# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robin Perutz' _publ_contact_author_email RNP1@YORK.AC.UK _publ_section_title ; Synthesis and structure of "16-electron" rhodium(III) catalysts for transfer hydrogenation of a cyclic imine: mechanistic implications ; loop_ _publ_author_name 'Robin Perutz' 'A. John Blacker' 'Simon B. Duckett' 'Jake Grace' 'David J. Taylor' ; A.C.Whitwood ; # Attachment 'rnp0614m_rev_Rh_C5Me5__TosNC6H4NH__sept_15.cif' data_rnp0614m _database_code_depnum_ccdc_archive 'CCDC 729047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H27 N2 O2 Rh S, 0.5(C7 H8) ' _chemical_formula_sum 'C26.50 H31 N2 O2 Rh S' _chemical_formula_weight 544.50 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 C2/c 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 24.313(2) _cell_length_b 13.1324(13) _cell_length_c 15.5915(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.223(2) _cell_angle_gamma 90.00 _cell_volume 4883.1(8) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9779 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 29.84 _exptl_crystal_description plate _exptl_crystal_colour dark _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details 'SADABS v2.03; (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26956 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 30.01 _reflns_number_total 7031 _reflns_number_gt 5978 _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, 1997)' _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. The toluene of crystallisation was disordered about the centre of inversion. The phenyl ring was constrained to be hexagonal with a C-C bond length which refined to 1.379 angstroms. The C(ipso)-CH3 bond length was restrained to 1.52 angstroms. Several of the atoms in the disordered toluene, particularly C30, show relatively large elongated ellipsoids. This is probably due to the presence of further disorder of the toluene in addition to that already modelled. ; _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^)+(0.0381P)^2^+2.9332P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7031 _refine_ls_number_parameters 325 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0380 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.25266(8) 0.18436(13) 0.31718(12) 0.0236(3) Uani 1 1 d . . . C2 C 0.24692(7) 0.19450(13) 0.22341(12) 0.0236(3) Uani 1 1 d . . . C3 C 0.28607(7) 0.12677(13) 0.19570(12) 0.0239(3) Uani 1 1 d . . . C4 C 0.31505(7) 0.07391(14) 0.27139(12) 0.0246(3) Uani 1 1 d . . . C5 C 0.29452(7) 0.11028(14) 0.34627(12) 0.0245(3) Uani 1 1 d . . . C6 C 0.22282(9) 0.24815(15) 0.37322(14) 0.0315(4) Uani 1 1 d . . . H6A H 0.2157 0.2075 0.4226 0.047 Uiso 1 1 calc R . . H6B H 0.1871 0.2718 0.3385 0.047 Uiso 1 1 calc R . . H6C H 0.2461 0.3070 0.3952 0.047 Uiso 1 1 calc R . . C7 C 0.20943(9) 0.26676(15) 0.16564(14) 0.0321(4) Uani 1 1 d . . . H7A H 0.2281 0.3330 0.1661 0.048 Uiso 1 1 calc R . . H7B H 0.1744 0.2748 0.1870 0.048 Uiso 1 1 calc R . . H7C H 0.2012 0.2399 0.1058 0.048 Uiso 1 1 calc R . . C8 C 0.29567(9) 0.11646(16) 0.10360(12) 0.0324(4) Uani 1 1 d . . . H8A H 0.2602 0.1270 0.0623 0.049 Uiso 1 1 calc R . . H8B H 0.3101 0.0482 0.0953 0.049 Uiso 1 1 calc R . . H8C H 0.3230 0.1675 0.0931 0.049 Uiso 1 1 calc R . . C9 C 0.36165(8) -0.00093(17) 0.27385(16) 0.0349(4) Uani 1 1 d . . . H9A H 0.3557 -0.0392 0.2189 0.052 Uiso 1 1 calc R . . H9B H 0.3623 -0.0481 0.3227 0.052 Uiso 1 1 calc R . . H9C H 0.3975 0.0355 0.2816 0.052 Uiso 1 1 calc R . . C10 C 0.31714(9) 0.07833(18) 0.43878(13) 0.0339(4) Uani 1 1 d . . . H10A H 0.3548 0.1069 0.4581 0.051 Uiso 1 1 calc R . . H10B H 0.3191 0.0039 0.4420 0.051 Uiso 1 1 calc R . . H10C H 0.2923 0.1034 0.4767 0.051 Uiso 1 1 calc R . . C11 C 0.15183(7) -0.11026(13) 0.15710(11) 0.0217(3) Uani 1 1 d . . . C12 C 0.12346(8) -0.17059(14) 0.08851(12) 0.0269(4) Uani 1 1 d . . . H12 H 0.1323 -0.1653 0.0319 0.032 Uiso 1 1 calc R . . C13 C 0.08264(8) -0.23770(15) 0.10327(13) 0.0305(4) Uani 1 1 d . . . H13 H 0.0628 -0.2776 0.0565 0.037 Uiso 1 1 calc R . . C14 C 0.07052(8) -0.24703(14) 0.18640(13) 0.0303(4) Uani 1 1 d . . . H14 H 0.0424 -0.2935 0.1959 0.036 Uiso 1 1 calc R . . C15 C 0.09895(8) -0.18941(14) 0.25582(12) 0.0273(4) Uani 1 1 d . . . H15 H 0.0907 -0.1976 0.3125 0.033 Uiso 1 1 calc R . . C16 C 0.13976(7) -0.11923(13) 0.24202(11) 0.0219(3) Uani 1 1 d . . . C17 C 0.09004(8) 0.01119(15) 0.38601(12) 0.0249(4) Uani 1 1 d . . . C18 C 0.08368(8) 0.11308(16) 0.36338(12) 0.0297(4) Uani 1 1 d . . . H18 H 0.1149 0.1514 0.3530 0.036 Uiso 1 1 calc R . . C19 C 0.03180(8) 0.15886(17) 0.35598(14) 0.0345(4) Uani 1 1 d . . . H19 H 0.0278 0.2290 0.3413 0.041 Uiso 1 1 calc R . . C20 C -0.01475(8) 0.10366(18) 0.36975(13) 0.0345(4) Uani 1 1 d . . . C21 C -0.00774(9) 0.00131(19) 0.39082(15) 0.0381(5) Uani 1 1 d . . . H21 H -0.0391 -0.0379 0.3992 0.046 Uiso 1 1 calc R . . C22 C 0.04445(9) -0.04484(16) 0.39989(14) 0.0335(4) Uani 1 1 d . . . H22 H 0.0488 -0.1147 0.4156 0.040 Uiso 1 1 calc R . . C23 C -0.07151(9) 0.1529(2) 0.36210(17) 0.0490(6) Uani 1 1 d . . . H23A H -0.1001 0.1098 0.3266 0.074 Uiso 1 1 calc R . . H23B H -0.0712 0.2198 0.3343 0.074 Uiso 1 1 calc R . . H23C H -0.0802 0.1613 0.4205 0.074 Uiso 1 1 calc R . . N1 N 0.19166(7) -0.03909(11) 0.14896(10) 0.0225(3) Uani 1 1 d . . . H1 H 0.1968(9) -0.0334(15) 0.1017(16) 0.020(5) Uiso 1 1 d . . . N2 N 0.17183(6) -0.05138(11) 0.30218(9) 0.0213(3) Uani 1 1 d . . . O1 O 0.19653(6) 0.02905(10) 0.44744(8) 0.0267(3) Uani 1 1 d . . . O2 O 0.15529(6) -0.14209(10) 0.43912(9) 0.0314(3) Uani 1 1 d . . . Rh1 Rh 0.226776(5) 0.040101(10) 0.249643(8) 0.01880(5) Uani 1 1 d . . . S2 S 0.157734(19) -0.04348(3) 0.39963(3) 0.02302(9) Uani 1 1 d . . . C24 C 1.0055(3) 0.5014(6) -0.0241(5) 0.080(3) Uani 0.50 1 d PGD A -1 C25 C 0.9731(2) 0.5883(5) -0.0387(3) 0.084(3) Uani 0.50 1 d PG A -1 H25 H 0.9710 0.6254 -0.0916 0.101 Uiso 0.50 1 calc PR A -1 C26 C 0.9438(2) 0.6213(4) 0.0234(4) 0.074(2) Uani 0.50 1 d PG A -1 H26 H 0.9215 0.6811 0.0134 0.089 Uiso 0.50 1 calc PR A -1 C27 C 0.9469(3) 0.5674(6) 0.1002(5) 0.082(3) Uani 0.50 1 d PG A -1 H27 H 0.9268 0.5902 0.1430 0.099 Uiso 0.50 1 calc PR A -1 C28 C 0.9793(4) 0.4806(6) 0.1148(5) 0.096(4) Uani 0.50 1 d PG A -1 H28 H 0.9815 0.4435 0.1677 0.115 Uiso 0.50 1 calc PR A -1 C29 C 1.0086(3) 0.4476(5) 0.0526(6) 0.110(5) Uani 0.50 1 d PG A -1 H29 H 1.0309 0.3878 0.0627 0.132 Uiso 0.50 1 calc PR A -1 C30 C 1.0401(7) 0.4623(17) -0.0880(11) 0.184(12) Uani 0.50 1 d PD A -1 H30A H 1.0155 0.4478 -0.1443 0.276 Uiso 0.50 1 calc PR A -1 H30B H 1.0596 0.3998 -0.0650 0.276 Uiso 0.50 1 calc PR A -1 H30C H 1.0678 0.5139 -0.0962 0.276 Uiso 0.50 1 calc PR 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 C1 0.0244(8) 0.0228(8) 0.0246(8) -0.0054(7) 0.0068(7) -0.0049(7) C2 0.0240(9) 0.0212(8) 0.0256(8) -0.0015(6) 0.0048(7) -0.0044(7) C3 0.0256(8) 0.0234(8) 0.0243(8) -0.0034(7) 0.0093(7) -0.0061(7) C4 0.0217(8) 0.0226(8) 0.0303(9) -0.0013(7) 0.0070(7) -0.0038(7) C5 0.0231(8) 0.0270(9) 0.0229(8) -0.0016(7) 0.0034(6) -0.0066(7) C6 0.0334(10) 0.0290(9) 0.0355(10) -0.0111(8) 0.0149(8) -0.0067(8) C7 0.0333(10) 0.0246(9) 0.0372(11) 0.0044(8) 0.0041(8) -0.0013(8) C8 0.0391(11) 0.0361(10) 0.0253(9) -0.0046(8) 0.0145(8) -0.0082(9) C9 0.0250(10) 0.0304(10) 0.0507(13) -0.0008(9) 0.0110(9) -0.0009(8) C10 0.0296(10) 0.0445(11) 0.0257(9) 0.0039(8) 0.0004(8) -0.0081(9) C11 0.0206(8) 0.0214(8) 0.0226(8) -0.0010(6) 0.0030(6) 0.0020(6) C12 0.0269(9) 0.0290(9) 0.0239(9) -0.0047(7) 0.0025(7) 0.0005(7) C13 0.0276(9) 0.0276(9) 0.0340(10) -0.0086(8) 0.0003(8) -0.0023(7) C14 0.0262(9) 0.0259(9) 0.0388(11) -0.0030(8) 0.0066(8) -0.0059(7) C15 0.0278(9) 0.0280(9) 0.0270(9) 0.0001(7) 0.0074(7) -0.0029(7) C16 0.0219(8) 0.0207(8) 0.0228(8) -0.0010(6) 0.0034(6) 0.0006(6) C17 0.0226(8) 0.0331(9) 0.0195(8) -0.0028(7) 0.0053(7) -0.0015(7) C18 0.0241(9) 0.0366(10) 0.0277(9) 0.0029(8) 0.0030(7) -0.0031(8) C19 0.0298(10) 0.0391(11) 0.0330(10) 0.0013(8) 0.0025(8) 0.0015(8) C20 0.0226(9) 0.0501(13) 0.0301(10) -0.0067(9) 0.0032(7) 0.0013(8) C21 0.0266(10) 0.0470(12) 0.0430(12) -0.0077(10) 0.0130(9) -0.0078(9) C22 0.0315(10) 0.0358(11) 0.0354(11) -0.0046(8) 0.0123(9) -0.0068(8) C23 0.0276(11) 0.0722(17) 0.0472(14) -0.0041(12) 0.0073(10) 0.0065(11) N1 0.0256(8) 0.0260(7) 0.0167(7) -0.0013(6) 0.0057(6) -0.0012(6) N2 0.0224(7) 0.0245(7) 0.0177(7) -0.0014(5) 0.0055(5) -0.0023(5) O1 0.0241(6) 0.0372(7) 0.0187(6) -0.0025(5) 0.0039(5) -0.0025(5) O2 0.0364(7) 0.0330(7) 0.0255(7) 0.0066(5) 0.0080(6) -0.0003(6) Rh1 0.01962(7) 0.01976(7) 0.01744(7) -0.00153(5) 0.00459(5) -0.00123(5) S2 0.0230(2) 0.0286(2) 0.01789(19) 0.00096(15) 0.00496(16) -0.00154(16) C24 0.063(5) 0.101(7) 0.081(7) -0.046(6) 0.026(5) -0.026(5) C25 0.075(6) 0.088(7) 0.081(6) 0.014(5) -0.008(4) -0.035(5) C26 0.065(4) 0.080(5) 0.073(5) 0.006(4) 0.001(4) -0.029(4) C27 0.058(6) 0.123(8) 0.067(5) -0.023(5) 0.016(4) -0.034(5) C28 0.099(10) 0.085(7) 0.095(7) 0.006(6) 0.001(6) 0.001(5) C29 0.073(6) 0.067(7) 0.164(12) -0.025(6) -0.041(7) 0.015(5) C30 0.083(9) 0.32(3) 0.174(17) -0.183(19) 0.088(11) -0.110(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 C1 C5 1.417(3) . ? C1 C2 1.447(2) . ? C1 C6 1.496(3) . ? C1 Rh1 2.1990(17) . ? C2 C3 1.430(2) . ? C2 C7 1.491(3) . ? C2 Rh1 2.1439(17) . ? C3 C4 1.431(3) . ? C3 C8 1.505(2) . ? C3 Rh1 2.1337(17) . ? C4 C5 1.438(3) . ? C4 C9 1.495(3) . ? C4 Rh1 2.1529(18) . ? C5 C10 1.500(3) . ? C5 Rh1 2.2059(17) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.369(2) . ? C11 C12 1.400(2) . ? C11 C16 1.416(2) . ? C12 C13 1.380(3) . ? C12 H12 0.9500 . ? C13 C14 1.389(3) . ? C13 H13 0.9500 . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 C16 1.401(2) . ? C15 H15 0.9500 . ? C16 N2 1.413(2) . ? C17 C22 1.382(3) . ? C17 C18 1.385(3) . ? C17 S2 1.7701(19) . ? C18 C19 1.382(3) . ? C18 H18 0.9500 . ? C19 C20 1.395(3) . ? C19 H19 0.9500 . ? C20 C21 1.386(4) . ? C20 C23 1.508(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N1 Rh1 1.9372(15) . ? N1 H1 0.77(2) . ? N2 S2 1.6247(15) . ? N2 Rh1 2.0796(14) . ? O1 S2 1.4419(13) . ? O2 S2 1.4402(14) . ? C24 C25 1.379(3) . ? C24 C29 1.379(3) . ? C24 C30 1.514(8) . ? C25 C26 1.379(3) . ? C25 H25 0.9500 . ? C26 C27 1.379(3) . ? C26 H26 0.9500 . ? C27 C28 1.379(3) . ? C27 H27 0.9500 . ? C28 C29 1.379(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 C5 C1 C2 107.96(15) . . ? C5 C1 C6 126.67(17) . . ? C2 C1 C6 125.17(17) . . ? C5 C1 Rh1 71.50(10) . . ? C2 C1 Rh1 68.49(9) . . ? C6 C1 Rh1 129.50(13) . . ? C3 C2 C1 108.00(15) . . ? C3 C2 C7 125.31(17) . . ? C1 C2 C7 126.60(17) . . ? C3 C2 Rh1 70.09(10) . . ? C1 C2 Rh1 72.60(10) . . ? C7 C2 Rh1 125.57(13) . . ? C2 C3 C4 107.61(15) . . ? C2 C3 C8 125.48(17) . . ? C4 C3 C8 126.89(17) . . ? C2 C3 Rh1 70.86(10) . . ? C4 C3 Rh1 71.23(10) . . ? C8 C3 Rh1 124.77(13) . . ? C3 C4 C5 108.39(16) . . ? C3 C4 C9 126.11(17) . . ? C5 C4 C9 125.36(18) . . ? C3 C4 Rh1 69.78(10) . . ? C5 C4 Rh1 72.75(10) . . ? C9 C4 Rh1 126.57(13) . . ? C1 C5 C4 108.02(16) . . ? C1 C5 C10 127.29(17) . . ? C4 C5 C10 124.59(18) . . ? C1 C5 Rh1 70.97(10) . . ? C4 C5 Rh1 68.76(10) . . ? C10 C5 Rh1 128.69(13) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 124.59(16) . . ? N1 C11 C16 114.99(15) . . ? C12 C11 C16 120.41(16) . . ? C13 C12 C11 119.84(17) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.13(17) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 121.00(17) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 119.89(17) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 N2 128.95(16) . . ? C15 C16 C11 118.70(16) . . ? N2 C16 C11 112.34(15) . . ? C22 C17 C18 120.07(18) . . ? C22 C17 S2 121.37(16) . . ? C18 C17 S2 118.54(14) . . ? C19 C18 C17 119.78(18) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 121.0(2) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 118.30(19) . . ? C21 C20 C23 120.2(2) . . ? C19 C20 C23 121.5(2) . . ? C20 C21 C22 121.0(2) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C17 C22 C21 119.8(2) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C11 N1 Rh1 119.96(12) . . ? C11 N1 H1 113.8(16) . . ? Rh1 N1 H1 126.2(15) . . ? C16 N2 S2 118.12(12) . . ? C16 N2 Rh1 114.63(11) . . ? S2 N2 Rh1 126.87(8) . . ? N1 Rh1 N2 78.08(6) . . ? N1 Rh1 C3 101.07(7) . . ? N2 Rh1 C3 176.83(6) . . ? N1 Rh1 C2 115.73(7) . . ? N2 Rh1 C2 144.06(6) . . ? C3 Rh1 C2 39.05(7) . . ? N1 Rh1 C4 120.46(7) . . ? N2 Rh1 C4 138.96(7) . . ? C3 Rh1 C4 38.99(7) . . ? C2 Rh1 C4 64.99(7) . . ? N1 Rh1 C1 152.92(7) . . ? N2 Rh1 C1 117.06(6) . . ? C3 Rh1 C1 64.97(7) . . ? C2 Rh1 C1 38.91(7) . . ? C4 Rh1 C1 64.11(7) . . ? N1 Rh1 C5 158.50(7) . . ? N2 Rh1 C5 115.08(6) . . ? C3 Rh1 C5 64.81(7) . . ? C2 Rh1 C5 64.35(7) . . ? C4 Rh1 C5 38.49(7) . . ? C1 Rh1 C5 37.53(7) . . ? O2 S2 O1 116.76(8) . . ? O2 S2 N2 112.09(8) . . ? O1 S2 N2 106.85(8) . . ? O2 S2 C17 107.53(9) . . ? O1 S2 C17 107.07(9) . . ? N2 S2 C17 105.91(8) . . ? C25 C24 C29 120.0 . . ? C25 C24 C30 123.0(10) . . ? C29 C24 C30 117.0(10) . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.0 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C28 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.0 . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 120.0 . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? 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 C1 C2 C3 -0.61(19) . . . . ? C6 C1 C2 C3 174.53(16) . . . . ? Rh1 C1 C2 C3 -61.51(12) . . . . ? C5 C1 C2 C7 -177.33(17) . . . . ? C6 C1 C2 C7 -2.2(3) . . . . ? Rh1 C1 C2 C7 121.77(18) . . . . ? C5 C1 C2 Rh1 60.90(12) . . . . ? C6 C1 C2 Rh1 -123.96(17) . . . . ? C1 C2 C3 C4 1.00(19) . . . . ? C7 C2 C3 C4 177.77(17) . . . . ? Rh1 C2 C3 C4 -62.12(12) . . . . ? C1 C2 C3 C8 -177.28(17) . . . . ? C7 C2 C3 C8 -0.5(3) . . . . ? Rh1 C2 C3 C8 119.60(18) . . . . ? C1 C2 C3 Rh1 63.13(12) . . . . ? C7 C2 C3 Rh1 -120.11(17) . . . . ? C2 C3 C4 C5 -1.0(2) . . . . ? C8 C3 C4 C5 177.23(17) . . . . ? Rh1 C3 C4 C5 -62.90(12) . . . . ? C2 C3 C4 C9 -176.96(17) . . . . ? C8 C3 C4 C9 1.3(3) . . . . ? Rh1 C3 C4 C9 121.15(19) . . . . ? C2 C3 C4 Rh1 61.89(12) . . . . ? C8 C3 C4 Rh1 -119.87(18) . . . . ? C2 C1 C5 C4 -0.02(19) . . . . ? C6 C1 C5 C4 -175.07(17) . . . . ? Rh1 C1 C5 C4 58.98(12) . . . . ? C2 C1 C5 C10 176.36(17) . . . . ? C6 C1 C5 C10 1.3(3) . . . . ? Rh1 C1 C5 C10 -124.64(19) . . . . ? C2 C1 C5 Rh1 -59.00(12) . . . . ? C6 C1 C5 Rh1 125.95(18) . . . . ? C3 C4 C5 C1 0.6(2) . . . . ? C9 C4 C5 C1 176.62(17) . . . . ? Rh1 C4 C5 C1 -60.37(12) . . . . ? C3 C4 C5 C10 -175.86(17) . . . . ? C9 C4 C5 C10 0.1(3) . . . . ? Rh1 C4 C5 C10 123.13(18) . . . . ? C3 C4 C5 Rh1 61.01(12) . . . . ? C9 C4 C5 Rh1 -123.01(19) . . . . ? N1 C11 C12 C13 -177.81(17) . . . . ? C16 C11 C12 C13 1.4(3) . . . . ? C11 C12 C13 C14 -1.4(3) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 1.3(3) . . . . ? C14 C15 C16 N2 177.64(17) . . . . ? C14 C15 C16 C11 -1.2(3) . . . . ? N1 C11 C16 C15 179.19(16) . . . . ? C12 C11 C16 C15 -0.1(3) . . . . ? N1 C11 C16 N2 0.1(2) . . . . ? C12 C11 C16 N2 -179.12(15) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? S2 C17 C18 C19 -177.24(15) . . . . ? C17 C18 C19 C20 -0.9(3) . . . . ? C18 C19 C20 C21 -0.2(3) . . . . ? C18 C19 C20 C23 179.8(2) . . . . ? C19 C20 C21 C22 1.4(3) . . . . ? C23 C20 C21 C22 -178.7(2) . . . . ? C18 C17 C22 C21 0.2(3) . . . . ? S2 C17 C22 C21 178.31(17) . . . . ? C20 C21 C22 C17 -1.4(3) . . . . ? C12 C11 N1 Rh1 179.22(14) . . . . ? C16 C11 N1 Rh1 0.0(2) . . . . ? C15 C16 N2 S2 -5.7(3) . . . . ? C11 C16 N2 S2 173.19(12) . . . . ? C15 C16 N2 Rh1 -179.15(15) . . . . ? C11 C16 N2 Rh1 -0.22(18) . . . . ? C11 N1 Rh1 N2 -0.09(13) . . . . ? C11 N1 Rh1 C3 176.79(13) . . . . ? C11 N1 Rh1 C2 -144.86(13) . . . . ? C11 N1 Rh1 C4 140.27(13) . . . . ? C11 N1 Rh1 C1 -127.59(16) . . . . ? C11 N1 Rh1 C5 130.15(18) . . . . ? C16 N2 Rh1 N1 0.17(12) . . . . ? S2 N2 Rh1 N1 -172.56(12) . . . . ? C16 N2 Rh1 C3 -74.6(11) . . . . ? S2 N2 Rh1 C3 112.7(11) . . . . ? C16 N2 Rh1 C2 117.87(13) . . . . ? S2 N2 Rh1 C2 -54.86(16) . . . . ? C16 N2 Rh1 C4 -122.96(13) . . . . ? S2 N2 Rh1 C4 64.31(15) . . . . ? C16 N2 Rh1 C1 156.24(11) . . . . ? S2 N2 Rh1 C1 -16.49(13) . . . . ? C16 N2 Rh1 C5 -161.84(11) . . . . ? S2 N2 Rh1 C5 25.43(13) . . . . ? C2 C3 Rh1 N1 117.46(10) . . . . ? C4 C3 Rh1 N1 -125.40(11) . . . . ? C8 C3 Rh1 N1 -3.00(17) . . . . ? C2 C3 Rh1 N2 -168.4(11) . . . . ? C4 C3 Rh1 N2 -51.3(11) . . . . ? C8 C3 Rh1 N2 71.1(12) . . . . ? C4 C3 Rh1 C2 117.14(15) . . . . ? C8 C3 Rh1 C2 -120.5(2) . . . . ? C2 C3 Rh1 C4 -117.14(15) . . . . ? C8 C3 Rh1 C4 122.4(2) . . . . ? C2 C3 Rh1 C1 -38.04(10) . . . . ? C4 C3 Rh1 C1 79.10(11) . . . . ? C8 C3 Rh1 C1 -158.50(19) . . . . ? C2 C3 Rh1 C5 -79.67(11) . . . . ? C4 C3 Rh1 C5 37.48(10) . . . . ? C8 C3 Rh1 C5 159.87(18) . . . . ? C3 C2 Rh1 N1 -75.17(12) . . . . ? C1 C2 Rh1 N1 167.57(10) . . . . ? C7 C2 Rh1 N1 44.62(18) . . . . ? C3 C2 Rh1 N2 178.92(10) . . . . ? C1 C2 Rh1 N2 61.66(15) . . . . ? C7 C2 Rh1 N2 -61.3(2) . . . . ? C1 C2 Rh1 C3 -117.25(15) . . . . ? C7 C2 Rh1 C3 119.8(2) . . . . ? C3 C2 Rh1 C4 38.16(10) . . . . ? C1 C2 Rh1 C4 -79.09(11) . . . . ? C7 C2 Rh1 C4 157.95(18) . . . . ? C3 C2 Rh1 C1 117.25(15) . . . . ? C7 C2 Rh1 C1 -123.0(2) . . . . ? C3 C2 Rh1 C5 80.93(11) . . . . ? C1 C2 Rh1 C5 -36.32(10) . . . . ? C7 C2 Rh1 C5 -159.28(18) . . . . ? C3 C4 Rh1 N1 68.13(12) . . . . ? C5 C4 Rh1 N1 -174.06(10) . . . . ? C9 C4 Rh1 N1 -52.45(19) . . . . ? C3 C4 Rh1 N2 176.23(9) . . . . ? C5 C4 Rh1 N2 -65.97(14) . . . . ? C9 C4 Rh1 N2 55.6(2) . . . . ? C5 C4 Rh1 C3 117.80(15) . . . . ? C9 C4 Rh1 C3 -120.6(2) . . . . ? C3 C4 Rh1 C2 -38.21(10) . . . . ? C5 C4 Rh1 C2 79.59(11) . . . . ? C9 C4 Rh1 C2 -158.80(19) . . . . ? C3 C4 Rh1 C1 -81.49(11) . . . . ? C5 C4 Rh1 C1 36.31(10) . . . . ? C9 C4 Rh1 C1 157.9(2) . . . . ? C3 C4 Rh1 C5 -117.80(15) . . . . ? C9 C4 Rh1 C5 121.6(2) . . . . ? C5 C1 Rh1 N1 -143.99(14) . . . . ? C2 C1 Rh1 N1 -25.20(19) . . . . ? C6 C1 Rh1 N1 93.3(2) . . . . ? C5 C1 Rh1 N2 96.68(11) . . . . ? C2 C1 Rh1 N2 -144.54(10) . . . . ? C6 C1 Rh1 N2 -26.0(2) . . . . ? C5 C1 Rh1 C3 -80.61(11) . . . . ? C2 C1 Rh1 C3 38.18(10) . . . . ? C6 C1 Rh1 C3 156.7(2) . . . . ? C5 C1 Rh1 C2 -118.78(15) . . . . ? C6 C1 Rh1 C2 118.5(2) . . . . ? C5 C1 Rh1 C4 -37.23(10) . . . . ? C2 C1 Rh1 C4 81.56(11) . . . . ? C6 C1 Rh1 C4 -159.9(2) . . . . ? C2 C1 Rh1 C5 118.78(15) . . . . ? C6 C1 Rh1 C5 -122.7(2) . . . . ? C1 C5 Rh1 N1 133.11(17) . . . . ? C4 C5 Rh1 N1 14.1(2) . . . . ? C10 C5 Rh1 N1 -103.9(2) . . . . ? C1 C5 Rh1 N2 -102.44(11) . . . . ? C4 C5 Rh1 N2 138.54(10) . . . . ? C10 C5 Rh1 N2 20.6(2) . . . . ? C1 C5 Rh1 C3 81.07(11) . . . . ? C4 C5 Rh1 C3 -37.96(11) . . . . ? C10 C5 Rh1 C3 -155.9(2) . . . . ? C1 C5 Rh1 C2 37.64(10) . . . . ? C4 C5 Rh1 C2 -81.39(11) . . . . ? C10 C5 Rh1 C2 160.6(2) . . . . ? C1 C5 Rh1 C4 119.03(15) . . . . ? C10 C5 Rh1 C4 -118.0(2) . . . . ? C4 C5 Rh1 C1 -119.03(15) . . . . ? C10 C5 Rh1 C1 123.0(2) . . . . ? C16 N2 S2 O2 50.13(15) . . . . ? Rh1 N2 S2 O2 -137.36(10) . . . . ? C16 N2 S2 O1 179.23(13) . . . . ? Rh1 N2 S2 O1 -8.27(12) . . . . ? C16 N2 S2 C17 -66.86(15) . . . . ? Rh1 N2 S2 C17 105.64(11) . . . . ? C22 C17 S2 O2 -9.24(19) . . . . ? C18 C17 S2 O2 168.91(15) . . . . ? C22 C17 S2 O1 -135.47(16) . . . . ? C18 C17 S2 O1 42.68(17) . . . . ? C22 C17 S2 N2 110.78(17) . . . . ? C18 C17 S2 N2 -71.07(16) . . . . ? C29 C24 C25 C26 0.0 . . . . ? C30 C24 C25 C26 -178.2(11) . . . . ? C24 C25 C26 C27 0.0 . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C27 C28 C29 0.0 . . . . ? C27 C28 C29 C24 0.0 . . . . ? C25 C24 C29 C28 0.0 . . . . ? C30 C24 C29 C28 178.3(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.77(2) 2.41(2) 3.170(2) 170(2) 6 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.839 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.086 # Attachment 'rnp0701m_Rh_C5Me5_tosNC6H4NTos__rev.cif' data_rnp0701m _database_code_depnum_ccdc_archive 'CCDC 729048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H33 N2 O4 Rh S2' _chemical_formula_sum 'C30 H33 N2 O4 Rh S2' _chemical_formula_weight 652.61 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6640(8) _cell_length_b 12.2229(11) _cell_length_c 14.2366(13) _cell_angle_alpha 76.388(2) _cell_angle_beta 84.315(2) _cell_angle_gamma 75.726(2) _cell_volume 1418.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6505 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.28 _exptl_crystal_description plates _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.015 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.695 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details 'SADABS v2.03;(Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14287 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.30 _reflns_number_total 6939 _reflns_number_gt 5967 _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, 1997)' _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^)+(0.0518P)^2^+0.3361P] 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 6939 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7201(3) 0.0017(2) 0.40846(17) 0.0162(5) Uani 1 1 d . . . C2 C 0.7229(3) -0.0378(2) 0.32208(17) 0.0167(5) Uani 1 1 d . . . C3 C 0.6315(3) 0.0554(2) 0.25327(17) 0.0173(5) Uani 1 1 d . . . C4 C 0.5604(3) 0.1496(2) 0.30084(17) 0.0172(5) Uani 1 1 d . . . C5 C 0.6177(3) 0.1175(2) 0.39611(17) 0.0160(5) Uani 1 1 d . . . C6 C 0.7995(3) -0.0643(2) 0.49959(17) 0.0208(5) Uani 1 1 d . . . H6A H 0.7197 -0.0897 0.5480 0.031 Uiso 1 1 calc R . . H6B H 0.8519 -0.0146 0.5240 0.031 Uiso 1 1 calc R . . H6C H 0.8793 -0.1320 0.4868 0.031 Uiso 1 1 calc R . . C7 C 0.7946(3) -0.1573(2) 0.30696(18) 0.0205(5) Uani 1 1 d . . . H7A H 0.8876 -0.1921 0.3468 0.031 Uiso 1 1 calc R . . H7B H 0.8276 -0.1535 0.2386 0.031 Uiso 1 1 calc R . . H7C H 0.7155 -0.2046 0.3255 0.031 Uiso 1 1 calc R . . C8 C 0.6111(3) 0.0510(2) 0.15160(18) 0.0227(5) Uani 1 1 d . . . H8A H 0.7134 0.0146 0.1237 0.034 Uiso 1 1 calc R . . H8B H 0.5741 0.1298 0.1135 0.034 Uiso 1 1 calc R . . H8C H 0.5325 0.0059 0.1507 0.034 Uiso 1 1 calc R . . C9 C 0.4416(3) 0.2571(2) 0.25759(19) 0.0229(5) Uani 1 1 d . . . H9A H 0.3364 0.2399 0.2602 0.034 Uiso 1 1 calc R . . H9B H 0.4744 0.2852 0.1901 0.034 Uiso 1 1 calc R . . H9C H 0.4364 0.3167 0.2941 0.034 Uiso 1 1 calc R . . C10 C 0.5739(3) 0.1826(2) 0.47535(18) 0.0211(5) Uani 1 1 d . . . H10A H 0.5010 0.2572 0.4512 0.032 Uiso 1 1 calc R . . H10B H 0.6705 0.1957 0.4970 0.032 Uiso 1 1 calc R . . H10C H 0.5216 0.1376 0.5297 0.032 Uiso 1 1 calc R . . C11 C 1.0963(3) 0.15372(19) 0.16289(16) 0.0141(4) Uani 1 1 d . . . C12 C 1.0082(3) 0.2664(2) 0.16426(16) 0.0142(4) Uani 1 1 d . . . C13 C 1.0511(3) 0.3596(2) 0.09771(17) 0.0182(5) Uani 1 1 d . . . H13 H 0.9950 0.4366 0.0991 0.022 Uiso 1 1 calc R . . C14 C 1.1755(3) 0.3398(2) 0.02953(18) 0.0195(5) Uani 1 1 d . . . H14 H 1.2047 0.4035 -0.0148 0.023 Uiso 1 1 calc R . . C15 C 1.2572(3) 0.2282(2) 0.02560(17) 0.0189(5) Uani 1 1 d . . . H15 H 1.3395 0.2153 -0.0226 0.023 Uiso 1 1 calc R . . C16 C 1.2180(3) 0.1345(2) 0.09294(17) 0.0171(5) Uani 1 1 d . . . H16 H 1.2743 0.0577 0.0909 0.020 Uiso 1 1 calc R . . C17 C 1.2211(3) -0.13800(19) 0.19406(16) 0.0146(4) Uani 1 1 d . . . C18 C 1.3648(3) -0.2210(2) 0.20118(18) 0.0185(5) Uani 1 1 d . . . H18 H 1.4379 -0.2257 0.2483 0.022 Uiso 1 1 calc R . . C19 C 1.4002(3) -0.2967(2) 0.13914(19) 0.0209(5) Uani 1 1 d . . . H19 H 1.4976 -0.3537 0.1443 0.025 Uiso 1 1 calc R . . C20 C 1.2944(3) -0.2898(2) 0.06936(19) 0.0215(5) Uani 1 1 d . . . C21 C 1.1522(3) -0.2057(2) 0.06233(18) 0.0206(5) Uani 1 1 d . . . H21 H 1.0795 -0.2002 0.0147 0.025 Uiso 1 1 calc R . . C22 C 1.1158(3) -0.1298(2) 0.12427(17) 0.0171(5) Uani 1 1 d . . . H22 H 1.0188 -0.0723 0.1188 0.021 Uiso 1 1 calc R . . C23 C 1.3336(4) -0.3737(3) 0.0035(2) 0.0353(7) Uani 1 1 d . . . H23A H 1.3060 -0.4466 0.0370 0.053 Uiso 1 1 calc R . . H23B H 1.4478 -0.3883 -0.0143 0.053 Uiso 1 1 calc R . . H23C H 1.2725 -0.3409 -0.0550 0.053 Uiso 1 1 calc R . . C24 C 0.9412(3) 0.4396(2) 0.30734(17) 0.0165(5) Uani 1 1 d . . . C25 C 1.0088(3) 0.3726(2) 0.39302(18) 0.0216(5) Uani 1 1 d . . . H25 H 0.9758 0.3039 0.4245 0.026 Uiso 1 1 calc R . . C26 C 1.1247(3) 0.4069(2) 0.4319(2) 0.0250(5) Uani 1 1 d . . . H26 H 1.1707 0.3614 0.4904 0.030 Uiso 1 1 calc R . . C27 C 1.1750(3) 0.5073(2) 0.38648(19) 0.0228(5) Uani 1 1 d . . . C28 C 1.1044(3) 0.5732(2) 0.30175(19) 0.0245(5) Uani 1 1 d . . . H28 H 1.1364 0.6423 0.2705 0.029 Uiso 1 1 calc R . . C29 C 0.9881(3) 0.5402(2) 0.26172(19) 0.0223(5) Uani 1 1 d . . . H29 H 0.9410 0.5862 0.2036 0.027 Uiso 1 1 calc R . . C30 C 1.3036(3) 0.5431(3) 0.4286(2) 0.0326(6) Uani 1 1 d . . . H30A H 1.4074 0.5136 0.3985 0.049 Uiso 1 1 calc R . . H30B H 1.3051 0.5113 0.4986 0.049 Uiso 1 1 calc R . . H30C H 1.2816 0.6277 0.4162 0.049 Uiso 1 1 calc R . . N1 N 1.0441(2) 0.06574(16) 0.23385(14) 0.0147(4) Uani 1 1 d . . . N2 N 0.8785(2) 0.27139(17) 0.23390(14) 0.0155(4) Uani 1 1 d . . . O1 O 1.32337(19) -0.01947(15) 0.29176(12) 0.0177(3) Uani 1 1 d . . . O2 O 1.1036(2) -0.11140(14) 0.36357(12) 0.0178(3) Uani 1 1 d . . . O3 O 0.7338(2) 0.48249(14) 0.17601(12) 0.0190(3) Uani 1 1 d . . . O4 O 0.6756(2) 0.37173(15) 0.33839(13) 0.0202(4) Uani 1 1 d . . . Rh1 Rh 0.81880(2) 0.116585(15) 0.290069(12) 0.01249(6) Uani 1 1 d . . . S1 S 1.17645(6) -0.04884(5) 0.27907(4) 0.01342(11) Uani 1 1 d . . . S2 S 0.79036(7) 0.39531(5) 0.26070(4) 0.01511(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0157(11) 0.0160(11) 0.0153(11) 0.0018(9) 0.0044(9) -0.0075(9) C2 0.0157(11) 0.0178(11) 0.0169(11) -0.0013(9) 0.0030(9) -0.0079(9) C3 0.0130(10) 0.0220(12) 0.0171(11) -0.0017(9) 0.0019(9) -0.0078(9) C4 0.0141(11) 0.0193(12) 0.0170(11) -0.0004(9) 0.0032(9) -0.0063(9) C5 0.0146(10) 0.0175(11) 0.0148(11) -0.0002(9) 0.0042(8) -0.0068(9) C6 0.0248(12) 0.0207(12) 0.0145(11) 0.0003(9) 0.0012(9) -0.0056(10) C7 0.0229(12) 0.0184(12) 0.0212(12) -0.0056(10) 0.0031(10) -0.0072(10) C8 0.0189(12) 0.0311(14) 0.0184(12) -0.0041(10) -0.0010(9) -0.0076(10) C9 0.0176(12) 0.0259(13) 0.0216(13) -0.0015(10) -0.0019(10) -0.0014(10) C10 0.0213(12) 0.0245(13) 0.0163(11) -0.0026(10) 0.0041(9) -0.0066(10) C11 0.0135(10) 0.0135(11) 0.0143(10) -0.0002(8) -0.0003(8) -0.0042(8) C12 0.0139(10) 0.0152(11) 0.0125(10) -0.0012(8) 0.0011(8) -0.0040(8) C13 0.0188(11) 0.0132(11) 0.0191(12) 0.0011(9) 0.0010(9) -0.0027(9) C14 0.0198(12) 0.0179(12) 0.0174(11) 0.0047(9) 0.0006(9) -0.0068(9) C15 0.0145(11) 0.0224(12) 0.0164(11) -0.0003(9) 0.0050(9) -0.0039(9) C16 0.0167(11) 0.0155(11) 0.0160(11) -0.0001(9) -0.0005(9) -0.0016(9) C17 0.0157(10) 0.0124(10) 0.0140(10) 0.0007(8) 0.0006(8) -0.0039(8) C18 0.0170(11) 0.0168(11) 0.0191(12) 0.0008(9) -0.0036(9) -0.0024(9) C19 0.0170(11) 0.0163(12) 0.0263(13) -0.0024(10) 0.0026(10) -0.0018(9) C20 0.0232(12) 0.0191(12) 0.0214(12) -0.0051(10) 0.0035(10) -0.0044(10) C21 0.0216(12) 0.0222(12) 0.0178(12) -0.0042(10) -0.0024(9) -0.0045(10) C22 0.0146(11) 0.0162(11) 0.0182(11) -0.0006(9) -0.0016(9) -0.0017(9) C23 0.0367(16) 0.0325(16) 0.0404(18) -0.0213(14) 0.0004(13) -0.0028(13) C24 0.0176(11) 0.0144(11) 0.0161(11) -0.0024(9) 0.0033(9) -0.0033(9) C25 0.0247(13) 0.0163(12) 0.0211(12) 0.0021(9) -0.0014(10) -0.0054(10) C26 0.0249(13) 0.0240(13) 0.0236(13) -0.0016(10) -0.0050(10) -0.0029(10) C27 0.0198(12) 0.0247(13) 0.0252(13) -0.0102(11) 0.0037(10) -0.0048(10) C28 0.0303(14) 0.0206(13) 0.0242(13) -0.0034(10) 0.0041(11) -0.0125(11) C29 0.0272(13) 0.0205(12) 0.0181(12) -0.0009(10) 0.0006(10) -0.0070(10) C30 0.0286(15) 0.0422(17) 0.0326(16) -0.0140(13) -0.0017(12) -0.0127(13) N1 0.0155(9) 0.0121(9) 0.0139(9) 0.0016(7) 0.0010(7) -0.0034(7) N2 0.0138(9) 0.0135(9) 0.0171(10) -0.0013(8) 0.0028(7) -0.0022(7) O1 0.0161(8) 0.0215(9) 0.0153(8) -0.0017(7) -0.0017(6) -0.0058(7) O2 0.0201(8) 0.0176(8) 0.0131(8) 0.0020(6) 0.0003(6) -0.0049(7) O3 0.0195(8) 0.0145(8) 0.0189(8) 0.0005(7) -0.0022(7) 0.0002(7) O4 0.0191(8) 0.0188(9) 0.0207(9) -0.0036(7) 0.0067(7) -0.0045(7) Rh1 0.01193(9) 0.01269(9) 0.01148(9) 0.00034(6) 0.00121(6) -0.00383(6) S1 0.0139(3) 0.0131(3) 0.0116(2) 0.0002(2) -0.0007(2) -0.0029(2) S2 0.0148(3) 0.0120(3) 0.0160(3) -0.0007(2) 0.0018(2) -0.0014(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 C1 C2 1.419(3) . ? C1 C5 1.455(3) . ? C1 C6 1.489(3) . ? C1 Rh1 2.176(2) . ? C2 C3 1.438(3) . ? C2 C7 1.497(3) . ? C2 Rh1 2.180(2) . ? C3 C4 1.448(3) . ? C3 C8 1.490(3) . ? C3 Rh1 2.102(2) . ? C4 C5 1.424(3) . ? C4 C9 1.498(3) . ? C4 Rh1 2.172(2) . ? C5 C10 1.496(3) . ? C5 Rh1 2.189(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C16 1.392(3) . ? C11 C12 1.404(3) . ? C11 N1 1.421(3) . ? C12 C13 1.401(3) . ? C12 N2 1.422(3) . ? C13 C14 1.392(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.399(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.384(3) . ? C17 C18 1.394(3) . ? C17 S1 1.767(2) . ? C18 C19 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.392(4) . ? C19 H19 0.9500 . ? C20 C21 1.391(3) . ? C20 C23 1.504(4) . ? C21 C22 1.387(3) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.385(3) . ? C24 C25 1.392(3) . ? C24 S2 1.770(2) . ? C25 C26 1.384(4) . ? C25 H25 0.9500 . ? C26 C27 1.395(4) . ? C26 H26 0.9500 . ? C27 C28 1.387(4) . ? C27 C30 1.514(4) . ? C28 C29 1.388(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? N1 S1 1.619(2) . ? N1 Rh1 2.0403(19) . ? N2 S2 1.633(2) . ? N2 Rh1 2.0435(19) . ? O1 S1 1.4433(17) . ? O2 S1 1.4440(16) . ? O3 S2 1.4436(17) . ? O4 S2 1.4385(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 108.5(2) . . ? C2 C1 C6 127.0(2) . . ? C5 C1 C6 124.4(2) . . ? C2 C1 Rh1 71.12(13) . . ? C5 C1 Rh1 71.01(12) . . ? C6 C1 Rh1 126.31(16) . . ? C1 C2 C3 107.5(2) . . ? C1 C2 C7 126.8(2) . . ? C3 C2 C7 125.5(2) . . ? C1 C2 Rh1 70.86(13) . . ? C3 C2 Rh1 67.49(13) . . ? C7 C2 Rh1 130.91(16) . . ? C2 C3 C4 108.5(2) . . ? C2 C3 C8 124.5(2) . . ? C4 C3 C8 127.0(2) . . ? C2 C3 Rh1 73.32(13) . . ? C4 C3 Rh1 72.80(13) . . ? C8 C3 Rh1 121.59(16) . . ? C5 C4 C3 107.4(2) . . ? C5 C4 C9 127.3(2) . . ? C3 C4 C9 125.2(2) . . ? C5 C4 Rh1 71.61(13) . . ? C3 C4 Rh1 67.63(13) . . ? C9 C4 Rh1 128.40(17) . . ? C4 C5 C1 107.8(2) . . ? C4 C5 C10 128.2(2) . . ? C1 C5 C10 123.7(2) . . ? C4 C5 Rh1 70.28(13) . . ? C1 C5 Rh1 70.06(12) . . ? C10 C5 Rh1 129.07(16) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C16 C11 C12 120.5(2) . . ? C16 C11 N1 125.1(2) . . ? C12 C11 N1 114.35(19) . . ? C13 C12 C11 118.9(2) . . ? C13 C12 N2 127.1(2) . . ? C11 C12 N2 113.96(19) . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 120.0(2) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C22 C17 C18 120.2(2) . . ? C22 C17 S1 121.91(18) . . ? C18 C17 S1 117.85(18) . . ? C19 C18 C17 119.6(2) . . ? C19 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? C18 C19 C20 120.6(2) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 119.2(2) . . ? C21 C20 C23 120.9(2) . . ? C19 C20 C23 120.0(2) . . ? C22 C21 C20 120.5(2) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C17 C22 C21 119.9(2) . . ? C17 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 120.4(2) . . ? C29 C24 S2 121.14(19) . . ? C25 C24 S2 118.38(18) . . ? C26 C25 C24 119.3(2) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 121.2(2) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 118.4(2) . . ? C28 C27 C30 120.9(2) . . ? C26 C27 C30 120.8(3) . . ? C27 C28 C29 121.3(2) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C24 C29 C28 119.4(2) . . ? C24 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C11 N1 S1 117.99(15) . . ? C11 N1 Rh1 114.13(14) . . ? S1 N1 Rh1 126.12(11) . . ? C12 N2 S2 119.34(16) . . ? C12 N2 Rh1 114.53(15) . . ? S2 N2 Rh1 126.12(11) . . ? N1 Rh1 N2 77.95(8) . . ? N1 Rh1 C3 120.08(9) . . ? N2 Rh1 C3 128.59(9) . . ? N1 Rh1 C4 157.64(9) . . ? N2 Rh1 C4 107.50(8) . . ? C3 Rh1 C4 39.57(9) . . ? N1 Rh1 C1 120.87(8) . . ? N2 Rh1 C1 150.13(9) . . ? C3 Rh1 C1 65.13(9) . . ? C4 Rh1 C1 64.70(9) . . ? N1 Rh1 C2 105.02(8) . . ? N2 Rh1 C2 167.30(8) . . ? C3 Rh1 C2 39.19(9) . . ? C4 Rh1 C2 65.12(9) . . ? C1 Rh1 C2 38.02(9) . . ? N1 Rh1 C5 157.84(8) . . ? N2 Rh1 C5 116.75(8) . . ? C3 Rh1 C5 65.26(9) . . ? C4 Rh1 C5 38.11(9) . . ? C1 Rh1 C5 38.94(9) . . ? C2 Rh1 C5 64.54(9) . . ? O1 S1 O2 117.03(10) . . ? O1 S1 N1 110.86(10) . . ? O2 S1 N1 107.61(10) . . ? O1 S1 C17 106.39(10) . . ? O2 S1 C17 106.83(10) . . ? N1 S1 C17 107.70(11) . . ? O4 S2 O3 117.40(11) . . ? O4 S2 N2 106.70(10) . . ? O3 S2 N2 112.00(10) . . ? O4 S2 C24 107.69(11) . . ? O3 S2 C24 107.35(11) . . ? N2 S2 C24 104.93(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 3.8(2) . . . . ? C6 C1 C2 C3 -179.4(2) . . . . ? Rh1 C1 C2 C3 -57.71(15) . . . . ? C5 C1 C2 C7 -171.2(2) . . . . ? C6 C1 C2 C7 5.6(4) . . . . ? Rh1 C1 C2 C7 127.3(2) . . . . ? C5 C1 C2 Rh1 61.49(15) . . . . ? C6 C1 C2 Rh1 -121.7(2) . . . . ? C1 C2 C3 C4 -5.0(2) . . . . ? C7 C2 C3 C4 170.1(2) . . . . ? Rh1 C2 C3 C4 -64.80(15) . . . . ? C1 C2 C3 C8 177.1(2) . . . . ? C7 C2 C3 C8 -7.9(4) . . . . ? Rh1 C2 C3 C8 117.2(2) . . . . ? C1 C2 C3 Rh1 59.82(16) . . . . ? C7 C2 C3 Rh1 -125.1(2) . . . . ? C2 C3 C4 C5 4.3(2) . . . . ? C8 C3 C4 C5 -177.8(2) . . . . ? Rh1 C3 C4 C5 -60.87(16) . . . . ? C2 C3 C4 C9 -172.7(2) . . . . ? C8 C3 C4 C9 5.2(4) . . . . ? Rh1 C3 C4 C9 122.1(2) . . . . ? C2 C3 C4 Rh1 65.15(15) . . . . ? C8 C3 C4 Rh1 -117.0(2) . . . . ? C3 C4 C5 C1 -1.9(2) . . . . ? C9 C4 C5 C1 175.0(2) . . . . ? Rh1 C4 C5 C1 -60.27(15) . . . . ? C3 C4 C5 C10 -176.9(2) . . . . ? C9 C4 C5 C10 0.0(4) . . . . ? Rh1 C4 C5 C10 124.7(2) . . . . ? C3 C4 C5 Rh1 58.35(15) . . . . ? C9 C4 C5 Rh1 -124.7(2) . . . . ? C2 C1 C5 C4 -1.2(2) . . . . ? C6 C1 C5 C4 -178.0(2) . . . . ? Rh1 C1 C5 C4 60.40(15) . . . . ? C2 C1 C5 C10 174.1(2) . . . . ? C6 C1 C5 C10 -2.8(3) . . . . ? Rh1 C1 C5 C10 -124.3(2) . . . . ? C2 C1 C5 Rh1 -61.56(15) . . . . ? C6 C1 C5 Rh1 121.6(2) . . . . ? C16 C11 C12 C13 -3.7(3) . . . . ? N1 C11 C12 C13 179.4(2) . . . . ? C16 C11 C12 N2 174.3(2) . . . . ? N1 C11 C12 N2 -2.5(3) . . . . ? C11 C12 C13 C14 2.1(4) . . . . ? N2 C12 C13 C14 -175.6(2) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C13 C14 C15 C16 -2.2(4) . . . . ? C12 C11 C16 C15 2.4(4) . . . . ? N1 C11 C16 C15 178.9(2) . . . . ? C14 C15 C16 C11 0.6(4) . . . . ? C22 C17 C18 C19 -1.2(4) . . . . ? S1 C17 C18 C19 176.58(18) . . . . ? C17 C18 C19 C20 0.6(4) . . . . ? C18 C19 C20 C21 0.2(4) . . . . ? C18 C19 C20 C23 -179.1(2) . . . . ? C19 C20 C21 C22 -0.3(4) . . . . ? C23 C20 C21 C22 179.0(2) . . . . ? C18 C17 C22 C21 1.1(3) . . . . ? S1 C17 C22 C21 -176.59(18) . . . . ? C20 C21 C22 C17 -0.4(4) . . . . ? C29 C24 C25 C26 -0.6(4) . . . . ? S2 C24 C25 C26 -178.6(2) . . . . ? C24 C25 C26 C27 -0.2(4) . . . . ? C25 C26 C27 C28 0.9(4) . . . . ? C25 C26 C27 C30 -179.0(3) . . . . ? C26 C27 C28 C29 -0.8(4) . . . . ? C30 C27 C28 C29 179.0(3) . . . . ? C25 C24 C29 C28 0.6(4) . . . . ? S2 C24 C29 C28 178.6(2) . . . . ? C27 C28 C29 C24 0.1(4) . . . . ? C16 C11 N1 S1 35.8(3) . . . . ? C12 C11 N1 S1 -147.53(17) . . . . ? C16 C11 N1 Rh1 -158.39(19) . . . . ? C12 C11 N1 Rh1 18.3(2) . . . . ? C13 C12 N2 S2 -15.6(3) . . . . ? C11 C12 N2 S2 166.53(16) . . . . ? C13 C12 N2 Rh1 163.5(2) . . . . ? C11 C12 N2 Rh1 -14.4(2) . . . . ? C11 N1 Rh1 N2 -19.89(16) . . . . ? S1 N1 Rh1 N2 144.56(15) . . . . ? C11 N1 Rh1 C3 107.94(17) . . . . ? S1 N1 Rh1 C3 -87.60(15) . . . . ? C11 N1 Rh1 C4 86.9(3) . . . . ? S1 N1 Rh1 C4 -108.6(2) . . . . ? C11 N1 Rh1 C1 -174.77(15) . . . . ? S1 N1 Rh1 C1 -10.32(18) . . . . ? C11 N1 Rh1 C2 147.41(16) . . . . ? S1 N1 Rh1 C2 -48.14(15) . . . . ? C11 N1 Rh1 C5 -154.0(2) . . . . ? S1 N1 Rh1 C5 10.5(3) . . . . ? C12 N2 Rh1 N1 18.60(16) . . . . ? S2 N2 Rh1 N1 -162.36(15) . . . . ? C12 N2 Rh1 C3 -100.43(17) . . . . ? S2 N2 Rh1 C3 78.60(17) . . . . ? C12 N2 Rh1 C4 -138.95(16) . . . . ? S2 N2 Rh1 C4 40.08(16) . . . . ? C12 N2 Rh1 C1 151.58(17) . . . . ? S2 N2 Rh1 C1 -29.4(3) . . . . ? C12 N2 Rh1 C2 -86.4(4) . . . . ? S2 N2 Rh1 C2 92.7(4) . . . . ? C12 N2 Rh1 C5 -179.05(15) . . . . ? S2 N2 Rh1 C5 -0.02(17) . . . . ? C2 C3 Rh1 N1 76.31(15) . . . . ? C4 C3 Rh1 N1 -167.63(12) . . . . ? C8 C3 Rh1 N1 -44.3(2) . . . . ? C2 C3 Rh1 N2 175.15(12) . . . . ? C4 C3 Rh1 N2 -68.80(16) . . . . ? C8 C3 Rh1 N2 54.5(2) . . . . ? C2 C3 Rh1 C4 -116.06(19) . . . . ? C8 C3 Rh1 C4 123.3(3) . . . . ? C2 C3 Rh1 C1 -36.33(13) . . . . ? C4 C3 Rh1 C1 79.73(14) . . . . ? C8 C3 Rh1 C1 -157.0(2) . . . . ? C4 C3 Rh1 C2 116.06(19) . . . . ? C8 C3 Rh1 C2 -120.6(3) . . . . ? C2 C3 Rh1 C5 -79.41(14) . . . . ? C4 C3 Rh1 C5 36.64(13) . . . . ? C8 C3 Rh1 C5 160.0(2) . . . . ? C5 C4 Rh1 N1 147.72(19) . . . . ? C3 C4 Rh1 N1 29.2(3) . . . . ? C9 C4 Rh1 N1 -88.8(3) . . . . ? C5 C4 Rh1 N2 -111.26(14) . . . . ? C3 C4 Rh1 N2 130.17(13) . . . . ? C9 C4 Rh1 N2 12.2(2) . . . . ? C5 C4 Rh1 C3 118.56(19) . . . . ? C9 C4 Rh1 C3 -118.0(3) . . . . ? C5 C4 Rh1 C1 37.68(13) . . . . ? C3 C4 Rh1 C1 -80.89(14) . . . . ? C9 C4 Rh1 C1 161.2(2) . . . . ? C5 C4 Rh1 C2 79.83(14) . . . . ? C3 C4 Rh1 C2 -38.73(13) . . . . ? C9 C4 Rh1 C2 -156.7(2) . . . . ? C3 C4 Rh1 C5 -118.56(19) . . . . ? C9 C4 Rh1 C5 123.5(3) . . . . ? C2 C1 Rh1 N1 -74.07(16) . . . . ? C5 C1 Rh1 N1 167.71(13) . . . . ? C6 C1 Rh1 N1 48.5(2) . . . . ? C2 C1 Rh1 N2 162.40(15) . . . . ? C5 C1 Rh1 N2 44.2(2) . . . . ? C6 C1 Rh1 N2 -75.1(3) . . . . ? C2 C1 Rh1 C3 37.43(14) . . . . ? C5 C1 Rh1 C3 -80.78(15) . . . . ? C6 C1 Rh1 C3 160.0(2) . . . . ? C2 C1 Rh1 C4 81.32(15) . . . . ? C5 C1 Rh1 C4 -36.89(13) . . . . ? C6 C1 Rh1 C4 -156.1(2) . . . . ? C5 C1 Rh1 C2 -118.2(2) . . . . ? C6 C1 Rh1 C2 122.5(3) . . . . ? C2 C1 Rh1 C5 118.2(2) . . . . ? C6 C1 Rh1 C5 -119.3(3) . . . . ? C1 C2 Rh1 N1 121.28(14) . . . . ? C3 C2 Rh1 N1 -119.49(14) . . . . ? C7 C2 Rh1 N1 -1.3(2) . . . . ? C1 C2 Rh1 N2 -136.7(3) . . . . ? C3 C2 Rh1 N2 -17.5(4) . . . . ? C7 C2 Rh1 N2 100.7(4) . . . . ? C1 C2 Rh1 C3 -119.2(2) . . . . ? C7 C2 Rh1 C3 118.2(3) . . . . ? C1 C2 Rh1 C4 -80.12(15) . . . . ? C3 C2 Rh1 C4 39.11(14) . . . . ? C7 C2 Rh1 C4 157.3(3) . . . . ? C3 C2 Rh1 C1 119.2(2) . . . . ? C7 C2 Rh1 C1 -122.6(3) . . . . ? C1 C2 Rh1 C5 -37.83(13) . . . . ? C3 C2 Rh1 C5 81.40(15) . . . . ? C7 C2 Rh1 C5 -160.4(3) . . . . ? C4 C5 Rh1 N1 -147.4(2) . . . . ? C1 C5 Rh1 N1 -29.0(3) . . . . ? C10 C5 Rh1 N1 88.8(3) . . . . ? C4 C5 Rh1 N2 84.44(15) . . . . ? C1 C5 Rh1 N2 -157.12(13) . . . . ? C10 C5 Rh1 N2 -39.3(2) . . . . ? C4 C5 Rh1 C3 -38.03(14) . . . . ? C1 C5 Rh1 C3 80.41(15) . . . . ? C10 C5 Rh1 C3 -161.8(2) . . . . ? C1 C5 Rh1 C4 118.4(2) . . . . ? C10 C5 Rh1 C4 -123.8(3) . . . . ? C4 C5 Rh1 C1 -118.4(2) . . . . ? C10 C5 Rh1 C1 117.8(3) . . . . ? C4 C5 Rh1 C2 -81.49(15) . . . . ? C1 C5 Rh1 C2 36.95(13) . . . . ? C10 C5 Rh1 C2 154.7(2) . . . . ? C11 N1 S1 O1 37.6(2) . . . . ? Rh1 N1 S1 O1 -126.31(13) . . . . ? C11 N1 S1 O2 166.74(17) . . . . ? Rh1 N1 S1 O2 2.82(16) . . . . ? C11 N1 S1 C17 -78.41(19) . . . . ? Rh1 N1 S1 C17 117.67(14) . . . . ? C22 C17 S1 O1 -141.69(19) . . . . ? C18 C17 S1 O1 40.6(2) . . . . ? C22 C17 S1 O2 92.6(2) . . . . ? C18 C17 S1 O2 -85.15(19) . . . . ? C22 C17 S1 N1 -22.8(2) . . . . ? C18 C17 S1 N1 159.49(18) . . . . ? C12 N2 S2 O4 -174.84(17) . . . . ? Rh1 N2 S2 O4 6.16(17) . . . . ? C12 N2 S2 O3 55.4(2) . . . . ? Rh1 N2 S2 O3 -123.59(13) . . . . ? C12 N2 S2 C24 -60.7(2) . . . . ? Rh1 N2 S2 C24 120.27(14) . . . . ? C29 C24 S2 O4 -129.0(2) . . . . ? C25 C24 S2 O4 49.1(2) . . . . ? C29 C24 S2 O3 -1.7(2) . . . . ? C25 C24 S2 O3 176.35(19) . . . . ? C29 C24 S2 N2 117.6(2) . . . . ? C25 C24 S2 N2 -64.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.186 _refine_diff_density_min -1.271 _refine_diff_density_rms 0.100 # Attachment 'rnp0832a_Rh_C5Me5__HNC6H4NH__rev.cif' data_rnp0832a _database_code_depnum_ccdc_archive 'CCDC 729049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H21 N2 Rh' _chemical_formula_sum 'C16 H21 N2 Rh' _chemical_formula_weight 344.26 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _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 20.8896(6) _cell_length_b 13.4599(4) _cell_length_c 21.1659(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.4840(10) _cell_angle_gamma 90.00 _cell_volume 5924.0(3) _cell_formula_units_Z 16 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8108 _cell_measurement_theta_min 2.249 _cell_measurement_theta_max 30.046 _exptl_crystal_description Shard _exptl_crystal_colour Purple _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66450 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 30.11 _reflns_number_total 17170 _reflns_number_gt 13425 _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, 1997)' _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. The additional symmetry reported by checkcif (ADDSYM) was investigated and found to be inexact with the position of one pair of the Cp* differing after transformation. This was checked further by use of the higher symmetry cell (with half the cell volume) which showed disorder of one of the Cp* in the asymmetric unit. Since this is not random disorder but a sytematic alternation of position of the Cp*, the structure was solved using the larger unit cell with 4 molecules in the asymmetric unit. ; _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^+5.1310P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17169 _refine_ls_number_parameters 737 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0790 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 C1 C 0.49010(11) -0.11792(17) 0.21178(11) 0.0256(5) Uani 1 1 d . . . C2 C 0.44430(11) -0.04265(17) 0.19546(11) 0.0254(5) Uani 1 1 d . . . C3 C 0.42245(10) -0.00425(17) 0.25296(11) 0.0239(4) Uani 1 1 d . . . C4 C 0.45523(11) -0.05766(17) 0.30501(10) 0.0233(4) Uani 1 1 d . . . C5 C 0.49668(11) -0.12805(16) 0.27965(11) 0.0242(4) Uani 1 1 d . . . C6 C 0.52388(15) -0.1802(2) 0.16654(16) 0.0516(9) Uani 1 1 d . . . H6A H 0.4991 -0.2410 0.1566 0.077 Uiso 1 1 calc R . . H6B H 0.5668 -0.1977 0.1860 0.077 Uiso 1 1 calc R . . H6C H 0.5278 -0.1426 0.1274 0.077 Uiso 1 1 calc R . . C7 C 0.42035(15) -0.0116(2) 0.12928(12) 0.0447(7) Uani 1 1 d . . . H7A H 0.4522 -0.0296 0.1001 0.067 Uiso 1 1 calc R . . H7B H 0.4136 0.0605 0.1281 0.067 Uiso 1 1 calc R . . H7C H 0.3796 -0.0453 0.1164 0.067 Uiso 1 1 calc R . . C8 C 0.37008(12) 0.0710(2) 0.25664(16) 0.0434(7) Uani 1 1 d . . . H8A H 0.3285 0.0370 0.2551 0.065 Uiso 1 1 calc R . . H8B H 0.3700 0.1169 0.2207 0.065 Uiso 1 1 calc R . . H8C H 0.3775 0.1081 0.2965 0.065 Uiso 1 1 calc R . . C9 C 0.44377(15) -0.0455(2) 0.37302(12) 0.0420(7) Uani 1 1 d . . . H9A H 0.4093 -0.0903 0.3832 0.063 Uiso 1 1 calc R . . H9B H 0.4313 0.0233 0.3807 0.063 Uiso 1 1 calc R . . H9C H 0.4832 -0.0614 0.3999 0.063 Uiso 1 1 calc R . . C10 C 0.53620(13) -0.20465(19) 0.31694(15) 0.0413(7) Uani 1 1 d . . . H10A H 0.5438 -0.1832 0.3613 0.062 Uiso 1 1 calc R . . H10B H 0.5775 -0.2127 0.2991 0.062 Uiso 1 1 calc R . . H10C H 0.5131 -0.2682 0.3149 0.062 Uiso 1 1 calc R . . C11 C 0.62321(10) 0.15836(15) 0.22347(10) 0.0189(4) Uani 1 1 d . . . C12 C 0.66668(11) 0.21584(17) 0.19171(11) 0.0249(4) Uani 1 1 d . . . H12 H 0.6712 0.2045 0.1481 0.030 Uiso 1 1 calc R . . C13 C 0.70272(11) 0.28888(17) 0.22464(11) 0.0271(5) Uani 1 1 d . . . H13 H 0.7320 0.3277 0.2034 0.033 Uiso 1 1 calc R . . C14 C 0.69639(11) 0.30598(17) 0.28908(11) 0.0266(5) Uani 1 1 d . . . H14 H 0.7215 0.3563 0.3110 0.032 Uiso 1 1 calc R . . C15 C 0.65407(11) 0.25044(16) 0.32124(11) 0.0239(4) Uani 1 1 d . . . H15 H 0.6503 0.2624 0.3650 0.029 Uiso 1 1 calc R . . N1 N 0.58380(9) 0.08547(14) 0.19782(9) 0.0214(4) Uani 1 1 d . . . N2 N 0.57231(9) 0.11541(14) 0.31257(9) 0.0215(4) Uani 1 1 d . . . Rh1 Rh 0.524821(8) 0.021541(11) 0.253025(7) 0.01661(4) Uani 1 1 d . . . C16 C 0.61670(10) 0.17606(15) 0.28868(10) 0.0195(4) Uani 1 1 d . . . C17 C 0.28669(11) 0.38352(16) 0.43396(11) 0.0244(4) Uani 1 1 d . . . C18 C 0.25011(12) 0.45381(18) 0.39525(11) 0.0290(5) Uani 1 1 d . . . C19 C 0.21097(11) 0.50847(18) 0.43727(14) 0.0355(6) Uani 1 1 d . . . C20 C 0.22594(13) 0.4719(2) 0.49990(13) 0.0368(6) Uani 1 1 d . . . C21 C 0.27266(12) 0.39524(19) 0.49771(11) 0.0310(5) Uani 1 1 d . . . C22 C 0.33028(14) 0.3083(2) 0.40802(16) 0.0474(7) Uani 1 1 d . . . H22A H 0.3667 0.2948 0.4396 0.071 Uiso 1 1 calc R . . H22B H 0.3463 0.3343 0.3692 0.071 Uiso 1 1 calc R . . H22C H 0.3064 0.2467 0.3983 0.071 Uiso 1 1 calc R . . C23 C 0.24838(17) 0.4683(2) 0.32604(13) 0.0505(8) Uani 1 1 d . . . H23A H 0.2901 0.4500 0.3118 0.076 Uiso 1 1 calc R . . H23B H 0.2392 0.5382 0.3158 0.076 Uiso 1 1 calc R . . H23C H 0.2147 0.4264 0.3045 0.076 Uiso 1 1 calc R . . C24 C 0.16159(15) 0.5837(2) 0.4146(2) 0.0652(11) Uani 1 1 d . . . H24A H 0.1234 0.5498 0.3946 0.098 Uiso 1 1 calc R . . H24B H 0.1792 0.6276 0.3836 0.098 Uiso 1 1 calc R . . H24C H 0.1498 0.6230 0.4507 0.098 Uiso 1 1 calc R . . C25 C 0.19579(17) 0.5009(3) 0.55846(16) 0.0595(10) Uani 1 1 d . . . H25A H 0.1696 0.5606 0.5500 0.089 Uiso 1 1 calc R . . H25B H 0.2295 0.5144 0.5928 0.089 Uiso 1 1 calc R . . H25C H 0.1685 0.4465 0.5710 0.089 Uiso 1 1 calc R . . C26 C 0.30089(16) 0.3346(2) 0.55366(13) 0.0499(8) Uani 1 1 d . . . H26A H 0.3058 0.3767 0.5916 0.075 Uiso 1 1 calc R . . H26B H 0.3430 0.3088 0.5449 0.075 Uiso 1 1 calc R . . H26C H 0.2721 0.2791 0.5608 0.075 Uiso 1 1 calc R . . C27 C 0.43099(10) 0.64059(15) 0.47910(9) 0.0187(4) Uani 1 1 d . . . C28 C 0.49525(10) 0.67091(17) 0.47830(10) 0.0233(4) Uani 1 1 d . . . H28 H 0.5262 0.6267 0.4638 0.028 Uiso 1 1 calc R . . C29 C 0.51341(11) 0.76559(17) 0.49873(11) 0.0256(5) Uani 1 1 d . . . H29 H 0.5569 0.7859 0.4977 0.031 Uiso 1 1 calc R . . C30 C 0.46896(11) 0.83151(17) 0.52074(10) 0.0243(4) Uani 1 1 d . . . H30 H 0.4823 0.8960 0.5348 0.029 Uiso 1 1 calc R . . N3 N 0.40482(9) 0.55145(14) 0.46031(8) 0.0201(3) Uani 1 1 d . . . N4 N 0.32517(9) 0.66904(14) 0.49973(9) 0.0220(4) Uani 1 1 d . . . Rh2 Rh 0.311479(8) 0.533069(12) 0.466726(8) 0.01882(4) Uani 1 1 d . . . C31 C 0.40531(11) 0.80288(16) 0.52211(10) 0.0225(4) Uani 1 1 d . . . H31 H 0.3751 0.8477 0.5371 0.027 Uiso 1 1 calc R . . C32 C 0.38564(10) 0.70769(16) 0.50136(9) 0.0194(4) Uani 1 1 d . . . C33 C -0.03813(10) 0.55653(16) 0.30155(10) 0.0210(4) Uani 1 1 d . . . C34 C -0.07607(11) 0.49739(17) 0.25621(11) 0.0255(4) Uani 1 1 d . . . C35 C -0.05943(11) 0.52491(17) 0.19388(11) 0.0267(5) Uani 1 1 d . . . C36 C -0.01169(11) 0.60005(17) 0.20128(11) 0.0251(5) Uani 1 1 d . . . C37 C 0.00128(10) 0.62026(15) 0.26785(11) 0.0221(4) Uani 1 1 d . . . C38 C -0.04198(13) 0.5575(2) 0.37142(11) 0.0333(5) Uani 1 1 d . . . H38A H -0.0701 0.6118 0.3824 0.050 Uiso 1 1 calc R . . H38B H 0.0011 0.5671 0.3932 0.050 Uiso 1 1 calc R . . H38C H -0.0595 0.4941 0.3846 0.050 Uiso 1 1 calc R . . C39 C -0.12758(12) 0.4262(2) 0.26987(16) 0.0423(7) Uani 1 1 d . . . H39A H -0.1157 0.3935 0.3107 0.063 Uiso 1 1 calc R . . H39B H -0.1327 0.3760 0.2362 0.063 Uiso 1 1 calc R . . H39C H -0.1682 0.4621 0.2717 0.063 Uiso 1 1 calc R . . C40 C -0.09024(14) 0.4868(2) 0.13200(13) 0.0452(7) Uani 1 1 d . . . H40A H -0.1314 0.5207 0.1215 0.068 Uiso 1 1 calc R . . H40B H -0.0976 0.4151 0.1353 0.068 Uiso 1 1 calc R . . H40C H -0.0619 0.4995 0.0986 0.068 Uiso 1 1 calc R . . C41 C 0.01736(14) 0.6543(2) 0.14910(13) 0.0400(7) Uani 1 1 d . . . H41A H 0.0307 0.6064 0.1181 0.060 Uiso 1 1 calc R . . H41B H 0.0549 0.6921 0.1670 0.060 Uiso 1 1 calc R . . H41C H -0.0145 0.7000 0.1282 0.060 Uiso 1 1 calc R . . C42 C 0.04530(12) 0.69951(17) 0.29625(13) 0.0349(6) Uani 1 1 d . . . H42A H 0.0244 0.7644 0.2900 0.052 Uiso 1 1 calc R . . H42B H 0.0853 0.6990 0.2755 0.052 Uiso 1 1 calc R . . H42C H 0.0550 0.6869 0.3418 0.052 Uiso 1 1 calc R . . C43 C 0.11435(10) 0.30835(15) 0.28471(10) 0.0187(4) Uani 1 1 d . . . C44 C 0.15220(10) 0.23472(16) 0.31765(10) 0.0231(4) Uani 1 1 d . . . H44 H 0.1480 0.2226 0.3613 0.028 Uiso 1 1 calc R . . C45 C 0.19546(11) 0.18023(17) 0.28623(11) 0.0267(5) Uani 1 1 d . . . H45 H 0.2212 0.1311 0.3086 0.032 Uiso 1 1 calc R . . N5 N 0.07035(9) 0.36970(13) 0.30809(9) 0.0206(4) Uani 1 1 d . . . N6 N 0.08235(9) 0.39862(14) 0.19345(9) 0.0210(4) Uani 1 1 d . . . Rh3 Rh 0.024648(8) 0.465558(11) 0.248494(7) 0.01676(4) Uani 1 1 d . . . C46 C 0.20183(11) 0.19657(17) 0.22175(12) 0.0280(5) Uani 1 1 d . . . H46 H 0.2318 0.1583 0.2010 0.034 Uiso 1 1 calc R . . C47 C 0.16511(11) 0.26777(17) 0.18794(11) 0.0245(4) Uani 1 1 d . . . H47 H 0.1694 0.2781 0.1441 0.029 Uiso 1 1 calc R . . C48 C 0.12110(10) 0.32498(15) 0.21925(10) 0.0182(4) Uani 1 1 d . . . C49 C 0.23002(11) 0.56496(18) 0.10814(11) 0.0279(5) Uani 1 1 d . . . C50 C 0.21434(11) 0.61663(17) 0.04995(12) 0.0261(5) Uani 1 1 d . . . C51 C 0.25210(12) 0.57459(18) 0.00270(11) 0.0283(5) Uani 1 1 d . . . C52 C 0.29107(11) 0.49725(18) 0.03377(13) 0.0298(5) Uani 1 1 d . . . C53 C 0.27691(11) 0.49139(18) 0.09776(12) 0.0302(5) Uani 1 1 d . . . C54 C 0.20350(14) 0.5866(2) 0.17021(12) 0.0410(6) Uani 1 1 d . . . H54A H 0.1885 0.5246 0.1882 0.062 Uiso 1 1 calc R . . H54B H 0.1675 0.6331 0.1632 0.062 Uiso 1 1 calc R . . H54C H 0.2372 0.6160 0.1997 0.062 Uiso 1 1 calc R . . C55 C 0.16856(13) 0.70190(19) 0.03950(15) 0.0410(6) Uani 1 1 d . . . H55A H 0.1327 0.6928 0.0655 0.062 Uiso 1 1 calc R . . H55B H 0.1521 0.7047 -0.0054 0.062 Uiso 1 1 calc R . . H55C H 0.1910 0.7640 0.0515 0.062 Uiso 1 1 calc R . . C56 C 0.25386(15) 0.6076(2) -0.06445(12) 0.0426(7) Uani 1 1 d . . . H56A H 0.2893 0.6546 -0.0671 0.064 Uiso 1 1 calc R . . H56B H 0.2131 0.6399 -0.0791 0.064 Uiso 1 1 calc R . . H56C H 0.2603 0.5498 -0.0913 0.064 Uiso 1 1 calc R . . C57 C 0.34006(14) 0.4367(2) 0.00386(18) 0.0510(8) Uani 1 1 d . . . H57A H 0.3815 0.4715 0.0082 0.076 Uiso 1 1 calc R . . H57B H 0.3261 0.4269 -0.0412 0.076 Uiso 1 1 calc R . . H57C H 0.3447 0.3720 0.0250 0.076 Uiso 1 1 calc R . . C58 C 0.30748(14) 0.4236(2) 0.14856(15) 0.0482(8) Uani 1 1 d . . . H58A H 0.3267 0.3665 0.1288 0.072 Uiso 1 1 calc R . . H58B H 0.2747 0.4004 0.1753 0.072 Uiso 1 1 calc R . . H58C H 0.3410 0.4599 0.1747 0.072 Uiso 1 1 calc R . . C59 C 0.07190(10) 0.35133(15) 0.01972(9) 0.0188(4) Uani 1 1 d . . . C60 C 0.00852(10) 0.31662(17) 0.02174(10) 0.0235(4) Uani 1 1 d . . . H60 H -0.0229 0.3582 0.0378 0.028 Uiso 1 1 calc R . . C61 C -0.00797(11) 0.22189(17) 0.00037(11) 0.0253(4) Uani 1 1 d . . . H61 H -0.0508 0.1989 0.0021 0.030 Uiso 1 1 calc R . . C62 C 0.03734(11) 0.15992(17) -0.02360(10) 0.0244(4) Uani 1 1 d . . . H62 H 0.0253 0.0951 -0.0379 0.029 Uiso 1 1 calc R . . C63 C 0.09997(11) 0.19245(16) -0.02667(10) 0.0229(4) Uani 1 1 d . . . H63 H 0.1306 0.1503 -0.0436 0.027 Uiso 1 1 calc R . . C64 C 0.11804(10) 0.28755(16) -0.00479(9) 0.0195(4) Uani 1 1 d . . . N7 N 0.09690(9) 0.44032(14) 0.04002(8) 0.0207(3) Uani 1 1 d . . . N8 N 0.17769(9) 0.32925(14) -0.00335(9) 0.0228(4) Uani 1 1 d . . . Rh4 Rh 0.190325(8) 0.461655(12) 0.035700(8) 0.01863(4) Uani 1 1 d . . . H3 H 0.4329(13) 0.509(2) 0.4484(12) 0.023(7) Uiso 1 1 d . . . H7 H 0.0674(13) 0.4781(19) 0.0513(12) 0.023(7) Uiso 1 1 d . . . H6 H 0.0862(15) 0.409(2) 0.1584(14) 0.042(9) Uiso 1 1 d . . . H5 H 0.0648(13) 0.360(2) 0.3450(13) 0.029(7) Uiso 1 1 d . . . H1 H 0.5856(14) 0.071(2) 0.1643(13) 0.030(8) Uiso 1 1 d . . . H2 H 0.5661(13) 0.126(2) 0.3523(13) 0.034(8) Uiso 1 1 d . . . H8 H 0.2060(14) 0.291(2) -0.0196(14) 0.041(8) Uiso 1 1 d . . . H4 H 0.2931(15) 0.709(2) 0.5115(14) 0.047(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0242(11) 0.0264(11) 0.0269(11) -0.0077(9) 0.0066(9) -0.0091(9) C2 0.0243(11) 0.0294(11) 0.0214(10) 0.0042(8) -0.0033(8) -0.0114(9) C3 0.0167(10) 0.0200(10) 0.0351(12) 0.0008(9) 0.0030(9) -0.0013(8) C4 0.0262(11) 0.0248(11) 0.0194(10) -0.0008(8) 0.0043(8) -0.0075(9) C5 0.0203(11) 0.0201(10) 0.0315(12) 0.0016(8) -0.0017(9) -0.0040(8) C6 0.0477(17) 0.0426(16) 0.069(2) -0.0356(15) 0.0302(16) -0.0189(13) C7 0.0482(17) 0.0573(18) 0.0255(13) 0.0117(12) -0.0128(11) -0.0221(14) C8 0.0234(13) 0.0317(14) 0.075(2) 0.0017(13) 0.0065(13) 0.0020(10) C9 0.0535(18) 0.0503(17) 0.0238(12) -0.0050(11) 0.0119(12) -0.0207(14) C10 0.0341(14) 0.0229(12) 0.0640(19) 0.0126(12) -0.0099(13) -0.0022(10) C11 0.0179(10) 0.0194(9) 0.0196(9) -0.0006(7) 0.0034(7) -0.0006(7) C12 0.0249(11) 0.0275(11) 0.0229(10) 0.0011(8) 0.0051(9) -0.0037(9) C13 0.0252(12) 0.0255(11) 0.0309(12) 0.0029(9) 0.0041(9) -0.0055(9) C14 0.0245(11) 0.0212(10) 0.0337(12) -0.0025(9) 0.0002(9) -0.0048(8) C15 0.0237(11) 0.0234(10) 0.0244(10) -0.0037(8) 0.0011(8) -0.0018(8) N1 0.0239(9) 0.0239(9) 0.0167(8) -0.0030(7) 0.0031(7) -0.0036(7) N2 0.0235(9) 0.0254(9) 0.0160(8) -0.0030(7) 0.0033(7) -0.0047(7) Rh1 0.01640(8) 0.01775(8) 0.01558(8) -0.00054(5) 0.00094(6) -0.00149(5) C16 0.0192(10) 0.0192(9) 0.0201(10) -0.0004(7) 0.0014(8) -0.0009(7) C17 0.0206(11) 0.0218(10) 0.0303(11) 0.0007(8) 0.0008(9) -0.0041(8) C18 0.0320(13) 0.0281(11) 0.0246(11) 0.0029(9) -0.0090(9) -0.0130(10) C19 0.0163(11) 0.0227(11) 0.0651(18) -0.0041(11) -0.0077(11) -0.0030(9) C20 0.0331(14) 0.0382(15) 0.0410(15) -0.0111(11) 0.0131(12) -0.0166(11) C21 0.0382(14) 0.0295(12) 0.0251(11) 0.0019(9) 0.0014(10) -0.0152(10) C22 0.0313(15) 0.0420(16) 0.069(2) -0.0171(15) 0.0059(14) 0.0025(12) C23 0.068(2) 0.0534(18) 0.0272(13) 0.0082(12) -0.0093(13) -0.0295(16) C24 0.0360(17) 0.0323(15) 0.121(3) -0.0085(18) -0.0279(18) 0.0029(12) C25 0.060(2) 0.059(2) 0.066(2) -0.0273(17) 0.0388(18) -0.0289(17) C26 0.071(2) 0.0410(16) 0.0337(14) 0.0122(12) -0.0135(14) -0.0245(15) C27 0.0184(10) 0.0218(10) 0.0156(9) 0.0025(7) -0.0001(7) -0.0019(7) C28 0.0195(10) 0.0267(11) 0.0239(10) 0.0028(8) 0.0040(8) -0.0014(8) C29 0.0197(11) 0.0302(12) 0.0262(11) 0.0058(9) -0.0007(9) -0.0069(8) C30 0.0265(11) 0.0227(10) 0.0226(10) 0.0028(8) -0.0045(8) -0.0072(8) N3 0.0178(9) 0.0220(9) 0.0208(8) 0.0004(7) 0.0028(7) -0.0007(7) N4 0.0173(9) 0.0239(9) 0.0247(9) -0.0022(7) 0.0013(7) -0.0018(7) Rh2 0.01648(8) 0.02117(8) 0.01860(8) 0.00059(6) 0.00067(6) -0.00357(6) C31 0.0238(11) 0.0224(10) 0.0208(10) 0.0000(8) -0.0006(8) -0.0012(8) C32 0.0174(10) 0.0229(10) 0.0177(9) 0.0011(7) 0.0005(7) -0.0026(8) C33 0.0214(10) 0.0207(10) 0.0210(10) 0.0006(8) 0.0030(8) 0.0045(8) C34 0.0190(10) 0.0237(11) 0.0338(12) -0.0051(9) 0.0021(9) 0.0019(8) C35 0.0245(11) 0.0306(12) 0.0234(11) -0.0064(9) -0.0059(9) 0.0118(9) C36 0.0244(11) 0.0260(11) 0.0253(11) 0.0060(8) 0.0040(9) 0.0102(9) C37 0.0201(10) 0.0173(9) 0.0280(11) 0.0034(8) -0.0015(8) 0.0041(8) C38 0.0406(14) 0.0385(14) 0.0218(11) 0.0018(10) 0.0074(10) 0.0127(11) C39 0.0240(13) 0.0302(13) 0.074(2) -0.0045(13) 0.0101(13) -0.0037(10) C40 0.0444(16) 0.0519(17) 0.0354(14) -0.0187(12) -0.0169(12) 0.0217(14) C41 0.0461(16) 0.0416(15) 0.0349(14) 0.0174(11) 0.0169(12) 0.0183(12) C42 0.0318(13) 0.0195(11) 0.0513(16) 0.0017(10) -0.0059(11) -0.0008(9) C43 0.0179(10) 0.0177(9) 0.0205(9) 0.0014(7) 0.0021(8) -0.0007(7) C44 0.0230(11) 0.0227(10) 0.0233(10) 0.0047(8) 0.0005(8) 0.0006(8) C45 0.0236(11) 0.0236(11) 0.0323(12) 0.0046(9) 0.0000(9) 0.0052(9) N5 0.0236(9) 0.0226(9) 0.0159(8) 0.0021(7) 0.0037(7) 0.0037(7) N6 0.0229(9) 0.0239(9) 0.0165(8) 0.0034(7) 0.0029(7) 0.0043(7) Rh3 0.01651(8) 0.01773(8) 0.01591(8) 0.00054(5) 0.00086(6) 0.00202(5) C46 0.0225(11) 0.0256(11) 0.0364(13) -0.0021(9) 0.0062(9) 0.0057(9) C47 0.0231(11) 0.0266(11) 0.0244(11) 0.0004(8) 0.0058(8) 0.0037(8) C48 0.0176(9) 0.0171(9) 0.0198(9) 0.0003(7) 0.0012(7) 0.0002(7) C49 0.0287(12) 0.0288(12) 0.0255(11) -0.0012(9) -0.0014(9) -0.0098(9) C50 0.0219(11) 0.0208(10) 0.0356(12) 0.0031(9) 0.0028(9) -0.0014(8) C51 0.0276(12) 0.0284(12) 0.0290(12) 0.0029(9) 0.0033(9) -0.0082(9) C52 0.0192(11) 0.0215(11) 0.0492(15) -0.0050(10) 0.0057(10) -0.0031(9) C53 0.0237(11) 0.0244(11) 0.0398(13) 0.0049(10) -0.0104(10) -0.0068(9) C54 0.0463(16) 0.0476(16) 0.0300(13) -0.0049(11) 0.0076(12) -0.0174(13) C55 0.0325(14) 0.0264(13) 0.0642(19) 0.0062(12) 0.0049(13) 0.0060(10) C56 0.0511(18) 0.0467(16) 0.0303(13) 0.0040(12) 0.0055(12) -0.0151(13) C57 0.0306(14) 0.0330(14) 0.093(3) -0.0079(15) 0.0250(16) -0.0015(11) C58 0.0399(16) 0.0365(15) 0.0619(19) 0.0132(13) -0.0275(14) -0.0078(12) C59 0.0187(10) 0.0214(10) 0.0160(9) 0.0015(7) 0.0009(7) 0.0009(8) C60 0.0193(10) 0.0281(11) 0.0234(10) 0.0001(8) 0.0032(8) -0.0007(8) C61 0.0215(11) 0.0290(11) 0.0250(11) 0.0050(9) 0.0008(8) -0.0043(9) C62 0.0286(12) 0.0218(10) 0.0216(10) 0.0021(8) -0.0040(9) -0.0043(8) C63 0.0240(11) 0.0223(10) 0.0219(10) -0.0009(8) -0.0002(8) 0.0036(8) C64 0.0187(10) 0.0225(10) 0.0169(9) 0.0005(7) -0.0008(7) 0.0001(8) N7 0.0197(9) 0.0233(9) 0.0193(8) -0.0006(7) 0.0031(7) 0.0022(7) N8 0.0170(9) 0.0249(9) 0.0266(9) -0.0037(7) 0.0031(7) 0.0023(7) Rh4 0.01587(8) 0.02058(8) 0.01919(8) 0.00066(6) 0.00033(6) -0.00106(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 C1 C2 1.413(3) . ? C1 C5 1.436(3) . ? C1 C6 1.499(3) . ? C1 Rh1 2.166(2) . ? C2 C3 1.436(3) . ? C2 C7 1.501(3) . ? C2 Rh1 2.161(2) . ? C3 C4 1.434(3) . ? C3 C8 1.498(3) . ? C3 Rh1 2.166(2) . ? C4 C5 1.423(3) . ? C4 C9 1.491(3) . ? C4 Rh1 2.183(2) . ? C5 C10 1.498(3) . ? C5 Rh1 2.186(2) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.360(3) . ? C11 C12 1.411(3) . ? C11 C16 1.420(3) . ? C12 C13 1.385(3) . ? C12 H12 0.9500 . ? C13 C14 1.402(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.408(3) . ? C15 H15 0.9500 . ? N1 Rh1 1.9745(19) . ? N1 H1 0.74(3) . ? N2 C16 1.368(3) . ? N2 Rh1 1.9824(18) . ? N2 H2 0.88(3) . ? C17 C21 1.417(3) . ? C17 C18 1.425(3) . ? C17 C22 1.500(3) . ? C17 Rh2 2.175(2) . ? C18 C19 1.463(4) . ? C18 C23 1.475(3) . ? C18 Rh2 2.168(2) . ? C19 C20 1.420(4) . ? C19 C24 1.491(4) . ? C19 Rh2 2.158(2) . ? C20 C21 1.424(4) . ? C20 C25 1.495(4) . ? C20 Rh2 2.145(2) . ? C21 C26 1.511(4) . ? C21 Rh2 2.152(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N3 1.362(3) . ? C27 C28 1.405(3) . ? C27 C32 1.421(3) . ? C28 C29 1.387(3) . ? C28 H28 0.9500 . ? C29 C30 1.396(3) . ? C29 H29 0.9500 . ? C30 C31 1.387(3) . ? C30 H30 0.9500 . ? N3 Rh2 1.9831(18) . ? N3 H3 0.87(3) . ? N4 C32 1.363(3) . ? N4 Rh2 1.9701(19) . ? N4 H4 0.91(3) . ? C31 C32 1.403(3) . ? C31 H31 0.9500 . ? C33 C37 1.426(3) . ? C33 C34 1.427(3) . ? C33 C38 1.489(3) . ? C33 Rh3 2.182(2) . ? C34 C35 1.444(3) . ? C34 C39 1.490(3) . ? C34 Rh3 2.169(2) . ? C35 C36 1.419(3) . ? C35 C40 1.494(3) . ? C35 Rh3 2.161(2) . ? C36 C37 1.435(3) . ? C36 C41 1.500(3) . ? C36 Rh3 2.169(2) . ? C37 C42 1.496(3) . ? C37 Rh3 2.186(2) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 N5 1.363(3) . ? C43 C44 1.410(3) . ? C43 C48 1.424(3) . ? C44 C45 1.383(3) . ? C44 H44 0.9500 . ? C45 C46 1.401(3) . ? C45 H45 0.9500 . ? N5 Rh3 1.9842(18) . ? N5 H5 0.81(3) . ? N6 C48 1.361(3) . ? N6 Rh3 1.9724(18) . ? N6 H6 0.77(3) . ? C46 C47 1.384(3) . ? C46 H46 0.9500 . ? C47 C48 1.412(3) . ? C47 H47 0.9500 . ? C49 C53 1.425(4) . ? C49 C50 1.425(3) . ? C49 C54 1.502(3) . ? C49 Rh4 2.175(2) . ? C50 C51 1.447(3) . ? C50 C55 1.497(3) . ? C50 Rh4 2.160(2) . ? C51 C52 1.441(3) . ? C51 C56 1.493(3) . ? C51 Rh4 2.153(2) . ? C52 C53 1.416(4) . ? C52 C57 1.496(3) . ? C52 Rh4 2.163(2) . ? C53 C58 1.505(3) . ? C53 Rh4 2.169(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 N7 1.360(3) . ? C59 C60 1.408(3) . ? C59 C64 1.425(3) . ? C60 C61 1.385(3) . ? C60 H60 0.9500 . ? C61 C62 1.393(3) . ? C61 H61 0.9500 . ? C62 C63 1.387(3) . ? C62 H62 0.9500 . ? C63 C64 1.401(3) . ? C63 H63 0.9500 . ? C64 N8 1.364(3) . ? N7 Rh4 1.9833(18) . ? N7 H7 0.85(3) . ? N8 Rh4 1.9716(19) . ? N8 H8 0.88(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 108.07(19) . . ? C2 C1 C6 126.4(2) . . ? C5 C1 C6 125.4(2) . . ? C2 C1 Rh1 70.73(13) . . ? C5 C1 Rh1 71.50(12) . . ? C6 C1 Rh1 125.60(16) . . ? C1 C2 C3 108.27(19) . . ? C1 C2 C7 125.8(2) . . ? C3 C2 C7 125.9(2) . . ? C1 C2 Rh1 71.13(12) . . ? C3 C2 Rh1 70.83(12) . . ? C7 C2 Rh1 125.94(16) . . ? C4 C3 C2 107.67(19) . . ? C4 C3 C8 126.6(2) . . ? C2 C3 C8 125.5(2) . . ? C4 C3 Rh1 71.39(12) . . ? C2 C3 Rh1 70.40(12) . . ? C8 C3 Rh1 128.13(17) . . ? C5 C4 C3 107.90(19) . . ? C5 C4 C9 126.7(2) . . ? C3 C4 C9 125.3(2) . . ? C5 C4 Rh1 71.12(12) . . ? C3 C4 Rh1 70.13(12) . . ? C9 C4 Rh1 127.52(16) . . ? C4 C5 C1 108.09(19) . . ? C4 C5 C10 125.7(2) . . ? C1 C5 C10 126.0(2) . . ? C4 C5 Rh1 70.87(12) . . ? C1 C5 Rh1 69.96(12) . . ? C10 C5 Rh1 128.43(16) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 126.71(19) . . ? N1 C11 C16 113.49(18) . . ? C12 C11 C16 119.79(19) . . ? C13 C12 C11 119.5(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.6(2) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 120.9(2) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.5(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 N1 Rh1 117.79(14) . . ? C11 N1 H1 119(2) . . ? Rh1 N1 H1 123(2) . . ? C16 N2 Rh1 117.45(14) . . ? C16 N2 H2 115.1(18) . . ? Rh1 N2 H2 127.3(18) . . ? N1 Rh1 N2 78.22(8) . . ? N1 Rh1 C2 109.68(8) . . ? N2 Rh1 C2 158.22(9) . . ? N1 Rh1 C1 110.06(8) . . ? N2 Rh1 C1 159.49(9) . . ? C2 Rh1 C1 38.14(9) . . ? N1 Rh1 C3 137.84(8) . . ? N2 Rh1 C3 122.44(8) . . ? C2 Rh1 C3 38.77(9) . . ? C1 Rh1 C3 64.43(9) . . ? N1 Rh1 C4 173.85(8) . . ? N2 Rh1 C4 107.92(8) . . ? C2 Rh1 C4 64.46(8) . . ? C1 Rh1 C4 64.31(8) . . ? C3 Rh1 C4 38.48(8) . . ? N1 Rh1 C5 138.78(8) . . ? N2 Rh1 C5 123.61(8) . . ? C2 Rh1 C5 64.09(8) . . ? C1 Rh1 C5 38.54(8) . . ? C3 Rh1 C5 64.08(8) . . ? C4 Rh1 C5 38.01(8) . . ? N2 C16 C15 127.36(19) . . ? N2 C16 C11 112.98(18) . . ? C15 C16 C11 119.66(19) . . ? C21 C17 C18 109.0(2) . . ? C21 C17 C22 127.7(2) . . ? C18 C17 C22 123.3(2) . . ? C21 C17 Rh2 70.00(13) . . ? C18 C17 Rh2 70.56(13) . . ? C22 C17 Rh2 127.36(17) . . ? C17 C18 C19 106.5(2) . . ? C17 C18 C23 128.3(3) . . ? C19 C18 C23 125.1(3) . . ? C17 C18 Rh2 71.13(13) . . ? C19 C18 Rh2 69.87(13) . . ? C23 C18 Rh2 125.78(17) . . ? C20 C19 C18 107.9(2) . . ? C20 C19 C24 128.2(3) . . ? C18 C19 C24 123.7(3) . . ? C20 C19 Rh2 70.25(14) . . ? C18 C19 Rh2 70.60(13) . . ? C24 C19 Rh2 127.78(19) . . ? C19 C20 C21 108.1(2) . . ? C19 C20 C25 127.7(3) . . ? C21 C20 C25 124.0(3) . . ? C19 C20 Rh2 71.21(14) . . ? C21 C20 Rh2 70.90(14) . . ? C25 C20 Rh2 127.00(19) . . ? C17 C21 C20 108.4(2) . . ? C17 C21 C26 125.8(3) . . ? C20 C21 C26 125.7(3) . . ? C17 C21 Rh2 71.78(13) . . ? C20 C21 Rh2 70.38(14) . . ? C26 C21 Rh2 125.04(17) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 127.6(2) . . ? N3 C27 C32 113.27(18) . . ? C28 C27 C32 119.16(19) . . ? C29 C28 C27 119.8(2) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 121.1(2) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C31 C30 C29 120.0(2) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C27 N3 Rh2 117.37(14) . . ? C27 N3 H3 113.5(17) . . ? Rh2 N3 H3 129.1(17) . . ? C32 N4 Rh2 117.79(15) . . ? C32 N4 H4 118(2) . . ? Rh2 N4 H4 124(2) . . ? N4 Rh2 N3 78.34(8) . . ? N4 Rh2 C20 109.73(9) . . ? N3 Rh2 C20 157.74(10) . . ? N4 Rh2 C21 137.64(9) . . ? N3 Rh2 C21 122.01(9) . . ? C20 Rh2 C21 38.72(10) . . ? N4 Rh2 C19 110.44(9) . . ? N3 Rh2 C19 159.28(10) . . ? C20 Rh2 C19 38.54(11) . . ? C21 Rh2 C19 64.61(10) . . ? N4 Rh2 C18 139.53(9) . . ? N3 Rh2 C18 122.23(9) . . ? C20 Rh2 C18 65.43(10) . . ? C21 Rh2 C18 64.76(9) . . ? C19 Rh2 C18 39.53(10) . . ? N4 Rh2 C17 174.12(8) . . ? N3 Rh2 C17 107.41(8) . . ? C20 Rh2 C17 64.48(9) . . ? C21 Rh2 C17 38.22(9) . . ? C19 Rh2 C17 64.57(9) . . ? C18 Rh2 C17 38.31(9) . . ? C30 C31 C32 120.0(2) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? N4 C32 C31 126.8(2) . . ? N4 C32 C27 113.22(18) . . ? C31 C32 C27 119.96(19) . . ? C37 C33 C34 108.01(19) . . ? C37 C33 C38 125.5(2) . . ? C34 C33 C38 126.4(2) . . ? C37 C33 Rh3 71.11(12) . . ? C34 C33 Rh3 70.34(12) . . ? C38 C33 Rh3 127.46(15) . . ? C33 C34 C35 107.7(2) . . ? C33 C34 C39 126.4(2) . . ? C35 C34 C39 125.7(2) . . ? C33 C34 Rh3 71.36(12) . . ? C35 C34 Rh3 70.24(13) . . ? C39 C34 Rh3 127.68(17) . . ? C36 C35 C34 108.06(19) . . ? C36 C35 C40 125.5(2) . . ? C34 C35 C40 126.3(2) . . ? C36 C35 Rh3 71.19(12) . . ? C34 C35 Rh3 70.79(12) . . ? C40 C35 Rh3 127.01(16) . . ? C35 C36 C37 107.96(19) . . ? C35 C36 C41 126.6(2) . . ? C37 C36 C41 125.4(2) . . ? C35 C36 Rh3 70.57(13) . . ? C37 C36 Rh3 71.40(12) . . ? C41 C36 Rh3 126.68(16) . . ? C33 C37 C36 108.25(19) . . ? C33 C37 C42 126.1(2) . . ? C36 C37 C42 125.5(2) . . ? C33 C37 Rh3 70.78(12) . . ? C36 C37 Rh3 70.13(12) . . ? C42 C37 Rh3 127.92(16) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C34 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C34 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C43 C44 127.73(19) . . ? N5 C43 C48 113.01(18) . . ? C44 C43 C48 119.25(19) . . ? C45 C44 C43 119.8(2) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.8(2) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C43 N5 Rh3 117.60(14) . . ? C43 N5 H5 114.8(19) . . ? Rh3 N5 H5 127.5(19) . . ? C48 N6 Rh3 118.00(14) . . ? C48 N6 H6 114(2) . . ? Rh3 N6 H6 128(2) . . ? N6 Rh3 N5 78.14(7) . . ? N6 Rh3 C35 111.36(8) . . ? N5 Rh3 C35 153.82(9) . . ? N6 Rh3 C34 141.89(8) . . ? N5 Rh3 C34 119.47(8) . . ? C35 Rh3 C34 38.97(9) . . ? N6 Rh3 C36 108.40(8) . . ? N5 Rh3 C36 164.01(8) . . ? C35 Rh3 C36 38.24(9) . . ? C34 Rh3 C36 64.57(9) . . ? N6 Rh3 C33 172.54(8) . . ? N5 Rh3 C33 108.30(8) . . ? C35 Rh3 C33 64.54(8) . . ? C34 Rh3 C33 38.30(8) . . ? C36 Rh3 C33 64.39(8) . . ? N6 Rh3 C37 134.89(8) . . ? N5 Rh3 C37 127.06(8) . . ? C35 Rh3 C37 64.13(8) . . ? C34 Rh3 C37 64.03(8) . . ? C36 Rh3 C37 38.47(8) . . ? C33 Rh3 C37 38.11(8) . . ? C47 C46 C45 120.9(2) . . ? C47 C46 H46 119.6 . . ? C45 C46 H46 119.6 . . ? C46 C47 C48 119.3(2) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? N6 C48 C47 126.72(19) . . ? N6 C48 C43 113.24(18) . . ? C47 C48 C43 120.04(19) . . ? C53 C49 C50 108.1(2) . . ? C53 C49 C54 125.9(2) . . ? C50 C49 C54 126.0(2) . . ? C53 C49 Rh4 70.63(13) . . ? C50 C49 Rh4 70.25(13) . . ? C54 C49 Rh4 126.35(17) . . ? C49 C50 C51 108.1(2) . . ? C49 C50 C55 126.4(2) . . ? C51 C50 C55 125.5(2) . . ? C49 C50 Rh4 71.37(13) . . ? C51 C50 Rh4 70.15(13) . . ? C55 C50 Rh4 125.69(17) . . ? C52 C51 C50 106.8(2) . . ? C52 C51 C56 125.8(2) . . ? C50 C51 C56 127.3(2) . . ? C52 C51 Rh4 70.85(13) . . ? C50 C51 Rh4 70.64(13) . . ? C56 C51 Rh4 126.08(18) . . ? C53 C52 C51 108.4(2) . . ? C53 C52 C57 126.1(3) . . ? C51 C52 C57 125.5(3) . . ? C53 C52 Rh4 71.15(13) . . ? C51 C52 Rh4 70.14(13) . . ? C57 C52 Rh4 126.42(18) . . ? C52 C53 C49 108.6(2) . . ? C52 C53 C58 127.2(3) . . ? C49 C53 C58 124.2(3) . . ? C52 C53 Rh4 70.69(13) . . ? C49 C53 Rh4 71.08(13) . . ? C58 C53 Rh4 126.39(17) . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C50 C55 H55A 109.5 . . ? C50 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C50 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C51 C56 H56A 109.5 . . ? C51 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C51 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C53 C58 H58A 109.5 . . ? C53 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C53 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? N7 C59 C60 128.0(2) . . ? N7 C59 C64 113.14(18) . . ? C60 C59 C64 118.79(19) . . ? C61 C60 C59 120.0(2) . . ? C61 C60 H60 120.0 . . ? C59 C60 H60 120.0 . . ? C60 C61 C62 120.9(2) . . ? C60 C61 H61 119.6 . . ? C62 C61 H61 119.6 . . ? C63 C62 C61 120.3(2) . . ? C63 C62 H62 119.8 . . ? C61 C62 H62 119.8 . . ? C62 C63 C64 119.9(2) . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? N8 C64 C63 126.9(2) . . ? N8 C64 C59 113.08(18) . . ? C63 C64 C59 120.05(19) . . ? C59 N7 Rh4 117.58(14) . . ? C59 N7 H7 110.4(18) . . ? Rh4 N7 H7 131.9(18) . . ? C64 N8 Rh4 117.82(14) . . ? C64 N8 H8 114(2) . . ? Rh4 N8 H8 129(2) . . ? N8 Rh4 N7 78.20(8) . . ? N8 Rh4 C51 124.23(9) . . ? N7 Rh4 C51 137.74(9) . . ? N8 Rh4 C50 162.09(9) . . ? N7 Rh4 C50 110.48(8) . . ? C51 Rh4 C50 39.20(9) . . ? N8 Rh4 C52 106.49(8) . . ? N7 Rh4 C52 175.28(8) . . ? C51 Rh4 C52 39.01(9) . . ? C50 Rh4 C52 64.87(9) . . ? N8 Rh4 C53 119.43(9) . . ? N7 Rh4 C53 140.02(9) . . ? C51 Rh4 C53 64.86(9) . . ? C50 Rh4 C53 64.41(9) . . ? C52 Rh4 C53 38.16(10) . . ? N8 Rh4 C49 154.20(9) . . ? N7 Rh4 C49 111.76(8) . . ? C51 Rh4 C49 65.00(9) . . ? C50 Rh4 C49 38.38(9) . . ? C52 Rh4 C49 64.24(9) . . ? C53 Rh4 C49 38.30(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 0.7(2) . . . . ? C6 C1 C2 C3 178.0(2) . . . . ? Rh1 C1 C2 C3 -61.43(15) . . . . ? C5 C1 C2 C7 -176.7(2) . . . . ? C6 C1 C2 C7 0.6(4) . . . . ? Rh1 C1 C2 C7 121.2(2) . . . . ? C5 C1 C2 Rh1 62.12(15) . . . . ? C6 C1 C2 Rh1 -120.6(2) . . . . ? C1 C2 C3 C4 -0.4(2) . . . . ? C7 C2 C3 C4 176.9(2) . . . . ? Rh1 C2 C3 C4 -62.03(15) . . . . ? C1 C2 C3 C8 -174.9(2) . . . . ? C7 C2 C3 C8 2.4(4) . . . . ? Rh1 C2 C3 C8 123.4(2) . . . . ? C1 C2 C3 Rh1 61.62(15) . . . . ? C7 C2 C3 Rh1 -121.0(2) . . . . ? C2 C3 C4 C5 0.0(2) . . . . ? C8 C3 C4 C5 174.4(2) . . . . ? Rh1 C3 C4 C5 -61.43(15) . . . . ? C2 C3 C4 C9 -176.1(2) . . . . ? C8 C3 C4 C9 -1.6(4) . . . . ? Rh1 C3 C4 C9 122.5(2) . . . . ? C2 C3 C4 Rh1 61.39(15) . . . . ? C8 C3 C4 Rh1 -124.2(2) . . . . ? C3 C4 C5 C1 0.5(2) . . . . ? C9 C4 C5 C1 176.4(2) . . . . ? Rh1 C4 C5 C1 -60.34(15) . . . . ? C3 C4 C5 C10 -175.1(2) . . . . ? C9 C4 C5 C10 0.9(4) . . . . ? Rh1 C4 C5 C10 124.1(2) . . . . ? C3 C4 C5 Rh1 60.80(15) . . . . ? C9 C4 C5 Rh1 -123.2(2) . . . . ? C2 C1 C5 C4 -0.7(2) . . . . ? C6 C1 C5 C4 -178.1(2) . . . . ? Rh1 C1 C5 C4 60.91(15) . . . . ? C2 C1 C5 C10 174.8(2) . . . . ? C6 C1 C5 C10 -2.5(4) . . . . ? Rh1 C1 C5 C10 -123.6(2) . . . . ? C2 C1 C5 Rh1 -61.63(15) . . . . ? C6 C1 C5 Rh1 121.0(2) . . . . ? N1 C11 C12 C13 178.8(2) . . . . ? C16 C11 C12 C13 0.2(3) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C12 C13 C14 C15 0.0(4) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C12 C11 N1 Rh1 -177.19(18) . . . . ? C16 C11 N1 Rh1 1.5(2) . . . . ? C11 N1 Rh1 N2 -2.12(16) . . . . ? C11 N1 Rh1 C2 156.77(16) . . . . ? C11 N1 Rh1 C1 -162.58(16) . . . . ? C11 N1 Rh1 C3 123.76(17) . . . . ? C11 N1 Rh1 C4 174.2(7) . . . . ? C11 N1 Rh1 C5 -130.44(16) . . . . ? C16 N2 Rh1 N1 2.39(16) . . . . ? C16 N2 Rh1 C2 -111.5(2) . . . . ? C16 N2 Rh1 C1 118.7(2) . . . . ? C16 N2 Rh1 C3 -137.49(16) . . . . ? C16 N2 Rh1 C4 -177.20(16) . . . . ? C16 N2 Rh1 C5 144.01(15) . . . . ? C1 C2 Rh1 N1 97.73(14) . . . . ? C3 C2 Rh1 N1 -144.27(13) . . . . ? C7 C2 Rh1 N1 -23.3(3) . . . . ? C1 C2 Rh1 N2 -154.17(19) . . . . ? C3 C2 Rh1 N2 -36.2(3) . . . . ? C7 C2 Rh1 N2 84.8(3) . . . . ? C3 C2 Rh1 C1 118.00(18) . . . . ? C7 C2 Rh1 C1 -121.1(3) . . . . ? C1 C2 Rh1 C3 -118.00(18) . . . . ? C7 C2 Rh1 C3 120.9(3) . . . . ? C1 C2 Rh1 C4 -80.24(14) . . . . ? C3 C2 Rh1 C4 37.76(13) . . . . ? C7 C2 Rh1 C4 158.7(3) . . . . ? C1 C2 Rh1 C5 -37.86(13) . . . . ? C3 C2 Rh1 C5 80.14(14) . . . . ? C7 C2 Rh1 C5 -158.9(3) . . . . ? C2 C1 Rh1 N1 -96.63(14) . . . . ? C5 C1 Rh1 N1 145.76(13) . . . . ? C6 C1 Rh1 N1 24.9(3) . . . . ? C2 C1 Rh1 N2 152.5(2) . . . . ? C5 C1 Rh1 N2 34.9(3) . . . . ? C6 C1 Rh1 N2 -85.9(3) . . . . ? C5 C1 Rh1 C2 -117.61(19) . . . . ? C6 C1 Rh1 C2 121.6(3) . . . . ? C2 C1 Rh1 C3 37.80(13) . . . . ? C5 C1 Rh1 C3 -79.81(14) . . . . ? C6 C1 Rh1 C3 159.4(3) . . . . ? C2 C1 Rh1 C4 80.68(14) . . . . ? C5 C1 Rh1 C4 -36.93(13) . . . . ? C6 C1 Rh1 C4 -157.8(3) . . . . ? C2 C1 Rh1 C5 117.61(19) . . . . ? C6 C1 Rh1 C5 -120.8(3) . . . . ? C4 C3 Rh1 N1 172.37(13) . . . . ? C2 C3 Rh1 N1 54.99(18) . . . . ? C8 C3 Rh1 N1 -65.2(3) . . . . ? C4 C3 Rh1 N2 -77.66(15) . . . . ? C2 C3 Rh1 N2 164.97(12) . . . . ? C8 C3 Rh1 N2 44.8(3) . . . . ? C4 C3 Rh1 C2 117.38(19) . . . . ? C8 C3 Rh1 C2 -120.2(3) . . . . ? C4 C3 Rh1 C1 80.19(14) . . . . ? C2 C3 Rh1 C1 -37.19(13) . . . . ? C8 C3 Rh1 C1 -157.4(3) . . . . ? C2 C3 Rh1 C4 -117.38(19) . . . . ? C8 C3 Rh1 C4 122.4(3) . . . . ? C4 C3 Rh1 C5 37.21(13) . . . . ? C2 C3 Rh1 C5 -80.17(14) . . . . ? C8 C3 Rh1 C5 159.6(3) . . . . ? C5 C4 Rh1 N1 61.7(8) . . . . ? C3 C4 Rh1 N1 -56.2(8) . . . . ? C9 C4 Rh1 N1 -176.1(7) . . . . ? C5 C4 Rh1 N2 -122.08(13) . . . . ? C3 C4 Rh1 N2 119.95(13) . . . . ? C9 C4 Rh1 N2 0.1(3) . . . . ? C5 C4 Rh1 C2 79.92(14) . . . . ? C3 C4 Rh1 C2 -38.04(13) . . . . ? C9 C4 Rh1 C2 -157.9(3) . . . . ? C5 C4 Rh1 C1 37.44(13) . . . . ? C3 C4 Rh1 C1 -80.53(14) . . . . ? C9 C4 Rh1 C1 159.7(3) . . . . ? C5 C4 Rh1 C3 117.96(19) . . . . ? C9 C4 Rh1 C3 -119.8(3) . . . . ? C3 C4 Rh1 C5 -117.96(19) . . . . ? C9 C4 Rh1 C5 122.2(3) . . . . ? C4 C5 Rh1 N1 -171.77(13) . . . . ? C1 C5 Rh1 N1 -53.32(18) . . . . ? C10 C5 Rh1 N1 67.3(3) . . . . ? C4 C5 Rh1 N2 75.48(15) . . . . ? C1 C5 Rh1 N2 -166.07(12) . . . . ? C10 C5 Rh1 N2 -45.5(3) . . . . ? C4 C5 Rh1 C2 -80.98(14) . . . . ? C1 C5 Rh1 C2 37.47(13) . . . . ? C10 C5 Rh1 C2 158.1(3) . . . . ? C4 C5 Rh1 C1 -118.45(19) . . . . ? C10 C5 Rh1 C1 120.6(3) . . . . ? C4 C5 Rh1 C3 -37.67(13) . . . . ? C1 C5 Rh1 C3 80.78(14) . . . . ? C10 C5 Rh1 C3 -158.6(3) . . . . ? C1 C5 Rh1 C4 118.45(19) . . . . ? C10 C5 Rh1 C4 -120.9(3) . . . . ? Rh1 N2 C16 C15 177.43(17) . . . . ? Rh1 N2 C16 C11 -2.3(2) . . . . ? C14 C15 C16 N2 -179.2(2) . . . . ? C14 C15 C16 C11 0.5(3) . . . . ? N1 C11 C16 N2 0.5(3) . . . . ? C12 C11 C16 N2 179.29(19) . . . . ? N1 C11 C16 C15 -179.26(19) . . . . ? C12 C11 C16 C15 -0.4(3) . . . . ? C21 C17 C18 C19 -1.6(2) . . . . ? C22 C17 C18 C19 176.2(2) . . . . ? Rh2 C17 C18 C19 -61.26(15) . . . . ? C21 C17 C18 C23 -179.2(2) . . . . ? C22 C17 C18 C23 -1.4(4) . . . . ? Rh2 C17 C18 C23 121.2(3) . . . . ? C21 C17 C18 Rh2 59.67(16) . . . . ? C22 C17 C18 Rh2 -122.5(2) . . . . ? C17 C18 C19 C20 1.4(3) . . . . ? C23 C18 C19 C20 179.1(2) . . . . ? Rh2 C18 C19 C20 -60.65(16) . . . . ? C17 C18 C19 C24 -174.8(2) . . . . ? C23 C18 C19 C24 2.9(4) . . . . ? Rh2 C18 C19 C24 123.1(2) . . . . ? C17 C18 C19 Rh2 62.09(15) . . . . ? C23 C18 C19 Rh2 -120.2(2) . . . . ? C18 C19 C20 C21 -0.8(3) . . . . ? C24 C19 C20 C21 175.3(2) . . . . ? Rh2 C19 C20 C21 -61.63(17) . . . . ? C18 C19 C20 C25 -176.4(2) . . . . ? C24 C19 C20 C25 -0.4(4) . . . . ? Rh2 C19 C20 C25 122.7(3) . . . . ? C18 C19 C20 Rh2 60.87(16) . . . . ? C24 C19 C20 Rh2 -123.1(3) . . . . ? C18 C17 C21 C20 1.1(3) . . . . ? C22 C17 C21 C20 -176.5(2) . . . . ? Rh2 C17 C21 C20 61.17(16) . . . . ? C18 C17 C21 C26 179.5(2) . . . . ? C22 C17 C21 C26 1.8(4) . . . . ? Rh2 C17 C21 C26 -120.5(2) . . . . ? C18 C17 C21 Rh2 -60.02(16) . . . . ? C22 C17 C21 Rh2 122.3(2) . . . . ? C19 C20 C21 C17 -0.2(3) . . . . ? C25 C20 C21 C17 175.6(2) . . . . ? Rh2 C20 C21 C17 -62.05(16) . . . . ? C19 C20 C21 C26 -178.5(2) . . . . ? C25 C20 C21 C26 -2.7(4) . . . . ? Rh2 C20 C21 C26 119.6(2) . . . . ? C19 C20 C21 Rh2 61.83(17) . . . . ? C25 C20 C21 Rh2 -122.3(3) . . . . ? N3 C27 C28 C29 179.3(2) . . . . ? C32 C27 C28 C29 -0.4(3) . . . . ? C27 C28 C29 C30 0.6(3) . . . . ? C28 C29 C30 C31 -0.4(3) . . . . ? C28 C27 N3 Rh2 -179.29(17) . . . . ? C32 C27 N3 Rh2 0.4(2) . . . . ? C32 N4 Rh2 N3 0.93(15) . . . . ? C32 N4 Rh2 C20 159.35(16) . . . . ? C32 N4 Rh2 C21 126.18(17) . . . . ? C32 N4 Rh2 C19 -159.51(16) . . . . ? C32 N4 Rh2 C18 -125.74(17) . . . . ? C32 N4 Rh2 C17 169.1(7) . . . . ? C27 N3 Rh2 N4 -0.72(15) . . . . ? C27 N3 Rh2 C20 -114.7(2) . . . . ? C27 N3 Rh2 C21 -140.26(15) . . . . ? C27 N3 Rh2 C19 116.8(3) . . . . ? C27 N3 Rh2 C18 141.30(15) . . . . ? C27 N3 Rh2 C17 -179.46(15) . . . . ? C19 C20 Rh2 N4 98.36(15) . . . . ? C21 C20 Rh2 N4 -143.89(14) . . . . ? C25 C20 Rh2 N4 -25.1(3) . . . . ? C19 C20 Rh2 N3 -153.6(2) . . . . ? C21 C20 Rh2 N3 -35.9(3) . . . . ? C25 C20 Rh2 N3 82.9(4) . . . . ? C19 C20 Rh2 C21 -117.8(2) . . . . ? C25 C20 Rh2 C21 118.7(4) . . . . ? C21 C20 Rh2 C19 117.8(2) . . . . ? C25 C20 Rh2 C19 -123.5(4) . . . . ? C19 C20 Rh2 C18 -38.08(15) . . . . ? C21 C20 Rh2 C18 79.67(15) . . . . ? C25 C20 Rh2 C18 -161.6(3) . . . . ? C19 C20 Rh2 C17 -80.54(15) . . . . ? C21 C20 Rh2 C17 37.22(14) . . . . ? C25 C20 Rh2 C17 156.0(3) . . . . ? C17 C21 Rh2 N4 173.52(13) . . . . ? C20 C21 Rh2 N4 55.4(2) . . . . ? C26 C21 Rh2 N4 -65.0(3) . . . . ? C17 C21 Rh2 N3 -77.09(15) . . . . ? C20 C21 Rh2 N3 164.83(14) . . . . ? C26 C21 Rh2 N3 44.4(3) . . . . ? C17 C21 Rh2 C20 118.1(2) . . . . ? C26 C21 Rh2 C20 -120.4(3) . . . . ? C17 C21 Rh2 C19 80.47(15) . . . . ? C20 C21 Rh2 C19 -37.62(15) . . . . ? C26 C21 Rh2 C19 -158.0(3) . . . . ? C17 C21 Rh2 C18 36.53(14) . . . . ? C20 C21 Rh2 C18 -81.56(16) . . . . ? C26 C21 Rh2 C18 158.0(3) . . . . ? C20 C21 Rh2 C17 -118.1(2) . . . . ? C26 C21 Rh2 C17 121.5(3) . . . . ? C20 C19 Rh2 N4 -96.33(15) . . . . ? C18 C19 Rh2 N4 145.48(13) . . . . ? C24 C19 Rh2 N4 27.3(3) . . . . ? C20 C19 Rh2 N3 151.6(2) . . . . ? C18 C19 Rh2 N3 33.4(3) . . . . ? C24 C19 Rh2 N3 -84.8(4) . . . . ? C18 C19 Rh2 C20 -118.2(2) . . . . ? C24 C19 Rh2 C20 123.6(4) . . . . ? C20 C19 Rh2 C21 37.79(15) . . . . ? C18 C19 Rh2 C21 -80.41(15) . . . . ? C24 C19 Rh2 C21 161.4(3) . . . . ? C20 C19 Rh2 C18 118.2(2) . . . . ? C24 C19 Rh2 C18 -118.2(4) . . . . ? C20 C19 Rh2 C17 80.28(16) . . . . ? C18 C19 Rh2 C17 -37.91(13) . . . . ? C24 C19 Rh2 C17 -156.1(3) . . . . ? C17 C18 Rh2 N4 -171.37(13) . . . . ? C19 C18 Rh2 N4 -54.91(19) . . . . ? C23 C18 Rh2 N4 64.5(3) . . . . ? C17 C18 Rh2 N3 76.85(15) . . . . ? C19 C18 Rh2 N3 -166.69(14) . . . . ? C23 C18 Rh2 N3 -47.3(3) . . . . ? C17 C18 Rh2 C20 -79.31(15) . . . . ? C19 C18 Rh2 C20 37.15(15) . . . . ? C23 C18 Rh2 C20 156.5(3) . . . . ? C17 C18 Rh2 C21 -36.45(14) . . . . ? C19 C18 Rh2 C21 80.01(16) . . . . ? C23 C18 Rh2 C21 -160.6(3) . . . . ? C17 C18 Rh2 C19 -116.5(2) . . . . ? C23 C18 Rh2 C19 119.4(3) . . . . ? C19 C18 Rh2 C17 116.5(2) . . . . ? C23 C18 Rh2 C17 -124.1(3) . . . . ? C21 C17 Rh2 N4 -47.9(8) . . . . ? C18 C17 Rh2 N4 71.8(8) . . . . ? C22 C17 Rh2 N4 -170.6(7) . . . . ? C21 C17 Rh2 N3 119.98(14) . . . . ? C18 C17 Rh2 N3 -120.31(14) . . . . ? C22 C17 Rh2 N3 -2.8(3) . . . . ? C21 C17 Rh2 C20 -37.70(15) . . . . ? C18 C17 Rh2 C20 82.01(16) . . . . ? C22 C17 Rh2 C20 -160.5(3) . . . . ? C18 C17 Rh2 C21 119.7(2) . . . . ? C22 C17 Rh2 C21 -122.8(3) . . . . ? C21 C17 Rh2 C19 -80.59(16) . . . . ? C18 C17 Rh2 C19 39.12(15) . . . . ? C22 C17 Rh2 C19 156.7(3) . . . . ? C21 C17 Rh2 C18 -119.7(2) . . . . ? C22 C17 Rh2 C18 117.5(3) . . . . ? C29 C30 C31 C32 0.0(3) . . . . ? Rh2 N4 C32 C31 179.04(17) . . . . ? Rh2 N4 C32 C27 -1.0(2) . . . . ? C30 C31 C32 N4 -179.9(2) . . . . ? C30 C31 C32 C27 0.2(3) . . . . ? N3 C27 C32 N4 0.3(3) . . . . ? C28 C27 C32 N4 -179.92(18) . . . . ? N3 C27 C32 C31 -179.67(18) . . . . ? C28 C27 C32 C31 0.1(3) . . . . ? C37 C33 C34 C35 0.3(2) . . . . ? C38 C33 C34 C35 176.2(2) . . . . ? Rh3 C33 C34 C35 -61.16(15) . . . . ? C37 C33 C34 C39 -175.0(2) . . . . ? C38 C33 C34 C39 0.9(4) . . . . ? Rh3 C33 C34 C39 123.6(2) . . . . ? C37 C33 C34 Rh3 61.46(15) . . . . ? C38 C33 C34 Rh3 -122.6(2) . . . . ? C33 C34 C35 C36 0.1(2) . . . . ? C39 C34 C35 C36 175.4(2) . . . . ? Rh3 C34 C35 C36 -61.79(15) . . . . ? C33 C34 C35 C40 -175.8(2) . . . . ? C39 C34 C35 C40 -0.5(4) . . . . ? Rh3 C34 C35 C40 122.3(2) . . . . ? C33 C34 C35 Rh3 61.88(15) . . . . ? C39 C34 C35 Rh3 -122.8(2) . . . . ? C34 C35 C36 C37 -0.4(2) . . . . ? C40 C35 C36 C37 175.5(2) . . . . ? Rh3 C35 C36 C37 -61.97(15) . . . . ? C34 C35 C36 C41 -176.7(2) . . . . ? C40 C35 C36 C41 -0.8(4) . . . . ? Rh3 C35 C36 C41 121.8(2) . . . . ? C34 C35 C36 Rh3 61.53(15) . . . . ? C40 C35 C36 Rh3 -122.6(2) . . . . ? C34 C33 C37 C36 -0.6(2) . . . . ? C38 C33 C37 C36 -176.5(2) . . . . ? Rh3 C33 C37 C36 60.39(15) . . . . ? C34 C33 C37 C42 175.6(2) . . . . ? C38 C33 C37 C42 -0.4(4) . . . . ? Rh3 C33 C37 C42 -123.5(2) . . . . ? C34 C33 C37 Rh3 -60.97(15) . . . . ? C38 C33 C37 Rh3 123.1(2) . . . . ? C35 C36 C37 C33 0.6(2) . . . . ? C41 C36 C37 C33 176.9(2) . . . . ? Rh3 C36 C37 C33 -60.81(15) . . . . ? C35 C36 C37 C42 -175.5(2) . . . . ? C41 C36 C37 C42 0.7(4) . . . . ? Rh3 C36 C37 C42 123.0(2) . . . . ? C35 C36 C37 Rh3 61.44(15) . . . . ? C41 C36 C37 Rh3 -122.3(2) . . . . ? N5 C43 C44 C45 -178.9(2) . . . . ? C48 C43 C44 C45 0.4(3) . . . . ? C43 C44 C45 C46 -0.6(3) . . . . ? C44 C43 N5 Rh3 -179.76(17) . . . . ? C48 C43 N5 Rh3 0.9(2) . . . . ? C48 N6 Rh3 N5 1.15(16) . . . . ? C48 N6 Rh3 C35 -153.33(16) . . . . ? C48 N6 Rh3 C34 -121.98(17) . . . . ? C48 N6 Rh3 C36 166.02(16) . . . . ? C48 N6 Rh3 C33 151.3(6) . . . . ? C48 N6 Rh3 C37 132.45(16) . . . . ? C43 N5 Rh3 N6 -1.13(16) . . . . ? C43 N5 Rh3 C35 113.5(2) . . . . ? C43 N5 Rh3 C34 142.45(15) . . . . ? C43 N5 Rh3 C36 -117.1(3) . . . . ? C43 N5 Rh3 C33 -177.23(15) . . . . ? C43 N5 Rh3 C37 -139.30(15) . . . . ? C36 C35 Rh3 N6 -92.95(14) . . . . ? C34 C35 Rh3 N6 149.30(13) . . . . ? C40 C35 Rh3 N6 27.8(3) . . . . ? C36 C35 Rh3 N5 159.89(16) . . . . ? C34 C35 Rh3 N5 42.1(2) . . . . ? C40 C35 Rh3 N5 -79.3(3) . . . . ? C36 C35 Rh3 C34 117.74(19) . . . . ? C40 C35 Rh3 C34 -121.5(3) . . . . ? C34 C35 Rh3 C36 -117.74(19) . . . . ? C40 C35 Rh3 C36 120.8(3) . . . . ? C36 C35 Rh3 C33 80.25(14) . . . . ? C34 C35 Rh3 C33 -37.49(13) . . . . ? C40 C35 Rh3 C33 -158.9(3) . . . . ? C36 C35 Rh3 C37 37.78(13) . . . . ? C34 C35 Rh3 C37 -79.96(14) . . . . ? C40 C35 Rh3 C37 158.6(3) . . . . ? C33 C34 Rh3 N6 -167.93(13) . . . . ? C35 C34 Rh3 N6 -50.38(19) . . . . ? C39 C34 Rh3 N6 70.0(3) . . . . ? C33 C34 Rh3 N5 82.33(14) . . . . ? C35 C34 Rh3 N5 -160.12(12) . . . . ? C39 C34 Rh3 N5 -39.7(3) . . . . ? C33 C34 Rh3 C35 -117.55(19) . . . . ? C39 C34 Rh3 C35 120.4(3) . . . . ? C33 C34 Rh3 C36 -80.21(14) . . . . ? C35 C34 Rh3 C36 37.34(13) . . . . ? C39 C34 Rh3 C36 157.8(3) . . . . ? C35 C34 Rh3 C33 117.55(19) . . . . ? C39 C34 Rh3 C33 -122.0(3) . . . . ? C33 C34 Rh3 C37 -37.32(13) . . . . ? C35 C34 Rh3 C37 80.23(14) . . . . ? C39 C34 Rh3 C37 -159.4(3) . . . . ? C35 C36 Rh3 N6 101.41(14) . . . . ? C37 C36 Rh3 N6 -140.97(13) . . . . ? C41 C36 Rh3 N6 -20.2(2) . . . . ? C35 C36 Rh3 N5 -146.6(3) . . . . ? C37 C36 Rh3 N5 -29.0(3) . . . . ? C41 C36 Rh3 N5 91.8(4) . . . . ? C37 C36 Rh3 C35 117.62(19) . . . . ? C41 C36 Rh3 C35 -121.7(3) . . . . ? C35 C36 Rh3 C34 -38.05(13) . . . . ? C37 C36 Rh3 C34 79.58(14) . . . . ? C41 C36 Rh3 C34 -159.7(3) . . . . ? C35 C36 Rh3 C33 -80.68(14) . . . . ? C37 C36 Rh3 C33 36.94(12) . . . . ? C41 C36 Rh3 C33 157.7(3) . . . . ? C35 C36 Rh3 C37 -117.62(19) . . . . ? C41 C36 Rh3 C37 120.7(3) . . . . ? C37 C33 Rh3 N6 -21.8(7) . . . . ? C34 C33 Rh3 N6 96.2(6) . . . . ? C38 C33 Rh3 N6 -142.5(6) . . . . ? C37 C33 Rh3 N5 127.36(12) . . . . ? C34 C33 Rh3 N5 -114.66(14) . . . . ? C38 C33 Rh3 N5 6.7(2) . . . . ? C37 C33 Rh3 C35 -79.85(14) . . . . ? C34 C33 Rh3 C35 38.14(14) . . . . ? C38 C33 Rh3 C35 159.5(2) . . . . ? C37 C33 Rh3 C34 -117.99(19) . . . . ? C38 C33 Rh3 C34 121.3(3) . . . . ? C37 C33 Rh3 C36 -37.28(13) . . . . ? C34 C33 Rh3 C36 80.70(15) . . . . ? C38 C33 Rh3 C36 -158.0(2) . . . . ? C34 C33 Rh3 C37 117.99(19) . . . . ? C38 C33 Rh3 C37 -120.7(3) . . . . ? C33 C37 Rh3 N6 176.10(12) . . . . ? C36 C37 Rh3 N6 57.51(17) . . . . ? C42 C37 Rh3 N6 -62.6(2) . . . . ? C33 C37 Rh3 N5 -71.03(15) . . . . ? C36 C37 Rh3 N5 170.38(12) . . . . ? C42 C37 Rh3 N5 50.3(2) . . . . ? C33 C37 Rh3 C35 81.04(14) . . . . ? C36 C37 Rh3 C35 -37.55(13) . . . . ? C42 C37 Rh3 C35 -157.6(2) . . . . ? C33 C37 Rh3 C34 37.50(13) . . . . ? C36 C37 Rh3 C34 -81.09(14) . . . . ? C42 C37 Rh3 C34 158.9(2) . . . . ? C33 C37 Rh3 C36 118.59(18) . . . . ? C42 C37 Rh3 C36 -120.1(3) . . . . ? C36 C37 Rh3 C33 -118.59(18) . . . . ? C42 C37 Rh3 C33 121.3(3) . . . . ? C44 C45 C46 C47 0.1(4) . . . . ? C45 C46 C47 C48 0.5(3) . . . . ? Rh3 N6 C48 C47 179.41(17) . . . . ? Rh3 N6 C48 C43 -1.0(2) . . . . ? C46 C47 C48 N6 178.9(2) . . . . ? C46 C47 C48 C43 -0.7(3) . . . . ? N5 C43 C48 N6 0.0(3) . . . . ? C44 C43 C48 N6 -179.34(19) . . . . ? N5 C43 C48 C47 179.65(19) . . . . ? C44 C43 C48 C47 0.3(3) . . . . ? C53 C49 C50 C51 -0.1(3) . . . . ? C54 C49 C50 C51 178.0(2) . . . . ? Rh4 C49 C50 C51 -60.83(16) . . . . ? C53 C49 C50 C55 -178.1(2) . . . . ? C54 C49 C50 C55 -0.1(4) . . . . ? Rh4 C49 C50 C55 121.1(2) . . . . ? C53 C49 C50 Rh4 60.78(16) . . . . ? C54 C49 C50 Rh4 -121.2(2) . . . . ? C49 C50 C51 C52 -0.4(3) . . . . ? C55 C50 C51 C52 177.7(2) . . . . ? Rh4 C50 C51 C52 -62.03(15) . . . . ? C49 C50 C51 C56 -177.3(2) . . . . ? C55 C50 C51 C56 0.8(4) . . . . ? Rh4 C50 C51 C56 121.1(3) . . . . ? C49 C50 C51 Rh4 61.61(16) . . . . ? C55 C50 C51 Rh4 -120.3(2) . . . . ? C50 C51 C52 C53 0.7(3) . . . . ? C56 C51 C52 C53 177.6(2) . . . . ? Rh4 C51 C52 C53 -61.15(16) . . . . ? C50 C51 C52 C57 -176.9(2) . . . . ? C56 C51 C52 C57 0.0(4) . . . . ? Rh4 C51 C52 C57 121.2(2) . . . . ? C50 C51 C52 Rh4 61.89(15) . . . . ? C56 C51 C52 Rh4 -121.2(2) . . . . ? C51 C52 C53 C49 -0.8(3) . . . . ? C57 C52 C53 C49 176.9(2) . . . . ? Rh4 C52 C53 C49 -61.30(16) . . . . ? C51 C52 C53 C58 -177.9(2) . . . . ? C57 C52 C53 C58 -0.3(4) . . . . ? Rh4 C52 C53 C58 121.5(2) . . . . ? C51 C52 C53 Rh4 60.52(16) . . . . ? C57 C52 C53 Rh4 -121.8(2) . . . . ? C50 C49 C53 C52 0.5(3) . . . . ? C54 C49 C53 C52 -177.5(2) . . . . ? Rh4 C49 C53 C52 61.06(16) . . . . ? C50 C49 C53 C58 177.8(2) . . . . ? C54 C49 C53 C58 -0.3(4) . . . . ? Rh4 C49 C53 C58 -121.7(2) . . . . ? C50 C49 C53 Rh4 -60.54(16) . . . . ? C54 C49 C53 Rh4 121.4(2) . . . . ? N7 C59 C60 C61 -178.1(2) . . . . ? C64 C59 C60 C61 0.3(3) . . . . ? C59 C60 C61 C62 -0.3(3) . . . . ? C60 C61 C62 C63 -0.2(3) . . . . ? C61 C62 C63 C64 0.9(3) . . . . ? C62 C63 C64 N8 178.5(2) . . . . ? C62 C63 C64 C59 -0.9(3) . . . . ? N7 C59 C64 N8 -0.5(3) . . . . ? C60 C59 C64 N8 -179.13(19) . . . . ? N7 C59 C64 C63 178.96(18) . . . . ? C60 C59 C64 C63 0.4(3) . . . . ? C60 C59 N7 Rh4 175.71(17) . . . . ? C64 C59 N7 Rh4 -2.7(2) . . . . ? C63 C64 N8 Rh4 -175.85(17) . . . . ? C59 C64 N8 Rh4 3.6(2) . . . . ? C64 N8 Rh4 N7 -3.91(15) . . . . ? C64 N8 Rh4 C51 -144.47(16) . . . . ? C64 N8 Rh4 C50 -125.0(3) . . . . ? C64 N8 Rh4 C52 176.67(16) . . . . ? C64 N8 Rh4 C53 137.42(16) . . . . ? C64 N8 Rh4 C49 112.1(2) . . . . ? C59 N7 Rh4 N8 3.59(15) . . . . ? C59 N7 Rh4 C51 132.24(16) . . . . ? C59 N7 Rh4 C50 167.26(15) . . . . ? C59 N7 Rh4 C52 176.8(10) . . . . ? C59 N7 Rh4 C53 -118.55(17) . . . . ? C59 N7 Rh4 C49 -151.50(15) . . . . ? C52 C51 Rh4 N8 -72.88(16) . . . . ? C50 C51 Rh4 N8 170.64(12) . . . . ? C56 C51 Rh4 N8 48.0(3) . . . . ? C52 C51 Rh4 N7 174.73(13) . . . . ? C50 C51 Rh4 N7 58.26(18) . . . . ? C56 C51 Rh4 N7 -64.4(3) . . . . ? C52 C51 Rh4 C50 116.5(2) . . . . ? C56 C51 Rh4 C50 -122.6(3) . . . . ? C50 C51 Rh4 C52 -116.5(2) . . . . ? C56 C51 Rh4 C52 120.9(3) . . . . ? C52 C51 Rh4 C53 36.82(14) . . . . ? C50 C51 Rh4 C53 -79.65(15) . . . . ? C56 C51 Rh4 C53 157.7(3) . . . . ? C52 C51 Rh4 C49 79.28(15) . . . . ? C50 C51 Rh4 C49 -37.19(14) . . . . ? C56 C51 Rh4 C49 -159.8(3) . . . . ? C49 C50 Rh4 N8 -144.0(2) . . . . ? C51 C50 Rh4 N8 -25.9(3) . . . . ? C55 C50 Rh4 N8 94.1(3) . . . . ? C49 C50 Rh4 N7 99.55(14) . . . . ? C51 C50 Rh4 N7 -142.37(13) . . . . ? C55 C50 Rh4 N7 -22.3(2) . . . . ? C49 C50 Rh4 C51 -118.1(2) . . . . ? C55 C50 Rh4 C51 120.0(3) . . . . ? C49 C50 Rh4 C52 -79.59(15) . . . . ? C51 C50 Rh4 C52 38.49(14) . . . . ? C55 C50 Rh4 C52 158.5(3) . . . . ? C49 C50 Rh4 C53 -37.17(14) . . . . ? C51 C50 Rh4 C53 80.91(15) . . . . ? C55 C50 Rh4 C53 -159.1(3) . . . . ? C51 C50 Rh4 C49 118.1(2) . . . . ? C55 C50 Rh4 C49 -121.9(3) . . . . ? C53 C52 Rh4 N8 -116.90(14) . . . . ? C51 C52 Rh4 N8 124.51(14) . . . . ? C57 C52 Rh4 N8 4.5(3) . . . . ? C53 C52 Rh4 N7 70.1(11) . . . . ? C51 C52 Rh4 N7 -48.5(11) . . . . ? C57 C52 Rh4 N7 -168.6(10) . . . . ? C53 C52 Rh4 C51 118.6(2) . . . . ? C57 C52 Rh4 C51 -120.0(3) . . . . ? C53 C52 Rh4 C50 79.91(15) . . . . ? C51 C52 Rh4 C50 -38.68(14) . . . . ? C57 C52 Rh4 C50 -158.7(3) . . . . ? C51 C52 Rh4 C53 -118.6(2) . . . . ? C57 C52 Rh4 C53 121.4(3) . . . . ? C53 C52 Rh4 C49 37.22(14) . . . . ? C51 C52 Rh4 C49 -81.37(15) . . . . ? C57 C52 Rh4 C49 158.6(3) . . . . ? C52 C53 Rh4 N8 79.03(15) . . . . ? C49 C53 Rh4 N8 -162.49(13) . . . . ? C58 C53 Rh4 N8 -43.4(3) . . . . ? C52 C53 Rh4 N7 -173.08(13) . . . . ? C49 C53 Rh4 N7 -54.61(19) . . . . ? C58 C53 Rh4 N7 64.5(3) . . . . ? C52 C53 Rh4 C51 -37.63(14) . . . . ? C49 C53 Rh4 C51 80.84(15) . . . . ? C58 C53 Rh4 C51 -160.1(3) . . . . ? C52 C53 Rh4 C50 -81.22(15) . . . . ? C49 C53 Rh4 C50 37.26(13) . . . . ? C58 C53 Rh4 C50 156.3(3) . . . . ? C49 C53 Rh4 C52 118.5(2) . . . . ? C58 C53 Rh4 C52 -122.5(3) . . . . ? C52 C53 Rh4 C49 -118.5(2) . . . . ? C58 C53 Rh4 C49 119.1(3) . . . . ? C53 C49 Rh4 N8 37.0(3) . . . . ? C50 C49 Rh4 N8 155.45(17) . . . . ? C54 C49 Rh4 N8 -83.8(3) . . . . ? C53 C49 Rh4 N7 145.67(13) . . . . ? C50 C49 Rh4 N7 -95.90(14) . . . . ? C54 C49 Rh4 N7 24.9(3) . . . . ? C53 C49 Rh4 C51 -80.46(15) . . . . ? C50 C49 Rh4 C51 37.98(14) . . . . ? C54 C49 Rh4 C51 158.7(3) . . . . ? C53 C49 Rh4 C50 -118.4(2) . . . . ? C54 C49 Rh4 C50 120.7(3) . . . . ? C53 C49 Rh4 C52 -37.09(14) . . . . ? C50 C49 Rh4 C52 81.35(15) . . . . ? C54 C49 Rh4 C52 -157.9(3) . . . . ? C50 C49 Rh4 C53 118.4(2) . . . . ? C54 C49 Rh4 C53 -120.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6 H6 N7 0.77(3) 2.57(3) 3.338(3) 179(3) . N1 H1 N3 0.74(3) 2.68(3) 3.409(3) 170(3) 2_645 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.11 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.707 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.099 # Attachment 'rnp0808m_Rh_C5Me5__TosNC6H4NH2_Cl_rev.cif' data_rnp0808m _database_code_depnum_ccdc_archive 'CCDC 729050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H28 Cl N2 O2 Rh S' _chemical_formula_sum 'C23 H28 Cl N2 O2 Rh S' _chemical_formula_weight 534.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0617(11) _cell_length_b 15.1303(15) _cell_length_c 16.2600(17) _cell_angle_alpha 117.247(2) _cell_angle_beta 104.377(2) _cell_angle_gamma 92.805(2) _cell_volume 2301.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7937 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 28.26 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.971 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details 'SADABS v2.03 (Sheldrick)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31550 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 28.29 _reflns_number_total 11375 _reflns_number_gt 10101 _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, 1997)' _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^)+(0.0293P)^2^+1.1670P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11375 _refine_ls_number_parameters 569 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0282 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0573 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 C1 C 0.55620(16) 0.35449(13) 0.32232(12) 0.0162(3) Uani 1 1 d . . . C2 C 0.60751(16) 0.30981(13) 0.24218(12) 0.0158(3) Uani 1 1 d . . . C3 C 0.53354(16) 0.21144(12) 0.17456(12) 0.0139(3) Uani 1 1 d . . . C4 C 0.43505(16) 0.19344(12) 0.21278(12) 0.0146(3) Uani 1 1 d . . . C5 C 0.45242(16) 0.28069(13) 0.30501(12) 0.0161(3) Uani 1 1 d . . . C6 C 0.60689(19) 0.45592(14) 0.41107(13) 0.0253(4) Uani 1 1 d . . . H6A H 0.6557 0.4473 0.4653 0.038 Uiso 1 1 calc R . . H6B H 0.5360 0.4892 0.4277 0.038 Uiso 1 1 calc R . . H6C H 0.6621 0.4977 0.3984 0.038 Uiso 1 1 calc R . . C7 C 0.72014(17) 0.35961(15) 0.23392(15) 0.0243(4) Uani 1 1 d . . . H7A H 0.7981 0.3512 0.2720 0.036 Uiso 1 1 calc R . . H7B H 0.7187 0.4319 0.2587 0.036 Uiso 1 1 calc R . . H7C H 0.7177 0.3284 0.1656 0.036 Uiso 1 1 calc R . . C8 C 0.55466(18) 0.13824(13) 0.08171(13) 0.0197(4) Uani 1 1 d . . . H8A H 0.6036 0.1749 0.0604 0.029 Uiso 1 1 calc R . . H8B H 0.4725 0.1026 0.0319 0.029 Uiso 1 1 calc R . . H8C H 0.6018 0.0891 0.0919 0.029 Uiso 1 1 calc R . . C9 C 0.33448(17) 0.10014(13) 0.16527(14) 0.0201(4) Uani 1 1 d . . . H9A H 0.3606 0.0562 0.1931 0.030 Uiso 1 1 calc R . . H9B H 0.3229 0.0639 0.0953 0.030 Uiso 1 1 calc R . . H9C H 0.2543 0.1194 0.1763 0.030 Uiso 1 1 calc R . . C10 C 0.3757(2) 0.29286(16) 0.37188(14) 0.0251(4) Uani 1 1 d . . . H10A H 0.2913 0.2499 0.3343 0.038 Uiso 1 1 calc R . . H10B H 0.3668 0.3638 0.4058 0.038 Uiso 1 1 calc R . . H10C H 0.4185 0.2729 0.4195 0.038 Uiso 1 1 calc R . . C11 C 0.15172(16) 0.22017(13) 0.05752(12) 0.0149(3) Uani 1 1 d . . . C12 C 0.06359(17) 0.13500(14) -0.01372(13) 0.0205(4) Uani 1 1 d . . . H12 H 0.0802 0.0919 -0.0726 0.025 Uiso 1 1 calc R . . C13 C -0.04999(18) 0.11269(15) 0.00136(15) 0.0249(4) Uani 1 1 d . . . H13 H -0.1112 0.0539 -0.0469 0.030 Uiso 1 1 calc R . . C14 C -0.07290(18) 0.17670(15) 0.08703(15) 0.0252(4) Uani 1 1 d . . . H14 H -0.1508 0.1618 0.0970 0.030 Uiso 1 1 calc R . . C15 C 0.01587(17) 0.26259(14) 0.15906(14) 0.0214(4) Uani 1 1 d . . . H15 H -0.0022 0.3061 0.2171 0.026 Uiso 1 1 calc R . . C16 C 0.13152(16) 0.28507(12) 0.14621(12) 0.0146(3) Uani 1 1 d . . . C17 C 0.11301(17) 0.51676(13) 0.23514(12) 0.0164(3) Uani 1 1 d . . . C18 C -0.00740(18) 0.52795(15) 0.24479(14) 0.0240(4) Uani 1 1 d . . . H18 H -0.0359 0.5095 0.2863 0.029 Uiso 1 1 calc R . . C19 C -0.0859(2) 0.56637(16) 0.19305(15) 0.0280(4) Uani 1 1 d . . . H19 H -0.1682 0.5743 0.1998 0.034 Uiso 1 1 calc R . . C20 C -0.04595(19) 0.59329(14) 0.13164(14) 0.0233(4) Uani 1 1 d . . . C21 C 0.07551(18) 0.58105(14) 0.12319(13) 0.0211(4) Uani 1 1 d . . . H21 H 0.1042 0.5994 0.0817 0.025 Uiso 1 1 calc R . . C22 C 0.15506(17) 0.54271(13) 0.17398(13) 0.0186(3) Uani 1 1 d . . . H22 H 0.2372 0.5343 0.1671 0.022 Uiso 1 1 calc R . . C23 C -0.1315(2) 0.63483(16) 0.07563(15) 0.0305(5) Uani 1 1 d . . . H23A H -0.2127 0.5874 0.0372 0.046 Uiso 1 1 calc R . . H23B H -0.0909 0.6439 0.0322 0.046 Uiso 1 1 calc R . . H23C H -0.1466 0.7002 0.1211 0.046 Uiso 1 1 calc R . . N1 N 0.27338(14) 0.24666(12) 0.04862(10) 0.0142(3) Uani 1 1 d . . . N2 N 0.23547(13) 0.36376(11) 0.21338(10) 0.0147(3) Uani 1 1 d . . . S1 S 0.21396(4) 0.46454(3) 0.29748(3) 0.01559(8) Uani 1 1 d . . . O1 O 0.14548(13) 0.44562(10) 0.35485(9) 0.0222(3) Uani 1 1 d . . . O2 O 0.33496(12) 0.53296(9) 0.35075(9) 0.0208(3) Uani 1 1 d . . . Cl1 Cl 0.45912(4) 0.44559(3) 0.14518(3) 0.02081(9) Uani 1 1 d . . . Rh1 Rh 0.411706(12) 0.320084(9) 0.190634(9) 0.01103(4) Uani 1 1 d . . . C24 C 0.35152(16) 0.77509(13) 0.31072(13) 0.0172(3) Uani 1 1 d . . . C25 C 0.45944(16) 0.72851(13) 0.29089(13) 0.0167(3) Uani 1 1 d . . . C26 C 0.46952(17) 0.72173(13) 0.20217(13) 0.0184(3) Uani 1 1 d . . . C27 C 0.36790(18) 0.76392(14) 0.16660(13) 0.0197(4) Uani 1 1 d . . . C28 C 0.29515(17) 0.79567(14) 0.23310(13) 0.0197(4) Uani 1 1 d . . . C29 C 0.30092(19) 0.78818(14) 0.39193(14) 0.0226(4) Uani 1 1 d . . . H29A H 0.2531 0.8435 0.4068 0.034 Uiso 1 1 calc R . . H29B H 0.3718 0.8042 0.4496 0.034 Uiso 1 1 calc R . . H29C H 0.2447 0.7254 0.3726 0.034 Uiso 1 1 calc R . . C30 C 0.54481(18) 0.69394(14) 0.35275(14) 0.0221(4) Uani 1 1 d . . . H30A H 0.5082 0.6249 0.3348 0.033 Uiso 1 1 calc R . . H30B H 0.5537 0.7394 0.4212 0.033 Uiso 1 1 calc R . . H30C H 0.6286 0.6949 0.3427 0.033 Uiso 1 1 calc R . . C31 C 0.5670(2) 0.67804(15) 0.15357(15) 0.0267(4) Uani 1 1 d . . . H31A H 0.6472 0.6901 0.2029 0.040 Uiso 1 1 calc R . . H31B H 0.5803 0.7103 0.1155 0.040 Uiso 1 1 calc R . . H31C H 0.5373 0.6050 0.1105 0.040 Uiso 1 1 calc R . . C32 C 0.3384(2) 0.76585(17) 0.07249(14) 0.0310(5) Uani 1 1 d . . . H32A H 0.2735 0.7067 0.0223 0.046 Uiso 1 1 calc R . . H32B H 0.4157 0.7644 0.0531 0.046 Uiso 1 1 calc R . . H32C H 0.3067 0.8278 0.0805 0.046 Uiso 1 1 calc R . . C33 C 0.18145(18) 0.84465(16) 0.22449(16) 0.0291(4) Uani 1 1 d . . . H33A H 0.1812 0.8727 0.1807 0.044 Uiso 1 1 calc R . . H33B H 0.1851 0.8992 0.2887 0.044 Uiso 1 1 calc R . . H33C H 0.1038 0.7941 0.1984 0.044 Uiso 1 1 calc R . . C34 C 0.75147(16) 0.91711(13) 0.42730(13) 0.0169(3) Uani 1 1 d . . . C35 C 0.84202(18) 0.89633(15) 0.48839(15) 0.0253(4) Uani 1 1 d . . . H35 H 0.8300 0.9017 0.5463 0.030 Uiso 1 1 calc R . . C36 C 0.9506(2) 0.86752(18) 0.46387(18) 0.0349(5) Uani 1 1 d . . . H36 H 1.0140 0.8528 0.5047 0.042 Uiso 1 1 calc R . . C37 C 0.9658(2) 0.86047(18) 0.37923(18) 0.0353(5) Uani 1 1 d . . . H37 H 1.0399 0.8401 0.3624 0.042 Uiso 1 1 calc R . . C38 C 0.87557(18) 0.88239(16) 0.31817(15) 0.0258(4) Uani 1 1 d . . . H38 H 0.8893 0.8788 0.2614 0.031 Uiso 1 1 calc R . . C39 C 0.76506(16) 0.90956(13) 0.34099(13) 0.0173(3) Uani 1 1 d . . . C40 C 0.77106(17) 1.08843(13) 0.28898(13) 0.0181(3) Uani 1 1 d . . . C41 C 0.73034(18) 1.16230(14) 0.36118(13) 0.0201(4) Uani 1 1 d . . . H41 H 0.6489 1.1489 0.3669 0.024 Uiso 1 1 calc R . . C42 C 0.80980(19) 1.25564(14) 0.42461(14) 0.0225(4) Uani 1 1 d . . . H42 H 0.7815 1.3062 0.4733 0.027 Uiso 1 1 calc R . . C43 C 0.9301(2) 1.27668(14) 0.41833(14) 0.0233(4) Uani 1 1 d . . . C44 C 0.9672(2) 1.20258(15) 0.34381(15) 0.0274(4) Uani 1 1 d . . . H44 H 1.0476 1.2165 0.3368 0.033 Uiso 1 1 calc R . . C45 C 0.88882(19) 1.10858(15) 0.27952(14) 0.0250(4) Uani 1 1 d . . . H45 H 0.9159 1.0586 0.2295 0.030 Uiso 1 1 calc R . . C46 C 1.0209(2) 1.37481(15) 0.49217(15) 0.0318(5) Uani 1 1 d . . . H46A H 0.9731 1.4260 0.5244 0.048 Uiso 1 1 calc R . . H46B H 1.0673 1.3981 0.4594 0.048 Uiso 1 1 calc R . . H46C H 1.0813 1.3640 0.5406 0.048 Uiso 1 1 calc R . . N3 N 0.63323(15) 0.94484(12) 0.44532(11) 0.0168(3) Uani 1 1 d . . . N4 N 0.65748(13) 0.92452(11) 0.28390(10) 0.0151(3) Uani 1 1 d . . . S2 S 0.67132(4) 0.96715(3) 0.21309(3) 0.01675(8) Uani 1 1 d . . . O3 O 0.73814(13) 0.90840(10) 0.14560(9) 0.0240(3) Uani 1 1 d . . . O4 O 0.54758(13) 0.97907(10) 0.16999(9) 0.0230(3) Uani 1 1 d . . . Cl2 Cl 0.43173(4) 1.04350(3) 0.36616(3) 0.01827(8) Uani 1 1 d . . . Rh2 Rh 0.488837(12) 0.877403(9) 0.307806(9) 0.01266(4) Uani 1 1 d . . . H1A H 0.272(2) 0.2948(17) 0.0389(15) 0.016(5) Uiso 1 1 d . . . H3A H 0.638(2) 1.0061(19) 0.4636(17) 0.025(6) Uiso 1 1 d . . . H1B H 0.291(2) 0.1963(18) 0.0045(17) 0.025(6) Uiso 1 1 d . . . H3B H 0.615(2) 0.9318(18) 0.4860(18) 0.032(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0161(8) 0.0169(8) 0.0122(8) 0.0059(7) 0.0008(6) 0.0047(6) C2 0.0129(8) 0.0162(8) 0.0177(8) 0.0081(7) 0.0035(6) 0.0041(6) C3 0.0149(8) 0.0151(8) 0.0141(8) 0.0086(7) 0.0043(6) 0.0071(6) C4 0.0160(8) 0.0150(8) 0.0156(8) 0.0099(7) 0.0038(6) 0.0056(6) C5 0.0188(8) 0.0193(8) 0.0153(8) 0.0114(7) 0.0063(7) 0.0088(7) C6 0.0251(10) 0.0207(9) 0.0157(9) 0.0014(7) -0.0024(7) 0.0042(7) C7 0.0157(9) 0.0250(10) 0.0320(10) 0.0134(8) 0.0082(8) 0.0027(7) C8 0.0270(9) 0.0174(8) 0.0176(8) 0.0086(7) 0.0106(7) 0.0090(7) C9 0.0192(9) 0.0170(8) 0.0266(9) 0.0133(7) 0.0057(7) 0.0027(7) C10 0.0332(11) 0.0301(10) 0.0242(10) 0.0183(8) 0.0165(8) 0.0141(8) C11 0.0129(8) 0.0157(8) 0.0175(8) 0.0100(7) 0.0027(6) 0.0034(6) C12 0.0203(9) 0.0180(8) 0.0176(8) 0.0060(7) 0.0025(7) 0.0028(7) C13 0.0170(9) 0.0212(9) 0.0290(10) 0.0102(8) 0.0001(8) -0.0028(7) C14 0.0139(8) 0.0284(10) 0.0360(11) 0.0180(9) 0.0073(8) 0.0021(7) C15 0.0179(9) 0.0226(9) 0.0261(9) 0.0121(8) 0.0096(7) 0.0067(7) C16 0.0150(8) 0.0140(8) 0.0162(8) 0.0089(7) 0.0035(6) 0.0044(6) C17 0.0185(8) 0.0138(8) 0.0147(8) 0.0051(6) 0.0044(6) 0.0061(6) C18 0.0247(10) 0.0302(10) 0.0243(9) 0.0162(8) 0.0117(8) 0.0124(8) C19 0.0246(10) 0.0356(11) 0.0318(11) 0.0192(9) 0.0135(8) 0.0177(9) C20 0.0264(10) 0.0205(9) 0.0213(9) 0.0096(8) 0.0044(8) 0.0106(7) C21 0.0270(10) 0.0181(8) 0.0189(9) 0.0092(7) 0.0076(7) 0.0060(7) C22 0.0196(9) 0.0172(8) 0.0184(8) 0.0076(7) 0.0065(7) 0.0053(7) C23 0.0345(11) 0.0308(11) 0.0283(10) 0.0162(9) 0.0071(9) 0.0174(9) N1 0.0159(7) 0.0146(7) 0.0112(7) 0.0059(6) 0.0035(5) 0.0039(6) N2 0.0132(7) 0.0141(7) 0.0153(7) 0.0053(6) 0.0055(5) 0.0041(5) S1 0.0182(2) 0.01581(19) 0.01290(18) 0.00615(16) 0.00588(16) 0.00693(16) O1 0.0267(7) 0.0285(7) 0.0188(6) 0.0138(6) 0.0130(5) 0.0126(6) O2 0.0211(6) 0.0175(6) 0.0156(6) 0.0031(5) 0.0021(5) 0.0038(5) Cl1 0.0228(2) 0.0182(2) 0.0258(2) 0.01434(18) 0.00765(17) 0.00204(16) Rh1 0.01178(6) 0.01061(6) 0.01056(6) 0.00506(5) 0.00329(5) 0.00258(4) C24 0.0167(8) 0.0172(8) 0.0179(8) 0.0085(7) 0.0060(7) 0.0001(6) C25 0.0173(8) 0.0133(8) 0.0179(8) 0.0072(7) 0.0040(7) 0.0003(6) C26 0.0221(9) 0.0141(8) 0.0172(8) 0.0052(7) 0.0084(7) 0.0004(7) C27 0.0219(9) 0.0198(9) 0.0139(8) 0.0077(7) 0.0018(7) -0.0021(7) C28 0.0151(8) 0.0207(9) 0.0227(9) 0.0119(7) 0.0025(7) -0.0002(7) C29 0.0262(10) 0.0207(9) 0.0208(9) 0.0079(7) 0.0124(8) 0.0005(7) C30 0.0237(9) 0.0184(9) 0.0251(9) 0.0130(8) 0.0041(8) 0.0032(7) C31 0.0344(11) 0.0201(9) 0.0279(10) 0.0087(8) 0.0192(9) 0.0062(8) C32 0.0367(12) 0.0369(12) 0.0166(9) 0.0150(9) 0.0016(8) -0.0037(9) C33 0.0179(9) 0.0329(11) 0.0380(12) 0.0200(10) 0.0050(8) 0.0065(8) C34 0.0149(8) 0.0153(8) 0.0194(8) 0.0088(7) 0.0031(7) 0.0016(6) C35 0.0221(9) 0.0285(10) 0.0276(10) 0.0190(9) 0.0013(8) 0.0020(8) C36 0.0207(10) 0.0444(13) 0.0498(14) 0.0343(12) 0.0035(9) 0.0102(9) C37 0.0179(10) 0.0469(13) 0.0540(14) 0.0325(12) 0.0137(10) 0.0158(9) C38 0.0197(9) 0.0317(10) 0.0333(11) 0.0193(9) 0.0121(8) 0.0087(8) C39 0.0161(8) 0.0154(8) 0.0201(8) 0.0091(7) 0.0043(7) 0.0027(6) C40 0.0236(9) 0.0179(8) 0.0163(8) 0.0105(7) 0.0077(7) 0.0032(7) C41 0.0228(9) 0.0210(9) 0.0215(9) 0.0126(7) 0.0095(7) 0.0072(7) C42 0.0326(10) 0.0172(8) 0.0213(9) 0.0105(7) 0.0109(8) 0.0087(8) C43 0.0351(11) 0.0176(9) 0.0203(9) 0.0121(7) 0.0084(8) 0.0013(8) C44 0.0297(10) 0.0262(10) 0.0267(10) 0.0113(8) 0.0138(8) -0.0026(8) C45 0.0311(10) 0.0230(9) 0.0209(9) 0.0077(8) 0.0145(8) 0.0019(8) C46 0.0451(13) 0.0205(10) 0.0270(10) 0.0089(8) 0.0136(10) -0.0032(9) N3 0.0205(8) 0.0174(8) 0.0137(7) 0.0086(6) 0.0052(6) 0.0035(6) N4 0.0154(7) 0.0184(7) 0.0159(7) 0.0110(6) 0.0061(6) 0.0048(6) S2 0.0199(2) 0.0185(2) 0.01320(19) 0.00791(16) 0.00704(16) 0.00227(16) O3 0.0281(7) 0.0239(7) 0.0162(6) 0.0041(5) 0.0126(5) 0.0004(6) O4 0.0232(7) 0.0306(7) 0.0199(6) 0.0169(6) 0.0050(5) 0.0039(6) Cl2 0.0221(2) 0.01858(19) 0.01871(19) 0.01054(16) 0.00966(16) 0.00895(16) Rh2 0.01330(7) 0.01420(6) 0.01245(6) 0.00753(5) 0.00486(5) 0.00330(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 C1 C5 1.439(2) . ? C1 C2 1.441(2) . ? C1 C6 1.496(2) . ? C1 Rh1 2.1468(17) . ? C2 C3 1.424(2) . ? C2 C7 1.491(2) . ? C2 Rh1 2.1607(17) . ? C3 C4 1.452(2) . ? C3 C8 1.493(2) . ? C3 Rh1 2.1413(16) . ? C4 C5 1.431(2) . ? C4 C9 1.499(2) . ? C4 Rh1 2.1219(16) . ? C5 C10 1.492(2) . ? C5 Rh1 2.1546(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.379(2) . ? C11 C16 1.407(2) . ? C11 N1 1.446(2) . ? C12 C13 1.393(3) . ? C12 H12 0.9500 . ? C13 C14 1.381(3) . ? C13 H13 0.9500 . ? C14 C15 1.391(3) . ? C14 H14 0.9500 . ? C15 C16 1.397(2) . ? C15 H15 0.9500 . ? C16 N2 1.409(2) . ? C17 C18 1.389(3) . ? C17 C22 1.389(2) . ? C17 S1 1.7766(17) . ? C18 C19 1.391(3) . ? C18 H18 0.9500 . ? C19 C20 1.390(3) . ? C19 H19 0.9500 . ? C20 C21 1.397(3) . ? C20 C23 1.508(3) . ? C21 C22 1.386(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N1 Rh1 2.1535(14) . ? N1 H1A 0.81(2) . ? N1 H1B 0.85(2) . ? N2 S1 1.5936(14) . ? N2 Rh1 2.1528(14) . ? S1 O2 1.4426(13) . ? S1 O1 1.4491(13) . ? Cl1 Rh1 2.4098(5) . ? C24 C28 1.438(2) . ? C24 C25 1.446(2) . ? C24 C29 1.495(2) . ? C24 Rh2 2.1397(17) . ? C25 C26 1.432(2) . ? C25 C30 1.495(2) . ? C25 Rh2 2.1385(17) . ? C26 C27 1.446(3) . ? C26 C31 1.496(3) . ? C26 Rh2 2.1466(17) . ? C27 C28 1.429(3) . ? C27 C32 1.498(2) . ? C27 Rh2 2.1562(18) . ? C28 C33 1.500(3) . ? C28 Rh2 2.1605(18) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.383(2) . ? C34 C39 1.402(2) . ? C34 N3 1.450(2) . ? C35 C36 1.387(3) . ? C35 H35 0.9500 . ? C36 C37 1.384(3) . ? C36 H36 0.9500 . ? C37 C38 1.390(3) . ? C37 H37 0.9500 . ? C38 C39 1.391(3) . ? C38 H38 0.9500 . ? C39 N4 1.414(2) . ? C40 C45 1.385(3) . ? C40 C41 1.393(2) . ? C40 S2 1.7775(18) . ? C41 C42 1.388(3) . ? C41 H41 0.9500 . ? C42 C43 1.392(3) . ? C42 H42 0.9500 . ? C43 C44 1.394(3) . ? C43 C46 1.509(3) . ? C44 C45 1.391(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? N3 Rh2 2.1377(15) . ? N3 H3A 0.83(2) . ? N3 H3B 0.84(3) . ? N4 S2 1.5883(14) . ? N4 Rh2 2.1502(14) . ? S2 O4 1.4355(14) . ? S2 O3 1.4542(13) . ? Cl2 Rh2 2.4259(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 C5 C1 C2 107.46(15) . . ? C5 C1 C6 125.84(16) . . ? C2 C1 C6 126.55(17) . . ? C5 C1 Rh1 70.75(9) . . ? C2 C1 Rh1 70.98(9) . . ? C6 C1 Rh1 126.97(12) . . ? C3 C2 C1 108.49(15) . . ? C3 C2 C7 126.79(16) . . ? C1 C2 C7 124.72(16) . . ? C3 C2 Rh1 69.93(9) . . ? C1 C2 Rh1 69.94(9) . . ? C7 C2 Rh1 126.43(13) . . ? C2 C3 C4 107.97(14) . . ? C2 C3 C8 126.35(16) . . ? C4 C3 C8 125.67(15) . . ? C2 C3 Rh1 71.40(9) . . ? C4 C3 Rh1 69.36(9) . . ? C8 C3 Rh1 125.87(12) . . ? C5 C4 C3 107.46(15) . . ? C5 C4 C9 126.08(16) . . ? C3 C4 C9 126.46(15) . . ? C5 C4 Rh1 71.69(9) . . ? C3 C4 Rh1 70.80(9) . . ? C9 C4 Rh1 123.52(12) . . ? C4 C5 C1 108.53(15) . . ? C4 C5 C10 125.63(17) . . ? C1 C5 C10 125.84(16) . . ? C4 C5 Rh1 69.22(9) . . ? C1 C5 Rh1 70.17(9) . . ? C10 C5 Rh1 126.48(12) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 122.04(16) . . ? C12 C11 N1 122.71(16) . . ? C16 C11 N1 115.19(15) . . ? C11 C12 C13 119.43(17) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C14 C13 C12 119.43(17) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.26(17) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 120.18(17) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 117.62(16) . . ? C15 C16 N2 127.98(16) . . ? C11 C16 N2 114.35(15) . . ? C18 C17 C22 120.72(16) . . ? C18 C17 S1 120.51(14) . . ? C22 C17 S1 118.72(13) . . ? C17 C18 C19 119.38(18) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 121.03(18) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 118.37(17) . . ? C19 C20 C23 120.82(18) . . ? C21 C20 C23 120.81(18) . . ? C22 C21 C20 121.46(18) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C17 119.04(17) . . ? C21 C22 H22 120.5 . . ? C17 C22 H22 120.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C11 N1 Rh1 108.74(10) . . ? C11 N1 H1A 109.0(15) . . ? Rh1 N1 H1A 98.2(15) . . ? C11 N1 H1B 111.0(16) . . ? Rh1 N1 H1B 116.8(15) . . ? H1A N1 H1B 112(2) . . ? C16 N2 S1 120.21(11) . . ? C16 N2 Rh1 110.93(10) . . ? S1 N2 Rh1 128.64(8) . . ? O2 S1 O1 116.14(8) . . ? O2 S1 N2 107.74(8) . . ? O1 S1 N2 113.29(8) . . ? O2 S1 C17 108.32(8) . . ? O1 S1 C17 106.11(8) . . ? N2 S1 C17 104.50(8) . . ? C4 Rh1 C3 39.84(6) . . ? C4 Rh1 C1 66.15(6) . . ? C3 Rh1 C1 65.67(6) . . ? C4 Rh1 N2 108.66(6) . . ? C3 Rh1 N2 147.87(6) . . ? C1 Rh1 N2 113.30(6) . . ? C4 Rh1 N1 99.90(6) . . ? C3 Rh1 N1 101.00(6) . . ? C1 Rh1 N1 165.36(6) . . ? N2 Rh1 N1 74.39(6) . . ? C4 Rh1 C5 39.09(6) . . ? C3 Rh1 C5 65.53(6) . . ? C1 Rh1 C5 39.08(7) . . ? N2 Rh1 C5 93.19(6) . . ? N1 Rh1 C5 131.28(6) . . ? C4 Rh1 C2 65.82(6) . . ? C3 Rh1 C2 38.67(6) . . ? C1 Rh1 C2 39.08(6) . . ? N2 Rh1 C2 152.36(6) . . ? N1 Rh1 C2 132.58(6) . . ? C5 Rh1 C2 65.09(7) . . ? C4 Rh1 Cl1 156.96(5) . . ? C3 Rh1 Cl1 117.12(5) . . ? C1 Rh1 Cl1 107.88(5) . . ? N2 Rh1 Cl1 94.20(4) . . ? N1 Rh1 Cl1 83.17(4) . . ? C5 Rh1 Cl1 145.42(5) . . ? C2 Rh1 Cl1 95.17(5) . . ? C28 C24 C25 107.75(15) . . ? C28 C24 C29 126.76(17) . . ? C25 C24 C29 125.18(16) . . ? C28 C24 Rh2 71.25(10) . . ? C25 C24 Rh2 70.20(10) . . ? C29 C24 Rh2 129.04(13) . . ? C26 C25 C24 107.90(15) . . ? C26 C25 C30 126.47(16) . . ? C24 C25 C30 125.63(16) . . ? C26 C25 Rh2 70.79(10) . . ? C24 C25 Rh2 70.29(10) . . ? C30 C25 Rh2 124.43(12) . . ? C25 C26 C27 108.07(15) . . ? C25 C26 C31 126.41(17) . . ? C27 C26 C31 125.52(17) . . ? C25 C26 Rh2 70.17(10) . . ? C27 C26 Rh2 70.72(10) . . ? C31 C26 Rh2 125.12(13) . . ? C28 C27 C26 107.90(15) . . ? C28 C27 C32 126.25(18) . . ? C26 C27 C32 125.68(18) . . ? C28 C27 Rh2 70.83(10) . . ? C26 C27 Rh2 70.00(10) . . ? C32 C27 Rh2 128.44(13) . . ? C27 C28 C24 108.38(16) . . ? C27 C28 C33 125.65(17) . . ? C24 C28 C33 125.95(17) . . ? C27 C28 Rh2 70.51(10) . . ? C24 C28 Rh2 69.69(10) . . ? C33 C28 Rh2 124.36(13) . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 122.37(17) . . ? C35 C34 N3 122.95(17) . . ? C39 C34 N3 114.65(15) . . ? C34 C35 C36 118.97(19) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? C37 C36 C35 119.29(19) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 121.92(19) . . ? C36 C37 H37 119.0 . . ? C38 C37 H37 119.0 . . ? C37 C38 C39 119.36(19) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C34 118.07(17) . . ? C38 C39 N4 127.77(17) . . ? C34 C39 N4 114.01(15) . . ? C45 C40 C41 120.30(17) . . ? C45 C40 S2 121.16(14) . . ? C41 C40 S2 118.50(14) . . ? C42 C41 C40 119.40(17) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C43 121.36(17) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? C42 C43 C44 118.14(18) . . ? C42 C43 C46 121.49(18) . . ? C44 C43 C46 120.31(19) . . ? C45 C44 C43 121.25(18) . . ? C45 C44 H44 119.4 . . ? C43 C44 H44 119.4 . . ? C40 C45 C44 119.49(18) . . ? C40 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C34 N3 Rh2 107.45(11) . . ? C34 N3 H3A 108.4(16) . . ? Rh2 N3 H3A 102.4(16) . . ? C34 N3 H3B 114.2(17) . . ? Rh2 N3 H3B 113.8(17) . . ? H3A N3 H3B 110(2) . . ? C39 N4 S2 121.01(12) . . ? C39 N4 Rh2 109.57(11) . . ? S2 N4 Rh2 129.40(8) . . ? O4 S2 O3 115.79(8) . . ? O4 S2 N4 107.69(8) . . ? O3 S2 N4 112.80(8) . . ? O4 S2 C40 109.04(8) . . ? O3 S2 C40 105.48(8) . . ? N4 S2 C40 105.50(8) . . ? N3 Rh2 C25 96.48(6) . . ? N3 Rh2 C24 106.72(7) . . ? C25 Rh2 C24 39.51(7) . . ? N3 Rh2 C26 121.20(7) . . ? C25 Rh2 C26 39.04(7) . . ? C24 Rh2 C26 65.75(7) . . ? N3 Rh2 N4 74.10(6) . . ? C25 Rh2 N4 117.23(6) . . ? C24 Rh2 N4 156.55(6) . . ? C26 Rh2 N4 93.37(6) . . ? N3 Rh2 C27 160.23(7) . . ? C25 Rh2 C27 65.68(7) . . ? C24 Rh2 C27 65.52(7) . . ? C26 Rh2 C27 39.27(7) . . ? N4 Rh2 C27 105.58(6) . . ? N3 Rh2 C28 143.07(7) . . ? C25 Rh2 C28 65.61(7) . . ? C24 Rh2 C28 39.06(7) . . ? C26 Rh2 C28 65.32(7) . . ? N4 Rh2 C28 142.51(6) . . ? C27 Rh2 C28 38.66(7) . . ? N3 Rh2 Cl2 84.80(4) . . ? C25 Rh2 Cl2 148.40(5) . . ? C24 Rh2 Cl2 109.86(5) . . ? C26 Rh2 Cl2 154.00(5) . . ? N4 Rh2 Cl2 93.58(4) . . ? C27 Rh2 Cl2 114.80(5) . . ? C28 Rh2 Cl2 94.74(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 C5 C1 C2 C3 2.19(19) . . . . ? C6 C1 C2 C3 178.04(16) . . . . ? Rh1 C1 C2 C3 -59.52(11) . . . . ? C5 C1 C2 C7 -177.22(16) . . . . ? C6 C1 C2 C7 -1.4(3) . . . . ? Rh1 C1 C2 C7 121.08(17) . . . . ? C5 C1 C2 Rh1 61.70(11) . . . . ? C6 C1 C2 Rh1 -122.44(18) . . . . ? C1 C2 C3 C4 -0.46(18) . . . . ? C7 C2 C3 C4 178.93(16) . . . . ? Rh1 C2 C3 C4 -59.99(11) . . . . ? C1 C2 C3 C8 -179.15(15) . . . . ? C7 C2 C3 C8 0.2(3) . . . . ? Rh1 C2 C3 C8 121.33(17) . . . . ? C1 C2 C3 Rh1 59.53(11) . . . . ? C7 C2 C3 Rh1 -121.08(18) . . . . ? C2 C3 C4 C5 -1.44(18) . . . . ? C8 C3 C4 C5 177.25(15) . . . . ? Rh1 C3 C4 C5 -62.73(11) . . . . ? C2 C3 C4 C9 179.30(16) . . . . ? C8 C3 C4 C9 -2.0(3) . . . . ? Rh1 C3 C4 C9 118.02(17) . . . . ? C2 C3 C4 Rh1 61.28(11) . . . . ? C8 C3 C4 Rh1 -120.02(16) . . . . ? C3 C4 C5 C1 2.81(18) . . . . ? C9 C4 C5 C1 -177.93(15) . . . . ? Rh1 C4 C5 C1 -59.34(11) . . . . ? C3 C4 C5 C10 -177.16(16) . . . . ? C9 C4 C5 C10 2.1(3) . . . . ? Rh1 C4 C5 C10 120.69(17) . . . . ? C3 C4 C5 Rh1 62.15(11) . . . . ? C9 C4 C5 Rh1 -118.59(17) . . . . ? C2 C1 C5 C4 -3.10(19) . . . . ? C6 C1 C5 C4 -178.99(16) . . . . ? Rh1 C1 C5 C4 58.76(11) . . . . ? C2 C1 C5 C10 176.87(16) . . . . ? C6 C1 C5 C10 1.0(3) . . . . ? Rh1 C1 C5 C10 -121.27(17) . . . . ? C2 C1 C5 Rh1 -61.85(11) . . . . ? C6 C1 C5 Rh1 122.25(17) . . . . ? C16 C11 C12 C13 0.9(3) . . . . ? N1 C11 C12 C13 177.96(16) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C16 -0.8(3) . . . . ? C14 C15 C16 C11 2.2(3) . . . . ? C14 C15 C16 N2 -174.98(17) . . . . ? C12 C11 C16 C15 -2.3(2) . . . . ? N1 C11 C16 C15 -179.52(15) . . . . ? C12 C11 C16 N2 175.25(15) . . . . ? N1 C11 C16 N2 -2.0(2) . . . . ? C22 C17 C18 C19 -0.5(3) . . . . ? S1 C17 C18 C19 -178.18(15) . . . . ? C17 C18 C19 C20 0.3(3) . . . . ? C18 C19 C20 C21 -0.1(3) . . . . ? C18 C19 C20 C23 179.95(19) . . . . ? C19 C20 C21 C22 0.3(3) . . . . ? C23 C20 C21 C22 -179.82(18) . . . . ? C20 C21 C22 C17 -0.5(3) . . . . ? C18 C17 C22 C21 0.6(3) . . . . ? S1 C17 C22 C21 178.35(14) . . . . ? C12 C11 N1 Rh1 -146.90(14) . . . . ? C16 C11 N1 Rh1 30.33(17) . . . . ? C15 C16 N2 S1 -25.7(2) . . . . ? C11 C16 N2 S1 157.06(12) . . . . ? C15 C16 N2 Rh1 149.48(15) . . . . ? C11 C16 N2 Rh1 -27.74(17) . . . . ? C16 N2 S1 O2 -176.68(12) . . . . ? Rh1 N2 S1 O2 9.06(13) . . . . ? C16 N2 S1 O1 53.44(15) . . . . ? Rh1 N2 S1 O1 -120.83(10) . . . . ? C16 N2 S1 C17 -61.61(15) . . . . ? Rh1 N2 S1 C17 124.12(10) . . . . ? C18 C17 S1 O2 -127.73(15) . . . . ? C22 C17 S1 O2 54.56(16) . . . . ? C18 C17 S1 O1 -2.37(17) . . . . ? C22 C17 S1 O1 179.91(14) . . . . ? C18 C17 S1 N2 117.62(15) . . . . ? C22 C17 S1 N2 -60.10(15) . . . . ? C5 C4 Rh1 C3 116.73(14) . . . . ? C9 C4 Rh1 C3 -121.61(18) . . . . ? C5 C4 Rh1 C1 36.71(10) . . . . ? C3 C4 Rh1 C1 -80.03(10) . . . . ? C9 C4 Rh1 C1 158.36(16) . . . . ? C5 C4 Rh1 N2 -71.19(11) . . . . ? C3 C4 Rh1 N2 172.08(9) . . . . ? C9 C4 Rh1 N2 50.47(15) . . . . ? C5 C4 Rh1 N1 -147.92(10) . . . . ? C3 C4 Rh1 N1 95.35(10) . . . . ? C9 C4 Rh1 N1 -26.27(15) . . . . ? C3 C4 Rh1 C5 -116.73(14) . . . . ? C9 C4 Rh1 C5 121.65(19) . . . . ? C5 C4 Rh1 C2 79.66(11) . . . . ? C3 C4 Rh1 C2 -37.07(9) . . . . ? C9 C4 Rh1 C2 -158.69(16) . . . . ? C5 C4 Rh1 Cl1 116.23(13) . . . . ? C3 C4 Rh1 Cl1 -0.50(18) . . . . ? C9 C4 Rh1 Cl1 -122.11(14) . . . . ? C2 C3 Rh1 C4 -118.34(14) . . . . ? C8 C3 Rh1 C4 119.77(19) . . . . ? C2 C3 Rh1 C1 -37.01(10) . . . . ? C4 C3 Rh1 C1 81.33(10) . . . . ? C8 C3 Rh1 C1 -158.90(17) . . . . ? C2 C3 Rh1 N2 -132.54(12) . . . . ? C4 C3 Rh1 N2 -14.20(16) . . . . ? C8 C3 Rh1 N2 105.57(16) . . . . ? C2 C3 Rh1 N1 149.35(10) . . . . ? C4 C3 Rh1 N1 -92.31(10) . . . . ? C8 C3 Rh1 N1 27.46(16) . . . . ? C2 C3 Rh1 C5 -80.11(11) . . . . ? C4 C3 Rh1 C5 38.23(10) . . . . ? C8 C3 Rh1 C5 158.00(17) . . . . ? C4 C3 Rh1 C2 118.34(14) . . . . ? C8 C3 Rh1 C2 -121.89(19) . . . . ? C2 C3 Rh1 Cl1 61.44(10) . . . . ? C4 C3 Rh1 Cl1 179.78(8) . . . . ? C8 C3 Rh1 Cl1 -60.45(16) . . . . ? C5 C1 Rh1 C4 -36.71(10) . . . . ? C2 C1 Rh1 C4 80.45(10) . . . . ? C6 C1 Rh1 C4 -157.61(18) . . . . ? C5 C1 Rh1 C3 -80.53(10) . . . . ? C2 C1 Rh1 C3 36.63(10) . . . . ? C6 C1 Rh1 C3 158.57(18) . . . . ? C5 C1 Rh1 N2 64.27(11) . . . . ? C2 C1 Rh1 N2 -178.56(9) . . . . ? C6 C1 Rh1 N2 -56.63(18) . . . . ? C5 C1 Rh1 N1 -55.0(3) . . . . ? C2 C1 Rh1 N1 62.1(3) . . . . ? C6 C1 Rh1 N1 -175.9(2) . . . . ? C2 C1 Rh1 C5 117.17(14) . . . . ? C6 C1 Rh1 C5 -120.9(2) . . . . ? C5 C1 Rh1 C2 -117.17(14) . . . . ? C6 C1 Rh1 C2 121.9(2) . . . . ? C5 C1 Rh1 Cl1 167.14(8) . . . . ? C2 C1 Rh1 Cl1 -75.69(10) . . . . ? C6 C1 Rh1 Cl1 46.25(17) . . . . ? C16 N2 Rh1 C4 -61.77(12) . . . . ? S1 N2 Rh1 C4 112.93(11) . . . . ? C16 N2 Rh1 C3 -52.22(17) . . . . ? S1 N2 Rh1 C3 122.48(12) . . . . ? C16 N2 Rh1 C1 -133.15(11) . . . . ? S1 N2 Rh1 C1 41.54(12) . . . . ? C16 N2 Rh1 N1 33.62(11) . . . . ? S1 N2 Rh1 N1 -151.68(12) . . . . ? C16 N2 Rh1 C5 -98.48(12) . . . . ? S1 N2 Rh1 C5 76.21(11) . . . . ? C16 N2 Rh1 C2 -135.10(13) . . . . ? S1 N2 Rh1 C2 39.59(19) . . . . ? C16 N2 Rh1 Cl1 115.33(11) . . . . ? S1 N2 Rh1 Cl1 -69.98(10) . . . . ? C11 N1 Rh1 C4 73.24(12) . . . . ? C11 N1 Rh1 C3 113.76(11) . . . . ? C11 N1 Rh1 C1 90.2(3) . . . . ? C11 N1 Rh1 N2 -33.53(11) . . . . ? C11 N1 Rh1 C5 46.78(14) . . . . ? C11 N1 Rh1 C2 139.40(11) . . . . ? C11 N1 Rh1 Cl1 -129.85(11) . . . . ? C1 C5 Rh1 C4 119.88(14) . . . . ? C10 C5 Rh1 C4 -119.6(2) . . . . ? C4 C5 Rh1 C3 -38.95(10) . . . . ? C1 C5 Rh1 C3 80.93(10) . . . . ? C10 C5 Rh1 C3 -158.58(18) . . . . ? C4 C5 Rh1 C1 -119.88(14) . . . . ? C10 C5 Rh1 C1 120.5(2) . . . . ? C4 C5 Rh1 N2 116.08(10) . . . . ? C1 C5 Rh1 N2 -124.04(10) . . . . ? C10 C5 Rh1 N2 -3.55(16) . . . . ? C4 C5 Rh1 N1 44.12(13) . . . . ? C1 C5 Rh1 N1 164.00(9) . . . . ? C10 C5 Rh1 N1 -75.51(18) . . . . ? C4 C5 Rh1 C2 -81.69(10) . . . . ? C1 C5 Rh1 C2 38.19(10) . . . . ? C10 C5 Rh1 C2 158.68(18) . . . . ? C4 C5 Rh1 Cl1 -141.78(9) . . . . ? C1 C5 Rh1 Cl1 -21.90(14) . . . . ? C10 C5 Rh1 Cl1 98.59(17) . . . . ? C3 C2 Rh1 C4 38.17(10) . . . . ? C1 C2 Rh1 C4 -81.35(11) . . . . ? C7 C2 Rh1 C4 159.69(17) . . . . ? C1 C2 Rh1 C3 -119.52(14) . . . . ? C7 C2 Rh1 C3 121.5(2) . . . . ? C3 C2 Rh1 C1 119.52(14) . . . . ? C7 C2 Rh1 C1 -119.0(2) . . . . ? C3 C2 Rh1 N2 122.37(13) . . . . ? C1 C2 Rh1 N2 2.84(18) . . . . ? C7 C2 Rh1 N2 -116.11(17) . . . . ? C3 C2 Rh1 N1 -42.81(13) . . . . ? C1 C2 Rh1 N1 -162.34(10) . . . . ? C7 C2 Rh1 N1 78.71(17) . . . . ? C3 C2 Rh1 C5 81.32(10) . . . . ? C1 C2 Rh1 C5 -38.20(10) . . . . ? C7 C2 Rh1 C5 -157.16(18) . . . . ? C3 C2 Rh1 Cl1 -128.28(9) . . . . ? C1 C2 Rh1 Cl1 112.19(9) . . . . ? C7 C2 Rh1 Cl1 -6.76(16) . . . . ? C28 C24 C25 C26 0.59(19) . . . . ? C29 C24 C25 C26 174.46(16) . . . . ? Rh2 C24 C25 C26 -61.12(12) . . . . ? C28 C24 C25 C30 -179.46(16) . . . . ? C29 C24 C25 C30 -5.6(3) . . . . ? Rh2 C24 C25 C30 118.83(17) . . . . ? C28 C24 C25 Rh2 61.71(12) . . . . ? C29 C24 C25 Rh2 -124.42(17) . . . . ? C24 C25 C26 C27 -0.07(19) . . . . ? C30 C25 C26 C27 179.99(16) . . . . ? Rh2 C25 C26 C27 -60.87(12) . . . . ? C24 C25 C26 C31 -179.60(17) . . . . ? C30 C25 C26 C31 0.5(3) . . . . ? Rh2 C25 C26 C31 119.60(18) . . . . ? C24 C25 C26 Rh2 60.80(12) . . . . ? C30 C25 C26 Rh2 -119.14(17) . . . . ? C25 C26 C27 C28 -0.5(2) . . . . ? C31 C26 C27 C28 179.05(17) . . . . ? Rh2 C26 C27 C28 -61.01(12) . . . . ? C25 C26 C27 C32 -175.89(17) . . . . ? C31 C26 C27 C32 3.7(3) . . . . ? Rh2 C26 C27 C32 123.59(19) . . . . ? C25 C26 C27 Rh2 60.52(12) . . . . ? C31 C26 C27 Rh2 -119.94(18) . . . . ? C26 C27 C28 C24 0.9(2) . . . . ? C32 C27 C28 C24 176.22(18) . . . . ? Rh2 C27 C28 C24 -59.63(12) . . . . ? C26 C27 C28 C33 179.36(17) . . . . ? C32 C27 C28 C33 -5.3(3) . . . . ? Rh2 C27 C28 C33 118.87(19) . . . . ? C26 C27 C28 Rh2 60.48(12) . . . . ? C32 C27 C28 Rh2 -124.15(19) . . . . ? C25 C24 C28 C27 -0.9(2) . . . . ? C29 C24 C28 C27 -174.64(17) . . . . ? Rh2 C24 C28 C27 60.14(12) . . . . ? C25 C24 C28 C33 -179.39(17) . . . . ? C29 C24 C28 C33 6.9(3) . . . . ? Rh2 C24 C28 C33 -118.36(19) . . . . ? C25 C24 C28 Rh2 -61.04(12) . . . . ? C29 C24 C28 Rh2 125.22(18) . . . . ? C39 C34 C35 C36 0.4(3) . . . . ? N3 C34 C35 C36 178.12(18) . . . . ? C34 C35 C36 C37 0.1(3) . . . . ? C35 C36 C37 C38 0.6(4) . . . . ? C36 C37 C38 C39 -1.8(3) . . . . ? C37 C38 C39 C34 2.2(3) . . . . ? C37 C38 C39 N4 -173.06(19) . . . . ? C35 C34 C39 C38 -1.5(3) . . . . ? N3 C34 C39 C38 -179.45(16) . . . . ? C35 C34 C39 N4 174.36(16) . . . . ? N3 C34 C39 N4 -3.6(2) . . . . ? C45 C40 C41 C42 -1.1(3) . . . . ? S2 C40 C41 C42 176.47(14) . . . . ? C40 C41 C42 C43 -0.7(3) . . . . ? C41 C42 C43 C44 2.5(3) . . . . ? C41 C42 C43 C46 -174.88(18) . . . . ? C42 C43 C44 C45 -2.5(3) . . . . ? C46 C43 C44 C45 174.95(19) . . . . ? C41 C40 C45 C44 1.2(3) . . . . ? S2 C40 C45 C44 -176.37(15) . . . . ? C43 C44 C45 C40 0.7(3) . . . . ? C35 C34 N3 Rh2 -143.44(15) . . . . ? C39 C34 N3 Rh2 34.47(18) . . . . ? C38 C39 N4 S2 -32.2(3) . . . . ? C34 C39 N4 S2 152.42(13) . . . . ? C38 C39 N4 Rh2 146.15(17) . . . . ? C34 C39 N4 Rh2 -29.26(18) . . . . ? C39 N4 S2 O4 -176.81(13) . . . . ? Rh2 N4 S2 O4 5.25(13) . . . . ? C39 N4 S2 O3 54.19(16) . . . . ? Rh2 N4 S2 O3 -123.75(10) . . . . ? C39 N4 S2 C40 -60.46(15) . . . . ? Rh2 N4 S2 C40 121.60(11) . . . . ? C45 C40 S2 O4 -128.05(16) . . . . ? C41 C40 S2 O4 54.37(16) . . . . ? C45 C40 S2 O3 -3.08(18) . . . . ? C41 C40 S2 O3 179.34(14) . . . . ? C45 C40 S2 N4 116.53(16) . . . . ? C41 C40 S2 N4 -61.05(16) . . . . ? C34 N3 Rh2 C25 79.15(12) . . . . ? C34 N3 Rh2 C24 118.20(12) . . . . ? C34 N3 Rh2 C26 46.83(14) . . . . ? C34 N3 Rh2 N4 -37.37(11) . . . . ? C34 N3 Rh2 C27 54.5(2) . . . . ? C34 N3 Rh2 C28 136.43(12) . . . . ? C34 N3 Rh2 Cl2 -132.60(11) . . . . ? C26 C25 Rh2 N3 -133.44(10) . . . . ? C24 C25 Rh2 N3 108.49(10) . . . . ? C30 C25 Rh2 N3 -11.82(16) . . . . ? C26 C25 Rh2 C24 118.07(15) . . . . ? C30 C25 Rh2 C24 -120.31(19) . . . . ? C24 C25 Rh2 C26 -118.07(15) . . . . ? C30 C25 Rh2 C26 121.6(2) . . . . ? C26 C25 Rh2 N4 -58.01(12) . . . . ? C24 C25 Rh2 N4 -176.08(9) . . . . ? C30 C25 Rh2 N4 63.61(16) . . . . ? C26 C25 Rh2 C27 37.67(10) . . . . ? C24 C25 Rh2 C27 -80.40(11) . . . . ? C30 C25 Rh2 C27 159.29(17) . . . . ? C26 C25 Rh2 C28 80.28(11) . . . . ? C24 C25 Rh2 C28 -37.79(10) . . . . ? C30 C25 Rh2 C28 -158.10(17) . . . . ? C26 C25 Rh2 Cl2 135.96(10) . . . . ? C24 C25 Rh2 Cl2 17.89(15) . . . . ? C30 C25 Rh2 Cl2 -102.43(16) . . . . ? C28 C24 Rh2 N3 162.64(10) . . . . ? C25 C24 Rh2 N3 -79.70(11) . . . . ? C29 C24 Rh2 N3 40.06(18) . . . . ? C28 C24 Rh2 C25 -117.67(15) . . . . ? C29 C24 Rh2 C25 119.8(2) . . . . ? C28 C24 Rh2 C26 -80.11(11) . . . . ? C25 C24 Rh2 C26 37.55(10) . . . . ? C29 C24 Rh2 C26 157.31(19) . . . . ? C28 C24 Rh2 N4 -108.88(16) . . . . ? C25 C24 Rh2 N4 8.8(2) . . . . ? C29 C24 Rh2 N4 128.55(17) . . . . ? C28 C24 Rh2 C27 -36.81(11) . . . . ? C25 C24 Rh2 C27 80.85(11) . . . . ? C29 C24 Rh2 C27 -159.39(19) . . . . ? C25 C24 Rh2 C28 117.67(15) . . . . ? C29 C24 Rh2 C28 -122.6(2) . . . . ? C28 C24 Rh2 Cl2 72.19(10) . . . . ? C25 C24 Rh2 Cl2 -170.14(8) . . . . ? C29 C24 Rh2 Cl2 -50.39(17) . . . . ? C25 C26 Rh2 N3 57.51(12) . . . . ? C27 C26 Rh2 N3 175.89(10) . . . . ? C31 C26 Rh2 N3 -63.68(18) . . . . ? C27 C26 Rh2 C25 118.38(15) . . . . ? C31 C26 Rh2 C25 -121.2(2) . . . . ? C25 C26 Rh2 C24 -38.00(10) . . . . ? C27 C26 Rh2 C24 80.38(11) . . . . ? C31 C26 Rh2 C24 -159.19(18) . . . . ? C25 C26 Rh2 N4 130.94(10) . . . . ? C27 C26 Rh2 N4 -110.68(10) . . . . ? C31 C26 Rh2 N4 9.75(16) . . . . ? C25 C26 Rh2 C27 -118.38(15) . . . . ? C31 C26 Rh2 C27 120.4(2) . . . . ? C25 C26 Rh2 C28 -81.09(11) . . . . ? C27 C26 Rh2 C28 37.29(10) . . . . ? C31 C26 Rh2 C28 157.72(18) . . . . ? C25 C26 Rh2 Cl2 -123.79(11) . . . . ? C27 C26 Rh2 Cl2 -5.41(17) . . . . ? C31 C26 Rh2 Cl2 115.02(16) . . . . ? C39 N4 Rh2 N3 36.72(11) . . . . ? S2 N4 Rh2 N3 -145.15(12) . . . . ? C39 N4 Rh2 C25 -52.45(13) . . . . ? S2 N4 Rh2 C25 125.68(11) . . . . ? C39 N4 Rh2 C24 -58.7(2) . . . . ? S2 N4 Rh2 C24 119.40(15) . . . . ? C39 N4 Rh2 C26 -84.80(12) . . . . ? S2 N4 Rh2 C26 93.33(11) . . . . ? C39 N4 Rh2 C27 -122.74(12) . . . . ? S2 N4 Rh2 C27 55.39(12) . . . . ? C39 N4 Rh2 C28 -137.16(12) . . . . ? S2 N4 Rh2 C28 40.97(16) . . . . ? C39 N4 Rh2 Cl2 120.27(11) . . . . ? S2 N4 Rh2 Cl2 -61.60(10) . . . . ? C28 C27 Rh2 N3 107.8(2) . . . . ? C26 C27 Rh2 N3 -10.4(2) . . . . ? C32 C27 Rh2 N3 -130.7(2) . . . . ? C28 C27 Rh2 C25 80.76(11) . . . . ? C26 C27 Rh2 C25 -37.45(10) . . . . ? C32 C27 Rh2 C25 -157.7(2) . . . . ? C28 C27 Rh2 C24 37.19(10) . . . . ? C26 C27 Rh2 C24 -81.02(11) . . . . ? C32 C27 Rh2 C24 158.7(2) . . . . ? C28 C27 Rh2 C26 118.21(15) . . . . ? C32 C27 Rh2 C26 -120.2(2) . . . . ? C28 C27 Rh2 N4 -165.96(10) . . . . ? C26 C27 Rh2 N4 75.84(10) . . . . ? C32 C27 Rh2 N4 -44.40(19) . . . . ? C26 C27 Rh2 C28 -118.21(15) . . . . ? C32 C27 Rh2 C28 121.6(2) . . . . ? C28 C27 Rh2 Cl2 -64.40(11) . . . . ? C26 C27 Rh2 Cl2 177.39(8) . . . . ? C32 C27 Rh2 Cl2 57.15(19) . . . . ? C27 C28 Rh2 N3 -147.59(11) . . . . ? C24 C28 Rh2 N3 -28.40(16) . . . . ? C33 C28 Rh2 N3 91.94(18) . . . . ? C27 C28 Rh2 C25 -80.97(11) . . . . ? C24 C28 Rh2 C25 38.22(10) . . . . ? C33 C28 Rh2 C25 158.57(18) . . . . ? C27 C28 Rh2 C24 -119.19(15) . . . . ? C33 C28 Rh2 C24 120.3(2) . . . . ? C27 C28 Rh2 C26 -37.88(10) . . . . ? C24 C28 Rh2 C26 81.32(11) . . . . ? C33 C28 Rh2 C26 -158.34(18) . . . . ? C27 C28 Rh2 N4 22.59(16) . . . . ? C24 C28 Rh2 N4 141.78(11) . . . . ? C33 C28 Rh2 N4 -97.88(18) . . . . ? C24 C28 Rh2 C27 119.19(15) . . . . ? C33 C28 Rh2 C27 -120.5(2) . . . . ? C27 C28 Rh2 Cl2 124.77(10) . . . . ? C24 C28 Rh2 Cl2 -116.04(10) . . . . ? C33 C28 Rh2 Cl2 4.31(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1B O3 0.85(2) 2.14(2) 2.9121(19) 151(2) 2_665 N3 H3B Cl2 0.84(3) 2.45(3) 3.2488(16) 160(2) 2_676 N1 H1A Cl1 0.81(3) 2.57(2) 3.0350(19) 117(2) . N3 H3A Cl2 0.83(3) 2.68(3) 3.0844(19) 112(2) . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.701 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.071