# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Synthesis and Structures of Half-Sandwich Iridium(III) and Rhodium(III) Complexes with Organochalcogen (S, Se) Ligands Bearing N-methylimidazole and Their Use as Catalysts for Norbornene Polymerization ; loop_ _publ_author_name 'Guo-Xin Jin.' 'Yuan-Biao Huang.' 'Wei-guo Jia.' 'Yue-Jian Lin.' data_f70926c _database_code_depnum_ccdc_archive 'CCDC 676479' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H27 Cl2 Ir N4 Se2' _chemical_formula_weight 732.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 9.943(3) _cell_length_b 10.212(3) _cell_length_c 12.125(4) _cell_angle_alpha 81.166(4) _cell_angle_beta 74.091(4) _cell_angle_gamma 85.754(4) _cell_volume 1169.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 961 _cell_measurement_theta_min 2.490 _cell_measurement_theta_max 27.045 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.080 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 9.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2644 _exptl_absorpt_correction_T_max 0.3434 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% 13.16 _diffrn_reflns_number 5882 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.15 _reflns_number_total 4962 _reflns_number_gt 3979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4962 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1454 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _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 Ir1 Ir 0.20494(4) 0.72026(3) 0.65808(3) 0.03611(15) Uani 1 1 d . . . Se1 Se -0.02190(10) 0.73798(10) 0.60365(8) 0.0405(2) Uani 1 1 d . . . Se2 Se 0.23035(10) 0.96528(9) 0.59826(8) 0.0401(2) Uani 1 1 d . . . Cl1 Cl 0.0857(3) 0.7480(2) 0.85474(19) 0.0442(5) Uani 1 1 d . . . Cl2 Cl 0.6057(3) 0.2510(3) 0.8652(3) 0.0654(8) Uani 1 1 d . . . N1 N -0.2321(8) 0.7149(8) 0.8204(7) 0.0419(18) Uani 1 1 d . . . N2 N -0.1872(8) 0.9195(8) 0.7533(7) 0.0398(17) Uani 1 1 d . . . N3 N -0.0160(8) 1.0728(7) 0.7510(7) 0.0409(18) Uani 1 1 d . . . N4 N 0.1674(8) 1.0701(8) 0.8138(7) 0.0400(18) Uani 1 1 d . . . C1 C -0.1505(9) 0.7947(10) 0.7326(8) 0.039(2) Uani 1 1 d . . . C2 C -0.3196(10) 0.7911(12) 0.8971(9) 0.050(3) Uani 1 1 d . . . H2 H -0.3851 0.7599 0.9654 0.060 Uiso 1 1 calc R . . C3 C -0.2920(10) 0.9207(12) 0.8540(9) 0.051(3) Uani 1 1 d . . . H3 H -0.3354 0.9949 0.8864 0.061 Uiso 1 1 calc R . . C4 C -0.1126(10) 1.0366(10) 0.6923(9) 0.046(2) Uani 1 1 d . . . H4A H -0.0617 1.0206 0.6148 0.055 Uiso 1 1 calc R . . H4B H -0.1793 1.1097 0.6855 0.055 Uiso 1 1 calc R . . C5 C 0.1231(9) 1.0363(9) 0.7289(8) 0.037(2) Uani 1 1 d . . . C6 C 0.0598(11) 1.1237(10) 0.8923(9) 0.048(2) Uani 1 1 d . . . H6 H 0.0647 1.1516 0.9606 0.058 Uiso 1 1 calc R . . C7 C -0.0540(12) 1.1285(10) 0.8530(10) 0.055(3) Uani 1 1 d . . . H7 H -0.1422 1.1629 0.8875 0.066 Uiso 1 1 calc R . . C8 C -0.2230(13) 0.5715(11) 0.8380(10) 0.060(3) Uani 1 1 d . . . H8A H -0.1999 0.5395 0.7645 0.089 Uiso 1 1 calc R . . H8B H -0.3113 0.5377 0.8845 0.089 Uiso 1 1 calc R . . H8C H -0.1517 0.5420 0.8769 0.089 Uiso 1 1 calc R . . C9 C 0.3081(12) 1.0359(12) 0.8335(11) 0.061(3) Uani 1 1 d . . . H9A H 0.3071 0.9497 0.8783 0.092 Uiso 1 1 calc R . . H9B H 0.3313 1.1004 0.8746 0.092 Uiso 1 1 calc R . . H9C H 0.3767 1.0356 0.7603 0.092 Uiso 1 1 calc R . . C10 C 0.4214(14) 0.6659(15) 0.6396(13) 0.072(4) Uani 1 1 d . . . C11 C 0.339(2) 0.563(2) 0.7163(13) 0.112(7) Uani 1 1 d . . . C12 C 0.2589(15) 0.5134(11) 0.6453(13) 0.080(5) Uani 1 1 d . . . C13 C 0.2958(11) 0.5857(10) 0.5361(10) 0.053(3) Uani 1 1 d . . . C14 C 0.3977(10) 0.6755(11) 0.5320(10) 0.052(3) Uani 1 1 d . . . C15 C 0.5315(17) 0.754(2) 0.664(2) 0.156(12) Uani 1 1 d . . . H15A H 0.6076 0.7707 0.5950 0.234 Uiso 1 1 calc R . . H15B H 0.5666 0.7088 0.7258 0.234 Uiso 1 1 calc R . . H15C H 0.4872 0.8371 0.6842 0.234 Uiso 1 1 calc R . . C16 C 0.338(3) 0.515(3) 0.8331(15) 0.221(19) Uani 1 1 d . . . H16A H 0.3983 0.4372 0.8350 0.331 Uiso 1 1 calc R . . H16B H 0.2449 0.4938 0.8775 0.331 Uiso 1 1 calc R . . H16C H 0.3718 0.5822 0.8656 0.331 Uiso 1 1 calc R . . C17 C 0.155(2) 0.4024(14) 0.684(2) 0.178(14) Uani 1 1 d . . . H17A H 0.0749 0.4279 0.6556 0.267 Uiso 1 1 calc R . . H17B H 0.1271 0.3857 0.7672 0.267 Uiso 1 1 calc R . . H17C H 0.1989 0.3234 0.6542 0.267 Uiso 1 1 calc R . . C18 C 0.2488(14) 0.5621(15) 0.4328(13) 0.083(5) Uani 1 1 d . . . H18A H 0.3251 0.5234 0.3790 0.125 Uiso 1 1 calc R . . H18B H 0.2192 0.6449 0.3959 0.125 Uiso 1 1 calc R . . H18C H 0.1723 0.5030 0.4579 0.125 Uiso 1 1 calc R . . C19 C 0.4676(13) 0.7691(13) 0.4225(13) 0.077(4) Uani 1 1 d . . . H19A H 0.4597 0.8584 0.4399 0.116 Uiso 1 1 calc R . . H19B H 0.4221 0.7641 0.3630 0.116 Uiso 1 1 calc R . . H19C H 0.5646 0.7433 0.3962 0.116 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0324(2) 0.0403(2) 0.0368(2) -0.00711(15) -0.01202(15) 0.00543(15) Se1 0.0364(5) 0.0509(6) 0.0383(5) -0.0108(4) -0.0137(4) -0.0039(4) Se2 0.0343(5) 0.0440(5) 0.0402(5) -0.0064(4) -0.0051(4) -0.0065(4) Cl1 0.0449(13) 0.0537(13) 0.0356(11) -0.0064(10) -0.0140(9) 0.0018(11) Cl2 0.0507(16) 0.0664(18) 0.0673(19) -0.0023(14) -0.0030(13) 0.0106(14) N1 0.036(4) 0.049(5) 0.045(4) -0.005(4) -0.015(3) -0.011(4) N2 0.028(4) 0.048(5) 0.043(4) -0.005(4) -0.010(3) 0.001(3) N3 0.036(4) 0.036(4) 0.048(5) -0.005(3) -0.008(3) -0.002(3) N4 0.042(5) 0.039(4) 0.042(4) -0.007(3) -0.014(3) -0.005(3) C1 0.026(4) 0.055(6) 0.042(5) -0.009(4) -0.014(4) -0.006(4) C2 0.029(5) 0.078(8) 0.044(5) -0.016(5) -0.001(4) -0.018(5) C3 0.034(5) 0.070(7) 0.046(6) -0.014(5) -0.006(4) -0.001(5) C4 0.043(6) 0.044(5) 0.053(6) -0.001(5) -0.019(4) 0.005(4) C5 0.035(5) 0.033(4) 0.043(5) -0.006(4) -0.010(4) -0.001(4) C6 0.057(7) 0.045(5) 0.043(5) -0.007(4) -0.012(5) -0.009(5) C7 0.051(7) 0.045(6) 0.059(7) -0.019(5) 0.013(5) -0.009(5) C8 0.069(8) 0.057(7) 0.056(7) -0.002(5) -0.020(6) -0.023(6) C9 0.046(6) 0.072(8) 0.073(8) -0.018(6) -0.023(6) -0.008(6) C10 0.067(8) 0.093(9) 0.075(9) -0.036(8) -0.049(7) 0.052(7) C11 0.120(14) 0.134(14) 0.068(9) -0.017(10) -0.032(10) 0.118(13) C12 0.077(9) 0.041(6) 0.085(10) 0.009(6) 0.025(8) 0.017(6) C13 0.043(6) 0.039(5) 0.072(7) -0.017(5) 0.000(5) 0.001(5) C14 0.032(5) 0.061(7) 0.065(7) -0.028(6) -0.002(5) -0.003(5) C15 0.068(10) 0.23(3) 0.23(3) -0.17(2) -0.094(14) 0.055(13) C16 0.25(3) 0.30(3) 0.059(11) 0.024(15) -0.032(14) 0.21(3) C17 0.122(17) 0.045(8) 0.27(3) -0.002(12) 0.109(18) -0.016(10) C18 0.061(8) 0.096(10) 0.109(12) -0.065(10) -0.025(8) 0.013(7) C19 0.048(7) 0.077(9) 0.093(10) -0.021(8) 0.011(7) -0.006(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 Ir1 C10 2.142(12) . ? Ir1 C13 2.144(10) . ? Ir1 C12 2.159(11) . ? Ir1 C11 2.165(11) . ? Ir1 C14 2.167(10) . ? Ir1 Cl1 2.404(2) . ? Ir1 Se1 2.5049(12) . ? Ir1 Se2 2.5072(12) . ? Se1 C1 1.868(9) . ? Se2 C5 1.867(9) . ? N1 C1 1.347(12) . ? N1 C2 1.380(13) . ? N1 C8 1.447(14) . ? N2 C1 1.340(12) . ? N2 C3 1.372(12) . ? N2 C4 1.445(13) . ? N3 C5 1.369(11) . ? N3 C7 1.387(13) . ? N3 C4 1.440(12) . ? N4 C5 1.323(12) . ? N4 C6 1.366(13) . ? N4 C9 1.491(13) . ? C2 C3 1.365(16) . ? C6 C7 1.339(17) . ? C10 C14 1.376(16) . ? C10 C11 1.43(2) . ? C10 C15 1.58(2) . ? C11 C16 1.43(2) . ? C11 C12 1.48(2) . ? C12 C13 1.380(18) . ? C12 C17 1.52(2) . ? C13 C14 1.402(14) . ? C13 C18 1.508(17) . ? C14 C19 1.537(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 Ir1 C13 63.8(4) . . ? C10 Ir1 C12 64.9(6) . . ? C13 Ir1 C12 37.4(5) . . ? C10 Ir1 C11 38.8(7) . . ? C13 Ir1 C11 64.9(5) . . ? C12 Ir1 C11 40.1(7) . . ? C10 Ir1 C14 37.2(5) . . ? C13 Ir1 C14 37.9(4) . . ? C12 Ir1 C14 63.1(4) . . ? C11 Ir1 C14 63.8(5) . . ? C10 Ir1 Cl1 111.4(4) . . ? C13 Ir1 Cl1 147.4(3) . . ? C12 Ir1 Cl1 110.1(4) . . ? C11 Ir1 Cl1 91.1(4) . . ? C14 Ir1 Cl1 148.6(3) . . ? C10 Ir1 Se1 155.6(3) . . ? C13 Ir1 Se1 92.4(3) . . ? C12 Ir1 Se1 99.8(5) . . ? C11 Ir1 Se1 137.0(7) . . ? C14 Ir1 Se1 119.7(3) . . ? Cl1 Ir1 Se1 91.28(6) . . ? C10 Ir1 Se2 98.2(5) . . ? C13 Ir1 Se2 120.1(3) . . ? C12 Ir1 Se2 155.3(3) . . ? C11 Ir1 Se2 133.5(7) . . ? C14 Ir1 Se2 92.4(3) . . ? Cl1 Ir1 Se2 92.36(7) . . ? Se1 Ir1 Se2 89.31(3) . . ? C1 Se1 Ir1 103.5(3) . . ? C5 Se2 Ir1 103.1(3) . . ? C1 N1 C2 109.4(9) . . ? C1 N1 C8 125.9(9) . . ? C2 N1 C8 124.5(9) . . ? C1 N2 C3 110.7(9) . . ? C1 N2 C4 125.8(8) . . ? C3 N2 C4 122.6(9) . . ? C5 N3 C7 108.3(8) . . ? C5 N3 C4 125.9(8) . . ? C7 N3 C4 124.8(9) . . ? C5 N4 C6 110.7(8) . . ? C5 N4 C9 125.5(8) . . ? C6 N4 C9 123.1(9) . . ? N2 C1 N1 106.6(8) . . ? N2 C1 Se1 128.1(7) . . ? N1 C1 Se1 125.2(7) . . ? C3 C2 N1 107.2(9) . . ? C2 C3 N2 106.1(9) . . ? N3 C4 N2 111.8(8) . . ? N4 C5 N3 106.4(7) . . ? N4 C5 Se2 127.3(7) . . ? N3 C5 Se2 126.1(7) . . ? C7 C6 N4 107.3(9) . . ? C6 C7 N3 107.2(9) . . ? C14 C10 C11 109.3(13) . . ? C14 C10 C15 121.7(16) . . ? C11 C10 C15 128.9(15) . . ? C14 C10 Ir1 72.4(6) . . ? C11 C10 Ir1 71.5(7) . . ? C15 C10 Ir1 124.9(9) . . ? C16 C11 C10 128(2) . . ? C16 C11 C12 128(2) . . ? C10 C11 C12 104.7(11) . . ? C16 C11 Ir1 126.8(10) . . ? C10 C11 Ir1 69.7(7) . . ? C12 C11 Ir1 69.7(6) . . ? C13 C12 C11 107.7(13) . . ? C13 C12 C17 125.6(19) . . ? C11 C12 C17 126.7(19) . . ? C13 C12 Ir1 70.7(6) . . ? C11 C12 Ir1 70.2(7) . . ? C17 C12 Ir1 124.8(10) . . ? C12 C13 C14 109.0(13) . . ? C12 C13 C18 126.1(13) . . ? C14 C13 C18 124.5(12) . . ? C12 C13 Ir1 71.9(7) . . ? C14 C13 Ir1 71.9(6) . . ? C18 C13 Ir1 128.0(8) . . ? C10 C14 C13 109.3(12) . . ? C10 C14 C19 127.1(12) . . ? C13 C14 C19 123.6(11) . . ? C10 C14 Ir1 70.4(7) . . ? C13 C14 Ir1 70.1(6) . . ? C19 C14 Ir1 125.1(8) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 2.981 _refine_diff_density_min -3.686 _refine_diff_density_rms 0.277 data_f70927a _database_code_depnum_ccdc_archive 'CCDC 676480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H29 Cl2 Ir N4 Se2' _chemical_formula_weight 746.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 9.878(3) _cell_length_b 10.131(4) _cell_length_c 12.619(4) _cell_angle_alpha 83.622(5) _cell_angle_beta 73.845(5) _cell_angle_gamma 87.650(5) _cell_volume 1205.5(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 764 _cell_measurement_theta_min 2.338 _cell_measurement_theta_max 22.224 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 8.794 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4734 _exptl_absorpt_correction_T_max 0.5397 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% 6.06 _diffrn_reflns_number 6134 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.15 _reflns_number_total 5154 _reflns_number_gt 4006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5154 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1438 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.21566(4) 0.21835(4) 0.66612(3) 0.03645(14) Uani 1 1 d . . . Se1 Se -0.01739(11) 0.20656(12) 0.62392(9) 0.0473(3) Uani 1 1 d . . . Se2 Se 0.23155(11) 0.46793(10) 0.61805(8) 0.0435(3) Uani 1 1 d . . . Cl1 Cl 0.0976(3) 0.2393(3) 0.8569(2) 0.0470(6) Uani 1 1 d . . . Cl2 Cl 0.3978(3) 0.2474(3) 0.1330(3) 0.0711(9) Uani 1 1 d . . . N1 N -0.2272(9) 0.2078(10) 0.8343(8) 0.051(2) Uani 1 1 d . . . N2 N -0.1898(8) 0.4059(9) 0.7459(7) 0.044(2) Uani 1 1 d . . . N3 N 0.0070(10) 0.6008(8) 0.7673(8) 0.049(2) Uani 1 1 d . . . N4 N 0.1814(10) 0.5556(9) 0.8334(7) 0.046(2) Uani 1 1 d . . . C1 C -0.1505(10) 0.2756(12) 0.7427(9) 0.045(3) Uani 1 1 d . . . C2 C -0.3178(12) 0.2975(16) 0.8972(10) 0.066(4) Uani 1 1 d . . . H2 H -0.3841 0.2766 0.9650 0.079 Uiso 1 1 calc R . . C3 C -0.2919(11) 0.4197(13) 0.8421(10) 0.052(3) Uani 1 1 d . . . H3 H -0.3356 0.4986 0.8654 0.063 Uiso 1 1 calc R . . C4 C -0.1342(13) 0.5120(12) 0.6574(10) 0.056(3) Uani 1 1 d . . . H4A H -0.0582 0.4754 0.6015 0.067 Uiso 1 1 calc R . . H4B H -0.2082 0.5409 0.6229 0.067 Uiso 1 1 calc R . . C5 C -0.0817(13) 0.6283(12) 0.6918(10) 0.059(3) Uani 1 1 d . . . H5A H -0.1619 0.6815 0.7274 0.071 Uiso 1 1 calc R . . H5B H -0.0282 0.6814 0.6259 0.071 Uiso 1 1 calc R . . C6 C 0.1340(10) 0.5445(9) 0.7475(8) 0.034(2) Uani 1 1 d . . . C7 C 0.0808(13) 0.6197(11) 0.9125(10) 0.054(3) Uani 1 1 d . . . H7 H 0.0880 0.6372 0.9815 0.065 Uiso 1 1 calc R . . C8 C -0.0254(13) 0.6504(11) 0.8714(10) 0.058(3) Uani 1 1 d . . . H8 H -0.1069 0.6963 0.9046 0.069 Uiso 1 1 calc R . . C9 C -0.2140(17) 0.0675(14) 0.8656(12) 0.085(5) Uani 1 1 d . . . H9A H -0.1530 0.0269 0.8043 0.128 Uiso 1 1 calc R . . H9B H -0.3052 0.0274 0.8857 0.128 Uiso 1 1 calc R . . H9C H -0.1749 0.0548 0.9277 0.128 Uiso 1 1 calc R . . C10 C 0.3167(14) 0.5034(13) 0.8493(10) 0.063(3) Uani 1 1 d . . . H10A H 0.3663 0.4583 0.7866 0.095 Uiso 1 1 calc R . . H10B H 0.2993 0.4424 0.9154 0.095 Uiso 1 1 calc R . . H10C H 0.3725 0.5756 0.8563 0.095 Uiso 1 1 calc R . . C11 C 0.4007(11) 0.1825(12) 0.5339(9) 0.050(3) Uani 1 1 d . . . C12 C 0.4429(11) 0.1843(13) 0.6293(11) 0.057(3) Uani 1 1 d . . . C13 C 0.3726(18) 0.0843(18) 0.7067(13) 0.087(5) Uani 1 1 d . . . C14 C 0.2843(15) 0.0155(13) 0.660(2) 0.110(8) Uani 1 1 d . . . C15 C 0.3059(13) 0.0805(14) 0.5472(13) 0.070(4) Uani 1 1 d . . . C16 C 0.4600(16) 0.2707(16) 0.4252(12) 0.089(5) Uani 1 1 d . . . H16A H 0.5544 0.2423 0.3906 0.134 Uiso 1 1 calc R . . H16B H 0.4609 0.3614 0.4406 0.134 Uiso 1 1 calc R . . H16C H 0.4020 0.2637 0.3765 0.134 Uiso 1 1 calc R . . C17 C 0.5528(15) 0.2783(19) 0.6428(17) 0.122(8) Uani 1 1 d . . . H17A H 0.6447 0.2525 0.6003 0.183 Uiso 1 1 calc R . . H17B H 0.5504 0.2739 0.7197 0.183 Uiso 1 1 calc R . . H17C H 0.5321 0.3675 0.6169 0.183 Uiso 1 1 calc R . . C18 C 0.384(3) 0.043(3) 0.8228(15) 0.23(2) Uani 1 1 d . . . H18A H 0.4210 -0.0456 0.8270 0.342 Uiso 1 1 calc R . . H18B H 0.2927 0.0473 0.8747 0.342 Uiso 1 1 calc R . . H18C H 0.4464 0.1027 0.8403 0.342 Uiso 1 1 calc R . . C19 C 0.190(2) -0.0983(18) 0.715(3) 0.32(3) Uani 1 1 d . . . H19A H 0.2416 -0.1803 0.7018 0.475 Uiso 1 1 calc R . . H19B H 0.1107 -0.0964 0.6852 0.475 Uiso 1 1 calc R . . H19C H 0.1584 -0.0916 0.7933 0.475 Uiso 1 1 calc R . . C20 C 0.2457(18) 0.037(2) 0.458(2) 0.161(12) Uani 1 1 d . . . H20A H 0.2165 0.1144 0.4184 0.241 Uiso 1 1 calc R . . H20B H 0.1660 -0.0186 0.4926 0.241 Uiso 1 1 calc R . . H20C H 0.3164 -0.0106 0.4082 0.241 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0313(2) 0.0363(2) 0.0407(2) -0.01020(15) -0.00577(15) -0.00038(14) Se1 0.0362(5) 0.0619(7) 0.0469(6) -0.0243(5) -0.0092(4) -0.0033(5) Se2 0.0486(6) 0.0399(6) 0.0371(6) -0.0081(4) -0.0013(4) -0.0079(4) Cl1 0.0471(14) 0.0543(16) 0.0390(14) -0.0098(11) -0.0084(11) -0.0043(11) Cl2 0.0561(18) 0.064(2) 0.077(2) -0.0146(16) 0.0112(15) 0.0058(15) N1 0.042(5) 0.065(6) 0.044(5) 0.000(4) -0.010(4) -0.017(4) N2 0.036(5) 0.057(6) 0.043(5) -0.016(4) -0.011(4) 0.000(4) N3 0.051(5) 0.036(5) 0.050(5) 0.001(4) 0.000(4) -0.007(4) N4 0.057(6) 0.040(5) 0.040(5) -0.010(4) -0.010(4) -0.008(4) C1 0.031(5) 0.063(7) 0.043(6) -0.013(5) -0.009(4) -0.010(5) C2 0.039(6) 0.116(12) 0.041(7) -0.031(7) 0.005(5) -0.009(7) C3 0.041(6) 0.065(8) 0.054(7) -0.022(6) -0.013(5) 0.004(5) C4 0.071(8) 0.054(7) 0.048(7) -0.008(5) -0.024(6) -0.001(6) C5 0.055(7) 0.059(8) 0.056(7) 0.006(6) -0.007(6) 0.003(6) C6 0.040(5) 0.026(5) 0.037(5) -0.006(4) -0.008(4) -0.006(4) C7 0.064(8) 0.042(6) 0.051(7) -0.010(5) -0.003(6) -0.002(5) C8 0.054(7) 0.042(6) 0.058(8) -0.008(5) 0.017(6) -0.006(5) C9 0.109(12) 0.058(9) 0.078(10) -0.002(7) -0.004(9) -0.039(8) C10 0.073(8) 0.072(9) 0.058(8) -0.022(6) -0.034(7) -0.004(7) C11 0.033(5) 0.061(7) 0.054(7) -0.026(5) -0.006(5) 0.017(5) C12 0.032(6) 0.071(8) 0.076(9) -0.016(7) -0.026(6) 0.009(5) C13 0.080(11) 0.094(12) 0.074(10) -0.005(9) -0.008(8) 0.042(10) C14 0.049(8) 0.038(7) 0.20(2) -0.010(10) 0.043(10) 0.003(6) C15 0.048(7) 0.059(8) 0.104(11) -0.053(8) -0.005(7) -0.001(6) C16 0.076(10) 0.103(12) 0.070(10) -0.013(9) 0.009(8) 0.022(9) C17 0.057(9) 0.146(17) 0.19(2) -0.101(16) -0.060(12) 0.038(10) C18 0.20(3) 0.36(4) 0.068(13) 0.063(18) -0.011(14) 0.20(3) C19 0.117(19) 0.045(10) 0.61(7) 0.04(2) 0.16(3) 0.006(11) C20 0.083(12) 0.21(2) 0.25(3) -0.20(2) -0.083(15) 0.065(14) _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 Ir1 C14 2.141(13) . ? Ir1 C15 2.148(11) . ? Ir1 C13 2.151(14) . ? Ir1 C11 2.154(10) . ? Ir1 C12 2.183(10) . ? Ir1 Cl1 2.395(3) . ? Ir1 Se1 2.5133(13) . ? Ir1 Se2 2.5347(14) . ? Se1 C1 1.878(10) . ? Se2 C6 1.882(9) . ? N1 C1 1.326(13) . ? N1 C2 1.398(15) . ? N1 C9 1.444(17) . ? N2 C3 1.362(13) . ? N2 C1 1.362(14) . ? N2 C4 1.464(14) . ? N3 C6 1.327(13) . ? N3 C8 1.408(14) . ? N3 C5 1.461(15) . ? N4 C6 1.312(12) . ? N4 C7 1.395(13) . ? N4 C10 1.474(15) . ? C2 C3 1.348(18) . ? C4 C5 1.461(17) . ? C7 C8 1.307(17) . ? C11 C12 1.381(16) . ? C11 C15 1.388(17) . ? C11 C16 1.532(18) . ? C12 C13 1.39(2) . ? C12 C17 1.528(19) . ? C13 C14 1.42(3) . ? C13 C18 1.51(2) . ? C14 C15 1.46(2) . ? C14 C19 1.49(2) . ? C15 C20 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Ir1 C15 39.8(7) . . ? C14 Ir1 C13 38.7(7) . . ? C15 Ir1 C13 64.4(6) . . ? C14 Ir1 C11 64.5(5) . . ? C15 Ir1 C11 37.6(5) . . ? C13 Ir1 C11 62.8(5) . . ? C14 Ir1 C12 64.1(5) . . ? C15 Ir1 C12 63.2(5) . . ? C13 Ir1 C12 37.3(6) . . ? C11 Ir1 C12 37.1(4) . . ? C14 Ir1 Cl1 105.7(6) . . ? C15 Ir1 Cl1 144.7(5) . . ? C13 Ir1 Cl1 92.9(4) . . ? C11 Ir1 Cl1 152.2(3) . . ? C12 Ir1 Cl1 115.2(4) . . ? C14 Ir1 Se1 100.8(6) . . ? C15 Ir1 Se1 90.3(4) . . ? C13 Ir1 Se1 138.4(6) . . ? C11 Ir1 Se1 116.4(3) . . ? C12 Ir1 Se1 152.5(3) . . ? Cl1 Ir1 Se1 90.49(7) . . ? C14 Ir1 Se2 156.8(4) . . ? C15 Ir1 Se2 122.7(4) . . ? C13 Ir1 Se2 128.0(6) . . ? C11 Ir1 Se2 92.7(3) . . ? C12 Ir1 Se2 95.3(3) . . ? Cl1 Ir1 Se2 92.47(7) . . ? Se1 Ir1 Se2 93.21(4) . . ? C1 Se1 Ir1 105.5(3) . . ? C6 Se2 Ir1 106.6(3) . . ? C1 N1 C2 107.9(11) . . ? C1 N1 C9 125.8(11) . . ? C2 N1 C9 126.2(11) . . ? C3 N2 C1 109.0(9) . . ? C3 N2 C4 126.1(10) . . ? C1 N2 C4 124.9(9) . . ? C6 N3 C8 108.7(10) . . ? C6 N3 C5 128.4(9) . . ? C8 N3 C5 122.4(10) . . ? C6 N4 C7 109.8(10) . . ? C6 N4 C10 126.5(9) . . ? C7 N4 C10 123.7(10) . . ? N1 C1 N2 108.1(9) . . ? N1 C1 Se1 127.0(9) . . ? N2 C1 Se1 124.8(8) . . ? C3 C2 N1 107.8(10) . . ? C2 C3 N2 107.2(10) . . ? C5 C4 N2 115.7(10) . . ? C4 C5 N3 115.8(10) . . ? N4 C6 N3 107.5(9) . . ? N4 C6 Se2 126.0(7) . . ? N3 C6 Se2 126.5(8) . . ? C8 C7 N4 107.1(11) . . ? C7 C8 N3 107.0(10) . . ? C12 C11 C15 110.1(12) . . ? C12 C11 C16 125.2(12) . . ? C15 C11 C16 124.5(13) . . ? C12 C11 Ir1 72.6(6) . . ? C15 C11 Ir1 71.0(6) . . ? C16 C11 Ir1 127.6(8) . . ? C11 C12 C13 108.1(13) . . ? C11 C12 C17 124.8(14) . . ? C13 C12 C17 127.1(15) . . ? C11 C12 Ir1 70.3(6) . . ? C13 C12 Ir1 70.0(7) . . ? C17 C12 Ir1 127.1(9) . . ? C12 C13 C14 109.5(14) . . ? C12 C13 C18 129(2) . . ? C14 C13 C18 122(2) . . ? C12 C13 Ir1 72.6(7) . . ? C14 C13 Ir1 70.3(8) . . ? C18 C13 Ir1 124.9(11) . . ? C13 C14 C15 105.1(12) . . ? C13 C14 C19 127(3) . . ? C15 C14 C19 128(3) . . ? C13 C14 Ir1 71.0(8) . . ? C15 C14 Ir1 70.4(7) . . ? C19 C14 Ir1 122.9(11) . . ? C11 C15 C14 107.2(13) . . ? C11 C15 C20 126.3(17) . . ? C14 C15 C20 126.3(17) . . ? C11 C15 Ir1 71.4(6) . . ? C14 C15 Ir1 69.8(7) . . ? C20 C15 Ir1 127.7(10) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.267 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.217 data_f70423a _database_code_depnum_ccdc_archive 'CCDC 676481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H27 Cl2 N4 Rh S2' _chemical_formula_weight 549.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 10.210(4) _cell_length_b 11.469(4) _cell_length_c 22.139(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2592.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 940 _cell_measurement_theta_min 2.714 _cell_measurement_theta_max 20.496 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 1.038 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8599 _exptl_absorpt_correction_T_max 0.9034 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% 5.02 _diffrn_reflns_number 12434 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.32 _reflns_number_total 3039 _reflns_number_gt 2395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3039 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.07394(3) 0.2500 0.631099(15) 0.04027(12) Uani 1 2 d S . . S1 S 0.03767(8) 0.10204(9) 0.55650(5) 0.0655(3) Uani 1 1 d . . . N1 N -0.2023(3) 0.0033(2) 0.57615(14) 0.0632(8) Uani 1 1 d . . . N2 N -0.2103(3) 0.1458(2) 0.51303(12) 0.0541(7) Uani 1 1 d . . . Cl1 Cl -0.15253(10) 0.2500 0.66174(5) 0.0526(3) Uani 1 2 d S . . Cl2 Cl 0.50190(18) 0.2500 0.39618(8) 0.0917(5) Uani 1 2 d S . . C1 C -0.1290(3) 0.0847(3) 0.54956(16) 0.0542(8) Uani 1 1 d . . . C2 C -0.3305(4) 0.0121(3) 0.55661(19) 0.0704(10) Uani 1 1 d . . . H2 H -0.4000 -0.0349 0.5685 0.084 Uiso 1 1 calc R . . C3 C -0.3362(3) 0.1009(3) 0.51743(17) 0.0635(9) Uani 1 1 d . . . H3 H -0.4102 0.1273 0.4971 0.076 Uiso 1 1 calc R . . C4 C -0.1565(5) -0.0795(4) 0.6211(2) 0.0937(15) Uani 1 1 d . . . H4A H -0.0845 -0.1233 0.6049 0.141 Uiso 1 1 calc R . . H4B H -0.2265 -0.1317 0.6315 0.141 Uiso 1 1 calc R . . H4C H -0.1284 -0.0383 0.6565 0.141 Uiso 1 1 calc R . . C5 C -0.1771(5) 0.2500 0.4800(2) 0.0631(13) Uani 1 2 d S . . H5A H -0.0839 0.2500 0.4715 0.076 Uiso 1 2 calc SR . . H5B H -0.2233 0.2500 0.4417 0.076 Uiso 1 2 calc SR . . C6 C 0.1513(3) 0.1874(3) 0.71632(15) 0.0524(8) Uani 1 1 d . . . C7 C 0.2347(3) 0.1499(3) 0.66942(17) 0.0584(9) Uani 1 1 d . . . C8 C 0.2825(4) 0.2500 0.6387(2) 0.0560(12) Uani 1 2 d S . . C9 C 0.0794(4) 0.1127(4) 0.76084(19) 0.0948(15) Uani 1 1 d . . . H9A H 0.0819 0.0330 0.7477 0.142 Uiso 1 1 calc R . . H9B H -0.0100 0.1382 0.7636 0.142 Uiso 1 1 calc R . . H9C H 0.1203 0.1192 0.7998 0.142 Uiso 1 1 calc R . . C10 C 0.2702(5) 0.0245(3) 0.6556(3) 0.1037(17) Uani 1 1 d . . . H10A H 0.3503 0.0047 0.6759 0.156 Uiso 1 1 calc R . . H10B H 0.2815 0.0152 0.6128 0.156 Uiso 1 1 calc R . . H10C H 0.2013 -0.0259 0.6694 0.156 Uiso 1 1 calc R . . C11 C 0.3784(6) 0.2500 0.5875(3) 0.108(2) Uani 1 2 d S . . H11A H 0.4657 0.2571 0.6031 0.163 Uiso 0.50 1 calc PR . . H11B H 0.3602 0.3145 0.5611 0.163 Uiso 0.50 1 calc PR . . H11C H 0.3707 0.1784 0.5653 0.163 Uiso 0.50 1 calc PR . . 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 0.03573(18) 0.0432(2) 0.0419(2) 0.000 0.00167(15) 0.000 S1 0.0474(5) 0.0739(6) 0.0753(7) -0.0328(5) -0.0103(4) 0.0158(4) N1 0.0652(19) 0.0445(17) 0.080(2) -0.0109(15) -0.0123(16) 0.0028(14) N2 0.0454(15) 0.0590(17) 0.0578(17) -0.0118(13) -0.0041(13) 0.0028(13) Cl1 0.0424(6) 0.0624(7) 0.0532(7) 0.000 0.0100(5) 0.000 Cl2 0.0934(11) 0.0755(10) 0.1061(12) 0.000 -0.0285(10) 0.000 C1 0.0524(18) 0.050(2) 0.060(2) -0.0230(16) -0.0064(17) 0.0102(16) C2 0.056(2) 0.062(2) 0.093(3) -0.012(2) -0.004(2) -0.0053(18) C3 0.050(2) 0.064(2) 0.076(3) -0.011(2) -0.0053(18) 0.0019(17) C4 0.103(4) 0.059(3) 0.119(4) 0.010(2) -0.024(3) -0.001(2) C5 0.049(3) 0.091(4) 0.049(3) 0.000 -0.004(2) 0.000 C6 0.0440(17) 0.062(2) 0.051(2) 0.0113(15) -0.0102(15) -0.0080(14) C7 0.0474(18) 0.055(2) 0.072(3) -0.0079(17) -0.0196(17) 0.0080(15) C8 0.034(2) 0.081(4) 0.053(3) 0.000 0.000(2) 0.000 C9 0.085(3) 0.123(4) 0.077(3) 0.044(3) -0.023(2) -0.033(3) C10 0.100(3) 0.069(3) 0.142(4) -0.032(3) -0.053(3) 0.034(2) C11 0.047(3) 0.195(8) 0.083(5) 0.000 0.014(3) 0.000 _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 C8 2.136(4) . ? Rh1 C6 2.168(3) 7_565 ? Rh1 C6 2.168(3) . ? Rh1 C7 2.176(3) 7_565 ? Rh1 C7 2.176(3) . ? Rh1 S1 2.3967(11) . ? Rh1 S1 2.3967(11) 7_565 ? Rh1 Cl1 2.4097(14) . ? S1 C1 1.720(3) . ? N1 C1 1.333(4) . ? N1 C2 1.382(4) . ? N1 C4 1.453(5) . ? N2 C1 1.354(4) . ? N2 C3 1.389(4) . ? N2 C5 1.441(4) . ? C2 C3 1.338(5) . ? C5 N2 1.441(4) 7_565 ? C6 C7 1.411(5) . ? C6 C6 1.435(6) 7_565 ? C6 C9 1.498(5) . ? C7 C8 1.421(4) . ? C7 C10 1.514(5) . ? C8 C7 1.421(4) 7_565 ? C8 C11 1.497(7) . ? 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 C8 Rh1 C6 64.43(14) . 7_565 ? C8 Rh1 C6 64.43(14) . . ? C6 Rh1 C6 38.66(17) 7_565 . ? C8 Rh1 C7 38.48(11) . 7_565 ? C6 Rh1 C7 37.90(12) 7_565 7_565 ? C6 Rh1 C7 63.92(12) . 7_565 ? C8 Rh1 C7 38.48(11) . . ? C6 Rh1 C7 63.92(12) 7_565 . ? C6 Rh1 C7 37.90(12) . . ? C7 Rh1 C7 63.72(18) 7_565 . ? C8 Rh1 S1 102.01(9) . . ? C6 Rh1 S1 152.93(8) 7_565 . ? C6 Rh1 S1 114.94(9) . . ? C7 Rh1 S1 139.38(10) 7_565 . ? C7 Rh1 S1 90.66(9) . . ? C8 Rh1 S1 102.01(9) . 7_565 ? C6 Rh1 S1 114.94(9) 7_565 7_565 ? C6 Rh1 S1 152.93(8) . 7_565 ? C7 Rh1 S1 90.66(9) 7_565 7_565 ? C7 Rh1 S1 139.38(10) . 7_565 ? S1 Rh1 S1 90.15(6) . 7_565 ? C8 Rh1 Cl1 159.15(13) . . ? C6 Rh1 Cl1 96.01(9) 7_565 . ? C6 Rh1 Cl1 96.01(9) . . ? C7 Rh1 Cl1 127.90(11) 7_565 . ? C7 Rh1 Cl1 127.90(11) . . ? S1 Rh1 Cl1 92.62(3) . . ? S1 Rh1 Cl1 92.62(3) 7_565 . ? C1 S1 Rh1 107.25(10) . . ? C1 N1 C2 110.0(3) . . ? C1 N1 C4 125.4(3) . . ? C2 N1 C4 124.5(3) . . ? C1 N2 C3 109.5(3) . . ? C1 N2 C5 126.0(3) . . ? C3 N2 C5 124.1(3) . . ? N1 C1 N2 106.4(3) . . ? N1 C1 S1 126.6(3) . . ? N2 C1 S1 126.8(3) . . ? C3 C2 N1 107.5(3) . . ? C2 C3 N2 106.7(3) . . ? N2 C5 N2 112.1(4) 7_565 . ? C7 C6 C6 107.8(2) . 7_565 ? C7 C6 C9 127.3(3) . . ? C6 C6 C9 124.9(2) 7_565 . ? C7 C6 Rh1 71.37(19) . . ? C6 C6 Rh1 70.67(8) 7_565 . ? C9 C6 Rh1 125.7(2) . . ? C6 C7 C8 108.2(3) . . ? C6 C7 C10 125.7(4) . . ? C8 C7 C10 126.1(4) . . ? C6 C7 Rh1 70.73(18) . . ? C8 C7 Rh1 69.2(2) . . ? C10 C7 Rh1 127.1(3) . . ? C7 C8 C7 107.8(4) 7_565 . ? C7 C8 C11 125.9(2) 7_565 . ? C7 C8 C11 125.9(2) . . ? C7 C8 Rh1 72.3(2) 7_565 . ? C7 C8 Rh1 72.3(2) . . ? C11 C8 Rh1 126.3(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.32 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.586 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.070 data_d:\data\jgx\jwg\70919b\work\f70919b _database_code_depnum_ccdc_archive 'CCDC 676482' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H42 Cl4 N4 Rh2 Se2' _chemical_formula_weight 952.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 23.485(9) _cell_length_b 11.516(5) _cell_length_c 13.329(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3605(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 919 _cell_measurement_theta_min 2.911 _cell_measurement_theta_max 24.632 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 3.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7366 _exptl_absorpt_correction_T_max 0.8541 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% 9.25 _diffrn_reflns_number 17536 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6078 _reflns_number_gt 5104 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(11) _refine_ls_number_reflns 6078 _refine_ls_number_parameters 382 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.62004(2) 0.40348(4) 0.67052(4) 0.03297(13) Uani 1 1 d . . . Rh2 Rh 0.88526(2) 0.00347(4) 0.65249(4) 0.03229(12) Uani 1 1 d . . . Se1 Se 0.69916(3) 0.39725(5) 0.54206(6) 0.04127(18) Uani 1 1 d . . . Se2 Se 0.68728(3) 0.47439(6) 0.80610(6) 0.04549(18) Uani 1 1 d . . . Cl1 Cl 0.59290(7) 0.59839(13) 0.62577(16) 0.0460(4) Uani 1 1 d . . . Cl2 Cl 0.93781(10) -0.03156(18) 0.49940(16) 0.0582(5) Uani 1 1 d . . . Cl3 Cl 0.79634(8) -0.00271(16) 0.55877(16) 0.0532(5) Uani 1 1 d . . . Cl4 Cl 0.87992(8) -0.20349(14) 0.68027(15) 0.0454(4) Uani 1 1 d . . . N1 N 0.6765(2) 0.5934(5) 0.4144(4) 0.0383(13) Uani 1 1 d . . . N2 N 0.7281(2) 0.6418(4) 0.5413(4) 0.0372(12) Uani 1 1 d . . . N3 N 0.7210(2) 0.6933(5) 0.7165(4) 0.0419(14) Uani 1 1 d . . . N4 N 0.6619(3) 0.7153(5) 0.8392(5) 0.0513(16) Uani 1 1 d . . . C1 C 0.7008(3) 0.5511(5) 0.4980(5) 0.0336(14) Uani 1 1 d . . . C2 C 0.6883(3) 0.7089(6) 0.4047(6) 0.0463(17) Uani 1 1 d . . . H2 H 0.6765 0.7569 0.3527 0.056 Uiso 1 1 calc R . . C3 C 0.7202(3) 0.7410(6) 0.4839(6) 0.0439(17) Uani 1 1 d . . . H3 H 0.7341 0.8149 0.4975 0.053 Uiso 1 1 calc R . . C4 C 0.6893(3) 0.6344(6) 0.7853(5) 0.0393(16) Uani 1 1 d . . . C5 C 0.7134(3) 0.8121(6) 0.7279(6) 0.054(2) Uani 1 1 d . . . H5 H 0.7301 0.8708 0.6902 0.065 Uiso 1 1 calc R . . C6 C 0.6763(4) 0.8247(6) 0.8060(7) 0.058(2) Uani 1 1 d . . . H6 H 0.6631 0.8946 0.8320 0.069 Uiso 1 1 calc R . . C7 C 0.7561(3) 0.6410(6) 0.6394(5) 0.0433(16) Uani 1 1 d . . . H7A H 0.7646 0.5615 0.6581 0.052 Uiso 1 1 calc R . . H7B H 0.7918 0.6830 0.6348 0.052 Uiso 1 1 calc R . . C8 C 0.6406(4) 0.5260(7) 0.3462(7) 0.059(2) Uani 1 1 d . . . H8A H 0.6601 0.4561 0.3272 0.088 Uiso 1 1 calc R . . H8B H 0.6325 0.5712 0.2874 0.088 Uiso 1 1 calc R . . H8C H 0.6056 0.5063 0.3793 0.088 Uiso 1 1 calc R . . C9 C 0.6206(4) 0.6925(8) 0.9197(8) 0.072(3) Uani 1 1 d . . . H9A H 0.5833 0.6830 0.8912 0.109 Uiso 1 1 calc R . . H9B H 0.6202 0.7568 0.9656 0.109 Uiso 1 1 calc R . . H9C H 0.6311 0.6230 0.9548 0.109 Uiso 1 1 calc R . . C10 C 0.5646(3) 0.2756(6) 0.5985(6) 0.0497(19) Uani 1 1 d . . . C11 C 0.6073(3) 0.2193(5) 0.6600(8) 0.0525(19) Uani 1 1 d . . . C12 C 0.5986(3) 0.2550(6) 0.7611(6) 0.0490(18) Uani 1 1 d . . . C13 C 0.5518(3) 0.3353(6) 0.7626(6) 0.052(2) Uani 1 1 d . . . C14 C 0.5314(3) 0.3469(6) 0.6629(7) 0.0529(19) Uani 1 1 d . . . C15 C 0.5561(5) 0.2593(8) 0.4868(7) 0.080(3) Uani 1 1 d . . . H15A H 0.5287 0.1989 0.4755 0.119 Uiso 1 1 calc R . . H15B H 0.5916 0.2382 0.4562 0.119 Uiso 1 1 calc R . . H15C H 0.5426 0.3305 0.4579 0.119 Uiso 1 1 calc R . . C16 C 0.6478(4) 0.1288(7) 0.6247(8) 0.078(3) Uani 1 1 d . . . H16A H 0.6860 0.1519 0.6408 0.117 Uiso 1 1 calc R . . H16B H 0.6442 0.1197 0.5534 0.117 Uiso 1 1 calc R . . H16C H 0.6393 0.0565 0.6572 0.117 Uiso 1 1 calc R . . C17 C 0.6304(4) 0.2088(8) 0.8501(7) 0.071(3) Uani 1 1 d . . . H17A H 0.6089 0.1471 0.8803 0.107 Uiso 1 1 calc R . . H17B H 0.6358 0.2700 0.8980 0.107 Uiso 1 1 calc R . . H17C H 0.6667 0.1798 0.8288 0.107 Uiso 1 1 calc R . . C18 C 0.5275(4) 0.3923(8) 0.8563(7) 0.077(3) Uani 1 1 d . . . H18A H 0.5116 0.4664 0.8391 0.115 Uiso 1 1 calc R . . H18B H 0.5573 0.4027 0.9048 0.115 Uiso 1 1 calc R . . H18C H 0.4983 0.3437 0.8842 0.115 Uiso 1 1 calc R . . C19 C 0.4819(3) 0.4214(7) 0.6299(9) 0.078(3) Uani 1 1 d . . . H19A H 0.4941 0.4728 0.5774 0.116 Uiso 1 1 calc R . . H19B H 0.4684 0.4661 0.6858 0.116 Uiso 1 1 calc R . . H19C H 0.4518 0.3726 0.6055 0.116 Uiso 1 1 calc R . . C20 C 0.9269(4) 0.1659(6) 0.6799(7) 0.057(2) Uani 1 1 d . . . C21 C 0.8689(4) 0.1731(7) 0.7101(7) 0.065(3) Uani 1 1 d . . . C22 C 0.8592(3) 0.0871(7) 0.7867(6) 0.055(2) Uani 1 1 d . . . C23 C 0.9113(3) 0.0314(6) 0.8065(6) 0.0478(17) Uani 1 1 d . . . C24 C 0.9535(3) 0.0751(6) 0.7381(6) 0.0475(18) Uani 1 1 d . . . C25 C 0.9572(5) 0.2408(9) 0.6037(8) 0.106(4) Uani 1 1 d . . . H25A H 0.9298 0.2872 0.5683 0.160 Uiso 1 1 calc R . . H25B H 0.9772 0.1922 0.5570 0.160 Uiso 1 1 calc R . . H25C H 0.9838 0.2907 0.6374 0.160 Uiso 1 1 calc R . . C26 C 0.8249(5) 0.2560(9) 0.6708(11) 0.128(6) Uani 1 1 d . . . H26A H 0.8430 0.3273 0.6513 0.192 Uiso 1 1 calc R . . H26B H 0.7973 0.2715 0.7222 0.192 Uiso 1 1 calc R . . H26C H 0.8063 0.2222 0.6137 0.192 Uiso 1 1 calc R . . C27 C 0.8033(5) 0.0681(12) 0.8417(10) 0.114(5) Uani 1 1 d . . . H27A H 0.7743 0.0465 0.7945 0.170 Uiso 1 1 calc R . . H27B H 0.7923 0.1385 0.8751 0.170 Uiso 1 1 calc R . . H27C H 0.8078 0.0073 0.8904 0.170 Uiso 1 1 calc R . . C28 C 0.9237(5) -0.0601(8) 0.8847(6) 0.076(3) Uani 1 1 d . . . H28A H 0.8889 -0.0822 0.9174 0.115 Uiso 1 1 calc R . . H28B H 0.9497 -0.0294 0.9335 0.115 Uiso 1 1 calc R . . H28C H 0.9403 -0.1268 0.8530 0.115 Uiso 1 1 calc R . . C29 C 1.0141(4) 0.0403(10) 0.7324(8) 0.087(3) Uani 1 1 d . . . H29A H 1.0356 0.0832 0.7810 0.131 Uiso 1 1 calc R . . H29B H 1.0284 0.0563 0.6664 0.131 Uiso 1 1 calc R . . H29C H 1.0174 -0.0413 0.7460 0.131 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0320(2) 0.0309(2) 0.0360(3) 0.0013(2) 0.0024(2) -0.00193(18) Rh2 0.0315(2) 0.0348(2) 0.0305(3) -0.0033(2) -0.0015(2) -0.00461(19) Se1 0.0442(4) 0.0365(3) 0.0431(4) -0.0002(3) 0.0089(3) 0.0032(3) Se2 0.0533(4) 0.0476(4) 0.0356(4) 0.0047(3) -0.0072(3) -0.0052(3) Cl1 0.0338(9) 0.0356(8) 0.0686(13) 0.0041(8) 0.0015(8) 0.0044(7) Cl2 0.0666(14) 0.0634(11) 0.0444(11) 0.0003(9) 0.0216(10) -0.0049(10) Cl3 0.0461(11) 0.0551(10) 0.0583(13) -0.0017(9) -0.0191(9) -0.0083(8) Cl4 0.0603(10) 0.0360(8) 0.0399(10) 0.0013(7) 0.0009(8) -0.0067(7) N1 0.035(3) 0.050(3) 0.029(3) 0.000(2) 0.004(2) -0.004(3) N2 0.037(3) 0.041(3) 0.034(3) 0.002(3) -0.003(3) -0.009(2) N3 0.047(4) 0.044(3) 0.035(3) -0.006(3) -0.010(3) -0.010(3) N4 0.056(4) 0.054(4) 0.044(4) -0.012(3) -0.002(3) -0.003(3) C1 0.030(3) 0.037(3) 0.034(4) 0.003(3) 0.003(3) -0.002(3) C2 0.062(5) 0.042(4) 0.035(4) 0.009(3) -0.001(4) 0.000(4) C3 0.051(4) 0.037(3) 0.043(4) 0.005(3) 0.003(4) -0.004(3) C4 0.046(4) 0.045(4) 0.027(4) -0.005(3) -0.006(3) -0.006(3) C5 0.068(6) 0.046(4) 0.047(5) 0.001(4) -0.004(4) -0.010(4) C6 0.075(6) 0.046(4) 0.052(5) -0.008(4) -0.009(5) 0.002(4) C7 0.037(4) 0.054(4) 0.039(4) 0.000(3) -0.004(3) -0.010(3) C8 0.064(6) 0.068(5) 0.044(5) -0.007(4) -0.014(4) -0.011(4) C9 0.080(7) 0.077(6) 0.060(6) -0.011(5) 0.029(5) 0.000(5) C10 0.052(5) 0.043(4) 0.054(5) 0.001(3) -0.002(4) -0.019(3) C11 0.057(4) 0.034(3) 0.067(5) -0.001(4) 0.016(5) -0.007(3) C12 0.052(4) 0.040(4) 0.055(5) 0.014(3) 0.002(4) -0.010(3) C13 0.042(4) 0.044(4) 0.069(6) 0.009(4) 0.019(4) -0.007(3) C14 0.044(4) 0.047(4) 0.069(5) 0.011(4) 0.003(4) -0.020(3) C15 0.090(8) 0.081(6) 0.068(6) -0.025(5) -0.011(6) -0.033(5) C16 0.079(6) 0.049(4) 0.105(9) -0.013(5) 0.028(6) -0.002(4) C17 0.081(6) 0.063(5) 0.071(7) 0.026(5) 0.005(5) -0.002(5) C18 0.080(7) 0.082(7) 0.069(7) 0.006(5) 0.039(6) 0.006(5) C19 0.037(4) 0.072(6) 0.125(10) 0.027(6) -0.013(5) -0.006(4) C20 0.071(5) 0.047(4) 0.054(5) -0.004(4) -0.014(4) -0.030(4) C21 0.081(7) 0.043(4) 0.070(6) -0.031(4) -0.032(5) 0.011(4) C22 0.044(4) 0.076(5) 0.045(5) -0.028(4) -0.003(4) -0.006(4) C23 0.059(5) 0.050(4) 0.035(4) -0.011(3) -0.009(4) -0.008(3) C24 0.040(4) 0.056(4) 0.047(4) -0.006(3) -0.012(3) -0.016(3) C25 0.143(10) 0.095(7) 0.081(8) 0.033(6) -0.031(7) -0.076(8) C26 0.156(10) 0.075(6) 0.154(12) -0.060(8) -0.096(10) 0.065(7) C27 0.075(8) 0.181(12) 0.084(9) -0.076(9) 0.018(6) -0.036(7) C28 0.103(8) 0.088(6) 0.038(5) 0.010(5) -0.018(5) -0.026(6) C29 0.048(6) 0.141(10) 0.072(7) -0.025(7) -0.011(5) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C11 2.147(6) . ? Rh1 C12 2.153(7) . ? Rh1 C13 2.166(7) . ? Rh1 C14 2.185(6) . ? Rh1 C10 2.187(7) . ? Rh1 Cl1 2.4084(18) . ? Rh1 Se1 2.5277(11) . ? Rh1 Se2 2.5351(11) . ? Rh2 C22 2.122(8) . ? Rh2 C24 2.133(7) . ? Rh2 C21 2.134(7) . ? Rh2 C20 2.142(7) . ? Rh2 C23 2.166(8) . ? Rh2 Cl4 2.4153(19) . ? Rh2 Cl2 2.418(2) . ? Rh2 Cl3 2.435(2) . ? Se1 C1 1.867(6) . ? Se2 C4 1.864(7) . ? N1 C1 1.344(8) . ? N1 C2 1.365(9) . ? N1 C8 1.462(9) . ? N2 C1 1.354(8) . ? N2 C3 1.387(8) . ? N2 C7 1.464(8) . ? N3 C4 1.362(9) . ? N3 C5 1.387(9) . ? N3 C7 1.448(9) . ? N4 C4 1.342(9) . ? N4 C6 1.379(9) . ? N4 C9 1.470(10) . ? C2 C3 1.346(10) . ? C5 C6 1.365(11) . ? C10 C14 1.422(11) . ? C10 C11 1.447(11) . ? C10 C15 1.515(12) . ? C11 C12 1.424(12) . ? C11 C16 1.487(10) . ? C12 C13 1.436(10) . ? C12 C17 1.499(11) . ? C13 C14 1.420(12) . ? C13 C18 1.522(11) . ? C14 C19 1.509(10) . ? C20 C21 1.423(12) . ? C20 C24 1.444(11) . ? C20 C25 1.510(12) . ? C21 C22 1.441(13) . ? C21 C26 1.501(12) . ? C22 C23 1.406(11) . ? C22 C27 1.520(12) . ? C23 C24 1.438(10) . ? C23 C28 1.511(11) . ? C24 C29 1.479(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Rh1 C12 38.7(3) . . ? C11 Rh1 C13 64.9(3) . . ? C12 Rh1 C13 38.8(3) . . ? C11 Rh1 C14 64.5(3) . . ? C12 Rh1 C14 64.3(3) . . ? C13 Rh1 C14 38.1(3) . . ? C11 Rh1 C10 39.0(3) . . ? C12 Rh1 C10 64.6(3) . . ? C13 Rh1 C10 64.2(3) . . ? C14 Rh1 C10 38.0(3) . . ? C11 Rh1 Cl1 150.2(2) . . ? C12 Rh1 Cl1 144.8(2) . . ? C13 Rh1 Cl1 106.4(2) . . ? C14 Rh1 Cl1 90.82(19) . . ? C10 Rh1 Cl1 111.2(2) . . ? C11 Rh1 Se1 91.7(2) . . ? C12 Rh1 Se1 122.0(2) . . ? C13 Rh1 Se1 156.6(2) . . ? C14 Rh1 Se1 131.4(3) . . ? C10 Rh1 Se1 96.9(2) . . ? Cl1 Rh1 Se1 93.05(5) . . ? C11 Rh1 Se2 116.9(3) . . ? C12 Rh1 Se2 90.1(2) . . ? C13 Rh1 Se2 100.0(2) . . ? C14 Rh1 Se2 136.3(3) . . ? C10 Rh1 Se2 154.2(2) . . ? Cl1 Rh1 Se2 92.36(5) . . ? Se1 Rh1 Se2 91.95(4) . . ? C22 Rh2 C24 65.8(3) . . ? C22 Rh2 C21 39.6(3) . . ? C24 Rh2 C21 65.7(3) . . ? C22 Rh2 C20 65.9(3) . . ? C24 Rh2 C20 39.5(3) . . ? C21 Rh2 C20 38.9(3) . . ? C22 Rh2 C23 38.3(3) . . ? C24 Rh2 C23 39.1(3) . . ? C21 Rh2 C23 64.7(3) . . ? C20 Rh2 C23 65.1(3) . . ? C22 Rh2 Cl4 107.7(2) . . ? C24 Rh2 Cl4 109.8(2) . . ? C21 Rh2 Cl4 147.0(3) . . ? C20 Rh2 Cl4 149.2(2) . . ? C23 Rh2 Cl4 90.9(2) . . ? C22 Rh2 Cl2 159.1(2) . . ? C24 Rh2 Cl2 97.6(2) . . ? C21 Rh2 Cl2 123.2(3) . . ? C20 Rh2 Cl2 93.2(2) . . ? C23 Rh2 Cl2 132.9(2) . . ? Cl4 Rh2 Cl2 89.50(7) . . ? C22 Rh2 Cl3 101.4(2) . . ? C24 Rh2 Cl3 158.5(2) . . ? C21 Rh2 Cl3 93.3(2) . . ? C20 Rh2 Cl3 120.3(2) . . ? C23 Rh2 Cl3 137.1(2) . . ? Cl4 Rh2 Cl3 90.30(6) . . ? Cl2 Rh2 Cl3 89.99(8) . . ? C1 Se1 Rh1 101.6(2) . . ? C4 Se2 Rh1 103.2(2) . . ? C1 N1 C2 110.1(6) . . ? C1 N1 C8 124.6(6) . . ? C2 N1 C8 125.2(7) . . ? C1 N2 C3 109.7(6) . . ? C1 N2 C7 126.1(5) . . ? C3 N2 C7 123.9(5) . . ? C4 N3 C5 110.3(6) . . ? C4 N3 C7 125.5(6) . . ? C5 N3 C7 124.2(6) . . ? C4 N4 C6 110.2(7) . . ? C4 N4 C9 125.8(7) . . ? C6 N4 C9 124.0(7) . . ? N1 C1 N2 106.0(5) . . ? N1 C1 Se1 126.6(5) . . ? N2 C1 Se1 127.4(5) . . ? C3 C2 N1 107.9(6) . . ? C2 C3 N2 106.3(6) . . ? N4 C4 N3 106.1(6) . . ? N4 C4 Se2 126.5(5) . . ? N3 C4 Se2 127.4(5) . . ? C6 C5 N3 105.8(7) . . ? C5 C6 N4 107.7(7) . . ? N3 C7 N2 112.1(5) . . ? C14 C10 C11 107.3(7) . . ? C14 C10 C15 126.3(8) . . ? C11 C10 C15 126.4(8) . . ? C14 C10 Rh1 70.9(4) . . ? C11 C10 Rh1 69.0(4) . . ? C15 C10 Rh1 126.4(6) . . ? C12 C11 C10 107.9(6) . . ? C12 C11 C16 126.4(9) . . ? C10 C11 C16 125.3(9) . . ? C12 C11 Rh1 70.9(4) . . ? C10 C11 Rh1 72.0(4) . . ? C16 C11 Rh1 128.6(5) . . ? C11 C12 C13 108.0(7) . . ? C11 C12 C17 125.1(7) . . ? C13 C12 C17 126.7(8) . . ? C11 C12 Rh1 70.4(4) . . ? C13 C12 Rh1 71.1(4) . . ? C17 C12 Rh1 127.5(5) . . ? C14 C13 C12 107.8(7) . . ? C14 C13 C18 127.0(7) . . ? C12 C13 C18 125.2(8) . . ? C14 C13 Rh1 71.7(4) . . ? C12 C13 Rh1 70.1(4) . . ? C18 C13 Rh1 125.9(5) . . ? C13 C14 C10 109.0(7) . . ? C13 C14 C19 125.9(9) . . ? C10 C14 C19 125.1(9) . . ? C13 C14 Rh1 70.3(4) . . ? C10 C14 Rh1 71.1(4) . . ? C19 C14 Rh1 125.3(5) . . ? C21 C20 C24 107.7(7) . . ? C21 C20 C25 127.4(9) . . ? C24 C20 C25 124.9(9) . . ? C21 C20 Rh2 70.3(4) . . ? C24 C20 Rh2 69.9(4) . . ? C25 C20 Rh2 126.8(7) . . ? C20 C21 C22 108.2(7) . . ? C20 C21 C26 126.7(10) . . ? C22 C21 C26 125.1(10) . . ? C20 C21 Rh2 70.9(4) . . ? C22 C21 Rh2 69.8(4) . . ? C26 C21 Rh2 125.4(6) . . ? C23 C22 C21 107.9(7) . . ? C23 C22 C27 126.6(10) . . ? C21 C22 C27 125.3(9) . . ? C23 C22 Rh2 72.5(4) . . ? C21 C22 Rh2 70.6(5) . . ? C27 C22 Rh2 126.2(6) . . ? C22 C23 C24 108.8(7) . . ? C22 C23 C28 128.0(8) . . ? C24 C23 C28 123.2(7) . . ? C22 C23 Rh2 69.2(4) . . ? C24 C23 Rh2 69.2(4) . . ? C28 C23 Rh2 127.2(5) . . ? C23 C24 C20 107.2(7) . . ? C23 C24 C29 126.9(8) . . ? C20 C24 C29 125.7(8) . . ? C23 C24 Rh2 71.7(4) . . ? C20 C24 Rh2 70.6(4) . . ? C29 C24 Rh2 126.2(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.020 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.128 data_f70603b _database_code_depnum_ccdc_archive 'CCDC 676483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H29 Cl2 N4 Rh S2' _chemical_formula_weight 563.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.789(3) _cell_length_b 10.128(2) _cell_length_c 12.405(3) _cell_angle_alpha 84.114(14) _cell_angle_beta 73.09(3) _cell_angle_gamma 88.317(12) _cell_volume 1170.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 884 _cell_measurement_theta_min 2.530 _cell_measurement_theta_max 26.986 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8463 _exptl_absorpt_correction_T_max 0.8936 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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_% 7.13 _diffrn_reflns_number 6894 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.12 _reflns_number_total 4971 _reflns_number_gt 4299 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.6098P] 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 4971 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0439 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0915 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.71706(2) 0.71858(2) 0.66388(2) 0.03098(9) Uani 1 1 d . . . Cl1 Cl 0.60334(9) 0.72978(9) 0.86166(7) 0.04325(19) Uani 1 1 d . . . Cl2 Cl 0.88841(10) 0.75397(10) 0.13286(9) 0.0559(2) Uani 1 1 d . . . N1 N 0.2790(3) 0.7014(3) 0.8322(2) 0.0422(6) Uani 1 1 d . . . N2 N 0.3201(3) 0.8961(3) 0.7417(2) 0.0366(6) Uani 1 1 d . . . N3 N 0.5172(3) 1.0949(3) 0.7632(2) 0.0371(6) Uani 1 1 d . . . N4 N 0.6914(3) 1.0478(3) 0.8344(2) 0.0382(6) Uani 1 1 d . . . S1 S 0.48742(8) 0.70274(9) 0.62891(7) 0.04005(19) Uani 1 1 d . . . S2 S 0.73526(9) 0.96012(8) 0.62393(7) 0.03661(18) Uani 1 1 d . . . C1 C 0.8752(5) 0.5785(4) 0.6968(4) 0.0627(12) Uani 1 1 d . . . C2 C 0.7814(4) 0.5180(4) 0.6417(4) 0.0640(13) Uani 1 1 d . . . C3 C 0.8036(4) 0.5879(4) 0.5333(4) 0.0489(9) Uani 1 1 d . . . C4 C 0.9018(3) 0.6910(3) 0.5205(3) 0.0412(7) Uani 1 1 d . . . C5 C 0.9471(3) 0.6857(4) 0.6209(3) 0.0436(8) Uani 1 1 d . . . C6 C 0.8934(7) 0.5350(7) 0.8094(5) 0.112(3) Uani 1 1 d . . . H6A H 0.9711 0.4731 0.8011 0.168 Uiso 1 1 calc R . . H6B H 0.8073 0.4930 0.8572 0.168 Uiso 1 1 calc R . . H6C H 0.9136 0.6106 0.8430 0.168 Uiso 1 1 calc R . . C7 C 0.6867(6) 0.3993(5) 0.6838(7) 0.123(3) Uani 1 1 d . . . H7A H 0.5961 0.4177 0.6701 0.185 Uiso 1 1 calc R . . H7B H 0.6728 0.3792 0.7636 0.185 Uiso 1 1 calc R . . H7C H 0.7303 0.3249 0.6448 0.185 Uiso 1 1 calc R . . C8 C 0.7391(5) 0.5568(5) 0.4403(5) 0.0808(17) Uani 1 1 d . . . H8A H 0.7012 0.6367 0.4114 0.121 Uiso 1 1 calc R . . H8B H 0.6639 0.4928 0.4710 0.121 Uiso 1 1 calc R . . H8C H 0.8118 0.5215 0.3802 0.121 Uiso 1 1 calc R . . C9 C 0.9576(4) 0.7859(5) 0.4168(3) 0.0598(10) Uani 1 1 d . . . H9A H 1.0533 0.7616 0.3776 0.090 Uiso 1 1 calc R . . H9B H 0.9571 0.8742 0.4384 0.090 Uiso 1 1 calc R . . H9C H 0.8979 0.7826 0.3678 0.090 Uiso 1 1 calc R . . C10 C 1.0582(4) 0.7752(5) 0.6357(5) 0.0688(13) Uani 1 1 d . . . H10A H 1.0428 0.7828 0.7149 0.103 Uiso 1 1 calc R . . H10B H 1.0518 0.8614 0.5973 0.103 Uiso 1 1 calc R . . H10C H 1.1513 0.7386 0.6044 0.103 Uiso 1 1 calc R . . C11 C 0.6464(3) 1.0337(3) 0.7434(3) 0.0330(6) Uani 1 1 d . . . C12 C 0.8249(4) 0.9951(4) 0.8508(4) 0.0527(9) Uani 1 1 d . . . H12A H 0.8061 0.9466 0.9243 0.079 Uiso 1 1 calc R . . H12B H 0.8890 1.0671 0.8454 0.079 Uiso 1 1 calc R . . H12C H 0.8675 0.9370 0.7937 0.079 Uiso 1 1 calc R . . C13 C 0.5919(4) 1.1167(3) 0.9094(3) 0.0459(8) Uani 1 1 d . . . H13 H 0.5987 1.1391 0.9785 0.055 Uiso 1 1 calc R . . C14 C 0.4835(4) 1.1462(3) 0.8666(3) 0.0442(8) Uani 1 1 d . . . H14 H 0.4010 1.1924 0.9000 0.053 Uiso 1 1 calc R . . C15 C 0.4311(4) 1.1213(4) 0.6848(3) 0.0460(8) Uani 1 1 d . . . H15A H 0.4870 1.1747 0.6180 0.055 Uiso 1 1 calc R . . H15B H 0.3485 1.1731 0.7205 0.055 Uiso 1 1 calc R . . C16 C 0.3805(4) 0.9994(4) 0.6483(3) 0.0467(8) Uani 1 1 d . . . H16A H 0.3086 1.0253 0.6105 0.056 Uiso 1 1 calc R . . H16B H 0.4602 0.9618 0.5936 0.056 Uiso 1 1 calc R . . C17 C 0.2126(4) 0.9108(4) 0.8387(3) 0.0463(8) Uani 1 1 d . . . H17 H 0.1666 0.9893 0.8612 0.056 Uiso 1 1 calc R . . C18 C 0.1866(4) 0.7894(4) 0.8952(3) 0.0523(10) Uani 1 1 d . . . H18 H 0.1185 0.7683 0.9644 0.063 Uiso 1 1 calc R . . C19 C 0.2887(5) 0.5604(4) 0.8649(4) 0.0645(11) Uani 1 1 d . . . H19A H 0.3069 0.5127 0.7992 0.097 Uiso 1 1 calc R . . H19B H 0.2004 0.5303 0.9186 0.097 Uiso 1 1 calc R . . H19C H 0.3652 0.5449 0.8986 0.097 Uiso 1 1 calc R . . C20 C 0.3611(3) 0.7686(3) 0.7377(3) 0.0348(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02591(13) 0.03284(14) 0.03249(15) -0.00513(9) -0.00502(9) -0.00143(9) Cl1 0.0444(4) 0.0522(5) 0.0315(4) -0.0047(3) -0.0078(3) -0.0058(4) Cl2 0.0465(5) 0.0542(5) 0.0557(6) -0.0072(4) 0.0031(4) 0.0038(4) N1 0.0345(14) 0.0527(17) 0.0370(15) -0.0036(12) -0.0056(12) -0.0130(12) N2 0.0304(13) 0.0455(15) 0.0354(14) -0.0089(11) -0.0101(11) -0.0013(11) N3 0.0344(13) 0.0353(13) 0.0368(15) -0.0003(11) -0.0038(11) -0.0020(11) N4 0.0408(14) 0.0365(14) 0.0366(15) -0.0067(11) -0.0087(12) -0.0050(11) S1 0.0295(4) 0.0546(5) 0.0366(4) -0.0160(4) -0.0062(3) -0.0028(3) S2 0.0377(4) 0.0367(4) 0.0309(4) -0.0044(3) -0.0019(3) -0.0051(3) C1 0.055(2) 0.066(3) 0.056(2) 0.010(2) -0.0077(19) 0.032(2) C2 0.0394(19) 0.0319(18) 0.100(4) -0.003(2) 0.010(2) 0.0041(15) C3 0.0338(17) 0.0427(19) 0.069(3) -0.0241(18) -0.0061(17) 0.0032(14) C4 0.0297(15) 0.0431(18) 0.0474(19) -0.0164(15) -0.0023(14) 0.0035(13) C5 0.0287(15) 0.051(2) 0.051(2) -0.0136(16) -0.0093(14) 0.0105(14) C6 0.103(5) 0.137(6) 0.077(4) 0.031(4) -0.015(3) 0.061(4) C7 0.079(4) 0.041(3) 0.197(8) 0.020(3) 0.033(4) -0.002(2) C8 0.054(3) 0.096(4) 0.107(4) -0.070(3) -0.027(3) 0.011(2) C9 0.049(2) 0.073(3) 0.044(2) -0.0022(19) 0.0051(17) 0.0038(19) C10 0.042(2) 0.082(3) 0.093(4) -0.037(3) -0.027(2) 0.002(2) C11 0.0340(15) 0.0279(14) 0.0343(16) -0.0020(12) -0.0049(13) -0.0069(12) C12 0.051(2) 0.061(2) 0.054(2) -0.0102(18) -0.0257(18) -0.0031(18) C13 0.060(2) 0.0410(18) 0.0329(18) -0.0078(14) -0.0049(16) -0.0079(16) C14 0.0476(19) 0.0348(17) 0.0392(18) -0.0035(13) 0.0049(15) -0.0033(14) C15 0.0421(18) 0.0465(19) 0.044(2) 0.0054(15) -0.0087(15) 0.0039(15) C16 0.048(2) 0.057(2) 0.0370(19) 0.0009(16) -0.0165(16) 0.0019(16) C17 0.0336(16) 0.061(2) 0.045(2) -0.0197(17) -0.0066(15) 0.0006(15) C18 0.0327(17) 0.085(3) 0.0353(19) -0.0200(19) 0.0025(14) -0.0125(18) C19 0.070(3) 0.055(2) 0.063(3) 0.004(2) -0.012(2) -0.022(2) C20 0.0261(14) 0.0467(18) 0.0334(16) -0.0078(13) -0.0097(12) -0.0053(12) _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 C2 2.131(4) . ? Rh1 C3 2.161(3) . ? Rh1 C1 2.167(4) . ? Rh1 C4 2.171(3) . ? Rh1 C5 2.181(3) . ? Rh1 Cl1 2.3942(11) . ? Rh1 S1 2.4228(11) . ? Rh1 S2 2.4470(10) . ? N1 C20 1.343(4) . ? N1 C18 1.380(5) . ? N1 C19 1.453(5) . ? N2 C20 1.342(4) . ? N2 C17 1.368(4) . ? N2 C16 1.475(4) . ? N3 C11 1.359(4) . ? N3 C14 1.381(4) . ? N3 C15 1.462(4) . ? N4 C11 1.347(4) . ? N4 C13 1.367(5) . ? N4 C12 1.458(5) . ? S1 C20 1.721(3) . ? S2 C11 1.717(3) . ? C1 C5 1.418(6) . ? C1 C2 1.473(7) . ? C1 C6 1.481(7) . ? C2 C3 1.414(6) . ? C2 C7 1.493(6) . ? C3 C4 1.406(5) . ? C3 C8 1.529(6) . ? C4 C5 1.434(5) . ? C4 C9 1.499(5) . ? C5 C10 1.499(5) . ? C13 C14 1.332(5) . ? C15 C16 1.502(5) . ? C17 C18 1.344(6) . ? 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 Rh1 C3 38.46(17) . . ? C2 Rh1 C1 40.08(19) . . ? C3 Rh1 C1 64.92(17) . . ? C2 Rh1 C4 64.49(14) . . ? C3 Rh1 C4 37.87(13) . . ? C1 Rh1 C4 64.26(15) . . ? C2 Rh1 C5 65.30(15) . . ? C3 Rh1 C5 64.21(13) . . ? C1 Rh1 C5 38.07(15) . . ? C4 Rh1 C5 38.48(13) . . ? C2 Rh1 Cl1 107.27(14) . . ? C3 Rh1 Cl1 145.11(11) . . ? C1 Rh1 Cl1 92.34(12) . . ? C4 Rh1 Cl1 152.69(10) . . ? C5 Rh1 Cl1 114.25(10) . . ? C2 Rh1 S1 97.15(13) . . ? C3 Rh1 S1 88.54(10) . . ? C1 Rh1 S1 135.55(14) . . ? C4 Rh1 S1 115.46(10) . . ? C5 Rh1 S1 152.24(10) . . ? Cl1 Rh1 S1 90.91(4) . . ? C2 Rh1 S2 155.88(11) . . ? C3 Rh1 S2 121.68(11) . . ? C1 Rh1 S2 128.79(14) . . ? C4 Rh1 S2 91.48(10) . . ? C5 Rh1 S2 94.92(10) . . ? Cl1 Rh1 S2 93.12(3) . . ? S1 Rh1 S2 95.22(3) . . ? C20 N1 C18 108.7(3) . . ? C20 N1 C19 125.8(3) . . ? C18 N1 C19 125.5(3) . . ? C20 N2 C17 110.3(3) . . ? C20 N2 C16 122.5(3) . . ? C17 N2 C16 127.1(3) . . ? C11 N3 C14 109.5(3) . . ? C11 N3 C15 127.5(3) . . ? C14 N3 C15 122.5(3) . . ? C11 N4 C13 109.6(3) . . ? C11 N4 C12 125.0(3) . . ? C13 N4 C12 125.4(3) . . ? C20 S1 Rh1 107.74(10) . . ? C11 S2 Rh1 109.61(11) . . ? C5 C1 C2 107.2(4) . . ? C5 C1 C6 126.1(5) . . ? C2 C1 C6 126.8(5) . . ? C5 C1 Rh1 71.5(2) . . ? C2 C1 Rh1 68.6(2) . . ? C6 C1 Rh1 125.7(3) . . ? C3 C2 C1 107.1(3) . . ? C3 C2 C7 124.1(5) . . ? C1 C2 C7 128.7(5) . . ? C3 C2 Rh1 71.9(2) . . ? C1 C2 Rh1 71.3(2) . . ? C7 C2 Rh1 125.4(3) . . ? C4 C3 C2 109.0(4) . . ? C4 C3 C8 123.7(4) . . ? C2 C3 C8 127.3(4) . . ? C4 C3 Rh1 71.45(19) . . ? C2 C3 Rh1 69.6(2) . . ? C8 C3 Rh1 127.0(3) . . ? C3 C4 C5 108.7(3) . . ? C3 C4 C9 126.0(4) . . ? C5 C4 C9 125.2(3) . . ? C3 C4 Rh1 70.7(2) . . ? C5 C4 Rh1 71.15(19) . . ? C9 C4 Rh1 126.9(3) . . ? C1 C5 C4 108.0(3) . . ? C1 C5 C10 127.8(4) . . ? C4 C5 C10 124.1(4) . . ? C1 C5 Rh1 70.4(2) . . ? C4 C5 Rh1 70.37(18) . . ? C10 C5 Rh1 127.6(3) . . ? N4 C11 N3 105.8(3) . . ? N4 C11 S2 127.7(2) . . ? N3 C11 S2 126.5(2) . . ? C14 C13 N4 108.3(3) . . ? C13 C14 N3 106.7(3) . . ? N3 C15 C16 114.7(3) . . ? N2 C16 C15 114.2(3) . . ? C18 C17 N2 106.4(3) . . ? C17 C18 N1 107.9(3) . . ? N2 C20 N1 106.7(3) . . ? N2 C20 S1 126.6(2) . . ? N1 C20 S1 126.7(3) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.847 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.088