Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_address ; Department of Chemistry Fudan University Shanghai Key Lab of Molecular Catal Shanghai 200433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; A Facile and General Approach to the Rh-M (M = Co, Rh) Single Bond Supported by ortho-Carborane-1,2-Dichalcogenolato Ligands ; loop_ _publ_author_name 'Guo-Xin Jin.' 'Shuang Liu.' data_f51206b _database_code_depnum_ccdc_archive 'CCDC 616710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H30 B10 Co Rh S2' _chemical_formula_weight 568.47 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 '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 20.444(7) _cell_length_b 12.367(4) _cell_length_c 9.933(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2511.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 759 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 22.17 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8654 _exptl_absorpt_correction_T_max 0.9293 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11020 _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.01 _reflns_number_total 2588 _reflns_number_gt 1665 _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^)+(0.0483P)^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 2588 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.941 _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 Co1 Co 0.25144(4) 0.2500 0.29490(8) 0.0533(3) Uani 1 2 d S . . Rh1 Rh 0.31085(2) 0.2500 0.51233(4) 0.04645(18) Uani 1 2 d S . . S1 S 0.22840(5) 0.12888(10) 0.45171(12) 0.0523(3) Uani 1 1 d . . . B3 B 0.1694(4) 0.2500 0.6842(7) 0.059(2) Uani 1 2 d S . . H3 H 0.2162 0.2500 0.7391 0.071 Uiso 1 2 calc SR . . B4 B 0.1200(3) 0.1338(5) 0.6757(6) 0.0731(18) Uani 1 1 d . . . H4 H 0.1346 0.0574 0.7238 0.088 Uiso 1 1 calc R . . B5 B 0.0773(3) 0.1351(6) 0.5220(6) 0.079(2) Uani 1 1 d . . . H5 H 0.0638 0.0595 0.4708 0.095 Uiso 1 1 calc R . . B6 B 0.1009(3) 0.2500 0.4305(8) 0.068(2) Uani 1 2 d S . . H6 H 0.1032 0.2500 0.3199 0.082 Uiso 1 2 calc SR . . B7 B 0.0949(4) 0.2500 0.7674(8) 0.071(3) Uani 1 2 d S . . H7 H 0.0919 0.2500 0.8779 0.085 Uiso 1 2 calc SR . . B8 B 0.0388(3) 0.1791(5) 0.6693(6) 0.080(2) Uani 1 1 d . . . H8 H -0.0010 0.1322 0.7158 0.096 Uiso 1 1 calc R . . B9 B 0.0281(4) 0.2500 0.5187(9) 0.084(3) Uani 1 2 d S . . H9 H -0.0191 0.2500 0.4655 0.101 Uiso 1 2 calc SR . . C1 C 0.1553(2) 0.1843(4) 0.5342(4) 0.0504(11) Uani 1 1 d . . . C2 C 0.36733(19) 0.1937(3) 0.6859(4) 0.0553(13) Uani 1 1 d . . . C3 C 0.3971(2) 0.1577(5) 0.5631(5) 0.0710(16) Uani 1 1 d . . . C4 C 0.4183(3) 0.2500 0.4912(7) 0.091(3) Uani 1 2 d S . . C5 C 0.3432(3) 0.1225(5) 0.7984(5) 0.098(2) Uani 1 1 d . . . H5A H 0.3256 0.0569 0.7615 0.147 Uiso 1 1 calc R . . H5B H 0.3097 0.1596 0.8479 0.147 Uiso 1 1 calc R . . H5C H 0.3789 0.1055 0.8575 0.147 Uiso 1 1 calc R . . C6 C 0.4092(3) 0.0405(5) 0.5301(7) 0.142(3) Uani 1 1 d . . . H6A H 0.4422 0.0121 0.5892 0.213 Uiso 1 1 calc R . . H6B H 0.4238 0.0343 0.4385 0.213 Uiso 1 1 calc R . . H6C H 0.3694 0.0003 0.5414 0.213 Uiso 1 1 calc R . . C7 C 0.4601(4) 0.2500 0.3683(8) 0.183(6) Uani 1 2 d S . . H7A H 0.4603 0.1790 0.3292 0.274 Uiso 0.50 1 calc PR . . H7B H 0.5039 0.2701 0.3921 0.274 Uiso 0.50 1 calc PR . . H7C H 0.4430 0.3009 0.3043 0.274 Uiso 0.50 1 calc PR . . C8 C 0.3145(3) 0.1969(5) 0.1506(5) 0.095(2) Uani 1 1 d . . . H8A H 0.3509 0.1536 0.1663 0.114 Uiso 1 1 calc R . . C9 C 0.2530(4) 0.1596(6) 0.1240(6) 0.110(3) Uani 1 1 d . . . H9A H 0.2405 0.0873 0.1206 0.132 Uiso 1 1 calc R . . C10 C 0.2112(5) 0.2500 0.1024(8) 0.124(5) Uani 1 2 d S . . H10 H 0.1671 0.2500 0.0795 0.149 Uiso 1 2 calc SR . . 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 Co1 0.0543(5) 0.0764(7) 0.0292(5) 0.000 0.0018(4) 0.000 Rh1 0.0369(3) 0.0705(4) 0.0320(3) 0.000 0.0017(2) 0.000 S1 0.0496(7) 0.0579(8) 0.0493(7) -0.0031(6) 0.0074(5) -0.0001(6) B3 0.050(4) 0.092(7) 0.036(4) 0.000 0.002(3) 0.000 B4 0.065(4) 0.092(5) 0.062(4) 0.014(3) 0.019(3) -0.012(3) B5 0.050(3) 0.106(5) 0.082(5) -0.021(4) 0.011(3) -0.024(3) B6 0.048(5) 0.111(8) 0.047(5) 0.000 -0.010(4) 0.000 B7 0.052(5) 0.115(8) 0.046(5) 0.000 0.016(4) 0.000 B8 0.045(3) 0.122(5) 0.073(4) 0.001(4) 0.020(3) -0.014(3) B9 0.040(4) 0.139(9) 0.073(6) 0.000 -0.001(4) 0.000 C1 0.040(2) 0.065(3) 0.047(3) -0.003(2) 0.004(2) -0.004(2) C2 0.038(2) 0.076(3) 0.052(3) 0.005(2) -0.011(2) 0.007(2) C3 0.041(3) 0.106(5) 0.066(3) -0.032(3) -0.011(3) 0.021(3) C4 0.034(4) 0.197(11) 0.041(4) 0.000 0.002(3) 0.000 C5 0.087(4) 0.126(5) 0.081(4) 0.046(4) -0.012(3) -0.007(4) C6 0.102(5) 0.150(7) 0.175(7) -0.088(6) -0.049(5) 0.062(5) C7 0.045(5) 0.45(2) 0.056(6) 0.000 0.026(4) 0.000 C8 0.113(5) 0.125(6) 0.046(3) -0.007(3) 0.030(3) 0.026(4) C9 0.170(8) 0.118(7) 0.042(4) -0.031(4) 0.022(4) -0.065(5) C10 0.080(7) 0.260(17) 0.031(4) 0.000 -0.015(4) 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 Co1 C9 2.033(6) . ? Co1 C9 2.033(6) 7_565 ? Co1 C8 2.036(5) 7_565 ? Co1 C8 2.036(5) . ? Co1 C10 2.082(8) . ? Co1 S1 2.2117(14) 7_565 ? Co1 S1 2.2117(14) . ? Co1 Rh1 2.4778(11) . ? Rh1 C3 2.161(5) 7_565 ? Rh1 C3 2.161(5) . ? Rh1 C2 2.189(4) 7_565 ? Rh1 C2 2.189(4) . ? Rh1 C4 2.206(7) . ? Rh1 S1 2.3339(13) . ? Rh1 S1 2.3339(13) 7_565 ? S1 C1 1.837(4) . ? B3 C1 1.722(7) . ? B3 C1 1.722(7) 7_565 ? B3 B7 1.734(10) . ? B3 B4 1.759(7) . ? B3 B4 1.759(7) 7_565 ? B3 H3 1.1000 . ? B4 C1 1.699(7) . ? B4 B8 1.754(8) . ? B4 B5 1.759(8) . ? B4 B7 1.777(7) . ? B4 H4 1.1000 . ? B5 C1 1.710(6) . ? B5 B9 1.741(8) . ? B5 B8 1.748(8) . ? B5 B6 1.754(8) . ? B5 H5 1.1000 . ? B6 C1 1.720(8) 7_565 ? B6 C1 1.720(8) . ? B6 B9 1.727(11) . ? B6 B5 1.754(8) 7_565 ? B6 H6 1.1000 . ? B7 B8 1.742(9) . ? B7 B8 1.742(9) 7_565 ? B7 B4 1.777(8) 7_565 ? B7 H7 1.1000 . ? B8 B9 1.748(9) . ? B8 B8 1.755(13) 7_565 ? B8 H8 1.1000 . ? B9 B5 1.741(8) 7_565 ? B9 B8 1.748(9) 7_565 ? B9 H9 1.1000 . ? C1 C1 1.626(9) 7_565 ? C2 C2 1.392(9) 7_565 ? C2 C3 1.435(6) . ? C2 C5 1.506(6) . ? C3 C4 1.414(6) . ? C3 C6 1.507(8) . ? C4 C3 1.414(6) 7_565 ? C4 C7 1.491(9) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C8 1.313(11) 7_565 ? C8 C9 1.365(7) . ? C8 H8A 0.9300 . ? C9 C10 1.423(8) . ? C9 H9A 0.9300 . ? C10 C9 1.423(8) 7_565 ? C10 H10 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Co1 C9 66.7(4) . 7_565 ? C9 Co1 C8 65.2(2) . 7_565 ? C9 Co1 C8 39.2(2) 7_565 7_565 ? C9 Co1 C8 39.2(2) . . ? C9 Co1 C8 65.2(2) 7_565 . ? C8 Co1 C8 37.6(3) 7_565 . ? C9 Co1 C10 40.4(2) . . ? C9 Co1 C10 40.4(2) 7_565 . ? C8 Co1 C10 66.6(3) 7_565 . ? C8 Co1 C10 66.6(3) . . ? C9 Co1 S1 164.5(2) . 7_565 ? C9 Co1 S1 102.6(2) 7_565 7_565 ? C8 Co1 S1 114.33(16) 7_565 7_565 ? C8 Co1 S1 148.10(18) . 7_565 ? C10 Co1 S1 124.25(16) . 7_565 ? C9 Co1 S1 102.6(2) . . ? C9 Co1 S1 164.5(2) 7_565 . ? C8 Co1 S1 148.10(18) 7_565 . ? C8 Co1 S1 114.33(16) . . ? C10 Co1 S1 124.25(16) . . ? S1 Co1 S1 85.26(7) 7_565 . ? C9 Co1 Rh1 136.1(2) . . ? C9 Co1 Rh1 136.1(2) 7_565 . ? C8 Co1 Rh1 107.66(18) 7_565 . ? C8 Co1 Rh1 107.66(18) . . ? C10 Co1 Rh1 173.9(3) . . ? S1 Co1 Rh1 59.37(4) 7_565 . ? S1 Co1 Rh1 59.37(4) . . ? C3 Rh1 C3 63.8(3) 7_565 . ? C3 Rh1 C2 38.51(16) 7_565 7_565 ? C3 Rh1 C2 63.49(17) . 7_565 ? C3 Rh1 C2 63.49(17) 7_565 . ? C3 Rh1 C2 38.51(16) . . ? C2 Rh1 C2 37.1(2) 7_565 . ? C3 Rh1 C4 37.77(16) 7_565 . ? C3 Rh1 C4 37.77(16) . . ? C2 Rh1 C4 63.3(2) 7_565 . ? C2 Rh1 C4 63.3(2) . . ? C3 Rh1 S1 171.42(15) 7_565 . ? C3 Rh1 S1 108.11(15) . . ? C2 Rh1 S1 142.03(12) 7_565 . ? C2 Rh1 S1 112.33(12) . . ? C4 Rh1 S1 133.97(9) . . ? C3 Rh1 S1 108.11(15) 7_565 7_565 ? C3 Rh1 S1 171.42(15) . 7_565 ? C2 Rh1 S1 112.33(12) 7_565 7_565 ? C2 Rh1 S1 142.03(12) . 7_565 ? C4 Rh1 S1 133.97(9) . 7_565 ? S1 Rh1 S1 79.85(6) . 7_565 ? C3 Rh1 Co1 127.12(13) 7_565 . ? C3 Rh1 Co1 127.12(13) . . ? C2 Rh1 Co1 160.94(11) 7_565 . ? C2 Rh1 Co1 160.94(11) . . ? C4 Rh1 Co1 113.89(18) . . ? S1 Rh1 Co1 54.63(3) . . ? S1 Rh1 Co1 54.63(3) 7_565 . ? C1 S1 Co1 103.57(15) . . ? C1 S1 Rh1 103.49(14) . . ? Co1 S1 Rh1 66.00(4) . . ? C1 B3 C1 56.3(4) . 7_565 ? C1 B3 B7 105.3(5) . . ? C1 B3 B7 105.3(5) 7_565 . ? C1 B3 B4 58.4(3) . . ? C1 B3 B4 104.3(5) 7_565 . ? B7 B3 B4 61.2(3) . . ? C1 B3 B4 104.3(5) . 7_565 ? C1 B3 B4 58.4(3) 7_565 7_565 ? B7 B3 B4 61.2(3) . 7_565 ? B4 B3 B4 109.6(6) . 7_565 ? C1 B3 H3 125.1 . . ? C1 B3 H3 125.1 7_565 . ? B7 B3 H3 121.8 . . ? B4 B3 H3 121.5 . . ? B4 B3 H3 121.5 7_565 . ? C1 B4 B8 104.8(4) . . ? C1 B4 B5 59.2(3) . . ? B8 B4 B5 59.7(3) . . ? C1 B4 B3 59.7(3) . . ? B8 B4 B3 106.6(5) . . ? B5 B4 B3 108.6(5) . . ? C1 B4 B7 104.5(4) . . ? B8 B4 B7 59.1(4) . . ? B5 B4 B7 107.1(5) . . ? B3 B4 B7 58.7(4) . . ? C1 B4 H4 124.0 . . ? B8 B4 H4 123.2 . . ? B5 B4 H4 121.3 . . ? B3 B4 H4 121.7 . . ? B7 B4 H4 123.4 . . ? C1 B5 B9 104.5(5) . . ? C1 B5 B8 104.5(4) . . ? B9 B5 B8 60.1(4) . . ? C1 B5 B6 59.5(3) . . ? B9 B5 B6 59.2(4) . . ? B8 B5 B6 107.8(5) . . ? C1 B5 B4 58.6(3) . . ? B9 B5 B4 108.1(5) . . ? B8 B5 B4 60.0(3) . . ? B6 B5 B4 108.7(4) . . ? C1 B5 H5 124.7 . . ? B9 B5 H5 122.7 . . ? B8 B5 H5 122.5 . . ? B6 B5 H5 121.3 . . ? B4 B5 H5 121.2 . . ? C1 B6 C1 56.4(4) 7_565 . ? C1 B6 B9 104.7(5) 7_565 . ? C1 B6 B9 104.7(5) . . ? C1 B6 B5 59.0(3) 7_565 7_565 ? C1 B6 B5 104.5(5) . 7_565 ? B9 B6 B5 60.0(3) . 7_565 ? C1 B6 B5 104.5(5) 7_565 . ? C1 B6 B5 59.0(3) . . ? B9 B6 B5 60.0(3) . . ? B5 B6 B5 108.2(6) 7_565 . ? C1 B6 H6 124.8 7_565 . ? C1 B6 H6 124.8 . . ? B9 B6 H6 122.9 . . ? B5 B6 H6 122.0 7_565 . ? B5 B6 H6 122.0 . . ? B3 B7 B8 108.2(5) . . ? B3 B7 B8 108.2(5) . 7_565 ? B8 B7 B8 60.5(5) . 7_565 ? B3 B7 B4 60.1(3) . 7_565 ? B8 B7 B4 108.1(5) . 7_565 ? B8 B7 B4 59.8(3) 7_565 7_565 ? B3 B7 B4 60.1(3) . . ? B8 B7 B4 59.8(3) . . ? B8 B7 B4 108.1(5) 7_565 . ? B4 B7 B4 107.9(6) 7_565 . ? B3 B7 H7 121.5 . . ? B8 B7 H7 121.5 . . ? B8 B7 H7 121.5 7_565 . ? B4 B7 H7 121.8 7_565 . ? B4 B7 H7 121.8 . . ? B7 B8 B9 108.0(5) . . ? B7 B8 B5 109.1(4) . . ? B9 B8 B5 59.7(4) . . ? B7 B8 B4 61.1(3) . . ? B9 B8 B4 108.1(5) . . ? B5 B8 B4 60.3(3) . . ? B7 B8 B8 59.8(3) . 7_565 ? B9 B8 B8 59.9(3) . 7_565 ? B5 B8 B8 108.1(3) . 7_565 ? B4 B8 B8 108.6(3) . 7_565 ? B7 B8 H8 121.1 . . ? B9 B8 H8 122.1 . . ? B5 B8 H8 121.4 . . ? B4 B8 H8 121.1 . . ? B8 B8 H8 121.8 7_565 . ? B6 B9 B5 60.7(3) . 7_565 ? B6 B9 B5 60.7(3) . . ? B5 B9 B5 109.3(6) 7_565 . ? B6 B9 B8 109.0(5) . 7_565 ? B5 B9 B8 60.1(3) 7_565 7_565 ? B5 B9 B8 108.7(6) . 7_565 ? B6 B9 B8 109.0(5) . . ? B5 B9 B8 108.7(6) 7_565 . ? B5 B9 B8 60.1(3) . . ? B8 B9 B8 60.3(5) 7_565 . ? B6 B9 H9 120.8 . . ? B5 B9 H9 121.1 7_565 . ? B5 B9 H9 121.1 . . ? B8 B9 H9 121.4 7_565 . ? B8 B9 H9 121.4 . . ? C1 C1 B4 111.6(3) 7_565 . ? C1 C1 B5 110.8(3) 7_565 . ? B4 C1 B5 62.1(3) . . ? C1 C1 B6 61.79(18) 7_565 . ? B4 C1 B6 113.2(4) . . ? B5 C1 B6 61.5(3) . . ? C1 C1 B3 61.83(19) 7_565 . ? B4 C1 B3 61.9(3) . . ? B5 C1 B3 112.7(4) . . ? B6 C1 B3 113.8(4) . . ? C1 C1 S1 111.90(14) 7_565 . ? B4 C1 S1 125.3(3) . . ? B5 C1 S1 126.5(3) . . ? B6 C1 S1 115.8(4) . . ? B3 C1 S1 115.2(3) . . ? C2 C2 C3 108.1(3) 7_565 . ? C2 C2 C5 125.8(3) 7_565 . ? C3 C2 C5 126.1(5) . . ? C2 C2 Rh1 71.45(11) 7_565 . ? C3 C2 Rh1 69.7(3) . . ? C5 C2 Rh1 126.7(3) . . ? C4 C3 C2 108.0(5) . . ? C4 C3 C6 128.1(5) . . ? C2 C3 C6 123.6(6) . . ? C4 C3 Rh1 72.8(4) . . ? C2 C3 Rh1 71.8(2) . . ? C6 C3 Rh1 126.3(4) . . ? C3 C4 C3 107.7(6) 7_565 . ? C3 C4 C7 126.1(3) 7_565 . ? C3 C4 C7 126.1(3) . . ? C3 C4 Rh1 69.4(3) 7_565 . ? C3 C4 Rh1 69.4(3) . . ? C7 C4 Rh1 130.5(5) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 C8 C9 109.8(4) 7_565 . ? C8 C8 Co1 71.18(16) 7_565 . ? C9 C8 Co1 70.3(3) . . ? C8 C8 H8A 125.1 7_565 . ? C9 C8 H8A 125.1 . . ? Co1 C8 H8A 125.0 . . ? C8 C9 C10 108.4(7) . . ? C8 C9 Co1 70.5(3) . . ? C10 C9 Co1 71.6(5) . . ? C8 C9 H9A 125.8 . . ? C10 C9 H9A 125.8 . . ? Co1 C9 H9A 123.7 . . ? C9 C10 C9 103.6(9) 7_565 . ? C9 C10 Co1 67.9(4) 7_565 . ? C9 C10 Co1 67.9(4) . . ? C9 C10 H10 128.2 7_565 . ? C9 C10 H10 128.2 . . ? Co1 C10 H10 127.4 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.892 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.091 # Attachment 'complex 3b-f60506a.cif' data_f60506a _database_code_depnum_ccdc_archive 'CCDC 616711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H30 B10 Co Rh Se2' _chemical_formula_weight 662.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 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 20.729(5) _cell_length_b 12.437(3) _cell_length_c 9.953(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2566.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 696 _cell_measurement_theta_min 2.621 _cell_measurement_theta_max 20.615 _exptl_crystal_description prism _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 4.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8201 _exptl_absorpt_correction_T_max 0.9219 _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_% 6.93 _diffrn_reflns_number 10335 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.01 _reflns_number_total 2369 _reflns_number_gt 1288 _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_number_reflns 2369 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0866 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.826 _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 Co1 Co 0.25512(6) 0.2500 0.28341(12) 0.0506(4) Uani 1 2 d S . . Rh1 Rh 0.31586(4) 0.2500 0.50149(8) 0.0488(3) Uani 1 2 d S . . Se1 Se 0.23204(3) 0.12203(6) 0.44460(7) 0.0532(2) Uani 1 1 d . . . B3 B 0.1720(6) 0.2500 0.6860(12) 0.065(4) Uani 1 2 d S . . H3 H 0.2186 0.2500 0.7387 0.078 Uiso 1 2 calc SR . . B4 B 0.1217(4) 0.1354(8) 0.6783(9) 0.072(3) Uani 1 1 d . . . H4 H 0.1366 0.0596 0.7261 0.086 Uiso 1 1 calc R . . B5 B 0.0783(4) 0.1348(9) 0.5243(10) 0.082(3) Uani 1 1 d . . . H5 H 0.0649 0.0597 0.4731 0.098 Uiso 1 1 calc R . . B6 B 0.1011(6) 0.2500 0.4357(14) 0.074(4) Uani 1 2 d S . . H6 H 0.1025 0.2500 0.3252 0.089 Uiso 1 2 calc SR . . B7 B 0.0972(7) 0.2500 0.7705(14) 0.086(5) Uani 1 2 d S . . H7 H 0.0949 0.2500 0.8809 0.103 Uiso 1 2 calc SR . . B8 B 0.0414(5) 0.1800(8) 0.6750(9) 0.086(3) Uani 1 1 d . . . H8 H 0.0025 0.1335 0.7229 0.103 Uiso 1 1 calc R . . B9 B 0.0300(6) 0.2500 0.5255(13) 0.082(5) Uani 1 2 d S . . H9 H -0.0172 0.2500 0.4747 0.098 Uiso 1 2 calc SR . . C1 C 0.1548(3) 0.1860(6) 0.5351(6) 0.054(2) Uani 1 1 d . . . C2 C 0.3725(3) 0.1961(6) 0.6731(7) 0.062(2) Uani 1 1 d . . . C3 C 0.4015(4) 0.1609(10) 0.5547(9) 0.102(4) Uani 1 1 d . . . C4 C 0.4208(6) 0.2500 0.4760(11) 0.124(9) Uani 1 2 d S . . C5 C 0.3493(4) 0.1252(9) 0.7856(9) 0.161(5) Uani 1 1 d . . . H5A H 0.3318 0.0601 0.7490 0.242 Uiso 1 1 calc R . . H5B H 0.3165 0.1621 0.8358 0.242 Uiso 1 1 calc R . . H5C H 0.3848 0.1083 0.8439 0.242 Uiso 1 1 calc R . . C6 C 0.4116(5) 0.0404(10) 0.5228(15) 0.234(9) Uani 1 1 d . . . H6A H 0.4539 0.0189 0.5514 0.351 Uiso 1 1 calc R . . H6B H 0.4075 0.0290 0.4277 0.351 Uiso 1 1 calc R . . H6C H 0.3798 -0.0015 0.5692 0.351 Uiso 1 1 calc R . . C7 C 0.4610(6) 0.2500 0.3554(12) 0.32(2) Uani 1 2 d S . . H7A H 0.4612 0.1794 0.3166 0.478 Uiso 0.50 1 calc PR . . H7B H 0.5042 0.2702 0.3789 0.478 Uiso 0.50 1 calc PR . . H7C H 0.4439 0.3005 0.2917 0.478 Uiso 0.50 1 calc PR . . C8 C 0.3145(5) 0.2001(8) 0.1373(8) 0.111(4) Uani 1 1 d . . . H8A H 0.3509 0.1579 0.1519 0.133 Uiso 1 1 calc R . . C9 C 0.2556(6) 0.1613(11) 0.1138(10) 0.128(6) Uani 1 1 d . . . H9A H 0.2437 0.0892 0.1108 0.153 Uiso 1 1 calc R . . C10 C 0.2152(9) 0.2500 0.0944(12) 0.138(10) Uani 1 2 d S . . H10 H 0.1714 0.2500 0.0735 0.166 Uiso 1 2 calc SR . . 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 Co1 0.0516(9) 0.0580(9) 0.0422(7) 0.000 0.0002(7) 0.000 Rh1 0.0335(4) 0.0675(6) 0.0455(4) 0.000 0.0004(4) 0.000 Se1 0.0485(5) 0.0513(4) 0.0599(5) 0.0022(4) 0.0055(4) -0.0015(4) B3 0.040(8) 0.096(11) 0.060(8) 0.000 0.011(7) 0.000 B4 0.054(6) 0.096(8) 0.066(6) 0.018(6) 0.015(5) -0.006(6) B5 0.048(6) 0.106(9) 0.091(8) -0.016(7) 0.009(6) -0.025(6) B6 0.051(9) 0.112(13) 0.059(8) 0.000 -0.015(7) 0.000 B7 0.064(10) 0.132(14) 0.062(9) 0.000 0.023(8) 0.000 B8 0.043(6) 0.133(9) 0.082(7) 0.001(7) 0.014(5) -0.020(6) B9 0.020(7) 0.160(16) 0.066(10) 0.000 -0.001(6) 0.000 C1 0.040(4) 0.065(5) 0.057(5) -0.002(4) 0.004(3) -0.008(4) C2 0.034(4) 0.089(6) 0.064(5) 0.010(4) -0.016(4) 0.003(4) C3 0.048(6) 0.173(12) 0.086(7) -0.060(7) -0.030(5) 0.062(7) C4 0.028(7) 0.32(3) 0.019(9) 0.000 0.006(5) 0.000 C5 0.082(8) 0.229(13) 0.172(11) 0.135(10) -0.036(7) -0.014(8) C6 0.141(11) 0.221(15) 0.340(19) -0.173(15) -0.130(12) 0.127(12) C7 0.039(10) 0.87(6) 0.046(9) 0.000 0.029(7) 0.000 C8 0.119(9) 0.151(14) 0.062(5) 0.000(6) 0.027(6) 0.053(7) C9 0.204(18) 0.118(11) 0.061(7) -0.035(7) 0.034(9) -0.082(11) C10 0.078(13) 0.32(3) 0.021(7) 0.000 -0.019(7) 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 Co1 C8 2.004(8) . ? Co1 C8 2.004(8) 7_565 ? Co1 C9 2.017(10) . ? Co1 C9 2.017(10) 7_565 ? Co1 C10 2.055(13) . ? Co1 Se1 2.3099(12) 7_565 ? Co1 Se1 2.3099(12) . ? Co1 Rh1 2.5092(16) . ? Rh1 C3 2.159(8) 7_565 ? Rh1 C3 2.159(8) . ? Rh1 C2 2.179(6) 7_565 ? Rh1 C2 2.179(6) . ? Rh1 C4 2.189(12) . ? Rh1 Se1 2.4233(10) . ? Rh1 Se1 2.4233(10) 7_565 ? Se1 C1 2.001(7) . ? B3 C1 1.737(12) . ? B3 C1 1.737(12) 7_565 ? B3 B7 1.763(17) . ? B3 B4 1.767(11) . ? B3 B4 1.767(11) 7_565 ? B4 C1 1.703(10) . ? B4 B8 1.755(13) . ? B4 B7 1.770(12) . ? B4 B5 1.777(12) . ? B5 C1 1.712(11) . ? B5 B6 1.748(12) . ? B5 B9 1.749(12) . ? B5 B8 1.775(12) . ? B6 C1 1.690(12) 7_565 ? B6 C1 1.690(12) . ? B6 B9 1.724(17) . ? B6 B5 1.748(12) 7_565 ? B7 B8 1.733(15) . ? B7 B8 1.733(15) 7_565 ? B7 B4 1.770(12) 7_565 ? B8 B9 1.740(14) . ? B8 B8 1.74(2) 7_565 ? B9 B8 1.740(14) 7_565 ? B9 B5 1.749(12) 7_565 ? C1 C1 1.593(14) 7_565 ? C2 C2 1.340(14) 7_565 ? C2 C3 1.394(10) . ? C2 C5 1.504(10) . ? C3 C4 1.415(12) . ? C3 C6 1.546(15) . ? C4 C3 1.415(12) 7_565 ? C4 C7 1.461(15) . ? C8 C8 1.24(2) 7_565 ? C8 C9 1.334(13) . ? C9 C10 1.399(14) . ? C10 C9 1.399(14) 7_565 ? 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 Co1 C8 36.1(6) . 7_565 ? C8 Co1 C9 38.7(4) . . ? C8 Co1 C9 63.8(4) 7_565 . ? C8 Co1 C9 63.8(4) . 7_565 ? C8 Co1 C9 38.7(4) 7_565 7_565 ? C9 Co1 C9 66.3(7) . 7_565 ? C8 Co1 C10 65.4(5) . . ? C8 Co1 C10 65.4(5) 7_565 . ? C9 Co1 C10 40.2(4) . . ? C9 Co1 C10 40.2(4) 7_565 . ? C8 Co1 Se1 147.6(3) . 7_565 ? C8 Co1 Se1 114.7(3) 7_565 7_565 ? C9 Co1 Se1 163.6(4) . 7_565 ? C9 Co1 Se1 101.9(4) 7_565 7_565 ? C10 Co1 Se1 123.5(3) . 7_565 ? C8 Co1 Se1 114.7(3) . . ? C8 Co1 Se1 147.6(3) 7_565 . ? C9 Co1 Se1 101.9(4) . . ? C9 Co1 Se1 163.6(4) 7_565 . ? C10 Co1 Se1 123.5(3) . . ? Se1 Co1 Se1 87.11(6) 7_565 . ? C8 Co1 Rh1 108.6(3) . . ? C8 Co1 Rh1 108.6(3) 7_565 . ? C9 Co1 Rh1 136.2(4) . . ? C9 Co1 Rh1 136.2(4) 7_565 . ? C10 Co1 Rh1 173.6(5) . . ? Se1 Co1 Rh1 60.21(4) 7_565 . ? Se1 Co1 Rh1 60.21(4) . . ? C3 Rh1 C3 61.8(6) 7_565 . ? C3 Rh1 C2 37.5(3) 7_565 7_565 ? C3 Rh1 C2 61.5(3) . 7_565 ? C3 Rh1 C2 61.5(3) 7_565 . ? C3 Rh1 C2 37.5(3) . . ? C2 Rh1 C2 35.8(4) 7_565 . ? C3 Rh1 C4 38.0(3) 7_565 . ? C3 Rh1 C4 38.0(3) . . ? C2 Rh1 C4 63.6(3) 7_565 . ? C2 Rh1 C4 63.6(3) . . ? C3 Rh1 Se1 169.8(3) 7_565 . ? C3 Rh1 Se1 108.0(3) . . ? C2 Rh1 Se1 140.5(2) 7_565 . ? C2 Rh1 Se1 111.57(19) . . ? C4 Rh1 Se1 133.24(13) . . ? C3 Rh1 Se1 108.0(3) 7_565 7_565 ? C3 Rh1 Se1 169.8(3) . 7_565 ? C2 Rh1 Se1 111.57(19) 7_565 7_565 ? C2 Rh1 Se1 140.5(2) . 7_565 ? C4 Rh1 Se1 133.24(13) . 7_565 ? Se1 Rh1 Se1 82.11(5) . 7_565 ? C3 Rh1 Co1 128.7(2) 7_565 . ? C3 Rh1 Co1 128.7(2) . . ? C2 Rh1 Co1 161.58(19) 7_565 . ? C2 Rh1 Co1 161.58(19) . . ? C4 Rh1 Co1 113.5(3) . . ? Se1 Rh1 Co1 55.82(3) . . ? Se1 Rh1 Co1 55.82(3) 7_565 . ? C1 Se1 Co1 101.8(2) . . ? C1 Se1 Rh1 102.0(2) . . ? Co1 Se1 Rh1 63.98(4) . . ? C1 B3 C1 54.6(6) . 7_565 ? C1 B3 B7 103.5(8) . . ? C1 B3 B7 103.5(8) 7_565 . ? C1 B3 B4 58.1(5) . . ? C1 B3 B4 102.2(8) 7_565 . ? B7 B3 B4 60.2(5) . . ? C1 B3 B4 102.2(8) . 7_565 ? C1 B3 B4 58.1(5) 7_565 7_565 ? B7 B3 B4 60.2(5) . 7_565 ? B4 B3 B4 107.5(9) . 7_565 ? C1 B4 B8 104.5(6) . . ? C1 B4 B3 60.0(5) . . ? B8 B4 B3 107.8(7) . . ? C1 B4 B7 104.6(7) . . ? B8 B4 B7 58.9(6) . . ? B3 B4 B7 59.8(6) . . ? C1 B4 B5 58.9(4) . . ? B8 B4 B5 60.3(5) . . ? B3 B4 B5 109.8(7) . . ? B7 B4 B5 107.8(8) . . ? C1 B5 B6 58.5(5) . . ? C1 B5 B9 103.1(7) . . ? B6 B5 B9 59.1(7) . . ? C1 B5 B8 103.2(6) . . ? B6 B5 B8 106.4(8) . . ? B9 B5 B8 59.2(6) . . ? C1 B5 B4 58.4(4) . . ? B6 B5 B4 107.2(7) . . ? B9 B5 B4 106.3(8) . . ? B8 B5 B4 59.2(5) . . ? C1 B6 C1 56.2(6) 7_565 . ? C1 B6 B9 105.1(8) 7_565 . ? C1 B6 B9 105.1(8) . . ? C1 B6 B5 105.6(8) 7_565 . ? C1 B6 B5 59.7(5) . . ? B9 B6 B5 60.5(5) . . ? C1 B6 B5 59.7(5) 7_565 7_565 ? C1 B6 B5 105.6(8) . 7_565 ? B9 B6 B5 60.5(5) . 7_565 ? B5 B6 B5 110.2(10) . 7_565 ? B8 B7 B8 60.4(8) . 7_565 ? B8 B7 B3 109.0(8) . . ? B8 B7 B3 109.0(8) 7_565 . ? B8 B7 B4 60.1(5) . . ? B8 B7 B4 108.2(9) 7_565 . ? B3 B7 B4 60.0(5) . . ? B8 B7 B4 108.2(9) . 7_565 ? B8 B7 B4 60.1(5) 7_565 7_565 ? B3 B7 B4 60.0(5) . 7_565 ? B4 B7 B4 107.3(9) . 7_565 ? B7 B8 B9 108.0(7) . . ? B7 B8 B8 59.8(4) . 7_565 ? B9 B8 B8 60.0(4) . 7_565 ? B7 B8 B4 61.0(5) . . ? B9 B8 B4 107.7(7) . . ? B8 B8 B4 108.4(5) 7_565 . ? B7 B8 B5 109.5(7) . . ? B9 B8 B5 59.7(5) . . ? B8 B8 B5 108.5(5) 7_565 . ? B4 B8 B5 60.4(5) . . ? B6 B9 B8 109.1(8) . 7_565 ? B6 B9 B8 109.1(8) . . ? B8 B9 B8 60.1(8) 7_565 . ? B6 B9 B5 60.4(5) . 7_565 ? B8 B9 B5 61.2(5) 7_565 7_565 ? B8 B9 B5 109.7(8) . 7_565 ? B6 B9 B5 60.4(5) . . ? B8 B9 B5 109.7(8) 7_565 . ? B8 B9 B5 61.2(5) . . ? B5 B9 B5 110.0(9) 7_565 . ? C1 C1 B6 61.9(3) 7_565 . ? C1 C1 B4 111.7(4) 7_565 . ? B6 C1 B4 113.5(7) . . ? C1 C1 B5 111.8(4) 7_565 . ? B6 C1 B5 61.8(5) . . ? B4 C1 B5 62.7(5) . . ? C1 C1 B3 62.7(3) 7_565 . ? B6 C1 B3 115.1(6) . . ? B4 C1 B3 61.8(5) . . ? B5 C1 B3 114.4(6) . . ? C1 C1 Se1 113.4(2) 7_565 . ? B6 C1 Se1 116.8(6) . . ? B4 C1 Se1 123.5(5) . . ? B5 C1 Se1 124.4(5) . . ? B3 C1 Se1 114.1(5) . . ? C2 C2 C3 108.3(6) 7_565 . ? C2 C2 C5 125.9(6) 7_565 . ? C3 C2 C5 125.7(9) . . ? C2 C2 Rh1 72.09(19) 7_565 . ? C3 C2 Rh1 70.5(4) . . ? C5 C2 Rh1 126.3(5) . . ? C2 C3 C4 110.1(10) . . ? C2 C3 C6 122.5(12) . . ? C4 C3 C6 127.4(9) . . ? C2 C3 Rh1 72.0(4) . . ? C4 C3 Rh1 72.2(7) . . ? C6 C3 Rh1 124.0(7) . . ? C3 C4 C3 103.2(10) . 7_565 ? C3 C4 C7 128.0(5) . . ? C3 C4 C7 128.0(5) 7_565 . ? C3 C4 Rh1 69.8(6) . . ? C3 C4 Rh1 69.8(6) 7_565 . ? C7 C4 Rh1 131.4(9) . . ? C8 C8 C9 111.2(8) 7_565 . ? C8 C8 Co1 72.0(3) 7_565 . ? C9 C8 Co1 71.2(6) . . ? C8 C9 C10 106.7(14) . . ? C8 C9 Co1 70.1(6) . . ? C10 C9 Co1 71.4(8) . . ? C9 C10 C9 104.1(17) 7_565 . ? C9 C10 Co1 68.4(7) 7_565 . ? C9 C10 Co1 68.4(7) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.400 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.136 # Attachment 'complex 4a-f60603a.cif' data_f60603a _database_code_depnum_ccdc_archive 'CCDC 616712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H30 B10 Rh2 S2' _chemical_formula_weight 612.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 20.371(7) _cell_length_b 12.197(4) _cell_length_c 10.192(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2532.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 881 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 27.01 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 1.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5263 _exptl_absorpt_correction_T_max 0.8667 _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_% ? _diffrn_reflns_number 12126 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2916 _reflns_number_gt 2263 _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^)+(0.0316P)^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 2916 _refine_ls_number_parameters 162 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh2 Rh 0.25181(2) 0.2500 0.29099(4) 0.03733(12) Uani 1 2 d S . . Rh1 Rh 0.309794(18) 0.2500 0.51516(3) 0.03661(12) Uani 1 2 d S . . S1 S 0.22701(4) 0.12665(8) 0.45778(9) 0.0400(2) Uani 1 1 d . . . B3 B 0.1683(3) 0.2500 0.6832(6) 0.0452(15) Uani 1 2 d S . . H3 H 0.2152 0.2500 0.7365 0.054 Uiso 1 2 calc SR . . B4 B 0.1176(2) 0.1321(5) 0.6747(5) 0.0573(13) Uani 1 1 d . . . H4 H 0.1317 0.0547 0.7223 0.069 Uiso 1 1 calc R . . B5 B 0.0760(2) 0.1323(5) 0.5229(5) 0.0628(15) Uani 1 1 d . . . H5 H 0.0633 0.0552 0.4730 0.075 Uiso 1 1 calc R . . B6 B 0.0993(3) 0.2500 0.4329(7) 0.0548(18) Uani 1 2 d S . . H6 H 0.1016 0.2500 0.3251 0.066 Uiso 1 2 calc SR . . B7 B 0.0924(3) 0.2500 0.7645(7) 0.0600(19) Uani 1 2 d S . . H7 H 0.0894 0.2500 0.8722 0.072 Uiso 1 2 calc SR . . B8 B 0.0358(2) 0.1776(5) 0.6668(5) 0.0687(16) Uani 1 1 d . . . H8 H -0.0044 0.1302 0.7113 0.082 Uiso 1 1 calc R . . B9 B 0.0254(3) 0.2500 0.5189(8) 0.075(2) Uani 1 2 d S . . H9 H -0.0218 0.2500 0.4667 0.090 Uiso 1 2 calc SR . . C1 C 0.15359(16) 0.1837(3) 0.5364(3) 0.0404(8) Uani 1 1 d . . . C2 C 0.36597(17) 0.1925(3) 0.6837(3) 0.0473(10) Uani 1 1 d . . . C3 C 0.39637(18) 0.1570(4) 0.5640(4) 0.0569(11) Uani 1 1 d . . . C4 C 0.4170(3) 0.2500 0.4947(6) 0.068(2) Uani 1 2 d S . . C5 C 0.3413(2) 0.1195(4) 0.7926(4) 0.0769(15) Uani 1 1 d . . . H5A H 0.3236 0.0534 0.7558 0.115 Uiso 1 1 calc R . . H5B H 0.3077 0.1570 0.8410 0.115 Uiso 1 1 calc R . . H5C H 0.3770 0.1016 0.8503 0.115 Uiso 1 1 calc R . . C6 C 0.4092(3) 0.0390(5) 0.5300(5) 0.106(2) Uani 1 1 d . . . H6A H 0.4402 0.0087 0.5908 0.158 Uiso 1 1 calc R . . H6B H 0.4265 0.0344 0.4426 0.158 Uiso 1 1 calc R . . H6C H 0.3688 -0.0016 0.5348 0.158 Uiso 1 1 calc R . . C7 C 0.4587(3) 0.2500 0.3719(6) 0.122(4) Uani 1 2 d S . . H7A H 0.4585 0.1781 0.3336 0.183 Uiso 0.50 1 calc PR . . H7B H 0.5029 0.2701 0.3939 0.183 Uiso 0.50 1 calc PR . . H7C H 0.4412 0.3018 0.3102 0.183 Uiso 0.50 1 calc PR . . C8 C 0.3168(2) 0.1945(4) 0.1354(4) 0.0759(15) Uani 1 1 d . . . H8A H 0.3529 0.1497 0.1512 0.091 Uiso 1 1 calc R . . C9 C 0.2539(3) 0.1595(5) 0.1079(4) 0.0855(17) Uani 1 1 d . . . H9A H 0.2406 0.0866 0.1039 0.103 Uiso 1 1 calc R . . C10 C 0.2131(4) 0.2500 0.0867(6) 0.094(3) Uani 1 2 d S . . H10 H 0.1689 0.2500 0.0638 0.113 Uiso 1 2 calc SR . . 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 Rh2 0.0434(2) 0.0439(2) 0.0247(2) 0.000 0.00203(16) 0.000 Rh1 0.0309(2) 0.0530(3) 0.0260(2) 0.000 0.00186(16) 0.000 S1 0.0426(5) 0.0400(5) 0.0373(5) 0.0008(4) 0.0068(4) 0.0007(4) B3 0.042(3) 0.060(4) 0.033(3) 0.000 0.002(3) 0.000 B4 0.050(3) 0.069(4) 0.052(3) 0.008(2) 0.017(2) -0.008(2) B5 0.041(3) 0.084(4) 0.063(3) -0.008(3) 0.009(2) -0.024(3) B6 0.039(3) 0.082(5) 0.044(4) 0.000 -0.009(3) 0.000 B7 0.048(4) 0.088(6) 0.045(4) 0.000 0.017(3) 0.000 B8 0.041(3) 0.097(4) 0.068(4) -0.001(3) 0.013(2) -0.013(3) B9 0.033(3) 0.125(8) 0.066(5) 0.000 0.003(3) 0.000 C1 0.0341(18) 0.053(2) 0.0335(19) -0.0007(16) 0.0039(14) -0.0008(16) C2 0.0343(19) 0.068(3) 0.039(2) 0.0050(17) -0.0066(16) 0.0037(17) C3 0.036(2) 0.079(3) 0.056(3) -0.012(2) -0.0073(19) 0.013(2) C4 0.032(3) 0.134(7) 0.040(3) 0.000 0.000(2) 0.000 C5 0.062(3) 0.104(4) 0.064(3) 0.034(3) -0.008(2) -0.002(3) C6 0.076(4) 0.115(5) 0.126(5) -0.048(4) -0.024(3) 0.047(3) C7 0.040(4) 0.271(13) 0.054(5) 0.000 0.018(3) 0.000 C8 0.094(4) 0.098(4) 0.036(2) -0.005(2) 0.023(2) 0.026(3) C9 0.137(5) 0.086(4) 0.034(3) -0.019(2) 0.023(3) -0.041(4) C10 0.070(5) 0.177(10) 0.035(4) 0.000 -0.011(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 Rh2 C9 2.169(4) . ? Rh2 C9 2.169(4) 7_565 ? Rh2 C8 2.174(4) . ? Rh2 C8 2.174(4) 7_565 ? Rh2 C10 2.227(6) . ? Rh2 S1 2.3256(11) 7_565 ? Rh2 S1 2.3256(11) . ? Rh2 Rh1 2.5721(8) . ? Rh1 C3 2.155(4) 7_565 ? Rh1 C3 2.155(4) . ? Rh1 C2 2.180(3) 7_565 ? Rh1 C2 2.180(3) . ? Rh1 C4 2.194(5) . ? Rh1 S1 2.3344(11) . ? Rh1 S1 2.3344(11) 7_565 ? S1 C1 1.834(3) . ? B3 C1 1.727(6) . ? B3 C1 1.727(6) 7_565 ? B3 B7 1.754(9) . ? B3 B4 1.773(6) . ? B3 B4 1.773(6) 7_565 ? B4 C1 1.709(5) . ? B4 B8 1.757(7) . ? B4 B5 1.764(7) . ? B4 B7 1.779(6) . ? B5 C1 1.707(5) . ? B5 B9 1.767(7) . ? B5 B8 1.768(7) . ? B5 B6 1.768(7) . ? B6 C1 1.730(6) 7_565 ? B6 C1 1.730(6) . ? B6 B9 1.741(9) . ? B6 B5 1.768(7) 7_565 ? B7 B8 1.760(8) . ? B7 B8 1.760(8) 7_565 ? B7 B4 1.779(6) 7_565 ? B8 B9 1.760(8) . ? B8 B8 1.766(12) 7_565 ? B9 B8 1.760(8) 7_565 ? B9 B5 1.767(7) 7_565 ? C1 C1 1.617(7) 7_565 ? C2 C2 1.402(8) 7_565 ? C2 C3 1.435(5) . ? C2 C5 1.509(5) . ? C3 C4 1.401(5) . ? C3 C6 1.504(7) . ? C4 C3 1.401(5) 7_565 ? C4 C7 1.513(8) . ? C8 C8 1.353(10) 7_565 ? C8 C9 1.380(6) . ? C9 C10 1.399(7) . ? C10 C9 1.399(7) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 Rh2 C9 61.2(3) . 7_565 ? C9 Rh2 C8 37.06(17) . . ? C9 Rh2 C8 61.25(17) 7_565 . ? C9 Rh2 C8 61.25(17) . 7_565 ? C9 Rh2 C8 37.06(17) 7_565 7_565 ? C8 Rh2 C8 36.3(3) . 7_565 ? C9 Rh2 C10 37.08(17) . . ? C9 Rh2 C10 37.08(17) 7_565 . ? C8 Rh2 C10 62.2(2) . . ? C8 Rh2 C10 62.2(2) 7_565 . ? C9 Rh2 S1 164.27(17) . 7_565 ? C9 Rh2 S1 107.69(15) 7_565 7_565 ? C8 Rh2 S1 150.10(14) . 7_565 ? C8 Rh2 S1 117.65(13) 7_565 7_565 ? C10 Rh2 S1 127.34(12) . 7_565 ? C9 Rh2 S1 107.69(15) . . ? C9 Rh2 S1 164.27(17) 7_565 . ? C8 Rh2 S1 117.65(13) . . ? C8 Rh2 S1 150.10(14) 7_565 . ? C10 Rh2 S1 127.34(12) . . ? S1 Rh2 S1 80.62(5) 7_565 . ? C9 Rh2 Rh1 139.07(17) . . ? C9 Rh2 Rh1 139.07(17) 7_565 . ? C8 Rh2 Rh1 111.61(13) . . ? C8 Rh2 Rh1 111.61(13) 7_565 . ? C10 Rh2 Rh1 173.4(2) . . ? S1 Rh2 Rh1 56.66(3) 7_565 . ? S1 Rh2 Rh1 56.66(3) . . ? C3 Rh1 C3 63.5(2) 7_565 . ? C3 Rh1 C2 38.66(14) 7_565 7_565 ? C3 Rh1 C2 63.73(14) . 7_565 ? C3 Rh1 C2 63.73(14) 7_565 . ? C3 Rh1 C2 38.66(14) . . ? C2 Rh1 C2 37.5(2) 7_565 . ? C3 Rh1 C4 37.57(13) 7_565 . ? C3 Rh1 C4 37.57(13) . . ? C2 Rh1 C4 63.41(17) 7_565 . ? C2 Rh1 C4 63.41(17) . . ? C3 Rh1 S1 171.20(12) 7_565 . ? C3 Rh1 S1 108.05(12) . . ? C2 Rh1 S1 141.61(10) 7_565 . ? C2 Rh1 S1 111.68(11) . . ? C4 Rh1 S1 134.05(7) . . ? C3 Rh1 S1 108.05(12) 7_565 7_565 ? C3 Rh1 S1 171.20(12) . 7_565 ? C2 Rh1 S1 111.68(11) 7_565 7_565 ? C2 Rh1 S1 141.61(10) . 7_565 ? C4 Rh1 S1 134.05(7) . 7_565 ? S1 Rh1 S1 80.25(5) . 7_565 ? C3 Rh1 Rh2 125.53(11) 7_565 . ? C3 Rh1 Rh2 125.53(11) . . ? C2 Rh1 Rh2 160.25(11) 7_565 . ? C2 Rh1 Rh2 160.25(11) . . ? C4 Rh1 Rh2 111.89(15) . . ? S1 Rh1 Rh2 56.34(3) . . ? S1 Rh1 Rh2 56.34(3) 7_565 . ? C1 S1 Rh2 104.54(12) . . ? C1 S1 Rh1 103.59(12) . . ? Rh2 S1 Rh1 67.00(3) . . ? C1 B3 C1 55.8(3) . 7_565 ? C1 B3 B7 104.9(4) . . ? C1 B3 B7 104.9(4) 7_565 . ? C1 B3 B4 58.5(2) . . ? C1 B3 B4 103.7(4) 7_565 . ? B7 B3 B4 60.6(2) . . ? C1 B3 B4 103.7(4) . 7_565 ? C1 B3 B4 58.5(2) 7_565 7_565 ? B7 B3 B4 60.6(2) . 7_565 ? B4 B3 B4 108.4(5) . 7_565 ? C1 B4 B8 104.7(4) . . ? C1 B4 B5 58.8(2) . . ? B8 B4 B5 60.3(3) . . ? C1 B4 B3 59.4(3) . . ? B8 B4 B3 107.4(4) . . ? B5 B4 B3 108.8(4) . . ? C1 B4 B7 104.5(4) . . ? B8 B4 B7 59.7(3) . . ? B5 B4 B7 108.2(4) . . ? B3 B4 B7 59.2(3) . . ? C1 B5 B4 59.0(2) . . ? C1 B5 B9 104.1(4) . . ? B4 B5 B9 107.5(4) . . ? C1 B5 B8 104.3(3) . . ? B4 B5 B8 59.7(3) . . ? B9 B5 B8 59.7(3) . . ? C1 B5 B6 59.7(3) . . ? B4 B5 B6 109.1(4) . . ? B9 B5 B6 59.0(3) . . ? B8 B5 B6 107.5(4) . . ? C1 B6 C1 55.7(3) 7_565 . ? C1 B6 B9 104.2(4) 7_565 . ? C1 B6 B9 104.2(4) . . ? C1 B6 B5 103.6(4) 7_565 . ? C1 B6 B5 58.4(2) . . ? B9 B6 B5 60.5(3) . . ? C1 B6 B5 58.4(2) 7_565 7_565 ? C1 B6 B5 103.6(4) . 7_565 ? B9 B6 B5 60.5(3) . 7_565 ? B5 B6 B5 108.5(5) . 7_565 ? B3 B7 B8 108.1(4) . . ? B3 B7 B8 108.1(4) . 7_565 ? B8 B7 B8 60.2(5) . 7_565 ? B3 B7 B4 60.2(2) . . ? B8 B7 B4 59.5(3) . . ? B8 B7 B4 107.6(5) 7_565 . ? B3 B7 B4 60.2(2) . 7_565 ? B8 B7 B4 107.6(5) . 7_565 ? B8 B7 B4 59.5(3) 7_565 7_565 ? B4 B7 B4 107.8(5) . 7_565 ? B4 B8 B9 108.2(4) . . ? B4 B8 B7 60.8(3) . . ? B9 B8 B7 108.2(4) . . ? B4 B8 B8 108.4(3) . 7_565 ? B9 B8 B8 59.9(2) . 7_565 ? B7 B8 B8 59.9(2) . 7_565 ? B4 B8 B5 60.1(3) . . ? B9 B8 B5 60.1(3) . . ? B7 B8 B5 108.8(4) . . ? B8 B8 B5 108.2(3) 7_565 . ? B6 B9 B8 109.1(4) . 7_565 ? B6 B9 B8 109.1(4) . . ? B8 B9 B8 60.2(4) 7_565 . ? B6 B9 B5 60.5(3) . 7_565 ? B8 B9 B5 60.2(3) 7_565 7_565 ? B8 B9 B5 108.5(5) . 7_565 ? B6 B9 B5 60.5(3) . . ? B8 B9 B5 108.5(5) 7_565 . ? B8 B9 B5 60.2(3) . . ? B5 B9 B5 108.7(5) 7_565 . ? C1 C1 B5 111.5(2) 7_565 . ? C1 C1 B4 111.6(2) 7_565 . ? B5 C1 B4 62.2(3) . . ? C1 C1 B3 62.09(15) 7_565 . ? B5 C1 B3 113.7(3) . . ? B4 C1 B3 62.1(2) . . ? C1 C1 B6 62.13(15) 7_565 . ? B5 C1 B6 61.9(3) . . ? B4 C1 B6 113.6(3) . . ? B3 C1 B6 114.9(3) . . ? C1 C1 S1 112.30(12) 7_565 . ? B5 C1 S1 125.5(3) . . ? B4 C1 S1 124.8(3) . . ? B3 C1 S1 114.5(3) . . ? B6 C1 S1 115.6(3) . . ? C2 C2 C3 107.6(3) 7_565 . ? C2 C2 C5 126.2(3) 7_565 . ? C3 C2 C5 126.2(4) . . ? C2 C2 Rh1 71.25(11) 7_565 . ? C3 C2 Rh1 69.7(2) . . ? C5 C2 Rh1 126.5(3) . . ? C4 C3 C2 108.3(4) . . ? C4 C3 C6 127.4(4) . . ? C2 C3 C6 124.0(4) . . ? C4 C3 Rh1 72.7(3) . . ? C2 C3 Rh1 71.6(2) . . ? C6 C3 Rh1 126.3(3) . . ? C3 C4 C3 108.1(5) . 7_565 ? C3 C4 C7 125.9(3) . . ? C3 C4 C7 125.9(3) 7_565 . ? C3 C4 Rh1 69.7(3) . . ? C3 C4 Rh1 69.7(3) 7_565 . ? C7 C4 Rh1 129.6(4) . . ? C8 C8 C9 108.0(3) 7_565 . ? C8 C8 Rh2 71.86(13) 7_565 . ? C9 C8 Rh2 71.3(2) . . ? C8 C9 C10 109.8(5) . . ? C8 C9 Rh2 71.6(3) . . ? C10 C9 Rh2 73.7(3) . . ? C9 C10 C9 104.3(7) 7_565 . ? C9 C10 Rh2 69.2(3) 7_565 . ? C9 C10 Rh2 69.2(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.729 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.088 # Attachment 'complex 4b-f60708a.cif' data_f60708a _database_code_depnum_ccdc_archive 'CCDC 616713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H30 B10 Rh2 Se2' _chemical_formula_weight 706.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.933(3) _cell_length_b 10.155(3) _cell_length_c 20.411(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.420(4) _cell_angle_gamma 90.00 _cell_volume 2584.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 712 _cell_measurement_theta_min 2.586 _cell_measurement_theta_max 19.379 _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 4.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4945 _exptl_absorpt_correction_T_max 0.5784 _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_% 4.96 _diffrn_reflns_number 11666 _diffrn_reflns_av_R_equivalents 0.0817 _diffrn_reflns_av_sigmaI/netI 0.1591 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5071 _reflns_number_gt 2363 _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^)+(0.0173P)^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 5071 _refine_ls_number_parameters 306 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 0.720 _refine_ls_restrained_S_all 0.728 _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 0.30477(4) 0.94448(5) 0.10089(3) 0.04095(18) Uani 1 1 d . A . Rh2 Rh 0.40842(5) 0.72499(6) 0.13912(3) 0.0620(2) Uani 1 1 d . . . Se1 Se 0.49727(6) 0.92403(8) 0.11916(4) 0.0513(2) Uani 1 1 d . A . Se2 Se 0.34689(6) 0.86546(8) 0.21683(4) 0.0557(3) Uani 1 1 d . A . B1 B 0.4865(7) 1.1231(9) 0.2310(5) 0.054(3) Uani 1 1 d . A . H1 H 0.4203 1.1738 0.1946 0.065 Uiso 1 1 calc R . . B2 B 0.6188(6) 1.1440(8) 0.2289(4) 0.050(3) Uani 1 1 d . A . H2 H 0.6409 1.2076 0.1911 0.060 Uiso 1 1 calc R . . B3 B 0.6876(7) 0.9952(8) 0.2551(5) 0.056(3) Uani 1 1 d . A . H3 H 0.7535 0.9623 0.2343 0.068 Uiso 1 1 calc R . . B4 B 0.5980(7) 0.8819(10) 0.2749(5) 0.060(3) Uani 1 1 d . A . H4 H 0.6047 0.7752 0.2676 0.072 Uiso 1 1 calc R . . B5 B 0.5547(8) 0.9478(11) 0.3411(5) 0.078(4) Uani 1 1 d . . . H5 H 0.5326 0.8829 0.3783 0.093 Uiso 1 1 calc R . . B6 B 0.4829(8) 1.0919(11) 0.3148(5) 0.072(3) Uani 1 1 d . . . H6 H 0.4145 1.1209 0.3340 0.087 Uiso 1 1 calc R . . B7 B 0.5742(7) 1.2070(10) 0.2957(5) 0.068(3) Uani 1 1 d . . . H7 H 0.5665 1.3136 0.3028 0.082 Uiso 1 1 calc R . . B8 B 0.6996(8) 1.1303(10) 0.3121(5) 0.065(3) Uani 1 1 d . . . H8 H 0.7743 1.1869 0.3301 0.078 Uiso 1 1 calc R . . B9 B 0.6871(8) 0.9681(11) 0.3399(6) 0.079(4) Uani 1 1 d . . . H9 H 0.7540 0.9182 0.3760 0.095 Uiso 1 1 calc R . . B10 B 0.6161(8) 1.0958(12) 0.3640(5) 0.084(4) Uani 1 1 d . . . H10 H 0.6361 1.1299 0.4170 0.101 Uiso 1 1 calc R . . C1 C 0.5551(5) 0.9954(7) 0.2110(3) 0.0419(19) Uani 1 1 d . . . C2 C 0.4812(5) 0.9671(8) 0.2601(4) 0.053(2) Uani 1 1 d . A . C3 C 0.2239(6) 0.9606(8) -0.0063(4) 0.055(2) Uani 1 1 d . A . C4 C 0.1509(6) 0.9097(7) 0.0282(4) 0.055(2) Uani 1 1 d . . . C5 C 0.1382(6) 1.0004(8) 0.0779(4) 0.049(2) Uani 1 1 d . . . C6 C 0.2003(6) 1.1143(7) 0.0712(4) 0.050(2) Uani 1 1 d . A . C7 C 0.2529(6) 1.0888(7) 0.0203(4) 0.048(2) Uani 1 1 d . . . C8 C 0.2569(7) 0.9021(9) -0.0670(4) 0.102(4) Uani 1 1 d . . . H8A H 0.2279 0.9550 -0.1066 0.153 Uiso 1 1 calc R G . H8B H 0.2298 0.8140 -0.0751 0.153 Uiso 1 1 calc R . . H8C H 0.3337 0.9008 -0.0572 0.153 Uiso 1 1 calc R . . C9 C 0.0924(6) 0.7793(8) 0.0134(4) 0.095(3) Uani 1 1 d . . . H9A H 0.0308 0.7892 -0.0248 0.143 Uiso 1 1 calc R . . H9B H 0.0698 0.7519 0.0524 0.143 Uiso 1 1 calc R . . H9C H 0.1396 0.7141 0.0031 0.143 Uiso 1 1 calc R . . C10 C 0.0661(6) 0.9870(9) 0.1246(4) 0.088(3) Uani 1 1 d . . . H10A H -0.0073 0.9974 0.0989 0.132 Uiso 1 1 calc R . . H10B H 0.0839 1.0535 0.1592 0.132 Uiso 1 1 calc R . . H10C H 0.0757 0.9015 0.1454 0.132 Uiso 1 1 calc R . . C11 C 0.2019(3) 1.2413(3) 0.1096(2) 0.085(3) Uani 1 1 d . . . H11A H 0.2735 1.2585 0.1367 0.127 Uiso 1 1 calc R G . H11B H 0.1547 1.2341 0.1387 0.127 Uiso 1 1 calc R . . H11C H 0.1786 1.3122 0.0780 0.127 Uiso 1 1 calc R . . C13 C 0.3727(3) 0.5283(3) 0.1590(2) 0.088(7) Uani 0.50 1 d PRU A 1 H13 H 0.3391 0.5082 0.1927 0.105 Uiso 0.50 1 calc PR B 1 C14 C 0.3206(3) 0.5595(3) 0.0903(2) 0.060(6) Uani 0.50 1 d PRU A 1 H14 H 0.2469 0.5633 0.0712 0.072 Uiso 0.50 1 calc PR C 1 C15 C 0.4009(3) 0.5838(3) 0.0560(2) 0.081(6) Uani 0.50 1 d PRU A 1 H15 H 0.3889 0.6064 0.0104 0.097 Uiso 0.50 1 calc PR D 1 C16 C 0.5025(3) 0.5677(3) 0.1034(2) 0.060(5) Uani 0.50 1 d PRU A 1 H16 H 0.5689 0.5779 0.0943 0.072 Uiso 0.50 1 calc PR E 1 C17 C 0.4852(3) 0.5334(3) 0.1671(2) 0.071(6) Uani 0.50 1 d PRU A 1 H17 H 0.5381 0.5172 0.2070 0.085 Uiso 0.50 1 calc PR F 1 C12 C 0.3257(3) 1.1821(3) -0.0027(2) 0.083(3) Uani 1 1 d . G 1 H12A H 0.3949 1.1422 0.0035 0.124 Uiso 1 1 calc R . . H12B H 0.3329 1.2616 0.0235 0.124 Uiso 1 1 calc R . . H12C H 0.2960 1.2023 -0.0500 0.124 Uiso 1 1 calc R . . C13' C 0.4170(3) 0.5160(3) 0.1752(2) 0.079(6) Uani 0.50 1 d PRU A 2 H13' H 0.4228 0.4928 0.2201 0.095 Uiso 0.50 1 calc PR H 2 C14' C 0.3200(3) 0.5395(3) 0.1244(2) 0.057(5) Uani 0.50 1 d PRU A 2 H14' H 0.2511 0.5344 0.1301 0.068 Uiso 0.50 1 calc PR I 2 C15' C 0.3465(3) 0.5721(3) 0.0632(2) 0.058(5) Uani 0.50 1 d PRU A 2 H15' H 0.2981 0.5921 0.0218 0.070 Uiso 0.50 1 calc PR J 2 C16' C 0.4600(3) 0.5687(3) 0.0762(2) 0.118(9) Uani 0.50 1 d PRU A 2 H16' H 0.4989 0.5862 0.0449 0.141 Uiso 0.50 1 calc PR K 2 C17' C 0.5035(3) 0.5341(3) 0.1455(2) 0.092(8) Uani 0.50 1 d PRU A 2 H17' H 0.5760 0.5248 0.1675 0.111 Uiso 0.50 1 calc PR L 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0429(4) 0.0403(4) 0.0385(4) -0.0003(3) 0.0087(3) -0.0033(3) Rh2 0.0553(4) 0.0405(4) 0.0796(5) -0.0030(4) -0.0006(4) -0.0014(3) Se1 0.0478(5) 0.0577(6) 0.0511(5) -0.0114(4) 0.0178(4) -0.0054(4) Se2 0.0491(5) 0.0678(6) 0.0471(5) 0.0114(5) 0.0075(4) -0.0155(4) B1 0.048(6) 0.065(7) 0.047(6) -0.008(5) 0.009(5) 0.007(5) B2 0.049(6) 0.047(6) 0.054(6) 0.001(5) 0.010(5) -0.016(5) B3 0.047(6) 0.041(6) 0.079(8) 0.003(5) 0.013(6) -0.007(5) B4 0.052(6) 0.061(7) 0.056(7) 0.012(6) -0.006(5) -0.004(5) B5 0.069(8) 0.107(9) 0.042(6) 0.031(7) -0.010(6) -0.019(7) B6 0.056(7) 0.112(10) 0.053(7) -0.036(7) 0.021(6) -0.021(6) B7 0.056(7) 0.073(7) 0.073(8) -0.024(6) 0.014(6) -0.005(6) B8 0.054(7) 0.065(7) 0.072(7) -0.008(6) 0.012(6) -0.012(6) B9 0.049(7) 0.094(10) 0.079(8) 0.009(7) -0.010(6) -0.021(6) B10 0.065(8) 0.136(11) 0.045(7) -0.018(7) 0.005(6) -0.033(8) C1 0.040(5) 0.049(5) 0.040(5) -0.002(4) 0.017(4) -0.011(4) C2 0.043(5) 0.067(6) 0.045(5) 0.001(4) 0.001(4) -0.018(4) C3 0.056(6) 0.059(6) 0.046(5) 0.005(5) 0.007(5) 0.006(5) C4 0.055(6) 0.044(5) 0.054(6) 0.000(4) -0.008(5) -0.003(4) C5 0.038(5) 0.066(6) 0.041(5) 0.023(5) 0.007(4) 0.005(4) C6 0.049(5) 0.038(5) 0.060(6) -0.002(4) 0.007(5) 0.008(4) C7 0.055(5) 0.044(5) 0.045(5) 0.014(4) 0.012(4) 0.016(4) C8 0.136(9) 0.133(9) 0.039(5) -0.012(6) 0.028(6) 0.049(7) C9 0.081(7) 0.068(6) 0.104(8) 0.017(6) -0.033(6) -0.021(5) C10 0.062(6) 0.131(9) 0.073(7) 0.020(6) 0.020(5) 0.014(6) C11 0.078(7) 0.086(7) 0.084(7) -0.003(6) 0.009(5) 0.025(5) C13 0.097(10) 0.049(9) 0.088(10) 0.007(8) -0.026(8) -0.005(8) C14 0.077(9) 0.039(8) 0.054(9) 0.013(7) 0.000(7) 0.003(7) C15 0.072(10) 0.073(10) 0.101(10) -0.026(8) 0.028(8) 0.007(8) C16 0.064(8) 0.045(8) 0.055(8) -0.019(7) -0.010(7) 0.015(7) C17 0.051(9) 0.050(9) 0.112(10) 0.000(8) 0.020(8) 0.015(7) C12 0.080(7) 0.078(7) 0.099(7) 0.040(6) 0.040(6) 0.003(5) C13' 0.097(10) 0.049(9) 0.078(9) 0.021(7) -0.002(8) 0.000(8) C14' 0.046(8) 0.039(8) 0.086(10) 0.000(7) 0.016(7) -0.023(7) C15' 0.066(9) 0.046(9) 0.062(9) -0.017(7) 0.017(8) -0.003(7) C16' 0.106(11) 0.110(12) 0.131(12) -0.016(9) 0.020(9) 0.011(9) C17' 0.103(11) 0.082(12) 0.097(11) -0.011(8) 0.034(9) 0.012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C5 2.155(7) . ? Rh1 C3 2.165(7) . ? Rh1 C4 2.172(7) . ? Rh1 C7 2.172(7) . ? Rh1 C6 2.175(7) . ? Rh1 Se2 2.4199(11) . ? Rh1 Se1 2.4262(11) . ? Rh1 Rh2 2.6112(10) . ? Rh2 C13 2.113(3) . ? Rh2 C14 2.122(3) . ? Rh2 C14' 2.183(3) . ? Rh2 C17 2.189(3) . ? Rh2 C15' 2.190(3) . ? Rh2 C15 2.204(3) . ? Rh2 C13' 2.240(3) . ? Rh2 C16 2.244(3) . ? Rh2 C16' 2.251(3) . ? Rh2 C17' 2.281(3) . ? Rh2 Se1 2.4126(11) . ? Rh2 Se2 2.4197(12) . ? Se1 C1 1.962(7) . ? Se2 C2 2.011(7) . ? B1 C1 1.682(11) . ? B1 C2 1.700(11) . ? B1 B7 1.721(12) . ? B1 B2 1.736(12) . ? B1 B6 1.752(12) . ? B2 C1 1.711(10) . ? B2 B7 1.738(12) . ? B2 B8 1.747(12) . ? B2 B3 1.763(11) . ? B3 C1 1.711(10) . ? B3 B4 1.754(12) . ? B3 B9 1.754(14) . ? B3 B8 1.779(13) . ? B4 C2 1.697(11) . ? B4 C1 1.719(11) . ? B4 B5 1.729(14) . ? B4 B9 1.744(12) . ? B5 C2 1.685(11) . ? B5 B10 1.706(14) . ? B5 B9 1.731(14) . ? B5 B6 1.739(14) . ? B6 C2 1.686(11) . ? B6 B10 1.748(13) . ? B6 B7 1.777(13) . ? B7 B8 1.749(13) . ? B7 B10 1.764(14) . ? B8 B10 1.738(14) . ? B8 B9 1.764(14) . ? B9 B10 1.734(15) . ? C1 C2 1.584(9) . ? C3 C4 1.417(10) . ? C3 C7 1.422(9) . ? C3 C8 1.533(10) . ? C4 C5 1.412(10) . ? C4 C9 1.515(9) . ? C5 C6 1.436(9) . ? C5 C10 1.506(10) . ? C6 C7 1.409(10) . ? C6 C11 1.507(8) . ? C7 C12 1.496(8) . ? C13 C14 1.4200 . ? C13 C17 1.4200 . ? C14 C15 1.4200 . ? C15 C16 1.4200 . ? C16 C17 1.4200 . ? C13' C14' 1.4200 . ? C13' C17' 1.4200 . ? C14' C15' 1.4200 . ? C15' C16' 1.4200 . ? C16' C17' 1.4200 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Rh1 C3 64.8(3) . . ? C5 Rh1 C4 38.1(3) . . ? C3 Rh1 C4 38.1(3) . . ? C5 Rh1 C7 64.4(3) . . ? C3 Rh1 C7 38.3(2) . . ? C4 Rh1 C7 63.3(3) . . ? C5 Rh1 C6 38.7(2) . . ? C3 Rh1 C6 64.0(3) . . ? C4 Rh1 C6 63.3(3) . . ? C7 Rh1 C6 37.8(3) . . ? C5 Rh1 Se2 104.6(2) . . ? C3 Rh1 Se2 159.3(2) . . ? C4 Rh1 Se2 122.8(2) . . ? C7 Rh1 Se2 155.3(2) . . ? C6 Rh1 Se2 119.8(2) . . ? C5 Rh1 Se1 168.9(2) . . ? C3 Rh1 Se1 111.2(2) . . ? C4 Rh1 Se1 143.9(3) . . ? C7 Rh1 Se1 105.8(2) . . ? C6 Rh1 Se1 130.3(2) . . ? Se2 Rh1 Se1 82.31(3) . . ? C5 Rh1 Rh2 133.9(2) . . ? C3 Rh1 Rh2 116.0(2) . . ? C4 Rh1 Rh2 111.7(2) . . ? C7 Rh1 Rh2 146.4(2) . . ? C6 Rh1 Rh2 172.6(2) . . ? Se2 Rh1 Rh2 57.35(3) . . ? Se1 Rh1 Rh2 57.09(3) . . ? C13 Rh2 C14 39.18(5) . . ? C13 Rh2 C14' 22.7 . . ? C14 Rh2 C14' 19.4 . . ? C13 Rh2 C17 38.49(5) . . ? C14 Rh2 C17 64.38(8) . . ? C14' Rh2 C17 56.89(7) . . ? C13 Rh2 C15' 53.73(7) . . ? C14 Rh2 C15' 19.4 . . ? C14' Rh2 C15' 37.89(5) . . ? C17 Rh2 C15' 67.01(8) . . ? C13 Rh2 C15 64.27(8) . . ? C14 Rh2 C15 38.26(5) . . ? C14' Rh2 C15 54.41(7) . . ? C17 Rh2 C15 63.06(8) . . ? C15' Rh2 C15 20.0 . . ? C13 Rh2 C13' 15.3 . . ? C14 Rh2 C13' 51.50(7) . . ? C14' Rh2 C13' 37.42(5) . . ? C17 Rh2 C13' 24.9 . . ? C15' Rh2 C13' 62.47(8) . . ? C15 Rh2 C13' 67.99(8) . . ? C13 Rh2 C16 63.56(8) . . ? C14 Rh2 C16 63.42(8) . . ? C14' Rh2 C16 69.55(8) . . ? C17 Rh2 C16 37.33(5) . . ? C15' Rh2 C16 52.63(7) . . ? C15 Rh2 C16 37.22(5) . . ? C13' Rh2 C16 56.56(7) . . ? C13 Rh2 C16' 63.65(8) . . ? C14 Rh2 C16' 51.43(7) . . ? C14' Rh2 C16' 62.40(8) . . ? C17 Rh2 C16' 48.69(6) . . ? C15' Rh2 C16' 37.26(5) . . ? C15 Rh2 C16' 20.2 . . ? C13' Rh2 C16' 61.54(7) . . ? C16 Rh2 C16' 17.1 . . ? C13 Rh2 C17' 47.76(6) . . ? C14 Rh2 C17' 64.31(8) . . ? C14' Rh2 C17' 61.91(8) . . ? C17 Rh2 C17' 14.0 . . ? C15' Rh2 C17' 61.80(8) . . ? C15 Rh2 C17' 53.39(7) . . ? C13' Rh2 C17' 36.6 . . ? C16 Rh2 C17' 23.5 . . ? C16' Rh2 C17' 36.5 . . ? C13 Rh2 Se1 164.22(11) . . ? C14 Rh2 Se1 143.46(12) . . ? C14' Rh2 Se1 162.81(11) . . ? C17 Rh2 Se1 125.81(11) . . ? C15' Rh2 Se1 125.12(11) . . ? C15 Rh2 Se1 109.90(11) . . ? C13' Rh2 Se1 149.92(10) . . ? C16 Rh2 Se1 102.56(10) . . ? C16' Rh2 Se1 105.53(10) . . ? C17' Rh2 Se1 116.61(10) . . ? C13 Rh2 Se2 107.74(11) . . ? C14 Rh2 Se2 123.12(11) . . ? C14' Rh2 Se2 110.35(11) . . ? C17 Rh2 Se2 123.94(11) . . ? C15' Rh2 Se2 139.47(11) . . ? C15 Rh2 Se2 158.96(10) . . ? C13' Rh2 Se2 109.82(11) . . ? C16 Rh2 Se2 159.05(10) . . ? C16' Rh2 Se2 171.29(10) . . ? C17' Rh2 Se2 136.90(11) . . ? Se1 Rh2 Se2 82.60(4) . . ? C1 Se1 Rh2 103.1(2) . . ? C1 Se1 Rh1 103.3(2) . . ? Rh2 Se1 Rh1 65.32(3) . . ? C2 Se2 Rh2 101.2(2) . . ? C2 Se2 Rh1 101.7(2) . . ? Rh2 Se2 Rh1 65.31(3) . . ? C1 B1 C2 55.9(4) . . ? C1 B1 B7 106.6(6) . . ? C2 B1 B7 105.8(6) . . ? C1 B1 B2 60.1(5) . . ? C2 B1 B2 104.7(6) . . ? B7 B1 B2 60.3(5) . . ? C1 B1 B6 104.5(7) . . ? C2 B1 B6 58.4(5) . . ? B7 B1 B6 61.5(5) . . ? B2 B1 B6 109.1(6) . . ? C1 B2 B1 58.4(4) . . ? C1 B2 B7 104.6(6) . . ? B1 B2 B7 59.4(5) . . ? C1 B2 B8 105.5(6) . . ? B1 B2 B8 107.8(7) . . ? B7 B2 B8 60.2(5) . . ? C1 B2 B3 59.0(5) . . ? B1 B2 B3 108.0(6) . . ? B7 B2 B3 108.8(7) . . ? B8 B2 B3 60.9(5) . . ? C1 B3 B4 59.5(4) . . ? C1 B3 B9 104.7(7) . . ? B4 B3 B9 59.6(5) . . ? C1 B3 B2 59.0(4) . . ? B4 B3 B2 108.7(7) . . ? B9 B3 B2 107.5(8) . . ? C1 B3 B8 104.1(6) . . ? B4 B3 B8 107.7(7) . . ? B9 B3 B8 59.9(6) . . ? B2 B3 B8 59.1(5) . . ? C2 B4 C1 55.3(4) . . ? C2 B4 B5 58.9(5) . . ? C1 B4 B5 103.1(7) . . ? C2 B4 B9 104.9(7) . . ? C1 B4 B9 104.8(6) . . ? B5 B4 B9 59.8(6) . . ? C2 B4 B3 103.6(6) . . ? C1 B4 B3 59.0(5) . . ? B5 B4 B3 107.3(7) . . ? B9 B4 B3 60.2(5) . . ? C2 B5 B10 105.5(7) . . ? C2 B5 B4 59.6(5) . . ? B10 B5 B4 109.3(8) . . ? C2 B5 B9 106.0(7) . . ? B10 B5 B9 60.6(6) . . ? B4 B5 B9 60.5(6) . . ? C2 B5 B6 59.0(5) . . ? B10 B5 B6 61.0(6) . . ? B4 B5 B6 110.0(7) . . ? B9 B5 B6 110.1(8) . . ? C2 B6 B5 58.9(5) . . ? C2 B6 B10 103.6(7) . . ? B5 B6 B10 58.6(6) . . ? C2 B6 B1 59.2(5) . . ? B5 B6 B1 107.6(7) . . ? B10 B6 B1 106.2(7) . . ? C2 B6 B7 104.0(7) . . ? B5 B6 B7 106.8(7) . . ? B10 B6 B7 60.0(5) . . ? B1 B6 B7 58.4(5) . . ? B1 B7 B2 60.3(5) . . ? B1 B7 B8 108.4(7) . . ? B2 B7 B8 60.2(5) . . ? B1 B7 B10 106.9(7) . . ? B2 B7 B10 106.8(7) . . ? B8 B7 B10 59.3(6) . . ? B1 B7 B6 60.1(5) . . ? B2 B7 B6 107.9(7) . . ? B8 B7 B6 107.5(7) . . ? B10 B7 B6 59.2(6) . . ? B10 B8 B2 107.5(7) . . ? B10 B8 B7 60.8(6) . . ? B2 B8 B7 59.6(5) . . ? B10 B8 B9 59.3(6) . . ? B2 B8 B9 107.7(7) . . ? B7 B8 B9 108.5(7) . . ? B10 B8 B3 106.4(7) . . ? B2 B8 B3 60.0(5) . . ? B7 B8 B3 107.6(6) . . ? B9 B8 B3 59.4(5) . . ? B5 B9 B10 59.0(6) . . ? B5 B9 B4 59.7(5) . . ? B10 B9 B4 107.4(7) . . ? B5 B9 B3 107.2(6) . . ? B10 B9 B3 107.7(8) . . ? B4 B9 B3 60.2(5) . . ? B5 B9 B8 106.9(8) . . ? B10 B9 B8 59.6(6) . . ? B4 B9 B8 108.8(7) . . ? B3 B9 B8 60.7(6) . . ? B5 B10 B9 60.4(6) . . ? B5 B10 B8 109.3(8) . . ? B9 B10 B8 61.1(6) . . ? B5 B10 B6 60.4(5) . . ? B9 B10 B6 109.6(7) . . ? B8 B10 B6 109.4(7) . . ? B5 B10 B7 108.9(7) . . ? B9 B10 B7 109.2(8) . . ? B8 B10 B7 59.9(6) . . ? B6 B10 B7 60.8(6) . . ? C2 C1 B1 62.6(5) . . ? C2 C1 B3 110.8(6) . . ? B1 C1 B3 113.1(6) . . ? C2 C1 B2 111.2(6) . . ? B1 C1 B2 61.5(5) . . ? B3 C1 B2 62.0(4) . . ? C2 C1 B4 61.7(5) . . ? B1 C1 B4 114.7(6) . . ? B3 C1 B4 61.5(5) . . ? B2 C1 B4 112.9(6) . . ? C2 C1 Se1 113.3(4) . . ? B1 C1 Se1 115.1(5) . . ? B3 C1 Se1 125.2(5) . . ? B2 C1 Se1 124.7(5) . . ? B4 C1 Se1 116.2(5) . . ? C1 C2 B5 111.3(6) . . ? C1 C2 B6 112.3(6) . . ? B5 C2 B6 62.1(6) . . ? C1 C2 B4 63.1(5) . . ? B5 C2 B4 61.5(5) . . ? B6 C2 B4 114.2(6) . . ? C1 C2 B1 61.5(5) . . ? B5 C2 B1 112.7(6) . . ? B6 C2 B1 62.3(5) . . ? B4 C2 B1 114.9(6) . . ? C1 C2 Se2 114.3(5) . . ? B5 C2 Se2 124.5(6) . . ? B6 C2 Se2 122.3(6) . . ? B4 C2 Se2 116.2(5) . . ? B1 C2 Se2 115.8(5) . . ? C4 C3 C7 106.7(7) . . ? C4 C3 C8 128.7(8) . . ? C7 C3 C8 124.1(8) . . ? C4 C3 Rh1 71.2(4) . . ? C7 C3 Rh1 71.1(4) . . ? C8 C3 Rh1 128.6(5) . . ? C5 C4 C3 109.8(7) . . ? C5 C4 C9 124.5(9) . . ? C3 C4 C9 125.7(9) . . ? C5 C4 Rh1 70.3(4) . . ? C3 C4 Rh1 70.7(4) . . ? C9 C4 Rh1 126.6(5) . . ? C4 C5 C6 106.4(7) . . ? C4 C5 C10 127.3(8) . . ? C6 C5 C10 126.1(8) . . ? C4 C5 Rh1 71.6(4) . . ? C6 C5 Rh1 71.4(4) . . ? C10 C5 Rh1 126.2(5) . . ? C7 C6 C5 108.3(7) . . ? C7 C6 C11 126.8(7) . . ? C5 C6 C11 124.8(7) . . ? C7 C6 Rh1 71.0(4) . . ? C5 C6 Rh1 69.9(4) . . ? C11 C6 Rh1 127.7(4) . . ? C6 C7 C3 108.6(7) . . ? C6 C7 C12 125.6(7) . . ? C3 C7 C12 125.8(7) . . ? C6 C7 Rh1 71.2(4) . . ? C3 C7 Rh1 70.6(4) . . ? C12 C7 Rh1 124.9(4) . . ? C14 C13 C17 108.0 . . ? C14 C13 Rh2 70.77(10) . . ? C17 C13 Rh2 73.67(10) . . ? C15 C14 C13 108.0 . . ? C15 C14 Rh2 73.98(11) . . ? C13 C14 Rh2 70.05(10) . . ? C16 C15 C14 108.0 . . ? C16 C15 Rh2 72.93(10) . . ? C14 C15 Rh2 67.75(10) . . ? C17 C16 C15 108.0 . . ? C17 C16 Rh2 69.24(10) . . ? C15 C16 Rh2 69.86(9) . . ? C16 C17 C13 108.0 . . ? C16 C17 Rh2 73.43(11) . . ? C13 C17 Rh2 67.84(10) . . ? C14' C13' C17' 108.0 . . ? C14' C13' Rh2 69.12(9) . . ? C17' C13' Rh2 73.28(10) . . ? C13' C14' C15' 108.0 . . ? C13' C14' Rh2 73.46(10) . . ? C15' C14' Rh2 71.32(11) . . ? C16' C15' C14' 108.0 . . ? C16' C15' Rh2 73.69(10) . . ? C14' C15' Rh2 70.78(11) . . ? C15' C16' C17' 108.0 . . ? C15' C16' Rh2 69.04(9) . . ? C17' C16' Rh2 72.89(10) . . ? C13' C17' C16' 108.0 . . ? C13' C17' Rh2 70.13(10) . . ? C16' C17' Rh2 70.59(10) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.768 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.107 # Attachment 'complex 5a-f60602d.cif' data_f60602d _database_code_depnum_ccdc_archive 'CCDC 616714' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H20 B10 Rh2 S2' _chemical_formula_weight 542.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 9.247(3) _cell_length_b 12.611(4) _cell_length_c 16.472(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1921.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 828 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 26.24 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.875 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 1.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5518 _exptl_absorpt_correction_T_max 0.8305 _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_% ? _diffrn_reflns_number 9089 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0545 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.14 _reflns_number_total 2196 _reflns_number_gt 1573 _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^)+(0.0239P)^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 2196 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 0.863 _refine_ls_restrained_S_all 0.863 _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 0.38757(3) 0.35161(2) 0.382883(15) 0.02617(9) Uani 1 1 d . . . S2 S 0.40229(13) 0.2500 0.50094(7) 0.0277(3) Uani 1 2 d S . . S1 S 0.17932(13) 0.2500 0.36865(7) 0.0278(3) Uani 1 2 d S . . B3 B 0.1211(4) 0.1345(3) 0.5246(2) 0.0310(9) Uani 1 1 d . . . H1 H 0.1659 0.0600 0.5006 0.037 Uiso 1 1 calc R . . B4 B -0.0519(5) 0.1793(3) 0.4965(3) 0.0361(11) Uani 1 1 d . . . H2 H -0.1197 0.1341 0.4539 0.043 Uiso 1 1 calc R . . B5 B 0.1620(5) 0.1796(3) 0.6237(3) 0.0356(10) Uani 1 1 d . . . H3 H 0.2340 0.1345 0.6641 0.043 Uiso 1 1 calc R . . B6 B -0.0154(5) 0.1358(4) 0.5973(3) 0.0433(12) Uani 1 1 d . . . H4 H -0.0612 0.0619 0.6216 0.052 Uiso 1 1 calc R . . B7 B -0.1247(7) 0.2500 0.5806(4) 0.0454(17) Uani 1 2 d S . . H5 H -0.2413 0.2500 0.5939 0.055 Uiso 1 2 calc SR . . B8 B 0.0081(7) 0.2500 0.6597(4) 0.0430(17) Uani 1 2 d S . . H6 H -0.0222 0.2500 0.7243 0.052 Uiso 1 2 calc SR . . C1 C 0.0977(5) 0.2500 0.4702(3) 0.0269(11) Uani 1 2 d S . . C2 C 0.2173(5) 0.2500 0.5413(3) 0.0234(10) Uani 1 2 d S . . C3 C 0.4358(5) 0.5245(3) 0.3835(2) 0.0495(11) Uani 1 1 d . . . H3A H 0.4024 0.5732 0.4215 0.059 Uiso 1 1 calc R . . C4 C 0.5636(5) 0.4645(4) 0.3883(3) 0.0545(12) Uani 1 1 d . . . H4A H 0.6279 0.4642 0.4316 0.065 Uiso 1 1 calc R . . C5 C 0.5780(4) 0.4049(4) 0.3165(3) 0.0496(12) Uani 1 1 d . . . H5A H 0.6550 0.3608 0.3031 0.059 Uiso 1 1 calc R . . C6 C 0.4561(4) 0.4237(3) 0.2692(2) 0.0450(10) Uani 1 1 d . . . H6A H 0.4358 0.3933 0.2191 0.054 Uiso 1 1 calc R . . C7 C 0.3690(4) 0.4970(3) 0.3109(2) 0.0458(11) Uani 1 1 d . . . H7 H 0.2806 0.5230 0.2928 0.055 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 0.02679(15) 0.02679(15) 0.02493(14) 0.00097(12) 0.00224(12) -0.00268(13) S2 0.0256(6) 0.0328(7) 0.0246(6) 0.000 -0.0017(5) 0.000 S1 0.0279(6) 0.0297(7) 0.0258(7) 0.000 -0.0038(5) 0.000 B3 0.035(2) 0.022(2) 0.036(2) 0.0023(17) 0.0046(19) -0.0039(19) B4 0.027(2) 0.031(3) 0.050(3) -0.0003(19) 0.007(2) -0.0058(18) B5 0.043(2) 0.034(2) 0.030(2) 0.0065(18) 0.0089(19) -0.0014(18) B6 0.042(3) 0.035(3) 0.052(3) 0.006(2) 0.014(2) -0.005(2) B7 0.032(4) 0.039(4) 0.065(4) 0.000 0.020(3) 0.000 B8 0.044(4) 0.041(4) 0.043(4) 0.000 0.019(3) 0.000 C1 0.021(2) 0.028(3) 0.032(3) 0.000 0.003(2) 0.000 C2 0.029(3) 0.020(3) 0.021(2) 0.000 0.0038(19) 0.000 C3 0.074(3) 0.032(2) 0.043(2) -0.0072(19) 0.019(2) -0.015(2) C4 0.048(3) 0.061(3) 0.055(3) 0.017(2) -0.009(2) -0.035(2) C5 0.038(3) 0.047(3) 0.064(3) 0.007(2) 0.024(2) -0.007(2) C6 0.060(3) 0.043(3) 0.032(2) 0.0041(19) 0.013(2) -0.016(2) C7 0.047(3) 0.038(3) 0.052(3) 0.020(2) 0.004(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C4 2.164(4) . ? Rh1 C6 2.175(4) . ? Rh1 C5 2.179(4) . ? Rh1 C7 2.190(4) . ? Rh1 C3 2.226(4) . ? Rh1 S1 2.3250(12) . ? Rh1 S2 2.3328(11) . ? Rh1 Rh1 2.5627(10) 7_565 ? S2 C2 1.835(5) . ? S2 Rh1 2.3328(11) 7_565 ? S1 C1 1.835(5) . ? S1 Rh1 2.3250(12) 7_565 ? B3 C1 1.725(5) . ? B3 C2 1.729(4) . ? B3 B6 1.739(6) . ? B3 B4 1.759(6) . ? B3 B5 1.769(6) . ? B4 C1 1.702(5) . ? B4 B7 1.780(7) . ? B4 B6 1.781(6) . ? B4 B4 1.783(8) 7_565 ? B5 C2 1.702(5) . ? B5 B5 1.777(8) 7_565 ? B5 B8 1.779(7) . ? B5 B6 1.784(6) . ? B6 B7 1.781(6) . ? B6 B8 1.782(6) . ? B7 B4 1.780(7) 7_565 ? B7 B6 1.781(6) 7_565 ? B7 B8 1.790(10) . ? B8 B5 1.779(7) 7_565 ? B8 B6 1.782(6) 7_565 ? C1 C2 1.611(6) . ? C1 B4 1.702(5) 7_565 ? C1 B3 1.725(5) 7_565 ? C2 B5 1.702(5) 7_565 ? C2 B3 1.729(4) 7_565 ? C3 C7 1.389(5) . ? C3 C4 1.405(6) . ? C4 C5 1.407(6) . ? C5 C6 1.390(5) . ? C6 C7 1.405(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Rh1 C6 62.69(16) . . ? C4 Rh1 C5 37.82(15) . . ? C6 Rh1 C5 37.24(14) . . ? C4 Rh1 C7 61.99(16) . . ? C6 Rh1 C7 37.53(14) . . ? C5 Rh1 C7 62.19(16) . . ? C4 Rh1 C3 37.31(15) . . ? C6 Rh1 C3 62.34(15) . . ? C5 Rh1 C3 62.49(17) . . ? C7 Rh1 C3 36.67(14) . . ? C4 Rh1 S1 171.73(13) . . ? C6 Rh1 S1 112.63(11) . . ? C5 Rh1 S1 142.05(13) . . ? C7 Rh1 S1 109.99(11) . . ? C3 Rh1 S1 134.94(13) . . ? C4 Rh1 S2 106.46(12) . . ? C6 Rh1 S2 158.43(12) . . ? C5 Rh1 S2 122.73(13) . . ? C7 Rh1 S2 156.30(12) . . ? C3 Rh1 S2 121.53(11) . . ? S1 Rh1 S2 80.19(4) . . ? C4 Rh1 Rh1 131.13(14) . 7_565 ? C6 Rh1 Rh1 114.71(11) . 7_565 ? C5 Rh1 Rh1 107.96(12) . 7_565 ? C7 Rh1 Rh1 146.84(12) . 7_565 ? C3 Rh1 Rh1 168.43(13) . 7_565 ? S1 Rh1 Rh1 56.56(2) . 7_565 ? S2 Rh1 Rh1 56.68(2) . 7_565 ? C2 S2 Rh1 104.32(12) . 7_565 ? C2 S2 Rh1 104.32(12) . . ? Rh1 S2 Rh1 66.64(4) 7_565 . ? C1 S1 Rh1 104.41(13) . . ? C1 S1 Rh1 104.41(13) . 7_565 ? Rh1 S1 Rh1 66.89(4) . 7_565 ? C1 B3 C2 55.6(2) . . ? C1 B3 B6 105.0(3) . . ? C2 B3 B6 104.8(3) . . ? C1 B3 B4 58.5(2) . . ? C2 B3 B4 103.8(3) . . ? B6 B3 B4 61.2(2) . . ? C1 B3 B5 103.6(3) . . ? C2 B3 B5 58.2(2) . . ? B6 B3 B5 61.1(2) . . ? B4 B3 B5 109.5(3) . . ? C1 B4 B3 59.8(2) . . ? C1 B4 B7 104.1(3) . . ? B3 B4 B7 107.5(4) . . ? C1 B4 B6 104.2(3) . . ? B3 B4 B6 58.9(2) . . ? B7 B4 B6 60.0(3) . . ? C1 B4 B4 58.41(16) . 7_565 ? B3 B4 B4 108.75(19) . 7_565 ? B7 B4 B4 59.94(17) . 7_565 ? B6 B4 B4 107.9(2) . 7_565 ? C2 B5 B3 59.7(2) . . ? C2 B5 B5 58.53(16) . 7_565 ? B3 B5 B5 108.76(18) . 7_565 ? C2 B5 B8 104.2(3) . . ? B3 B5 B8 107.3(4) . . ? B5 B5 B8 60.05(16) 7_565 . ? C2 B5 B6 104.1(3) . . ? B3 B5 B6 58.6(2) . . ? B5 B5 B6 108.0(2) 7_565 . ? B8 B5 B6 60.0(3) . . ? B3 B6 B4 59.9(2) . . ? B3 B6 B7 108.3(3) . . ? B4 B6 B7 60.0(3) . . ? B3 B6 B8 108.5(3) . . ? B4 B6 B8 108.2(3) . . ? B7 B6 B8 60.3(3) . . ? B3 B6 B5 60.2(2) . . ? B4 B6 B5 107.8(3) . . ? B7 B6 B5 108.0(3) . . ? B8 B6 B5 59.9(3) . . ? B4 B7 B4 60.1(3) . 7_565 ? B4 B7 B6 108.1(4) . 7_565 ? B4 B7 B6 60.0(2) 7_565 7_565 ? B4 B7 B6 60.0(2) . . ? B4 B7 B6 108.1(4) 7_565 . ? B6 B7 B6 107.9(5) 7_565 . ? B4 B7 B8 107.9(4) . . ? B4 B7 B8 107.9(4) 7_565 . ? B6 B7 B8 59.9(3) 7_565 . ? B6 B7 B8 59.9(3) . . ? B5 B8 B5 59.9(3) 7_565 . ? B5 B8 B6 108.0(4) 7_565 . ? B5 B8 B6 60.1(2) . . ? B5 B8 B6 60.1(2) 7_565 7_565 ? B5 B8 B6 108.0(4) . 7_565 ? B6 B8 B6 107.8(5) . 7_565 ? B5 B8 B7 107.8(4) 7_565 . ? B5 B8 B7 107.8(4) . . ? B6 B8 B7 59.8(3) . . ? B6 B8 B7 59.8(3) 7_565 . ? C2 C1 B4 111.9(3) . . ? C2 C1 B4 111.9(3) . 7_565 ? B4 C1 B4 63.2(3) . 7_565 ? C2 C1 B3 62.3(2) . 7_565 ? B4 C1 B3 114.3(3) . 7_565 ? B4 C1 B3 61.8(2) 7_565 7_565 ? C2 C1 B3 62.3(2) . . ? B4 C1 B3 61.8(2) . . ? B4 C1 B3 114.3(3) 7_565 . ? B3 C1 B3 115.3(4) 7_565 . ? C2 C1 S1 112.3(3) . . ? B4 C1 S1 124.5(3) . . ? B4 C1 S1 124.5(3) 7_565 . ? B3 C1 S1 115.0(2) 7_565 . ? B3 C1 S1 115.0(2) . . ? C1 C2 B5 111.9(3) . 7_565 ? C1 C2 B5 111.9(3) . . ? B5 C2 B5 62.9(3) 7_565 . ? C1 C2 B3 62.1(2) . . ? B5 C2 B3 114.3(3) 7_565 . ? B5 C2 B3 62.1(2) . . ? C1 C2 B3 62.1(2) . 7_565 ? B5 C2 B3 62.1(2) 7_565 7_565 ? B5 C2 B3 114.3(3) . 7_565 ? B3 C2 B3 114.8(4) . 7_565 ? C1 C2 S2 112.2(3) . . ? B5 C2 S2 124.7(3) 7_565 . ? B5 C2 S2 124.7(3) . . ? B3 C2 S2 115.0(2) . . ? B3 C2 S2 115.0(2) 7_565 . ? C7 C3 C4 106.7(4) . . ? C7 C3 Rh1 70.3(2) . . ? C4 C3 Rh1 69.0(2) . . ? C3 C4 C5 108.7(4) . . ? C3 C4 Rh1 73.7(2) . . ? C5 C4 Rh1 71.6(2) . . ? C6 C5 C4 107.6(4) . . ? C6 C5 Rh1 71.2(2) . . ? C4 C5 Rh1 70.5(2) . . ? C5 C6 C7 107.7(4) . . ? C5 C6 Rh1 71.5(2) . . ? C7 C6 Rh1 71.8(2) . . ? C3 C7 C6 109.3(4) . . ? C3 C7 Rh1 73.1(2) . . ? C6 C7 Rh1 70.7(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.684 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.104