2 N1 C5 125.4(10) . . . . ? S2 Rh2 N1 C5 -55.4(9) . . . . ? Rh3 Rh2 N1 C5 -5.8(9) . . . . ? Rh1 Rh2 N1 C5 -24.6(8) . . . . ? C12 Rh2 N1 C6 41(7) . . . . ? C11 Rh2 N1 C6 -67.5(10) . . . . ? S2 Rh2 N1 C6 111.7(9) . . . . ? Rh3 Rh2 N1 C6 161.3(9) . . . . ? Rh1 Rh2 N1 C6 142.5(10) . . . . ? C10 Rh1 N3 C1 -120(5) . . . . ? C9 Rh1 N3 C1 131.2(10) . . . . ? S1 Rh1 N3 C1 -50.0(10) . . . . ? Rh3 Rh1 N3 C1 -0.1(10) . . . . ? Rh2 Rh1 N3 C1 -20.5(9) . . . . ? C10 Rh1 N3 C2 44(5) . . . . ? C9 Rh1 N3 C2 -64.6(10) . . . . ? S1 Rh1 N3 C2 114.3(9) . . . . ? Rh3 Rh1 N3 C2 164.1(9) . . . . ? Rh2 Rh1 N3 C2 143.8(10) . . . . ? C2 N3 C1 N4 -1.3(13) . . . . ? Rh1 N3 C1 N4 165.3(8) . . . . ? C2 N3 C1 S2 174.4(8) . . . . ? Rh1 N3 C1 S2 -18.9(15) . . . . ? C3 N4 C1 N3 1.3(13) . . . . ? C4 N4 C1 N3 -179.0(11) . . . . ? C3 N4 C1 S2 -174.4(9) . . . . ? C4 N4 C1 S2 5.3(17) . . . . ? Rh3 S2 C1 N3 29.8(10) . . . . ? Rh2 S2 C1 N3 114.9(9) . . . . ? Rh3 S2 C1 N4 -155.0(9) . . . . ? Rh2 S2 C1 N4 -69.9(10) . . . . ? C1 N3 C2 C3 0.8(13) . . . . ? Rh1 N3 C2 C3 -166.7(8) . . . . ? N3 C2 C3 N4 0.0(14) . . . . ? C1 N4 C3 C2 -0.7(13) . . . . ? C4 N4 C3 C2 179.6(11) . . . . ? C6 N1 C5 N2 1.1(12) . . . . ? Rh2 N1 C5 N2 170.1(7) . . . . ? C6 N1 C5 S1 178.2(8) . . . . ? Rh2 N1 C5 S1 -12.7(14) . . . . ? C7 N2 C5 N1 -0.7(13) . . . . ? C8 N2 C5 N1 -180.0(11) . . . . ? C7 N2 C5 S1 -177.9(9) . . . . ? C8 N2 C5 S1 2.8(17) . . . . ? Rh3 S1 C5 N1 28.1(11) . . . . ? Rh1 S1 C5 N1 112.1(9) . . . . ? Rh3 S1 C5 N2 -155.1(9) . . . . ? Rh1 S1 C5 N2 -71.1(10) . . . . ? C5 N1 C6 C7 -1.1(13) . . . . ? Rh2 N1 C6 C7 -170.3(8) . . . . ? N1 C6 C7 N2 0.7(13) . . . . ? C5 N2 C7 C6 -0.1(13) . . . . ? C8 N2 C7 C6 179.2(12) . . . . ? C10 Rh1 C9 O1 -26(34) . . . . ? N3 Rh1 C9 O1 148(34) . . . . ? S1 Rh1 C9 O1 12(45) . . . . ? Rh3 Rh1 C9 O1 -125(34) . . . . ? Rh2 Rh1 C9 O1 -174(34) . . . . ? C9 Rh1 C10 O2 37(12) . . . . ? N3 Rh1 C10 O2 -72(14) . . . . ? S1 Rh1 C10 O2 -142(12) . . . . ? Rh3 Rh1 C10 O2 168(12) . . . . ? Rh2 Rh1 C10 O2 -168(12) . . . . ? C12 Rh2 C11 O3 4(26) . . . . ? N1 Rh2 C11 O3 -180(100) . . . . ? S2 Rh2 C11 O3 47(44) . . . . ? Rh3 Rh2 C11 O3 -91(26) . . . . ? Rh1 Rh2 C11 O3 -140(26) . . . . ? C11 Rh2 C12 O4 -21(58) . . . . ? N1 Rh2 C12 O4 -129(56) . . . . ? S2 Rh2 C12 O4 160(58) . . . . ? Rh3 Rh2 C12 O4 110(58) . . . . ? Rh1 Rh2 C12 O4 131(58) . . . . ? C17 Rh3 C13 C14 65.3(8) . . . . ? C18 Rh3 C13 C14 99.3(7) . . . . ? S1 Rh3 C13 C14 168.7(5) . . . . ? S2 Rh3 C13 C14 -86.0(7) . . . . ? Rh1 Rh3 C13 C14 -169.7(6) . . . . ? Rh2 Rh3 C13 C14 -45.3(8) . . . . ? C17 Rh3 C13 C20 -56.2(8) . . . . ? C14 Rh3 C13 C20 -121.5(11) . . . . ? C18 Rh3 C13 C20 -22.2(8) . . . . ? S1 Rh3 C13 C20 47.2(11) . . . . ? S2 Rh3 C13 C20 152.5(8) . . . . ? Rh1 Rh3 C13 C20 68.7(8) . . . . ? Rh2 Rh3 C13 C20 -166.9(6) . . . . ? C20 C13 C14 C15 -2(2) . . . . ? Rh3 C13 C14 C15 -104.4(11) . . . . ? C20 C13 C14 Rh3 102.6(12) . . . . ? C17 Rh3 C14 C13 -114.5(8) . . . . ? C18 Rh3 C14 C13 -77.2(7) . . . . ? S1 Rh3 C14 C13 -142.5(17) . . . . ? S2 Rh3 C14 C13 93.7(7) . . . . ? Rh1 Rh3 C14 C13 15.1(9) . . . . ? Rh2 Rh3 C14 C13 143.6(7) . . . . ? C17 Rh3 C14 C15 5.6(9) . . . . ? C13 Rh3 C14 C15 120.1(12) . . . . ? C18 Rh3 C14 C15 42.9(9) . . . . ? S1 Rh3 C14 C15 -22(3) . . . . ? S2 Rh3 C14 C15 -146.2(8) . . . . ? Rh1 Rh3 C14 C15 135.2(7) . . . . ? Rh2 Rh3 C14 C15 -96.3(8) . . . . ? C13 C14 C15 C16 93.1(14) . . . . ? Rh3 C14 C15 C16 12.5(13) . . . . ? C14 C15 C16 C17 -32.9(15) . . . . ? C15 C16 C17 C18 -45.4(16) . . . . ? C15 C16 C17 Rh3 37.1(12) . . . . ? C13 Rh3 C17 C18 64.6(8) . . . . ? C14 Rh3 C17 C18 98.8(8) . . . . ? S1 Rh3 C17 C18 -85.6(7) . . . . ? S2 Rh3 C17 C18 170.1(6) . . . . ? Rh1 Rh3 C17 C18 -43.5(8) . . . . ? Rh2 Rh3 C17 C18 -168.3(7) . . . . ? C13 Rh3 C17 C16 -57.0(9) . . . . ? C14 Rh3 C17 C16 -22.8(8) . . . . ? C18 Rh3 C17 C16 -121.6(12) . . . . ? S1 Rh3 C17 C16 152.8(8) . . . . ? S2 Rh3 C17 C16 48.4(12) . . . . ? Rh1 Rh3 C17 C16 -165.1(7) . . . . ? Rh2 Rh3 C17 C16 70.1(8) . . . . ? C16 C17 C18 C19 -0.6(19) . . . . ? Rh3 C17 C18 C19 -102.8(12) . . . . ? C16 C17 C18 Rh3 102.3(11) . . . . ? C13 Rh3 C18 C17 -115.1(8) . . . . ? C14 Rh3 C18 C17 -77.8(8) . . . . ? S1 Rh3 C18 C17 93.6(7) . . . . ? S2 Rh3 C18 C17 -148.8(17) . . . . ? Rh1 Rh3 C18 C17 144.3(7) . . . . ? Rh2 Rh3 C18 C17 17.6(10) . . . . ? C17 Rh3 C18 C19 121.0(12) . . . . ? C13 Rh3 C18 C19 5.9(8) . . . . ? C14 Rh3 C18 C19 43.2(8) . . . . ? S1 Rh3 C18 C19 -145.4(8) . . . . ? S2 Rh3 C18 C19 -28(3) . . . . ? Rh1 Rh3 C18 C19 -94.7(8) . . . . ? Rh2 Rh3 C18 C19 138.6(6) . . . . ? C17 C18 C19 C20 91.0(14) . . . . ? Rh3 C18 C19 C20 11.6(12) . . . . ? C14 C13 C20 C19 -46.5(17) . . . . ? Rh3 C13 C20 C19 35.6(12) . . . . ? C18 C19 C20 C13 -31.3(14) . . . . ? B1B F1 B1A F3A -55(7) . . . . ? B1B F1 B1A F4A 71(7) . . . . ? B1B F1 B1A F2A -175(8) . . . . ? B1A F1 B1B F4B 67(7) . . . . ? B1A F1 B1B F3B -54(7) . . . . ? B1A F1 B1B F2B -179(9) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.975 _refine_diff_density_min -2.333 _refine_diff_density_rms 0.300