# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_berry266 _database_code_depnum_ccdc_archive 'CCDC 900048' #TrackingRef '13730_web_deposit_cif_file_0_KatherineKornecki_ #1346775504.Rh2(espn)2Cl_2,2isomer.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Rh2 (C16 H22 N2 O2)2 Cl, 3(C H2 Cl2)' _chemical_formula_sum 'C35 H50 Cl7 N4 O4 Rh2' _chemical_formula_weight 1044.76 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' Cl Cl 0.1484 0.1585 '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' 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 12.6948(6) _cell_length_b 13.6859(6) _cell_length_c 14.8577(7) _cell_angle_alpha 71.541(3) _cell_angle_beta 65.929(2) _cell_angle_gamma 66.835(3) _cell_volume 2129.04(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9829 _cell_measurement_theta_min 2.4466 _cell_measurement_theta_max 26.4555 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.6335 _exptl_absorpt_correction_T_max 0.8847 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed xray tube' _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '0.60\% \w and 0.6\% \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 8751 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8751 _reflns_number_gt 6646 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT Ver. 7.24A (Bruker-AXS, 2007)' _computing_data_reduction 'SAINT Ver. 7.24A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL, OLEX2 (Dolomanov et al., 2009)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0829P)^2^+8.8084P] 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 undef _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8751 _refine_ls_number_parameters 494 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1643 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.41727(4) 0.02103(4) 0.57588(4) 0.01883(16) Uani 1 1 d . . . Rh2 Rh 0.07509(4) 0.02000(4) 0.92032(3) 0.01837(15) Uani 1 1 d . . . Cl1 Cl 0.24055(14) 0.04651(15) 0.74577(11) 0.0278(4) Uani 1 1 d . . . Cl1S Cl 0.0187(2) 0.0862(2) 0.60389(19) 0.0501(5) Uani 1 1 d . . . Cl2S Cl -0.0523(2) 0.32096(19) 0.58041(16) 0.0501(6) Uani 1 1 d . . . Cl3S Cl 0.0737(4) 0.4955(4) 0.6410(3) 0.1237(17) Uani 1 1 d . . . Cl4S Cl 0.2387(2) 0.3542(2) 0.74947(18) 0.0513(5) Uani 1 1 d . . . Cl5S Cl 0.47012(18) -0.02554(17) 0.88596(16) 0.0407(5) Uani 1 1 d . . . Cl6S Cl 0.43800(18) 0.20082(17) 0.87348(15) 0.0392(5) Uani 1 1 d . . . O1 O 0.3322(4) 0.1554(4) 0.4930(3) 0.0244(10) Uani 1 1 d . . . O2 O 0.5036(4) 0.1072(4) 0.5943(3) 0.0238(10) Uani 1 1 d . . . O3 O -0.0549(4) 0.1511(4) 0.8798(3) 0.0227(10) Uani 1 1 d . . . O4 O 0.1118(4) 0.1115(4) 0.9825(3) 0.0230(10) Uani 1 1 d . . . N1 N 0.5101(5) -0.1112(5) 0.6460(4) 0.0253(12) Uani 1 1 d . . . H1 H 0.484(7) -0.129(7) 0.717(7) 0.03(2) Uiso 1 1 d . . . N2 N 0.3433(5) -0.0631(5) 0.5471(4) 0.0242(12) Uani 1 1 d . . . H2 H 0.273(8) -0.059(6) 0.577(6) 0.03(2) Uiso 1 1 d . . . N3 N 0.1926(5) -0.1095(5) 0.9703(4) 0.0225(12) Uani 1 1 d . . . H3 H 0.261(7) -0.130(6) 0.936(5) 0.014(18) Uiso 1 1 d . . . N4 N 0.0300(5) -0.0709(5) 0.8709(4) 0.0248(12) Uani 1 1 d . . . H4 H 0.067(8) -0.087(7) 0.813(7) 0.03(2) Uiso 1 1 d . . . C1 C 0.3852(6) 0.1752(6) 0.3978(5) 0.0247(14) Uani 1 1 d . . . C1S C 0.0399(7) 0.1947(7) 0.6266(6) 0.0394(19) Uani 1 1 d . . . H1SA H 0.1261 0.1921 0.5939 0.047 Uiso 1 1 calc R . . H1SB H 0.0201 0.1874 0.6997 0.047 Uiso 1 1 calc R . . C2 C 0.3167(6) 0.2754(6) 0.3379(5) 0.0298(16) Uani 1 1 d . . . C2S C 0.1434(9) 0.3575(11) 0.6926(7) 0.070(3) Uani 1 1 d . . . H2SA H 0.0800 0.3250 0.7422 0.084 Uiso 1 1 calc R . . H2SB H 0.1898 0.3147 0.6384 0.084 Uiso 1 1 calc R . . C3 C 0.2031(7) 0.2561(7) 0.3436(6) 0.0379(18) Uani 1 1 d . . . H3A H 0.1574 0.3196 0.3063 0.057 Uiso 1 1 calc R . . H3B H 0.1523 0.2435 0.4139 0.057 Uiso 1 1 calc R . . H3C H 0.2267 0.1926 0.3143 0.057 Uiso 1 1 calc R . . C3S C 0.3927(7) 0.1120(6) 0.8426(6) 0.0313(16) Uani 1 1 d . . . H3SA H 0.4120 0.1250 0.7690 0.038 Uiso 1 1 calc R . . H3SB H 0.3041 0.1256 0.8742 0.038 Uiso 1 1 calc R . . C4 C 0.3937(7) 0.2982(7) 0.2271(5) 0.0370(18) Uani 1 1 d . . . H4A H 0.4651 0.3134 0.2226 0.055 Uiso 1 1 calc R . . H4B H 0.3455 0.3608 0.1911 0.055 Uiso 1 1 calc R . . H4C H 0.4196 0.2348 0.1971 0.055 Uiso 1 1 calc R . . C5 C 0.2800(7) 0.3738(7) 0.3865(6) 0.0354(18) Uani 1 1 d . . . H5A H 0.2363 0.4388 0.3476 0.043 Uiso 1 1 calc R . . H5B H 0.2228 0.3616 0.4552 0.043 Uiso 1 1 calc R . . C6 C 0.3838(7) 0.3964(6) 0.3924(6) 0.0342(17) Uani 1 1 d . . . C7 C 0.4287(7) 0.3417(6) 0.4734(5) 0.0314(16) Uani 1 1 d . . . H7 H 0.3892 0.2940 0.5259 0.038 Uiso 1 1 calc R . . C8 C 0.5283(7) 0.3550(6) 0.4789(5) 0.0317(16) Uani 1 1 d . . . C9 C 0.5831(8) 0.4282(7) 0.4025(6) 0.041(2) Uani 1 1 d . . . H9 H 0.6500 0.4406 0.4055 0.050 Uiso 1 1 calc R . . C10 C 0.5406(9) 0.4814(7) 0.3242(7) 0.048(2) Uani 1 1 d . . . H10 H 0.5788 0.5304 0.2724 0.057 Uiso 1 1 calc R . . C11 C 0.4424(8) 0.4654(7) 0.3185(6) 0.043(2) Uani 1 1 d . . . H11 H 0.4152 0.5028 0.2623 0.052 Uiso 1 1 calc R . . C12 C 0.5761(7) 0.2905(7) 0.5654(6) 0.0338(17) Uani 1 1 d . . . H12A H 0.5068 0.2814 0.6268 0.041 Uiso 1 1 calc R . . H12B H 0.6162 0.3322 0.5772 0.041 Uiso 1 1 calc R . . C13 C 0.6679(6) 0.1764(7) 0.5478(5) 0.0302(16) Uani 1 1 d . . . C14 C 0.7026(7) 0.1143(7) 0.6433(6) 0.0367(18) Uani 1 1 d . . . H14A H 0.6305 0.1021 0.6986 0.055 Uiso 1 1 calc R . . H14B H 0.7356 0.1567 0.6610 0.055 Uiso 1 1 calc R . . H14C H 0.7638 0.0445 0.6308 0.055 Uiso 1 1 calc R . . C15 C 0.7820(6) 0.1902(7) 0.4604(6) 0.0340(18) Uani 1 1 d . . . H15A H 0.8155 0.2351 0.4744 0.051 Uiso 1 1 calc R . . H15B H 0.7613 0.2253 0.3986 0.051 Uiso 1 1 calc R . . H15C H 0.8423 0.1191 0.4522 0.051 Uiso 1 1 calc R . . C16 C 0.3933(6) -0.1132(6) 0.4706(5) 0.0253(15) Uani 1 1 d . . . C17 C -0.1641(6) 0.1705(5) 0.9421(5) 0.0210(13) Uani 1 1 d . . . C18 C -0.2578(6) 0.2685(6) 0.9052(5) 0.0256(15) Uani 1 1 d . . . C19 C -0.2762(7) 0.2410(7) 0.8208(6) 0.0323(16) Uani 1 1 d . . . H19A H -0.1989 0.2243 0.7665 0.049 Uiso 1 1 calc R . . H19B H -0.3353 0.3031 0.7947 0.049 Uiso 1 1 calc R . . H19C H -0.3063 0.1782 0.8474 0.049 Uiso 1 1 calc R . . C20 C -0.3802(6) 0.2957(6) 0.9880(6) 0.0326(17) Uani 1 1 d . . . H20A H -0.4357 0.3616 0.9621 0.049 Uiso 1 1 calc R . . H20B H -0.3690 0.3073 1.0450 0.049 Uiso 1 1 calc R . . H20C H -0.4141 0.2358 1.0100 0.049 Uiso 1 1 calc R . . C21 C -0.2087(6) 0.3682(6) 0.8625(5) 0.0268(15) Uani 1 1 d . . . H21A H -0.1343 0.3521 0.8042 0.032 Uiso 1 1 calc R . . H21B H -0.2697 0.4311 0.8380 0.032 Uiso 1 1 calc R . . C22 C -0.1800(6) 0.3990(6) 0.9377(5) 0.0272(15) Uani 1 1 d . . . C23 C -0.2618(7) 0.4757(6) 0.9934(6) 0.0349(17) Uani 1 1 d . . . H23 H -0.3387 0.5132 0.9844 0.042 Uiso 1 1 calc R . . C24 C -0.2326(7) 0.4994(6) 1.0636(6) 0.0364(18) Uani 1 1 d . . . H24 H -0.2890 0.5549 1.1002 0.044 Uiso 1 1 calc R . . C25 C -0.1246(7) 0.4439(6) 1.0806(6) 0.0346(17) Uani 1 1 d . . . H25 H -0.1077 0.4600 1.1300 0.041 Uiso 1 1 calc R . . C26 C -0.0394(6) 0.3644(6) 1.0263(5) 0.0269(15) Uani 1 1 d . . . C27 C -0.0679(6) 0.3450(6) 0.9534(5) 0.0273(15) Uani 1 1 d . . . H27 H -0.0092 0.2934 0.9132 0.033 Uiso 1 1 calc R . . C28 C 0.0798(7) 0.3013(6) 1.0436(5) 0.0292(16) Uani 1 1 d . . . H28A H 0.1008 0.3460 1.0708 0.035 Uiso 1 1 calc R . . H28B H 0.1428 0.2888 0.9780 0.035 Uiso 1 1 calc R . . C29 C 0.0839(6) 0.1898(6) 1.1163(5) 0.0276(16) Uani 1 1 d . . . C30 C -0.0056(7) 0.2090(7) 1.2206(5) 0.0323(17) Uani 1 1 d . . . H30A H -0.0885 0.2372 1.2183 0.048 Uiso 1 1 calc R . . H30B H 0.0105 0.2615 1.2414 0.048 Uiso 1 1 calc R . . H30C H 0.0041 0.1406 1.2688 0.048 Uiso 1 1 calc R . . C31 C 0.2113(7) 0.1314(7) 1.1220(6) 0.0338(17) Uani 1 1 d . . . H31A H 0.2388 0.1793 1.1383 0.051 Uiso 1 1 calc R . . H31B H 0.2661 0.1112 1.0571 0.051 Uiso 1 1 calc R . . H31C H 0.2110 0.0662 1.1741 0.051 Uiso 1 1 calc R . . C32 C -0.0507(6) -0.1210(6) 0.9253(5) 0.0215(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0179(3) 0.0242(3) 0.0129(2) -0.00059(19) -0.00116(19) -0.0112(2) Rh2 0.0170(3) 0.0233(3) 0.0134(3) -0.00102(19) -0.00068(19) -0.0109(2) Cl1 0.0206(8) 0.0463(10) 0.0145(7) -0.0036(7) 0.0015(6) -0.0172(7) Cl1S 0.0369(11) 0.0542(13) 0.0590(14) -0.0100(11) -0.0142(10) -0.0155(10) Cl2S 0.0444(12) 0.0521(13) 0.0312(10) 0.0020(9) -0.0049(9) -0.0073(10) Cl3S 0.115(3) 0.109(3) 0.105(3) -0.003(3) -0.063(3) 0.023(3) Cl4S 0.0477(13) 0.0600(14) 0.0446(12) -0.0089(10) -0.0097(10) -0.0212(11) Cl5S 0.0365(10) 0.0450(11) 0.0421(11) -0.0047(9) -0.0123(8) -0.0171(9) Cl6S 0.0371(10) 0.0525(12) 0.0349(10) -0.0136(9) -0.0004(8) -0.0280(9) O1 0.024(2) 0.030(3) 0.016(2) 0.0026(19) -0.0035(19) -0.013(2) O2 0.021(2) 0.038(3) 0.016(2) -0.0036(19) 0.0010(18) -0.020(2) O3 0.020(2) 0.026(3) 0.019(2) 0.0007(18) -0.0039(18) -0.0103(19) O4 0.020(2) 0.033(3) 0.017(2) -0.0064(19) 0.0000(18) -0.014(2) N1 0.022(3) 0.033(3) 0.016(3) 0.000(2) -0.001(2) -0.012(2) N2 0.018(3) 0.035(3) 0.021(3) -0.007(2) 0.000(2) -0.015(2) N3 0.017(3) 0.024(3) 0.022(3) -0.002(2) 0.000(2) -0.009(2) N4 0.024(3) 0.039(4) 0.014(3) -0.005(2) -0.002(2) -0.017(3) C1 0.023(3) 0.033(4) 0.017(3) 0.000(3) -0.002(3) -0.017(3) C1S 0.031(4) 0.052(5) 0.030(4) -0.004(4) -0.002(3) -0.018(4) C2 0.025(4) 0.037(4) 0.018(3) -0.001(3) -0.003(3) -0.007(3) C2S 0.053(6) 0.126(11) 0.037(5) -0.027(6) 0.014(5) -0.054(7) C3 0.030(4) 0.055(5) 0.026(4) -0.009(4) -0.010(3) -0.009(4) C3S 0.027(4) 0.044(4) 0.028(4) -0.010(3) -0.003(3) -0.019(3) C4 0.040(4) 0.036(4) 0.018(3) -0.001(3) -0.001(3) -0.006(3) C5 0.034(4) 0.037(4) 0.023(4) -0.003(3) -0.005(3) -0.005(3) C6 0.040(4) 0.024(4) 0.026(4) -0.004(3) -0.003(3) -0.008(3) C7 0.032(4) 0.032(4) 0.023(4) -0.008(3) 0.004(3) -0.015(3) C8 0.036(4) 0.032(4) 0.025(4) -0.013(3) 0.003(3) -0.016(3) C9 0.040(5) 0.038(5) 0.043(5) -0.015(4) 0.005(4) -0.021(4) C10 0.059(6) 0.037(5) 0.037(5) -0.001(4) 0.002(4) -0.026(4) C11 0.052(5) 0.037(5) 0.031(4) -0.001(3) -0.008(4) -0.015(4) C12 0.032(4) 0.044(4) 0.031(4) -0.013(3) 0.000(3) -0.023(3) C13 0.026(4) 0.047(5) 0.022(3) -0.011(3) 0.005(3) -0.025(3) C14 0.027(4) 0.058(5) 0.032(4) -0.015(4) -0.001(3) -0.023(4) C15 0.023(4) 0.058(5) 0.027(4) -0.019(3) 0.007(3) -0.025(3) C16 0.020(3) 0.040(4) 0.018(3) -0.010(3) 0.001(3) -0.015(3) C17 0.014(3) 0.028(3) 0.019(3) -0.002(3) -0.003(2) -0.009(3) C18 0.020(3) 0.032(4) 0.019(3) 0.002(3) -0.001(3) -0.012(3) C19 0.025(4) 0.041(4) 0.031(4) 0.005(3) -0.012(3) -0.016(3) C20 0.019(3) 0.036(4) 0.034(4) 0.001(3) -0.003(3) -0.010(3) C21 0.020(3) 0.031(4) 0.022(3) 0.000(3) -0.002(3) -0.011(3) C22 0.032(4) 0.025(4) 0.019(3) 0.007(3) -0.005(3) -0.016(3) C23 0.029(4) 0.034(4) 0.029(4) -0.003(3) 0.001(3) -0.010(3) C24 0.035(4) 0.035(4) 0.029(4) -0.011(3) 0.003(3) -0.012(3) C25 0.044(5) 0.037(4) 0.026(4) -0.007(3) -0.003(3) -0.024(4) C26 0.031(4) 0.029(4) 0.020(3) 0.001(3) 0.000(3) -0.021(3) C27 0.028(4) 0.031(4) 0.022(3) -0.003(3) -0.001(3) -0.018(3) C28 0.037(4) 0.037(4) 0.019(3) -0.003(3) -0.003(3) -0.025(3) C29 0.027(4) 0.044(4) 0.014(3) -0.009(3) 0.003(3) -0.020(3) C30 0.038(4) 0.046(5) 0.016(3) -0.007(3) 0.002(3) -0.026(4) C31 0.034(4) 0.050(5) 0.023(4) -0.006(3) -0.006(3) -0.024(4) C32 0.024(3) 0.031(4) 0.013(3) 0.000(3) -0.006(2) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N2 1.970(6) . ? Rh1 N1 1.970(6) . ? Rh1 O2 2.033(5) . ? Rh1 O1 2.038(5) . ? Rh1 Rh1 2.4155(9) 2_656 ? Rh1 Cl1 2.6170(16) . ? Rh2 N4 1.974(6) . ? Rh2 N3 1.977(6) . ? Rh2 O3 2.026(5) . ? Rh2 O4 2.044(5) . ? Rh2 Rh2 2.4204(9) 2_557 ? Rh2 Cl1 2.6134(15) . ? Cl1S C1S 1.761(9) . ? Cl2S C1S 1.772(9) . ? Cl3S C2S 1.806(14) . ? Cl4S C2S 1.715(11) . ? Cl5S C3S 1.793(8) . ? Cl6S C3S 1.771(7) . ? O1 C1 1.284(8) . ? O2 C16 1.286(8) 2_656 ? O3 C17 1.291(8) . ? O4 C32 1.290(8) 2_557 ? N1 C1 1.303(9) 2_656 ? N1 H1 0.94(9) . ? N2 C16 1.314(9) . ? N2 H2 0.81(8) . ? N3 C17 1.299(9) 2_557 ? N3 H3 0.79(7) . ? N4 C32 1.304(9) . ? N4 H4 0.85(9) . ? C1 N1 1.303(9) 2_656 ? C1 C2 1.534(10) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2 C3 1.531(11) . ? C2 C4 1.537(9) . ? C2 C5 1.548(11) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3S H3SA 0.9900 . ? C3S H3SB 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.509(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C11 1.371(11) . ? C6 C7 1.409(11) . ? C7 C8 1.384(11) . ? C7 H7 0.9500 . ? C8 C9 1.399(11) . ? C8 C12 1.515(11) . ? C9 C10 1.357(13) . ? C9 H9 0.9500 . ? C10 C11 1.387(13) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.563(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C16 1.511(10) 2_656 ? C13 C15 1.532(9) . ? C13 C14 1.543(11) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O2 1.286(8) 2_656 ? C16 C13 1.511(10) 2_656 ? C17 N3 1.299(9) 2_557 ? C17 C18 1.524(9) . ? C18 C20 1.530(9) . ? C18 C19 1.543(11) . ? C18 C21 1.565(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.520(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.363(11) . ? C22 C27 1.399(10) . ? C23 C24 1.398(12) . ? C23 H23 0.9500 . ? C24 C25 1.365(12) . ? C24 H24 0.9500 . ? C25 C26 1.387(11) . ? C25 H25 0.9500 . ? C26 C27 1.398(10) . ? C26 C28 1.499(11) . ? C27 H27 0.9500 . ? C28 C29 1.562(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C31 1.520(11) . ? C29 C32 1.529(9) 2_557 ? C29 C30 1.532(9) . ? 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 O4 1.290(8) 2_557 ? C32 C29 1.529(9) 2_557 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 N1 91.1(3) . . ? N2 Rh1 O2 175.4(2) . . ? N1 Rh1 O2 89.5(2) . . ? N2 Rh1 O1 88.7(2) . . ? N1 Rh1 O1 175.5(2) . . ? O2 Rh1 O1 90.4(2) . . ? N2 Rh1 Rh1 86.24(17) . 2_656 ? N1 Rh1 Rh1 86.20(17) . 2_656 ? O2 Rh1 Rh1 89.21(12) . 2_656 ? O1 Rh1 Rh1 89.27(13) . 2_656 ? N2 Rh1 Cl1 90.32(17) . . ? N1 Rh1 Cl1 89.51(17) . . ? O2 Rh1 Cl1 94.28(13) . . ? O1 Rh1 Cl1 95.01(13) . . ? Rh1 Rh1 Cl1 174.45(5) 2_656 . ? N4 Rh2 N3 90.4(3) . . ? N4 Rh2 O3 89.8(2) . . ? N3 Rh2 O3 175.5(2) . . ? N4 Rh2 O4 175.4(2) . . ? N3 Rh2 O4 89.3(2) . . ? O3 Rh2 O4 90.2(2) . . ? N4 Rh2 Rh2 86.38(17) . 2_557 ? N3 Rh2 Rh2 86.42(17) . 2_557 ? O3 Rh2 Rh2 89.16(12) . 2_557 ? O4 Rh2 Rh2 89.03(12) . 2_557 ? N4 Rh2 Cl1 89.39(17) . . ? N3 Rh2 Cl1 90.99(17) . . ? O3 Rh2 Cl1 93.46(13) . . ? O4 Rh2 Cl1 95.20(13) . . ? Rh2 Rh2 Cl1 175.01(5) 2_557 . ? Rh2 Cl1 Rh1 165.62(8) . . ? C1 O1 Rh1 118.3(4) . . ? C16 O2 Rh1 119.1(4) 2_656 . ? C17 O3 Rh2 118.5(4) . . ? C32 O4 Rh2 118.5(4) 2_557 . ? C1 N1 Rh1 124.5(5) 2_656 . ? C1 N1 H1 115(5) 2_656 . ? Rh1 N1 H1 121(5) . . ? C16 N2 Rh1 124.8(5) . . ? C16 N2 H2 115(6) . . ? Rh1 N2 H2 120(6) . . ? C17 N3 Rh2 123.7(5) 2_557 . ? C17 N3 H3 115(5) 2_557 . ? Rh2 N3 H3 121(5) . . ? C32 N4 Rh2 124.6(5) . . ? C32 N4 H4 112(6) . . ? Rh2 N4 H4 123(6) . . ? O1 C1 N1 121.7(6) . 2_656 ? O1 C1 C2 116.6(6) . . ? N1 C1 C2 121.6(6) 2_656 . ? Cl1S C1S Cl2S 111.5(5) . . ? Cl1S C1S H1SA 109.3 . . ? Cl2S C1S H1SA 109.3 . . ? Cl1S C1S H1SB 109.3 . . ? Cl2S C1S H1SB 109.3 . . ? H1SA C1S H1SB 108.0 . . ? C3 C2 C1 108.2(6) . . ? C3 C2 C4 108.9(6) . . ? C1 C2 C4 112.2(6) . . ? C3 C2 C5 109.8(6) . . ? C1 C2 C5 108.2(6) . . ? C4 C2 C5 109.5(6) . . ? Cl4S C2S Cl3S 110.0(7) . . ? Cl4S C2S H2SA 109.7 . . ? Cl3S C2S H2SA 109.7 . . ? Cl4S C2S H2SB 109.7 . . ? Cl3S C2S H2SB 109.7 . . ? H2SA C2S H2SB 108.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Cl6S C3S Cl5S 109.8(4) . . ? Cl6S C3S H3SA 109.7 . . ? Cl5S C3S H3SA 109.7 . . ? Cl6S C3S H3SB 109.7 . . ? Cl5S C3S H3SB 109.7 . . ? H3SA C3S H3SB 108.2 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C2 115.0(6) . . ? C6 C5 H5A 108.5 . . ? C2 C5 H5A 108.5 . . ? C6 C5 H5B 108.5 . . ? C2 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C11 C6 C7 117.2(8) . . ? C11 C6 C5 122.5(8) . . ? C7 C6 C5 120.2(7) . . ? C8 C7 C6 122.3(7) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? C7 C8 C9 118.2(8) . . ? C7 C8 C12 120.1(7) . . ? C9 C8 C12 121.7(7) . . ? C10 C9 C8 120.0(8) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 121.2(8) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C6 C11 C10 121.1(8) . . ? C6 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C8 C12 C13 113.8(6) . . ? C8 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? C8 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C16 C13 C15 112.8(6) 2_656 . ? C16 C13 C14 107.4(6) 2_656 . ? C15 C13 C14 109.2(6) . . ? C16 C13 C12 108.7(6) 2_656 . ? C15 C13 C12 109.2(6) . . ? C14 C13 C12 109.6(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 N2 120.6(6) 2_656 . ? O2 C16 C13 116.9(6) 2_656 2_656 ? N2 C16 C13 122.4(6) . 2_656 ? O3 C17 N3 122.2(6) . 2_557 ? O3 C17 C18 115.6(5) . . ? N3 C17 C18 122.2(6) 2_557 . ? C17 C18 C20 112.4(6) . . ? C17 C18 C19 107.5(6) . . ? C20 C18 C19 108.3(6) . . ? C17 C18 C21 109.3(5) . . ? C20 C18 C21 109.8(6) . . ? C19 C18 C21 109.5(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C18 114.3(6) . . ? C22 C21 H21A 108.7 . . ? C18 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? C18 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C27 118.3(7) . . ? C23 C22 C21 122.0(7) . . ? C27 C22 C21 119.6(7) . . ? C22 C23 C24 120.0(8) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 121.1(7) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.6(7) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 C27 117.5(7) . . ? C25 C26 C28 122.0(7) . . ? C27 C26 C28 120.5(7) . . ? C26 C27 C22 122.3(7) . . ? C26 C27 H27 118.8 . . ? C22 C27 H27 118.8 . . ? C26 C28 C29 115.3(6) . . ? C26 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? C26 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C31 C29 C32 108.5(6) . 2_557 ? C31 C29 C30 110.0(6) . . ? C32 C29 C30 111.1(6) 2_557 . ? C31 C29 C28 109.9(6) . . ? C32 C29 C28 108.5(6) 2_557 . ? C30 C29 C28 108.9(6) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 C32 N4 121.4(6) 2_557 . ? O4 C32 C29 115.6(5) 2_557 2_557 ? N4 C32 C29 122.9(6) . 2_557 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Rh2 Cl1 Rh1 -43.9(3) . . . . ? N3 Rh2 Cl1 Rh1 46.5(3) . . . . ? O3 Rh2 Cl1 Rh1 -133.7(3) . . . . ? O4 Rh2 Cl1 Rh1 135.8(3) . . . . ? Rh2 Rh2 Cl1 Rh1 -12.1(8) 2_557 . . . ? N2 Rh1 Cl1 Rh2 46.9(3) . . . . ? N1 Rh1 Cl1 Rh2 -44.1(3) . . . . ? O2 Rh1 Cl1 Rh2 -133.5(3) . . . . ? O1 Rh1 Cl1 Rh2 135.6(3) . . . . ? Rh1 Rh1 Cl1 Rh2 -4.7(8) 2_656 . . . ? N2 Rh1 O1 C1 -86.6(5) . . . . ? N1 Rh1 O1 C1 0(3) . . . . ? O2 Rh1 O1 C1 88.8(5) . . . . ? Rh1 Rh1 O1 C1 -0.4(5) 2_656 . . . ? Cl1 Rh1 O1 C1 -176.8(5) . . . . ? N2 Rh1 O2 C16 -10(3) . . . 2_656 ? N1 Rh1 O2 C16 86.0(5) . . . 2_656 ? O1 Rh1 O2 C16 -89.5(5) . . . 2_656 ? Rh1 Rh1 O2 C16 -0.2(5) 2_656 . . 2_656 ? Cl1 Rh1 O2 C16 175.5(5) . . . 2_656 ? N4 Rh2 O3 C17 85.6(5) . . . . ? N3 Rh2 O3 C17 -7(3) . . . . ? O4 Rh2 O3 C17 -89.8(5) . . . . ? Rh2 Rh2 O3 C17 -0.7(5) 2_557 . . . ? Cl1 Rh2 O3 C17 175.0(5) . . . . ? N4 Rh2 O4 C32 -2(3) . . . 2_557 ? N3 Rh2 O4 C32 -87.6(5) . . . 2_557 ? O3 Rh2 O4 C32 88.0(5) . . . 2_557 ? Rh2 Rh2 O4 C32 -1.2(5) 2_557 . . 2_557 ? Cl1 Rh2 O4 C32 -178.5(5) . . . 2_557 ? N2 Rh1 N1 C1 85.7(6) . . . 2_656 ? O2 Rh1 N1 C1 -89.7(6) . . . 2_656 ? O1 Rh1 N1 C1 -1(3) . . . 2_656 ? Rh1 Rh1 N1 C1 -0.5(6) 2_656 . . 2_656 ? Cl1 Rh1 N1 C1 176.0(6) . . . 2_656 ? N1 Rh1 N2 C16 -84.3(6) . . . . ? O2 Rh1 N2 C16 12(3) . . . . ? O1 Rh1 N2 C16 91.1(6) . . . . ? Rh1 Rh1 N2 C16 1.8(6) 2_656 . . . ? Cl1 Rh1 N2 C16 -173.9(6) . . . . ? N4 Rh2 N3 C17 -85.9(6) . . . 2_557 ? O3 Rh2 N3 C17 7(3) . . . 2_557 ? O4 Rh2 N3 C17 89.5(6) . . . 2_557 ? Rh2 Rh2 N3 C17 0.4(6) 2_557 . . 2_557 ? Cl1 Rh2 N3 C17 -175.3(6) . . . 2_557 ? N3 Rh2 N4 C32 85.3(6) . . . . ? O3 Rh2 N4 C32 -90.3(6) . . . . ? O4 Rh2 N4 C32 0(3) . . . . ? Rh2 Rh2 N4 C32 -1.1(6) 2_557 . . . ? Cl1 Rh2 N4 C32 176.3(6) . . . . ? Rh1 O1 C1 N1 0.8(9) . . . 2_656 ? Rh1 O1 C1 C2 178.5(5) . . . . ? O1 C1 C2 C3 -66.0(8) . . . . ? N1 C1 C2 C3 111.7(7) 2_656 . . . ? O1 C1 C2 C4 173.9(7) . . . . ? N1 C1 C2 C4 -8.5(10) 2_656 . . . ? O1 C1 C2 C5 53.0(8) . . . . ? N1 C1 C2 C5 -129.4(7) 2_656 . . . ? C3 C2 C5 C6 175.7(6) . . . . ? C1 C2 C5 C6 57.8(8) . . . . ? C4 C2 C5 C6 -64.7(8) . . . . ? C2 C5 C6 C11 91.5(9) . . . . ? C2 C5 C6 C7 -85.0(9) . . . . ? C11 C6 C7 C8 -0.6(11) . . . . ? C5 C6 C7 C8 176.0(7) . . . . ? C6 C7 C8 C9 2.1(11) . . . . ? C6 C7 C8 C12 -177.4(7) . . . . ? C7 C8 C9 C10 -2.0(12) . . . . ? C12 C8 C9 C10 177.5(8) . . . . ? C8 C9 C10 C11 0.5(13) . . . . ? C7 C6 C11 C10 -0.9(12) . . . . ? C5 C6 C11 C10 -177.5(8) . . . . ? C9 C10 C11 C6 1.0(14) . . . . ? C7 C8 C12 C13 86.2(8) . . . . ? C9 C8 C12 C13 -93.2(8) . . . . ? C8 C12 C13 C16 -58.3(8) . . . 2_656 ? C8 C12 C13 C15 65.1(8) . . . . ? C8 C12 C13 C14 -175.4(6) . . . . ? Rh1 N2 C16 O2 -2.1(10) . . . 2_656 ? Rh1 N2 C16 C13 -179.8(5) . . . 2_656 ? Rh2 O3 C17 N3 0.6(9) . . . 2_557 ? Rh2 O3 C17 C18 -178.2(4) . . . . ? O3 C17 C18 C20 -171.8(6) . . . . ? N3 C17 C18 C20 9.4(10) 2_557 . . . ? O3 C17 C18 C19 69.2(7) . . . . ? N3 C17 C18 C19 -109.7(7) 2_557 . . . ? O3 C17 C18 C21 -49.6(8) . . . . ? N3 C17 C18 C21 131.6(7) 2_557 . . . ? C17 C18 C21 C22 -59.1(8) . . . . ? C20 C18 C21 C22 64.6(8) . . . . ? C19 C18 C21 C22 -176.7(6) . . . . ? C18 C21 C22 C23 -94.2(8) . . . . ? C18 C21 C22 C27 83.6(8) . . . . ? C27 C22 C23 C24 0.4(11) . . . . ? C21 C22 C23 C24 178.2(6) . . . . ? C22 C23 C24 C25 -2.4(12) . . . . ? C23 C24 C25 C26 1.8(12) . . . . ? C24 C25 C26 C27 0.9(10) . . . . ? C24 C25 C26 C28 -179.5(7) . . . . ? C25 C26 C27 C22 -3.0(10) . . . . ? C28 C26 C27 C22 177.4(6) . . . . ? C23 C22 C27 C26 2.4(10) . . . . ? C21 C22 C27 C26 -175.5(6) . . . . ? C25 C26 C28 C29 95.5(8) . . . . ? C27 C26 C28 C29 -84.9(8) . . . . ? C26 C28 C29 C31 176.4(6) . . . . ? C26 C28 C29 C32 57.9(8) . . . 2_557 ? C26 C28 C29 C30 -63.1(8) . . . . ? Rh2 N4 C32 O4 2.4(10) . . . 2_557 ? Rh2 N4 C32 C29 179.3(5) . . . 2_557 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.665 _refine_diff_density_min -1.376 _refine_diff_density_rms 0.205 data_berry276 _database_code_depnum_ccdc_archive 'CCDC 900049' #TrackingRef 'web_deposit_cif_file_1_KatherineKornecki_1346775504.Rh2(espn)2Cl_4,0isomer.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Rh2 (C16 H22 N2 O2)2 Cl, 2(C H2 Cl2)' _chemical_formula_sum 'C34 H48 Cl5 N4 O4 Rh2' _chemical_formula_weight 959.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c 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 13.2750(3) _cell_length_b 12.8783(3) _cell_length_c 23.4841(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.6270(10) _cell_angle_gamma 90.00 _cell_volume 3884.71(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 2.2394 _cell_measurement_theta_max 24.6763 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.236 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed xray tube' _diffrn_radiation_monochromator 'mirror optics' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '0.60\% \w and 0.6\% \f scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 71139 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 24.76 _reflns_number_total 6654 _reflns_number_gt 4916 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)' _computing_cell_refinement 'SAINT Ver. 7.24A (Bruker-AXS, 2007)' _computing_data_reduction 'SAINT Ver. 7.24A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL, OLEX2 (Dolomanov et al., 2009)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6654 _refine_ls_number_parameters 462 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.76900(2) 0.52004(2) 0.095681(12) 0.01372(8) Uani 1 1 d . . . Rh2 Rh 0.87051(2) 0.58282(2) 0.189516(12) 0.01420(8) Uani 1 1 d . . . Cl1 Cl 0.67178(7) 0.45396(7) 0.00151(4) 0.0233(2) Uani 1 1 d . . . Cl1S Cl 1.14602(10) 0.80167(9) -0.04018(5) 0.0477(3) Uani 1 1 d . . . Cl2S Cl 1.22546(9) 0.86872(12) 0.08010(5) 0.0689(4) Uani 1 1 d . . . Cl3S Cl 0.56052(10) 0.81421(12) 0.37740(6) 0.0701(4) Uani 1 1 d . . . Cl4S Cl 0.49325(11) 0.73019(10) 0.47661(7) 0.0697(4) Uani 1 1 d . . . O1 O 0.88257(19) 0.71846(18) 0.15030(11) 0.0269(6) Uani 1 1 d . . . O2 O 0.73942(18) 0.62613(18) 0.20811(11) 0.0263(6) Uani 1 1 d . . . O3 O 0.85296(18) 0.44327(18) 0.22424(10) 0.0198(6) Uani 1 1 d . . . O4 O 1.00006(17) 0.53343(17) 0.16922(10) 0.0158(5) Uani 1 1 d . . . N1 N 0.7837(2) 0.6616(2) 0.06254(12) 0.0113(6) Uani 1 1 d D . . H1 H 0.753(2) 0.674(3) 0.0330(9) 0.017 Uiso 1 1 d D . . N2 N 0.6423(2) 0.5718(2) 0.12002(12) 0.0098(6) Uani 1 1 d D . . H2 H 0.5915(17) 0.570(3) 0.0975(12) 0.015 Uiso 1 1 d D . . N3 N 0.7601(2) 0.3851(2) 0.13550(12) 0.0136(7) Uani 1 1 d D . . H3 H 0.732(2) 0.3327(19) 0.1200(14) 0.020 Uiso 1 1 d D . . N4 N 0.9051(2) 0.4735(2) 0.08190(12) 0.0147(7) Uani 1 1 d D . . H4 H 0.905(3) 0.442(2) 0.0511(11) 0.022 Uiso 1 1 d D . . C1 C 0.8337(3) 0.7336(3) 0.09451(16) 0.0183(8) Uani 1 1 d . . . C1S C 1.2505(3) 0.7992(3) 0.0227(2) 0.0487(13) Uani 1 1 d . . . H1SA H 1.2658 0.7263 0.0352 0.058 Uiso 1 1 calc R . . H1SB H 1.3130 0.8282 0.0128 0.058 Uiso 1 1 calc R . . C2 C 0.8456(3) 0.8433(3) 0.07002(16) 0.0244(9) Uani 1 1 d . . . C2S C 0.5189(4) 0.8399(4) 0.4405(2) 0.0625(15) Uani 1 1 d . . . H2SA H 0.5731 0.8812 0.4679 0.075 Uiso 1 1 calc R . . H2SB H 0.4550 0.8828 0.4296 0.075 Uiso 1 1 calc R . . C3 C 0.7766(3) 0.8549(3) 0.00770(16) 0.0365(11) Uani 1 1 d . . . H3A H 0.7038 0.8434 0.0080 0.055 Uiso 1 1 calc R . . H3B H 0.7973 0.8038 -0.0181 0.055 Uiso 1 1 calc R . . H3C H 0.7844 0.9251 -0.0068 0.055 Uiso 1 1 calc R . . C4 C 0.9600(3) 0.8565(3) 0.06898(18) 0.0362(11) Uani 1 1 d . . . H4A H 0.9708 0.9265 0.0553 0.054 Uiso 1 1 calc R . . H4B H 0.9777 0.8051 0.0423 0.054 Uiso 1 1 calc R . . H4C H 1.0047 0.8462 0.1087 0.054 Uiso 1 1 calc R . . C5 C 0.8185(3) 0.9267(3) 0.11122(16) 0.0271(9) Uani 1 1 d . . . H5A H 0.8690 0.9210 0.1501 0.032 Uiso 1 1 calc R . . H5B H 0.8277 0.9960 0.0951 0.032 Uiso 1 1 calc R . . C6 C 0.7105(3) 0.9204(3) 0.12008(16) 0.0246(9) Uani 1 1 d . . . C7 C 0.6270(3) 0.9762(3) 0.08591(17) 0.0331(10) Uani 1 1 d . . . H7 H 0.6381 1.0210 0.0559 0.040 Uiso 1 1 calc R . . C8 C 0.5282(3) 0.9676(3) 0.09475(18) 0.0386(11) Uani 1 1 d . . . H8 H 0.4727 1.0082 0.0720 0.046 Uiso 1 1 calc R . . C9 C 0.5105(3) 0.9000(3) 0.13660(18) 0.0318(10) Uani 1 1 d . . . H9 H 0.4421 0.8933 0.1418 0.038 Uiso 1 1 calc R . . C10 C 0.5909(3) 0.8414(3) 0.17142(16) 0.0253(9) Uani 1 1 d . . . C11 C 0.6904(3) 0.8550(3) 0.16315(16) 0.0256(9) Uani 1 1 d . . . H11 H 0.7467 0.8182 0.1879 0.031 Uiso 1 1 calc R . . C12 C 0.5724(3) 0.7632(3) 0.21487(16) 0.0260(9) Uani 1 1 d . . . H12A H 0.5110 0.7850 0.2285 0.031 Uiso 1 1 calc R . . H12B H 0.6332 0.7630 0.2495 0.031 Uiso 1 1 calc R . . C13 C 0.5542(3) 0.6503(3) 0.19023(15) 0.0221(9) Uani 1 1 d . . . C14 C 0.5430(3) 0.5774(3) 0.24044(16) 0.0321(10) Uani 1 1 d . . . H14A H 0.5317 0.5062 0.2256 0.048 Uiso 1 1 calc R . . H14B H 0.4836 0.5996 0.2551 0.048 Uiso 1 1 calc R . . H14C H 0.6067 0.5803 0.2725 0.048 Uiso 1 1 calc R . . C15 C 0.4561(3) 0.6449(3) 0.13971(16) 0.0304(10) Uani 1 1 d . . . H15A H 0.4654 0.6875 0.1069 0.046 Uiso 1 1 calc R . . H15B H 0.3966 0.6710 0.1531 0.046 Uiso 1 1 calc R . . H15C H 0.4431 0.5727 0.1267 0.046 Uiso 1 1 calc R . . C16 C 0.6493(3) 0.6139(3) 0.16977(15) 0.0171(8) Uani 1 1 d . . . C17 C 0.8016(3) 0.3706(3) 0.19065(16) 0.0171(8) Uani 1 1 d . . . C18 C 0.7920(3) 0.2686(3) 0.22180(16) 0.0204(9) Uani 1 1 d . . . C19 C 0.7229(3) 0.2909(3) 0.26402(16) 0.0326(11) Uani 1 1 d . . . H19A H 0.7542 0.3465 0.2913 0.049 Uiso 1 1 calc R . . H19B H 0.7168 0.2279 0.2864 0.049 Uiso 1 1 calc R . . H19C H 0.6536 0.3125 0.2413 0.049 Uiso 1 1 calc R . . C20 C 0.7416(3) 0.1828(3) 0.17892(17) 0.0298(10) Uani 1 1 d . . . H20A H 0.6712 0.2042 0.1577 0.045 Uiso 1 1 calc R . . H20B H 0.7377 0.1188 0.2009 0.045 Uiso 1 1 calc R . . H20C H 0.7835 0.1704 0.1507 0.045 Uiso 1 1 calc R . . C21 C 0.9000(3) 0.2340(3) 0.25808(15) 0.0204(9) Uani 1 1 d . . . H21A H 0.9260 0.2863 0.2892 0.024 Uiso 1 1 calc R . . H21B H 0.8920 0.1677 0.2779 0.024 Uiso 1 1 calc R . . C22 C 0.9815(3) 0.2191(3) 0.22404(15) 0.0159(8) Uani 1 1 d . . . C23 C 1.0002(3) 0.1230(3) 0.20182(15) 0.0211(9) Uani 1 1 d . . . H23 H 0.9634 0.0636 0.2096 0.025 Uiso 1 1 calc R . . C24 C 1.0723(3) 0.1130(3) 0.16830(15) 0.0228(9) Uani 1 1 d . . . H24 H 1.0850 0.0468 0.1537 0.027 Uiso 1 1 calc R . . C25 C 1.1256(3) 0.1990(3) 0.15625(15) 0.0218(9) Uani 1 1 d . . . H25 H 1.1739 0.1913 0.1328 0.026 Uiso 1 1 calc R . . C26 C 1.1098(3) 0.2960(3) 0.17763(14) 0.0158(8) Uani 1 1 d . . . C27 C 1.0383(3) 0.3038(3) 0.21243(14) 0.0171(8) Uani 1 1 d . . . H27 H 1.0283 0.3694 0.2287 0.021 Uiso 1 1 calc R . . C28 C 1.1618(3) 0.3928(3) 0.16341(15) 0.0182(8) Uani 1 1 d . . . H28A H 1.2299 0.3735 0.1564 0.022 Uiso 1 1 calc R . . H28B H 1.1755 0.4393 0.1981 0.022 Uiso 1 1 calc R . . C29 C 1.0985(3) 0.4535(3) 0.10911(15) 0.0159(8) Uani 1 1 d . . . C30 C 1.1573(3) 0.5541(3) 0.10282(16) 0.0218(9) Uani 1 1 d . . . H30A H 1.1168 0.5943 0.0694 0.033 Uiso 1 1 calc R . . H30B H 1.2253 0.5367 0.0962 0.033 Uiso 1 1 calc R . . H30C H 1.1672 0.5953 0.1389 0.033 Uiso 1 1 calc R . . C31 C 1.0862(3) 0.3887(3) 0.05385(14) 0.0198(9) Uani 1 1 d . . . H31A H 1.0457 0.3262 0.0568 0.030 Uiso 1 1 calc R . . H31B H 1.1551 0.3685 0.0495 0.030 Uiso 1 1 calc R . . H31C H 1.0500 0.4294 0.0195 0.030 Uiso 1 1 calc R . . C32 C 0.9935(3) 0.4865(3) 0.11950(15) 0.0142(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01485(15) 0.01240(15) 0.01504(15) -0.00019(13) 0.00590(12) 0.00030(12) Rh2 0.01529(15) 0.01382(16) 0.01497(16) -0.00122(13) 0.00654(12) 0.00128(13) Cl1 0.0247(5) 0.0279(6) 0.0175(5) -0.0034(4) 0.0055(4) -0.0013(4) Cl1S 0.0687(8) 0.0390(7) 0.0374(7) -0.0029(5) 0.0170(6) -0.0097(6) Cl2S 0.0373(7) 0.1263(13) 0.0393(8) -0.0109(8) 0.0028(6) 0.0079(8) Cl3S 0.0603(9) 0.0954(11) 0.0651(10) -0.0087(8) 0.0352(7) 0.0012(8) Cl4S 0.0702(9) 0.0448(8) 0.1154(12) 0.0027(8) 0.0630(9) 0.0061(7) O1 0.0273(15) 0.0236(15) 0.0318(17) 0.0003(13) 0.0115(13) 0.0041(12) O2 0.0234(15) 0.0263(16) 0.0296(16) 0.0005(12) 0.0075(12) 0.0040(12) O3 0.0224(14) 0.0206(15) 0.0174(14) -0.0001(11) 0.0073(11) 0.0010(11) O4 0.0174(13) 0.0154(13) 0.0161(14) -0.0015(11) 0.0067(11) 0.0006(11) N1 0.0119(16) 0.0096(16) 0.0117(16) 0.0004(14) 0.0013(13) -0.0015(13) N2 0.0073(14) 0.0148(16) 0.0057(16) -0.0018(13) -0.0013(11) 0.0000(13) N3 0.0154(16) 0.0116(17) 0.0149(17) -0.0031(13) 0.0061(13) -0.0050(13) N4 0.0200(17) 0.0126(16) 0.0135(16) -0.0010(13) 0.0079(14) -0.0003(14) C1 0.019(2) 0.019(2) 0.021(2) 0.0062(18) 0.0106(17) 0.0101(17) C1S 0.036(3) 0.041(3) 0.070(4) 0.003(3) 0.017(2) 0.005(2) C2 0.034(2) 0.015(2) 0.028(2) 0.0035(18) 0.0145(19) 0.0003(18) C2S 0.089(4) 0.041(3) 0.072(4) -0.012(3) 0.047(3) -0.002(3) C3 0.062(3) 0.020(2) 0.032(3) 0.010(2) 0.020(2) 0.012(2) C4 0.044(3) 0.021(2) 0.055(3) 0.005(2) 0.032(2) -0.002(2) C5 0.039(2) 0.011(2) 0.034(2) 0.0026(18) 0.0140(19) 0.0002(18) C6 0.034(2) 0.012(2) 0.028(2) -0.0044(18) 0.0088(18) 0.0054(18) C7 0.052(3) 0.017(2) 0.029(2) 0.0008(19) 0.007(2) 0.007(2) C8 0.037(3) 0.029(3) 0.042(3) -0.003(2) -0.004(2) 0.016(2) C9 0.026(2) 0.030(3) 0.040(3) -0.008(2) 0.009(2) 0.0046(19) C10 0.022(2) 0.026(2) 0.029(2) -0.0113(19) 0.0082(18) 0.0057(18) C11 0.029(2) 0.019(2) 0.027(2) -0.0084(18) 0.0041(18) 0.0055(18) C12 0.018(2) 0.035(2) 0.027(2) -0.0086(19) 0.0102(17) 0.0042(18) C13 0.019(2) 0.026(2) 0.024(2) -0.0041(18) 0.0099(17) 0.0030(17) C14 0.030(2) 0.042(3) 0.032(2) -0.001(2) 0.0219(19) 0.001(2) C15 0.016(2) 0.040(3) 0.036(2) -0.010(2) 0.0080(18) 0.0017(19) C16 0.014(2) 0.015(2) 0.021(2) 0.0031(16) 0.0025(17) 0.0001(15) C17 0.0128(19) 0.018(2) 0.024(2) 0.0003(17) 0.0108(17) -0.0015(16) C18 0.019(2) 0.020(2) 0.025(2) 0.0077(17) 0.0091(17) 0.0009(17) C19 0.029(2) 0.042(3) 0.034(3) 0.020(2) 0.022(2) 0.009(2) C20 0.020(2) 0.017(2) 0.049(3) 0.009(2) 0.0042(19) -0.0031(17) C21 0.022(2) 0.020(2) 0.020(2) 0.0089(17) 0.0079(17) -0.0001(17) C22 0.0148(19) 0.017(2) 0.0144(19) 0.0031(16) 0.0012(15) 0.0016(16) C23 0.022(2) 0.020(2) 0.020(2) 0.0094(17) 0.0028(17) 0.0026(17) C24 0.033(2) 0.014(2) 0.021(2) 0.0010(16) 0.0058(18) 0.0050(17) C25 0.023(2) 0.024(2) 0.021(2) 0.0078(17) 0.0110(17) 0.0085(18) C26 0.0136(19) 0.018(2) 0.015(2) 0.0041(16) 0.0021(15) 0.0040(16) C27 0.0181(19) 0.018(2) 0.015(2) 0.0021(16) 0.0041(16) 0.0030(16) C28 0.0158(19) 0.020(2) 0.021(2) 0.0028(16) 0.0094(16) 0.0046(16) C29 0.0160(19) 0.014(2) 0.021(2) 0.0005(16) 0.0111(16) 0.0010(15) C30 0.023(2) 0.021(2) 0.025(2) 0.0040(17) 0.0127(17) -0.0025(17) C31 0.024(2) 0.018(2) 0.021(2) 0.0020(16) 0.0118(17) 0.0069(16) C32 0.0178(19) 0.0090(19) 0.018(2) 0.0057(16) 0.0090(16) -0.0013(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N3 1.991(3) . ? Rh1 N4 2.006(3) . ? Rh1 N1 2.011(3) . ? Rh1 N2 2.021(3) . ? Rh1 Rh2 2.4136(4) . ? Rh1 Cl1 2.4165(9) . ? Rh2 O2 1.978(2) . ? Rh2 O1 2.000(2) . ? Rh2 O4 2.001(2) . ? Rh2 O3 2.011(2) . ? Cl1S C1S 1.752(4) . ? Cl2S C1S 1.719(4) . ? Cl3S C2S 1.739(4) . ? Cl4S C2S 1.725(5) . ? O1 C1 1.322(4) . ? O2 C16 1.313(4) . ? O3 C17 1.301(4) . ? O4 C32 1.298(4) . ? N1 C1 1.269(4) . ? N1 H1 0.730(17) . ? N2 C16 1.270(4) . ? N2 H2 0.746(17) . ? N3 C17 1.286(4) . ? N3 H3 0.811(18) . ? N4 C32 1.290(4) . ? N4 H4 0.825(18) . ? C1 C2 1.549(5) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2 C3 1.525(5) . ? C2 C4 1.535(5) . ? C2 C5 1.547(5) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.501(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.393(5) . ? C6 C11 1.393(5) . ? C7 C8 1.383(5) . ? C7 H7 0.9500 . ? C8 C9 1.376(5) . ? C8 H8 0.9500 . ? C9 C10 1.392(5) . ? C9 H9 0.9500 . ? C10 C11 1.393(5) . ? C10 C12 1.498(5) . ? C11 H11 0.9500 . ? C12 C13 1.561(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C15 1.526(5) . ? C13 C16 1.533(5) . ? C13 C14 1.543(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C18 1.524(5) . ? C18 C20 1.531(5) . ? C18 C21 1.537(5) . ? C18 C19 1.539(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.510(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.389(5) . ? C22 C27 1.393(4) . ? C23 C24 1.391(5) . ? C23 H23 0.9500 . ? C24 C25 1.381(5) . ? C24 H24 0.9500 . ? C25 C26 1.382(5) . ? C25 H25 0.9500 . ? C26 C27 1.404(4) . ? C26 C28 1.502(4) . ? C27 H27 0.9500 . ? C28 C29 1.551(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C31 1.517(4) . ? C29 C32 1.534(4) . ? C29 C30 1.538(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 N3 Rh1 N4 88.69(11) . . ? N3 Rh1 N1 174.93(11) . . ? N4 Rh1 N1 91.69(11) . . ? N3 Rh1 N2 90.17(11) . . ? N4 Rh1 N2 172.70(11) . . ? N1 Rh1 N2 88.81(11) . . ? N3 Rh1 Rh2 87.09(8) . . ? N4 Rh1 Rh2 85.96(8) . . ? N1 Rh1 Rh2 87.90(8) . . ? N2 Rh1 Rh2 86.78(7) . . ? N3 Rh1 Cl1 92.36(8) . . ? N4 Rh1 Cl1 92.39(8) . . ? N1 Rh1 Cl1 92.67(8) . . ? N2 Rh1 Cl1 94.86(8) . . ? Rh2 Rh1 Cl1 178.27(3) . . ? O2 Rh2 O1 91.87(10) . . ? O2 Rh2 O4 177.55(10) . . ? O1 Rh2 O4 89.68(9) . . ? O2 Rh2 O3 87.94(9) . . ? O1 Rh2 O3 176.51(10) . . ? O4 Rh2 O3 90.40(9) . . ? O2 Rh2 Rh1 88.66(7) . . ? O1 Rh2 Rh1 87.90(7) . . ? O4 Rh2 Rh1 89.50(6) . . ? O3 Rh2 Rh1 88.61(7) . . ? C1 O1 Rh2 120.6(2) . . ? C16 O2 Rh2 121.0(2) . . ? C17 O3 Rh2 119.6(2) . . ? C32 O4 Rh2 119.8(2) . . ? C1 N1 Rh1 121.3(2) . . ? C1 N1 H1 119(3) . . ? Rh1 N1 H1 119(3) . . ? C16 N2 Rh1 121.9(2) . . ? C16 N2 H2 121(3) . . ? Rh1 N2 H2 117(3) . . ? C17 N3 Rh1 122.6(2) . . ? C17 N3 H3 111(2) . . ? Rh1 N3 H3 126(2) . . ? C32 N4 Rh1 123.5(2) . . ? C32 N4 H4 118(2) . . ? Rh1 N4 H4 119(2) . . ? N1 C1 O1 122.1(3) . . ? N1 C1 C2 122.3(3) . . ? O1 C1 C2 115.6(3) . . ? Cl2S C1S Cl1S 112.5(2) . . ? Cl2S C1S H1SA 109.1 . . ? Cl1S C1S H1SA 109.1 . . ? Cl2S C1S H1SB 109.1 . . ? Cl1S C1S H1SB 109.1 . . ? H1SA C1S H1SB 107.8 . . ? C3 C2 C4 109.3(3) . . ? C3 C2 C5 110.7(3) . . ? C4 C2 C5 108.7(3) . . ? C3 C2 C1 110.7(3) . . ? C4 C2 C1 107.5(3) . . ? C5 C2 C1 109.8(3) . . ? Cl4S C2S Cl3S 114.1(3) . . ? Cl4S C2S H2SA 108.7 . . ? Cl3S C2S H2SA 108.7 . . ? Cl4S C2S H2SB 108.7 . . ? Cl3S C2S H2SB 108.7 . . ? H2SA C2S H2SB 107.6 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C2 115.5(3) . . ? C6 C5 H5A 108.4 . . ? C2 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? C2 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C11 117.3(4) . . ? C7 C6 C5 122.8(4) . . ? C11 C6 C5 119.8(3) . . ? C8 C7 C6 121.3(4) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 121.2(4) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C11 117.6(4) . . ? C9 C10 C12 122.1(3) . . ? C11 C10 C12 120.2(3) . . ? C10 C11 C6 122.6(4) . . ? C10 C11 H11 118.7 . . ? C6 C11 H11 118.7 . . ? C10 C12 C13 114.3(3) . . ? C10 C12 H12A 108.7 . . ? C13 C12 H12A 108.7 . . ? C10 C12 H12B 108.7 . . ? C13 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C15 C13 C16 110.6(3) . . ? C15 C13 C14 109.8(3) . . ? C16 C13 C14 107.4(3) . . ? C15 C13 C12 110.7(3) . . ? C16 C13 C12 109.7(3) . . ? C14 C13 C12 108.6(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 O2 121.6(3) . . ? N2 C16 C13 123.0(3) . . ? O2 C16 C13 115.4(3) . . ? N3 C17 O3 122.1(3) . . ? N3 C17 C18 122.8(3) . . ? O3 C17 C18 115.1(3) . . ? C17 C18 C20 112.5(3) . . ? C17 C18 C21 109.7(3) . . ? C20 C18 C21 110.3(3) . . ? C17 C18 C19 106.5(3) . . ? C20 C18 C19 109.0(3) . . ? C21 C18 C19 108.8(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C18 115.8(3) . . ? C22 C21 H21A 108.3 . . ? C18 C21 H21A 108.3 . . ? C22 C21 H21B 108.3 . . ? C18 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? C23 C22 C27 117.9(3) . . ? C23 C22 C21 122.2(3) . . ? C27 C22 C21 120.0(3) . . ? C22 C23 C24 120.6(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 120.2(3) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 121.2(3) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C27 117.6(3) . . ? C25 C26 C28 123.3(3) . . ? C27 C26 C28 119.1(3) . . ? C22 C27 C26 122.5(3) . . ? C22 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C26 C28 C29 114.6(3) . . ? C26 C28 H28A 108.6 . . ? C29 C28 H28A 108.6 . . ? C26 C28 H28B 108.6 . . ? C29 C28 H28B 108.6 . . ? H28A C28 H28B 107.6 . . ? C31 C29 C32 112.5(3) . . ? C31 C29 C30 109.2(3) . . ? C32 C29 C30 106.6(3) . . ? C31 C29 C28 110.1(3) . . ? C32 C29 C28 109.6(3) . . ? C30 C29 C28 108.7(3) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 O4 121.3(3) . . ? N4 C32 C29 124.2(3) . . ? O4 C32 C29 114.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Rh1 Rh2 O2 -88.95(11) . . . . ? N4 Rh1 Rh2 O2 -177.85(11) . . . . ? N1 Rh1 Rh2 O2 90.31(11) . . . . ? N2 Rh1 Rh2 O2 1.38(11) . . . . ? Cl1 Rh1 Rh2 O2 -160.4(9) . . . . ? N3 Rh1 Rh2 O1 179.13(11) . . . . ? N4 Rh1 Rh2 O1 90.23(11) . . . . ? N1 Rh1 Rh2 O1 -1.61(11) . . . . ? N2 Rh1 Rh2 O1 -90.54(11) . . . . ? Cl1 Rh1 Rh2 O1 107.7(9) . . . . ? N3 Rh1 Rh2 O4 89.44(10) . . . . ? N4 Rh1 Rh2 O4 0.54(10) . . . . ? N1 Rh1 Rh2 O4 -91.30(10) . . . . ? N2 Rh1 Rh2 O4 179.77(10) . . . . ? Cl1 Rh1 Rh2 O4 18.0(9) . . . . ? N3 Rh1 Rh2 O3 -0.98(11) . . . . ? N4 Rh1 Rh2 O3 -89.88(10) . . . . ? N1 Rh1 Rh2 O3 178.28(10) . . . . ? N2 Rh1 Rh2 O3 89.35(10) . . . . ? Cl1 Rh1 Rh2 O3 -72.4(9) . . . . ? O2 Rh2 O1 C1 -84.8(2) . . . . ? O4 Rh2 O1 C1 93.3(2) . . . . ? O3 Rh2 O1 C1 2.0(17) . . . . ? Rh1 Rh2 O1 C1 3.8(2) . . . . ? O1 Rh2 O2 C16 85.8(3) . . . . ? O4 Rh2 O2 C16 -43(2) . . . . ? O3 Rh2 O2 C16 -90.7(3) . . . . ? Rh1 Rh2 O2 C16 -2.1(2) . . . . ? O2 Rh2 O3 C17 89.9(2) . . . . ? O1 Rh2 O3 C17 3.0(17) . . . . ? O4 Rh2 O3 C17 -88.3(2) . . . . ? Rh1 Rh2 O3 C17 1.2(2) . . . . ? O2 Rh2 O4 C32 40(2) . . . . ? O1 Rh2 O4 C32 -89.3(2) . . . . ? O3 Rh2 O4 C32 87.2(2) . . . . ? Rh1 Rh2 O4 C32 -1.4(2) . . . . ? N3 Rh1 N1 C1 8.3(15) . . . . ? N4 Rh1 N1 C1 -86.0(3) . . . . ? N2 Rh1 N1 C1 86.7(3) . . . . ? Rh2 Rh1 N1 C1 -0.1(3) . . . . ? Cl1 Rh1 N1 C1 -178.5(3) . . . . ? N3 Rh1 N2 C16 85.9(3) . . . . ? N4 Rh1 N2 C16 4.9(11) . . . . ? N1 Rh1 N2 C16 -89.2(3) . . . . ? Rh2 Rh1 N2 C16 -1.2(3) . . . . ? Cl1 Rh1 N2 C16 178.2(3) . . . . ? N4 Rh1 N3 C17 87.1(3) . . . . ? N1 Rh1 N3 C17 -7.3(15) . . . . ? N2 Rh1 N3 C17 -85.7(3) . . . . ? Rh2 Rh1 N3 C17 1.1(3) . . . . ? Cl1 Rh1 N3 C17 179.5(3) . . . . ? N3 Rh1 N4 C32 -87.0(3) . . . . ? N1 Rh1 N4 C32 88.0(3) . . . . ? N2 Rh1 N4 C32 -5.9(11) . . . . ? Rh2 Rh1 N4 C32 0.2(3) . . . . ? Cl1 Rh1 N4 C32 -179.3(3) . . . . ? Rh1 N1 C1 O1 3.1(5) . . . . ? Rh1 N1 C1 C2 -179.7(2) . . . . ? Rh2 O1 C1 N1 -5.0(4) . . . . ? Rh2 O1 C1 C2 177.6(2) . . . . ? N1 C1 C2 C3 8.8(5) . . . . ? O1 C1 C2 C3 -173.8(3) . . . . ? N1 C1 C2 C4 -110.5(4) . . . . ? O1 C1 C2 C4 66.8(4) . . . . ? N1 C1 C2 C5 131.4(4) . . . . ? O1 C1 C2 C5 -51.3(4) . . . . ? C3 C2 C5 C6 63.5(4) . . . . ? C4 C2 C5 C6 -176.4(3) . . . . ? C1 C2 C5 C6 -59.0(4) . . . . ? C2 C5 C6 C7 -93.1(4) . . . . ? C2 C5 C6 C11 85.4(4) . . . . ? C11 C6 C7 C8 0.6(6) . . . . ? C5 C6 C7 C8 179.2(4) . . . . ? C6 C7 C8 C9 -2.4(6) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C8 C9 C10 C11 1.1(6) . . . . ? C8 C9 C10 C12 -176.6(3) . . . . ? C9 C10 C11 C6 -3.0(5) . . . . ? C12 C10 C11 C6 174.7(3) . . . . ? C7 C6 C11 C10 2.2(5) . . . . ? C5 C6 C11 C10 -176.4(3) . . . . ? C9 C10 C12 C13 93.3(4) . . . . ? C11 C10 C12 C13 -84.3(4) . . . . ? C10 C12 C13 C15 -62.8(4) . . . . ? C10 C12 C13 C16 59.4(4) . . . . ? C10 C12 C13 C14 176.6(3) . . . . ? Rh1 N2 C16 O2 0.0(5) . . . . ? Rh1 N2 C16 C13 -177.7(2) . . . . ? Rh2 O2 C16 N2 1.7(4) . . . . ? Rh2 O2 C16 C13 179.6(2) . . . . ? C15 C13 C16 N2 -9.2(5) . . . . ? C14 C13 C16 N2 110.6(4) . . . . ? C12 C13 C16 N2 -131.5(3) . . . . ? C15 C13 C16 O2 172.9(3) . . . . ? C14 C13 C16 O2 -67.3(4) . . . . ? C12 C13 C16 O2 50.6(4) . . . . ? Rh1 N3 C17 O3 -0.5(5) . . . . ? Rh1 N3 C17 C18 177.9(2) . . . . ? Rh2 O3 C17 N3 -0.7(4) . . . . ? Rh2 O3 C17 C18 -179.3(2) . . . . ? N3 C17 C18 C20 7.9(5) . . . . ? O3 C17 C18 C20 -173.6(3) . . . . ? N3 C17 C18 C21 131.0(3) . . . . ? O3 C17 C18 C21 -50.5(4) . . . . ? N3 C17 C18 C19 -111.5(4) . . . . ? O3 C17 C18 C19 67.1(4) . . . . ? C17 C18 C21 C22 -58.0(4) . . . . ? C20 C18 C21 C22 66.4(4) . . . . ? C19 C18 C21 C22 -174.2(3) . . . . ? C18 C21 C22 C23 -93.7(4) . . . . ? C18 C21 C22 C27 84.3(4) . . . . ? C27 C22 C23 C24 -1.0(5) . . . . ? C21 C22 C23 C24 176.9(3) . . . . ? C22 C23 C24 C25 -0.6(5) . . . . ? C23 C24 C25 C26 0.9(5) . . . . ? C24 C25 C26 C27 0.5(5) . . . . ? C24 C25 C26 C28 -177.0(3) . . . . ? C23 C22 C27 C26 2.5(5) . . . . ? C21 C22 C27 C26 -175.5(3) . . . . ? C25 C26 C27 C22 -2.2(5) . . . . ? C28 C26 C27 C22 175.3(3) . . . . ? C25 C26 C28 C29 92.2(4) . . . . ? C27 C26 C28 C29 -85.2(4) . . . . ? C26 C28 C29 C31 -64.6(4) . . . . ? C26 C28 C29 C32 59.7(4) . . . . ? C26 C28 C29 C30 175.8(3) . . . . ? Rh1 N4 C32 O4 -1.3(5) . . . . ? Rh1 N4 C32 C29 -178.6(2) . . . . ? Rh2 O4 C32 N4 2.0(4) . . . . ? Rh2 O4 C32 C29 179.48(19) . . . . ? C31 C29 C32 N4 -9.0(5) . . . . ? C30 C29 C32 N4 110.7(4) . . . . ? C28 C29 C32 N4 -131.9(3) . . . . ? C31 C29 C32 O4 173.6(3) . . . . ? C30 C29 C32 O4 -66.8(3) . . . . ? C28 C29 C32 O4 50.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.76 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.435 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.081