# 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 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Synthesis and Characterization of Heterometallic M-Ru (M = Co, Rh, Ir) Clusters Containing nido-Dicarborane 1,2-Dithiolato Chelating Ligand ; loop_ _publ_author_name 'Guo-Xin Jin.' 'Yue-Jian Lin.' 'JiaSheng Zhang.' # Attachment '1a.cif' data_f70714b _database_code_depnum_ccdc_archive 'CCDC 673411' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 B9 Cl2 Ir Ru S2' _chemical_formula_weight 817.10 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 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 11.088(4) _cell_length_b 15.594(5) _cell_length_c 18.032(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.590(5) _cell_angle_gamma 90.00 _cell_volume 3116.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 962 _cell_measurement_theta_min 2.544 _cell_measurement_theta_max 25.930 _exptl_crystal_description prism _exptl_crystal_colour ? _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 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 5.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6312 _exptl_absorpt_correction_T_max 0.6873 _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_% 9.78 _diffrn_reflns_number 15318 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.14 _reflns_number_total 6794 _reflns_number_gt 5085 _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^)+(0.0555P)^2^+18.1081P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6794 _refine_ls_number_parameters 346 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1468 _refine_ls_wR_factor_gt 0.1343 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.85084(3) 0.32276(2) 0.23260(2) 0.03373(13) Uani 1 1 d . . . Ru1 Ru 0.87766(8) 0.20358(5) 0.12081(4) 0.0389(2) Uani 1 1 d . . . S1 S 0.8943(2) 0.17852(16) 0.25158(13) 0.0369(5) Uani 1 1 d . . . S2 S 1.0160(2) 0.31436(16) 0.15762(14) 0.0397(6) Uani 1 1 d . . . B1 B 1.2272(11) 0.0836(9) 0.1671(8) 0.051(3) Uani 1 1 d . . . H1 H 1.2581 0.0339 0.1287 0.061 Uiso 1 1 calc R . . B2 B 1.1097(11) 0.0654(8) 0.2260(7) 0.046(3) Uani 1 1 d . . . H2 H 1.0595 0.0046 0.2236 0.055 Uiso 1 1 calc R . . B3 B 1.0886(10) 0.1379(7) 0.1573(7) 0.039(3) Uani 1 1 d D . . H3 H 1.020(4) 0.127(4) 0.112(3) 0.001(16) Uiso 1 1 d D . . B4 B 1.2235(11) 0.1928(7) 0.1406(8) 0.045(3) Uani 1 1 d . . . H4 H 1.2470 0.2138 0.0846 0.053 Uiso 1 1 calc R . . B5 B 1.3302(11) 0.1561(9) 0.2087(7) 0.047(3) Uani 1 1 d . . . H5 H 1.4268 0.1546 0.1963 0.057 Uiso 1 1 calc R . . B6 B 1.2568(11) 0.0758(9) 0.2659(9) 0.055(3) Uani 1 1 d . . . H6 H 1.3026 0.0208 0.2926 0.066 Uiso 1 1 calc R . . B9 B 1.2540(11) 0.2566(9) 0.2219(6) 0.044(3) Uani 1 1 d . . . H9 H 1.2737 0.3243 0.2343 0.052 Uiso 1 1 calc R . . B10 B 1.2882(12) 0.1779(9) 0.3009(6) 0.047(3) Uani 1 1 d . . . H10 H 1.3312 0.2046 0.3515 0.057 Uiso 1 1 calc R . . H10' H 1.217(7) 0.234(5) 0.301(4) 0.02(2) Uiso 1 1 d . . . B11 B 1.1417(11) 0.1268(8) 0.3087(7) 0.042(3) Uani 1 1 d . . . H11 H 1.1048 0.1319 0.3645 0.050 Uiso 1 1 calc R . . C1 C 0.8709(9) 0.4244(7) 0.3126(6) 0.044(2) Uani 1 1 d . . . C2 C 0.8262(9) 0.4598(6) 0.2441(6) 0.039(2) Uani 1 1 d . . . C3 C 0.7119(9) 0.4223(7) 0.2255(5) 0.040(2) Uani 1 1 d . . . C4 C 0.6829(9) 0.3642(7) 0.2840(6) 0.044(2) Uani 1 1 d . . . C5 C 0.7803(10) 0.3661(7) 0.3376(5) 0.043(2) Uani 1 1 d . . . C6 C 0.9832(11) 0.4484(9) 0.3554(7) 0.065(3) Uani 1 1 d . . . H6A H 1.0437 0.4666 0.3217 0.097 Uiso 1 1 calc R . . H6B H 1.0122 0.3997 0.3832 0.097 Uiso 1 1 calc R . . H6C H 0.9659 0.4944 0.3889 0.097 Uiso 1 1 calc R . . C7 C 1.0556(8) 0.1668(6) 0.2470(6) 0.037(2) Uani 1 1 d . . . C8 C 1.1174(9) 0.2363(6) 0.1978(5) 0.034(2) Uani 1 1 d . . . C9 C 0.8893(11) 0.5288(8) 0.1958(7) 0.058(3) Uani 1 1 d . . . H9A H 0.9738 0.5159 0.1933 0.087 Uiso 1 1 calc R . . H9B H 0.8792 0.5844 0.2177 0.087 Uiso 1 1 calc R . . H9C H 0.8538 0.5286 0.1466 0.087 Uiso 1 1 calc R . . C10 C 0.6374(12) 0.4456(9) 0.1574(7) 0.066(3) Uani 1 1 d . . . H10A H 0.5943 0.4978 0.1662 0.098 Uiso 1 1 calc R . . H10B H 0.5810 0.4003 0.1463 0.098 Uiso 1 1 calc R . . H10C H 0.6894 0.4534 0.1162 0.098 Uiso 1 1 calc R . . C11 C 0.5705(11) 0.3146(9) 0.2941(9) 0.073(4) Uani 1 1 d . . . H11A H 0.5885 0.2638 0.3223 0.109 Uiso 1 1 calc R . . H11B H 0.5366 0.2989 0.2465 0.109 Uiso 1 1 calc R . . H11C H 0.5137 0.3491 0.3200 0.109 Uiso 1 1 calc R . . C12 C 0.7906(15) 0.3168(9) 0.4080(8) 0.082(4) Uani 1 1 d . . . H12A H 0.7852 0.3554 0.4493 0.123 Uiso 1 1 calc R . . H12B H 0.8668 0.2876 0.4106 0.123 Uiso 1 1 calc R . . H12C H 0.7264 0.2756 0.4096 0.123 Uiso 1 1 calc R . . C13 C 0.8130(12) 0.2652(9) 0.0152(6) 0.062(3) Uani 1 1 d . . . H13 H 0.8370 0.3175 0.0358 0.075 Uiso 1 1 calc R . . C14 C 0.9001(14) 0.2062(9) -0.0013(6) 0.064(3) Uani 1 1 d . . . H14 H 0.9796 0.2233 0.0074 0.077 Uiso 1 1 calc R . . C15 C 0.8831(17) 0.1208(11) -0.0306(8) 0.091(5) Uani 1 1 d . . . H15A H 0.8480 0.1265 -0.0803 0.110 Uiso 1 1 calc R . . H15B H 0.9625 0.0956 -0.0357 0.110 Uiso 1 1 calc R . . C16 C 0.811(2) 0.0606(13) 0.0083(8) 0.116(7) Uani 1 1 d . . . H16A H 0.8519 0.0054 0.0081 0.140 Uiso 1 1 calc R . . H16B H 0.7349 0.0539 -0.0184 0.140 Uiso 1 1 calc R . . C17 C 0.7862(11) 0.0851(8) 0.0898(7) 0.059(3) Uani 1 1 d . . . H17 H 0.8323 0.0582 0.1268 0.071 Uiso 1 1 calc R . . C18 C 0.7013(11) 0.1431(8) 0.1116(6) 0.056(3) Uani 1 1 d . . . H18 H 0.6936 0.1532 0.1621 0.067 Uiso 1 1 calc R . . C19 C 0.6179(14) 0.1924(11) 0.0565(9) 0.091(5) Uani 1 1 d . . . H19A H 0.5689 0.1511 0.0290 0.109 Uiso 1 1 calc R . . H19B H 0.5637 0.2278 0.0847 0.109 Uiso 1 1 calc R . . C20 C 0.6809(14) 0.2490(12) 0.0017(8) 0.090(5) Uani 1 1 d . . . H20A H 0.6705 0.2234 -0.0472 0.108 Uiso 1 1 calc R . . H20B H 0.6400 0.3040 0.0003 0.108 Uiso 1 1 calc R . . C21 C 0.726(2) 0.5664(13) 0.9409(11) 0.121(7) Uani 1 1 d . . . H21A H 0.6935 0.5201 0.9103 0.145 Uiso 1 1 calc R . . H21B H 0.7493 0.6121 0.9078 0.145 Uiso 1 1 calc R . . Cl1 Cl 0.8475(8) 0.5312(7) 0.9853(4) 0.221(5) Uani 1 1 d . . . Cl2 Cl 0.6141(6) 0.6033(5) 0.9937(4) 0.145(2) 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 Ir1 0.02833(19) 0.0368(2) 0.0360(2) -0.00091(17) 0.00075(13) 0.00046(16) Ru1 0.0424(4) 0.0418(5) 0.0326(4) -0.0011(3) 0.0014(3) -0.0055(3) S1 0.0337(11) 0.0402(13) 0.0371(12) 0.0012(11) 0.0033(9) -0.0032(11) S2 0.0342(12) 0.0398(14) 0.0454(14) 0.0036(11) 0.0057(10) -0.0013(10) B1 0.037(6) 0.046(7) 0.070(9) -0.016(6) 0.007(6) 0.009(5) B2 0.041(6) 0.036(6) 0.060(8) -0.006(6) 0.002(6) 0.000(5) B3 0.038(6) 0.033(6) 0.045(7) -0.004(5) -0.002(5) 0.004(5) B4 0.038(6) 0.036(7) 0.060(8) -0.003(5) 0.011(5) 0.005(5) B5 0.037(6) 0.060(8) 0.044(7) -0.005(6) 0.001(5) 0.002(5) B6 0.039(7) 0.038(7) 0.087(11) -0.001(7) 0.003(7) 0.002(5) B9 0.039(6) 0.054(8) 0.038(6) -0.005(5) 0.002(5) -0.003(5) B10 0.051(7) 0.063(8) 0.029(6) -0.004(6) 0.001(5) 0.000(6) B11 0.044(7) 0.039(7) 0.042(6) -0.003(5) 0.000(5) 0.001(5) C1 0.036(5) 0.042(6) 0.054(6) -0.005(5) -0.014(5) 0.005(4) C2 0.034(5) 0.037(6) 0.046(6) -0.005(4) -0.003(4) 0.005(4) C3 0.037(5) 0.044(6) 0.040(5) -0.009(5) -0.006(4) 0.005(4) C4 0.034(5) 0.036(6) 0.063(7) -0.010(5) 0.007(5) 0.000(4) C5 0.053(6) 0.046(6) 0.029(5) -0.005(4) 0.011(4) 0.010(5) C6 0.056(7) 0.070(9) 0.066(8) -0.016(7) -0.027(6) -0.004(6) C7 0.027(4) 0.032(5) 0.052(6) 0.000(4) -0.001(4) -0.002(4) C8 0.040(5) 0.040(5) 0.023(4) -0.001(4) 0.009(4) -0.001(4) C9 0.061(7) 0.049(7) 0.066(8) 0.010(6) 0.001(6) 0.000(6) C10 0.069(8) 0.075(9) 0.052(7) -0.009(7) -0.006(6) 0.019(7) C11 0.047(7) 0.076(10) 0.096(11) 0.000(8) 0.019(7) -0.008(6) C12 0.104(12) 0.072(10) 0.070(9) 0.004(8) 0.024(9) 0.000(8) C13 0.063(8) 0.082(9) 0.042(6) 0.020(6) -0.014(6) -0.005(7) C14 0.085(10) 0.077(9) 0.030(6) 0.000(6) 0.002(6) 0.001(7) C15 0.128(15) 0.104(13) 0.043(8) -0.018(8) 0.007(8) -0.004(11) C16 0.18(2) 0.110(15) 0.057(9) -0.033(10) 0.022(11) -0.021(14) C17 0.059(8) 0.057(8) 0.060(7) -0.010(6) 0.000(6) -0.019(6) C18 0.058(7) 0.064(8) 0.045(6) 0.007(6) -0.018(5) -0.021(6) C19 0.073(10) 0.102(12) 0.096(11) 0.011(9) -0.041(9) -0.025(9) C20 0.076(10) 0.132(15) 0.061(9) 0.028(9) -0.018(7) -0.008(10) C21 0.17(2) 0.084(13) 0.104(14) -0.002(11) -0.008(14) 0.011(13) Cl1 0.174(7) 0.364(13) 0.128(5) 0.131(7) 0.036(5) 0.066(8) Cl2 0.137(5) 0.163(6) 0.136(5) 0.010(4) 0.008(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.151(10) . ? Ir1 C2 2.165(10) . ? Ir1 C5 2.176(9) . ? Ir1 C3 2.189(10) . ? Ir1 C4 2.200(10) . ? Ir1 S2 2.310(3) . ? Ir1 S1 2.324(3) . ? Ir1 Ru1 2.7640(11) . ? Ru1 C18 2.173(11) . ? Ru1 C17 2.174(11) . ? Ru1 C14 2.224(11) . ? Ru1 C13 2.233(11) . ? Ru1 S2 2.392(3) . ? Ru1 S1 2.392(3) . ? Ru1 B3 2.620(11) . ? S1 C7 1.801(9) . ? S2 C8 1.795(10) . ? B1 B2 1.727(18) . ? B1 B3 1.759(16) . ? B1 B5 1.760(18) . ? B1 B4 1.769(18) . ? B1 B6 1.81(2) . ? B2 B3 1.688(17) . ? B2 C7 1.737(15) . ? B2 B6 1.773(18) . ? B2 B11 1.799(17) . ? B3 C8 1.726(15) . ? B3 C7 1.728(15) . ? B3 B4 1.757(17) . ? B4 C8 1.725(14) . ? B4 B5 1.775(18) . ? B4 B9 1.797(18) . ? B5 B10 1.772(16) . ? B5 B9 1.799(19) . ? B5 B6 1.828(19) . ? B6 B11 1.706(17) . ? B6 B10 1.744(19) . ? B9 C8 1.596(15) . ? B9 B10 1.910(18) . ? B10 B11 1.819(18) . ? B11 C7 1.575(15) . ? C1 C2 1.429(14) . ? C1 C5 1.436(15) . ? C1 C6 1.495(14) . ? C2 C3 1.427(14) . ? C2 C9 1.563(15) . ? C3 C4 1.435(15) . ? C3 C10 1.505(15) . ? C4 C5 1.429(15) . ? C4 C11 1.482(15) . ? C5 C12 1.486(17) . ? C7 C8 1.570(13) . ? C13 C14 1.373(19) . ? C13 C20 1.500(19) . ? C14 C15 1.44(2) . ? C15 C16 1.43(2) . ? C16 C17 1.550(18) . ? C17 C18 1.371(18) . ? C18 C19 1.544(18) . ? C19 C20 1.51(2) . ? C21 Cl1 1.65(2) . ? C21 Cl2 1.68(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 C1 Ir1 C2 38.7(4) . . ? C1 Ir1 C5 38.8(4) . . ? C2 Ir1 C5 63.9(4) . . ? C1 Ir1 C3 64.9(3) . . ? C2 Ir1 C3 38.3(4) . . ? C5 Ir1 C3 64.0(4) . . ? C1 Ir1 C4 64.8(4) . . ? C2 Ir1 C4 63.9(4) . . ? C5 Ir1 C4 38.1(4) . . ? C3 Ir1 C4 38.2(4) . . ? C1 Ir1 S2 111.4(3) . . ? C2 Ir1 S2 102.5(3) . . ? C5 Ir1 S2 146.8(3) . . ? C3 Ir1 S2 125.0(3) . . ? C4 Ir1 S2 163.2(3) . . ? C1 Ir1 S1 126.7(3) . . ? C2 Ir1 S1 165.4(3) . . ? C5 Ir1 S1 104.5(3) . . ? C3 Ir1 S1 146.9(3) . . ? C4 Ir1 S1 113.4(3) . . ? S2 Ir1 S1 82.33(9) . . ? C1 Ir1 Ru1 166.8(3) . . ? C2 Ir1 Ru1 138.6(3) . . ? C5 Ir1 Ru1 153.1(3) . . ? C3 Ir1 Ru1 121.6(3) . . ? C4 Ir1 Ru1 127.9(3) . . ? S2 Ir1 Ru1 55.38(7) . . ? S1 Ir1 Ru1 55.28(6) . . ? C18 Ru1 C17 36.8(5) . . ? C18 Ru1 C14 93.3(5) . . ? C17 Ru1 C14 79.9(5) . . ? C18 Ru1 C13 81.7(5) . . ? C17 Ru1 C13 90.6(5) . . ? C14 Ru1 C13 35.9(5) . . ? C18 Ru1 S2 154.6(4) . . ? C17 Ru1 S2 167.5(4) . . ? C14 Ru1 S2 100.0(4) . . ? C13 Ru1 S2 96.5(4) . . ? C18 Ru1 S1 92.8(3) . . ? C17 Ru1 S1 97.9(4) . . ? C14 Ru1 S1 166.3(4) . . ? C13 Ru1 S1 157.7(4) . . ? S2 Ru1 S1 79.22(9) . . ? C18 Ru1 B3 130.1(4) . . ? C17 Ru1 B3 98.0(5) . . ? C14 Ru1 B3 97.6(5) . . ? C13 Ru1 B3 130.2(4) . . ? S2 Ru1 B3 69.6(3) . . ? S1 Ru1 B3 69.2(3) . . ? C18 Ru1 Ir1 103.5(4) . . ? C17 Ru1 Ir1 134.5(3) . . ? C14 Ru1 Ir1 136.7(4) . . ? C13 Ru1 Ir1 107.1(4) . . ? S2 Ru1 Ir1 52.64(6) . . ? S1 Ru1 Ir1 52.98(7) . . ? B3 Ru1 Ir1 101.1(3) . . ? C7 S1 Ir1 107.1(3) . . ? C7 S1 Ru1 91.2(3) . . ? Ir1 S1 Ru1 71.74(7) . . ? C8 S2 Ir1 107.5(3) . . ? C8 S2 Ru1 90.7(3) . . ? Ir1 S2 Ru1 71.98(7) . . ? B2 B1 B3 57.9(7) . . ? B2 B1 B5 109.6(9) . . ? B3 B1 B5 106.7(9) . . ? B2 B1 B4 108.2(9) . . ? B3 B1 B4 59.7(7) . . ? B5 B1 B4 60.4(7) . . ? B2 B1 B6 60.2(7) . . ? B3 B1 B6 105.4(9) . . ? B5 B1 B6 61.6(8) . . ? B4 B1 B6 109.5(9) . . ? B3 B2 B1 62.0(7) . . ? B3 B2 C7 60.6(7) . . ? B1 B2 C7 104.8(9) . . ? B3 B2 B6 110.1(9) . . ? B1 B2 B6 62.2(8) . . ? C7 B2 B6 98.5(8) . . ? B3 B2 B11 105.8(9) . . ? B1 B2 B11 106.7(9) . . ? C7 B2 B11 52.9(6) . . ? B6 B2 B11 57.1(7) . . ? B2 B3 C8 105.4(8) . . ? B2 B3 C7 61.1(7) . . ? C8 B3 C7 54.1(5) . . ? B2 B3 B4 110.5(9) . . ? C8 B3 B4 59.4(6) . . ? C7 B3 B4 103.7(8) . . ? B2 B3 B1 60.1(7) . . ? C8 B3 B1 103.6(8) . . ? C7 B3 B1 103.8(8) . . ? B4 B3 B1 60.4(7) . . ? B2 B3 Ru1 123.4(7) . . ? C8 B3 Ru1 84.9(5) . . ? C7 B3 Ru1 85.5(5) . . ? B4 B3 Ru1 121.7(7) . . ? B1 B3 Ru1 169.9(8) . . ? C8 B4 B3 59.4(6) . . ? C8 B4 B1 103.2(8) . . ? B3 B4 B1 59.9(7) . . ? C8 B4 B5 99.5(9) . . ? B3 B4 B5 106.2(9) . . ? B1 B4 B5 59.6(7) . . ? C8 B4 B9 53.8(6) . . ? B3 B4 B9 105.8(9) . . ? B1 B4 B9 108.1(10) . . ? B5 B4 B9 60.5(7) . . ? B1 B5 B10 109.8(9) . . ? B1 B5 B4 60.0(7) . . ? B10 B5 B4 113.6(9) . . ? B1 B5 B9 108.3(9) . . ? B10 B5 B9 64.7(7) . . ? B4 B5 B9 60.4(7) . . ? B1 B5 B6 60.4(8) . . ? B10 B5 B6 57.9(7) . . ? B4 B5 B6 108.2(9) . . ? B9 B5 B6 107.7(9) . . ? B11 B6 B10 63.6(7) . . ? B11 B6 B2 62.2(7) . . ? B10 B6 B2 113.8(9) . . ? B11 B6 B1 107.3(9) . . ? B10 B6 B1 109.0(9) . . ? B2 B6 B1 57.7(7) . . ? B11 B6 B5 106.6(9) . . ? B10 B6 B5 59.4(7) . . ? B2 B6 B5 104.6(9) . . ? B1 B6 B5 57.9(7) . . ? C8 B9 B4 60.8(6) . . ? C8 B9 B5 103.7(9) . . ? B4 B9 B5 59.2(7) . . ? C8 B9 B10 104.1(8) . . ? B4 B9 B10 106.4(9) . . ? B5 B9 B10 57.0(7) . . ? B6 B10 B5 62.7(8) . . ? B6 B10 B11 57.2(7) . . ? B5 B10 B11 104.3(8) . . ? B6 B10 B9 106.4(9) . . ? B5 B10 B9 58.3(7) . . ? B11 B10 B9 100.3(8) . . ? C7 B11 B6 108.2(9) . . ? C7 B11 B2 61.5(7) . . ? B6 B11 B2 60.7(7) . . ? C7 B11 B10 107.3(9) . . ? B6 B11 B10 59.2(7) . . ? B2 B11 B10 109.0(8) . . ? C2 C1 C5 106.7(9) . . ? C2 C1 C6 127.9(11) . . ? C5 C1 C6 125.2(10) . . ? C2 C1 Ir1 71.2(6) . . ? C5 C1 Ir1 71.5(6) . . ? C6 C1 Ir1 126.9(8) . . ? C3 C2 C1 109.2(9) . . ? C3 C2 C9 124.0(9) . . ? C1 C2 C9 126.7(9) . . ? C3 C2 Ir1 71.8(6) . . ? C1 C2 Ir1 70.2(6) . . ? C9 C2 Ir1 124.6(7) . . ? C2 C3 C4 107.5(9) . . ? C2 C3 C10 123.8(10) . . ? C4 C3 C10 128.6(10) . . ? C2 C3 Ir1 69.9(6) . . ? C4 C3 Ir1 71.3(6) . . ? C10 C3 Ir1 126.0(7) . . ? C5 C4 C3 107.7(9) . . ? C5 C4 C11 123.4(11) . . ? C3 C4 C11 128.7(11) . . ? C5 C4 Ir1 70.0(5) . . ? C3 C4 Ir1 70.5(6) . . ? C11 C4 Ir1 128.5(8) . . ? C4 C5 C1 108.9(9) . . ? C4 C5 C12 127.2(11) . . ? C1 C5 C12 123.9(11) . . ? C4 C5 Ir1 71.9(6) . . ? C1 C5 Ir1 69.7(6) . . ? C12 C5 Ir1 124.2(8) . . ? C8 C7 B11 114.0(8) . . ? C8 C7 B3 62.9(6) . . ? B11 C7 B3 114.7(8) . . ? C8 C7 B2 110.3(8) . . ? B11 C7 B2 65.6(7) . . ? B3 C7 B2 58.3(7) . . ? C8 C7 S1 113.9(7) . . ? B11 C7 S1 126.2(8) . . ? B3 C7 S1 107.8(6) . . ? B2 C7 S1 116.8(6) . . ? C7 C8 B9 114.1(8) . . ? C7 C8 B4 112.4(8) . . ? B9 C8 B4 65.4(7) . . ? C7 C8 B3 63.0(6) . . ? B9 C8 B3 117.0(8) . . ? B4 C8 B3 61.2(6) . . ? C7 C8 S2 114.7(6) . . ? B9 C8 S2 123.7(7) . . ? B4 C8 S2 117.1(7) . . ? B3 C8 S2 109.0(6) . . ? C14 C13 C20 122.7(14) . . ? C14 C13 Ru1 71.7(7) . . ? C20 C13 Ru1 110.8(8) . . ? C13 C14 C15 127.9(15) . . ? C13 C14 Ru1 72.4(7) . . ? C15 C14 Ru1 109.2(9) . . ? C16 C15 C14 119.7(13) . . ? C15 C16 C17 115.0(14) . . ? C18 C17 C16 125.3(14) . . ? C18 C17 Ru1 71.6(7) . . ? C16 C17 Ru1 111.0(10) . . ? C17 C18 C19 123.2(13) . . ? C17 C18 Ru1 71.7(7) . . ? C19 C18 Ru1 110.8(8) . . ? C20 C19 C18 115.6(12) . . ? C13 C20 C19 117.3(11) . . ? Cl1 C21 Cl2 116.4(12) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.14 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.603 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.178 # Attachment '1b.cif' data_f70711b _database_code_depnum_ccdc_archive 'CCDC 673412' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 B9 Ir O Ru S2' _chemical_formula_weight 762.20 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' Ru Ru -1.2594 0.8363 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 10.219(9) _cell_length_b 15.734(14) _cell_length_c 18.237(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.603(13) _cell_angle_gamma 90.00 _cell_volume 2932(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 905 _cell_measurement_theta_min 2.820 _cell_measurement_theta_max 27.012 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 5.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4224 _exptl_absorpt_correction_T_max 0.6241 _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_% 17.37 _diffrn_reflns_number 6872 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4769 _reflns_number_gt 3583 _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^)+(0.1746P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4769 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2084 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.009 _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 0.10352(5) 0.83681(3) 0.21720(2) 0.0325(3) Uani 1 1 d . . . Ru1 Ru -0.09519(10) 0.92361(7) 0.28596(5) 0.0333(3) Uani 1 1 d . . . S1 S 0.1254(3) 0.9109(2) 0.32755(15) 0.0347(7) Uani 1 1 d . . . S2 S -0.0664(4) 0.7720(2) 0.28251(15) 0.0366(8) Uani 1 1 d . . . O1 O -0.1397(10) 0.8985(6) 0.4061(5) 0.046(2) Uani 1 1 d . . . B1 B -0.030(2) 0.7866(12) 0.5201(8) 0.058(5) Uani 1 1 d . . . H1 H -0.0895 0.8021 0.5683 0.070 Uiso 1 1 calc R . . B2 B 0.089(2) 0.8575(13) 0.4873(8) 0.058(5) Uani 1 1 d . . . H2 H 0.1049 0.9200 0.5129 0.069 Uiso 1 1 calc R . . B3 B -0.0531(19) 0.8372(10) 0.4336(8) 0.043(4) Uani 1 1 d . . . B4 B -0.0958(19) 0.7288(12) 0.4438(8) 0.051(5) Uani 1 1 d . . . H4 H -0.1988 0.7087 0.4411 0.061 Uiso 1 1 calc R . . B5 B 0.020(2) 0.6814(13) 0.5009(11) 0.065(6) Uani 1 1 d . . . H5 H -0.0088 0.6279 0.5360 0.078 Uiso 1 1 calc R . . B6 B 0.137(2) 0.7615(15) 0.5283(8) 0.072(7) Uani 1 1 d . . . H6 H 0.1874 0.7612 0.5820 0.087 Uiso 1 1 calc R . . B9 B 0.033(2) 0.6668(10) 0.4044(10) 0.047(4) Uani 1 1 d . . . H9 H 0.0418 0.6158 0.3634 0.057 Uiso 1 1 calc R . . B10 B 0.184(3) 0.6833(14) 0.4644(10) 0.062(6) Uani 1 1 d . . . H10 H 0.2657 0.6389 0.4572 0.074 Uiso 1 1 calc R . . H10' H 0.20(2) 0.705(13) 0.432(11) 0.10(8) Uiso 1 1 d . . . B11 B 0.219(2) 0.7985(12) 0.4474(9) 0.054(5) Uani 1 1 d . . . H11 H 0.3177 0.8122 0.4267 0.064 Uiso 1 1 calc R . . C1 C -0.2558(18) 0.9106(14) 0.4470(9) 0.078(6) Uani 1 1 d . . . H1A H -0.3139 0.8635 0.4389 0.117 Uiso 1 1 calc R . . H1B H -0.2979 0.9622 0.4316 0.117 Uiso 1 1 calc R . . H1C H -0.2341 0.9142 0.4983 0.117 Uiso 1 1 calc R . . C2 C 0.2947(17) 0.7885(9) 0.1921(7) 0.053(4) Uani 1 1 d . . . C3 C 0.1958(17) 0.7342(9) 0.1615(8) 0.053(4) Uani 1 1 d . . . C4 C 0.1241(14) 0.7771(11) 0.1106(7) 0.049(4) Uani 1 1 d . . . C5 C 0.175(2) 0.8635(13) 0.1039(8) 0.073(6) Uani 1 1 d . . . C6 C 0.2738(18) 0.8693(12) 0.1551(8) 0.060(5) Uani 1 1 d . . . C7 C 0.0987(14) 0.8297(8) 0.3960(6) 0.036(3) Uani 1 1 d . . . C8 C 0.0032(13) 0.7599(8) 0.3726(6) 0.034(3) Uani 1 1 d . . . C9 C 0.406(2) 0.7702(18) 0.2465(11) 0.106(9) Uani 1 1 d . . . H9A H 0.3984 0.7132 0.2647 0.159 Uiso 1 1 calc R . . H9B H 0.4021 0.8095 0.2867 0.159 Uiso 1 1 calc R . . H9C H 0.4888 0.7764 0.2223 0.159 Uiso 1 1 calc R . . C10 C 0.193(3) 0.6421(13) 0.1839(12) 0.104(9) Uani 1 1 d . . . H10A H 0.1116 0.6171 0.1679 0.156 Uiso 1 1 calc R . . H10B H 0.2000 0.6379 0.2363 0.156 Uiso 1 1 calc R . . H10C H 0.2643 0.6126 0.1617 0.156 Uiso 1 1 calc R . . C11 C 0.016(2) 0.739(2) 0.0619(12) 0.131(12) Uani 1 1 d . . . H11A H 0.0551 0.7086 0.0222 0.196 Uiso 1 1 calc R . . H11B H -0.0375 0.7842 0.0426 0.196 Uiso 1 1 calc R . . H11C H -0.0364 0.7013 0.0903 0.196 Uiso 1 1 calc R . . C12 C 0.133(2) 0.9308(18) 0.0543(10) 0.131(12) Uani 1 1 d . . . H12A H 0.1308 0.9839 0.0803 0.196 Uiso 1 1 calc R . . H12B H 0.0465 0.9181 0.0358 0.196 Uiso 1 1 calc R . . H12C H 0.1923 0.9348 0.0142 0.196 Uiso 1 1 calc R . . C13 C 0.361(2) 0.9458(12) 0.1689(13) 0.103(9) Uani 1 1 d . . . H13A H 0.4435 0.9375 0.1449 0.155 Uiso 1 1 calc R . . H13B H 0.3762 0.9522 0.2207 0.155 Uiso 1 1 calc R . . H13C H 0.3196 0.9960 0.1499 0.155 Uiso 1 1 calc R . . C14 C -0.1196(17) 1.0563(9) 0.3096(8) 0.051(4) Uani 1 1 d . . . H14A H -0.0572 1.0787 0.3458 0.061 Uiso 1 1 calc R . . C15 C -0.0682(16) 1.0476(9) 0.2384(7) 0.049(4) Uani 1 1 d . . . H15A H 0.0237 1.0647 0.2347 0.058 Uiso 1 1 calc R . . C16 C -0.149(2) 1.0667(11) 0.1703(9) 0.072(6) Uani 1 1 d . . . H16A H -0.0920 1.0883 0.1324 0.087 Uiso 1 1 calc R . . H16B H -0.2123 1.1106 0.1815 0.087 Uiso 1 1 calc R . . C17 C -0.2240(19) 0.9850(12) 0.1403(8) 0.067(5) Uani 1 1 d . . . H17A H -0.3083 1.0023 0.1204 0.080 Uiso 1 1 calc R . . H17B H -0.1741 0.9603 0.1006 0.080 Uiso 1 1 calc R . . C18 C -0.2451(16) 0.9177(11) 0.1990(8) 0.057(4) Uani 1 1 d . . . H18A H -0.2621 0.8605 0.1799 0.069 Uiso 1 1 calc R . . C19 C -0.3059(16) 0.9356(11) 0.2679(8) 0.055(4) Uani 1 1 d . . . H19A H -0.3580 0.8888 0.2878 0.066 Uiso 1 1 calc R . . C20 C -0.3570(17) 1.0254(11) 0.2865(10) 0.063(5) Uani 1 1 d . . . H20A H -0.3879 1.0524 0.2418 0.076 Uiso 1 1 calc R . . H20B H -0.4310 1.0201 0.3191 0.076 Uiso 1 1 calc R . . C21 C -0.2562(18) 1.0817(12) 0.3221(9) 0.067(5) Uani 1 1 d . . . H21A H -0.2683 1.1391 0.3040 0.080 Uiso 1 1 calc R . . H21B H -0.2713 1.0825 0.3745 0.080 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 0.0282(4) 0.0465(4) 0.0230(3) -0.00046(18) 0.0051(2) -0.0004(2) Ru1 0.0275(7) 0.0475(7) 0.0249(5) -0.0051(4) -0.0014(5) 0.0018(5) S1 0.031(2) 0.0478(17) 0.0250(13) 0.0004(13) -0.0003(13) -0.0040(15) S2 0.036(2) 0.0476(18) 0.0267(14) -0.0044(13) 0.0049(13) -0.0059(16) O1 0.045(7) 0.060(6) 0.033(4) -0.001(4) 0.010(4) 0.009(5) B1 0.079(15) 0.067(11) 0.030(7) 0.009(8) 0.021(8) 0.003(11) B2 0.075(15) 0.083(12) 0.015(6) -0.008(7) 0.002(8) -0.020(11) B3 0.047(12) 0.050(9) 0.032(7) -0.004(6) 0.018(8) -0.004(8) B4 0.051(12) 0.073(11) 0.029(7) 0.011(7) 0.012(7) -0.006(9) B5 0.082(17) 0.066(11) 0.048(10) 0.023(9) 0.022(11) 0.004(11) B6 0.068(16) 0.120(19) 0.029(8) 0.027(10) -0.022(9) -0.018(14) B9 0.051(12) 0.044(9) 0.048(9) 0.001(7) 0.008(9) -0.003(8) B10 0.079(17) 0.069(12) 0.037(9) 0.014(9) -0.007(10) 0.010(11) B11 0.060(14) 0.061(10) 0.040(8) 0.014(8) -0.003(8) -0.002(10) C1 0.057(13) 0.123(15) 0.055(9) 0.001(10) 0.037(9) 0.016(12) C2 0.065(12) 0.055(8) 0.039(7) 0.001(7) 0.018(7) 0.035(9) C3 0.060(11) 0.052(8) 0.048(8) -0.013(7) 0.030(8) -0.010(8) C4 0.020(8) 0.099(12) 0.026(6) -0.015(7) -0.006(5) 0.010(8) C5 0.096(16) 0.097(12) 0.026(7) 0.028(8) 0.033(9) 0.043(12) C6 0.057(12) 0.078(10) 0.044(8) -0.012(8) 0.020(8) -0.013(9) C7 0.032(9) 0.059(8) 0.016(5) 0.003(5) 0.001(5) 0.001(6) C8 0.040(8) 0.044(7) 0.020(5) 0.003(5) 0.006(5) -0.008(6) C9 0.065(15) 0.18(2) 0.074(13) 0.003(15) 0.015(11) 0.058(16) C10 0.13(2) 0.080(12) 0.108(17) 0.001(12) 0.076(16) 0.026(14) C11 0.059(15) 0.25(3) 0.081(14) -0.089(19) 0.001(11) 0.005(19) C12 0.13(2) 0.20(3) 0.063(12) 0.069(15) 0.053(13) 0.09(2) C13 0.11(2) 0.077(12) 0.122(18) -0.018(12) 0.076(16) -0.029(13) C14 0.061(12) 0.047(8) 0.044(7) -0.012(7) -0.003(7) 0.018(8) C15 0.045(10) 0.056(8) 0.045(7) -0.003(7) 0.002(7) 0.008(7) C16 0.101(17) 0.068(10) 0.048(9) 0.021(8) 0.000(9) 0.023(11) C17 0.054(12) 0.099(13) 0.047(8) -0.005(9) -0.020(8) 0.009(10) C18 0.048(11) 0.069(10) 0.055(9) -0.015(8) -0.013(8) 0.016(8) C19 0.043(11) 0.074(10) 0.049(8) -0.014(8) -0.013(7) 0.014(8) C20 0.035(10) 0.085(11) 0.070(10) -0.016(9) -0.009(8) 0.030(9) C21 0.060(13) 0.079(11) 0.062(10) -0.020(9) -0.018(9) 0.031(10) _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 C3 2.132(14) . ? Ir1 C6 2.147(15) . ? Ir1 C2 2.150(15) . ? Ir1 C4 2.172(12) . ? Ir1 C5 2.239(13) . ? Ir1 S1 2.335(3) . ? Ir1 S2 2.349(4) . ? Ir1 Ru1 2.7596(19) . ? Ru1 C14 2.147(13) . ? Ru1 C15 2.154(15) . ? Ru1 C19 2.183(16) . ? Ru1 C18 2.196(16) . ? Ru1 O1 2.277(9) . ? Ru1 S1 2.380(4) . ? Ru1 S2 2.405(4) . ? S1 C7 1.810(12) . ? S2 C8 1.793(12) . ? O1 B3 1.40(2) . ? O1 C1 1.422(17) . ? B1 B2 1.76(3) . ? B1 B6 1.76(3) . ? B1 B5 1.77(3) . ? B1 B3 1.78(2) . ? B1 B4 1.79(3) . ? B2 C7 1.726(18) . ? B2 B6 1.76(3) . ? B2 B3 1.77(3) . ? B2 B11 1.79(3) . ? B3 C7 1.71(2) . ? B3 C8 1.749(18) . ? B3 B4 1.77(2) . ? B4 C8 1.725(18) . ? B4 B5 1.74(3) . ? B4 B9 1.80(2) . ? B5 B9 1.78(3) . ? B5 B10 1.80(3) . ? B5 B6 1.81(3) . ? B6 B10 1.76(3) . ? B6 B11 1.80(2) . ? B9 C8 1.60(2) . ? B9 B10 1.90(3) . ? B10 B11 1.87(3) . ? B11 C7 1.62(2) . ? C2 C3 1.43(2) . ? C2 C6 1.45(2) . ? C2 C9 1.53(2) . ? C3 C4 1.36(2) . ? C3 C10 1.51(2) . ? C4 C5 1.46(3) . ? C4 C11 1.53(2) . ? C5 C6 1.37(3) . ? C5 C12 1.46(2) . ? C6 C13 1.52(3) . ? C7 C8 1.527(18) . ? C14 C15 1.41(2) . ? C14 C21 1.47(2) . ? C15 C16 1.51(2) . ? C16 C17 1.59(3) . ? C17 C18 1.52(2) . ? C18 C19 1.43(2) . ? C19 C20 1.55(2) . ? C20 C21 1.50(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 C3 Ir1 C6 64.2(6) . . ? C3 Ir1 C2 39.0(6) . . ? C6 Ir1 C2 39.6(6) . . ? C3 Ir1 C4 36.7(6) . . ? C6 Ir1 C4 62.9(6) . . ? C2 Ir1 C4 63.9(6) . . ? C3 Ir1 C5 63.4(6) . . ? C6 Ir1 C5 36.3(7) . . ? C2 Ir1 C5 64.1(6) . . ? C4 Ir1 C5 38.7(7) . . ? C3 Ir1 S1 138.6(5) . . ? C6 Ir1 S1 105.4(4) . . ? C2 Ir1 S1 106.3(5) . . ? C4 Ir1 S1 168.1(4) . . ? C5 Ir1 S1 132.2(6) . . ? C3 Ir1 S2 104.2(4) . . ? C6 Ir1 S2 168.0(5) . . ? C2 Ir1 S2 129.2(4) . . ? C4 Ir1 S2 110.2(4) . . ? C5 Ir1 S2 143.1(6) . . ? S1 Ir1 S2 81.06(12) . . ? C3 Ir1 Ru1 157.3(4) . . ? C6 Ir1 Ru1 136.6(5) . . ? C2 Ir1 Ru1 161.2(5) . . ? C4 Ir1 Ru1 134.4(4) . . ? C5 Ir1 Ru1 125.1(5) . . ? S1 Ir1 Ru1 54.93(10) . . ? S2 Ir1 Ru1 55.46(11) . . ? C14 Ru1 C15 38.3(5) . . ? C14 Ru1 C19 80.2(6) . . ? C15 Ru1 C19 89.5(6) . . ? C14 Ru1 C18 96.0(6) . . ? C15 Ru1 C18 80.7(6) . . ? C19 Ru1 C18 38.3(6) . . ? C14 Ru1 O1 87.2(5) . . ? C15 Ru1 O1 124.9(4) . . ? C19 Ru1 O1 87.4(5) . . ? C18 Ru1 O1 122.9(5) . . ? C14 Ru1 S1 97.4(5) . . ? C15 Ru1 S1 94.5(4) . . ? C19 Ru1 S1 170.1(4) . . ? C18 Ru1 S1 151.4(4) . . ? O1 Ru1 S1 82.9(3) . . ? C14 Ru1 S2 169.9(4) . . ? C15 Ru1 S2 150.7(4) . . ? C19 Ru1 S2 101.7(5) . . ? C18 Ru1 S2 91.4(4) . . ? O1 Ru1 S2 83.0(3) . . ? S1 Ru1 S2 79.00(12) . . ? C14 Ru1 Ir1 131.3(5) . . ? C15 Ru1 Ir1 99.6(4) . . ? C19 Ru1 Ir1 134.7(4) . . ? C18 Ru1 Ir1 99.3(4) . . ? O1 Ru1 Ir1 120.4(3) . . ? S1 Ru1 Ir1 53.42(9) . . ? S2 Ru1 Ir1 53.57(8) . . ? C7 S1 Ir1 103.2(4) . . ? C7 S1 Ru1 97.5(5) . . ? Ir1 S1 Ru1 71.65(10) . . ? C8 S2 Ir1 102.9(4) . . ? C8 S2 Ru1 97.4(4) . . ? Ir1 S2 Ru1 70.97(10) . . ? B3 O1 C1 115.7(12) . . ? B3 O1 Ru1 109.5(8) . . ? C1 O1 Ru1 131.2(10) . . ? B2 B1 B6 59.8(12) . . ? B2 B1 B5 108.8(14) . . ? B6 B1 B5 61.4(13) . . ? B2 B1 B3 60.0(10) . . ? B6 B1 B3 107.1(12) . . ? B5 B1 B3 106.2(11) . . ? B2 B1 B4 108.2(10) . . ? B6 B1 B4 107.9(13) . . ? B5 B1 B4 58.5(12) . . ? B3 B1 B4 59.6(9) . . ? C7 B2 B6 99.9(12) . . ? C7 B2 B1 102.4(12) . . ? B6 B2 B1 60.2(11) . . ? C7 B2 B3 58.5(8) . . ? B6 B2 B3 107.9(13) . . ? B1 B2 B3 60.6(10) . . ? C7 B2 B11 54.7(9) . . ? B6 B2 B11 61.1(11) . . ? B1 B2 B11 109.3(14) . . ? B3 B2 B11 106.9(12) . . ? O1 B3 C7 118.6(11) . . ? O1 B3 C8 117.5(12) . . ? C7 B3 C8 52.4(7) . . ? O1 B3 B2 125.8(13) . . ? C7 B3 B2 59.5(10) . . ? C8 B3 B2 101.9(12) . . ? O1 B3 B4 123.1(15) . . ? C7 B3 B4 101.6(11) . . ? C8 B3 B4 58.7(8) . . ? B2 B3 B4 108.5(13) . . ? O1 B3 B1 134.6(12) . . ? C7 B3 B1 102.4(13) . . ? C8 B3 B1 102.2(11) . . ? B2 B3 B1 59.4(11) . . ? B4 B3 B1 60.4(9) . . ? C8 B4 B5 99.9(12) . . ? C8 B4 B3 60.0(8) . . ? B5 B4 B3 108.0(14) . . ? C8 B4 B1 102.9(12) . . ? B5 B4 B1 60.3(11) . . ? B3 B4 B1 60.0(10) . . ? C8 B4 B9 54.2(8) . . ? B5 B4 B9 60.5(11) . . ? B3 B4 B9 107.4(12) . . ? B1 B4 B9 108.6(14) . . ? B4 B5 B1 61.2(11) . . ? B4 B5 B9 61.3(11) . . ? B1 B5 B9 109.9(12) . . ? B4 B5 B10 113.6(12) . . ? B1 B5 B10 109.3(15) . . ? B9 B5 B10 63.9(11) . . ? B4 B5 B6 108.2(14) . . ? B1 B5 B6 59.1(13) . . ? B9 B5 B6 107.9(12) . . ? B10 B5 B6 58.5(12) . . ? B2 B6 B10 113.4(11) . . ? B2 B6 B1 60.0(11) . . ? B10 B6 B1 111.6(14) . . ? B2 B6 B11 60.4(10) . . ? B10 B6 B11 63.5(11) . . ? B1 B6 B11 108.5(12) . . ? B2 B6 B5 107.4(13) . . ? B10 B6 B5 60.8(13) . . ? B1 B6 B5 59.5(11) . . ? B11 B6 B5 108.1(12) . . ? C8 B9 B5 102.9(11) . . ? C8 B9 B4 60.7(9) . . ? B5 B9 B4 58.1(11) . . ? C8 B9 B10 103.5(12) . . ? B5 B9 B10 58.7(12) . . ? B4 B9 B10 106.8(13) . . ? B6 B10 B5 60.8(12) . . ? B6 B10 B11 59.3(11) . . ? B5 B10 B11 105.0(15) . . ? B6 B10 B9 104.8(15) . . ? B5 B10 B9 57.5(12) . . ? B11 B10 B9 101.2(13) . . ? C7 B11 B2 60.7(10) . . ? C7 B11 B6 102.4(14) . . ? B2 B11 B6 58.6(11) . . ? C7 B11 B10 104.0(14) . . ? B2 B11 B10 106.7(14) . . ? B6 B11 B10 57.3(11) . . ? C3 C2 C6 104.0(14) . . ? C3 C2 C9 131.2(16) . . ? C6 C2 C9 124.7(18) . . ? C3 C2 Ir1 69.8(9) . . ? C6 C2 Ir1 70.1(8) . . ? C9 C2 Ir1 126.9(10) . . ? C4 C3 C2 110.1(13) . . ? C4 C3 C10 130.6(18) . . ? C2 C3 C10 119.1(18) . . ? C4 C3 Ir1 73.2(9) . . ? C2 C3 Ir1 71.2(7) . . ? C10 C3 Ir1 126.1(10) . . ? C3 C4 C5 109.2(14) . . ? C3 C4 C11 125.8(19) . . ? C5 C4 C11 124.7(19) . . ? C3 C4 Ir1 70.0(8) . . ? C5 C4 Ir1 73.1(8) . . ? C11 C4 Ir1 127.8(10) . . ? C6 C5 C12 126(2) . . ? C6 C5 C4 105.4(14) . . ? C12 C5 C4 129(2) . . ? C6 C5 Ir1 68.2(8) . . ? C12 C5 Ir1 127.7(12) . . ? C4 C5 Ir1 68.2(7) . . ? C5 C6 C2 111.2(16) . . ? C5 C6 C13 126.4(19) . . ? C2 C6 C13 122.2(18) . . ? C5 C6 Ir1 75.5(10) . . ? C2 C6 Ir1 70.3(9) . . ? C13 C6 Ir1 125.5(11) . . ? C8 C7 B11 115.1(11) . . ? C8 C7 B3 65.2(9) . . ? B11 C7 B3 118.6(11) . . ? C8 C7 B2 114.0(10) . . ? B11 C7 B2 64.6(11) . . ? B3 C7 B2 62.0(10) . . ? C8 C7 S1 114.6(8) . . ? B11 C7 S1 119.7(11) . . ? B3 C7 S1 111.9(9) . . ? B2 C7 S1 119.8(10) . . ? C7 C8 B9 115.9(12) . . ? C7 C8 B4 111.8(10) . . ? B9 C8 B4 65.2(10) . . ? C7 C8 B3 62.3(9) . . ? B9 C8 B3 117.9(10) . . ? B4 C8 B3 61.3(9) . . ? C7 C8 S2 115.2(8) . . ? B9 C8 S2 120.0(10) . . ? B4 C8 S2 119.3(10) . . ? B3 C8 S2 112.3(10) . . ? C15 C14 C21 122.1(15) . . ? C15 C14 Ru1 71.1(8) . . ? C21 C14 Ru1 114.0(12) . . ? C14 C15 C16 122.0(16) . . ? C14 C15 Ru1 70.6(8) . . ? C16 C15 Ru1 116.0(11) . . ? C15 C16 C17 112.3(13) . . ? C18 C17 C16 113.0(12) . . ? C19 C18 C17 123.0(15) . . ? C19 C18 Ru1 70.4(9) . . ? C17 C18 Ru1 112.0(12) . . ? C18 C19 C20 121.5(15) . . ? C18 C19 Ru1 71.4(9) . . ? C20 C19 Ru1 112.4(11) . . ? C21 C20 C19 113.7(13) . . ? C14 C21 C20 114.9(13) . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 4.762 _refine_diff_density_min -6.563 _refine_diff_density_rms 0.333 # Attachment '1c.cif' data_f50917b _database_code_depnum_ccdc_archive 'CCDC 673413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H58 B20 Ir2 Ru S4' _chemical_formula_weight 1260.68 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' Ru Ru -1.2594 0.8363 '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 Monoclinic _symmetry_space_group_name_H-M 'C2/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.142(7) _cell_length_b 23.203(13) _cell_length_c 18.029(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.374(7) _cell_angle_gamma 90.00 _cell_volume 4961(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 2.714 _cell_measurement_theta_max 26.277 _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 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2424 _exptl_absorpt_coefficient_mu 5.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4743 _exptl_absorpt_correction_T_max 0.5926 _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_% 10.04 _diffrn_reflns_number 14040 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.19 _reflns_number_total 5395 _reflns_number_gt 3732 _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^)+(0.0591P)^2^+2.9144P] 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 5395 _refine_ls_number_parameters 284 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.87611(3) 0.120435(12) 0.122127(16) 0.03420(11) Uani 1 1 d . . . Ru2 Ru 1.0000 0.07254(3) 0.2500 0.0311(2) Uani 1 2 d S . . S1 S 0.80008(16) 0.08194(8) 0.22171(11) 0.0359(4) Uani 1 1 d . . . S2 S 0.94629(16) 0.02498(8) 0.12882(10) 0.0345(4) Uani 1 1 d . . . B3 B 0.8257(8) -0.0468(4) 0.2254(5) 0.042(2) Uani 1 1 d . . . H3 H 0.8973 -0.0443 0.2744 0.050 Uiso 1 1 calc R . . B4 B 0.6852(8) -0.0386(5) 0.2359(6) 0.051(3) Uani 1 1 d . . . H4 H 0.6652 -0.0307 0.2917 0.061 Uiso 1 1 calc R . . B5 B 0.6047(8) -0.0056(5) 0.1528(6) 0.055(3) Uani 1 1 d . . . H5 H 0.5340 0.0234 0.1555 0.067 Uiso 1 1 calc R . . B6 B 0.6950(8) 0.0067(4) 0.0890(5) 0.047(2) Uani 1 1 d . . . H6 H 0.6820 0.0436 0.0498 0.057 Uiso 1 1 calc R . . B7 B 0.8275(10) -0.0932(4) 0.1476(5) 0.050(3) Uani 1 1 d . . . H7 H 0.9001 -0.1210 0.1456 0.060 Uiso 1 1 calc R . . B8 B 0.7357(10) -0.1059(4) 0.2099(6) 0.054(3) Uani 1 1 d . . . H8 H 0.7482 -0.1429 0.2490 0.065 Uiso 1 1 calc R . . B9 B 0.5982(10) -0.0817(5) 0.1648(7) 0.065(3) Uani 1 1 d . . . H9 H 0.5214 -0.1028 0.1744 0.078 Uiso 1 1 calc R . . B10 B 0.6068(9) -0.0535(4) 0.0750(6) 0.060(3) Uani 1 1 d . . . H10 H 0.5353 -0.0564 0.0260 0.072 Uiso 1 1 calc R . . B11 B 0.7474(9) -0.0599(4) 0.0640(6) 0.054(3) Uani 1 1 d . . . H11 H 0.7694 -0.0662 0.0085 0.065 Uiso 1 1 calc R . . B12 B 0.6862(11) -0.1142(5) 0.1107(7) 0.062(3) Uani 1 1 d . . . H12 H 0.6662 -0.1569 0.0850 0.074 Uiso 1 1 calc R . . C1 C 0.7456(6) 0.0104(3) 0.1858(4) 0.0378(17) Uani 1 1 d . . . C2 C 0.8250(6) -0.0193(3) 0.1365(4) 0.0346(17) Uani 1 1 d . . . C3 C 0.8098(8) 0.2074(4) 0.0999(6) 0.054(2) Uani 1 1 d . . . C4 C 0.9192(8) 0.2058(4) 0.0880(5) 0.061(3) Uani 1 1 d . . . C5 C 0.9213(9) 0.1651(5) 0.0285(6) 0.068(3) Uani 1 1 d U . . C6 C 0.8143(10) 0.1438(5) 0.0044(6) 0.069(3) Uani 1 1 d U . . C7 C 0.7444(8) 0.1699(4) 0.0438(7) 0.075(4) Uani 1 1 d . . . C8 C 0.7658(12) 0.2443(6) 0.1550(8) 0.116(5) Uani 1 1 d U . . H8A H 0.8245 0.2508 0.1991 0.174 Uiso 1 1 calc R . . H8B H 0.7036 0.2252 0.1696 0.174 Uiso 1 1 calc R . . H8C H 0.7410 0.2805 0.1316 0.174 Uiso 1 1 calc R . . C9 C 1.0084(13) 0.2432(7) 0.1318(9) 0.134(6) Uani 1 1 d U . . H9A H 1.0115 0.2785 0.1046 0.200 Uiso 1 1 calc R . . H9B H 1.0797 0.2239 0.1389 0.200 Uiso 1 1 calc R . . H9C H 0.9918 0.2516 0.1804 0.200 Uiso 1 1 calc R . . C10 C 1.0261(15) 0.1527(8) 0.0000(11) 0.164(7) Uani 1 1 d U . . H10A H 1.0539 0.1152 0.0168 0.246 Uiso 1 1 calc R . . H10B H 1.0823 0.1812 0.0195 0.246 Uiso 1 1 calc R . . H10C H 1.0091 0.1539 -0.0545 0.246 Uiso 1 1 calc R . . C11 C 0.7721(15) 0.1031(7) -0.0607(9) 0.139(6) Uani 1 1 d U . . H11A H 0.8341 0.0908 -0.0821 0.209 Uiso 1 1 calc R . . H11B H 0.7172 0.1224 -0.0988 0.209 Uiso 1 1 calc R . . H11C H 0.7380 0.0701 -0.0425 0.209 Uiso 1 1 calc R . . C12 C 0.6181(11) 0.1629(7) 0.0378(8) 0.120(5) Uani 1 1 d U . . H12A H 0.5870 0.1987 0.0506 0.180 Uiso 1 1 calc R . . H12B H 0.6050 0.1334 0.0721 0.180 Uiso 1 1 calc R . . H12C H 0.5827 0.1523 -0.0132 0.180 Uiso 1 1 calc R . . C13 C 0.5000 0.2638(9) 0.2500 0.165(10) Uani 1 2 d SDU . . H13 H 0.5000 0.3039 0.2500 0.198 Uiso 1 2 calc SR . . C14 C 0.5774(11) 0.2401(6) 0.3080(8) 0.141(6) Uani 1 1 d DU . . H14 H 0.6266 0.2619 0.3439 0.170 Uiso 1 1 calc R . . C15 C 0.5760(13) 0.1811(6) 0.3086(8) 0.157(7) Uani 1 1 d DU . . C16 C 0.5000 0.1559(8) 0.2500 0.112(7) Uani 1 2 d SDU . . H16 H 0.5000 0.1159 0.2500 0.134 Uiso 1 2 calc SR . . C17 C 0.641(3) 0.1537(11) 0.3642(15) 0.187(18) Uani 0.50 1 d PDU . . H17A H 0.5976 0.1253 0.3842 0.280 Uiso 0.50 1 calc PR . . H17B H 0.6727 0.1805 0.4035 0.280 Uiso 0.50 1 calc PR . . H17C H 0.7005 0.1350 0.3459 0.280 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 Ir1 0.04042(18) 0.02752(16) 0.03185(16) 0.00282(12) 0.00153(11) 0.00049(14) Ru2 0.0340(5) 0.0264(4) 0.0306(4) 0.000 0.0016(3) 0.000 S1 0.0373(10) 0.0310(10) 0.0383(10) -0.0025(8) 0.0060(8) 0.0023(8) S2 0.0381(11) 0.0309(10) 0.0336(10) -0.0006(7) 0.0059(8) 0.0016(8) B3 0.050(6) 0.035(5) 0.039(5) 0.003(4) 0.007(4) 0.000(4) B4 0.043(6) 0.049(6) 0.061(7) 0.005(5) 0.015(5) -0.004(5) B5 0.034(5) 0.057(7) 0.072(7) 0.006(5) 0.006(5) -0.012(5) B6 0.043(5) 0.045(6) 0.046(6) 0.003(4) -0.010(4) -0.006(5) B7 0.073(7) 0.028(5) 0.044(6) -0.006(4) 0.003(5) -0.008(5) B8 0.065(7) 0.039(6) 0.055(6) 0.004(5) 0.005(5) -0.015(5) B9 0.061(7) 0.055(7) 0.073(8) 0.011(6) 0.003(6) -0.026(6) B10 0.059(7) 0.041(6) 0.068(7) -0.001(5) -0.012(5) -0.018(5) B11 0.066(7) 0.044(6) 0.046(6) -0.003(5) -0.002(5) -0.010(5) B12 0.075(8) 0.041(6) 0.062(7) 0.001(5) -0.001(6) -0.024(6) C1 0.036(4) 0.035(4) 0.039(4) -0.004(3) 0.000(3) 0.000(3) C2 0.041(4) 0.028(4) 0.030(4) 0.002(3) -0.001(3) -0.001(3) C3 0.066(6) 0.027(4) 0.073(7) 0.013(4) 0.023(5) 0.009(4) C4 0.064(6) 0.052(6) 0.054(6) 0.031(5) -0.015(5) -0.023(5) C5 0.075(5) 0.074(5) 0.063(4) 0.025(4) 0.036(4) 0.014(4) C6 0.094(5) 0.060(4) 0.047(4) 0.004(4) 0.002(4) 0.001(4) C7 0.048(6) 0.049(6) 0.106(9) 0.043(6) -0.032(6) -0.006(5) C8 0.127(6) 0.108(6) 0.114(6) 0.000(4) 0.033(5) 0.015(5) C9 0.134(7) 0.124(7) 0.136(7) 0.016(5) 0.012(5) -0.017(5) C10 0.166(8) 0.170(8) 0.164(8) 0.013(5) 0.052(5) 0.008(5) C11 0.155(7) 0.131(7) 0.126(7) 0.002(5) 0.021(5) -0.005(5) C12 0.109(6) 0.116(6) 0.127(6) 0.017(5) 0.009(5) 0.000(5) C13 0.164(11) 0.167(11) 0.165(11) 0.000 0.039(5) 0.000 C14 0.144(7) 0.143(7) 0.143(7) -0.003(5) 0.042(5) -0.001(5) C15 0.155(8) 0.162(8) 0.159(8) 0.000(5) 0.046(5) 0.002(5) C16 0.111(8) 0.113(8) 0.113(8) 0.000 0.029(5) 0.000 C17 0.186(18) 0.190(18) 0.185(18) 0.002(5) 0.040(6) 0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C5 2.150(9) . ? Ir1 C6 2.163(10) . ? Ir1 C4 2.170(8) . ? Ir1 C3 2.177(8) . ? Ir1 C7 2.213(8) . ? Ir1 S1 2.363(2) . ? Ir1 S2 2.367(2) . ? Ir1 Ru2 2.7068(11) . ? Ru2 S1 2.381(2) 2_755 ? Ru2 S1 2.381(2) . ? Ru2 S2 2.409(2) . ? Ru2 S2 2.409(2) 2_755 ? Ru2 Ir1 2.7068(11) 2_755 ? S1 C1 1.853(8) . ? S2 C2 1.825(8) . ? B3 C1 1.708(12) . ? B3 C2 1.723(11) . ? B3 B8 1.739(13) . ? B3 B4 1.767(13) . ? B3 B7 1.771(13) . ? B3 H3 1.1000 . ? B4 C1 1.712(12) . ? B4 B8 1.776(15) . ? B4 B5 1.778(15) . ? B4 B9 1.782(15) . ? B4 H4 1.1000 . ? B5 C1 1.726(12) . ? B5 B6 1.774(15) . ? B5 B9 1.782(16) . ? B5 B10 1.792(16) . ? B5 H5 1.1000 . ? B6 C1 1.723(12) . ? B6 C2 1.734(12) . ? B6 B10 1.744(14) . ? B6 B11 1.765(15) . ? B6 H6 1.1000 . ? B7 C2 1.725(12) . ? B7 B8 1.768(15) . ? B7 B12 1.770(15) . ? B7 B11 1.785(14) . ? B7 H7 1.1000 . ? B8 B12 1.770(16) . ? B8 B9 1.784(16) . ? B8 H8 1.1000 . ? B9 B12 1.763(18) . ? B9 B10 1.769(16) . ? B9 H9 1.1000 . ? B10 B12 1.751(16) . ? B10 B11 1.767(16) . ? B10 H10 1.1000 . ? B11 C2 1.719(12) . ? B11 B12 1.766(15) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.600(10) . ? C3 C4 1.390(13) . ? C3 C7 1.437(14) . ? C3 C8 1.494(15) . ? C4 C5 1.434(14) . ? C4 C9 1.478(16) . ? C5 C6 1.370(14) . ? C5 C10 1.498(18) . ? C6 C7 1.360(15) . ? C6 C11 1.508(17) . ? C7 C12 1.522(15) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.364(9) 2_655 ? C13 C14 1.364(9) . ? C13 H13 0.9300 . ? C14 C15 1.369(9) . ? C14 H14 0.9300 . ? C15 C17 1.301(19) . ? C15 C16 1.375(9) . ? C16 C15 1.375(9) 2_655 ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? 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 Ir1 C6 37.0(4) . . ? C5 Ir1 C4 38.8(4) . . ? C6 Ir1 C4 63.1(4) . . ? C5 Ir1 C3 63.6(4) . . ? C6 Ir1 C3 63.3(4) . . ? C4 Ir1 C3 37.3(4) . . ? C5 Ir1 C7 61.3(4) . . ? C6 Ir1 C7 36.2(4) . . ? C4 Ir1 C7 62.0(3) . . ? C3 Ir1 C7 38.2(4) . . ? C5 Ir1 S1 170.4(3) . . ? C6 Ir1 S1 136.9(3) . . ? C4 Ir1 S1 135.8(3) . . ? C3 Ir1 S1 107.5(2) . . ? C7 Ir1 S1 109.5(3) . . ? C5 Ir1 S2 109.9(3) . . ? C6 Ir1 S2 109.3(3) . . ? C4 Ir1 S2 139.6(3) . . ? C3 Ir1 S2 172.5(3) . . ? C7 Ir1 S2 136.1(3) . . ? S1 Ir1 S2 78.61(7) . . ? C5 Ir1 Ru2 132.7(3) . . ? C6 Ir1 Ru2 162.0(3) . . ? C4 Ir1 Ru2 119.5(2) . . ? C3 Ir1 Ru2 130.8(3) . . ? C7 Ir1 Ru2 161.8(4) . . ? S1 Ir1 Ru2 55.53(6) . . ? S2 Ir1 Ru2 56.22(5) . . ? S1 Ru2 S1 169.49(10) 2_755 . ? S1 Ru2 S2 107.56(7) 2_755 . ? S1 Ru2 S2 77.42(6) . . ? S1 Ru2 S2 77.42(6) 2_755 2_755 ? S1 Ru2 S2 107.56(7) . 2_755 ? S2 Ru2 S2 125.49(10) . 2_755 ? S1 Ru2 Ir1 54.90(5) 2_755 2_755 ? S1 Ru2 Ir1 119.99(5) . 2_755 ? S2 Ru2 Ir1 162.44(5) . 2_755 ? S2 Ru2 Ir1 54.74(5) 2_755 2_755 ? S1 Ru2 Ir1 119.99(5) 2_755 . ? S1 Ru2 Ir1 54.90(5) . . ? S2 Ru2 Ir1 54.74(5) . . ? S2 Ru2 Ir1 162.44(5) 2_755 . ? Ir1 Ru2 Ir1 131.52(4) 2_755 . ? C1 S1 Ir1 104.0(3) . . ? C1 S1 Ru2 105.3(2) . . ? Ir1 S1 Ru2 69.58(6) . . ? C2 S2 Ir1 104.1(2) . . ? C2 S2 Ru2 104.8(2) . . ? Ir1 S2 Ru2 69.04(6) . . ? C1 B3 C2 55.6(5) . . ? C1 B3 B8 105.2(7) . . ? C2 B3 B8 105.3(7) . . ? C1 B3 B4 59.0(5) . . ? C2 B3 B4 104.3(6) . . ? B8 B3 B4 60.9(6) . . ? C1 B3 B7 104.1(6) . . ? C2 B3 B7 59.1(5) . . ? B8 B3 B7 60.5(6) . . ? B4 B3 B7 109.0(7) . . ? C1 B3 H3 125.2 . . ? C2 B3 H3 125.0 . . ? B8 B3 H3 122.1 . . ? B4 B3 H3 121.5 . . ? B7 B3 H3 121.7 . . ? C1 B4 B3 58.8(5) . . ? C1 B4 B8 103.5(7) . . ? B3 B4 B8 58.8(6) . . ? C1 B4 B5 59.2(5) . . ? B3 B4 B5 108.9(7) . . ? B8 B4 B5 108.3(8) . . ? C1 B4 B9 104.3(7) . . ? B3 B4 B9 107.5(8) . . ? B8 B4 B9 60.2(6) . . ? B5 B4 B9 60.1(6) . . ? C1 B4 H4 125.1 . . ? B3 B4 H4 121.6 . . ? B8 B4 H4 123.0 . . ? B5 B4 H4 120.6 . . ? B9 B4 H4 122.6 . . ? C1 B5 B6 59.0(5) . . ? C1 B5 B4 58.5(5) . . ? B6 B5 B4 108.2(7) . . ? C1 B5 B9 103.7(7) . . ? B6 B5 B9 106.7(8) . . ? B4 B5 B9 60.1(6) . . ? C1 B5 B10 102.9(7) . . ? B6 B5 B10 58.6(6) . . ? B4 B5 B10 107.2(8) . . ? B9 B5 B10 59.3(6) . . ? C1 B5 H5 125.4 . . ? B6 B5 H5 121.8 . . ? B4 B5 H5 121.3 . . ? B9 B5 H5 123.0 . . ? B10 B5 H5 123.7 . . ? C1 B6 C2 55.1(4) . . ? C1 B6 B10 105.1(7) . . ? C2 B6 B10 105.0(7) . . ? C1 B6 B11 103.4(6) . . ? C2 B6 B11 58.8(5) . . ? B10 B6 B11 60.5(6) . . ? C1 B6 B5 59.1(5) . . ? C2 B6 B5 104.3(7) . . ? B10 B6 B5 61.2(6) . . ? B11 B6 B5 109.4(8) . . ? C1 B6 H6 125.6 . . ? C2 B6 H6 125.3 . . ? B10 B6 H6 122.1 . . ? B11 B6 H6 121.9 . . ? B5 B6 H6 121.1 . . ? C2 B7 B8 104.0(7) . . ? C2 B7 B12 103.8(7) . . ? B8 B7 B12 60.0(6) . . ? C2 B7 B3 59.0(5) . . ? B8 B7 B3 58.8(6) . . ? B12 B7 B3 106.8(8) . . ? C2 B7 B11 58.6(5) . . ? B8 B7 B11 107.8(8) . . ? B12 B7 B11 59.6(6) . . ? B3 B7 B11 108.0(7) . . ? C2 B7 H7 125.0 . . ? B8 B7 H7 122.8 . . ? B12 B7 H7 123.0 . . ? B3 B7 H7 121.9 . . ? B11 B7 H7 121.4 . . ? B3 B8 B7 60.7(5) . . ? B3 B8 B12 108.3(7) . . ? B7 B8 B12 60.0(6) . . ? B3 B8 B4 60.4(5) . . ? B7 B8 B4 108.8(7) . . ? B12 B8 B4 107.5(8) . . ? B3 B8 B9 108.7(7) . . ? B7 B8 B9 108.3(8) . . ? B12 B8 B9 59.5(7) . . ? B4 B8 B9 60.1(6) . . ? B3 B8 H8 121.1 . . ? B7 B8 H8 121.2 . . ? B12 B8 H8 122.2 . . ? B4 B8 H8 121.6 . . ? B9 B8 H8 121.7 . . ? B12 B9 B10 59.4(7) . . ? B12 B9 B5 108.0(8) . . ? B10 B9 B5 60.6(6) . . ? B12 B9 B4 107.5(8) . . ? B10 B9 B4 108.0(7) . . ? B5 B9 B4 59.8(6) . . ? B12 B9 B8 59.9(7) . . ? B10 B9 B8 107.5(8) . . ? B5 B9 B8 107.8(7) . . ? B4 B9 B8 59.7(6) . . ? B12 B9 H9 122.1 . . ? B10 B9 H9 121.8 . . ? B5 B9 H9 121.5 . . ? B4 B9 H9 121.9 . . ? B8 B9 H9 122.0 . . ? B6 B10 B12 108.5(7) . . ? B6 B10 B11 60.3(6) . . ? B12 B10 B11 60.3(6) . . ? B6 B10 B9 108.6(7) . . ? B12 B10 B9 60.1(7) . . ? B11 B10 B9 108.6(8) . . ? B6 B10 B5 60.2(6) . . ? B12 B10 B5 108.1(8) . . ? B11 B10 B5 108.4(7) . . ? B9 B10 B5 60.0(6) . . ? B6 B10 H10 121.3 . . ? B12 B10 H10 121.6 . . ? B11 B10 H10 121.3 . . ? B9 B10 H10 121.4 . . ? B5 B10 H10 121.7 . . ? C2 B11 B6 59.7(5) . . ? C2 B11 B12 104.2(7) . . ? B6 B11 B12 106.9(8) . . ? C2 B11 B10 104.7(7) . . ? B6 B11 B10 59.2(6) . . ? B12 B11 B10 59.4(7) . . ? C2 B11 B7 59.0(5) . . ? B6 B11 B7 108.9(7) . . ? B12 B11 B7 59.8(6) . . ? B10 B11 B7 107.8(8) . . ? C2 B11 H11 124.4 . . ? B6 B11 H11 121.4 . . ? B12 B11 H11 123.2 . . ? B10 B11 H11 122.9 . . ? B7 B11 H11 121.1 . . ? B10 B12 B9 60.5(7) . . ? B10 B12 B11 60.3(6) . . ? B9 B12 B11 109.0(8) . . ? B10 B12 B7 109.2(7) . . ? B9 B12 B7 109.1(8) . . ? B11 B12 B7 60.6(6) . . ? B10 B12 B8 108.9(8) . . ? B9 B12 B8 60.6(7) . . ? B11 B12 B8 108.5(7) . . ? B7 B12 B8 59.9(6) . . ? B10 B12 H12 121.0 . . ? B9 B12 H12 120.9 . . ? B11 B12 H12 121.3 . . ? B7 B12 H12 121.0 . . ? B8 B12 H12 121.4 . . ? C2 C1 B3 62.7(5) . . ? C2 C1 B4 112.6(6) . . ? B3 C1 B4 62.2(5) . . ? C2 C1 B6 62.8(5) . . ? B3 C1 B6 115.6(6) . . ? B4 C1 B6 113.7(6) . . ? C2 C1 B5 112.7(6) . . ? B3 C1 B5 114.3(7) . . ? B4 C1 B5 62.3(6) . . ? B6 C1 B5 61.9(5) . . ? C2 C1 S1 111.5(5) . . ? B3 C1 S1 114.9(5) . . ? B4 C1 S1 124.9(6) . . ? B6 C1 S1 114.9(5) . . ? B5 C1 S1 124.5(6) . . ? C1 C2 B11 111.1(6) . . ? C1 C2 B3 61.7(5) . . ? B11 C2 B3 113.4(6) . . ? C1 C2 B7 111.1(6) . . ? B11 C2 B7 62.4(5) . . ? B3 C2 B7 61.8(5) . . ? C1 C2 B6 62.1(5) . . ? B11 C2 B6 61.5(5) . . ? B3 C2 B6 114.3(6) . . ? B7 C2 B6 113.2(6) . . ? C1 C2 S2 113.1(5) . . ? B11 C2 S2 124.8(6) . . ? B3 C2 S2 115.8(5) . . ? B7 C2 S2 125.0(6) . . ? B6 C2 S2 115.5(5) . . ? C4 C3 C7 106.1(9) . . ? C4 C3 C8 127.4(10) . . ? C7 C3 C8 126.3(10) . . ? C4 C3 Ir1 71.1(5) . . ? C7 C3 Ir1 72.3(5) . . ? C8 C3 Ir1 125.4(8) . . ? C3 C4 C5 107.7(8) . . ? C3 C4 C9 121.1(11) . . ? C5 C4 C9 131.2(11) . . ? C3 C4 Ir1 71.6(5) . . ? C5 C4 Ir1 69.8(5) . . ? C9 C4 Ir1 125.3(8) . . ? C6 C5 C4 107.9(9) . . ? C6 C5 C10 129.8(13) . . ? C4 C5 C10 122.3(13) . . ? C6 C5 Ir1 72.0(6) . . ? C4 C5 Ir1 71.4(5) . . ? C10 C5 Ir1 123.7(10) . . ? C7 C6 C5 109.2(10) . . ? C7 C6 C11 122.6(12) . . ? C5 C6 C11 127.8(12) . . ? C7 C6 Ir1 73.9(6) . . ? C5 C6 Ir1 70.9(6) . . ? C11 C6 Ir1 126.5(9) . . ? C6 C7 C3 109.0(9) . . ? C6 C7 C12 130.3(11) . . ? C3 C7 C12 120.7(12) . . ? C6 C7 Ir1 69.9(6) . . ? C3 C7 Ir1 69.5(5) . . ? C12 C7 Ir1 124.7(8) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C14 132.4(19) 2_655 . ? C14 C13 H13 113.8 2_655 . ? C14 C13 H13 113.8 . . ? C13 C14 C15 113.7(13) . . ? C13 C14 H14 123.2 . . ? C15 C14 H14 123.2 . . ? C17 C15 C14 119.2(14) . . ? C17 C15 C16 125.5(14) . . ? C14 C15 C16 115.2(13) . . ? C15 C16 C15 129.8(18) . 2_655 ? C15 C16 H16 115.1 . . ? C15 C16 H16 115.1 2_655 . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.19 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.399 _refine_diff_density_min -1.239 _refine_diff_density_rms 0.166 # Attachment '1d.cif' data_f70326c _database_code_depnum_ccdc_archive 'CCDC 673414' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H29 B10 Ir O2 S2' _chemical_formula_weight 593.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 '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 11.403(3) _cell_length_b 14.648(4) _cell_length_c 13.756(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.747(4) _cell_angle_gamma 90.00 _cell_volume 2292.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 901 _cell_measurement_theta_min 2.249 _cell_measurement_theta_max 27.092 _exptl_crystal_description prism _exptl_crystal_colour blue _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 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 6.014 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3792 _exptl_absorpt_correction_T_max 0.4657 _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_% 8.23 _diffrn_reflns_number 9854 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 27.12 _reflns_number_total 4946 _reflns_number_gt 4055 _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^)+(0.0290P)^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 4946 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 0.286354(12) 0.085128(10) 0.258685(10) 0.02956(6) Uani 1 1 d . . . S1 S 0.42081(8) 0.00335(7) 0.18273(7) 0.0345(2) Uani 1 1 d . . . S2 S 0.42633(9) 0.18121(7) 0.32266(8) 0.0390(2) Uani 1 1 d . . . O1 O 0.4788(3) 0.2094(2) 0.0969(2) 0.0477(7) Uani 1 1 d . . . O2 O 0.5748(3) 0.0051(2) 0.3988(2) 0.0546(8) Uani 1 1 d . . . B3 B 0.5715(4) 0.1700(3) 0.1456(3) 0.0385(11) Uani 1 1 d . . . B4 B 0.6527(4) 0.0706(3) 0.1153(3) 0.0391(11) Uani 1 1 d . . . H4 H 0.6372 0.0407 0.0422 0.047 Uiso 1 1 calc R . . B5 B 0.6863(4) 0.0002(4) 0.2198(3) 0.0427(12) Uani 1 1 d . . . H5 H 0.6920 -0.0745 0.2129 0.051 Uiso 1 1 calc R . . B6 B 0.6295(4) 0.0464(4) 0.3258(3) 0.0430(12) Uani 1 1 d . . . B7 B 0.6906(4) 0.1577(4) 0.3417(4) 0.0487(13) Uani 1 1 d . . . H7 H 0.6991 0.1875 0.4152 0.058 Uiso 1 1 calc R . . B8 B 0.6583(4) 0.2275(4) 0.2386(4) 0.0470(12) Uani 1 1 d . . . H8 H 0.6470 0.3015 0.2474 0.056 Uiso 1 1 calc R . . B9 B 0.7239(4) 0.1772(4) 0.1368(4) 0.0483(13) Uani 1 1 d . . . H9 H 0.7593 0.2177 0.0781 0.058 Uiso 1 1 calc R . . B10 B 0.7929(4) 0.0745(4) 0.1779(4) 0.0506(14) Uani 1 1 d . . . H10 H 0.8710 0.0482 0.1443 0.061 Uiso 1 1 calc R . . B11 B 0.7785(5) 0.0634(4) 0.3040(4) 0.0518(14) Uani 1 1 d . . . H11 H 0.8484 0.0317 0.3515 0.062 Uiso 1 1 calc R . . B12 B 0.7964(4) 0.1735(4) 0.2547(4) 0.0552(15) Uani 1 1 d . . . H12 H 0.8771 0.2131 0.2721 0.066 Uiso 1 1 calc R . . C1 C 0.5577(3) 0.0596(3) 0.2050(3) 0.0309(8) Uani 1 1 d . . . C2 C 0.5600(3) 0.1482(3) 0.2741(3) 0.0329(8) Uani 1 1 d . . . C3 C 0.4328(4) 0.1790(4) 0.0053(3) 0.0614(13) Uani 1 1 d . . . H3A H 0.4912 0.1441 -0.0254 0.092 Uiso 1 1 calc R . . H3B H 0.4106 0.2307 -0.0347 0.092 Uiso 1 1 calc R . . H3C H 0.3650 0.1416 0.0134 0.092 Uiso 1 1 calc R . . C4 C 0.5548(5) -0.0890(3) 0.4052(4) 0.0667(15) Uani 1 1 d . . . H4A H 0.4970 -0.1070 0.3550 0.100 Uiso 1 1 calc R . . H4B H 0.5268 -0.1031 0.4678 0.100 Uiso 1 1 calc R . . H4C H 0.6268 -0.1212 0.3972 0.100 Uiso 1 1 calc R . . C5 C 0.1229(3) 0.1202(3) 0.1830(3) 0.0429(10) Uani 1 1 d . . . C6 C 0.1229(3) 0.0224(3) 0.1957(3) 0.0385(9) Uani 1 1 d . . . C7 C 0.1350(3) 0.0058(3) 0.2986(3) 0.0396(10) Uani 1 1 d . . . C8 C 0.1366(4) 0.0937(3) 0.3479(3) 0.0389(10) Uani 1 1 d . . . C9 C 0.1285(3) 0.1638(3) 0.2778(3) 0.0393(10) Uani 1 1 d . . . C10 C 0.1087(4) 0.1681(4) 0.0865(3) 0.0664(14) Uani 1 1 d . . . H10A H 0.1435 0.1319 0.0379 0.100 Uiso 1 1 calc R . . H10B H 0.1468 0.2265 0.0913 0.100 Uiso 1 1 calc R . . H10C H 0.0266 0.1765 0.0687 0.100 Uiso 1 1 calc R . . C11 C 0.1135(4) -0.0473(4) 0.1171(4) 0.0635(14) Uani 1 1 d . . . H11A H 0.0323 -0.0627 0.1027 0.095 Uiso 1 1 calc R . . H11B H 0.1561 -0.1011 0.1382 0.095 Uiso 1 1 calc R . . H11C H 0.1459 -0.0234 0.0597 0.095 Uiso 1 1 calc R . . C12 C 0.1364(5) -0.0853(3) 0.3464(4) 0.0622(14) Uani 1 1 d . . . H12A H 0.0598 -0.0986 0.3676 0.093 Uiso 1 1 calc R . . H12B H 0.1926 -0.0850 0.4015 0.093 Uiso 1 1 calc R . . H12C H 0.1579 -0.1310 0.3008 0.093 Uiso 1 1 calc R . . C13 C 0.1391(5) 0.1045(4) 0.4559(3) 0.0673(16) Uani 1 1 d . . . H13A H 0.1687 0.1640 0.4736 0.101 Uiso 1 1 calc R . . H13B H 0.1892 0.0587 0.4864 0.101 Uiso 1 1 calc R . . H13C H 0.0610 0.0978 0.4770 0.101 Uiso 1 1 calc R . . C14 C 0.1261(4) 0.2637(3) 0.2959(4) 0.0528(12) Uani 1 1 d . . . H14A H 0.0464 0.2831 0.3013 0.079 Uiso 1 1 calc R . . H14B H 0.1589 0.2952 0.2428 0.079 Uiso 1 1 calc R . . H14C H 0.1715 0.2774 0.3554 0.079 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 0.02073(8) 0.03012(9) 0.03809(9) -0.00052(7) 0.00382(5) -0.00080(6) S1 0.0264(5) 0.0320(5) 0.0456(5) -0.0080(4) 0.0056(4) -0.0024(4) S2 0.0280(5) 0.0391(6) 0.0500(6) -0.0139(5) 0.0043(4) -0.0012(4) O1 0.0432(18) 0.0458(18) 0.0531(18) 0.0075(14) -0.0049(14) 0.0094(14) O2 0.062(2) 0.058(2) 0.0445(17) 0.0080(15) 0.0089(16) 0.0010(17) B3 0.031(2) 0.038(3) 0.047(3) 0.008(2) 0.003(2) -0.003(2) B4 0.031(2) 0.046(3) 0.041(2) 0.005(2) 0.011(2) 0.005(2) B5 0.028(2) 0.051(3) 0.050(3) 0.008(2) 0.008(2) 0.013(2) B6 0.036(3) 0.054(3) 0.039(3) 0.005(2) 0.000(2) 0.006(2) B7 0.026(2) 0.060(4) 0.058(3) -0.006(3) -0.008(2) -0.004(3) B8 0.034(3) 0.040(3) 0.067(3) -0.001(2) 0.002(2) -0.010(2) B9 0.030(3) 0.055(3) 0.061(3) 0.011(3) 0.011(2) -0.008(2) B10 0.026(2) 0.067(4) 0.060(3) 0.005(3) 0.009(2) 0.006(2) B11 0.028(3) 0.071(4) 0.056(3) 0.003(3) -0.005(2) 0.006(3) B12 0.024(2) 0.069(4) 0.072(4) 0.002(3) -0.002(2) -0.012(3) C1 0.0233(19) 0.031(2) 0.038(2) 0.0014(16) 0.0046(15) 0.0018(16) C2 0.0238(19) 0.034(2) 0.041(2) -0.0031(17) 0.0018(16) -0.0020(17) C3 0.054(3) 0.079(4) 0.050(3) 0.018(3) -0.003(2) 0.009(3) C4 0.080(4) 0.060(4) 0.060(3) 0.017(3) 0.003(3) -0.009(3) C5 0.023(2) 0.051(3) 0.054(3) 0.001(2) -0.0005(18) -0.0002(19) C6 0.022(2) 0.042(2) 0.051(2) -0.0039(19) 0.0012(17) -0.0033(18) C7 0.024(2) 0.036(2) 0.059(3) 0.0061(19) 0.0106(18) -0.0061(17) C8 0.031(2) 0.042(2) 0.045(2) -0.0016(19) 0.0114(18) -0.0012(18) C9 0.0197(19) 0.034(2) 0.065(3) -0.0033(19) 0.0051(18) 0.0001(17) C10 0.055(3) 0.077(4) 0.066(3) 0.020(3) -0.006(3) 0.003(3) C11 0.048(3) 0.066(3) 0.076(3) -0.029(3) -0.003(3) -0.001(3) C12 0.062(3) 0.044(3) 0.083(4) 0.011(3) 0.026(3) -0.001(2) C13 0.074(4) 0.078(4) 0.052(3) -0.011(3) 0.022(3) -0.005(3) C14 0.031(2) 0.038(3) 0.091(4) -0.003(2) 0.011(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 Ir1 C5 2.137(4) . ? Ir1 C9 2.167(4) . ? Ir1 C8 2.170(4) . ? Ir1 C7 2.180(4) . ? Ir1 C6 2.204(4) . ? Ir1 S1 2.2554(10) . ? Ir1 S2 2.2626(11) . ? S1 C1 1.774(4) . ? S2 C2 1.771(4) . ? O1 B3 1.343(5) . ? O1 C3 1.406(5) . ? O2 B6 1.358(5) . ? O2 C4 1.400(5) . ? B3 B9 1.753(6) . ? B3 B8 1.778(7) . ? B3 B4 1.788(7) . ? B3 C2 1.809(6) . ? B3 C1 1.824(6) . ? B4 C1 1.702(5) . ? B4 B10 1.767(7) . ? B4 B9 1.776(7) . ? B4 B5 1.791(7) . ? B5 C1 1.706(6) . ? B5 B10 1.757(7) . ? B5 B6 1.768(6) . ? B5 B11 1.773(8) . ? B6 B11 1.763(7) . ? B6 B7 1.780(8) . ? B6 C2 1.813(6) . ? B6 C1 1.814(6) . ? B7 C2 1.709(6) . ? B7 B8 1.768(8) . ? B7 B12 1.770(7) . ? B7 B11 1.803(8) . ? B8 C2 1.707(6) . ? B8 B12 1.764(7) . ? B8 B9 1.789(7) . ? B9 B12 1.772(8) . ? B9 B10 1.773(8) . ? B10 B11 1.760(8) . ? B10 B12 1.792(8) . ? B11 B12 1.767(8) . ? C1 C2 1.608(5) . ? C5 C6 1.443(6) . ? C5 C9 1.449(6) . ? C5 C10 1.501(6) . ? C6 C7 1.435(6) . ? C6 C11 1.486(6) . ? C7 C8 1.454(5) . ? C7 C12 1.487(6) . ? C8 C9 1.407(6) . ? C8 C13 1.492(6) . ? C9 C14 1.485(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Ir1 C9 39.35(16) . . ? C5 Ir1 C8 64.42(16) . . ? C9 Ir1 C8 37.86(15) . . ? C5 Ir1 C7 64.61(16) . . ? C9 Ir1 C7 64.86(16) . . ? C8 Ir1 C7 39.05(14) . . ? C5 Ir1 C6 38.79(16) . . ? C9 Ir1 C6 65.27(15) . . ? C8 Ir1 C6 64.54(15) . . ? C7 Ir1 C6 38.19(15) . . ? C5 Ir1 S1 119.99(12) . . ? C9 Ir1 S1 159.01(12) . . ? C8 Ir1 S1 151.20(11) . . ? C7 Ir1 S1 114.02(11) . . ? C6 Ir1 S1 100.34(11) . . ? C5 Ir1 S2 127.62(13) . . ? C9 Ir1 S2 101.09(11) . . ? C8 Ir1 S2 107.76(12) . . ? C7 Ir1 S2 141.56(12) . . ? C6 Ir1 S2 165.73(11) . . ? S1 Ir1 S2 91.54(4) . . ? C1 S1 Ir1 106.90(13) . . ? C2 S2 Ir1 106.62(13) . . ? B3 O1 C3 123.1(4) . . ? B6 O2 C4 124.7(4) . . ? O1 B3 B9 133.7(4) . . ? O1 B3 B8 122.5(4) . . ? B9 B3 B8 60.9(3) . . ? O1 B3 B4 129.5(4) . . ? B9 B3 B4 60.2(3) . . ? B8 B3 B4 106.3(3) . . ? O1 B3 C2 117.2(3) . . ? B9 B3 C2 102.3(3) . . ? B8 B3 C2 56.8(2) . . ? B4 B3 C2 99.0(3) . . ? O1 B3 C1 121.1(3) . . ? B9 B3 C1 101.5(3) . . ? B8 B3 C1 99.1(3) . . ? B4 B3 C1 56.2(2) . . ? C2 B3 C1 52.5(2) . . ? C1 B4 B10 104.3(3) . . ? C1 B4 B9 105.6(3) . . ? B10 B4 B9 60.1(3) . . ? C1 B4 B3 62.9(2) . . ? B10 B4 B3 109.0(4) . . ? B9 B4 B3 58.9(3) . . ? C1 B4 B5 58.4(2) . . ? B10 B4 B5 59.2(3) . . ? B9 B4 B5 107.5(4) . . ? B3 B4 B5 111.6(3) . . ? C1 B5 B10 104.6(4) . . ? C1 B5 B6 62.9(3) . . ? B10 B5 B6 109.4(4) . . ? C1 B5 B11 106.3(4) . . ? B10 B5 B11 59.8(3) . . ? B6 B5 B11 59.7(3) . . ? C1 B5 B4 58.2(2) . . ? B10 B5 B4 59.7(3) . . ? B6 B5 B4 111.8(3) . . ? B11 B5 B4 108.1(4) . . ? O2 B6 B11 133.1(4) . . ? O2 B6 B5 130.5(4) . . ? B11 B6 B5 60.3(3) . . ? O2 B6 B7 120.8(4) . . ? B11 B6 B7 61.2(3) . . ? B5 B6 B7 106.8(3) . . ? O2 B6 C2 116.5(4) . . ? B11 B6 C2 102.6(3) . . ? B5 B6 C2 99.5(3) . . ? B7 B6 C2 56.8(3) . . ? O2 B6 C1 121.5(4) . . ? B11 B6 C1 102.2(3) . . ? B5 B6 C1 56.8(2) . . ? B7 B6 C1 99.5(3) . . ? C2 B6 C1 52.6(2) . . ? C2 B7 B8 58.8(3) . . ? C2 B7 B12 104.5(3) . . ? B8 B7 B12 59.8(3) . . ? C2 B7 B6 62.6(3) . . ? B8 B7 B6 111.8(4) . . ? B12 B7 B6 108.4(4) . . ? C2 B7 B11 105.2(4) . . ? B8 B7 B11 107.7(4) . . ? B12 B7 B11 59.3(3) . . ? B6 B7 B11 58.9(3) . . ? C2 B8 B12 104.9(4) . . ? C2 B8 B7 58.9(3) . . ? B12 B8 B7 60.1(3) . . ? C2 B8 B3 62.5(3) . . ? B12 B8 B3 109.2(4) . . ? B7 B8 B3 112.4(4) . . ? C2 B8 B9 105.1(3) . . ? B12 B8 B9 59.8(3) . . ? B7 B8 B9 108.3(4) . . ? B3 B8 B9 58.9(3) . . ? B3 B9 B12 109.9(3) . . ? B3 B9 B10 110.4(3) . . ? B12 B9 B10 60.7(3) . . ? B3 B9 B4 60.9(3) . . ? B12 B9 B4 107.9(4) . . ? B10 B9 B4 59.7(3) . . ? B3 B9 B8 60.2(3) . . ? B12 B9 B8 59.4(3) . . ? B10 B9 B8 107.4(4) . . ? B4 B9 B8 106.4(3) . . ? B5 B10 B11 60.6(3) . . ? B5 B10 B4 61.1(3) . . ? B11 B10 B4 109.8(3) . . ? B5 B10 B9 109.2(3) . . ? B11 B10 B9 109.0(4) . . ? B4 B10 B9 60.2(3) . . ? B5 B10 B12 107.3(3) . . ? B11 B10 B12 59.7(3) . . ? B4 B10 B12 107.3(3) . . ? B9 B10 B12 59.6(3) . . ? B10 B11 B6 109.5(4) . . ? B10 B11 B12 61.1(3) . . ? B6 B11 B12 109.3(4) . . ? B10 B11 B5 59.6(3) . . ? B6 B11 B5 60.0(3) . . ? B12 B11 B5 107.7(4) . . ? B10 B11 B7 107.6(4) . . ? B6 B11 B7 59.9(3) . . ? B12 B11 B7 59.4(3) . . ? B5 B11 B7 105.7(3) . . ? B8 B12 B11 109.4(4) . . ? B8 B12 B7 60.0(3) . . ? B11 B12 B7 61.3(3) . . ? B8 B12 B9 60.8(3) . . ? B11 B12 B9 108.7(4) . . ? B7 B12 B9 108.9(3) . . ? B8 B12 B10 107.7(4) . . ? B11 B12 B10 59.3(3) . . ? B7 B12 B10 107.6(4) . . ? B9 B12 B10 59.7(3) . . ? C2 C1 B4 111.4(3) . . ? C2 C1 B5 111.1(3) . . ? B4 C1 B5 63.4(3) . . ? C2 C1 S1 117.2(2) . . ? B4 C1 S1 120.9(3) . . ? B5 C1 S1 121.6(3) . . ? C2 C1 B6 63.6(3) . . ? B4 C1 B6 113.8(3) . . ? B5 C1 B6 60.2(3) . . ? S1 C1 B6 116.6(3) . . ? C2 C1 B3 63.3(2) . . ? B4 C1 B3 60.8(2) . . ? B5 C1 B3 114.0(3) . . ? S1 C1 B3 115.8(3) . . ? B6 C1 B3 117.3(3) . . ? C1 C2 B8 111.5(3) . . ? C1 C2 B7 111.5(3) . . ? B8 C2 B7 62.3(3) . . ? C1 C2 S2 117.5(2) . . ? B8 C2 S2 121.3(3) . . ? B7 C2 S2 120.9(3) . . ? C1 C2 B3 64.2(2) . . ? B8 C2 B3 60.7(3) . . ? B7 C2 B3 113.6(3) . . ? S2 C2 B3 116.1(3) . . ? C1 C2 B6 63.7(2) . . ? B8 C2 B6 113.2(3) . . ? B7 C2 B6 60.6(3) . . ? S2 C2 B6 116.2(2) . . ? B3 C2 B6 118.1(3) . . ? C6 C5 C9 109.2(4) . . ? C6 C5 C10 124.7(4) . . ? C9 C5 C10 125.9(4) . . ? C6 C5 Ir1 73.1(2) . . ? C9 C5 Ir1 71.4(2) . . ? C10 C5 Ir1 125.7(3) . . ? C7 C6 C5 106.6(4) . . ? C7 C6 C11 126.8(4) . . ? C5 C6 C11 126.6(4) . . ? C7 C6 Ir1 70.0(2) . . ? C5 C6 Ir1 68.1(2) . . ? C11 C6 Ir1 126.3(3) . . ? C6 C7 C8 107.9(3) . . ? C6 C7 C12 125.8(4) . . ? C8 C7 C12 126.1(4) . . ? C6 C7 Ir1 71.8(2) . . ? C8 C7 Ir1 70.1(2) . . ? C12 C7 Ir1 127.1(3) . . ? C9 C8 C7 109.1(4) . . ? C9 C8 C13 126.9(4) . . ? C7 C8 C13 123.9(4) . . ? C9 C8 Ir1 70.9(2) . . ? C7 C8 Ir1 70.8(2) . . ? C13 C8 Ir1 127.2(3) . . ? C8 C9 C5 107.0(4) . . ? C8 C9 C14 127.3(4) . . ? C5 C9 C14 125.8(4) . . ? C8 C9 Ir1 71.2(2) . . ? C5 C9 Ir1 69.2(2) . . ? C14 C9 Ir1 124.7(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.852 _refine_diff_density_min -1.251 _refine_diff_density_rms 0.133 # Attachment '1e.cif' data_f50403b _database_code_depnum_ccdc_archive 'CCDC 673415' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H54 B20 Ir2 O2 S4' _chemical_formula_weight 1127.53 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' O O 0.0106 0.0060 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.495(17) _cell_length_b 15.357(20) _cell_length_c 21.68(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.542(19) _cell_angle_gamma 90.00 _cell_volume 4455(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 968 _cell_measurement_theta_min 2.582 _cell_measurement_theta_max 21.303 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 6.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5768 _exptl_absorpt_correction_T_max 0.7474 _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 18364 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.0753 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7831 _reflns_number_gt 5138 _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^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7831 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0791 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 0.24285(2) 0.44192(2) 0.088327(15) 0.04341(11) Uani 1 1 d . . . S1 S 0.23921(17) 0.44981(13) -0.01584(10) 0.0517(6) Uani 1 1 d . . . S2 S 0.2820(2) 0.29919(15) 0.08952(10) 0.0680(8) Uani 1 1 d . . . O1 O 0.0896(5) 0.2872(5) -0.0197(3) 0.087(2) Uani 1 1 d . . . C1 C 0.2688(6) 0.3443(5) -0.0408(3) 0.042(2) Uani 1 1 d . . . C2 C 0.2930(6) 0.2688(5) 0.0119(3) 0.043(2) Uani 1 1 d . . . C3 C 0.0404(9) 0.2358(8) 0.0232(6) 0.130(5) Uani 1 1 d . . . H3A H -0.0031 0.1942 0.0004 0.195 Uiso 1 1 calc R . . H3B H 0.0020 0.2734 0.0463 0.195 Uiso 1 1 calc R . . H3C H 0.0897 0.2057 0.0514 0.195 Uiso 1 1 calc R . . C4 C 0.2075(8) 0.5762(5) 0.1082(4) 0.055(2) Uani 1 1 d . . . C5 C 0.3022(7) 0.5535(6) 0.1391(4) 0.055(2) Uani 1 1 d . . . C6 C 0.2904(7) 0.4858(5) 0.1830(4) 0.050(2) Uani 1 1 d . . . C7 C 0.1877(7) 0.4651(5) 0.1755(4) 0.049(2) Uani 1 1 d . . . C8 C 0.1364(6) 0.5208(6) 0.1296(4) 0.054(2) Uani 1 1 d . . . C9 C 0.1859(9) 0.6503(6) 0.0612(4) 0.099(4) Uani 1 1 d . . . H9A H 0.1231 0.6401 0.0361 0.148 Uiso 1 1 calc R . . H9B H 0.2381 0.6529 0.0352 0.148 Uiso 1 1 calc R . . H9C H 0.1832 0.7045 0.0830 0.148 Uiso 1 1 calc R . . C10 C 0.4021(8) 0.5977(7) 0.1304(5) 0.106(4) Uani 1 1 d . . . H10A H 0.3976 0.6218 0.0892 0.159 Uiso 1 1 calc R . . H10B H 0.4550 0.5554 0.1359 0.159 Uiso 1 1 calc R . . H10C H 0.4160 0.6434 0.1605 0.159 Uiso 1 1 calc R . . C11 C 0.3717(8) 0.4438(7) 0.2274(5) 0.105(4) Uani 1 1 d . . . H11A H 0.3752 0.4713 0.2674 0.158 Uiso 1 1 calc R . . H11B H 0.4346 0.4504 0.2117 0.158 Uiso 1 1 calc R . . H11C H 0.3573 0.3830 0.2313 0.158 Uiso 1 1 calc R . . C12 C 0.1388(8) 0.4006(6) 0.2141(4) 0.080(3) Uani 1 1 d . . . H12A H 0.1134 0.4304 0.2476 0.120 Uiso 1 1 calc R . . H12B H 0.1869 0.3578 0.2307 0.120 Uiso 1 1 calc R . . H12C H 0.0847 0.3723 0.1885 0.120 Uiso 1 1 calc R . . C13 C 0.0234(7) 0.5195(7) 0.1084(6) 0.100(4) Uani 1 1 d . . . H13A H -0.0101 0.5523 0.1371 0.150 Uiso 1 1 calc R . . H13B H -0.0002 0.4605 0.1070 0.150 Uiso 1 1 calc R . . H13C H 0.0098 0.5450 0.0677 0.150 Uiso 1 1 calc R . . B3 B 0.1763(7) 0.2626(7) -0.0391(5) 0.049(3) Uani 1 1 d . . . B4 B 0.2130(8) 0.3015(7) -0.1091(5) 0.055(3) Uani 1 1 d . . . H4 H 0.1594 0.3370 -0.1425 0.065 Uiso 1 1 calc R . . B5 B 0.3425(8) 0.3295(7) -0.0974(5) 0.065(3) Uani 1 1 d . . . H5 H 0.3718 0.3830 -0.1234 0.078 Uiso 1 1 calc R . . B6 B 0.3946(8) 0.3111(7) -0.0181(6) 0.069(3) Uani 1 1 d . . . H6 H 0.4549 0.3505 0.0071 0.083 Uiso 1 1 calc R . . B7 B 0.2508(8) 0.1711(6) -0.0175(5) 0.057(3) Uani 1 1 d . . . H7 H 0.2210 0.1199 0.0105 0.068 Uiso 1 1 calc R . . B8 B 0.2027(8) 0.1884(7) -0.0953(5) 0.059(3) Uani 1 1 d . . . H8 H 0.1429 0.1481 -0.1200 0.070 Uiso 1 1 calc R . . B9 B 0.3026(9) 0.2298(7) -0.1328(5) 0.066(3) Uani 1 1 d . . . H9 H 0.3066 0.2174 -0.1824 0.080 Uiso 1 1 calc R . . B10 B 0.4124(8) 0.2336(7) -0.0777(6) 0.073(4) Uani 1 1 d . . . H10 H 0.4870 0.2228 -0.0916 0.087 Uiso 1 1 calc R . . B11 B 0.3798(8) 0.1976(7) -0.0055(5) 0.062(3) Uani 1 1 d . . . H11 H 0.4327 0.1634 0.0291 0.075 Uiso 1 1 calc R . . B12 B 0.3259(9) 0.1470(8) -0.0755(5) 0.071(3) Uani 1 1 d . . . H12 H 0.3451 0.0799 -0.0871 0.085 Uiso 1 1 calc R . . Ir2 Ir 0.25913(2) 0.95290(2) 0.195848(14) 0.04061(10) Uani 1 1 d . . . S3 S 0.36199(15) 0.84140(14) 0.22872(10) 0.0515(6) Uani 1 1 d . . . S4 S 0.15904(16) 0.92715(13) 0.26926(11) 0.0524(6) Uani 1 1 d . . . O2 O 0.1566(5) 0.7344(4) 0.2047(3) 0.0703(18) Uani 1 1 d . . . C14 C 0.3071(6) 0.7894(5) 0.2888(4) 0.041(2) Uani 1 1 d . . . C15 C 0.2058(6) 0.8318(5) 0.3098(3) 0.041(2) Uani 1 1 d . . . C16 C 0.0504(7) 0.7433(8) 0.1846(5) 0.101(4) Uani 1 1 d . . . H16A H 0.0172 0.6896 0.1918 0.152 Uiso 1 1 calc R . . H16B H 0.0395 0.7569 0.1410 0.152 Uiso 1 1 calc R . . H16C H 0.0239 0.7892 0.2076 0.152 Uiso 1 1 calc R . . C17 C 0.1704(6) 1.0184(6) 0.1213(4) 0.057(2) Uani 1 1 d . . . C18 C 0.2575(9) 0.9780(5) 0.0989(4) 0.065(3) Uani 1 1 d . . . C19 C 0.3430(7) 1.0185(6) 0.1307(4) 0.051(2) Uani 1 1 d . . . C20 C 0.3132(6) 1.0790(5) 0.1719(4) 0.047(2) Uani 1 1 d . . . C21 C 0.2064(6) 1.0807(5) 0.1650(4) 0.048(2) Uani 1 1 d . . . C22 C 0.0622(8) 1.0003(8) 0.0981(6) 0.131(5) Uani 1 1 d . . . H22A H 0.0217 1.0161 0.1296 0.197 Uiso 1 1 calc R . . H22B H 0.0537 0.9395 0.0887 0.197 Uiso 1 1 calc R . . H22C H 0.0422 1.0339 0.0612 0.197 Uiso 1 1 calc R . . C23 C 0.2544(11) 0.9105(7) 0.0489(5) 0.134(6) Uani 1 1 d . . . H23A H 0.3154 0.8776 0.0543 0.201 Uiso 1 1 calc R . . H23B H 0.2468 0.9385 0.0089 0.201 Uiso 1 1 calc R . . H23C H 0.1988 0.8721 0.0513 0.201 Uiso 1 1 calc R . . C24 C 0.4494(8) 0.9988(7) 0.1194(6) 0.111(5) Uani 1 1 d . . . H24A H 0.4952 1.0326 0.1474 0.166 Uiso 1 1 calc R . . H24B H 0.4574 1.0134 0.0773 0.166 Uiso 1 1 calc R . . H24C H 0.4630 0.9380 0.1264 0.166 Uiso 1 1 calc R . . C25 C 0.3820(7) 1.1347(6) 0.2160(4) 0.082(3) Uani 1 1 d . . . H25A H 0.4435 1.1040 0.2281 0.123 Uiso 1 1 calc R . . H25B H 0.3507 1.1474 0.2522 0.123 Uiso 1 1 calc R . . H25C H 0.3957 1.1881 0.1957 0.123 Uiso 1 1 calc R . . C26 C 0.1427(8) 1.1421(6) 0.1992(5) 0.095(4) Uani 1 1 d . . . H26A H 0.1392 1.1982 0.1794 0.142 Uiso 1 1 calc R . . H26B H 0.1724 1.1481 0.2417 0.142 Uiso 1 1 calc R . . H26C H 0.0766 1.1186 0.1979 0.142 Uiso 1 1 calc R . . B13 B 0.1938(7) 0.7327(6) 0.2656(5) 0.051(3) Uani 1 1 d . . . B14 B 0.3065(7) 0.6777(6) 0.2943(5) 0.053(3) Uani 1 1 d . . . H14 H 0.3423 0.6338 0.2638 0.064 Uiso 1 1 calc R . . B15 B 0.3789(8) 0.7430(7) 0.3514(4) 0.055(3) Uani 1 1 d . . . H15 H 0.4611 0.7404 0.3576 0.067 Uiso 1 1 calc R . . B16 B 0.3155(7) 0.8432(7) 0.3598(4) 0.052(3) Uani 1 1 d . . . H16 H 0.3551 0.9050 0.3712 0.062 Uiso 1 1 calc R . . B17 B 0.1278(7) 0.7531(7) 0.3305(5) 0.055(3) Uani 1 1 d . . . H17 H 0.0458 0.7585 0.3237 0.066 Uiso 1 1 calc R . . B18 B 0.1916(8) 0.6529(7) 0.3237(5) 0.067(3) Uani 1 1 d . . . H18 H 0.1516 0.5912 0.3133 0.081 Uiso 1 1 calc R . . B19 B 0.3048(9) 0.6573(8) 0.3745(5) 0.078(4) Uani 1 1 d . . . H19 H 0.3388 0.5980 0.3966 0.094 Uiso 1 1 calc R . . B20 B 0.3101(8) 0.7578(8) 0.4140(5) 0.068(3) Uani 1 1 d . . . H20 H 0.3469 0.7639 0.4622 0.082 Uiso 1 1 calc R . . B21 B 0.2011(8) 0.8164(7) 0.3857(5) 0.059(3) Uani 1 1 d . . . H21 H 0.1658 0.8624 0.4150 0.070 Uiso 1 1 calc R . . B22 B 0.1946(9) 0.7039(7) 0.3959(5) 0.070(4) Uani 1 1 d . . . H22 H 0.1558 0.6753 0.4326 0.084 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 0.0509(2) 0.04018(19) 0.0388(2) -0.00172(15) 0.00456(15) -0.00045(17) S1 0.0737(16) 0.0383(12) 0.0439(13) 0.0031(10) 0.0110(11) 0.0076(12) S2 0.116(2) 0.0452(14) 0.0400(14) 0.0050(11) 0.0000(14) 0.0137(14) O1 0.073(5) 0.091(5) 0.102(6) 0.025(4) 0.029(4) 0.001(4) C1 0.047(5) 0.042(5) 0.037(5) 0.001(4) 0.007(4) -0.002(4) C2 0.056(6) 0.035(5) 0.038(5) 0.000(4) 0.004(4) 0.001(4) C3 0.105(10) 0.149(13) 0.146(12) 0.048(10) 0.058(9) -0.022(9) C4 0.094(8) 0.024(4) 0.047(6) -0.002(4) 0.011(5) 0.001(5) C5 0.059(6) 0.059(6) 0.052(6) -0.016(5) 0.025(5) -0.018(5) C6 0.063(6) 0.048(5) 0.037(5) -0.010(4) 0.002(4) -0.005(5) C7 0.061(6) 0.041(5) 0.048(5) -0.001(4) 0.018(4) -0.014(4) C8 0.056(6) 0.050(5) 0.058(6) -0.014(5) 0.015(5) 0.015(5) C9 0.175(12) 0.065(7) 0.064(7) 0.020(6) 0.047(7) 0.033(8) C10 0.104(9) 0.118(10) 0.105(10) -0.025(8) 0.047(7) -0.058(8) C11 0.092(9) 0.127(11) 0.086(9) -0.009(7) -0.031(7) 0.015(8) C12 0.113(9) 0.062(6) 0.073(7) 0.002(5) 0.044(6) -0.018(6) C13 0.052(7) 0.106(9) 0.139(11) -0.016(8) 0.007(7) 0.014(6) B3 0.046(6) 0.054(6) 0.050(7) -0.001(5) 0.019(5) -0.004(5) B4 0.058(7) 0.067(7) 0.038(6) -0.003(5) 0.002(5) -0.008(6) B5 0.062(7) 0.061(7) 0.076(9) 0.006(6) 0.026(6) -0.002(6) B6 0.055(7) 0.058(7) 0.100(10) 0.024(7) 0.030(7) 0.015(6) B7 0.071(8) 0.039(6) 0.062(7) 0.004(5) 0.016(6) 0.006(5) B8 0.055(7) 0.060(7) 0.060(8) -0.009(6) 0.009(6) -0.007(6) B9 0.091(9) 0.057(7) 0.058(8) 0.002(6) 0.034(7) 0.004(6) B10 0.044(7) 0.057(7) 0.120(11) -0.004(7) 0.019(7) 0.001(6) B11 0.061(7) 0.047(6) 0.077(9) 0.001(6) 0.002(6) 0.013(5) B12 0.087(9) 0.055(7) 0.074(9) -0.019(6) 0.028(7) -0.002(7) Ir2 0.0446(2) 0.03849(19) 0.0401(2) 0.00670(15) 0.01050(15) 0.00268(16) S3 0.0457(13) 0.0554(14) 0.0577(15) 0.0166(11) 0.0228(11) 0.0118(11) S4 0.0539(13) 0.0477(13) 0.0606(15) 0.0170(11) 0.0256(11) 0.0200(11) O2 0.066(5) 0.090(5) 0.054(4) -0.016(4) 0.003(3) -0.005(4) C14 0.047(5) 0.037(4) 0.044(5) 0.004(4) 0.019(4) 0.007(4) C15 0.039(5) 0.051(5) 0.037(5) 0.005(4) 0.014(4) 0.010(4) C16 0.070(8) 0.141(11) 0.086(9) -0.013(8) -0.018(6) -0.019(8) C17 0.038(5) 0.060(6) 0.068(7) 0.026(5) -0.007(5) -0.009(5) C18 0.128(10) 0.033(5) 0.035(6) 0.001(4) 0.012(6) 0.001(6) C19 0.063(6) 0.050(5) 0.044(6) 0.009(4) 0.020(5) 0.006(5) C20 0.056(6) 0.041(5) 0.045(5) 0.012(4) 0.005(4) -0.006(4) C21 0.055(6) 0.043(5) 0.050(6) 0.018(4) 0.016(5) 0.006(4) C22 0.091(9) 0.137(11) 0.148(12) 0.072(10) -0.051(8) -0.043(8) C23 0.282(19) 0.067(8) 0.057(8) -0.011(6) 0.033(10) -0.003(10) C24 0.093(9) 0.105(9) 0.146(12) 0.065(8) 0.060(8) 0.041(8) C25 0.093(8) 0.064(7) 0.083(8) 0.016(6) -0.012(6) -0.028(6) C26 0.115(9) 0.075(7) 0.107(9) 0.032(7) 0.059(7) 0.047(7) B13 0.050(6) 0.049(6) 0.055(7) -0.004(5) 0.014(5) 0.007(5) B14 0.056(7) 0.048(6) 0.059(7) 0.008(5) 0.018(5) 0.024(5) B15 0.051(6) 0.074(8) 0.043(7) 0.012(5) 0.012(5) 0.016(6) B16 0.047(6) 0.073(7) 0.033(6) -0.010(5) 0.002(5) 0.000(5) B17 0.042(6) 0.060(7) 0.065(8) 0.019(6) 0.014(5) -0.004(5) B18 0.069(8) 0.056(7) 0.082(9) 0.016(6) 0.027(7) 0.002(6) B19 0.082(9) 0.079(9) 0.078(9) 0.038(7) 0.029(7) 0.024(7) B20 0.058(7) 0.094(9) 0.050(7) 0.014(7) -0.005(6) 0.016(7) B21 0.064(7) 0.074(8) 0.045(7) 0.015(6) 0.032(6) 0.015(6) B22 0.076(8) 0.071(8) 0.072(9) 0.025(7) 0.043(7) 0.018(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C5 2.135(8) . ? Ir1 C7 2.149(8) . ? Ir1 C8 2.161(8) . ? Ir1 C4 2.173(8) . ? Ir1 C6 2.177(8) . ? Ir1 S2 2.254(4) . ? Ir1 S1 2.256(4) . ? S1 C1 1.771(8) . ? S2 C2 1.771(8) . ? O1 B3 1.348(10) . ? O1 C3 1.446(11) . ? C1 C2 1.631(10) . ? C1 B5 1.693(12) . ? C1 B4 1.702(12) . ? C1 B3 1.774(12) . ? C1 B6 1.779(13) . ? C2 B11 1.681(12) . ? C2 B7 1.699(12) . ? C2 B6 1.721(12) . ? C2 B3 1.804(12) . ? C4 C8 1.406(12) . ? C4 C5 1.408(12) . ? C4 C9 1.530(11) . ? C5 C6 1.432(11) . ? C5 C10 1.544(11) . ? C6 C7 1.410(11) . ? C6 C11 1.506(12) . ? C7 C8 1.421(11) . ? C7 C12 1.505(11) . ? C8 C13 1.534(12) . ? B3 B8 1.740(14) . ? B3 B7 1.756(14) . ? B3 B4 1.761(13) . ? B4 B9 1.761(14) . ? B4 B8 1.770(14) . ? B4 B5 1.785(14) . ? B5 B9 1.765(15) . ? B5 B10 1.770(15) . ? B5 B6 1.793(16) . ? B6 B11 1.779(15) . ? B6 B10 1.797(16) . ? B7 B8 1.748(14) . ? B7 B12 1.755(15) . ? B7 B11 1.773(15) . ? B8 B12 1.779(16) . ? B8 B9 1.780(15) . ? B9 B12 1.777(16) . ? B9 B10 1.778(16) . ? B10 B11 1.770(16) . ? B10 B12 1.775(15) . ? B11 B12 1.774(15) . ? Ir2 C17 2.133(8) . ? Ir2 C18 2.135(9) . ? Ir2 C20 2.156(8) . ? Ir2 C21 2.163(8) . ? Ir2 C19 2.172(8) . ? Ir2 S4 2.254(3) . ? Ir2 S3 2.260(3) . ? S3 C14 1.771(8) . ? S4 C15 1.780(8) . ? O2 B13 1.351(11) . ? O2 C16 1.450(10) . ? C14 C15 1.632(10) . ? C14 B15 1.715(12) . ? C14 B14 1.719(12) . ? C14 B16 1.738(12) . ? C14 B13 1.773(12) . ? C15 B21 1.673(12) . ? C15 B17 1.703(12) . ? C15 B16 1.725(12) . ? C15 B13 1.794(13) . ? C17 C21 1.388(12) . ? C17 C18 1.468(12) . ? C17 C22 1.506(12) . ? C18 C19 1.410(12) . ? C18 C23 1.496(12) . ? C19 C20 1.385(11) . ? C19 C24 1.518(12) . ? C20 C21 1.429(11) . ? C20 C25 1.509(11) . ? C21 C26 1.532(11) . ? B13 B18 1.760(15) . ? B13 B14 1.778(13) . ? B13 B17 1.790(14) . ? B14 B19 1.769(14) . ? B14 B15 1.782(15) . ? B14 B18 1.792(14) . ? B15 B20 1.759(14) . ? B15 B19 1.765(15) . ? B15 B16 1.782(14) . ? B16 B21 1.760(14) . ? B16 B20 1.770(15) . ? B17 B21 1.745(15) . ? B17 B22 1.749(15) . ? B17 B18 1.778(15) . ? B18 B22 1.748(16) . ? B18 B19 1.764(17) . ? B19 B20 1.764(17) . ? B19 B22 1.768(15) . ? B20 B22 1.763(16) . ? B20 B21 1.765(14) . ? B21 B22 1.745(15) . ? 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 Ir1 C7 64.1(3) . . ? C5 Ir1 C8 64.0(3) . . ? C7 Ir1 C8 38.5(3) . . ? C5 Ir1 C4 38.1(3) . . ? C7 Ir1 C4 63.8(3) . . ? C8 Ir1 C4 37.9(3) . . ? C5 Ir1 C6 38.8(3) . . ? C7 Ir1 C6 38.0(3) . . ? C8 Ir1 C6 64.2(3) . . ? C4 Ir1 C6 64.1(3) . . ? C5 Ir1 S2 134.6(3) . . ? C7 Ir1 S2 105.0(2) . . ? C8 Ir1 S2 135.1(3) . . ? C4 Ir1 S2 167.9(2) . . ? C6 Ir1 S2 104.5(2) . . ? C5 Ir1 S1 115.5(3) . . ? C7 Ir1 S1 155.1(3) . . ? C8 Ir1 S1 117.2(3) . . ? C4 Ir1 S1 99.9(2) . . ? C6 Ir1 S1 153.3(2) . . ? S2 Ir1 S1 92.18(8) . . ? C1 S1 Ir1 106.3(3) . . ? C2 S2 Ir1 107.1(3) . . ? B3 O1 C3 122.6(8) . . ? C2 C1 B5 109.3(7) . . ? C2 C1 B4 111.1(6) . . ? B5 C1 B4 63.4(6) . . ? C2 C1 S1 117.9(5) . . ? B5 C1 S1 121.5(6) . . ? B4 C1 S1 121.9(6) . . ? C2 C1 B3 63.8(5) . . ? B5 C1 B3 113.7(7) . . ? B4 C1 B3 60.8(5) . . ? S1 C1 B3 116.9(5) . . ? C2 C1 B6 60.4(5) . . ? B5 C1 B6 62.1(6) . . ? B4 C1 B6 115.3(7) . . ? S1 C1 B6 115.0(6) . . ? B3 C1 B6 116.1(7) . . ? C1 C2 B11 112.7(7) . . ? C1 C2 B7 109.8(6) . . ? B11 C2 B7 63.3(6) . . ? C1 C2 B6 64.1(5) . . ? B11 C2 B6 63.0(6) . . ? B7 C2 B6 115.8(7) . . ? C1 C2 S2 116.4(5) . . ? B11 C2 S2 122.2(6) . . ? B7 C2 S2 121.6(6) . . ? B6 C2 S2 115.5(6) . . ? C1 C2 B3 61.9(5) . . ? B11 C2 B3 113.9(7) . . ? B7 C2 B3 60.1(5) . . ? B6 C2 B3 117.6(7) . . ? S2 C2 B3 114.9(5) . . ? C8 C4 C5 108.0(7) . . ? C8 C4 C9 126.3(9) . . ? C5 C4 C9 125.6(9) . . ? C8 C4 Ir1 70.6(4) . . ? C5 C4 Ir1 69.5(5) . . ? C9 C4 Ir1 127.0(6) . . ? C4 C5 C6 108.8(8) . . ? C4 C5 C10 125.9(9) . . ? C6 C5 C10 125.2(9) . . ? C4 C5 Ir1 72.4(5) . . ? C6 C5 Ir1 72.2(5) . . ? C10 C5 Ir1 124.4(6) . . ? C7 C6 C5 106.3(8) . . ? C7 C6 C11 126.9(9) . . ? C5 C6 C11 126.8(9) . . ? C7 C6 Ir1 69.9(5) . . ? C5 C6 Ir1 69.0(5) . . ? C11 C6 Ir1 124.7(7) . . ? C6 C7 C8 109.1(7) . . ? C6 C7 C12 125.5(8) . . ? C8 C7 C12 125.2(8) . . ? C6 C7 Ir1 72.0(5) . . ? C8 C7 Ir1 71.2(5) . . ? C12 C7 Ir1 127.5(6) . . ? C4 C8 C7 107.7(8) . . ? C4 C8 C13 127.1(9) . . ? C7 C8 C13 125.2(9) . . ? C4 C8 Ir1 71.5(5) . . ? C7 C8 Ir1 70.3(5) . . ? C13 C8 Ir1 123.9(6) . . ? O1 B3 B8 132.0(9) . . ? O1 B3 B7 129.1(8) . . ? B8 B3 B7 60.0(6) . . ? O1 B3 B4 121.9(8) . . ? B8 B3 B4 60.7(6) . . ? B7 B3 B4 106.5(7) . . ? O1 B3 C1 116.8(8) . . ? B8 B3 C1 103.8(6) . . ? B7 B3 C1 101.0(7) . . ? B4 B3 C1 57.6(5) . . ? O1 B3 C2 121.1(8) . . ? B8 B3 C2 102.8(7) . . ? B7 B3 C2 57.0(5) . . ? B4 B3 C2 100.9(6) . . ? C1 B3 C2 54.2(4) . . ? C1 B4 B9 104.7(7) . . ? C1 B4 B3 61.6(5) . . ? B9 B4 B3 108.8(8) . . ? C1 B4 B8 105.6(7) . . ? B9 B4 B8 60.6(6) . . ? B3 B4 B8 59.1(6) . . ? C1 B4 B5 58.0(5) . . ? B9 B4 B5 59.7(6) . . ? B3 B4 B5 109.9(7) . . ? B8 B4 B5 108.0(8) . . ? C1 B5 B9 104.9(7) . . ? C1 B5 B10 106.4(8) . . ? B9 B5 B10 60.4(6) . . ? C1 B5 B4 58.5(5) . . ? B9 B5 B4 59.5(6) . . ? B10 B5 B4 108.3(8) . . ? C1 B5 B6 61.3(6) . . ? B9 B5 B6 109.9(8) . . ? B10 B5 B6 60.6(7) . . ? B4 B5 B6 110.6(7) . . ? C2 B6 B11 57.4(5) . . ? C2 B6 C1 55.5(5) . . ? B11 B6 C1 101.6(8) . . ? C2 B6 B5 101.0(8) . . ? B11 B6 B5 105.3(9) . . ? C1 B6 B5 56.6(5) . . ? C2 B6 B10 102.2(8) . . ? B11 B6 B10 59.3(6) . . ? C1 B6 B10 101.7(8) . . ? B5 B6 B10 59.1(7) . . ? C2 B7 B8 107.0(7) . . ? C2 B7 B12 105.0(7) . . ? B8 B7 B12 61.0(6) . . ? C2 B7 B3 62.9(5) . . ? B8 B7 B3 59.6(6) . . ? B12 B7 B3 110.0(8) . . ? C2 B7 B11 57.9(5) . . ? B8 B7 B11 109.8(8) . . ? B12 B7 B11 60.4(6) . . ? B3 B7 B11 111.8(7) . . ? B3 B8 B7 60.5(6) . . ? B3 B8 B4 60.2(6) . . ? B7 B8 B4 106.5(7) . . ? B3 B8 B12 109.6(8) . . ? B7 B8 B12 59.7(6) . . ? B4 B8 B12 107.4(8) . . ? B3 B8 B9 108.8(7) . . ? B7 B8 B9 106.7(8) . . ? B4 B8 B9 59.5(6) . . ? B12 B8 B9 59.9(6) . . ? B4 B9 B5 60.8(6) . . ? B4 B9 B12 107.9(8) . . ? B5 B9 B12 107.5(8) . . ? B4 B9 B10 109.1(8) . . ? B5 B9 B10 60.0(6) . . ? B12 B9 B10 59.9(6) . . ? B4 B9 B8 60.0(6) . . ? B5 B9 B8 108.5(8) . . ? B12 B9 B8 60.0(6) . . ? B10 B9 B8 108.6(8) . . ? B11 B10 B5 106.6(8) . . ? B11 B10 B12 60.0(6) . . ? B5 B10 B12 107.3(8) . . ? B11 B10 B9 107.5(8) . . ? B5 B10 B9 59.6(6) . . ? B12 B10 B9 60.0(6) . . ? B11 B10 B6 59.8(6) . . ? B5 B10 B6 60.3(6) . . ? B12 B10 B6 109.0(8) . . ? B9 B10 B6 109.1(8) . . ? C2 B11 B10 104.9(7) . . ? C2 B11 B7 58.9(5) . . ? B10 B11 B7 107.2(8) . . ? C2 B11 B12 105.0(7) . . ? B10 B11 B12 60.1(6) . . ? B7 B11 B12 59.3(6) . . ? C2 B11 B6 59.6(5) . . ? B10 B11 B6 60.8(6) . . ? B7 B11 B6 109.3(7) . . ? B12 B11 B6 109.9(9) . . ? B7 B12 B11 60.3(6) . . ? B7 B12 B10 107.8(8) . . ? B11 B12 B10 59.8(6) . . ? B7 B12 B9 106.6(8) . . ? B11 B12 B9 107.4(8) . . ? B10 B12 B9 60.1(6) . . ? B7 B12 B8 59.3(6) . . ? B11 B12 B8 108.4(7) . . ? B10 B12 B8 108.8(8) . . ? B9 B12 B8 60.1(6) . . ? C17 Ir2 C18 40.2(3) . . ? C17 Ir2 C20 64.4(3) . . ? C18 Ir2 C20 64.0(3) . . ? C17 Ir2 C21 37.7(3) . . ? C18 Ir2 C21 64.6(3) . . ? C20 Ir2 C21 38.6(3) . . ? C17 Ir2 C19 65.0(3) . . ? C18 Ir2 C19 38.2(3) . . ? C20 Ir2 C19 37.3(3) . . ? C21 Ir2 C19 63.6(3) . . ? C17 Ir2 S4 106.8(3) . . ? C18 Ir2 S4 142.9(3) . . ? C20 Ir2 S4 125.5(2) . . ? C21 Ir2 S4 100.1(2) . . ? C19 Ir2 S4 162.4(2) . . ? C17 Ir2 S3 149.0(3) . . ? C18 Ir2 S3 111.9(3) . . ? C20 Ir2 S3 122.9(2) . . ? C21 Ir2 S3 161.5(2) . . ? C19 Ir2 S3 101.9(2) . . ? S4 Ir2 S3 92.55(10) . . ? C14 S3 Ir2 106.0(3) . . ? C15 S4 Ir2 106.6(3) . . ? B13 O2 C16 121.5(7) . . ? C15 C14 B15 110.6(6) . . ? C15 C14 B14 111.5(6) . . ? B15 C14 B14 62.5(6) . . ? C15 C14 B16 61.5(5) . . ? B15 C14 B16 62.1(5) . . ? B14 C14 B16 114.4(7) . . ? C15 C14 S3 118.1(5) . . ? B15 C14 S3 121.5(6) . . ? B14 C14 S3 120.5(5) . . ? B16 C14 S3 116.9(6) . . ? C15 C14 B13 63.4(5) . . ? B15 C14 B13 113.4(6) . . ? B14 C14 B13 61.2(5) . . ? B16 C14 B13 116.0(6) . . ? S3 C14 B13 116.2(6) . . ? C14 C15 B21 111.1(6) . . ? C14 C15 B17 111.1(6) . . ? B21 C15 B17 62.2(6) . . ? C14 C15 B16 62.3(5) . . ? B21 C15 B16 62.4(5) . . ? B17 C15 B16 114.5(7) . . ? C14 C15 S4 116.5(5) . . ? B21 C15 S4 123.1(6) . . ? B17 C15 S4 121.5(6) . . ? B16 C15 S4 116.5(6) . . ? C14 C15 B13 62.1(5) . . ? B21 C15 B13 113.1(7) . . ? B17 C15 B13 61.5(5) . . ? B16 C15 B13 115.6(6) . . ? S4 C15 B13 115.6(6) . . ? C21 C17 C18 107.1(8) . . ? C21 C17 C22 126.3(10) . . ? C18 C17 C22 126.5(10) . . ? C21 C17 Ir2 72.3(5) . . ? C18 C17 Ir2 70.0(5) . . ? C22 C17 Ir2 126.1(6) . . ? C19 C18 C17 106.9(8) . . ? C19 C18 C23 127.1(11) . . ? C17 C18 C23 125.9(11) . . ? C19 C18 Ir2 72.3(5) . . ? C17 C18 Ir2 69.8(5) . . ? C23 C18 Ir2 125.8(7) . . ? C20 C19 C18 108.8(8) . . ? C20 C19 C24 126.8(10) . . ? C18 C19 C24 124.4(9) . . ? C20 C19 Ir2 70.7(5) . . ? C18 C19 Ir2 69.5(5) . . ? C24 C19 Ir2 126.7(6) . . ? C19 C20 C21 108.7(8) . . ? C19 C20 C25 125.6(9) . . ? C21 C20 C25 125.7(8) . . ? C19 C20 Ir2 71.9(5) . . ? C21 C20 Ir2 71.0(4) . . ? C25 C20 Ir2 123.8(6) . . ? C17 C21 C20 108.5(8) . . ? C17 C21 C26 125.9(9) . . ? C20 C21 C26 125.7(9) . . ? C17 C21 Ir2 70.0(5) . . ? C20 C21 Ir2 70.4(4) . . ? C26 C21 Ir2 126.2(6) . . ? O2 B13 B18 132.3(9) . . ? O2 B13 C14 117.6(8) . . ? B18 B13 C14 103.6(7) . . ? O2 B13 B14 122.8(8) . . ? B18 B13 B14 60.9(6) . . ? C14 B13 B14 57.9(5) . . ? O2 B13 B17 127.3(8) . . ? B18 B13 B17 60.1(6) . . ? C14 B13 B17 101.1(7) . . ? B14 B13 B17 107.4(7) . . ? O2 B13 C15 120.2(7) . . ? B18 B13 C15 102.6(7) . . ? C14 B13 C15 54.5(5) . . ? B14 B13 C15 101.7(7) . . ? B17 B13 C15 56.8(5) . . ? C14 B14 B19 104.3(7) . . ? C14 B14 B13 60.9(5) . . ? B19 B14 B13 107.9(7) . . ? C14 B14 B15 58.6(5) . . ? B19 B14 B15 59.6(6) . . ? B13 B14 B15 109.9(7) . . ? C14 B14 B18 104.4(7) . . ? B19 B14 B18 59.4(6) . . ? B13 B14 B18 59.1(6) . . ? B15 B14 B18 107.1(8) . . ? C14 B15 B20 104.9(7) . . ? C14 B15 B19 104.6(7) . . ? B20 B15 B19 60.1(6) . . ? C14 B15 B14 58.9(5) . . ? B20 B15 B14 108.2(8) . . ? B19 B15 B14 59.8(6) . . ? C14 B15 B16 59.6(5) . . ? B20 B15 B16 60.0(6) . . ? B19 B15 B16 108.5(7) . . ? B14 B15 B16 109.3(7) . . ? C15 B16 C14 56.2(4) . . ? C15 B16 B21 57.4(5) . . ? C14 B16 B21 102.3(7) . . ? C15 B16 B20 103.6(7) . . ? C14 B16 B20 103.5(8) . . ? B21 B16 B20 60.0(6) . . ? C15 B16 B15 103.4(7) . . ? C14 B16 B15 58.3(5) . . ? B21 B16 B15 106.5(8) . . ? B20 B16 B15 59.4(6) . . ? C15 B17 B21 58.0(5) . . ? C15 B17 B22 104.5(7) . . ? B21 B17 B22 59.9(6) . . ? C15 B17 B18 105.6(7) . . ? B21 B17 B18 107.6(8) . . ? B22 B17 B18 59.4(6) . . ? C15 B17 B13 61.7(5) . . ? B21 B17 B13 109.9(7) . . ? B22 B17 B13 107.8(7) . . ? B18 B17 B13 59.1(6) . . ? B22 B18 B13 109.2(8) . . ? B22 B18 B19 60.4(7) . . ? B13 B18 B19 109.0(8) . . ? B22 B18 B17 59.5(6) . . ? B13 B18 B17 60.8(6) . . ? B19 B18 B17 107.7(9) . . ? B22 B18 B14 107.7(8) . . ? B13 B18 B14 60.1(5) . . ? B19 B18 B14 59.7(6) . . ? B17 B18 B14 107.3(7) . . ? B20 B19 B18 108.2(8) . . ? B20 B19 B15 59.8(7) . . ? B18 B19 B15 109.1(8) . . ? B20 B19 B22 59.9(7) . . ? B18 B19 B22 59.3(7) . . ? B15 B19 B22 107.4(8) . . ? B20 B19 B14 108.5(8) . . ? B18 B19 B14 61.0(6) . . ? B15 B19 B14 60.5(6) . . ? B22 B19 B14 107.8(8) . . ? B15 B20 B22 108.0(8) . . ? B15 B20 B19 60.2(6) . . ? B22 B20 B19 60.2(7) . . ? B15 B20 B21 107.3(7) . . ? B22 B20 B21 59.3(6) . . ? B19 B20 B21 107.4(8) . . ? B15 B20 B16 60.7(6) . . ? B22 B20 B16 108.2(7) . . ? B19 B20 B16 109.2(8) . . ? B21 B20 B16 59.7(6) . . ? C15 B21 B17 59.7(5) . . ? C15 B21 B22 105.9(8) . . ? B17 B21 B22 60.1(6) . . ? C15 B21 B16 60.3(5) . . ? B17 B21 B16 110.7(7) . . ? B22 B21 B16 109.4(8) . . ? C15 B21 B20 106.1(7) . . ? B17 B21 B20 109.0(8) . . ? B22 B21 B20 60.3(7) . . ? B16 B21 B20 60.3(6) . . ? B21 B22 B18 109.0(8) . . ? B21 B22 B17 59.9(6) . . ? B18 B22 B17 61.1(6) . . ? B21 B22 B20 60.4(6) . . ? B18 B22 B20 109.0(8) . . ? B17 B22 B20 109.0(8) . . ? B21 B22 B19 108.1(8) . . ? B18 B22 B19 60.2(6) . . ? B17 B22 B19 108.9(8) . . ? B20 B22 B19 59.9(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.131 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.128 # Attachment '2a.cif' data_f71017c _database_code_depnum_ccdc_archive 'CCDC 673416' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 B9 Cl2 Rh Ru S2' _chemical_formula_weight 727.81 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ru Ru -1.2594 0.8363 '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 11.072(4) _cell_length_b 15.593(6) _cell_length_c 18.035(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.234(5) _cell_angle_gamma 90.00 _cell_volume 3113(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 937 _cell_measurement_theta_min 2.541 _cell_measurement_theta_max 23.961 _exptl_crystal_description prism _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 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 1.333 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8251 _exptl_absorpt_correction_T_max 0.8782 _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_% 7.06 _diffrn_reflns_number 15414 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.15 _reflns_number_total 6837 _reflns_number_gt 5162 _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^)+(0.0678P)^2^+6.7288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6837 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0707 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1422 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.85041(4) 0.17751(3) 0.23239(2) 0.03529(13) Uani 1 1 d . . . Ru1 Ru 0.87600(4) 0.29585(3) 0.12079(2) 0.04003(14) Uani 1 1 d . . . S1 S 1.01627(12) 0.18593(9) 0.15649(8) 0.0406(3) Uani 1 1 d . . . S2 S 0.89228(12) 0.32201(9) 0.25080(7) 0.0378(3) Uani 1 1 d . . . B1 B 1.2261(6) 0.4166(5) 0.1649(4) 0.0462(15) Uani 1 1 d . . . H1 H 1.2558 0.4657 0.1255 0.055 Uiso 1 1 calc R . . B2 B 1.2246(6) 0.3077(4) 0.1407(4) 0.0452(15) Uani 1 1 d . . . H2 H 1.2498 0.2862 0.0851 0.054 Uiso 1 1 calc R . . B3 B 1.0902(6) 0.3622(4) 0.1559(4) 0.0414(14) Uani 1 1 d . . . H3 H 1.012(4) 0.376(3) 0.101(2) 0.021(11) Uiso 1 1 d . . . B4 B 1.1084(6) 0.4356(4) 0.2274(4) 0.0444(15) Uani 1 1 d . . . H4 H 1.0586 0.4966 0.2273 0.053 Uiso 1 1 calc R . . H9 H 1.099(5) 0.390(4) 0.361(3) 0.048(16) Uiso 1 1 d . . . B5 B 1.2553(6) 0.4251(5) 0.2627(4) 0.0498(16) Uani 1 1 d . . . H5 H 1.3018 0.4812 0.2868 0.060 Uiso 1 1 calc R . . B6 B 1.3298(6) 0.3432(5) 0.2089(4) 0.0484(16) Uani 1 1 d . . . H6 H 1.4268 0.3439 0.1970 0.058 Uiso 1 1 calc R . . B9 B 1.1374(6) 0.3733(5) 0.3102(4) 0.0441(14) Uani 1 1 d . . . B10 B 1.2863(7) 0.3219(5) 0.3008(4) 0.0503(16) Uani 1 1 d . . . H10 H 1.353(6) 0.310(4) 0.347(3) 0.048(16) Uiso 1 1 d . . . H10' H 1.228(7) 0.261(5) 0.308(4) 0.09(2) Uiso 1 1 d . . . B11 B 1.2535(6) 0.2445(4) 0.2252(4) 0.0456(15) Uani 1 1 d . . . H11 H 1.296(6) 0.174(4) 0.222(3) 0.055(18) Uiso 1 1 d . . . C1 C 0.6837(5) 0.1363(4) 0.2838(3) 0.0455(13) Uani 1 1 d . . . C2 C 0.7137(5) 0.0764(4) 0.2258(3) 0.0451(13) Uani 1 1 d . . . C3 C 0.8264(5) 0.0400(4) 0.2432(3) 0.0423(12) Uani 1 1 d . . . C4 C 0.8700(5) 0.0768(4) 0.3116(3) 0.0446(13) Uani 1 1 d . . . C5 C 0.7798(5) 0.1341(4) 0.3367(3) 0.0460(13) Uani 1 1 d . . . C6 C 0.5683(6) 0.1864(5) 0.2885(5) 0.078(2) Uani 1 1 d . . . H6A H 0.5090 0.1528 0.3134 0.116 Uiso 1 1 calc R . . H6B H 0.5392 0.2001 0.2394 0.116 Uiso 1 1 calc R . . H6C H 0.5830 0.2385 0.3157 0.116 Uiso 1 1 calc R . . C7 C 1.1173(4) 0.2641(3) 0.1975(3) 0.0359(11) Uani 1 1 d . . . C8 C 1.0535(5) 0.3347(3) 0.2456(3) 0.0358(11) Uani 1 1 d . . . C9 C 0.6368(7) 0.0546(5) 0.1577(4) 0.0677(19) Uani 1 1 d . . . H9A H 0.6858 0.0564 0.1145 0.102 Uiso 1 1 calc R . . H9B H 0.5724 0.0955 0.1525 0.102 Uiso 1 1 calc R . . H9C H 0.6035 -0.0018 0.1630 0.102 Uiso 1 1 calc R . . C10 C 0.8890(6) -0.0283(4) 0.1990(4) 0.0570(16) Uani 1 1 d . . . H10A H 0.8780 -0.0831 0.2222 0.085 Uiso 1 1 calc R . . H10B H 0.9737 -0.0156 0.1971 0.085 Uiso 1 1 calc R . . H10C H 0.8552 -0.0297 0.1495 0.085 Uiso 1 1 calc R . . C11 C 0.9834(6) 0.0529(5) 0.3526(4) 0.0673(19) Uani 1 1 d . . . H11A H 1.0096 0.1001 0.3831 0.101 Uiso 1 1 calc R . . H11B H 1.0450 0.0393 0.3178 0.101 Uiso 1 1 calc R . . H11C H 0.9686 0.0039 0.3833 0.101 Uiso 1 1 calc R . . C12 C 0.7849(9) 0.1833(5) 0.4084(4) 0.081(2) Uani 1 1 d . . . H12A H 0.7408 0.2360 0.4026 0.121 Uiso 1 1 calc R . . H12B H 0.8676 0.1958 0.4215 0.121 Uiso 1 1 calc R . . H12C H 0.7497 0.1496 0.4468 0.121 Uiso 1 1 calc R . . C13 C 0.9010(8) 0.2923(5) -0.0002(4) 0.0667(19) Uani 1 1 d . . . H13 H 0.9768 0.2654 -0.0150 0.080 Uiso 1 1 calc R . . C14 C 0.8107(7) 0.2342(6) 0.0167(3) 0.068(2) Uani 1 1 d . . . H14 H 0.8346 0.1740 0.0118 0.081 Uiso 1 1 calc R . . C15 C 0.6781(8) 0.2500(7) 0.0033(4) 0.092(3) Uani 1 1 d . . . H15A H 0.6673 0.2729 -0.0464 0.110 Uiso 1 1 calc R . . H15B H 0.6370 0.1951 0.0045 0.110 Uiso 1 1 calc R . . C16 C 0.6161(8) 0.3090(6) 0.0556(5) 0.091(3) Uani 1 1 d . . . H16A H 0.5595 0.2757 0.0841 0.110 Uiso 1 1 calc R . . H16B H 0.5697 0.3504 0.0267 0.110 Uiso 1 1 calc R . . C17 C 0.6989(6) 0.3577(5) 0.1095(4) 0.0593(18) Uani 1 1 d . . . H17 H 0.6617 0.3712 0.1569 0.071 Uiso 1 1 calc R . . C18 C 0.7854(7) 0.4151(5) 0.0889(4) 0.0608(18) Uani 1 1 d . . . H18 H 0.7983 0.4617 0.1246 0.073 Uiso 1 1 calc R . . C19 C 0.8093(11) 0.4404(7) 0.0110(5) 0.106(4) Uani 1 1 d . . . H19A H 0.8529 0.4943 0.0119 0.128 Uiso 1 1 calc R . . H19B H 0.7323 0.4505 -0.0141 0.128 Uiso 1 1 calc R . . C20 C 0.8791(11) 0.3777(6) -0.0339(4) 0.098(3) Uani 1 1 d . . . H20A H 0.8363 0.3694 -0.0808 0.117 Uiso 1 1 calc R . . H20B H 0.9567 0.4031 -0.0446 0.117 Uiso 1 1 calc R . . C21 C 0.7228(11) 0.9333(7) 0.9393(5) 0.109(3) Uani 1 1 d . . . H21A H 0.6893 0.9787 0.9085 0.130 Uiso 1 1 calc R . . H21B H 0.7471 0.8872 0.9067 0.130 Uiso 1 1 calc R . . Cl1 Cl 0.6137(4) 0.8965(3) 0.9940(2) 0.1416(12) Uani 1 1 d . . . Cl2 Cl 0.8475(4) 0.9714(4) 0.9846(3) 0.230(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0283(2) 0.0366(2) 0.0411(2) 0.00083(17) 0.00115(16) -0.00064(16) Ru1 0.0405(3) 0.0429(3) 0.0368(2) 0.00048(18) 0.00187(18) 0.00442(19) S1 0.0350(7) 0.0382(7) 0.0487(7) -0.0053(6) 0.0059(6) 0.0016(5) S2 0.0307(6) 0.0396(7) 0.0434(7) -0.0029(5) 0.0035(5) 0.0019(5) B1 0.037(3) 0.048(4) 0.054(4) 0.006(3) 0.004(3) -0.006(3) B2 0.037(3) 0.053(4) 0.046(3) 0.005(3) 0.008(3) -0.006(3) B3 0.034(3) 0.045(4) 0.046(3) 0.009(3) 0.003(3) 0.005(3) B4 0.045(4) 0.035(3) 0.054(4) 0.007(3) 0.006(3) 0.000(3) B5 0.043(4) 0.050(4) 0.056(4) -0.001(3) -0.001(3) -0.008(3) B6 0.029(3) 0.056(4) 0.061(4) 0.009(3) 0.001(3) -0.004(3) B9 0.033(3) 0.055(4) 0.043(3) -0.003(3) -0.002(3) -0.002(3) B10 0.041(4) 0.062(5) 0.047(4) 0.002(3) -0.005(3) -0.001(3) B11 0.033(3) 0.047(4) 0.057(4) 0.007(3) 0.005(3) 0.005(3) C1 0.038(3) 0.043(3) 0.056(3) 0.010(3) 0.009(3) 0.000(2) C2 0.039(3) 0.047(3) 0.049(3) 0.007(3) 0.002(2) -0.008(2) C3 0.036(3) 0.039(3) 0.053(3) 0.004(2) 0.003(2) -0.004(2) C4 0.038(3) 0.044(3) 0.051(3) 0.005(2) -0.005(2) -0.002(2) C5 0.050(3) 0.044(3) 0.045(3) 0.003(2) 0.005(3) -0.006(3) C6 0.038(4) 0.073(5) 0.123(7) 0.014(5) 0.030(4) 0.012(3) C7 0.027(3) 0.040(3) 0.041(3) -0.002(2) 0.005(2) 0.000(2) C8 0.033(3) 0.034(3) 0.040(3) -0.002(2) 0.000(2) 0.001(2) C9 0.060(4) 0.077(5) 0.066(4) 0.012(4) -0.012(3) -0.019(4) C10 0.058(4) 0.047(4) 0.066(4) -0.003(3) 0.002(3) 0.001(3) C11 0.054(4) 0.066(4) 0.080(5) 0.012(4) -0.032(4) -0.002(3) C12 0.110(7) 0.082(6) 0.050(4) -0.009(4) 0.014(4) -0.007(5) C13 0.071(5) 0.083(5) 0.046(4) -0.002(3) 0.006(3) 0.003(4) C14 0.074(5) 0.089(5) 0.041(3) -0.022(3) -0.010(3) 0.016(4) C15 0.075(6) 0.143(9) 0.056(4) -0.020(5) -0.009(4) -0.005(6) C16 0.071(6) 0.110(7) 0.092(6) -0.019(5) -0.027(5) 0.021(5) C17 0.050(4) 0.079(5) 0.049(3) -0.010(3) -0.014(3) 0.027(3) C18 0.070(5) 0.055(4) 0.057(4) 0.010(3) 0.007(3) 0.024(3) C19 0.134(9) 0.102(7) 0.084(6) 0.041(5) 0.027(6) 0.032(7) C20 0.151(10) 0.090(6) 0.052(4) 0.018(4) 0.014(5) 0.001(6) C21 0.155(11) 0.099(7) 0.071(6) 0.003(5) -0.008(6) 0.013(7) Cl1 0.137(3) 0.154(3) 0.134(3) -0.012(2) 0.010(2) -0.011(2) Cl2 0.157(4) 0.367(8) 0.169(4) -0.160(5) 0.042(3) -0.071(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C4 2.130(6) . ? Rh1 C5 2.161(5) . ? Rh1 C3 2.170(6) . ? Rh1 C1 2.180(5) . ? Rh1 C2 2.188(6) . ? Rh1 S1 2.3179(15) . ? Rh1 S2 2.3228(16) . ? Rh1 Ru1 2.7498(9) . ? Ru1 C18 2.184(6) . ? Ru1 C17 2.191(6) . ? Ru1 C13 2.206(7) . ? Ru1 C14 2.217(6) . ? Ru1 S2 2.3831(16) . ? Ru1 S1 2.3920(16) . ? Ru1 B3 2.652(7) . ? S1 C7 1.802(5) . ? S2 C8 1.801(5) . ? B1 B3 1.732(9) . ? B1 B2 1.753(10) . ? B1 B4 1.766(9) . ? B1 B5 1.791(10) . ? B1 B6 1.793(10) . ? B2 C7 1.726(8) . ? B2 B3 1.741(9) . ? B2 B6 1.764(10) . ? B2 B11 1.836(10) . ? B3 C7 1.728(8) . ? B3 C8 1.731(8) . ? B3 B4 1.732(10) . ? B4 C8 1.721(8) . ? B4 B5 1.741(10) . ? B4 B9 1.804(9) . ? B5 B9 1.770(10) . ? B5 B10 1.781(11) . ? B5 B6 1.812(11) . ? B6 B10 1.768(10) . ? B6 B11 1.783(10) . ? B9 C8 1.591(8) . ? B9 B10 1.845(10) . ? B10 B11 1.850(11) . ? B11 C7 1.609(8) . ? C1 C5 1.414(8) . ? C1 C2 1.447(8) . ? C1 C6 1.501(8) . ? C2 C3 1.401(8) . ? C2 C9 1.518(9) . ? C3 C4 1.434(8) . ? C3 C10 1.508(8) . ? C4 C5 1.422(8) . ? C4 C11 1.490(8) . ? C5 C12 1.504(9) . ? C7 C8 1.578(7) . ? C13 C14 1.388(11) . ? C13 C20 1.481(11) . ? C14 C15 1.503(11) . ? C15 C16 1.494(12) . ? C16 C17 1.524(11) . ? C17 C18 1.369(10) . ? C18 C19 1.487(10) . ? C19 C20 1.496(13) . ? C21 Cl1 1.676(11) . ? C21 Cl2 1.697(12) . ? 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 C5 38.7(2) . . ? C4 Rh1 C3 38.9(2) . . ? C5 Rh1 C3 64.2(2) . . ? C4 Rh1 C1 64.7(2) . . ? C5 Rh1 C1 38.0(2) . . ? C3 Rh1 C1 64.2(2) . . ? C4 Rh1 C2 64.2(2) . . ? C5 Rh1 C2 63.8(2) . . ? C3 Rh1 C2 37.5(2) . . ? C1 Rh1 C2 38.7(2) . . ? C4 Rh1 S1 111.52(16) . . ? C5 Rh1 S1 146.92(17) . . ? C3 Rh1 S1 102.07(15) . . ? C1 Rh1 S1 163.09(17) . . ? C2 Rh1 S1 124.40(16) . . ? C4 Rh1 S2 127.01(16) . . ? C5 Rh1 S2 104.73(16) . . ? C3 Rh1 S2 165.95(16) . . ? C1 Rh1 S2 113.15(16) . . ? C2 Rh1 S2 147.45(16) . . ? S1 Rh1 S2 82.60(5) . . ? C4 Rh1 Ru1 167.06(16) . . ? C5 Rh1 Ru1 153.14(16) . . ? C3 Rh1 Ru1 138.05(15) . . ? C1 Rh1 Ru1 127.62(15) . . ? C2 Rh1 Ru1 121.76(15) . . ? S1 Rh1 Ru1 55.54(4) . . ? S2 Rh1 Ru1 55.27(4) . . ? C18 Ru1 C17 36.5(3) . . ? C18 Ru1 C13 80.1(3) . . ? C17 Ru1 C13 92.9(3) . . ? C18 Ru1 C14 90.4(3) . . ? C17 Ru1 C14 80.6(3) . . ? C13 Ru1 C14 36.6(3) . . ? C18 Ru1 S2 97.94(19) . . ? C17 Ru1 S2 93.71(17) . . ? C13 Ru1 S2 165.7(2) . . ? C14 Ru1 S2 157.5(2) . . ? C18 Ru1 S1 166.6(2) . . ? C17 Ru1 S1 156.2(2) . . ? C13 Ru1 S1 98.8(2) . . ? C14 Ru1 S1 96.6(2) . . ? S2 Ru1 S1 79.80(5) . . ? C18 Ru1 B3 97.7(3) . . ? C17 Ru1 B3 130.1(3) . . ? C13 Ru1 B3 96.6(3) . . ? C14 Ru1 B3 130.2(3) . . ? S2 Ru1 B3 69.50(14) . . ? S1 Ru1 B3 69.09(14) . . ? C18 Ru1 Rh1 135.26(18) . . ? C17 Ru1 Rh1 104.9(2) . . ? C13 Ru1 Rh1 136.4(2) . . ? C14 Ru1 Rh1 107.0(2) . . ? S2 Ru1 Rh1 53.23(4) . . ? S1 Ru1 Rh1 53.03(4) . . ? B3 Ru1 Rh1 101.11(13) . . ? C7 S1 Rh1 106.75(17) . . ? C7 S1 Ru1 91.12(18) . . ? Rh1 S1 Ru1 71.42(4) . . ? C8 S2 Rh1 107.12(17) . . ? C8 S2 Ru1 91.26(17) . . ? Rh1 S2 Ru1 71.50(4) . . ? B3 B1 B2 59.9(4) . . ? B3 B1 B4 59.4(4) . . ? B2 B1 B4 108.6(5) . . ? B3 B1 B5 105.5(5) . . ? B2 B1 B5 108.5(5) . . ? B4 B1 B5 58.6(4) . . ? B3 B1 B6 106.0(5) . . ? B2 B1 B6 59.7(4) . . ? B4 B1 B6 107.4(5) . . ? B5 B1 B6 60.8(4) . . ? C7 B2 B3 59.8(3) . . ? C7 B2 B1 103.7(4) . . ? B3 B2 B1 59.4(4) . . ? C7 B2 B6 99.4(4) . . ? B3 B2 B6 106.9(5) . . ? B1 B2 B6 61.3(4) . . ? C7 B2 B11 53.6(3) . . ? B3 B2 B11 105.4(4) . . ? B1 B2 B11 108.2(5) . . ? B6 B2 B11 59.3(4) . . ? C7 B3 C8 54.3(3) . . ? C7 B3 B1 104.5(4) . . ? C8 B3 B1 104.7(5) . . ? C7 B3 B4 104.2(4) . . ? C8 B3 B4 59.6(3) . . ? B1 B3 B4 61.3(4) . . ? C7 B3 B2 59.7(3) . . ? C8 B3 B2 104.2(4) . . ? B1 B3 B2 60.6(4) . . ? B4 B3 B2 110.7(5) . . ? C7 B3 Ru1 84.5(3) . . ? C8 B3 Ru1 84.3(3) . . ? B1 B3 Ru1 169.8(4) . . ? B4 B3 Ru1 121.7(4) . . ? B2 B3 Ru1 122.4(4) . . ? C8 B4 B3 60.2(3) . . ? C8 B4 B5 100.1(4) . . ? B3 B4 B5 107.6(5) . . ? C8 B4 B1 103.7(4) . . ? B3 B4 B1 59.3(4) . . ? B5 B4 B1 61.4(4) . . ? C8 B4 B9 53.6(3) . . ? B3 B4 B9 106.0(5) . . ? B5 B4 B9 59.9(4) . . ? B1 B4 B9 108.5(5) . . ? B4 B5 B9 61.8(4) . . ? B4 B5 B10 113.4(5) . . ? B9 B5 B10 62.6(4) . . ? B4 B5 B1 60.0(4) . . ? B9 B5 B1 108.9(5) . . ? B10 B5 B1 110.0(5) . . ? B4 B5 B6 107.6(5) . . ? B9 B5 B6 106.7(5) . . ? B10 B5 B6 58.9(4) . . ? B1 B5 B6 59.7(4) . . ? B2 B6 B10 113.9(5) . . ? B2 B6 B11 62.4(4) . . ? B10 B6 B11 62.8(4) . . ? B2 B6 B1 59.1(4) . . ? B10 B6 B1 110.5(5) . . ? B11 B6 B1 108.8(5) . . ? B2 B6 B5 107.1(5) . . ? B10 B6 B5 59.6(4) . . ? B11 B6 B5 107.3(5) . . ? B1 B6 B5 59.6(4) . . ? C8 B9 B5 104.1(5) . . ? C8 B9 B4 60.5(4) . . ? B5 B9 B4 58.3(4) . . ? C8 B9 B10 106.1(5) . . ? B5 B9 B10 59.0(4) . . ? B4 B9 B10 107.6(5) . . ? B6 B10 B5 61.4(4) . . ? B6 B10 B9 105.4(5) . . ? B5 B10 B9 58.4(4) . . ? B6 B10 B11 59.0(4) . . ? B5 B10 B11 105.8(5) . . ? B9 B10 B11 100.9(5) . . ? C7 B11 B6 103.3(5) . . ? C7 B11 B2 59.7(4) . . ? B6 B11 B2 58.3(4) . . ? C7 B11 B10 105.8(5) . . ? B6 B11 B10 58.2(4) . . ? B2 B11 B10 106.8(5) . . ? C5 C1 C2 106.9(5) . . ? C5 C1 C6 127.1(6) . . ? C2 C1 C6 125.9(6) . . ? C5 C1 Rh1 70.3(3) . . ? C2 C1 Rh1 71.0(3) . . ? C6 C1 Rh1 126.9(4) . . ? C3 C2 C1 108.5(5) . . ? C3 C2 C9 124.9(6) . . ? C1 C2 C9 126.6(6) . . ? C3 C2 Rh1 70.6(3) . . ? C1 C2 Rh1 70.4(3) . . ? C9 C2 Rh1 125.5(4) . . ? C2 C3 C4 108.2(5) . . ? C2 C3 C10 125.8(6) . . ? C4 C3 C10 126.0(5) . . ? C2 C3 Rh1 71.9(3) . . ? C4 C3 Rh1 69.0(3) . . ? C10 C3 Rh1 126.3(4) . . ? C5 C4 C3 107.4(5) . . ? C5 C4 C11 126.1(6) . . ? C3 C4 C11 126.2(6) . . ? C5 C4 Rh1 71.8(3) . . ? C3 C4 Rh1 72.0(3) . . ? C11 C4 Rh1 126.1(4) . . ? C1 C5 C4 108.9(5) . . ? C1 C5 C12 125.6(6) . . ? C4 C5 C12 125.5(6) . . ? C1 C5 Rh1 71.7(3) . . ? C4 C5 Rh1 69.5(3) . . ? C12 C5 Rh1 125.5(5) . . ? C8 C7 B11 112.9(4) . . ? C8 C7 B2 111.9(4) . . ? B11 C7 B2 66.7(4) . . ? C8 C7 B3 62.9(3) . . ? B11 C7 B3 117.1(4) . . ? B2 C7 B3 60.6(4) . . ? C8 C7 S1 114.7(3) . . ? B11 C7 S1 124.7(4) . . ? B2 C7 S1 116.9(4) . . ? B3 C7 S1 108.7(4) . . ? C7 C8 B9 113.9(4) . . ? C7 C8 B4 111.7(4) . . ? B9 C8 B4 65.9(4) . . ? C7 C8 B3 62.8(3) . . ? B9 C8 B3 116.4(5) . . ? B4 C8 B3 60.3(4) . . ? C7 C8 S2 114.0(3) . . ? B9 C8 S2 124.6(4) . . ? B4 C8 S2 117.7(4) . . ? B3 C8 S2 109.2(3) . . ? C14 C13 C20 124.3(8) . . ? C14 C13 Ru1 72.1(4) . . ? C20 C13 Ru1 111.1(5) . . ? C13 C14 C15 124.3(8) . . ? C13 C14 Ru1 71.3(4) . . ? C15 C14 Ru1 111.3(5) . . ? C16 C15 C14 117.4(7) . . ? C15 C16 C17 115.5(7) . . ? C18 C17 C16 124.6(7) . . ? C18 C17 Ru1 71.5(4) . . ? C16 C17 Ru1 111.4(5) . . ? C17 C18 C19 124.7(8) . . ? C17 C18 Ru1 72.0(4) . . ? C19 C18 Ru1 112.6(5) . . ? C18 C19 C20 116.3(7) . . ? C13 C20 C19 116.6(7) . . ? Cl1 C21 Cl2 115.2(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.15 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.170 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.116 # Attachment '3a.cif' data_f71010c _database_code_depnum_ccdc_archive 'CCDC 673417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H39 B9 Cl2 Co Ru S2' _chemical_formula_weight 683.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 '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' Ru Ru -1.2594 0.8363 '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 10.965(5) _cell_length_b 15.267(7) _cell_length_c 18.019(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(7) _cell_angle_gamma 90.00 _cell_volume 3016(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1010 _cell_measurement_theta_min 2.287 _cell_measurement_theta_max 23.457 _exptl_crystal_description prism _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 1.378 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7701 _exptl_absorpt_correction_T_max 0.8745 _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_% 7.32 _diffrn_reflns_number 14731 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.25 _reflns_number_total 6596 _reflns_number_gt 4632 _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^)+(0.0781P)^2^+1.4949P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6596 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1394 _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 Ru1 Ru 0.87211(4) 0.70394(3) 0.12376(2) 0.03578(14) Uani 1 1 d . . . Co1 Co 0.84956(6) 0.81884(4) 0.23115(3) 0.03382(17) Uani 1 1 d . . . S1 S 0.88233(11) 0.68001(8) 0.25327(7) 0.0353(3) Uani 1 1 d . . . S2 S 1.01090(11) 0.81572(7) 0.15988(7) 0.0375(3) Uani 1 1 d . . . B1 B 1.2209(5) 0.5795(4) 0.1679(3) 0.0429(13) Uani 1 1 d . . . H1 H 1.2512 0.5286 0.1288 0.051 Uiso 1 1 calc R . . B2 B 1.0993(5) 0.5612(4) 0.2310(3) 0.0399(13) Uani 1 1 d . . . H2 H 1.0481 0.4993 0.2315 0.048 Uiso 1 1 calc R . . B3 B 1.0838(5) 0.6371(4) 0.1585(3) 0.0389(12) Uani 1 1 d . . . H3 H 1.014(5) 0.627(3) 0.121(3) 0.041(13) Uiso 1 1 d . . . B4 B 1.2213(6) 0.6924(4) 0.1431(4) 0.0432(13) Uani 1 1 d . . . H4 H 1.2486 0.7147 0.0875 0.052 Uiso 1 1 calc R . . B5 B 1.3246(5) 0.6546(4) 0.2107(3) 0.0443(14) Uani 1 1 d . . . H5 H 1.4228 0.6533 0.1983 0.053 Uiso 1 1 calc R . . B6 B 1.2479(5) 0.5709(4) 0.2653(3) 0.0447(14) Uani 1 1 d . . . H6 H 1.2941 0.5136 0.2893 0.054 Uiso 1 1 calc R . . B9 B 1.2482(5) 0.7552(4) 0.2269(3) 0.0420(13) Uani 1 1 d . . . H9 H 1.289(5) 0.824(4) 0.223(3) 0.055(16) Uiso 1 1 d . . . B10 B 1.2775(6) 0.6771(4) 0.3028(4) 0.0462(14) Uani 1 1 d . . . H10 H 1.348(5) 0.685(4) 0.347(3) 0.059(17) Uiso 1 1 d . . . H10' H 1.206(6) 0.721(5) 0.314(4) 0.08(2) Uiso 1 1 d . . . B11 B 1.1267(5) 0.6258(4) 0.3130(3) 0.0402(12) Uani 1 1 d . . . H11 H 1.087(5) 0.620(3) 0.364(3) 0.045(14) Uiso 1 1 d . . . C1 C 0.8345(5) 0.9531(3) 0.2388(3) 0.0409(11) Uani 1 1 d . . . C2 C 0.7192(5) 0.9176(3) 0.2221(3) 0.0423(12) Uani 1 1 d . . . C3 C 0.6869(5) 0.8562(3) 0.2797(3) 0.0434(12) Uani 1 1 d . . . C4 C 0.7836(5) 0.8567(3) 0.3324(3) 0.0433(12) Uani 1 1 d . . . C5 C 0.8752(5) 0.9143(3) 0.3064(3) 0.0399(11) Uani 1 1 d . . . C6 C 0.8984(6) 1.0215(4) 0.1935(3) 0.0566(15) Uani 1 1 d . . . H6A H 0.8726 1.0786 0.2093 0.085 Uiso 1 1 calc R . . H6B H 0.8785 1.0137 0.1420 0.085 Uiso 1 1 calc R . . H6C H 0.9850 1.0160 0.2001 0.085 Uiso 1 1 calc R . . C7 C 1.0452(4) 0.6645(3) 0.2488(3) 0.0334(10) Uani 1 1 d . . . C8 C 1.1115(4) 0.7361(3) 0.2005(3) 0.0350(10) Uani 1 1 d . . . C9 C 0.6446(6) 0.9400(4) 0.1547(3) 0.0631(16) Uani 1 1 d . . . H9A H 0.6122 0.9981 0.1599 0.095 Uiso 1 1 calc R . . H9B H 0.5788 0.8990 0.1499 0.095 Uiso 1 1 calc R . . H9C H 0.6952 0.9373 0.1113 0.095 Uiso 1 1 calc R . . C10 C 0.5715(6) 0.8049(4) 0.2853(4) 0.072(2) Uani 1 1 d . . . H10A H 0.5867 0.7514 0.3118 0.108 Uiso 1 1 calc R . . H10B H 0.5422 0.7915 0.2364 0.108 Uiso 1 1 calc R . . H10C H 0.5113 0.8387 0.3114 0.108 Uiso 1 1 calc R . . C11 C 0.7860(8) 0.8069(4) 0.4039(3) 0.073(2) Uani 1 1 d . . . H11A H 0.7523 0.8425 0.4428 0.110 Uiso 1 1 calc R . . H11B H 0.8686 0.7918 0.4160 0.110 Uiso 1 1 calc R . . H11C H 0.7385 0.7544 0.3989 0.110 Uiso 1 1 calc R . . C12 C 0.9918(5) 0.9359(4) 0.3456(4) 0.0635(17) Uani 1 1 d . . . H12A H 1.0505 0.9571 0.3104 0.095 Uiso 1 1 calc R . . H12B H 1.0230 0.8842 0.3694 0.095 Uiso 1 1 calc R . . H12C H 0.9768 0.9802 0.3823 0.095 Uiso 1 1 calc R . . C13 C 0.8119(6) 0.7667(4) 0.0190(3) 0.0575(15) Uani 1 1 d . . . H13 H 0.8344 0.8286 0.0141 0.069 Uiso 1 1 calc R . . C14 C 0.9044(6) 0.7085(4) 0.0037(3) 0.0587(16) Uani 1 1 d . . . H14 H 0.9815 0.7366 -0.0102 0.070 Uiso 1 1 calc R . . C15 C 0.8867(7) 0.6193(5) -0.0304(4) 0.076(2) Uani 1 1 d . . . H15A H 0.8528 0.6268 -0.0797 0.092 Uiso 1 1 calc R . . H15B H 0.9660 0.5919 -0.0359 0.092 Uiso 1 1 calc R . . C16 C 0.8055(7) 0.5580(5) 0.0123(4) 0.081(2) Uani 1 1 d . . . H16A H 0.7283 0.5536 -0.0137 0.097 Uiso 1 1 calc R . . H16B H 0.8425 0.5003 0.0117 0.097 Uiso 1 1 calc R . . C17 C 0.7795(5) 0.5818(4) 0.0912(3) 0.0518(13) Uani 1 1 d . . . H17 H 0.7915 0.5334 0.1263 0.062 Uiso 1 1 calc R . . C18 C 0.6927(5) 0.6410(4) 0.1132(3) 0.0495(13) Uani 1 1 d . . . H18 H 0.6539 0.6270 0.1607 0.059 Uiso 1 1 calc R . . C19 C 0.6121(7) 0.6923(6) 0.0601(5) 0.084(2) Uani 1 1 d . . . H19A H 0.5610 0.6512 0.0332 0.100 Uiso 1 1 calc R . . H19B H 0.5587 0.7297 0.0889 0.100 Uiso 1 1 calc R . . C20 C 0.6784(6) 0.7473(6) 0.0054(4) 0.078(2) Uani 1 1 d . . . H20A H 0.6359 0.8029 0.0019 0.093 Uiso 1 1 calc R . . H20B H 0.6718 0.7191 -0.0426 0.093 Uiso 1 1 calc R . . C21 C 0.7247(8) 0.0677(6) 0.9396(4) 0.092(2) Uani 1 1 d . . . H21A H 0.6951 0.0188 0.9102 0.110 Uiso 1 1 calc R . . H21B H 0.7472 0.1141 0.9054 0.110 Uiso 1 1 calc R . . Cl1 Cl 0.6090(2) 0.1042(2) 0.99415(16) 0.1217(9) Uani 1 1 d . . . Cl2 Cl 0.8493(3) 0.0358(4) 0.9851(2) 0.210(2) 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 Ru1 0.0346(2) 0.0383(2) 0.0345(2) 0.00039(15) -0.00102(15) -0.00049(16) Co1 0.0301(4) 0.0333(3) 0.0380(4) -0.0010(2) 0.0013(3) 0.0014(3) S1 0.0299(6) 0.0368(6) 0.0392(6) 0.0026(5) 0.0024(5) -0.0010(5) S2 0.0342(7) 0.0346(6) 0.0438(7) 0.0049(5) 0.0043(5) -0.0005(5) B1 0.035(3) 0.045(3) 0.049(3) -0.007(2) 0.004(3) 0.008(2) B2 0.042(3) 0.033(3) 0.045(3) -0.001(2) -0.002(3) 0.005(2) B3 0.039(3) 0.040(3) 0.037(3) -0.004(2) -0.005(2) 0.002(2) B4 0.037(3) 0.045(3) 0.048(3) 0.000(2) 0.009(3) 0.000(2) B5 0.030(3) 0.051(3) 0.052(4) -0.002(3) 0.005(3) 0.000(2) B6 0.040(3) 0.047(3) 0.047(3) 0.004(3) -0.003(3) 0.009(3) B9 0.032(3) 0.044(3) 0.050(3) -0.004(2) -0.002(3) -0.004(2) B10 0.041(3) 0.053(3) 0.044(3) -0.004(3) -0.008(3) 0.003(3) B11 0.039(3) 0.043(3) 0.038(3) 0.005(2) 0.001(2) 0.002(2) C1 0.042(3) 0.032(2) 0.049(3) -0.003(2) 0.006(2) 0.004(2) C2 0.036(3) 0.040(3) 0.050(3) -0.007(2) -0.001(2) 0.014(2) C3 0.038(3) 0.040(3) 0.053(3) -0.012(2) 0.011(2) 0.003(2) C4 0.052(3) 0.037(2) 0.041(3) -0.003(2) 0.005(2) 0.006(2) C5 0.037(3) 0.040(2) 0.043(3) -0.006(2) -0.002(2) 0.004(2) C6 0.063(4) 0.042(3) 0.064(4) 0.002(3) 0.009(3) -0.003(3) C7 0.031(2) 0.031(2) 0.038(3) 0.0003(18) 0.0013(19) 0.0002(19) C8 0.031(2) 0.036(2) 0.038(3) 0.0019(19) 0.002(2) -0.001(2) C9 0.060(4) 0.066(4) 0.064(4) -0.009(3) -0.011(3) 0.019(3) C10 0.049(4) 0.070(4) 0.097(5) -0.015(4) 0.020(4) -0.013(3) C11 0.107(6) 0.064(4) 0.048(4) 0.007(3) 0.013(4) 0.009(4) C12 0.058(4) 0.062(4) 0.071(4) -0.010(3) -0.027(3) 0.001(3) C13 0.071(4) 0.064(4) 0.037(3) 0.010(3) -0.013(3) 0.000(3) C14 0.063(4) 0.075(4) 0.038(3) 0.002(3) 0.013(3) 0.000(3) C15 0.097(6) 0.080(5) 0.052(4) -0.016(3) 0.008(4) 0.002(4) C16 0.091(6) 0.070(5) 0.080(5) -0.030(4) 0.020(4) -0.012(4) C17 0.055(3) 0.051(3) 0.049(3) -0.004(2) -0.003(3) -0.015(3) C18 0.041(3) 0.064(3) 0.043(3) -0.004(3) -0.007(2) -0.011(3) C19 0.066(5) 0.099(6) 0.086(5) 0.013(4) -0.019(4) -0.001(4) C20 0.070(5) 0.103(6) 0.060(4) 0.018(4) -0.003(4) 0.011(4) C21 0.120(7) 0.090(6) 0.065(5) 0.001(4) -0.006(5) -0.005(5) Cl1 0.1091(19) 0.141(2) 0.1152(19) -0.0038(16) 0.0067(16) 0.0112(17) Cl2 0.124(2) 0.351(6) 0.154(3) 0.154(4) 0.042(2) 0.067(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C14 2.194(5) . ? Ru1 C18 2.197(5) . ? Ru1 C17 2.203(5) . ? Ru1 C13 2.218(5) . ? Ru1 S1 2.3646(17) . ? Ru1 S2 2.3773(15) . ? Ru1 B3 2.612(6) . ? Ru1 Co1 2.6234(11) . ? Co1 C5 2.010(5) . ? Co1 C4 2.046(5) . ? Co1 C1 2.060(5) . ? Co1 C3 2.067(5) . ? Co1 C2 2.084(5) . ? Co1 S1 2.1864(17) . ? Co1 S2 2.1866(16) . ? S1 C7 1.803(5) . ? S2 C8 1.797(5) . ? B1 B3 1.750(8) . ? B1 B2 1.773(8) . ? B1 B4 1.781(8) . ? B1 B6 1.784(9) . ? B1 B5 1.790(9) . ? B2 C7 1.715(7) . ? B2 B6 1.749(8) . ? B2 B3 1.754(8) . ? B2 B11 1.801(8) . ? B3 C8 1.718(7) . ? B3 C7 1.732(7) . ? B3 B4 1.750(8) . ? B4 C8 1.722(7) . ? B4 B5 1.760(9) . ? B4 B9 1.812(8) . ? B5 B10 1.771(9) . ? B5 B9 1.774(8) . ? B5 B6 1.818(9) . ? B6 B10 1.786(9) . ? B6 B11 1.790(8) . ? B9 C8 1.599(7) . ? B9 B10 1.843(9) . ? B10 B11 1.838(9) . ? B11 C7 1.577(7) . ? C1 C2 1.408(7) . ? C1 C5 1.425(7) . ? C1 C6 1.500(7) . ? C2 C3 1.443(7) . ? C2 C9 1.504(8) . ? C3 C4 1.423(8) . ? C3 C10 1.492(8) . ? C4 C5 1.415(7) . ? C4 C11 1.497(8) . ? C5 C12 1.498(7) . ? C7 C8 1.575(6) . ? C13 C14 1.377(9) . ? C13 C20 1.513(9) . ? C14 C15 1.507(9) . ? C15 C16 1.504(10) . ? C16 C17 1.495(8) . ? C17 C18 1.371(8) . ? C18 C19 1.520(9) . ? C19 C20 1.485(10) . ? C21 Cl2 1.667(9) . ? C21 Cl1 1.699(8) . ? 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 Ru1 C18 94.2(2) . . ? C14 Ru1 C17 80.7(2) . . ? C18 Ru1 C17 36.3(2) . . ? C14 Ru1 C13 36.4(2) . . ? C18 Ru1 C13 81.3(2) . . ? C17 Ru1 C13 90.1(2) . . ? C14 Ru1 S1 166.10(18) . . ? C18 Ru1 S1 93.46(15) . . ? C17 Ru1 S1 98.83(15) . . ? C13 Ru1 S1 157.05(17) . . ? C14 Ru1 S2 98.27(18) . . ? C18 Ru1 S2 155.59(16) . . ? C17 Ru1 S2 167.32(17) . . ? C13 Ru1 S2 96.51(18) . . ? S1 Ru1 S2 79.07(4) . . ? C14 Ru1 B3 96.1(2) . . ? C18 Ru1 B3 130.2(2) . . ? C17 Ru1 B3 98.2(2) . . ? C13 Ru1 B3 129.6(2) . . ? S1 Ru1 B3 70.18(13) . . ? S2 Ru1 B3 69.26(14) . . ? C14 Ru1 Co1 136.17(18) . . ? C18 Ru1 Co1 105.78(15) . . ? C17 Ru1 Co1 135.96(15) . . ? C13 Ru1 Co1 108.10(18) . . ? S1 Ru1 Co1 51.68(4) . . ? S2 Ru1 Co1 51.57(4) . . ? B3 Ru1 Co1 99.68(13) . . ? C5 Co1 C4 40.8(2) . . ? C5 Co1 C1 41.0(2) . . ? C4 Co1 C1 68.3(2) . . ? C5 Co1 C3 68.6(2) . . ? C4 Co1 C3 40.5(2) . . ? C1 Co1 C3 68.2(2) . . ? C5 Co1 C2 67.9(2) . . ? C4 Co1 C2 67.8(2) . . ? C1 Co1 C2 39.7(2) . . ? C3 Co1 C2 40.7(2) . . ? C5 Co1 S1 123.85(15) . . ? C4 Co1 S1 99.77(15) . . ? C1 Co1 S1 164.79(16) . . ? C3 Co1 S1 109.40(15) . . ? C2 Co1 S1 145.95(16) . . ? C5 Co1 S2 107.36(15) . . ? C4 Co1 S2 144.67(16) . . ? C1 Co1 S2 97.23(14) . . ? C3 Co1 S2 162.33(16) . . ? C2 Co1 S2 121.64(15) . . ? S1 Co1 S2 87.30(5) . . ? C5 Co1 Ru1 165.68(15) . . ? C4 Co1 Ru1 151.65(15) . . ? C1 Co1 Ru1 136.23(15) . . ? C3 Co1 Ru1 125.33(15) . . ? C2 Co1 Ru1 119.40(15) . . ? S1 Co1 Ru1 58.05(4) . . ? S2 Co1 Ru1 58.40(4) . . ? C7 S1 Co1 106.37(15) . . ? C7 S1 Ru1 91.30(15) . . ? Co1 S1 Ru1 70.28(4) . . ? C8 S2 Co1 105.80(16) . . ? C8 S2 Ru1 91.10(16) . . ? Co1 S2 Ru1 70.03(5) . . ? B3 B1 B2 59.7(3) . . ? B3 B1 B4 59.4(3) . . ? B2 B1 B4 108.3(4) . . ? B3 B1 B6 105.9(4) . . ? B2 B1 B6 58.9(3) . . ? B4 B1 B6 108.5(4) . . ? B3 B1 B5 105.4(4) . . ? B2 B1 B5 107.6(4) . . ? B4 B1 B5 59.1(4) . . ? B6 B1 B5 61.2(3) . . ? C7 B2 B6 100.3(4) . . ? C7 B2 B3 59.9(3) . . ? B6 B2 B3 107.3(4) . . ? C7 B2 B1 103.6(4) . . ? B6 B2 B1 60.9(3) . . ? B3 B2 B1 59.5(3) . . ? C7 B2 B11 53.2(3) . . ? B6 B2 B11 60.5(3) . . ? B3 B2 B11 105.4(4) . . ? B1 B2 B11 108.3(4) . . ? C8 B3 C7 54.3(3) . . ? C8 B3 B1 104.4(4) . . ? C7 B3 B1 103.9(4) . . ? C8 B3 B4 59.5(3) . . ? C7 B3 B4 104.1(4) . . ? B1 B3 B4 61.2(3) . . ? C8 B3 B2 103.7(4) . . ? C7 B3 B2 58.9(3) . . ? B1 B3 B2 60.8(3) . . ? B4 B3 B2 110.7(4) . . ? C8 B3 Ru1 85.4(3) . . ? C7 B3 Ru1 85.0(3) . . ? B1 B3 Ru1 169.4(4) . . ? B4 B3 Ru1 122.6(3) . . ? B2 B3 Ru1 121.5(3) . . ? C8 B4 B3 59.3(3) . . ? C8 B4 B5 99.3(4) . . ? B3 B4 B5 106.7(4) . . ? C8 B4 B1 102.9(4) . . ? B3 B4 B1 59.4(3) . . ? B5 B4 B1 60.7(4) . . ? C8 B4 B9 53.7(3) . . ? B3 B4 B9 105.3(4) . . ? B5 B4 B9 59.5(3) . . ? B1 B4 B9 107.7(4) . . ? B4 B5 B10 113.4(4) . . ? B4 B5 B9 61.7(3) . . ? B10 B5 B9 62.7(4) . . ? B4 B5 B1 60.2(3) . . ? B10 B5 B1 110.0(4) . . ? B9 B5 B1 109.0(4) . . ? B4 B5 B6 107.9(4) . . ? B10 B5 B6 59.7(3) . . ? B9 B5 B6 107.5(4) . . ? B1 B5 B6 59.3(3) . . ? B2 B6 B1 60.2(3) . . ? B2 B6 B10 112.3(4) . . ? B1 B6 B10 109.6(4) . . ? B2 B6 B11 61.2(3) . . ? B1 B6 B11 108.3(4) . . ? B10 B6 B11 61.9(4) . . ? B2 B6 B5 107.4(4) . . ? B1 B6 B5 59.6(3) . . ? B10 B6 B5 58.9(4) . . ? B11 B6 B5 105.9(4) . . ? C8 B9 B5 103.6(4) . . ? C8 B9 B4 60.2(3) . . ? B5 B9 B4 58.8(3) . . ? C8 B9 B10 105.4(4) . . ? B5 B9 B10 58.6(3) . . ? B4 B9 B10 107.7(4) . . ? B5 B10 B6 61.5(4) . . ? B5 B10 B11 105.8(4) . . ? B6 B10 B11 59.2(3) . . ? B5 B10 B9 58.7(3) . . ? B6 B10 B9 106.0(4) . . ? B11 B10 B9 101.1(4) . . ? C7 B11 B6 104.1(4) . . ? C7 B11 B2 60.6(3) . . ? B6 B11 B2 58.3(3) . . ? C7 B11 B10 106.1(4) . . ? B6 B11 B10 59.0(3) . . ? B2 B11 B10 107.5(4) . . ? C2 C1 C5 107.7(4) . . ? C2 C1 C6 124.8(5) . . ? C5 C1 C6 127.4(5) . . ? C2 C1 Co1 71.1(3) . . ? C5 C1 Co1 67.6(3) . . ? C6 C1 Co1 128.2(4) . . ? C1 C2 C3 108.4(5) . . ? C1 C2 C9 125.0(5) . . ? C3 C2 C9 126.5(5) . . ? C1 C2 Co1 69.2(3) . . ? C3 C2 Co1 69.0(3) . . ? C9 C2 Co1 126.9(4) . . ? C4 C3 C2 107.0(5) . . ? C4 C3 C10 126.1(5) . . ? C2 C3 C10 126.8(6) . . ? C4 C3 Co1 69.0(3) . . ? C2 C3 Co1 70.3(3) . . ? C10 C3 Co1 128.0(4) . . ? C5 C4 C3 108.2(4) . . ? C5 C4 C11 126.1(5) . . ? C3 C4 C11 125.7(5) . . ? C5 C4 Co1 68.2(3) . . ? C3 C4 Co1 70.6(3) . . ? C11 C4 Co1 128.2(4) . . ? C4 C5 C1 108.6(4) . . ? C4 C5 C12 125.9(5) . . ? C1 C5 C12 125.4(5) . . ? C4 C5 Co1 70.9(3) . . ? C1 C5 Co1 71.4(3) . . ? C12 C5 Co1 126.7(4) . . ? C8 C7 B11 113.8(4) . . ? C8 C7 B2 112.0(4) . . ? B11 C7 B2 66.2(3) . . ? C8 C7 B3 62.4(3) . . ? B11 C7 B3 117.4(4) . . ? B2 C7 B3 61.2(3) . . ? C8 C7 S1 113.0(3) . . ? B11 C7 S1 125.3(3) . . ? B2 C7 S1 118.2(3) . . ? B3 C7 S1 108.4(3) . . ? C7 C8 B9 113.3(4) . . ? C7 C8 B3 63.3(3) . . ? B9 C8 B3 117.2(4) . . ? C7 C8 B4 112.6(4) . . ? B9 C8 B4 66.0(3) . . ? B3 C8 B4 61.2(3) . . ? C7 C8 S2 114.2(3) . . ? B9 C8 S2 125.0(4) . . ? B3 C8 S2 107.9(3) . . ? B4 C8 S2 116.5(3) . . ? C14 C13 C20 123.6(7) . . ? C14 C13 Ru1 70.9(3) . . ? C20 C13 Ru1 109.9(4) . . ? C13 C14 C15 124.8(7) . . ? C13 C14 Ru1 72.8(3) . . ? C15 C14 Ru1 110.6(4) . . ? C16 C15 C14 115.5(5) . . ? C17 C16 C15 116.6(6) . . ? C18 C17 C16 124.5(6) . . ? C18 C17 Ru1 71.6(3) . . ? C16 C17 Ru1 111.8(4) . . ? C17 C18 C19 124.2(6) . . ? C17 C18 Ru1 72.1(3) . . ? C19 C18 Ru1 110.5(4) . . ? C20 C19 C18 115.1(6) . . ? C19 C20 C13 118.5(6) . . ? Cl2 C21 Cl1 115.0(5) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.919 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.105