Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_address ; Department of Chemistry Fudan University Shanghai 200433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Synthesis and Characterization of Binuclear Half-sandwich Metal (Co, Ir and Ru) Complexes Containing Ancillary ortho-Carborane-1,2-Dithiolato Ligands ; loop_ _publ_author_name 'Guo-Xin Jin.' 'Shuang Liu.' 'Xin Wang.' 'JiaSheng Zhang.' # Attachment 'f50405c-complex 4.cif' data_f50405c _database_code_depnum_ccdc_archive 'CCDC 611979' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H56 B20 Cl4 N2 Ru2 S4' _chemical_formula_weight 1133.15 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.399(5) _cell_length_b 11.160(5) _cell_length_c 12.289(6) _cell_angle_alpha 75.781(6) _cell_angle_beta 67.108(6) _cell_angle_gamma 76.583(6) _cell_volume 1258.6(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 570 _exptl_absorpt_coefficient_mu 1.007 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8240 _exptl_absorpt_correction_T_max 0.9060 _exptl_absorpt_process_details ? _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 5815 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4847 _reflns_number_gt 4164 _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^)+(0.0533P)^2^+2.4894P] 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 4847 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1255 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 0.85038(4) -0.04812(3) 0.80572(3) 0.03097(13) Uani 1 1 d . . . S1 S 0.95391(12) 0.11851(11) 0.65972(10) 0.0387(3) Uani 1 1 d . . . S2 S 0.65083(12) 0.09627(10) 0.89163(10) 0.0390(3) Uani 1 1 d . . . N1 N 0.9397(4) -0.0123(3) 0.9207(3) 0.0342(8) Uani 1 1 d . . . C1 C 0.8398(5) 0.2592(4) 0.6987(4) 0.0356(10) Uani 1 1 d . . . C2 C 0.6894(5) 0.2475(4) 0.8151(4) 0.0372(10) Uani 1 1 d . . . C3 C 0.9857(6) -0.2356(4) 0.7871(5) 0.0485(12) Uani 1 1 d . . . C4 C 0.9682(6) -0.1782(5) 0.6771(5) 0.0460(12) Uani 1 1 d . . . H4 H 1.0505 -0.1539 0.6076 0.055 Uiso 1 1 calc R . . C5 C 0.8312(6) -0.1354(5) 0.6713(5) 0.0464(12) Uani 1 1 d . . . H5 H 0.8218 -0.0821 0.5976 0.056 Uiso 1 1 calc R . . C6 C 0.7101(6) -0.1487(5) 0.7731(5) 0.0452(11) Uani 1 1 d . . . C7 C 0.7268(6) -0.2042(4) 0.8845(5) 0.0466(12) Uani 1 1 d . . . H7 H 0.6450 -0.1998 0.9590 0.056 Uiso 1 1 calc R . . C8 C 0.8612(6) -0.2452(4) 0.8900(5) 0.0472(12) Uani 1 1 d . . . H8 H 0.8706 -0.2680 0.9691 0.057 Uiso 1 1 calc R . . C9 C 1.1308(7) -0.2861(6) 0.7964(7) 0.0719(18) Uani 1 1 d . . . H9 H 1.1310 -0.2618 0.8677 0.086 Uiso 1 1 calc R . . C10 C 1.2517(8) -0.2378(9) 0.6920(9) 0.104(3) Uani 1 1 d . . . H10A H 1.2653 -0.2728 0.6237 0.156 Uiso 1 1 calc R . . H10B H 1.3359 -0.2612 0.7117 0.156 Uiso 1 1 calc R . . H10C H 1.2315 -0.1483 0.6737 0.156 Uiso 1 1 calc R . . C11 C 1.1498(11) -0.4289(8) 0.8179(12) 0.135(4) Uani 1 1 d . . . H11A H 1.1661 -0.4564 0.7448 0.202 Uiso 1 1 calc R . . H11B H 1.0660 -0.4571 0.8788 0.202 Uiso 1 1 calc R . . H11C H 1.2290 -0.4629 0.8435 0.202 Uiso 1 1 calc R . . C12 C 0.5656(6) -0.1038(6) 0.7669(6) 0.0643(16) Uani 1 1 d . . . H12A H 0.5704 -0.0385 0.6986 0.096 Uiso 1 1 calc R . . H12B H 0.5041 -0.0721 0.8387 0.096 Uiso 1 1 calc R . . H12C H 0.5295 -0.1719 0.7594 0.096 Uiso 1 1 calc R . . C13 C 0.8673(5) -0.0203(4) 1.0386(4) 0.0393(10) Uani 1 1 d . . . H13 H 0.7742 -0.0346 1.0688 0.047 Uiso 1 1 calc R . . C14 C 1.0726(5) 0.0079(4) 0.8840(4) 0.0377(10) Uani 1 1 d . . . H14 H 1.1267 0.0138 0.8027 0.045 Uiso 1 1 calc R . . B3 B 0.6836(6) 0.2906(5) 0.6711(5) 0.0445(13) Uani 1 1 d . . . H3 H 0.6543 0.2319 0.6271 0.053 Uiso 1 1 calc R . . B4 B 0.8164(7) 0.3841(5) 0.5911(5) 0.0496(14) Uani 1 1 d . . . H4A H 0.8733 0.3870 0.4943 0.060 Uiso 1 1 calc R . . B5 B 0.9034(7) 0.3914(5) 0.6879(6) 0.0520(15) Uani 1 1 d . . . H5A H 1.0165 0.3987 0.6543 0.062 Uiso 1 1 calc R . . B6 B 0.8222(6) 0.3034(5) 0.8295(5) 0.0429(12) Uani 1 1 d . . . H6 H 0.8821 0.2532 0.8881 0.052 Uiso 1 1 calc R . . B7 B 0.5581(7) 0.3634(6) 0.7907(6) 0.0518(15) Uani 1 1 d . . . H7A H 0.4461 0.3523 0.8249 0.062 Uiso 1 1 calc R . . B8 B 0.6375(8) 0.4542(6) 0.6498(6) 0.0588(16) Uani 1 1 d . . . H8A H 0.5767 0.5043 0.5919 0.071 Uiso 1 1 calc R . . B9 B 0.7747(8) 0.5176(6) 0.6584(6) 0.0593(17) Uani 1 1 d . . . H9A H 0.8040 0.6085 0.6055 0.071 Uiso 1 1 calc R . . B10 B 0.7762(8) 0.4672(6) 0.8062(6) 0.0582(17) Uani 1 1 d . . . H10 H 0.8058 0.5261 0.8499 0.070 Uiso 1 1 calc R . . B11 B 0.6442(7) 0.3721(5) 0.8870(6) 0.0496(14) Uani 1 1 d . . . H11 H 0.5876 0.3669 0.9842 0.059 Uiso 1 1 calc R . . B12 B 0.6139(8) 0.5044(6) 0.7828(7) 0.0628(18) Uani 1 1 d . . . H12 H 0.5377 0.5872 0.8115 0.075 Uiso 1 1 calc R . . C15 C 0.3144(13) 0.2605(14) 0.6017(13) 0.248(11) Uani 1 1 d . . . H15A H 0.3824 0.3176 0.5574 0.297 Uiso 1 1 calc R . . H15B H 0.2301 0.2942 0.5816 0.297 Uiso 1 1 calc R . . Cl1 Cl 0.2752(4) 0.2559(3) 0.7407(4) 0.1575(13) Uani 1 1 d . . . Cl2 Cl 0.3849(4) 0.1158(6) 0.5545(4) 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 Ru1 0.0376(2) 0.0291(2) 0.02654(19) -0.00779(13) -0.01058(15) -0.00404(14) S1 0.0423(6) 0.0358(6) 0.0293(6) -0.0064(5) -0.0039(5) -0.0041(5) S2 0.0388(6) 0.0346(6) 0.0352(6) -0.0067(5) -0.0044(5) -0.0046(5) N1 0.042(2) 0.0324(19) 0.0280(18) -0.0048(15) -0.0114(16) -0.0064(16) C1 0.043(3) 0.030(2) 0.030(2) -0.0040(17) -0.0091(19) -0.0057(18) C2 0.043(3) 0.032(2) 0.036(2) -0.0092(19) -0.013(2) -0.0031(19) C3 0.058(3) 0.030(2) 0.061(3) -0.017(2) -0.026(3) 0.004(2) C4 0.055(3) 0.040(3) 0.042(3) -0.022(2) -0.007(2) -0.007(2) C5 0.063(3) 0.044(3) 0.040(3) -0.017(2) -0.021(2) -0.008(2) C6 0.054(3) 0.040(3) 0.051(3) -0.015(2) -0.022(2) -0.011(2) C7 0.053(3) 0.038(3) 0.048(3) -0.011(2) -0.011(2) -0.015(2) C8 0.072(4) 0.030(2) 0.043(3) -0.006(2) -0.026(3) -0.006(2) C9 0.067(4) 0.056(4) 0.102(5) -0.027(4) -0.044(4) 0.014(3) C10 0.055(4) 0.118(7) 0.142(8) -0.055(6) -0.029(5) 0.008(4) C11 0.109(7) 0.063(5) 0.234(13) -0.028(6) -0.086(8) 0.029(5) C12 0.060(4) 0.076(4) 0.073(4) -0.026(3) -0.032(3) -0.012(3) C13 0.039(2) 0.047(3) 0.031(2) -0.007(2) -0.009(2) -0.011(2) C14 0.041(3) 0.044(3) 0.026(2) -0.0077(19) -0.0072(19) -0.008(2) B3 0.051(3) 0.040(3) 0.046(3) -0.007(2) -0.023(3) -0.003(2) B4 0.065(4) 0.039(3) 0.041(3) 0.003(2) -0.020(3) -0.009(3) B5 0.065(4) 0.034(3) 0.057(4) -0.003(3) -0.018(3) -0.019(3) B6 0.054(3) 0.040(3) 0.040(3) -0.013(2) -0.017(3) -0.009(2) B7 0.046(3) 0.047(3) 0.055(4) -0.012(3) -0.016(3) 0.007(3) B8 0.067(4) 0.043(3) 0.058(4) 0.001(3) -0.025(3) 0.002(3) B9 0.078(5) 0.031(3) 0.062(4) 0.000(3) -0.024(4) -0.006(3) B10 0.075(5) 0.037(3) 0.067(4) -0.018(3) -0.024(4) -0.010(3) B11 0.059(4) 0.038(3) 0.046(3) -0.019(3) -0.009(3) -0.001(3) B12 0.071(4) 0.038(3) 0.068(4) -0.010(3) -0.019(4) 0.005(3) C15 0.125(10) 0.236(16) 0.177(13) 0.143(12) 0.008(9) 0.061(10) Cl1 0.215(4) 0.130(2) 0.187(3) -0.019(2) -0.123(3) -0.054(2) Cl2 0.160(3) 0.364(7) 0.151(3) -0.114(4) -0.077(3) 0.103(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 Ru1 N1 2.119(4) . ? Ru1 C8 2.186(5) . ? Ru1 C5 2.203(5) . ? Ru1 C7 2.205(5) . ? Ru1 C4 2.214(5) . ? Ru1 C6 2.233(5) . ? Ru1 C3 2.242(5) . ? Ru1 S2 2.3658(14) . ? Ru1 S1 2.3713(14) . ? S1 C1 1.779(5) . ? S2 C2 1.770(5) . ? N1 C14 1.332(6) . ? N1 C13 1.339(6) . ? C1 C2 1.665(6) . ? C1 B5 1.709(7) . ? C1 B4 1.714(7) . ? C1 B6 1.725(7) . ? C1 B3 1.727(7) . ? C2 B11 1.707(7) . ? C2 B7 1.713(7) . ? C2 B6 1.724(7) . ? C2 B3 1.736(7) . ? C3 C4 1.409(7) . ? C3 C8 1.418(8) . ? C3 C9 1.522(8) . ? C4 C5 1.418(7) . ? C4 H4 0.9800 . ? C5 C6 1.394(7) . ? C5 H5 0.9800 . ? C6 C7 1.417(7) . ? C6 C12 1.495(8) . ? C7 C8 1.388(8) . ? C7 H7 0.9800 . ? C8 H8 0.9800 . ? C9 C10 1.496(11) . ? C9 C11 1.528(10) . ? C9 H9 0.9800 . ? 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 1.372(6) 2_757 ? C13 H13 0.9300 . ? C14 C13 1.372(6) 2_757 ? C14 H14 0.9300 . ? B3 B4 1.752(9) . ? B3 B8 1.758(8) . ? B3 B7 1.768(8) . ? B3 H3 1.1000 . ? B4 B9 1.767(9) . ? B4 B8 1.775(10) . ? B4 B5 1.778(9) . ? B4 H4A 1.1000 . ? B5 B6 1.763(8) . ? B5 B9 1.778(9) . ? B5 B10 1.780(9) . ? B5 H5A 1.1000 . ? B6 B10 1.760(8) . ? B6 B11 1.762(9) . ? B6 H6 1.1000 . ? B7 B8 1.767(9) . ? B7 B12 1.768(10) . ? B7 B11 1.770(9) . ? B7 H7A 1.1000 . ? B8 B12 1.766(10) . ? B8 B9 1.780(10) . ? B8 H8A 1.1000 . ? B9 B10 1.769(10) . ? B9 B12 1.780(10) . ? B9 H9A 1.1000 . ? B10 B12 1.759(11) . ? B10 B11 1.760(9) . ? B10 H10 1.1000 . ? B11 B12 1.758(9) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C15 Cl1 1.584(16) . ? C15 Cl2 1.750(18) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? 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 N1 Ru1 C8 90.01(17) . . ? N1 Ru1 C5 158.51(17) . . ? C8 Ru1 C5 78.29(19) . . ? N1 Ru1 C7 113.74(17) . . ? C8 Ru1 C7 36.9(2) . . ? C5 Ru1 C7 66.4(2) . . ? N1 Ru1 C4 121.22(18) . . ? C8 Ru1 C4 66.39(19) . . ? C5 Ru1 C4 37.44(19) . . ? C7 Ru1 C4 78.88(19) . . ? N1 Ru1 C6 150.63(17) . . ? C8 Ru1 C6 66.69(19) . . ? C5 Ru1 C6 36.62(19) . . ? C7 Ru1 C6 37.23(19) . . ? C4 Ru1 C6 66.99(19) . . ? N1 Ru1 C3 92.77(17) . . ? C8 Ru1 C3 37.3(2) . . ? C5 Ru1 C3 67.01(19) . . ? C7 Ru1 C3 67.2(2) . . ? C4 Ru1 C3 36.85(19) . . ? C6 Ru1 C3 79.55(19) . . ? N1 Ru1 S2 86.95(11) . . ? C8 Ru1 S2 119.32(15) . . ? C5 Ru1 S2 114.48(15) . . ? C7 Ru1 S2 91.50(15) . . ? C4 Ru1 S2 151.80(15) . . ? C6 Ru1 S2 89.29(14) . . ? C3 Ru1 S2 156.63(15) . . ? N1 Ru1 S1 88.61(10) . . ? C8 Ru1 S1 150.92(15) . . ? C5 Ru1 S1 92.96(14) . . ? C7 Ru1 S1 157.65(14) . . ? C4 Ru1 S1 89.75(14) . . ? C6 Ru1 S1 120.50(14) . . ? C3 Ru1 S1 113.75(15) . . ? S2 Ru1 S1 89.61(5) . . ? C1 S1 Ru1 106.79(15) . . ? C2 S2 Ru1 106.94(16) . . ? C14 N1 C13 116.0(4) . . ? C14 N1 Ru1 123.1(3) . . ? C13 N1 Ru1 120.6(3) . . ? C2 C1 B5 110.6(4) . . ? C2 C1 B4 110.3(4) . . ? B5 C1 B4 62.6(3) . . ? C2 C1 B6 61.1(3) . . ? B5 C1 B6 61.8(3) . . ? B4 C1 B6 112.9(4) . . ? C2 C1 B3 61.6(3) . . ? B5 C1 B3 113.0(4) . . ? B4 C1 B3 61.2(3) . . ? B6 C1 B3 113.1(4) . . ? C2 C1 S1 117.9(3) . . ? B5 C1 S1 122.0(4) . . ? B4 C1 S1 121.4(3) . . ? B6 C1 S1 118.4(3) . . ? B3 C1 S1 116.9(3) . . ? C1 C2 B11 110.3(4) . . ? C1 C2 B7 110.5(4) . . ? B11 C2 B7 62.3(4) . . ? C1 C2 B6 61.2(3) . . ? B11 C2 B6 61.8(3) . . ? B7 C2 B6 113.1(4) . . ? C1 C2 B3 61.0(3) . . ? B11 C2 B3 112.5(4) . . ? B7 C2 B3 61.7(3) . . ? B6 C2 B3 112.7(4) . . ? C1 C2 S2 118.4(3) . . ? B11 C2 S2 122.6(3) . . ? B7 C2 S2 120.3(4) . . ? B6 C2 S2 119.2(3) . . ? B3 C2 S2 116.5(3) . . ? C4 C3 C8 116.9(5) . . ? C4 C3 C9 122.1(5) . . ? C8 C3 C9 121.0(5) . . ? C4 C3 Ru1 70.5(3) . . ? C8 C3 Ru1 69.2(3) . . ? C9 C3 Ru1 131.5(4) . . ? C3 C4 C5 120.5(5) . . ? C3 C4 Ru1 72.7(3) . . ? C5 C4 Ru1 70.9(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? Ru1 C4 H4 119.3 . . ? C6 C5 C4 121.6(5) . . ? C6 C5 Ru1 72.8(3) . . ? C4 C5 Ru1 71.7(3) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? Ru1 C5 H5 118.7 . . ? C5 C6 C7 118.2(5) . . ? C5 C6 C12 121.6(5) . . ? C7 C6 C12 120.2(5) . . ? C5 C6 Ru1 70.5(3) . . ? C7 C6 Ru1 70.3(3) . . ? C12 C6 Ru1 129.7(4) . . ? C8 C7 C6 120.0(5) . . ? C8 C7 Ru1 70.8(3) . . ? C6 C7 Ru1 72.5(3) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? Ru1 C7 H7 119.5 . . ? C7 C8 C3 122.7(5) . . ? C7 C8 Ru1 72.3(3) . . ? C3 C8 Ru1 73.5(3) . . ? C7 C8 H8 118.2 . . ? C3 C8 H8 118.2 . . ? Ru1 C8 H8 118.2 . . ? C10 C9 C3 115.1(6) . . ? C10 C9 C11 111.1(7) . . ? C3 C9 C11 108.1(6) . . ? C10 C9 H9 107.4 . . ? C3 C9 H9 107.4 . . ? C11 C9 H9 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 C14 121.6(4) . 2_757 ? N1 C13 H13 119.2 . . ? C14 C13 H13 119.2 2_757 . ? N1 C14 C13 122.5(4) . 2_757 ? N1 C14 H14 118.8 . . ? C13 C14 H14 118.8 2_757 . ? C1 B3 C2 57.5(3) . . ? C1 B3 B4 59.0(3) . . ? C2 B3 B4 105.3(4) . . ? C1 B3 B8 105.9(4) . . ? C2 B3 B8 105.2(4) . . ? B4 B3 B8 60.7(4) . . ? C1 B3 B7 105.1(4) . . ? C2 B3 B7 58.5(3) . . ? B4 B3 B7 108.5(4) . . ? B8 B3 B7 60.1(4) . . ? C1 B3 H3 124.0 . . ? C2 B3 H3 124.4 . . ? B4 B3 H3 121.6 . . ? B8 B3 H3 122.3 . . ? B7 B3 H3 122.1 . . ? C1 B4 B3 59.7(3) . . ? C1 B4 B9 105.5(4) . . ? B3 B4 B9 108.4(5) . . ? C1 B4 B8 105.7(4) . . ? B3 B4 B8 59.8(4) . . ? B9 B4 B8 60.3(4) . . ? C1 B4 B5 58.6(3) . . ? B3 B4 B5 108.5(4) . . ? B9 B4 B5 60.2(4) . . ? B8 B4 B5 108.4(5) . . ? C1 B4 H4A 124.0 . . ? B3 B4 H4A 121.1 . . ? B9 B4 H4A 122.0 . . ? B8 B4 H4A 122.1 . . ? B5 B4 H4A 121.4 . . ? C1 B5 B6 59.6(3) . . ? C1 B5 B9 105.2(5) . . ? B6 B5 B9 107.7(5) . . ? C1 B5 B4 58.8(3) . . ? B6 B5 B4 108.1(4) . . ? B9 B5 B4 59.6(4) . . ? C1 B5 B10 105.2(4) . . ? B6 B5 B10 59.6(3) . . ? B9 B5 B10 59.6(4) . . ? B4 B5 B10 107.1(5) . . ? C1 B5 H5A 123.9 . . ? B6 B5 H5A 121.4 . . ? B9 B5 H5A 122.6 . . ? B4 B5 H5A 121.9 . . ? B10 B5 H5A 122.8 . . ? C2 B6 C1 57.7(3) . . ? C2 B6 B10 105.2(4) . . ? C1 B6 B10 105.4(4) . . ? C2 B6 B11 58.6(3) . . ? C1 B6 B11 105.0(4) . . ? B10 B6 B11 60.0(4) . . ? C2 B6 B5 105.4(4) . . ? C1 B6 B5 58.7(3) . . ? B10 B6 B5 60.7(4) . . ? B11 B6 B5 108.5(4) . . ? C2 B6 H6 124.2 . . ? C1 B6 H6 124.2 . . ? B10 B6 H6 122.6 . . ? B11 B6 H6 122.1 . . ? B5 B6 H6 121.7 . . ? C2 B7 B8 105.9(4) . . ? C2 B7 B3 59.8(3) . . ? B8 B7 B3 59.6(4) . . ? C2 B7 B12 105.0(5) . . ? B8 B7 B12 59.9(4) . . ? B3 B7 B12 107.5(5) . . ? C2 B7 B11 58.7(3) . . ? B8 B7 B11 107.7(5) . . ? B3 B7 B11 108.1(4) . . ? B12 B7 B11 59.6(4) . . ? C2 B7 H7A 123.8 . . ? B8 B7 H7A 122.2 . . ? B3 B7 H7A 121.4 . . ? B12 B7 H7A 122.7 . . ? B11 B7 H7A 121.8 . . ? B3 B8 B12 108.1(4) . . ? B3 B8 B7 60.2(3) . . ? B12 B8 B7 60.1(4) . . ? B3 B8 B4 59.5(3) . . ? B12 B8 B4 107.6(5) . . ? B7 B8 B4 107.6(4) . . ? B3 B8 B9 107.6(5) . . ? B12 B8 B9 60.3(4) . . ? B7 B8 B9 108.2(5) . . ? B4 B8 B9 59.6(4) . . ? B3 B8 H8A 121.9 . . ? B12 B8 H8A 121.6 . . ? B7 B8 H8A 121.6 . . ? B4 B8 H8A 122.3 . . ? B9 B8 H8A 121.8 . . ? B4 B9 B10 108.0(4) . . ? B4 B9 B5 60.2(4) . . ? B10 B9 B5 60.2(4) . . ? B4 B9 B12 107.4(5) . . ? B10 B9 B12 59.4(4) . . ? B5 B9 B12 107.6(5) . . ? B4 B9 B8 60.1(4) . . ? B10 B9 B8 107.4(5) . . ? B5 B9 B8 108.2(4) . . ? B12 B9 B8 59.5(4) . . ? B4 B9 H9A 121.7 . . ? B10 B9 H9A 121.9 . . ? B5 B9 H9A 121.5 . . ? B12 B9 H9A 122.4 . . ? B8 B9 H9A 121.9 . . ? B12 B10 B11 59.9(4) . . ? B12 B10 B6 108.3(4) . . ? B11 B10 B6 60.1(3) . . ? B12 B10 B9 60.6(4) . . ? B11 B10 B9 108.4(5) . . ? B6 B10 B9 108.2(4) . . ? B12 B10 B5 108.4(5) . . ? B11 B10 B5 107.8(4) . . ? B6 B10 B5 59.7(3) . . ? B9 B10 B5 60.1(4) . . ? B12 B10 H10 121.3 . . ? B11 B10 H10 121.8 . . ? B6 B10 H10 121.7 . . ? B9 B10 H10 121.3 . . ? B5 B10 H10 121.8 . . ? C2 B11 B12 105.8(4) . . ? C2 B11 B10 105.9(4) . . ? B12 B11 B10 60.0(4) . . ? C2 B11 B6 59.6(3) . . ? B12 B11 B6 108.2(5) . . ? B10 B11 B6 60.0(4) . . ? C2 B11 B7 59.0(3) . . ? B12 B11 B7 60.2(4) . . ? B10 B11 B7 108.3(5) . . ? B6 B11 B7 108.6(4) . . ? C2 B11 H11 123.7 . . ? B12 B11 H11 122.1 . . ? B10 B11 H11 122.1 . . ? B6 B11 H11 121.2 . . ? B7 B11 H11 121.3 . . ? B11 B12 B10 60.0(4) . . ? B11 B12 B8 108.3(4) . . ? B10 B12 B8 108.5(5) . . ? B11 B12 B7 60.3(4) . . ? B10 B12 B7 108.4(4) . . ? B8 B12 B7 60.0(4) . . ? B11 B12 B9 108.0(5) . . ? B10 B12 B9 60.0(4) . . ? B8 B12 B9 60.3(4) . . ? B7 B12 B9 108.1(5) . . ? B11 B12 H12 121.6 . . ? B10 B12 H12 121.5 . . ? B8 B12 H12 121.4 . . ? B7 B12 H12 121.6 . . ? B9 B12 H12 121.7 . . ? Cl1 C15 Cl2 114.6(6) . . ? Cl1 C15 H15A 108.6 . . ? Cl2 C15 H15A 108.6 . . ? Cl1 C15 H15B 108.6 . . ? Cl2 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.211 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.110 # Attachment 'f51222d-complex 8b.cif' data_f51222d _database_code_depnum_ccdc_archive 'CCDC 611980' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H59 B20 Cl3 Ir2 N4 O Se4' _chemical_formula_weight 1598.67 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 12.307(3) _cell_length_b 18.558(4) _cell_length_c 25.785(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.006(4) _cell_angle_gamma 90.00 _cell_volume 5881(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 918 _cell_measurement_theta_min 2.171 _cell_measurement_theta_max 20.725 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 7.168 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7158 _exptl_absorpt_correction_T_max 0.7158 _exptl_absorpt_process_details ? _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_% 7.81 _diffrn_reflns_number 24538 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1128 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10355 _reflns_number_gt 5819 _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^)+(0.0262P)^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 10355 _refine_ls_number_parameters 670 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 0.772 _refine_ls_restrained_S_all 0.772 _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 0.76856(3) 0.359713(16) 0.417288(13) 0.04353(10) Uani 1 1 d . . . Ir2 Ir 0.24596(3) -0.066318(18) 0.762812(14) 0.04876(11) Uani 1 1 d . . . Se2 Se 0.87828(7) 0.26862(5) 0.37394(3) 0.0562(3) Uani 1 1 d . . . Se1 Se 0.88565(7) 0.35110(5) 0.49765(4) 0.0601(3) Uani 1 1 d . . . Se4 Se 0.31834(7) -0.18682(4) 0.74148(4) 0.0534(2) Uani 1 1 d . . . Se3 Se 0.42226(7) -0.02998(5) 0.80348(4) 0.0633(3) Uani 1 1 d . . . N1 N 0.6690(5) 0.2748(3) 0.4429(3) 0.0423(16) Uani 1 1 d . . . N2 N 0.4160(5) 0.0578(4) 0.4622(3) 0.0532(19) Uani 1 1 d . . . N3 N 0.3618(5) 0.0151(3) 0.4972(3) 0.0526(19) Uani 1 1 d . . . N4 N 0.2937(5) -0.0307(3) 0.6891(3) 0.0468(17) Uani 1 1 d . . . O1 O 0.4336(4) 0.1067(3) 0.5396(2) 0.0527(15) Uani 1 1 d . . . C4 C 0.6290(7) 0.4310(5) 0.4011(4) 0.060(3) Uani 1 1 d . . . C5 C 0.6757(7) 0.4112(4) 0.3531(3) 0.048(2) Uani 1 1 d . . . C1 C 0.7812(7) 0.4373(5) 0.3548(4) 0.060(3) Uani 1 1 d . . . C2 C 0.8038(10) 0.4719(5) 0.4011(5) 0.083(4) Uani 1 1 d . . . C3 C 0.7111(12) 0.4688(5) 0.4317(4) 0.081(4) Uani 1 1 d . . . C9 C 0.5188(7) 0.4179(6) 0.4178(5) 0.144(6) Uani 1 1 d . . . H6A H 0.4743 0.4594 0.4101 0.216 Uiso 1 1 calc R . . H6B H 0.5216 0.4090 0.4545 0.216 Uiso 1 1 calc R . . H6C H 0.4884 0.3768 0.3998 0.216 Uiso 1 1 calc R . . C10 C 0.6144(9) 0.3770(5) 0.3088(4) 0.115(5) Uani 1 1 d . . . H7A H 0.5828 0.4136 0.2865 0.172 Uiso 1 1 calc R . . H7B H 0.5577 0.3472 0.3215 0.172 Uiso 1 1 calc R . . H7C H 0.6628 0.3478 0.2897 0.172 Uiso 1 1 calc R . . C6 C 0.8549(9) 0.4318(7) 0.3099(5) 0.160(7) Uani 1 1 d . . . H8A H 0.8696 0.4792 0.2971 0.240 Uiso 1 1 calc R . . H8B H 0.8199 0.4035 0.2827 0.240 Uiso 1 1 calc R . . H8C H 0.9220 0.4091 0.3214 0.240 Uiso 1 1 calc R . . C7 C 0.9124(9) 0.5113(5) 0.4141(6) 0.171(8) Uani 1 1 d . . . H9A H 0.9711 0.4844 0.4005 0.256 Uiso 1 1 calc R . . H9B H 0.9237 0.5157 0.4511 0.256 Uiso 1 1 calc R . . H9C H 0.9098 0.5585 0.3988 0.256 Uiso 1 1 calc R . . C8 C 0.7047(12) 0.5076(6) 0.4813(4) 0.172(7) Uani 1 1 d . . . H10A H 0.7708 0.5002 0.5021 0.258 Uiso 1 1 calc R . . H10B H 0.6442 0.4897 0.4995 0.258 Uiso 1 1 calc R . . H10C H 0.6951 0.5581 0.4746 0.258 Uiso 1 1 calc R . . C34 C 0.9890(6) 0.2405(4) 0.4264(4) 0.061(3) Uani 1 1 d . . . C33 C 0.9932(7) 0.2795(4) 0.4832(4) 0.063(3) Uani 1 1 d . . . C21 C 0.6228(7) 0.2276(4) 0.4090(3) 0.052(2) Uani 1 1 d . . . H13 H 0.6420 0.2299 0.3746 0.062 Uiso 1 1 calc R . . C22 C 0.5493(7) 0.1766(4) 0.4220(3) 0.057(2) Uani 1 1 d . . . H14 H 0.5160 0.1472 0.3967 0.068 Uiso 1 1 calc R . . C23 C 0.5250(6) 0.1693(4) 0.4732(3) 0.046(2) Uani 1 1 d . . . C24 C 0.5692(7) 0.2180(5) 0.5080(4) 0.067(3) Uani 1 1 d . . . H16 H 0.5508 0.2165 0.5425 0.081 Uiso 1 1 calc R . . C25 C 0.6407(7) 0.2690(5) 0.4920(4) 0.061(2) Uani 1 1 d . . . H17 H 0.6708 0.3011 0.5165 0.073 Uiso 1 1 calc R . . C26 C 0.4564(6) 0.1101(4) 0.4889(3) 0.045(2) Uani 1 1 d . . . C27 C 0.3744(6) 0.0455(4) 0.5416(4) 0.047(2) Uani 1 1 d . . . C28 C 0.3424(6) 0.0207(4) 0.5918(3) 0.048(2) Uani 1 1 d . . . C29 C 0.2792(6) -0.0396(4) 0.5965(3) 0.050(2) Uani 1 1 d . . . H21 H 0.2511 -0.0635 0.5671 0.060 Uiso 1 1 calc R . . C30 C 0.2582(6) -0.0637(4) 0.6444(3) 0.051(2) Uani 1 1 d . . . H22 H 0.2169 -0.1054 0.6469 0.061 Uiso 1 1 calc R . . C31 C 0.3512(7) 0.0304(4) 0.6831(4) 0.062(3) Uani 1 1 d . . . H23 H 0.3749 0.0559 0.7127 0.074 Uiso 1 1 calc R . . C32 C 0.3764(7) 0.0565(4) 0.6357(4) 0.062(3) Uani 1 1 d . . . H24 H 0.4166 0.0987 0.6334 0.075 Uiso 1 1 calc R . . C13 C 0.1621(7) -0.0450(6) 0.8330(4) 0.070(3) Uani 1 1 d . . . C14 C 0.1168(7) -0.1046(6) 0.8086(5) 0.070(3) Uani 1 1 d . . . C15 C 0.0683(7) -0.0834(7) 0.7590(5) 0.082(4) Uani 1 1 d . . . C11 C 0.0933(8) -0.0095(7) 0.7545(4) 0.082(3) Uani 1 1 d . . . C12 C 0.1467(8) 0.0152(6) 0.7986(4) 0.071(3) Uani 1 1 d . . . C18 C 0.2133(9) -0.0380(7) 0.8877(4) 0.132(5) Uani 1 1 d . . . H30A H 0.1579 -0.0268 0.9113 0.198 Uiso 1 1 calc R . . H30B H 0.2665 -0.0001 0.8886 0.198 Uiso 1 1 calc R . . H30C H 0.2478 -0.0826 0.8978 0.198 Uiso 1 1 calc R . . C19 C 0.1060(10) -0.1772(6) 0.8333(6) 0.174(7) Uani 1 1 d . . . H31A H 0.1646 -0.1841 0.8589 0.261 Uiso 1 1 calc R . . H31B H 0.1087 -0.2139 0.8072 0.261 Uiso 1 1 calc R . . H31C H 0.0378 -0.1799 0.8497 0.261 Uiso 1 1 calc R . . C20 C 0.0027(8) -0.1283(8) 0.7224(5) 0.178(8) Uani 1 1 d . . . H32A H -0.0725 -0.1253 0.7302 0.267 Uiso 1 1 calc R . . H32B H 0.0266 -0.1775 0.7253 0.267 Uiso 1 1 calc R . . H32C H 0.0113 -0.1116 0.6876 0.267 Uiso 1 1 calc R . . C16 C 0.0578(10) 0.0381(7) 0.7078(5) 0.174(7) Uani 1 1 d . . . H33A H 0.0834 0.0864 0.7138 0.261 Uiso 1 1 calc R . . H33B H -0.0202 0.0383 0.7035 0.261 Uiso 1 1 calc R . . H33C H 0.0879 0.0194 0.6770 0.261 Uiso 1 1 calc R . . C17 C 0.1804(10) 0.0927(6) 0.8104(5) 0.158(6) Uani 1 1 d . . . H34A H 0.1804 0.1197 0.7786 0.236 Uiso 1 1 calc R . . H34B H 0.2521 0.0933 0.8270 0.236 Uiso 1 1 calc R . . H34C H 0.1299 0.1141 0.8330 0.236 Uiso 1 1 calc R . . C36 C 0.4686(6) -0.1863(4) 0.7685(3) 0.052(2) Uani 1 1 d . . . C35 C 0.5159(6) -0.1126(4) 0.7983(3) 0.051(2) Uani 1 1 d . . . B3 B 1.0890(9) 0.3008(7) 0.4437(6) 0.090(5) Uani 1 1 d . . . H3 H 1.0971 0.3546 0.4265 0.108 Uiso 1 1 calc R . . B4 B 1.1151(9) 0.2206(7) 0.4086(6) 0.110(6) Uani 1 1 d . . . H4 H 1.1407 0.2215 0.3684 0.132 Uiso 1 1 calc R . . B5 B 1.0285(10) 0.1541(6) 0.4313(5) 0.088(4) Uani 1 1 d . . . H5 H 0.9971 0.1111 0.4053 0.106 Uiso 1 1 calc R . . B6 B 0.9502(10) 0.1903(5) 0.4767(5) 0.074(4) Uani 1 1 d . . . H6 H 0.8662 0.1717 0.4809 0.089 Uiso 1 1 calc R . . B7 B 1.1195(11) 0.2844(8) 0.5094(6) 0.113(6) Uani 1 1 d . . . H7 H 1.1472 0.3275 0.5362 0.135 Uiso 1 1 calc R . . B8 B 1.2024(11) 0.2475(9) 0.4625(8) 0.131(6) Uani 1 1 d . . . H8 H 1.2861 0.2659 0.4574 0.157 Uiso 1 1 calc R . . B9 B 1.1626(13) 0.1563(8) 0.4550(7) 0.137(7) Uani 1 1 d . . . H9 H 1.2202 0.1138 0.4451 0.164 Uiso 1 1 calc R . . B10 B 1.0609(13) 0.1394(7) 0.4975(6) 0.114(6) Uani 1 1 d . . . H10 H 1.0516 0.0867 0.5162 0.137 Uiso 1 1 calc R . . B11 B 1.0344(12) 0.2178(6) 0.5315(5) 0.096(5) Uani 1 1 d . . . H11 H 1.0066 0.2171 0.5714 0.115 Uiso 1 1 calc R . . B12 B 1.1696(15) 0.1979(10) 0.5153(8) 0.155(9) Uani 1 1 d . . . H12 H 1.2338 0.1839 0.5449 0.186 Uiso 1 1 calc R . . B13 B 0.5594(7) -0.1327(5) 0.7390(4) 0.055(3) Uani 1 1 d . . . H13A H 0.5396 -0.1006 0.7039 0.066 Uiso 1 1 calc R . . B14 B 0.5693(8) -0.2269(6) 0.7374(5) 0.071(3) Uani 1 1 d . . . H14A H 0.5565 -0.2567 0.7007 0.085 Uiso 1 1 calc R . . B15 B 0.5255(9) -0.2603(5) 0.7973(4) 0.065(3) Uani 1 1 d . . . H15 H 0.4831 -0.3123 0.7999 0.079 Uiso 1 1 calc R . . B16 B 0.4902(9) -0.1867(5) 0.8363(4) 0.063(3) Uani 1 1 d . . . H16A H 0.4253 -0.1899 0.8639 0.076 Uiso 1 1 calc R . . B17 B 0.6488(8) -0.1017(6) 0.7887(5) 0.068(3) Uani 1 1 d . . . H17A H 0.6889 -0.0490 0.7855 0.081 Uiso 1 1 calc R . . B18 B 0.6852(9) -0.1761(6) 0.7520(5) 0.085(4) Uani 1 1 d . . . H18 H 0.7511 -0.1734 0.7248 0.102 Uiso 1 1 calc R . . B19 B 0.6653(9) -0.2542(7) 0.7871(6) 0.090(4) Uani 1 1 d . . . H19 H 0.7160 -0.3025 0.7829 0.108 Uiso 1 1 calc R . . B20 B 0.6182(10) -0.2280(6) 0.8482(6) 0.091(4) Uani 1 1 d . . . H20 H 0.6386 -0.2591 0.8837 0.109 Uiso 1 1 calc R . . B21 B 0.6067(9) -0.1338(6) 0.8489(5) 0.074(4) Uani 1 1 d . . . H21A H 0.6178 -0.1023 0.8849 0.088 Uiso 1 1 calc R . . B22 B 0.7124(10) -0.1751(7) 0.8192(6) 0.090(4) Uani 1 1 d . . . H22A H 0.7958 -0.1709 0.8364 0.108 Uiso 1 1 calc R . . C37 C 0.2633(9) 0.9425(6) 0.3845(5) 0.105(4) Uani 1 1 d . . . H37 H 0.3153 0.9575 0.4125 0.126 Uiso 1 1 calc R . . Cl1 Cl 0.1362(4) 0.9415(3) 0.40777(19) 0.1940(19) Uani 1 1 d . . . Cl2 Cl 0.2676(4) 1.0016(3) 0.33652(19) 0.230(3) Uani 1 1 d . . . Cl3 Cl 0.2951(5) 0.8595(3) 0.3661(3) 0.280(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 Ir1 0.0488(2) 0.04172(18) 0.0401(2) 0.00122(16) 0.00271(16) 0.00750(16) Ir2 0.0499(2) 0.0537(2) 0.0430(2) -0.00272(18) 0.00463(17) -0.00172(18) Se2 0.0616(6) 0.0589(6) 0.0483(6) -0.0042(5) 0.0037(5) 0.0185(5) Se1 0.0702(6) 0.0606(6) 0.0483(6) -0.0097(5) -0.0093(5) 0.0161(5) Se4 0.0536(6) 0.0474(5) 0.0581(6) -0.0057(5) -0.0064(5) -0.0066(4) Se3 0.0637(6) 0.0539(6) 0.0710(7) -0.0197(5) -0.0086(5) -0.0027(5) N1 0.045(4) 0.047(4) 0.035(4) 0.000(3) 0.003(3) -0.001(3) N2 0.052(5) 0.058(5) 0.049(5) 0.007(4) 0.001(4) -0.004(4) N3 0.054(5) 0.052(5) 0.051(5) 0.003(4) -0.005(4) 0.005(4) N4 0.058(5) 0.044(4) 0.040(5) -0.001(3) 0.011(4) -0.006(3) O1 0.061(4) 0.047(3) 0.052(4) 0.008(3) 0.014(3) -0.002(3) C4 0.036(6) 0.050(6) 0.095(9) 0.026(6) 0.020(6) 0.017(4) C5 0.050(6) 0.036(5) 0.055(6) -0.001(4) -0.015(5) 0.008(4) C1 0.047(6) 0.052(6) 0.080(8) 0.033(6) 0.013(6) 0.015(5) C2 0.118(11) 0.033(6) 0.093(10) 0.013(6) -0.037(9) -0.002(6) C3 0.138(11) 0.071(7) 0.034(6) -0.001(5) -0.004(7) 0.067(8) C9 0.067(8) 0.157(11) 0.214(15) 0.135(11) 0.064(8) 0.052(7) C10 0.160(11) 0.055(6) 0.121(10) -0.013(6) -0.080(9) 0.012(7) C6 0.149(12) 0.171(13) 0.170(14) 0.118(11) 0.105(10) 0.078(10) C7 0.145(12) 0.068(8) 0.29(2) 0.048(10) -0.120(13) -0.039(8) C8 0.36(2) 0.103(9) 0.049(8) -0.027(7) -0.038(11) 0.117(12) C34 0.034(5) 0.052(6) 0.096(8) -0.013(5) 0.003(5) 0.006(4) C33 0.063(6) 0.059(6) 0.065(7) -0.015(5) -0.021(5) 0.007(5) C21 0.067(6) 0.054(6) 0.034(5) 0.006(5) 0.006(5) -0.004(5) C22 0.062(6) 0.063(6) 0.045(6) -0.004(5) -0.004(5) -0.001(5) C23 0.046(5) 0.049(5) 0.043(6) 0.012(5) 0.008(4) 0.013(4) C24 0.092(8) 0.065(6) 0.046(6) 0.002(5) 0.022(6) -0.011(6) C25 0.074(7) 0.059(6) 0.049(6) 0.002(5) 0.012(5) -0.003(5) C26 0.044(5) 0.051(5) 0.039(6) 0.011(5) 0.004(4) 0.007(4) C27 0.043(5) 0.041(5) 0.058(7) 0.012(5) 0.003(5) 0.003(4) C28 0.055(6) 0.037(5) 0.052(6) 0.002(5) 0.006(5) -0.001(4) C29 0.057(6) 0.050(5) 0.042(6) 0.003(4) 0.004(5) 0.004(4) C30 0.053(6) 0.049(5) 0.052(6) -0.014(5) 0.006(5) -0.004(4) C31 0.075(7) 0.045(5) 0.066(7) -0.021(5) 0.013(5) -0.017(5) C32 0.083(7) 0.038(5) 0.066(7) 0.009(5) 0.016(6) -0.012(5) C13 0.060(7) 0.110(9) 0.043(7) 0.004(6) 0.016(5) 0.004(6) C14 0.046(6) 0.074(7) 0.091(9) 0.009(7) 0.010(6) -0.001(5) C15 0.032(6) 0.133(11) 0.083(9) -0.053(8) 0.015(6) -0.024(6) C11 0.057(7) 0.128(11) 0.065(8) 0.009(8) 0.024(6) 0.022(7) C12 0.070(7) 0.083(8) 0.062(8) 0.002(7) 0.021(6) 0.003(6) C18 0.109(10) 0.234(15) 0.053(8) -0.014(9) 0.007(7) 0.004(9) C19 0.169(13) 0.087(9) 0.28(2) 0.070(11) 0.147(13) 0.018(8) C20 0.059(8) 0.316(19) 0.161(14) -0.153(14) 0.032(8) -0.070(10) C16 0.160(13) 0.278(18) 0.086(11) 0.084(11) 0.039(9) 0.139(13) C17 0.181(13) 0.088(10) 0.214(17) -0.036(10) 0.112(12) -0.001(9) C36 0.065(6) 0.047(5) 0.043(6) -0.002(4) -0.003(5) -0.007(4) C35 0.047(5) 0.056(5) 0.049(6) -0.008(5) -0.008(4) 0.003(4) B3 0.046(8) 0.078(9) 0.146(15) -0.036(9) 0.019(8) 0.001(6) B4 0.047(8) 0.116(12) 0.167(16) -0.068(11) 0.011(9) 0.014(8) B5 0.098(10) 0.068(8) 0.095(11) -0.021(8) -0.022(9) 0.033(8) B6 0.090(9) 0.048(7) 0.079(9) 0.001(6) -0.038(8) -0.001(6) B7 0.081(10) 0.129(13) 0.122(14) -0.037(11) -0.054(10) 0.026(10) B8 0.057(10) 0.142(15) 0.19(2) -0.053(15) -0.022(12) 0.021(10) B9 0.106(13) 0.127(14) 0.169(19) -0.053(13) -0.071(13) 0.073(11) B10 0.152(15) 0.074(9) 0.111(13) -0.010(9) -0.039(12) 0.054(10) B11 0.134(13) 0.074(9) 0.075(10) 0.006(8) -0.048(9) 0.024(9) B12 0.146(17) 0.138(15) 0.168(19) -0.066(14) -0.113(15) 0.086(13) B13 0.044(6) 0.062(7) 0.060(8) -0.006(6) 0.000(5) -0.008(5) B14 0.057(8) 0.069(8) 0.085(10) -0.038(7) 0.001(7) -0.004(6) B15 0.078(8) 0.042(6) 0.074(9) 0.005(6) -0.021(7) 0.001(6) B16 0.081(8) 0.057(7) 0.051(7) 0.008(6) -0.008(6) -0.016(6) B17 0.049(7) 0.073(8) 0.079(9) -0.013(7) -0.003(6) -0.010(6) B18 0.059(8) 0.085(9) 0.112(12) -0.027(8) 0.020(8) 0.002(7) B19 0.066(9) 0.075(9) 0.127(13) -0.016(9) -0.023(9) 0.017(7) B20 0.079(9) 0.077(9) 0.112(12) 0.004(8) -0.043(9) 0.003(8) B21 0.076(8) 0.070(8) 0.070(9) -0.012(7) -0.039(7) -0.009(7) B22 0.056(8) 0.092(9) 0.117(13) -0.028(9) -0.031(8) 0.012(7) C37 0.117(10) 0.120(10) 0.077(9) -0.032(8) -0.002(8) -0.038(8) Cl1 0.164(4) 0.261(5) 0.158(5) 0.011(4) 0.010(3) 0.001(4) Cl2 0.305(6) 0.246(5) 0.133(4) 0.057(4) -0.032(4) -0.124(5) Cl3 0.318(7) 0.204(5) 0.313(8) -0.070(5) -0.021(6) 0.120(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 N1 2.123(6) . ? Ir1 C1 2.171(8) . ? Ir1 C2 2.172(9) . ? Ir1 C5 2.181(8) . ? Ir1 C3 2.182(9) . ? Ir1 C4 2.190(8) . ? Ir1 Se1 2.4664(10) . ? Ir1 Se2 2.4676(9) . ? Ir2 N4 2.124(6) . ? Ir2 C14 2.150(10) . ? Ir2 C11 2.155(10) . ? Ir2 C13 2.166(9) . ? Ir2 C12 2.179(10) . ? Ir2 C15 2.206(9) . ? Ir2 Se3 2.4542(10) . ? Ir2 Se4 2.4795(10) . ? Se2 C34 1.941(9) . ? Se1 C33 1.926(8) . ? Se4 C36 1.942(8) . ? Se3 C35 1.928(8) . ? N1 C25 1.336(9) . ? N1 C21 1.342(9) . ? N2 C26 1.276(9) . ? N2 N3 1.397(9) . ? N3 C27 1.278(10) . ? N4 C31 1.350(9) . ? N4 C30 1.356(9) . ? O1 C26 1.352(9) . ? O1 C27 1.353(8) . ? C4 C3 1.431(13) . ? C4 C5 1.438(12) . ? C4 C9 1.465(11) . ? C5 C1 1.384(11) . ? C5 C10 1.480(11) . ? C1 C2 1.372(13) . ? C1 C6 1.512(13) . ? C2 C3 1.422(14) . ? C2 C7 1.544(13) . ? C3 C8 1.473(12) . ? C9 H6A 0.9600 . ? C9 H6B 0.9600 . ? C9 H6C 0.9600 . ? C10 H7A 0.9600 . ? C10 H7B 0.9600 . ? C10 H7C 0.9600 . ? C6 H8A 0.9600 . ? C6 H8B 0.9600 . ? C6 H8C 0.9600 . ? C7 H9A 0.9600 . ? C7 H9B 0.9600 . ? C7 H9C 0.9600 . ? C8 H10A 0.9600 . ? C8 H10B 0.9600 . ? C8 H10C 0.9600 . ? C34 C33 1.632(12) . ? C34 B5 1.677(13) . ? C34 B4 1.683(13) . ? C34 B6 1.686(14) . ? C34 B3 1.706(13) . ? C33 B3 1.646(15) . ? C33 B7 1.664(14) . ? C33 B6 1.744(12) . ? C33 B11 1.748(14) . ? C21 C22 1.364(10) . ? C21 H13 0.9300 . ? C22 C23 1.375(10) . ? C22 H14 0.9300 . ? C23 C24 1.366(10) . ? C23 C26 1.456(10) . ? C24 C25 1.370(10) . ? C24 H16 0.9300 . ? C25 H17 0.9300 . ? C27 C28 1.448(11) . ? C28 C32 1.358(11) . ? C28 C29 1.371(10) . ? C29 C30 1.351(10) . ? C29 H21 0.9300 . ? C30 H22 0.9300 . ? C31 C32 1.367(11) . ? C31 H23 0.9300 . ? C32 H24 0.9300 . ? C13 C14 1.375(12) . ? C13 C12 1.432(12) . ? C13 C18 1.522(12) . ? C14 C15 1.438(13) . ? C14 C19 1.499(12) . ? C15 C11 1.411(13) . ? C15 C20 1.470(12) . ? C11 C12 1.363(13) . ? C11 C16 1.539(13) . ? C12 C17 1.524(13) . ? C18 H30A 0.9600 . ? C18 H30B 0.9600 . ? C18 H30C 0.9600 . ? C19 H31A 0.9600 . ? C19 H31B 0.9600 . ? C19 H31C 0.9600 . ? C20 H32A 0.9600 . ? C20 H32B 0.9600 . ? C20 H32C 0.9600 . ? C16 H33A 0.9600 . ? C16 H33B 0.9600 . ? C16 H33C 0.9600 . ? C17 H34A 0.9600 . ? C17 H34B 0.9600 . ? C17 H34C 0.9600 . ? C36 C35 1.659(10) . ? C36 B14 1.687(13) . ? C36 B15 1.695(12) . ? C36 B13 1.705(12) . ? C36 B16 1.754(12) . ? C35 B17 1.678(12) . ? C35 B13 1.688(12) . ? C35 B21 1.717(12) . ? C35 B16 1.726(12) . ? B3 B7 1.744(19) . ? B3 B8 1.757(18) . ? B3 B4 1.779(16) . ? B3 H3 1.1000 . ? B4 B5 1.750(18) . ? B4 B9 1.77(2) . ? B4 B8 1.78(2) . ? B4 H4 1.1000 . ? B5 B6 1.695(17) . ? B5 B9 1.730(18) . ? B5 B10 1.755(18) . ? B5 H5 1.1000 . ? B6 B10 1.720(16) . ? B6 B11 1.783(15) . ? B6 H6 1.1000 . ? B7 B12 1.72(2) . ? B7 B11 1.734(19) . ? B7 B8 1.76(2) . ? B7 H7 1.1000 . ? B8 B12 1.71(2) . ? B8 B9 1.77(2) . ? B8 H8 1.1000 . ? B9 B12 1.73(2) . ? B9 B10 1.73(2) . ? B9 H9 1.1000 . ? B10 B11 1.739(18) . ? B10 B12 1.77(2) . ? B10 H10 1.1000 . ? B11 B12 1.78(2) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? B13 B17 1.743(14) . ? B13 B14 1.752(13) . ? B13 B18 1.762(14) . ? B13 H13A 1.1000 . ? B14 B18 1.734(14) . ? B14 B19 1.772(15) . ? B14 B15 1.775(15) . ? B14 H14A 1.1000 . ? B15 B19 1.759(16) . ? B15 B16 1.764(14) . ? B15 B20 1.795(15) . ? B15 H15 1.1000 . ? B16 B21 1.753(14) . ? B16 B20 1.764(15) . ? B16 H16A 1.1000 . ? B17 B22 1.739(16) . ? B17 B18 1.746(15) . ? B17 B21 1.764(16) . ? B17 H17A 1.1000 . ? B18 B19 1.732(17) . ? B18 B22 1.748(17) . ? B18 H18 1.1000 . ? B19 B22 1.768(16) . ? B19 B20 1.774(18) . ? B19 H19 1.1000 . ? B20 B22 1.719(18) . ? B20 B21 1.755(15) . ? B20 H20 1.1000 . ? B21 B22 1.723(16) . ? B21 H21A 1.1000 . ? B22 H22A 1.1000 . ? C37 Cl2 1.655(12) . ? C37 Cl3 1.664(11) . ? C37 Cl1 1.705(11) . ? C37 H37 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C1 142.0(3) . . ? N1 Ir1 C2 153.6(4) . . ? C1 Ir1 C2 36.8(3) . . ? N1 Ir1 C5 105.8(3) . . ? C1 Ir1 C5 37.1(3) . . ? C2 Ir1 C5 62.4(3) . . ? N1 Ir1 C3 116.0(4) . . ? C1 Ir1 C3 63.1(4) . . ? C2 Ir1 C3 38.1(4) . . ? C5 Ir1 C3 64.0(3) . . ? N1 Ir1 C4 92.8(3) . . ? C1 Ir1 C4 62.9(3) . . ? C2 Ir1 C4 63.1(4) . . ? C5 Ir1 C4 38.4(3) . . ? C3 Ir1 C4 38.2(3) . . ? N1 Ir1 Se1 90.69(17) . . ? C1 Ir1 Se1 127.2(3) . . ? C2 Ir1 Se1 96.3(3) . . ? C5 Ir1 Se1 157.7(2) . . ? C3 Ir1 Se1 95.6(3) . . ? C4 Ir1 Se1 128.1(3) . . ? N1 Ir1 Se2 88.34(17) . . ? C1 Ir1 Se2 93.2(3) . . ? C2 Ir1 Se2 116.8(4) . . ? C5 Ir1 Se2 103.5(2) . . ? C3 Ir1 Se2 154.5(4) . . ? C4 Ir1 Se2 140.3(3) . . ? Se1 Ir1 Se2 91.53(3) . . ? N4 Ir2 C14 147.3(4) . . ? N4 Ir2 C11 92.2(3) . . ? C14 Ir2 C11 63.3(4) . . ? N4 Ir2 C13 149.0(3) . . ? C14 Ir2 C13 37.1(3) . . ? C11 Ir2 C13 62.8(4) . . ? N4 Ir2 C12 110.5(3) . . ? C14 Ir2 C12 63.2(4) . . ? C11 Ir2 C12 36.6(3) . . ? C13 Ir2 C12 38.5(3) . . ? N4 Ir2 C15 108.9(4) . . ? C14 Ir2 C15 38.5(4) . . ? C11 Ir2 C15 37.7(4) . . ? C13 Ir2 C15 63.2(4) . . ? C12 Ir2 C15 62.8(4) . . ? N4 Ir2 Se3 90.99(17) . . ? C14 Ir2 Se3 121.2(3) . . ? C11 Ir2 Se3 130.9(4) . . ? C13 Ir2 Se3 92.4(3) . . ? C12 Ir2 Se3 97.5(3) . . ? C15 Ir2 Se3 155.5(3) . . ? N4 Ir2 Se4 87.86(17) . . ? C14 Ir2 Se4 96.2(3) . . ? C11 Ir2 Se4 137.8(4) . . ? C13 Ir2 Se4 122.9(3) . . ? C12 Ir2 Se4 159.3(3) . . ? C15 Ir2 Se4 103.1(3) . . ? Se3 Ir2 Se4 91.30(3) . . ? C34 Se2 Ir1 104.4(3) . . ? C33 Se1 Ir1 105.0(3) . . ? C36 Se4 Ir2 105.2(2) . . ? C35 Se3 Ir2 105.7(2) . . ? C25 N1 C21 116.3(7) . . ? C25 N1 Ir1 122.6(6) . . ? C21 N1 Ir1 120.9(6) . . ? C26 N2 N3 105.5(7) . . ? C27 N3 N2 106.8(7) . . ? C31 N4 C30 115.4(7) . . ? C31 N4 Ir2 122.3(6) . . ? C30 N4 Ir2 121.9(5) . . ? C26 O1 C27 102.5(7) . . ? C3 C4 C5 107.3(8) . . ? C3 C4 C9 123.8(12) . . ? C5 C4 C9 128.9(11) . . ? C3 C4 Ir1 70.6(5) . . ? C5 C4 Ir1 70.4(4) . . ? C9 C4 Ir1 124.9(6) . . ? C1 C5 C4 107.4(8) . . ? C1 C5 C10 127.9(10) . . ? C4 C5 C10 124.3(9) . . ? C1 C5 Ir1 71.1(5) . . ? C4 C5 Ir1 71.1(5) . . ? C10 C5 Ir1 128.6(6) . . ? C2 C1 C5 109.8(9) . . ? C2 C1 C6 126.6(11) . . ? C5 C1 C6 123.5(11) . . ? C2 C1 Ir1 71.6(6) . . ? C5 C1 Ir1 71.8(5) . . ? C6 C1 Ir1 126.4(6) . . ? C1 C2 C3 109.3(10) . . ? C1 C2 C7 123.0(13) . . ? C3 C2 C7 127.6(13) . . ? C1 C2 Ir1 71.6(5) . . ? C3 C2 Ir1 71.3(6) . . ? C7 C2 Ir1 126.3(7) . . ? C2 C3 C4 106.1(9) . . ? C2 C3 C8 122.8(14) . . ? C4 C3 C8 130.6(13) . . ? C2 C3 Ir1 70.5(5) . . ? C4 C3 Ir1 71.2(5) . . ? C8 C3 Ir1 129.3(7) . . ? C4 C9 H6A 109.5 . . ? C4 C9 H6B 109.5 . . ? H6A C9 H6B 109.5 . . ? C4 C9 H6C 109.5 . . ? H6A C9 H6C 109.5 . . ? H6B C9 H6C 109.5 . . ? C5 C10 H7A 109.5 . . ? C5 C10 H7B 109.5 . . ? H7A C10 H7B 109.5 . . ? C5 C10 H7C 109.5 . . ? H7A C10 H7C 109.5 . . ? H7B C10 H7C 109.5 . . ? C1 C6 H8A 109.5 . . ? C1 C6 H8B 109.5 . . ? H8A C6 H8B 109.5 . . ? C1 C6 H8C 109.5 . . ? H8A C6 H8C 109.5 . . ? H8B C6 H8C 109.5 . . ? C2 C7 H9A 109.5 . . ? C2 C7 H9B 109.5 . . ? H9A C7 H9B 109.5 . . ? C2 C7 H9C 109.5 . . ? H9A C7 H9C 109.5 . . ? H9B C7 H9C 109.5 . . ? C3 C8 H10A 109.5 . . ? C3 C8 H10B 109.5 . . ? H10A C8 H10B 109.5 . . ? C3 C8 H10C 109.5 . . ? H10A C8 H10C 109.5 . . ? H10B C8 H10C 109.5 . . ? C33 C34 B5 111.2(8) . . ? C33 C34 B4 110.8(7) . . ? B5 C34 B4 62.8(7) . . ? C33 C34 B6 63.4(6) . . ? B5 C34 B6 60.5(7) . . ? B4 C34 B6 113.0(9) . . ? C33 C34 B3 59.0(6) . . ? B5 C34 B3 113.9(7) . . ? B4 C34 B3 63.3(6) . . ? B6 C34 B3 113.0(8) . . ? C33 C34 Se2 119.6(5) . . ? B5 C34 Se2 120.0(6) . . ? B4 C34 Se2 119.5(8) . . ? B6 C34 Se2 117.9(6) . . ? B3 C34 Se2 118.4(7) . . ? C34 C33 B3 62.7(6) . . ? C34 C33 B7 112.0(8) . . ? B3 C33 B7 63.6(8) . . ? C34 C33 B6 59.8(6) . . ? B3 C33 B6 113.1(8) . . ? B7 C33 B6 111.3(8) . . ? C34 C33 B11 110.1(7) . . ? B3 C33 B11 114.1(9) . . ? B7 C33 B11 61.1(7) . . ? B6 C33 B11 61.4(6) . . ? C34 C33 Se1 119.3(5) . . ? B3 C33 Se1 118.4(7) . . ? B7 C33 Se1 121.4(7) . . ? B6 C33 Se1 117.7(6) . . ? B11 C33 Se1 119.3(7) . . ? N1 C21 C22 123.7(8) . . ? N1 C21 H13 118.1 . . ? C22 C21 H13 118.1 . . ? C21 C22 C23 119.0(8) . . ? C21 C22 H14 120.5 . . ? C23 C22 H14 120.5 . . ? C24 C23 C22 117.8(8) . . ? C24 C23 C26 122.2(8) . . ? C22 C23 C26 120.0(8) . . ? C23 C24 C25 119.9(9) . . ? C23 C24 H16 120.0 . . ? C25 C24 H16 120.0 . . ? N1 C25 C24 122.9(8) . . ? N1 C25 H17 118.5 . . ? C24 C25 H17 118.5 . . ? N2 C26 O1 113.1(7) . . ? N2 C26 C23 129.7(9) . . ? O1 C26 C23 117.2(8) . . ? N3 C27 O1 112.1(8) . . ? N3 C27 C28 129.4(8) . . ? O1 C27 C28 118.3(8) . . ? C32 C28 C29 118.5(8) . . ? C32 C28 C27 120.1(8) . . ? C29 C28 C27 121.4(8) . . ? C30 C29 C28 119.2(8) . . ? C30 C29 H21 120.4 . . ? C28 C29 H21 120.4 . . ? C29 C30 N4 124.0(8) . . ? C29 C30 H22 118.0 . . ? N4 C30 H22 118.0 . . ? N4 C31 C32 123.0(8) . . ? N4 C31 H23 118.5 . . ? C32 C31 H23 118.5 . . ? C28 C32 C31 119.8(8) . . ? C28 C32 H24 120.1 . . ? C31 C32 H24 120.1 . . ? C14 C13 C12 107.9(9) . . ? C14 C13 C18 129.1(11) . . ? C12 C13 C18 122.8(11) . . ? C14 C13 Ir2 70.8(6) . . ? C12 C13 Ir2 71.2(6) . . ? C18 C13 Ir2 126.8(7) . . ? C13 C14 C15 109.0(9) . . ? C13 C14 C19 124.8(12) . . ? C15 C14 C19 125.6(12) . . ? C13 C14 Ir2 72.1(6) . . ? C15 C14 Ir2 72.9(6) . . ? C19 C14 Ir2 127.9(7) . . ? C11 C15 C14 104.9(9) . . ? C11 C15 C20 127.8(14) . . ? C14 C15 C20 127.3(14) . . ? C11 C15 Ir2 69.1(5) . . ? C14 C15 Ir2 68.6(5) . . ? C20 C15 Ir2 128.3(7) . . ? C12 C11 C15 110.8(10) . . ? C12 C11 C16 124.4(13) . . ? C15 C11 C16 124.7(13) . . ? C12 C11 Ir2 72.6(6) . . ? C15 C11 Ir2 73.1(6) . . ? C16 C11 Ir2 124.7(7) . . ? C11 C12 C13 107.3(10) . . ? C11 C12 C17 126.7(12) . . ? C13 C12 C17 126.0(11) . . ? C11 C12 Ir2 70.7(6) . . ? C13 C12 Ir2 70.3(6) . . ? C17 C12 Ir2 126.0(7) . . ? C13 C18 H30A 109.5 . . ? C13 C18 H30B 109.5 . . ? H30A C18 H30B 109.5 . . ? C13 C18 H30C 109.5 . . ? H30A C18 H30C 109.5 . . ? H30B C18 H30C 109.5 . . ? C14 C19 H31A 109.5 . . ? C14 C19 H31B 109.5 . . ? H31A C19 H31B 109.5 . . ? C14 C19 H31C 109.5 . . ? H31A C19 H31C 109.5 . . ? H31B C19 H31C 109.5 . . ? C15 C20 H32A 109.5 . . ? C15 C20 H32B 109.5 . . ? H32A C20 H32B 109.5 . . ? C15 C20 H32C 109.5 . . ? H32A C20 H32C 109.5 . . ? H32B C20 H32C 109.5 . . ? C11 C16 H33A 109.5 . . ? C11 C16 H33B 109.5 . . ? H33A C16 H33B 109.5 . . ? C11 C16 H33C 109.5 . . ? H33A C16 H33C 109.5 . . ? H33B C16 H33C 109.5 . . ? C12 C17 H34A 109.5 . . ? C12 C17 H34B 109.5 . . ? H34A C17 H34B 109.5 . . ? C12 C17 H34C 109.5 . . ? H34A C17 H34C 109.5 . . ? H34B C17 H34C 109.5 . . ? C35 C36 B14 109.8(6) . . ? C35 C36 B15 109.8(6) . . ? B14 C36 B15 63.3(6) . . ? C35 C36 B13 60.2(5) . . ? B14 C36 B13 62.2(6) . . ? B15 C36 B13 113.8(7) . . ? C35 C36 B16 60.7(5) . . ? B14 C36 B16 113.3(7) . . ? B15 C36 B16 61.5(6) . . ? B13 C36 B16 112.2(6) . . ? C35 C36 Se4 118.3(5) . . ? B14 C36 Se4 122.4(6) . . ? B15 C36 Se4 121.1(6) . . ? B13 C36 Se4 118.4(6) . . ? B16 C36 Se4 116.7(6) . . ? C36 C35 B17 110.7(7) . . ? C36 C35 B13 61.2(5) . . ? B17 C35 B13 62.4(6) . . ? C36 C35 B21 111.2(6) . . ? B17 C35 B21 62.6(6) . . ? B13 C35 B21 114.4(7) . . ? C36 C35 B16 62.4(5) . . ? B17 C35 B16 112.9(7) . . ? B13 C35 B16 114.5(7) . . ? B21 C35 B16 61.2(6) . . ? C36 C35 Se3 119.4(5) . . ? B17 C35 Se3 120.3(6) . . ? B13 C35 Se3 117.2(6) . . ? B21 C35 Se3 119.8(6) . . ? B16 C35 Se3 117.8(6) . . ? C33 B3 C34 58.2(6) . . ? C33 B3 B7 58.7(8) . . ? C34 B3 B7 104.7(10) . . ? C33 B3 B8 106.1(11) . . ? C34 B3 B8 104.7(9) . . ? B7 B3 B8 60.4(9) . . ? C33 B3 B4 105.5(9) . . ? C34 B3 B4 57.7(6) . . ? B7 B3 B4 108.2(10) . . ? B8 B3 B4 60.5(7) . . ? C33 B3 H3 123.5 . . ? C34 B3 H3 124.8 . . ? B7 B3 H3 122.1 . . ? B8 B3 H3 122.3 . . ? B4 B3 H3 122.1 . . ? C34 B4 B5 58.4(6) . . ? C34 B4 B9 103.9(12) . . ? B5 B4 B9 58.9(9) . . ? C34 B4 B3 59.0(6) . . ? B5 B4 B3 106.9(9) . . ? B9 B4 B3 106.4(11) . . ? C34 B4 B8 104.6(10) . . ? B5 B4 B8 106.9(12) . . ? B9 B4 B8 59.8(9) . . ? B3 B4 B8 59.1(8) . . ? C34 B4 H4 124.6 . . ? B5 B4 H4 122.3 . . ? B9 B4 H4 123.3 . . ? B3 B4 H4 122.3 . . ? B8 B4 H4 122.7 . . ? C34 B5 B6 60.0(6) . . ? C34 B5 B9 105.8(9) . . ? B6 B5 B9 108.2(10) . . ? C34 B5 B4 58.8(6) . . ? B6 B5 B4 109.3(9) . . ? B9 B5 B4 61.0(9) . . ? C34 B5 B10 105.7(9) . . ? B6 B5 B10 59.8(8) . . ? B9 B5 B10 59.7(8) . . ? B4 B5 B10 108.8(10) . . ? C34 B5 H5 123.9 . . ? B6 B5 H5 120.9 . . ? B9 B5 H5 122.1 . . ? B4 B5 H5 120.7 . . ? B10 B5 H5 122.3 . . ? C34 B6 B5 59.5(7) . . ? C34 B6 B10 106.9(10) . . ? B5 B6 B10 61.8(8) . . ? C34 B6 C33 56.8(5) . . ? B5 B6 C33 105.1(9) . . ? B10 B6 C33 105.0(8) . . ? C34 B6 B11 106.0(8) . . ? B5 B6 B11 109.5(9) . . ? B10 B6 B11 59.5(7) . . ? C33 B6 B11 59.4(6) . . ? C34 B6 H6 123.6 . . ? B5 B6 H6 121.0 . . ? B10 B6 H6 122.1 . . ? C33 B6 H6 124.8 . . ? B11 B6 H6 121.5 . . ? C33 B7 B12 108.0(11) . . ? C33 B7 B11 61.9(7) . . ? B12 B7 B11 61.8(10) . . ? C33 B7 B3 57.7(6) . . ? B12 B7 B3 107.9(11) . . ? B11 B7 B3 110.0(10) . . ? C33 B7 B8 105.2(10) . . ? B12 B7 B8 58.8(9) . . ? B11 B7 B8 109.3(11) . . ? B3 B7 B8 60.2(9) . . ? C33 B7 H7 123.2 . . ? B12 B7 H7 121.6 . . ? B11 B7 H7 119.0 . . ? B3 B7 H7 121.8 . . ? B8 B7 H7 122.8 . . ? B12 B8 B3 107.8(11) . . ? B12 B8 B7 59.5(10) . . ? B3 B8 B7 59.4(7) . . ? B12 B8 B9 59.8(10) . . ? B3 B8 B9 107.3(10) . . ? B7 B8 B9 106.2(13) . . ? B12 B8 B4 108.2(12) . . ? B3 B8 B4 60.4(7) . . ? B7 B8 B4 107.3(9) . . ? B9 B8 B4 59.7(8) . . ? B12 B8 H8 121.6 . . ? B3 B8 H8 121.8 . . ? B7 B8 H8 122.8 . . ? B9 B8 H8 122.6 . . ? B4 B8 H8 121.6 . . ? B5 B9 B12 109.3(12) . . ? B5 B9 B10 60.9(9) . . ? B12 B9 B10 61.2(12) . . ? B5 B9 B4 60.1(7) . . ? B12 B9 B4 107.8(11) . . ? B10 B9 B4 109.0(10) . . ? B5 B9 B8 108.3(10) . . ? B12 B9 B8 58.4(9) . . ? B10 B9 B8 108.0(12) . . ? B4 B9 B8 60.5(9) . . ? B5 B9 H9 121.0 . . ? B12 B9 H9 121.7 . . ? B10 B9 H9 120.8 . . ? B4 B9 H9 121.4 . . ? B8 B9 H9 122.3 . . ? B6 B10 B9 106.9(11) . . ? B6 B10 B11 62.1(7) . . ? B9 B10 B11 109.1(12) . . ? B6 B10 B5 58.4(7) . . ? B9 B10 B5 59.4(9) . . ? B11 B10 B5 108.8(9) . . ? B6 B10 B12 108.7(9) . . ? B9 B10 B12 59.4(10) . . ? B11 B10 B12 60.9(8) . . ? B5 B10 B12 106.7(13) . . ? B6 B10 H10 121.7 . . ? B9 B10 H10 122.2 . . ? B11 B10 H10 119.8 . . ? B5 B10 H10 122.8 . . ? B12 B10 H10 121.9 . . ? B7 B11 B10 107.3(12) . . ? B7 B11 C33 57.1(6) . . ? B10 B11 C33 104.1(9) . . ? B7 B11 B12 58.8(9) . . ? B10 B11 B12 60.3(9) . . ? C33 B11 B12 102.0(11) . . ? B7 B11 B6 106.2(10) . . ? B10 B11 B6 58.4(7) . . ? C33 B11 B6 59.2(5) . . ? B12 B11 B6 105.5(10) . . ? B7 B11 H11 122.6 . . ? B10 B11 H11 122.4 . . ? C33 B11 H11 125.6 . . ? B12 B11 H11 124.0 . . ? B6 B11 H11 122.7 . . ? B8 B12 B7 61.7(10) . . ? B8 B12 B9 61.8(11) . . ? B7 B12 B9 109.5(13) . . ? B8 B12 B10 109.3(11) . . ? B7 B12 B10 106.6(10) . . ? B9 B12 B10 59.4(9) . . ? B8 B12 B11 109.8(10) . . ? B7 B12 B11 59.4(8) . . ? B9 B12 B11 107.5(10) . . ? B10 B12 B11 58.8(9) . . ? B8 B12 H12 119.3 . . ? B7 B12 H12 121.5 . . ? B9 B12 H12 121.1 . . ? B10 B12 H12 122.8 . . ? B11 B12 H12 122.2 . . ? C35 B13 C36 58.5(5) . . ? C35 B13 B17 58.5(6) . . ? C36 B13 B17 105.5(8) . . ? C35 B13 B14 105.5(7) . . ? C36 B13 B14 58.4(5) . . ? B17 B13 B14 107.7(8) . . ? C35 B13 B18 104.2(8) . . ? C36 B13 B18 103.8(7) . . ? B17 B13 B18 59.8(6) . . ? B14 B13 B18 59.2(6) . . ? C35 B13 H13A 123.9 . . ? C36 B13 H13A 124.2 . . ? B17 B13 H13A 122.0 . . ? B14 B13 H13A 122.3 . . ? B18 B13 H13A 124.0 . . ? C36 B14 B18 105.7(7) . . ? C36 B14 B13 59.4(5) . . ? B18 B14 B13 60.7(6) . . ? C36 B14 B19 105.2(8) . . ? B18 B14 B19 59.2(6) . . ? B13 B14 B19 108.2(7) . . ? C36 B14 B15 58.5(6) . . ? B18 B14 B15 106.6(8) . . ? B13 B14 B15 107.7(7) . . ? B19 B14 B15 59.5(7) . . ? C36 B14 H14A 123.9 . . ? B18 B14 H14A 122.6 . . ? B13 B14 H14A 121.0 . . ? B19 B14 H14A 122.5 . . ? B15 B14 H14A 122.5 . . ? C36 B15 B19 105.5(8) . . ? C36 B15 B16 60.9(5) . . ? B19 B15 B16 107.9(8) . . ? C36 B15 B14 58.1(5) . . ? B19 B15 B14 60.2(7) . . ? B16 B15 B14 108.6(7) . . ? C36 B15 B20 106.3(7) . . ? B19 B15 B20 59.9(7) . . ? B16 B15 B20 59.4(6) . . ? B14 B15 B20 108.0(8) . . ? C36 B15 H15 123.4 . . ? B19 B15 H15 122.4 . . ? B16 B15 H15 121.0 . . ? B14 B15 H15 121.7 . . ? B20 B15 H15 122.3 . . ? C35 B16 B21 59.2(5) . . ? C35 B16 C36 56.9(5) . . ? B21 B16 C36 105.2(7) . . ? C35 B16 B20 104.9(8) . . ? B21 B16 B20 59.9(6) . . ? C36 B16 B20 105.2(8) . . ? C35 B16 B15 103.6(8) . . ? B21 B16 B15 108.5(8) . . ? C36 B16 B15 57.6(5) . . ? B20 B16 B15 61.2(6) . . ? C35 B16 H16A 124.9 . . ? B21 B16 H16A 121.6 . . ? C36 B16 H16A 124.7 . . ? B20 B16 H16A 122.4 . . ? B15 B16 H16A 122.4 . . ? C35 B17 B22 104.9(8) . . ? C35 B17 B13 59.1(5) . . ? B22 B17 B13 109.0(8) . . ? C35 B17 B18 105.3(7) . . ? B22 B17 B18 60.2(7) . . ? B13 B17 B18 60.6(6) . . ? C35 B17 B21 59.8(6) . . ? B22 B17 B21 58.9(7) . . ? B13 B17 B21 109.4(7) . . ? B18 B17 B21 107.8(9) . . ? C35 B17 H17A 124.2 . . ? B22 B17 H17A 122.5 . . ? B13 B17 H17A 120.4 . . ? B18 B17 H17A 122.2 . . ? B21 B17 H17A 121.3 . . ? B19 B18 B14 61.5(7) . . ? B19 B18 B17 109.3(10) . . ? B14 B18 B17 108.4(8) . . ? B19 B18 B22 61.0(7) . . ? B14 B18 B22 109.5(9) . . ? B17 B18 B22 59.7(7) . . ? B19 B18 B13 109.6(8) . . ? B14 B18 B13 60.1(6) . . ? B17 B18 B13 59.6(6) . . ? B22 B18 B13 107.7(8) . . ? B19 B18 H18 120.0 . . ? B14 B18 H18 120.8 . . ? B17 B18 H18 121.8 . . ? B22 B18 H18 121.5 . . ? B13 B18 H18 121.8 . . ? B18 B19 B15 107.4(8) . . ? B18 B19 B22 59.9(7) . . ? B15 B19 B22 106.4(9) . . ? B18 B19 B14 59.3(7) . . ? B15 B19 B14 60.4(6) . . ? B22 B19 B14 106.9(8) . . ? B18 B19 B20 107.2(9) . . ? B15 B19 B20 61.1(7) . . ? B22 B19 B20 58.1(7) . . ? B14 B19 B20 109.1(8) . . ? B18 B19 H19 122.2 . . ? B15 B19 H19 121.8 . . ? B22 B19 H19 123.3 . . ? B14 B19 H19 121.5 . . ? B20 B19 H19 121.6 . . ? B22 B20 B21 59.5(7) . . ? B22 B20 B16 107.0(8) . . ? B21 B20 B16 59.7(6) . . ? B22 B20 B19 60.8(8) . . ? B21 B20 B19 108.2(10) . . ? B16 B20 B19 107.2(8) . . ? B22 B20 B15 106.9(10) . . ? B21 B20 B15 107.0(8) . . ? B16 B20 B15 59.4(6) . . ? B19 B20 B15 59.0(7) . . ? B22 B20 H20 122.1 . . ? B21 B20 H20 121.9 . . ? B16 B20 H20 122.4 . . ? B19 B20 H20 121.6 . . ? B15 B20 H20 122.8 . . ? C35 B21 B22 103.9(8) . . ? C35 B21 B16 59.6(5) . . ? B22 B21 B16 107.3(8) . . ? C35 B21 B20 105.6(7) . . ? B22 B21 B20 59.2(7) . . ? B16 B21 B20 60.4(6) . . ? C35 B21 B17 57.6(5) . . ? B22 B21 B17 59.8(7) . . ? B16 B21 B17 107.5(7) . . ? B20 B21 B17 107.4(9) . . ? C35 B21 H21A 124.6 . . ? B22 B21 H21A 123.2 . . ? B16 B21 H21A 121.3 . . ? B20 B21 H21A 122.2 . . ? B17 B21 H21A 122.2 . . ? B20 B22 B21 61.3(7) . . ? B20 B22 B17 110.2(8) . . ? B21 B22 B17 61.3(6) . . ? B20 B22 B18 109.0(9) . . ? B21 B22 B18 109.6(8) . . ? B17 B22 B18 60.1(7) . . ? B20 B22 B19 61.2(7) . . ? B21 B22 B19 109.9(9) . . ? B17 B22 B19 108.1(8) . . ? B18 B22 B19 59.0(7) . . ? B20 B22 H22A 120.2 . . ? B21 B22 H22A 120.0 . . ? B17 B22 H22A 121.0 . . ? B18 B22 H22A 121.8 . . ? B19 B22 H22A 121.6 . . ? Cl2 C37 Cl3 112.5(8) . . ? Cl2 C37 Cl1 109.6(7) . . ? Cl3 C37 Cl1 108.9(7) . . ? Cl2 C37 H37 108.6 . . ? Cl3 C37 H37 108.6 . . ? Cl1 C37 H37 108.6 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.528 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.125 # Attachment 'f60222c-complex 8a.cif' data_f60222c _database_code_depnum_ccdc_archive 'CCDC 611981' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H60 B20 Cl2 Ir2 N4 O S4' _chemical_formula_weight 1376.63 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 12.197(4) _cell_length_b 18.310(5) _cell_length_c 25.776(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.502(5) _cell_angle_gamma 90.00 _cell_volume 5739(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 850 _cell_measurement_theta_min 2.640 _cell_measurement_theta_max 20.348 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 4.906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6397 _exptl_absorpt_correction_T_max 0.7915 _exptl_absorpt_process_details ? _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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.10 _diffrn_reflns_number 23918 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.1122 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10104 _reflns_number_gt 5823 _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^)+(0.0130P)^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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10104 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0544 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 0.708 _refine_ls_restrained_S_all 0.708 _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 0.22046(2) 0.363378(13) 1.080361(9) 0.04150(8) Uani 1 1 d . . . Ir2 Ir 0.74018(2) -0.072253(14) 0.740288(9) 0.04604(8) Uani 1 1 d . . . S1 S 0.11420(15) 0.35112(9) 1.00017(6) 0.0551(5) Uani 1 1 d . . . S2 S 0.11925(15) 0.26824(9) 1.11637(6) 0.0562(5) Uani 1 1 d . . . S3 S 0.56806(15) -0.03809(8) 0.70058(6) 0.0535(5) Uani 1 1 d . . . S4 S 0.66880(14) -0.18755(8) 0.76163(6) 0.0502(5) Uani 1 1 d . . . N1 N 0.3301(4) 0.2823(2) 1.05720(19) 0.0419(13) Uani 1 1 d . . . N2 N 0.5852(4) 0.0632(3) 1.03978(18) 0.0498(14) Uani 1 1 d . . . N3 N 0.6353(4) 0.0168(3) 1.0048(2) 0.0470(14) Uani 1 1 d . . . N4 N 0.6935(4) -0.0348(3) 0.81229(18) 0.0392(13) Uani 1 1 d . . . O1 O 0.5645(3) 0.1107(2) 0.96125(15) 0.0458(11) Uani 1 1 d . . . C1 C 0.2032(6) 0.4355(3) 1.1467(2) 0.0533(18) Uani 1 1 d . . . C2 C 0.1673(6) 0.4716(4) 1.1005(3) 0.064(2) Uani 1 1 d . . . C3 C 0.2571(7) 0.4786(3) 1.0698(2) 0.058(2) Uani 1 1 d . . . C4 C 0.3490(6) 0.4438(3) 1.0965(3) 0.0490(18) Uani 1 1 d . . . C5 C 0.3149(6) 0.4165(3) 1.1449(2) 0.0450(17) Uani 1 1 d . . . C6 C 0.1347(6) 0.4212(4) 1.1917(3) 0.106(3) Uani 1 1 d . . . H6A H 0.1385 0.4626 1.2146 0.159 Uiso 1 1 calc R . . H6B H 0.1622 0.3788 1.2104 0.159 Uiso 1 1 calc R . . H6C H 0.0597 0.4131 1.1789 0.159 Uiso 1 1 calc R . . C7 C 0.0549(6) 0.5058(4) 1.0887(3) 0.126(4) Uani 1 1 d . . . H7A H -0.0009 0.4697 1.0923 0.188 Uiso 1 1 calc R . . H7B H 0.0491 0.5243 1.0537 0.188 Uiso 1 1 calc R . . H7C H 0.0455 0.5452 1.1126 0.188 Uiso 1 1 calc R . . C8 C 0.2598(8) 0.5195(4) 1.0187(2) 0.125(4) Uani 1 1 d . . . H8A H 0.2752 0.5702 1.0256 0.187 Uiso 1 1 calc R . . H8B H 0.1897 0.5151 0.9992 0.187 Uiso 1 1 calc R . . H8C H 0.3160 0.4993 0.9990 0.187 Uiso 1 1 calc R . . C9 C 0.4629(6) 0.4394(4) 1.0790(3) 0.098(3) Uani 1 1 d . . . H9A H 0.4592 0.4335 1.0419 0.147 Uiso 1 1 calc R . . H9B H 0.5005 0.3984 1.0954 0.147 Uiso 1 1 calc R . . H9C H 0.5021 0.4834 1.0886 0.147 Uiso 1 1 calc R . . C10 C 0.3845(6) 0.3828(3) 1.1881(2) 0.083(3) Uani 1 1 d . . . H10A H 0.4095 0.4199 1.2126 0.125 Uiso 1 1 calc R . . H10B H 0.4468 0.3596 1.1745 0.125 Uiso 1 1 calc R . . H10C H 0.3424 0.3471 1.2053 0.125 Uiso 1 1 calc R . . C11 C 0.8925(6) -0.0082(5) 0.7451(3) 0.065(2) Uani 1 1 d . . . C12 C 0.8317(6) 0.0054(5) 0.6976(3) 0.073(2) Uani 1 1 d . . . C13 C 0.8206(6) -0.0610(6) 0.6703(3) 0.074(3) Uani 1 1 d . . . C14 C 0.8762(7) -0.1153(4) 0.7002(4) 0.077(2) Uani 1 1 d . . . C15 C 0.9188(6) -0.0824(5) 0.7481(3) 0.062(2) Uani 1 1 d . . . C16 C 0.9217(7) 0.0488(4) 0.7862(3) 0.129(4) Uani 1 1 d . . . H16A H 0.9602 0.0261 0.8159 0.194 Uiso 1 1 calc R . . H16B H 0.8556 0.0712 0.7966 0.194 Uiso 1 1 calc R . . H16C H 0.9677 0.0854 0.7724 0.194 Uiso 1 1 calc R . . C17 C 0.7926(7) 0.0799(4) 0.6778(4) 0.156(4) Uani 1 1 d . . . H17A H 0.7972 0.1142 0.7061 0.235 Uiso 1 1 calc R . . H17B H 0.7177 0.0765 0.6635 0.235 Uiso 1 1 calc R . . H17C H 0.8381 0.0962 0.6514 0.235 Uiso 1 1 calc R . . C18 C 0.7704(7) -0.0676(6) 0.6149(3) 0.177(5) Uani 1 1 d . . . H18A H 0.8152 -0.0418 0.5920 0.265 Uiso 1 1 calc R . . H18B H 0.6978 -0.0471 0.6125 0.265 Uiso 1 1 calc R . . H18C H 0.7664 -0.1182 0.6052 0.265 Uiso 1 1 calc R . . C19 C 0.8913(7) -0.1929(4) 0.6843(4) 0.199(6) Uani 1 1 d . . . H19A H 0.8297 -0.2079 0.6612 0.298 Uiso 1 1 calc R . . H19B H 0.8963 -0.2235 0.7146 0.298 Uiso 1 1 calc R . . H19C H 0.9576 -0.1972 0.6667 0.298 Uiso 1 1 calc R . . C20 C 0.9910(6) -0.1177(5) 0.7906(3) 0.157(5) Uani 1 1 d . . . H20A H 1.0666 -0.1076 0.7855 0.236 Uiso 1 1 calc R . . H20B H 0.9791 -0.1695 0.7899 0.236 Uiso 1 1 calc R . . H20C H 0.9736 -0.0985 0.8236 0.236 Uiso 1 1 calc R . . C21 C 0.3775(5) 0.2352(3) 1.0918(2) 0.0463(17) Uani 1 1 d . . . H21A H 0.3593 0.2379 1.1261 0.056 Uiso 1 1 calc R . . C22 C 0.4511(5) 0.1834(3) 1.0790(2) 0.0472(17) Uani 1 1 d . . . H22A H 0.4827 0.1526 1.1046 0.057 Uiso 1 1 calc R . . C23 C 0.4794(5) 0.1762(3) 1.0280(2) 0.0450(17) Uani 1 1 d . . . C24 C 0.4341(5) 0.2271(3) 0.9928(2) 0.0543(19) Uani 1 1 d . . . H24 H 0.4529 0.2263 0.9585 0.065 Uiso 1 1 calc R . . C25 C 0.3620(5) 0.2787(3) 1.0081(2) 0.0538(19) Uani 1 1 d . . . H25 H 0.3338 0.3126 0.9837 0.065 Uiso 1 1 calc R . . C26 C 0.5461(5) 0.1159(3) 1.0125(2) 0.0405(16) Uani 1 1 d . . . C27 C 0.6202(5) 0.0469(3) 0.9598(3) 0.0434(17) Uani 1 1 d . . . C28 C 0.6494(5) 0.0207(3) 0.9097(2) 0.0410(16) Uani 1 1 d . . . C29 C 0.7124(5) -0.0415(3) 0.9054(2) 0.0467(17) Uani 1 1 d . . . H29 H 0.7408 -0.0659 0.9351 0.056 Uiso 1 1 calc R . . C30 C 0.7329(5) -0.0670(3) 0.8572(2) 0.0436(16) Uani 1 1 d . . . H30 H 0.7760 -0.1087 0.8552 0.052 Uiso 1 1 calc R . . C31 C 0.6352(5) 0.0264(3) 0.8174(2) 0.0522(19) Uani 1 1 d . . . H31 H 0.6099 0.0512 0.7873 0.063 Uiso 1 1 calc R . . C32 C 0.6107(5) 0.0546(3) 0.8644(2) 0.0528(19) Uani 1 1 d . . . H32 H 0.5679 0.0965 0.8656 0.063 Uiso 1 1 calc R . . C33 C 0.0245(6) 0.2759(3) 1.0071(2) 0.059(2) Uani 1 1 d . . . C34 C 0.0271(5) 0.2339(3) 1.0644(2) 0.0554(19) Uani 1 1 d . . . C35 C 0.4788(5) -0.1142(3) 0.7045(2) 0.0498(18) Uani 1 1 d . . . C36 C 0.5288(5) -0.1886(3) 0.7349(2) 0.0444(17) Uani 1 1 d . . . B3 B 0.0838(8) 0.1891(4) 1.0143(3) 0.065(3) Uani 1 1 d . . . H3 H 0.1719 0.1773 1.0127 0.078 Uiso 1 1 calc R . . B4 B -0.0039(9) 0.2134(5) 0.9584(4) 0.088(3) Uani 1 1 d . . . H4 H 0.0281 0.2171 0.9198 0.105 Uiso 1 1 calc R . . B5 B -0.1037(8) 0.2745(5) 0.9767(4) 0.095(3) Uani 1 1 d . . . H5 H -0.1369 0.3176 0.9503 0.114 Uiso 1 1 calc R . . B6 B -0.0830(7) 0.2890(5) 1.0444(4) 0.082(3) Uani 1 1 d . . . H6 H -0.1019 0.3414 1.0626 0.099 Uiso 1 1 calc R . . B7 B -0.0003(8) 0.1449(5) 1.0571(3) 0.076(3) Uani 1 1 d . . . H7 H 0.0342 0.1034 1.0846 0.092 Uiso 1 1 calc R . . B8 B -0.0210(9) 0.1275(5) 0.9896(4) 0.098(4) Uani 1 1 d . . . H8 H -0.0011 0.0750 0.9718 0.118 Uiso 1 1 calc R . . B9 B -0.1345(10) 0.1812(6) 0.9669(5) 0.124(5) Uani 1 1 d . . . H9 H -0.1902 0.1632 0.9337 0.149 Uiso 1 1 calc R . . B10 B -0.1848(9) 0.2279(6) 1.0196(5) 0.113(4) Uani 1 1 d . . . H10 H -0.2726 0.2404 1.0214 0.136 Uiso 1 1 calc R . . B11 B -0.1004(8) 0.2032(5) 1.0753(4) 0.097(4) Uani 1 1 d . . . H11 H -0.1325 0.1996 1.1139 0.116 Uiso 1 1 calc R . . B12 B -0.1310(9) 0.1373(6) 1.0268(4) 0.113(4) Uani 1 1 d . . . H12 H -0.1838 0.0900 1.0331 0.136 Uiso 1 1 calc R . . B13 B 0.5065(7) -0.1902(4) 0.6679(3) 0.061(2) Uani 1 1 d . . . H13 H 0.5722 -0.1931 0.6410 0.073 Uiso 1 1 calc R . . B14 B 0.3880(7) -0.1388(4) 0.6535(3) 0.069(3) Uani 1 1 d . . . H14 H 0.3758 -0.1079 0.6169 0.082 Uiso 1 1 calc R . . B15 B 0.3441(7) -0.1046(4) 0.7122(3) 0.069(3) Uani 1 1 d . . . H15 H 0.3029 -0.0513 0.7138 0.083 Uiso 1 1 calc R . . B16 B 0.4347(6) -0.1357(4) 0.7646(3) 0.059(2) Uani 1 1 d . . . H16 H 0.4537 -0.1036 0.8002 0.071 Uiso 1 1 calc R . . B17 B 0.4730(7) -0.2641(4) 0.7066(3) 0.066(3) Uani 1 1 d . . . H17 H 0.5170 -0.3164 0.7053 0.079 Uiso 1 1 calc R . . B18 B 0.3808(8) -0.2335(4) 0.6551(4) 0.085(3) Uani 1 1 d . . . H18 H 0.3627 -0.2659 0.6195 0.102 Uiso 1 1 calc R . . B19 B 0.2791(8) -0.1810(5) 0.6812(4) 0.093(4) Uani 1 1 d . . . H19 H 0.1944 -0.1785 0.6632 0.111 Uiso 1 1 calc R . . B20 B 0.3081(7) -0.1791(4) 0.7506(4) 0.078(3) Uani 1 1 d . . . H20 H 0.2423 -0.1756 0.7773 0.094 Uiso 1 1 calc R . . B21 B 0.4279(6) -0.2308(4) 0.7656(3) 0.061(2) Uani 1 1 d . . . H21 H 0.4414 -0.2610 0.8024 0.073 Uiso 1 1 calc R . . B22 B 0.3330(8) -0.2597(5) 0.7139(4) 0.086(3) Uani 1 1 d . . . H22 H 0.2835 -0.3095 0.7168 0.103 Uiso 1 1 calc R . . C37 C 0.2268(12) 0.0569(5) 0.8879(3) 0.235(8) Uani 1 1 d . . . H37A H 0.1482 0.0595 0.8912 0.282 Uiso 1 1 calc R . . H37B H 0.2631 0.0376 0.9198 0.282 Uiso 1 1 calc R . . Cl1 Cl 0.2566(4) 0.0064(3) 0.83454(17) 0.310(3) Uani 1 1 d . . . Cl2 Cl 0.2796(4) 0.1398(2) 0.87206(19) 0.315(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 Ir1 0.04358(17) 0.04175(15) 0.03879(15) -0.00175(13) 0.00093(12) -0.00119(15) Ir2 0.04713(18) 0.05203(17) 0.03934(16) -0.00136(14) 0.00585(13) 0.00117(16) S1 0.0635(13) 0.0531(11) 0.0464(10) 0.0071(9) -0.0103(9) -0.0103(10) S2 0.0589(13) 0.0607(12) 0.0489(11) 0.0076(9) 0.0038(9) -0.0101(10) S3 0.0575(13) 0.0468(10) 0.0549(11) 0.0087(9) -0.0044(9) -0.0002(9) S4 0.0540(12) 0.0443(10) 0.0507(11) 0.0020(8) -0.0052(9) 0.0078(9) N1 0.051(4) 0.037(3) 0.038(3) -0.004(3) 0.005(3) -0.004(3) N2 0.053(4) 0.050(4) 0.045(3) -0.010(3) -0.002(3) 0.003(3) N3 0.047(4) 0.048(3) 0.045(3) -0.004(3) 0.000(3) 0.007(3) N4 0.031(3) 0.044(3) 0.043(3) -0.002(3) 0.000(3) -0.002(3) O1 0.056(3) 0.040(3) 0.042(3) -0.001(2) 0.008(2) 0.004(2) C1 0.070(6) 0.046(4) 0.044(4) -0.014(4) 0.010(4) -0.001(4) C2 0.050(5) 0.054(5) 0.085(6) -0.011(4) -0.011(5) 0.007(4) C3 0.090(7) 0.045(4) 0.038(4) -0.003(3) 0.000(4) -0.017(5) C4 0.051(5) 0.042(4) 0.057(5) -0.016(4) 0.019(4) -0.009(4) C5 0.050(5) 0.028(4) 0.054(4) -0.004(3) -0.016(4) -0.005(3) C6 0.114(8) 0.134(7) 0.075(6) -0.039(5) 0.042(5) -0.042(6) C7 0.089(8) 0.087(6) 0.192(10) -0.050(6) -0.047(7) 0.041(6) C8 0.252(12) 0.072(6) 0.046(5) 0.018(4) -0.021(6) -0.048(6) C9 0.082(7) 0.096(6) 0.121(7) -0.055(5) 0.036(5) -0.039(5) C10 0.104(7) 0.052(5) 0.086(6) 0.011(4) -0.042(5) 0.000(4) C11 0.047(5) 0.080(6) 0.070(6) -0.019(5) 0.010(4) -0.023(5) C12 0.055(6) 0.097(7) 0.067(6) 0.034(5) 0.011(5) 0.006(5) C13 0.056(6) 0.128(8) 0.040(5) -0.020(5) 0.011(4) -0.016(6) C14 0.067(6) 0.073(6) 0.096(7) -0.028(5) 0.045(5) -0.004(5) C15 0.041(5) 0.079(6) 0.068(6) 0.016(5) 0.014(4) 0.006(5) C16 0.097(8) 0.153(8) 0.143(8) -0.067(7) 0.042(6) -0.062(7) C17 0.119(9) 0.142(8) 0.217(11) 0.117(8) 0.066(8) 0.022(7) C18 0.108(8) 0.379(16) 0.046(6) -0.031(8) 0.027(5) -0.055(9) C19 0.141(10) 0.112(8) 0.366(16) -0.115(10) 0.170(11) -0.038(7) C20 0.051(6) 0.266(13) 0.156(9) 0.118(9) 0.021(6) 0.054(7) C21 0.050(5) 0.057(5) 0.032(4) -0.004(3) 0.003(3) 0.003(4) C22 0.051(5) 0.052(4) 0.037(4) 0.004(3) -0.002(3) 0.006(4) C23 0.047(5) 0.043(4) 0.045(4) -0.002(3) 0.006(4) -0.004(4) C24 0.065(5) 0.061(5) 0.038(4) -0.001(4) 0.011(4) 0.008(4) C25 0.067(5) 0.054(5) 0.041(4) 0.006(4) 0.010(4) 0.001(4) C26 0.039(4) 0.043(4) 0.040(4) -0.008(3) 0.007(3) -0.005(3) C27 0.041(4) 0.037(4) 0.052(5) -0.012(4) 0.000(4) -0.004(3) C28 0.043(4) 0.039(4) 0.040(4) -0.005(3) 0.002(3) -0.005(3) C29 0.053(5) 0.049(4) 0.037(4) 0.001(3) -0.001(3) 0.004(4) C30 0.038(4) 0.045(4) 0.048(4) -0.001(4) 0.005(3) 0.013(3) C31 0.065(5) 0.042(4) 0.049(5) 0.008(4) 0.003(4) 0.001(4) C32 0.074(5) 0.034(4) 0.050(4) -0.010(3) 0.006(4) 0.014(4) C33 0.059(5) 0.053(5) 0.061(5) 0.009(4) -0.022(4) -0.012(4) C34 0.044(5) 0.059(5) 0.062(5) 0.017(4) -0.005(4) -0.004(4) C35 0.053(5) 0.045(4) 0.049(4) 0.004(3) -0.008(4) 0.006(4) C36 0.053(5) 0.032(4) 0.047(4) 0.002(3) -0.002(3) 0.001(3) B3 0.083(7) 0.050(5) 0.059(6) 0.005(4) -0.019(5) -0.006(5) B4 0.107(9) 0.070(7) 0.079(7) 0.000(6) -0.038(6) -0.025(7) B5 0.075(8) 0.089(8) 0.110(9) 0.023(7) -0.048(7) -0.015(7) B6 0.049(7) 0.093(8) 0.103(8) 0.019(6) -0.003(6) -0.001(6) B7 0.071(7) 0.058(6) 0.097(7) 0.020(5) -0.020(6) -0.016(6) B8 0.115(10) 0.067(7) 0.104(8) 0.017(6) -0.045(8) -0.037(7) B9 0.109(11) 0.097(9) 0.153(12) 0.031(8) -0.076(9) -0.057(8) B10 0.062(8) 0.126(10) 0.148(11) 0.035(9) -0.022(8) -0.015(8) B11 0.049(7) 0.110(9) 0.129(9) 0.051(8) -0.004(6) -0.022(7) B12 0.090(9) 0.106(9) 0.134(10) 0.033(8) -0.052(8) -0.042(8) B13 0.080(7) 0.056(5) 0.044(5) -0.006(4) -0.014(5) 0.000(5) B14 0.078(7) 0.066(6) 0.056(6) 0.004(5) -0.034(5) 0.003(6) B15 0.051(6) 0.062(6) 0.091(7) 0.015(5) -0.010(5) 0.007(5) B16 0.059(6) 0.062(6) 0.056(5) 0.015(5) 0.010(4) 0.015(5) B17 0.073(7) 0.053(6) 0.067(6) -0.003(5) -0.027(5) -0.003(5) B18 0.098(9) 0.058(6) 0.088(8) 0.006(5) -0.050(7) -0.006(6) B19 0.047(7) 0.087(7) 0.136(10) 0.034(7) -0.042(6) -0.016(6) B20 0.056(7) 0.075(7) 0.105(8) 0.040(6) 0.017(6) -0.007(6) B21 0.052(6) 0.058(6) 0.073(6) 0.026(5) 0.004(5) -0.002(5) B22 0.075(8) 0.055(6) 0.121(9) 0.023(6) -0.034(7) -0.013(6) C37 0.52(3) 0.123(9) 0.057(7) 0.034(6) -0.002(10) -0.027(12) Cl1 0.347(7) 0.334(6) 0.231(4) -0.083(4) -0.083(4) 0.068(5) Cl2 0.374(7) 0.185(4) 0.380(6) 0.012(4) -0.015(5) 0.011(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 N1 2.115(5) . ? Ir1 C2 2.162(7) . ? Ir1 C4 2.167(6) . ? Ir1 C5 2.178(6) . ? Ir1 C3 2.178(6) . ? Ir1 C1 2.184(6) . ? Ir1 S1 2.3626(16) . ? Ir1 S2 2.3663(17) . ? Ir2 N4 2.099(5) . ? Ir2 C13 2.129(7) . ? Ir2 C12 2.161(7) . ? Ir2 C14 2.171(7) . ? Ir2 C15 2.180(7) . ? Ir2 C11 2.192(7) . ? Ir2 S3 2.3470(18) . ? Ir2 S4 2.3648(17) . ? S1 C33 1.776(6) . ? S2 C34 1.793(6) . ? S3 C35 1.777(6) . ? S4 C36 1.791(6) . ? N1 C21 1.338(6) . ? N1 C25 1.355(6) . ? N2 C26 1.266(6) . ? N2 N3 1.413(6) . ? N3 C27 1.285(6) . ? N4 C31 1.340(6) . ? N4 C30 1.353(6) . ? O1 C27 1.354(6) . ? O1 C26 1.360(6) . ? C1 C2 1.402(8) . ? C1 C5 1.410(8) . ? C1 C6 1.505(8) . ? C2 C3 1.408(9) . ? C2 C7 1.516(9) . ? C3 C4 1.419(8) . ? C3 C8 1.517(7) . ? C4 C5 1.438(8) . ? C4 C9 1.495(8) . ? C5 C10 1.481(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 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 C15 1.396(9) . ? C11 C12 1.404(8) . ? C11 C16 1.510(8) . ? C12 C13 1.405(9) . ? C12 C17 1.521(9) . ? C13 C14 1.399(9) . ? C13 C18 1.513(9) . ? C14 C15 1.435(9) . ? C14 C19 1.495(9) . ? C15 C20 1.497(9) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.363(7) . ? C21 H21A 0.9300 . ? C22 C23 1.391(7) . ? C22 H22A 0.9300 . ? C23 C24 1.386(7) . ? C23 C26 1.445(7) . ? C24 C25 1.368(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C27 C28 1.446(7) . ? C28 C32 1.374(7) . ? C28 C29 1.383(7) . ? C29 C30 1.369(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.372(7) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.663(8) . ? C33 B5 1.693(11) . ? C33 B6 1.702(11) . ? C33 B4 1.714(10) . ? C33 B3 1.751(10) . ? C34 B7 1.672(9) . ? C34 B11 1.698(11) . ? C34 B3 1.720(10) . ? C34 B6 1.726(10) . ? C35 C36 1.663(7) . ? C35 B15 1.679(10) . ? C35 B14 1.712(9) . ? C35 B16 1.723(9) . ? C35 B13 1.730(9) . ? C36 B17 1.683(9) . ? C36 B21 1.700(9) . ? C36 B16 1.726(9) . ? C36 B13 1.728(9) . ? B3 B7 1.762(12) . ? B3 B4 1.782(11) . ? B3 B8 1.784(11) . ? B3 H3 1.1000 . ? B4 B9 1.729(14) . ? B4 B5 1.745(13) . ? B4 B8 1.785(12) . ? B4 H4 1.1000 . ? B5 B10 1.760(14) . ? B5 B9 1.763(13) . ? B5 B6 1.763(13) . ? B5 H5 1.1000 . ? B6 B10 1.755(13) . ? B6 B11 1.782(12) . ? B6 H6 1.1000 . ? B7 B11 1.715(13) . ? B7 B12 1.725(13) . ? B7 B8 1.769(12) . ? B7 H7 1.1000 . ? B8 B12 1.720(15) . ? B8 B9 1.760(15) . ? B8 H8 1.1000 . ? B9 B12 1.738(14) . ? B9 B10 1.755(15) . ? B9 H9 1.1000 . ? B10 B11 1.759(13) . ? B10 B12 1.788(15) . ? B10 H10 1.1000 . ? B11 B12 1.756(14) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? B13 B18 1.734(12) . ? B13 B14 1.740(11) . ? B13 B17 1.749(10) . ? B13 H13 1.1000 . ? B14 B18 1.737(11) . ? B14 B19 1.738(12) . ? B14 B15 1.759(11) . ? B14 H14 1.1000 . ? B15 B20 1.761(10) . ? B15 B19 1.766(11) . ? B15 B16 1.771(10) . ? B15 H15 1.1000 . ? B16 B21 1.744(10) . ? B16 B20 1.749(11) . ? B16 H16 1.1000 . ? B17 B22 1.734(12) . ? B17 B18 1.763(11) . ? B17 B21 1.766(11) . ? B17 H17 1.1000 . ? B18 B22 1.733(13) . ? B18 B19 1.746(13) . ? B18 H18 1.1000 . ? B19 B22 1.769(11) . ? B19 B20 1.795(12) . ? B19 H19 1.1000 . ? B20 B21 1.758(11) . ? B20 B22 1.792(12) . ? B20 H20 1.1000 . ? B21 B22 1.776(11) . ? B21 H21 1.1000 . ? B22 H22 1.1000 . ? C37 Cl2 1.710(9) . ? C37 Cl1 1.720(10) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? 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 N1 Ir1 C2 156.9(2) . . ? N1 Ir1 C4 93.9(2) . . ? C2 Ir1 C4 63.7(3) . . ? N1 Ir1 C5 102.8(2) . . ? C2 Ir1 C5 63.7(2) . . ? C4 Ir1 C5 38.6(2) . . ? N1 Ir1 C3 120.3(3) . . ? C2 Ir1 C3 37.9(2) . . ? C4 Ir1 C3 38.1(2) . . ? C5 Ir1 C3 64.0(2) . . ? N1 Ir1 C1 138.4(2) . . ? C2 Ir1 C1 37.7(2) . . ? C4 Ir1 C1 63.4(2) . . ? C5 Ir1 C1 37.7(2) . . ? C3 Ir1 C1 63.0(2) . . ? N1 Ir1 S1 90.10(14) . . ? C2 Ir1 S1 98.2(2) . . ? C4 Ir1 S1 124.82(19) . . ? C5 Ir1 S1 158.77(16) . . ? C3 Ir1 S1 94.95(18) . . ? C1 Ir1 S1 131.5(2) . . ? N1 Ir1 S2 87.40(14) . . ? C2 Ir1 S2 113.9(2) . . ? C4 Ir1 S2 144.77(19) . . ? C5 Ir1 S2 106.84(18) . . ? C3 Ir1 S2 151.7(2) . . ? C1 Ir1 S2 93.01(18) . . ? S1 Ir1 S2 90.34(6) . . ? N4 Ir2 C13 153.2(3) . . ? N4 Ir2 C12 115.0(3) . . ? C13 Ir2 C12 38.2(2) . . ? N4 Ir2 C14 144.1(3) . . ? C13 Ir2 C14 37.9(2) . . ? C12 Ir2 C14 63.4(3) . . ? N4 Ir2 C15 106.5(2) . . ? C13 Ir2 C15 64.1(3) . . ? C12 Ir2 C15 63.3(3) . . ? C14 Ir2 C15 38.5(2) . . ? N4 Ir2 C11 93.6(2) . . ? C13 Ir2 C11 63.4(3) . . ? C12 Ir2 C11 37.6(2) . . ? C14 Ir2 C11 63.0(3) . . ? C15 Ir2 C11 37.3(2) . . ? N4 Ir2 S3 90.18(14) . . ? C13 Ir2 S3 93.5(2) . . ? C12 Ir2 S3 94.7(2) . . ? C14 Ir2 S3 125.4(3) . . ? C15 Ir2 S3 156.36(18) . . ? C11 Ir2 S3 127.4(2) . . ? N4 Ir2 S4 87.44(13) . . ? C13 Ir2 S4 119.1(3) . . ? C12 Ir2 S4 156.9(2) . . ? C14 Ir2 S4 95.5(2) . . ? C15 Ir2 S4 106.6(2) . . ? C11 Ir2 S4 142.2(2) . . ? S3 Ir2 S4 90.36(6) . . ? C33 S1 Ir1 106.6(2) . . ? C34 S2 Ir1 106.3(2) . . ? C35 S3 Ir2 107.3(2) . . ? C36 S4 Ir2 106.08(19) . . ? C21 N1 C25 116.7(5) . . ? C21 N1 Ir1 120.9(4) . . ? C25 N1 Ir1 122.2(4) . . ? C26 N2 N3 105.5(5) . . ? C27 N3 N2 106.3(5) . . ? C31 N4 C30 115.9(5) . . ? C31 N4 Ir2 122.9(4) . . ? C30 N4 Ir2 120.7(4) . . ? C27 O1 C26 102.1(5) . . ? C2 C1 C5 109.1(6) . . ? C2 C1 C6 125.5(7) . . ? C5 C1 C6 125.4(7) . . ? C2 C1 Ir1 70.3(4) . . ? C5 C1 Ir1 70.9(3) . . ? C6 C1 Ir1 126.3(5) . . ? C1 C2 C3 108.4(7) . . ? C1 C2 C7 125.7(8) . . ? C3 C2 C7 125.5(8) . . ? C1 C2 Ir1 72.0(4) . . ? C3 C2 Ir1 71.7(4) . . ? C7 C2 Ir1 127.9(5) . . ? C2 C3 C4 107.8(6) . . ? C2 C3 C8 127.1(8) . . ? C4 C3 C8 125.0(8) . . ? C2 C3 Ir1 70.4(4) . . ? C4 C3 Ir1 70.5(4) . . ? C8 C3 Ir1 127.3(4) . . ? C3 C4 C5 107.9(6) . . ? C3 C4 C9 126.5(7) . . ? C5 C4 C9 125.5(7) . . ? C3 C4 Ir1 71.4(4) . . ? C5 C4 Ir1 71.1(3) . . ? C9 C4 Ir1 125.5(4) . . ? C1 C5 C4 106.8(6) . . ? C1 C5 C10 125.2(7) . . ? C4 C5 C10 127.6(7) . . ? C1 C5 Ir1 71.4(3) . . ? C4 C5 Ir1 70.3(3) . . ? C10 C5 Ir1 128.8(4) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 108.9(7) . . ? C15 C11 C16 126.4(8) . . ? C12 C11 C16 124.7(9) . . ? C15 C11 Ir2 70.9(4) . . ? C12 C11 Ir2 70.0(4) . . ? C16 C11 Ir2 124.2(5) . . ? C11 C12 C13 107.8(7) . . ? C11 C12 C17 125.6(9) . . ? C13 C12 C17 126.4(9) . . ? C11 C12 Ir2 72.4(4) . . ? C13 C12 Ir2 69.7(4) . . ? C17 C12 Ir2 126.9(5) . . ? C14 C13 C12 108.4(7) . . ? C14 C13 C18 127.2(10) . . ? C12 C13 C18 123.9(10) . . ? C14 C13 Ir2 72.6(4) . . ? C12 C13 Ir2 72.1(4) . . ? C18 C13 Ir2 127.7(5) . . ? C13 C14 C15 107.6(7) . . ? C13 C14 C19 126.2(10) . . ? C15 C14 C19 126.2(9) . . ? C13 C14 Ir2 69.4(4) . . ? C15 C14 Ir2 71.1(4) . . ? C19 C14 Ir2 126.2(5) . . ? C11 C15 C14 107.2(6) . . ? C11 C15 C20 125.4(8) . . ? C14 C15 C20 127.0(9) . . ? C11 C15 Ir2 71.8(4) . . ? C14 C15 Ir2 70.4(4) . . ? C20 C15 Ir2 129.1(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 C22 123.0(6) . . ? N1 C21 H21A 118.5 . . ? C22 C21 H21A 118.5 . . ? C21 C22 C23 120.8(6) . . ? C21 C22 H22A 119.6 . . ? C23 C22 H22A 119.6 . . ? C24 C23 C22 116.0(6) . . ? C24 C23 C26 122.5(6) . . ? C22 C23 C26 121.4(6) . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? N1 C25 C24 122.7(6) . . ? N1 C25 H25 118.6 . . ? C24 C25 H25 118.6 . . ? N2 C26 O1 113.7(5) . . ? N2 C26 C23 128.6(6) . . ? O1 C26 C23 117.5(6) . . ? N3 C27 O1 112.4(5) . . ? N3 C27 C28 129.4(6) . . ? O1 C27 C28 118.1(6) . . ? C32 C28 C29 117.4(6) . . ? C32 C28 C27 121.0(6) . . ? C29 C28 C27 121.5(6) . . ? C30 C29 C28 119.8(6) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? N4 C30 C29 123.3(6) . . ? N4 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? N4 C31 C32 123.7(6) . . ? N4 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C31 C32 C28 119.8(6) . . ? C31 C32 H32 120.1 . . ? C28 C32 H32 120.1 . . ? C34 C33 B5 110.9(6) . . ? C34 C33 B6 61.7(4) . . ? B5 C33 B6 62.6(5) . . ? C34 C33 B4 109.2(5) . . ? B5 C33 B4 61.6(5) . . ? B6 C33 B4 112.8(6) . . ? C34 C33 B3 60.5(4) . . ? B5 C33 B3 113.2(6) . . ? B6 C33 B3 113.5(6) . . ? B4 C33 B3 61.9(4) . . ? C34 C33 S1 118.6(4) . . ? B5 C33 S1 121.3(5) . . ? B6 C33 S1 117.1(5) . . ? B4 C33 S1 122.3(5) . . ? B3 C33 S1 117.5(5) . . ? C33 C34 B7 111.2(5) . . ? C33 C34 B11 110.2(5) . . ? B7 C34 B11 61.2(5) . . ? C33 C34 B3 62.3(4) . . ? B7 C34 B3 62.6(5) . . ? B11 C34 B3 113.2(6) . . ? C33 C34 B6 60.3(4) . . ? B7 C34 B6 113.1(6) . . ? B11 C34 B6 62.7(5) . . ? B3 C34 B6 113.8(5) . . ? C33 C34 S2 117.9(4) . . ? B7 C34 S2 122.2(5) . . ? B11 C34 S2 121.4(5) . . ? B3 C34 S2 117.6(5) . . ? B6 C34 S2 116.4(5) . . ? C36 C35 B15 110.9(5) . . ? C36 C35 B14 109.8(5) . . ? B15 C35 B14 62.5(5) . . ? C36 C35 B16 61.3(4) . . ? B15 C35 B16 62.7(4) . . ? B14 C35 B16 113.7(6) . . ? C36 C35 B13 61.2(4) . . ? B15 C35 B13 112.5(5) . . ? B14 C35 B13 60.7(4) . . ? B16 C35 B13 113.3(5) . . ? C36 C35 S3 117.7(4) . . ? B15 C35 S3 122.3(4) . . ? B14 C35 S3 121.6(4) . . ? B16 C35 S3 117.8(4) . . ? B13 C35 S3 116.9(5) . . ? C35 C36 B17 110.4(5) . . ? C35 C36 B21 109.8(5) . . ? B17 C36 B21 62.9(4) . . ? C35 C36 B16 61.1(4) . . ? B17 C36 B16 113.1(6) . . ? B21 C36 B16 61.2(4) . . ? C35 C36 B13 61.3(4) . . ? B17 C36 B13 61.7(4) . . ? B21 C36 B13 113.2(5) . . ? B16 C36 B13 113.2(5) . . ? C35 C36 S4 118.5(4) . . ? B17 C36 S4 121.1(4) . . ? B21 C36 S4 121.9(4) . . ? B16 C36 S4 118.1(4) . . ? B13 C36 S4 117.1(5) . . ? C34 B3 C33 57.2(4) . . ? C34 B3 B7 57.4(5) . . ? C33 B3 B7 103.1(6) . . ? C34 B3 B4 103.7(6) . . ? C33 B3 B4 58.0(4) . . ? B7 B3 B4 106.2(7) . . ? C34 B3 B8 104.5(7) . . ? C33 B3 B8 104.9(6) . . ? B7 B3 B8 59.8(5) . . ? B4 B3 B8 60.1(5) . . ? C34 B3 H3 125.0 . . ? C33 B3 H3 124.8 . . ? B7 B3 H3 123.6 . . ? B4 B3 H3 123.0 . . ? B8 B3 H3 122.5 . . ? C33 B4 B9 105.7(8) . . ? C33 B4 B5 58.6(5) . . ? B9 B4 B5 61.0(6) . . ? C33 B4 B3 60.1(4) . . ? B9 B4 B3 108.3(7) . . ? B5 B4 B3 109.2(7) . . ? C33 B4 B8 106.4(6) . . ? B9 B4 B8 60.1(6) . . ? B5 B4 B8 109.5(8) . . ? B3 B4 B8 60.0(5) . . ? C33 B4 H4 123.8 . . ? B9 B4 H4 122.1 . . ? B5 B4 H4 120.6 . . ? B3 B4 H4 121.0 . . ? B8 B4 H4 121.6 . . ? C33 B5 B4 59.8(5) . . ? C33 B5 B10 105.2(7) . . ? B4 B5 B10 107.3(7) . . ? C33 B5 B9 105.1(7) . . ? B4 B5 B9 59.1(6) . . ? B10 B5 B9 59.8(6) . . ? C33 B5 B6 59.0(5) . . ? B4 B5 B6 108.4(6) . . ? B10 B5 B6 59.8(6) . . ? B9 B5 B6 107.5(7) . . ? C33 B5 H5 123.9 . . ? B4 B5 H5 121.5 . . ? B10 B5 H5 122.6 . . ? B9 B5 H5 122.8 . . ? B6 B5 H5 121.5 . . ? C33 B6 C34 58.0(4) . . ? C33 B6 B10 105.0(7) . . ? C34 B6 B10 104.3(7) . . ? C33 B6 B5 58.5(5) . . ? C34 B6 B5 104.7(7) . . ? B10 B6 B5 60.0(6) . . ? C33 B6 B11 104.6(7) . . ? C34 B6 B11 57.9(5) . . ? B10 B6 B11 59.7(5) . . ? B5 B6 B11 107.2(7) . . ? C33 B6 H6 124.1 . . ? C34 B6 H6 124.5 . . ? B10 B6 H6 123.0 . . ? B5 B6 H6 122.4 . . ? B11 B6 H6 122.8 . . ? C34 B7 B11 60.2(5) . . ? C34 B7 B12 107.4(7) . . ? B11 B7 B12 61.4(6) . . ? C34 B7 B3 60.1(4) . . ? B11 B7 B3 110.3(6) . . ? B12 B7 B3 108.4(7) . . ? C34 B7 B8 107.3(6) . . ? B11 B7 B8 109.4(7) . . ? B12 B7 B8 59.0(6) . . ? B3 B7 B8 60.7(5) . . ? C34 B7 H7 122.5 . . ? B11 B7 H7 119.9 . . ? B12 B7 H7 122.0 . . ? B3 B7 H7 120.6 . . ? B8 B7 H7 121.9 . . ? B12 B8 B9 59.9(7) . . ? B12 B8 B7 59.3(6) . . ? B9 B8 B7 105.9(9) . . ? B12 B8 B3 107.7(8) . . ? B9 B8 B3 106.8(6) . . ? B7 B8 B3 59.5(5) . . ? B12 B8 B4 106.4(8) . . ? B9 B8 B4 58.4(5) . . ? B7 B8 B4 105.8(6) . . ? B3 B8 B4 59.9(4) . . ? B12 B8 H8 122.0 . . ? B9 B8 H8 122.9 . . ? B7 B8 H8 123.2 . . ? B3 B8 H8 121.8 . . ? B4 B8 H8 123.1 . . ? B4 B9 B12 108.1(7) . . ? B4 B9 B10 108.3(7) . . ? B12 B9 B10 61.6(7) . . ? B4 B9 B8 61.5(6) . . ? B12 B9 B8 58.9(6) . . ? B10 B9 B8 109.2(8) . . ? B4 B9 B5 60.0(5) . . ? B12 B9 B5 109.3(8) . . ? B10 B9 B5 60.0(6) . . ? B8 B9 B5 109.9(7) . . ? B4 B9 H9 121.5 . . ? B12 B9 H9 121.5 . . ? B10 B9 H9 121.0 . . ? B8 B9 H9 120.8 . . ? B5 B9 H9 120.9 . . ? B6 B10 B9 108.2(8) . . ? B6 B10 B11 60.9(5) . . ? B9 B10 B11 106.8(8) . . ? B6 B10 B5 60.2(5) . . ? B9 B10 B5 60.2(6) . . ? B11 B10 B5 108.4(7) . . ? B6 B10 B12 108.1(7) . . ? B9 B10 B12 58.7(6) . . ? B11 B10 B12 59.3(6) . . ? B5 B10 B12 107.2(9) . . ? B6 B10 H10 121.0 . . ? B9 B10 H10 122.4 . . ? B11 B10 H10 121.8 . . ? B5 B10 H10 121.6 . . ? B12 B10 H10 122.6 . . ? C34 B11 B7 58.7(5) . . ? C34 B11 B12 104.8(8) . . ? B7 B11 B12 59.6(6) . . ? C34 B11 B10 105.3(7) . . ? B7 B11 B10 108.7(8) . . ? B12 B11 B10 61.1(6) . . ? C34 B11 B6 59.4(4) . . ? B7 B11 B6 108.3(7) . . ? B12 B11 B6 108.3(7) . . ? B10 B11 B6 59.4(5) . . ? C34 B11 H11 124.4 . . ? B7 B11 H11 121.4 . . ? B12 B11 H11 122.1 . . ? B10 B11 H11 121.8 . . ? B6 B11 H11 121.4 . . ? B8 B12 B7 61.8(6) . . ? B8 B12 B9 61.2(7) . . ? B7 B12 B9 108.8(8) . . ? B8 B12 B11 109.7(7) . . ? B7 B12 B11 59.0(5) . . ? B9 B12 B11 107.7(8) . . ? B8 B12 B10 109.6(8) . . ? B7 B12 B10 106.9(7) . . ? B9 B12 B10 59.7(6) . . ? B11 B12 B10 59.5(6) . . ? B8 B12 H12 119.5 . . ? B7 B12 H12 121.8 . . ? B9 B12 H12 121.5 . . ? B11 B12 H12 122.0 . . ? B10 B12 H12 122.1 . . ? C36 B13 C35 57.5(3) . . ? C36 B13 B18 105.4(6) . . ? C35 B13 B18 105.3(6) . . ? C36 B13 B14 105.5(6) . . ? C35 B13 B14 59.1(4) . . ? B18 B13 B14 60.0(5) . . ? C36 B13 B17 57.9(4) . . ? C35 B13 B17 104.3(6) . . ? B18 B13 B17 60.8(5) . . ? B14 B13 B17 108.3(7) . . ? C36 B13 H13 124.3 . . ? C35 B13 H13 124.4 . . ? B18 B13 H13 122.4 . . ? B14 B13 H13 121.7 . . ? B17 B13 H13 122.4 . . ? C35 B14 B18 105.9(5) . . ? C35 B14 B19 105.6(6) . . ? B18 B14 B19 60.3(5) . . ? C35 B14 B13 60.1(4) . . ? B18 B14 B13 59.8(5) . . ? B19 B14 B13 108.7(6) . . ? C35 B14 B15 57.8(4) . . ? B18 B14 B15 108.4(7) . . ? B19 B14 B15 60.7(5) . . ? B13 B14 B15 108.2(5) . . ? C35 B14 H14 124.0 . . ? B18 B14 H14 122.0 . . ? B19 B14 H14 121.7 . . ? B13 B14 H14 121.0 . . ? B15 B14 H14 121.7 . . ? C35 B15 B14 59.7(4) . . ? C35 B15 B20 105.9(6) . . ? B14 B15 B20 108.3(6) . . ? C35 B15 B19 105.8(6) . . ? B14 B15 B19 59.1(5) . . ? B20 B15 B19 61.2(5) . . ? C35 B15 B16 59.8(4) . . ? B14 B15 B16 109.1(6) . . ? B20 B15 B16 59.4(4) . . ? B19 B15 B16 108.7(6) . . ? C35 B15 H15 123.5 . . ? B14 B15 H15 121.3 . . ? B20 B15 H15 122.0 . . ? B19 B15 H15 122.0 . . ? B16 B15 H15 121.0 . . ? C35 B16 C36 57.6(4) . . ? C35 B16 B21 105.1(5) . . ? C36 B16 B21 58.7(4) . . ? C35 B16 B20 104.6(6) . . ? C36 B16 B20 105.1(6) . . ? B21 B16 B20 60.4(4) . . ? C35 B16 B15 57.4(4) . . ? C36 B16 B15 103.9(5) . . ? B21 B16 B15 107.7(6) . . ? B20 B16 B15 60.0(4) . . ? C35 B16 H16 124.7 . . ? C36 B16 H16 124.5 . . ? B21 B16 H16 121.8 . . ? B20 B16 H16 122.6 . . ? B15 B16 H16 122.9 . . ? C36 B17 B22 106.5(6) . . ? C36 B17 B13 60.4(4) . . ? B22 B17 B13 107.5(6) . . ? C36 B17 B18 106.1(5) . . ? B22 B17 B18 59.4(5) . . ? B13 B17 B18 59.2(5) . . ? C36 B17 B21 59.0(4) . . ? B22 B17 B21 61.0(5) . . ? B13 B17 B21 109.0(6) . . ? B18 B17 B21 108.4(7) . . ? C36 B17 H17 123.1 . . ? B22 B17 H17 122.1 . . ? B13 B17 H17 121.4 . . ? B18 B17 H17 122.6 . . ? B21 B17 H17 120.8 . . ? B22 B18 B13 108.3(6) . . ? B22 B18 B14 108.6(7) . . ? B13 B18 B14 60.2(4) . . ? B22 B18 B19 61.1(6) . . ? B13 B18 B19 108.6(6) . . ? B14 B18 B19 59.9(5) . . ? B22 B18 B17 59.5(5) . . ? B13 B18 B17 60.0(5) . . ? B14 B18 B17 107.8(6) . . ? B19 B18 B17 108.4(7) . . ? B22 B18 H18 121.3 . . ? B13 B18 H18 121.5 . . ? B14 B18 H18 121.7 . . ? B19 B18 H18 121.1 . . ? B17 B18 H18 122.0 . . ? B14 B19 B18 59.8(5) . . ? B14 B19 B15 60.2(5) . . ? B18 B19 B15 107.6(6) . . ? B14 B19 B22 106.9(7) . . ? B18 B19 B22 59.1(5) . . ? B15 B19 B22 107.1(6) . . ? B14 B19 B20 107.7(6) . . ? B18 B19 B20 107.7(6) . . ? B15 B19 B20 59.3(5) . . ? B22 B19 B20 60.4(5) . . ? B14 B19 H19 122.0 . . ? B18 B19 H19 122.1 . . ? B15 B19 H19 122.1 . . ? B22 B19 H19 122.5 . . ? B20 B19 H19 121.8 . . ? B16 B20 B21 59.7(5) . . ? B16 B20 B15 60.6(4) . . ? B21 B20 B15 107.6(6) . . ? B16 B20 B22 107.5(6) . . ? B21 B20 B22 60.0(5) . . ? B15 B20 B22 106.3(6) . . ? B16 B20 B19 108.4(6) . . ? B21 B20 B19 107.7(7) . . ? B15 B20 B19 59.5(4) . . ? B22 B20 B19 59.1(5) . . ? B16 B20 H20 121.4 . . ? B21 B20 H20 121.9 . . ? B15 B20 H20 122.3 . . ? B22 B20 H20 122.7 . . ? B19 B20 H20 121.9 . . ? C36 B21 B16 60.1(4) . . ? C36 B21 B20 105.8(5) . . ? B16 B21 B20 59.9(4) . . ? C36 B21 B17 58.1(4) . . ? B16 B21 B17 108.3(5) . . ? B20 B21 B17 107.8(6) . . ? C36 B21 B22 103.8(6) . . ? B16 B21 B22 108.4(5) . . ? B20 B21 B22 60.9(5) . . ? B17 B21 B22 58.6(5) . . ? C36 B21 H21 124.5 . . ? B16 B21 H21 120.8 . . ? B20 B21 H21 121.7 . . ? B17 B21 H21 122.2 . . ? B22 B21 H21 122.8 . . ? B18 B22 B17 61.1(5) . . ? B18 B22 B19 59.8(5) . . ? B17 B22 B19 108.6(7) . . ? B18 B22 B21 109.2(7) . . ? B17 B22 B21 60.4(5) . . ? B19 B22 B21 108.1(6) . . ? B18 B22 B20 108.4(6) . . ? B17 B22 B20 107.7(6) . . ? B19 B22 B20 60.5(5) . . ? B21 B22 B20 59.0(5) . . ? B18 B22 H22 120.9 . . ? B17 B22 H22 121.2 . . ? B19 B22 H22 121.5 . . ? B21 B22 H22 121.6 . . ? B20 B22 H22 122.1 . . ? Cl2 C37 Cl1 100.3(6) . . ? Cl2 C37 H37A 111.7 . . ? Cl1 C37 H37A 111.7 . . ? Cl2 C37 H37B 111.7 . . ? Cl1 C37 H37B 111.7 . . ? H37A C37 H37B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.992 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.092 # Attachment 'f60314d-complex 6.cif' data_f60314d _database_code_depnum_ccdc_archive 'CCDC 611982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H62 B20 Cl4 Co2 N2 S4' _chemical_formula_weight 1126.98 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.062(8) _cell_length_b 11.190(9) _cell_length_c 13.775(11) _cell_angle_alpha 100.182(11) _cell_angle_beta 108.453(10) _cell_angle_gamma 96.283(11) _cell_volume 1425(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 834 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 27.153 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 578 _exptl_absorpt_coefficient_mu 0.946 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8333 _exptl_absorpt_correction_T_max 0.9542 _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 5933 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.01 _reflns_number_total 4924 _reflns_number_gt 4030 _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^)+(0.1357P)^2^+0.3204P] 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 4924 _refine_ls_number_parameters 322 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1886 _refine_ls_wR_factor_gt 0.1785 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.68876(5) 0.89922(5) 0.25561(4) 0.0317(2) Uani 1 1 d . . . S1 S 0.81187(11) 1.05970(10) 0.39045(8) 0.0393(3) Uani 1 1 d . . . S2 S 0.51549(11) 1.00466(10) 0.18702(8) 0.0387(3) Uani 1 1 d . . . N1 N 0.8020(3) 0.9436(3) 0.1662(3) 0.0344(7) Uani 1 1 d . . . C1 C 0.7275(4) 1.1881(4) 0.3616(3) 0.0356(9) Uani 1 1 d . . . C2 C 0.5775(4) 1.1598(4) 0.2598(3) 0.0386(9) Uani 1 1 d . . . C3 C 0.9450(4) 0.9689(5) 0.2034(3) 0.0437(10) Uani 1 1 d . . . H3 H 0.9923 0.9715 0.2739 0.052 Uiso 1 1 calc R . . C4 C 1.0250(4) 0.9914(5) 0.1406(3) 0.0481(12) Uani 1 1 d . . . H4 H 1.1239 1.0083 0.1698 0.058 Uiso 1 1 calc R . . C5 C 0.9596(4) 0.9890(4) 0.0352(3) 0.0372(9) Uani 1 1 d . . . C6 C 0.8109(4) 0.9634(5) -0.0019(3) 0.0419(10) Uani 1 1 d . . . H6 H 0.7607 0.9607 -0.0720 0.050 Uiso 1 1 calc R . . C7 C 0.7384(4) 0.9421(4) 0.0646(3) 0.0411(10) Uani 1 1 d . . . H7 H 0.6395 0.9257 0.0373 0.049 Uiso 1 1 calc R . . C8 C 0.7771(5) 0.7491(4) 0.3021(3) 0.0429(10) Uani 1 1 d . . . C9 C 0.6954(5) 0.7891(4) 0.3666(3) 0.0439(10) Uani 1 1 d . . . C10 C 0.5529(5) 0.7823(4) 0.3007(4) 0.0460(11) Uani 1 1 d . . . C11 C 0.5447(5) 0.7327(4) 0.1939(4) 0.0468(11) Uani 1 1 d . . . C12 C 0.6793(5) 0.7121(4) 0.1952(3) 0.0437(10) Uani 1 1 d . . . C13 C 0.9292(6) 0.7364(5) 0.3412(4) 0.0608(14) Uani 1 1 d . . . H13A H 0.9379 0.6652 0.3711 0.091 Uiso 1 1 calc R . . H13B H 0.9830 0.8088 0.3938 0.091 Uiso 1 1 calc R . . H13C H 0.9650 0.7271 0.2840 0.091 Uiso 1 1 calc R . . C14 C 0.7503(6) 0.8255(5) 0.4850(4) 0.0606(14) Uani 1 1 d . . . H14A H 0.6966 0.8831 0.5080 0.091 Uiso 1 1 calc R . . H14B H 0.8489 0.8630 0.5095 0.091 Uiso 1 1 calc R . . H14C H 0.7402 0.7534 0.5127 0.091 Uiso 1 1 calc R . . C15 C 0.4312(6) 0.8103(6) 0.3352(5) 0.0691(16) Uani 1 1 d . . . H15A H 0.4063 0.7479 0.3692 0.104 Uiso 1 1 calc R . . H15B H 0.3509 0.8118 0.2751 0.104 Uiso 1 1 calc R . . H15C H 0.4580 0.8893 0.3834 0.104 Uiso 1 1 calc R . . C16 C 0.4082(6) 0.7005(6) 0.1008(4) 0.0668(15) Uani 1 1 d . . . H16A H 0.4299 0.6943 0.0373 0.100 Uiso 1 1 calc R . . H16B H 0.3519 0.7637 0.1060 0.100 Uiso 1 1 calc R . . H16C H 0.3560 0.6230 0.1000 0.100 Uiso 1 1 calc R . . C17 C 0.7168(7) 0.6537(5) 0.1026(4) 0.0597(14) Uani 1 1 d . . . H17A H 0.6920 0.5656 0.0895 0.090 Uiso 1 1 calc R . . H17B H 0.8172 0.6766 0.1174 0.090 Uiso 1 1 calc R . . H17C H 0.6652 0.6817 0.0419 0.090 Uiso 1 1 calc R . . B3 B 0.7295(6) 1.2398(5) 0.2508(4) 0.0448(12) Uani 1 1 d . . . H3A H 0.7857 1.2031 0.1986 0.054 Uiso 1 1 calc R . . B4 B 0.8229(6) 1.3330(5) 0.3778(4) 0.0500(13) Uani 1 1 d . . . H4A H 0.9398 1.3565 0.4079 0.060 Uiso 1 1 calc R . . B5 B 0.7218(6) 1.3032(5) 0.4612(4) 0.0481(12) Uani 1 1 d . . . H5 H 0.7741 1.3078 0.5454 0.058 Uiso 1 1 calc R . . B6 B 0.5684(6) 1.1919(5) 0.3851(4) 0.0462(12) Uani 1 1 d . . . H6A H 0.5215 1.1243 0.4196 0.055 Uiso 1 1 calc R . . B7 B 0.5610(7) 1.2840(6) 0.2015(5) 0.0565(14) Uani 1 1 d . . . H7A H 0.5078 1.2760 0.1169 0.068 Uiso 1 1 calc R . . B8 B 0.7156(7) 1.3976(6) 0.2790(5) 0.0624(16) Uani 1 1 d . . . H8 H 0.7632 1.4654 0.2451 0.075 Uiso 1 1 calc R . . B9 B 0.7124(7) 1.4386(5) 0.4091(6) 0.0617(16) Uani 1 1 d . . . H9 H 0.7580 1.5314 0.4595 0.074 Uiso 1 1 calc R . . B10 B 0.5536(7) 1.3497(6) 0.4108(5) 0.0604(16) Uani 1 1 d . . . H10 H 0.4961 1.3862 0.4622 0.072 Uiso 1 1 calc R . . B11 B 0.4637(6) 1.2553(6) 0.2845(5) 0.0568(15) Uani 1 1 d . . . H11 H 0.3471 1.2286 0.2533 0.068 Uiso 1 1 calc R . . B12 B 0.5492(8) 1.4072(6) 0.2974(6) 0.0705(19) Uani 1 1 d . . . H12 H 0.4891 1.4803 0.2750 0.085 Uiso 1 1 calc R . . C18 C 0.0901(18) 0.3557(15) 0.2068(14) 0.219(7) Uani 1 1 d U . . H18A H 0.0262 0.3311 0.2426 0.263 Uiso 1 1 calc R . . H18B H 0.1725 0.3155 0.2240 0.263 Uiso 1 1 calc R . . Cl1 Cl 0.0049(10) 0.3369(8) 0.0716(7) 0.393(5) Uani 1 1 d U . . Cl2 Cl 0.1340(7) 0.5121(7) 0.2263(6) 0.371(4) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0330(3) 0.0338(4) 0.0270(3) 0.0053(2) 0.0091(2) 0.0065(2) S1 0.0420(6) 0.0355(6) 0.0326(6) 0.0033(4) 0.0032(4) 0.0101(5) S2 0.0333(5) 0.0439(6) 0.0342(6) 0.0051(5) 0.0062(4) 0.0101(5) N1 0.0330(17) 0.0361(19) 0.0338(18) 0.0037(14) 0.0131(14) 0.0065(14) C1 0.039(2) 0.034(2) 0.034(2) 0.0074(17) 0.0118(17) 0.0101(18) C2 0.038(2) 0.040(2) 0.038(2) 0.0073(18) 0.0128(18) 0.0098(19) C3 0.036(2) 0.061(3) 0.034(2) 0.014(2) 0.0094(18) 0.011(2) C4 0.029(2) 0.077(4) 0.037(2) 0.015(2) 0.0099(18) 0.008(2) C5 0.032(2) 0.045(3) 0.034(2) 0.0082(18) 0.0105(17) 0.0090(18) C6 0.033(2) 0.062(3) 0.028(2) 0.0075(19) 0.0082(17) 0.008(2) C7 0.032(2) 0.058(3) 0.032(2) 0.0067(19) 0.0104(17) 0.0076(19) C8 0.055(3) 0.035(2) 0.040(2) 0.0123(19) 0.014(2) 0.012(2) C9 0.060(3) 0.039(2) 0.032(2) 0.0107(19) 0.015(2) 0.005(2) C10 0.051(3) 0.044(3) 0.043(3) 0.013(2) 0.017(2) 0.000(2) C11 0.051(3) 0.038(2) 0.041(2) 0.0035(19) 0.008(2) -0.006(2) C12 0.060(3) 0.029(2) 0.038(2) 0.0030(18) 0.014(2) 0.006(2) C13 0.065(3) 0.055(3) 0.061(3) 0.017(3) 0.012(3) 0.026(3) C14 0.079(4) 0.065(3) 0.035(3) 0.017(2) 0.014(2) 0.011(3) C15 0.065(3) 0.085(4) 0.064(4) 0.018(3) 0.036(3) -0.001(3) C16 0.061(3) 0.069(4) 0.049(3) 0.004(3) 0.002(2) -0.009(3) C17 0.091(4) 0.043(3) 0.046(3) 0.003(2) 0.027(3) 0.016(3) B3 0.047(3) 0.049(3) 0.042(3) 0.017(2) 0.016(2) 0.007(2) B4 0.056(3) 0.042(3) 0.051(3) 0.011(2) 0.017(3) 0.005(3) B5 0.054(3) 0.041(3) 0.046(3) 0.001(2) 0.019(2) 0.008(2) B6 0.048(3) 0.048(3) 0.045(3) 0.002(2) 0.022(2) 0.011(2) B7 0.061(3) 0.052(3) 0.059(4) 0.024(3) 0.014(3) 0.019(3) B8 0.075(4) 0.042(3) 0.072(4) 0.026(3) 0.021(3) 0.011(3) B9 0.071(4) 0.032(3) 0.078(4) 0.005(3) 0.024(3) 0.010(3) B10 0.058(3) 0.050(4) 0.075(4) 0.006(3) 0.025(3) 0.021(3) B11 0.050(3) 0.050(3) 0.072(4) 0.013(3) 0.019(3) 0.025(3) B12 0.076(4) 0.048(4) 0.086(5) 0.019(3) 0.016(4) 0.034(3) C18 0.189(10) 0.238(11) 0.239(11) 0.064(9) 0.068(8) 0.070(9) Cl1 0.437(9) 0.381(9) 0.356(8) 0.030(6) 0.163(7) 0.063(7) Cl2 0.252(6) 0.335(7) 0.435(8) -0.166(6) 0.147(6) -0.008(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 Co1 N1 2.010(3) . ? Co1 C11 2.089(5) . ? Co1 C8 2.090(5) . ? Co1 C12 2.093(5) . ? Co1 C10 2.097(4) . ? Co1 C9 2.117(4) . ? Co1 S1 2.2553(17) . ? Co1 S2 2.2640(17) . ? S1 C1 1.788(4) . ? S2 C2 1.778(5) . ? N1 C7 1.339(5) . ? N1 C3 1.344(5) . ? C1 C2 1.656(6) . ? C1 B5 1.728(7) . ? C1 B3 1.730(6) . ? C1 B4 1.730(7) . ? C1 B6 1.735(6) . ? C2 B11 1.719(7) . ? C2 B7 1.721(7) . ? C2 B6 1.734(7) . ? C2 B3 1.736(7) . ? C3 C4 1.390(6) . ? C4 C5 1.386(6) . ? C5 C6 1.397(6) . ? C5 C5 1.484(8) 2_775 ? C6 C7 1.374(6) . ? C8 C9 1.437(6) . ? C8 C12 1.444(6) . ? C8 C13 1.485(7) . ? C9 C10 1.419(7) . ? C9 C14 1.509(6) . ? C10 C11 1.451(7) . ? C10 C15 1.491(7) . ? C11 C12 1.394(7) . ? C11 C16 1.508(7) . ? C12 C17 1.502(6) . ? B3 B4 1.769(8) . ? B3 B8 1.770(8) . ? B3 B7 1.776(8) . ? B4 B8 1.769(8) . ? B4 B9 1.796(9) . ? B4 B5 1.807(8) . ? B5 B6 1.768(8) . ? B5 B9 1.787(8) . ? B5 B10 1.788(8) . ? B6 B11 1.767(8) . ? B6 B10 1.772(8) . ? B7 B11 1.771(9) . ? B7 B12 1.775(10) . ? B7 B8 1.792(9) . ? B8 B9 1.781(10) . ? B8 B12 1.782(10) . ? B9 B10 1.797(9) . ? B9 B12 1.808(10) . ? B10 B11 1.763(9) . ? B10 B12 1.782(10) . ? B11 B12 1.771(10) . ? C18 Cl2 1.708(17) . ? C18 Cl1 1.750(16) . ? 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 N1 Co1 C11 115.49(17) . . ? N1 Co1 C8 100.37(16) . . ? C11 Co1 C8 67.0(2) . . ? N1 Co1 C12 89.68(16) . . ? C11 Co1 C12 38.94(19) . . ? C8 Co1 C12 40.41(18) . . ? N1 Co1 C10 155.30(17) . . ? C11 Co1 C10 40.55(18) . . ? C8 Co1 C10 67.30(19) . . ? C12 Co1 C10 66.91(19) . . ? N1 Co1 C9 138.68(17) . . ? C11 Co1 C9 66.60(19) . . ? C8 Co1 C9 39.95(18) . . ? C12 Co1 C9 66.68(18) . . ? C10 Co1 C9 39.35(18) . . ? N1 Co1 S1 92.97(11) . . ? C11 Co1 S1 150.88(14) . . ? C8 Co1 S1 103.48(14) . . ? C12 Co1 S1 143.39(14) . . ? C10 Co1 S1 110.41(14) . . ? C9 Co1 S1 88.28(14) . . ? N1 Co1 S2 93.63(11) . . ? C11 Co1 S2 90.90(15) . . ? C8 Co1 S2 157.33(14) . . ? C12 Co1 S2 122.86(14) . . ? C10 Co1 S2 92.83(15) . . ? C9 Co1 S2 127.55(14) . . ? S1 Co1 S2 93.43(7) . . ? C1 S1 Co1 105.40(15) . . ? C2 S2 Co1 105.63(15) . . ? C7 N1 C3 116.6(3) . . ? C7 N1 Co1 121.3(3) . . ? C3 N1 Co1 122.0(3) . . ? C2 C1 B5 110.6(3) . . ? C2 C1 B3 61.7(3) . . ? B5 C1 B3 113.2(4) . . ? C2 C1 B4 111.0(3) . . ? B5 C1 B4 63.0(3) . . ? B3 C1 B4 61.5(3) . . ? C2 C1 B6 61.5(3) . . ? B5 C1 B6 61.4(3) . . ? B3 C1 B6 113.6(3) . . ? B4 C1 B6 113.5(4) . . ? C2 C1 S1 117.3(3) . . ? B5 C1 S1 120.9(3) . . ? B3 C1 S1 118.8(3) . . ? B4 C1 S1 122.5(3) . . ? B6 C1 S1 115.8(3) . . ? C1 C2 B11 110.3(4) . . ? C1 C2 B7 110.6(4) . . ? B11 C2 B7 62.0(3) . . ? C1 C2 B6 61.5(3) . . ? B11 C2 B6 61.6(3) . . ? B7 C2 B6 112.8(4) . . ? C1 C2 B3 61.3(3) . . ? B11 C2 B3 112.5(4) . . ? B7 C2 B3 61.8(3) . . ? B6 C2 B3 113.3(4) . . ? C1 C2 S2 117.2(3) . . ? B11 C2 S2 122.2(3) . . ? B7 C2 S2 122.7(3) . . ? B6 C2 S2 116.7(3) . . ? B3 C2 S2 118.1(3) . . ? N1 C3 C4 122.6(4) . . ? C5 C4 C3 120.9(4) . . ? C4 C5 C6 115.7(4) . . ? C4 C5 C5 122.9(4) . 2_775 ? C6 C5 C5 121.4(4) . 2_775 ? C7 C6 C5 120.3(4) . . ? N1 C7 C6 123.9(4) . . ? C9 C8 C12 106.8(4) . . ? C9 C8 C13 125.5(4) . . ? C12 C8 C13 127.4(4) . . ? C9 C8 Co1 71.0(3) . . ? C12 C8 Co1 69.9(2) . . ? C13 C8 Co1 129.0(3) . . ? C10 C9 C8 108.6(4) . . ? C10 C9 C14 125.6(4) . . ? C8 C9 C14 125.6(4) . . ? C10 C9 Co1 69.6(2) . . ? C8 C9 Co1 69.0(2) . . ? C14 C9 Co1 129.8(3) . . ? C9 C10 C11 107.2(4) . . ? C9 C10 C15 126.6(4) . . ? C11 C10 C15 126.1(5) . . ? C9 C10 Co1 71.1(3) . . ? C11 C10 Co1 69.4(2) . . ? C15 C10 Co1 128.6(4) . . ? C12 C11 C10 108.6(4) . . ? C12 C11 C16 127.3(5) . . ? C10 C11 C16 123.9(5) . . ? C12 C11 Co1 70.7(3) . . ? C10 C11 Co1 70.0(2) . . ? C16 C11 Co1 129.0(4) . . ? C11 C12 C8 108.8(4) . . ? C11 C12 C17 126.3(4) . . ? C8 C12 C17 124.8(5) . . ? C11 C12 Co1 70.4(3) . . ? C8 C12 Co1 69.7(2) . . ? C17 C12 Co1 128.7(3) . . ? C1 B3 C2 57.1(2) . . ? C1 B3 B4 59.3(3) . . ? C2 B3 B4 105.5(4) . . ? C1 B3 B8 105.1(4) . . ? C2 B3 B8 105.5(4) . . ? B4 B3 B8 60.0(3) . . ? C1 B3 B7 104.8(4) . . ? C2 B3 B7 58.7(3) . . ? B4 B3 B7 108.7(4) . . ? B8 B3 B7 60.7(4) . . ? C1 B4 B3 59.2(3) . . ? C1 B4 B8 105.1(4) . . ? B3 B4 B8 60.0(3) . . ? C1 B4 B9 104.9(4) . . ? B3 B4 B9 108.1(4) . . ? B8 B4 B9 59.9(4) . . ? C1 B4 B5 58.5(3) . . ? B3 B4 B5 107.7(4) . . ? B8 B4 B5 107.1(4) . . ? B9 B4 B5 59.5(3) . . ? C1 B5 B6 59.5(3) . . ? C1 B5 B9 105.3(4) . . ? B6 B5 B9 108.6(4) . . ? C1 B5 B10 105.2(4) . . ? B6 B5 B10 59.8(3) . . ? B9 B5 B10 60.4(4) . . ? C1 B5 B4 58.6(3) . . ? B6 B5 B4 108.3(4) . . ? B9 B5 B4 60.0(3) . . ? B10 B5 B4 107.9(4) . . ? C2 B6 C1 57.0(2) . . ? C2 B6 B11 58.8(3) . . ? C1 B6 B11 104.6(4) . . ? C2 B6 B5 105.2(4) . . ? C1 B6 B5 59.1(3) . . ? B11 B6 B5 108.1(4) . . ? C2 B6 B10 105.3(4) . . ? C1 B6 B10 105.6(4) . . ? B11 B6 B10 59.8(4) . . ? B5 B6 B10 60.7(3) . . ? C2 B7 B11 58.9(3) . . ? C2 B7 B12 105.7(4) . . ? B11 B7 B12 59.9(4) . . ? C2 B7 B3 59.5(3) . . ? B11 B7 B3 108.2(4) . . ? B12 B7 B3 108.1(4) . . ? C2 B7 B8 105.1(4) . . ? B11 B7 B8 107.4(5) . . ? B12 B7 B8 60.0(4) . . ? B3 B7 B8 59.5(3) . . ? B4 B8 B3 60.0(3) . . ? B4 B8 B9 60.8(3) . . ? B3 B8 B9 108.8(4) . . ? B4 B8 B12 109.3(5) . . ? B3 B8 B12 108.1(4) . . ? B9 B8 B12 61.0(4) . . ? B4 B8 B7 108.1(4) . . ? B3 B8 B7 59.8(3) . . ? B9 B8 B7 108.5(5) . . ? B12 B8 B7 59.5(4) . . ? B8 B9 B5 107.4(4) . . ? B8 B9 B4 59.3(3) . . ? B5 B9 B4 60.5(3) . . ? B8 B9 B10 107.0(5) . . ? B5 B9 B10 59.8(3) . . ? B4 B9 B10 107.9(4) . . ? B8 B9 B12 59.5(4) . . ? B5 B9 B12 107.0(4) . . ? B4 B9 B12 107.0(5) . . ? B10 B9 B12 59.2(4) . . ? B11 B10 B6 60.0(3) . . ? B11 B10 B12 59.9(4) . . ? B6 B10 B12 108.2(4) . . ? B11 B10 B5 107.4(4) . . ? B6 B10 B5 59.6(3) . . ? B12 B10 B5 108.1(4) . . ? B11 B10 B9 108.3(5) . . ? B6 B10 B9 108.0(4) . . ? B12 B10 B9 60.7(4) . . ? B5 B10 B9 59.8(3) . . ? C2 B11 B10 106.4(4) . . ? C2 B11 B6 59.6(3) . . ? B10 B11 B6 60.2(3) . . ? C2 B11 B7 59.1(3) . . ? B10 B11 B7 108.8(5) . . ? B6 B11 B7 108.9(4) . . ? C2 B11 B12 106.0(4) . . ? B10 B11 B12 60.6(4) . . ? B6 B11 B12 108.9(5) . . ? B7 B11 B12 60.1(4) . . ? B11 B12 B7 59.9(4) . . ? B11 B12 B10 59.5(4) . . ? B7 B12 B10 107.8(4) . . ? B11 B12 B8 107.8(4) . . ? B7 B12 B8 60.5(4) . . ? B10 B12 B8 107.6(4) . . ? B11 B12 B9 107.5(4) . . ? B7 B12 B9 108.0(4) . . ? B10 B12 B9 60.1(4) . . ? B8 B12 B9 59.5(4) . . ? Cl2 C18 Cl1 92.9(10) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.988 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.095 # Attachment 'f60401a-complex 5.cif' data_f60401a _database_code_depnum_ccdc_archive 'CCDC 611983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H54 B20 Co2 N2 S4' _chemical_formula_weight 881.03 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.024(3) _cell_length_b 11.157(4) _cell_length_c 13.317(4) _cell_angle_alpha 95.035(5) _cell_angle_beta 91.109(5) _cell_angle_gamma 110.409(4) _cell_volume 1111.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 542 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 21.23 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 454 _exptl_absorpt_coefficient_mu 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8693 _exptl_absorpt_correction_T_max 0.9535 _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 5679 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.1730 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.22 _reflns_number_total 4792 _reflns_number_gt 2191 _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^)+(0.0196P)^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 4792 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.0724 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 0.680 _refine_ls_restrained_S_all 0.680 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.07763(5) -0.10134(4) 0.22159(4) 0.03857(15) Uani 1 1 d . . . S1 S 0.09376(10) 0.08376(7) 0.31053(7) 0.0432(2) Uani 1 1 d . . . S2 S 0.37574(10) -0.03486(7) 0.20976(7) 0.0465(3) Uani 1 1 d . . . N1 N 0.0339(3) -0.0404(2) 0.0922(2) 0.0400(7) Uani 1 1 d . . . B1 B 0.4790(5) 0.1856(4) 0.3695(3) 0.0535(12) Uani 1 1 d . . . H1 H 0.4595 0.1217 0.4300 0.064 Uiso 1 1 calc R . . B2 B 0.4142(5) 0.3213(3) 0.3794(3) 0.0543(12) Uani 1 1 d . . . H2 H 0.3522 0.3464 0.4472 0.065 Uiso 1 1 calc R . . B3 B 0.3475(5) 0.3455(3) 0.2571(3) 0.0524(12) Uani 1 1 d . . . H3 H 0.2426 0.3859 0.2452 0.063 Uiso 1 1 calc R . . B4 B 0.3727(5) 0.2257(3) 0.1723(3) 0.0468(11) Uani 1 1 d . . . H4 H 0.2831 0.1872 0.1044 0.056 Uiso 1 1 calc R . . B5 B 0.5969(5) 0.2407(4) 0.1723(4) 0.0611(13) Uani 1 1 d . . . H5 H 0.6554 0.2124 0.1043 0.073 Uiso 1 1 calc R . . B6 B 0.6636(5) 0.2174(4) 0.2932(4) 0.0624(14) Uani 1 1 d . . . H6 H 0.7658 0.1741 0.3040 0.075 Uiso 1 1 calc R . . B7 B 0.6418(6) 0.3401(4) 0.3797(4) 0.0698(15) Uani 1 1 d . . . H7 H 0.7309 0.3790 0.4477 0.084 Uiso 1 1 calc R . . B8 B 0.5612(6) 0.4382(4) 0.3111(3) 0.0644(14) Uani 1 1 d . . . H8 H 0.5972 0.5415 0.3345 0.077 Uiso 1 1 calc R . . B9 B 0.5357(5) 0.3787(4) 0.1822(3) 0.0603(13) Uani 1 1 d . . . H9 H 0.5559 0.4422 0.1214 0.072 Uiso 1 1 calc R . . B10 B 0.7158(6) 0.3741(4) 0.2591(4) 0.0722(15) Uani 1 1 d . . . H10 H 0.8540 0.4351 0.2484 0.087 Uiso 1 1 calc R . . C1 C 0.3097(4) 0.1945(3) 0.2922(2) 0.0403(9) Uani 1 1 d . . . C2 C 0.4542(4) 0.1341(3) 0.2421(3) 0.0433(9) Uani 1 1 d . . . C3 C -0.0813(4) 0.0205(3) 0.0817(3) 0.0398(8) Uani 1 1 d . . . H3A H -0.1413 0.0361 0.1375 0.048 Uiso 1 1 calc R . . C4 C 0.1143(4) -0.0607(3) 0.0085(3) 0.0385(8) Uani 1 1 d . . . H4A H 0.1950 -0.1033 0.0117 0.046 Uiso 1 1 calc R . . C5 C -0.1361(4) -0.1982(3) 0.3054(3) 0.0399(9) Uani 1 1 d . . . C6 C -0.1702(4) -0.2472(3) 0.2035(3) 0.0415(9) Uani 1 1 d . . . C7 C -0.0330(5) -0.2955(3) 0.1742(3) 0.0497(10) Uani 1 1 d . . . C8 C 0.0817(4) -0.2781(3) 0.2606(3) 0.0509(10) Uani 1 1 d . . . C9 C 0.0239(4) -0.2142(3) 0.3402(3) 0.0482(9) Uani 1 1 d . . . C10 C -0.2503(4) -0.1458(3) 0.3686(3) 0.0616(11) Uani 1 1 d . . . H10A H -0.3030 -0.0997 0.3284 0.092 Uiso 1 1 calc R . . H10B H -0.1792 -0.0887 0.4239 0.092 Uiso 1 1 calc R . . H10C H -0.3426 -0.2152 0.3944 0.092 Uiso 1 1 calc R . . C11 C -0.3305(4) -0.2559(3) 0.1398(3) 0.0630(11) Uani 1 1 d . . . H11A H -0.4291 -0.3305 0.1530 0.095 Uiso 1 1 calc R . . H11B H -0.3054 -0.2624 0.0697 0.095 Uiso 1 1 calc R . . H11C H -0.3600 -0.1803 0.1557 0.095 Uiso 1 1 calc R . . C12 C -0.0281(5) -0.3637(3) 0.0721(3) 0.0839(14) Uani 1 1 d . . . H12A H 0.0926 -0.3554 0.0592 0.126 Uiso 1 1 calc R . . H12B H -0.0739 -0.3260 0.0211 0.126 Uiso 1 1 calc R . . H12C H -0.0996 -0.4530 0.0710 0.126 Uiso 1 1 calc R . . C13 C 0.2328(4) -0.3276(3) 0.2666(3) 0.0927(16) Uani 1 1 d . . . H13A H 0.1976 -0.4029 0.3022 0.139 Uiso 1 1 calc R . . H13B H 0.3342 -0.2626 0.3018 0.139 Uiso 1 1 calc R . . H13C H 0.2631 -0.3488 0.1997 0.139 Uiso 1 1 calc R . . C14 C 0.1042(5) -0.1816(3) 0.4449(3) 0.0827(13) Uani 1 1 d . . . H14A H 0.0553 -0.2541 0.4828 0.124 Uiso 1 1 calc R . . H14B H 0.0783 -0.1096 0.4762 0.124 Uiso 1 1 calc R . . H14C H 0.2308 -0.1598 0.4434 0.124 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 Co1 0.0399(3) 0.0346(3) 0.0413(3) 0.0034(2) 0.0055(2) 0.0131(2) S1 0.0466(5) 0.0396(5) 0.0433(6) 0.0001(5) 0.0095(5) 0.0154(4) S2 0.0407(5) 0.0388(5) 0.0616(7) 0.0037(5) 0.0045(5) 0.0159(4) N1 0.0391(16) 0.0352(16) 0.046(2) 0.0007(15) 0.0013(15) 0.0146(13) B1 0.059(3) 0.056(3) 0.045(3) 0.011(2) -0.008(2) 0.020(2) B2 0.070(3) 0.042(3) 0.046(3) -0.005(2) -0.001(3) 0.016(2) B3 0.067(3) 0.031(2) 0.058(3) 0.006(2) -0.004(3) 0.016(2) B4 0.051(3) 0.046(3) 0.046(3) 0.012(2) 0.006(2) 0.019(2) B5 0.051(3) 0.053(3) 0.074(4) 0.014(3) 0.017(3) 0.008(2) B6 0.038(3) 0.051(3) 0.089(4) 0.008(3) -0.008(3) 0.005(2) B7 0.068(3) 0.045(3) 0.075(4) -0.005(3) -0.029(3) -0.002(2) B8 0.075(3) 0.035(3) 0.069(4) 0.002(3) -0.002(3) 0.003(2) B9 0.065(3) 0.045(3) 0.066(4) 0.019(3) 0.008(3) 0.009(2) B10 0.055(3) 0.050(3) 0.096(4) 0.012(3) 0.008(3) -0.003(2) C1 0.048(2) 0.0325(19) 0.041(2) 0.0020(17) 0.0010(18) 0.0157(17) C2 0.041(2) 0.036(2) 0.051(3) 0.0054(18) 0.0042(19) 0.0114(17) C3 0.042(2) 0.040(2) 0.038(2) -0.0019(18) 0.0033(18) 0.0161(17) C4 0.0398(19) 0.0348(19) 0.043(2) -0.0028(19) 0.0016(19) 0.0169(16) C5 0.042(2) 0.034(2) 0.043(2) 0.0113(18) 0.0091(19) 0.0107(17) C6 0.043(2) 0.036(2) 0.041(2) 0.0078(18) 0.0048(19) 0.0063(17) C7 0.059(2) 0.029(2) 0.059(3) 0.004(2) 0.019(2) 0.0112(19) C8 0.042(2) 0.032(2) 0.082(3) 0.019(2) 0.010(2) 0.0122(18) C9 0.052(2) 0.035(2) 0.054(3) 0.010(2) -0.002(2) 0.0103(18) C10 0.062(2) 0.058(2) 0.065(3) 0.009(2) 0.024(2) 0.018(2) C11 0.046(2) 0.061(2) 0.067(3) 0.005(2) -0.003(2) 0.0007(19) C12 0.103(3) 0.052(2) 0.082(3) -0.019(2) 0.041(3) 0.012(2) C13 0.061(3) 0.056(3) 0.173(5) 0.032(3) 0.017(3) 0.029(2) C14 0.099(3) 0.079(3) 0.060(3) 0.015(3) -0.022(3) 0.018(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 Co1 N1 1.975(3) . ? Co1 C9 2.065(3) . ? Co1 C7 2.067(3) . ? Co1 C6 2.078(3) . ? Co1 C5 2.085(3) . ? Co1 C8 2.093(3) . ? Co1 S1 2.2501(10) . ? Co1 S2 2.2571(11) . ? S1 C1 1.779(3) . ? S2 C2 1.777(3) . ? N1 C3 1.337(3) . ? N1 C4 1.340(3) . ? B1 C1 1.724(5) . ? B1 C2 1.727(5) . ? B1 B7 1.755(5) . ? B1 B2 1.760(5) . ? B1 B6 1.763(5) . ? B2 C1 1.703(5) . ? B2 B8 1.759(6) . ? B2 B7 1.764(6) . ? B2 B3 1.777(6) . ? B3 C1 1.713(4) . ? B3 B4 1.742(5) . ? B3 B8 1.764(6) . ? B3 B9 1.773(5) . ? B4 C1 1.713(5) . ? B4 C2 1.716(5) . ? B4 B9 1.743(5) . ? B4 B5 1.747(5) . ? B5 C2 1.696(5) . ? B5 B6 1.756(6) . ? B5 B9 1.767(5) . ? B5 B10 1.768(6) . ? B6 C2 1.704(5) . ? B6 B10 1.753(6) . ? B6 B7 1.769(6) . ? B7 B10 1.750(6) . ? B7 B8 1.759(6) . ? B8 B10 1.759(6) . ? B8 B9 1.766(6) . ? B9 B10 1.773(6) . ? C1 C2 1.656(4) . ? C3 C4 1.371(4) 2 ? C4 C3 1.371(4) 2 ? C5 C6 1.403(4) . ? C5 C9 1.430(4) . ? C5 C10 1.486(4) . ? C6 C7 1.430(4) . ? C6 C11 1.497(4) . ? C7 C8 1.415(4) . ? C7 C12 1.507(4) . ? C8 C9 1.401(4) . ? C8 C13 1.500(4) . ? C9 C14 1.484(4) . ? 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 N1 Co1 C9 157.43(11) . . ? N1 Co1 C7 96.36(13) . . ? C9 Co1 C7 67.25(14) . . ? N1 Co1 C6 90.28(12) . . ? C9 Co1 C6 67.16(13) . . ? C7 Co1 C6 40.37(11) . . ? N1 Co1 C5 120.04(12) . . ? C9 Co1 C5 40.31(11) . . ? C7 Co1 C5 67.06(13) . . ? C6 Co1 C5 39.39(11) . . ? N1 Co1 C8 132.98(14) . . ? C9 Co1 C8 39.38(12) . . ? C7 Co1 C8 39.76(12) . . ? C6 Co1 C8 66.66(13) . . ? C5 Co1 C8 66.41(12) . . ? N1 Co1 S1 92.67(8) . . ? C9 Co1 S1 97.02(10) . . ? C7 Co1 S1 155.60(10) . . ? C6 Co1 S1 117.25(10) . . ? C5 Co1 S1 88.80(9) . . ? C8 Co1 S1 134.11(12) . . ? N1 Co1 S2 94.37(8) . . ? C9 Co1 S2 105.51(10) . . ? C7 Co1 S2 109.49(10) . . ? C6 Co1 S2 149.85(10) . . ? C5 Co1 S2 145.49(10) . . ? C8 Co1 S2 88.96(9) . . ? S1 Co1 S2 92.31(3) . . ? C1 S1 Co1 105.37(10) . . ? C2 S2 Co1 105.65(10) . . ? C3 N1 C4 115.6(3) . . ? C3 N1 Co1 122.3(2) . . ? C4 N1 Co1 122.1(2) . . ? C1 B1 C2 57.34(19) . . ? C1 B1 B7 105.1(3) . . ? C2 B1 B7 105.1(3) . . ? C1 B1 B2 58.5(2) . . ? C2 B1 B2 104.8(3) . . ? B7 B1 B2 60.3(2) . . ? C1 B1 B6 104.7(3) . . ? C2 B1 B6 58.5(2) . . ? B7 B1 B6 60.4(2) . . ? B2 B1 B6 108.2(3) . . ? C1 B2 B8 105.1(3) . . ? C1 B2 B1 59.7(2) . . ? B8 B2 B1 107.8(3) . . ? C1 B2 B7 105.6(3) . . ? B8 B2 B7 59.9(2) . . ? B1 B2 B7 59.7(2) . . ? C1 B2 B3 58.9(2) . . ? B8 B2 B3 59.8(2) . . ? B1 B2 B3 108.6(3) . . ? B7 B2 B3 108.0(3) . . ? C1 B3 B4 59.43(19) . . ? C1 B3 B8 104.5(3) . . ? B4 B3 B8 107.0(3) . . ? C1 B3 B9 105.4(3) . . ? B4 B3 B9 59.5(2) . . ? B8 B3 B9 59.9(2) . . ? C1 B3 B2 58.4(2) . . ? B4 B3 B2 107.5(3) . . ? B8 B3 B2 59.6(2) . . ? B9 B3 B2 107.7(3) . . ? C1 B4 C2 57.74(19) . . ? C1 B4 B3 59.4(2) . . ? C2 B4 B3 106.4(3) . . ? C1 B4 B9 106.7(3) . . ? C2 B4 B9 106.3(3) . . ? B3 B4 B9 61.1(2) . . ? C1 B4 B5 105.5(3) . . ? C2 B4 B5 58.6(2) . . ? B3 B4 B5 109.6(3) . . ? B9 B4 B5 60.8(2) . . ? C2 B5 B4 59.8(2) . . ? C2 B5 B6 59.1(2) . . ? B4 B5 B6 108.4(3) . . ? C2 B5 B9 106.2(3) . . ? B4 B5 B9 59.5(2) . . ? B6 B5 B9 108.4(3) . . ? C2 B5 B10 105.3(3) . . ? B4 B5 B10 107.3(3) . . ? B6 B5 B10 59.6(2) . . ? B9 B5 B10 60.2(2) . . ? C2 B6 B10 105.6(3) . . ? C2 B6 B5 58.7(2) . . ? B10 B6 B5 60.5(2) . . ? C2 B6 B1 59.7(2) . . ? B10 B6 B1 107.7(3) . . ? B5 B6 B1 108.4(3) . . ? C2 B6 B7 105.5(3) . . ? B10 B6 B7 59.6(2) . . ? B5 B6 B7 108.0(3) . . ? B1 B6 B7 59.6(2) . . ? B10 B7 B1 108.2(3) . . ? B10 B7 B8 60.2(3) . . ? B1 B7 B8 108.1(3) . . ? B10 B7 B2 108.1(3) . . ? B1 B7 B2 60.0(2) . . ? B8 B7 B2 59.9(2) . . ? B10 B7 B6 59.8(3) . . ? B1 B7 B6 60.0(2) . . ? B8 B7 B6 107.7(3) . . ? B2 B7 B6 107.7(3) . . ? B7 B8 B2 60.2(2) . . ? B7 B8 B10 59.6(3) . . ? B2 B8 B10 107.9(3) . . ? B7 B8 B3 108.9(3) . . ? B2 B8 B3 60.6(2) . . ? B10 B8 B3 108.5(3) . . ? B7 B8 B9 108.6(3) . . ? B2 B8 B9 108.8(3) . . ? B10 B8 B9 60.4(3) . . ? B3 B8 B9 60.3(2) . . ? B4 B9 B8 106.9(3) . . ? B4 B9 B5 59.7(2) . . ? B8 B9 B5 107.3(3) . . ? B4 B9 B3 59.4(2) . . ? B8 B9 B3 59.8(2) . . ? B5 B9 B3 107.3(3) . . ? B4 B9 B10 107.3(3) . . ? B8 B9 B10 59.6(3) . . ? B5 B9 B10 59.9(2) . . ? B3 B9 B10 107.5(3) . . ? B7 B10 B6 60.7(3) . . ? B7 B10 B8 60.2(3) . . ? B6 B10 B8 108.4(3) . . ? B7 B10 B5 108.3(3) . . ? B6 B10 B5 59.8(2) . . ? B8 B10 B5 107.6(3) . . ? B7 B10 B9 108.7(3) . . ? B6 B10 B9 108.3(3) . . ? B8 B10 B9 60.0(2) . . ? B5 B10 B9 59.9(2) . . ? C2 C1 B2 110.7(2) . . ? C2 C1 B4 61.21(19) . . ? B2 C1 B4 112.4(2) . . ? C2 C1 B3 110.5(2) . . ? B2 C1 B3 62.7(2) . . ? B4 C1 B3 61.1(2) . . ? C2 C1 B1 61.44(19) . . ? B2 C1 B1 61.8(2) . . ? B4 C1 B1 113.0(3) . . ? B3 C1 B1 113.5(3) . . ? C2 C1 S1 116.90(19) . . ? B2 C1 S1 121.2(2) . . ? B4 C1 S1 119.6(2) . . ? B3 C1 S1 123.4(2) . . ? B1 C1 S1 115.3(2) . . ? C1 C2 B5 110.6(2) . . ? C1 C2 B6 110.5(2) . . ? B5 C2 B6 62.2(2) . . ? C1 C2 B4 61.05(19) . . ? B5 C2 B4 61.6(2) . . ? B6 C2 B4 112.4(2) . . ? C1 C2 B1 61.22(19) . . ? B5 C2 B1 113.0(3) . . ? B6 C2 B1 61.8(2) . . ? B4 C2 B1 112.6(3) . . ? C1 C2 S2 116.40(19) . . ? B5 C2 S2 123.4(2) . . ? B6 C2 S2 122.4(2) . . ? B4 C2 S2 118.4(2) . . ? B1 C2 S2 116.2(2) . . ? N1 C3 C4 122.4(3) . 2 ? N1 C4 C3 122.0(3) . 2 ? C6 C5 C9 107.9(3) . . ? C6 C5 C10 126.5(3) . . ? C9 C5 C10 125.5(3) . . ? C6 C5 Co1 70.01(19) . . ? C9 C5 Co1 69.07(18) . . ? C10 C5 Co1 129.1(2) . . ? C5 C6 C7 108.1(3) . . ? C5 C6 C11 125.2(3) . . ? C7 C6 C11 126.5(3) . . ? C5 C6 Co1 70.60(18) . . ? C7 C6 Co1 69.43(18) . . ? C11 C6 Co1 129.1(2) . . ? C8 C7 C6 107.3(3) . . ? C8 C7 C12 127.9(3) . . ? C6 C7 C12 124.5(4) . . ? C8 C7 Co1 71.11(19) . . ? C6 C7 Co1 70.20(18) . . ? C12 C7 Co1 128.5(2) . . ? C9 C8 C7 108.7(3) . . ? C9 C8 C13 126.1(4) . . ? C7 C8 C13 125.1(4) . . ? C9 C8 Co1 69.21(19) . . ? C7 C8 Co1 69.13(19) . . ? C13 C8 Co1 130.4(2) . . ? C8 C9 C5 107.8(3) . . ? C8 C9 C14 125.8(4) . . ? C5 C9 C14 126.1(3) . . ? C8 C9 Co1 71.4(2) . . ? C5 C9 Co1 70.62(19) . . ? C14 C9 Co1 128.3(2) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.22 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.576 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.056 # Attachment 'f60415a-complex 7.cif' data_f60415a _database_code_depnum_ccdc_archive 'CCDC 611984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H76 B20 Co2 N2 O2 S4' _chemical_formula_weight 1127.37 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.241(3) _cell_length_b 11.148(3) _cell_length_c 13.910(4) _cell_angle_alpha 76.265(5) _cell_angle_beta 74.636(5) _cell_angle_gamma 87.557(5) _cell_volume 1487.2(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 554 _cell_measurement_theta_min 2.822 _cell_measurement_theta_max 20.893 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8977 _exptl_absorpt_correction_T_max 0.9435 _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 6333 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.1227 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5182 _reflns_number_gt 2817 _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^)+(0.1161P)^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 5182 _refine_ls_number_parameters 324 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1383 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2260 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.970 _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 C22 C 0.141(2) 0.4912(14) 0.7344(12) 0.273(11) Uiso 1 1 d D . . H22A H 0.2000 0.5504 0.6792 0.328 Uiso 1 1 calc R . . H22B H 0.0567 0.4866 0.7157 0.328 Uiso 1 1 calc R . . Co1 Co 0.61403(10) 0.89213(8) 0.72476(7) 0.0447(3) Uani 1 1 d . . . S1 S 0.6289(2) 1.05486(16) 0.59003(13) 0.0535(5) Uani 1 1 d . . . S2 S 0.7135(2) 0.99767(17) 0.80699(14) 0.0520(5) Uani 1 1 d . . . N1 N 0.4254(6) 0.9314(5) 0.7945(4) 0.0477(15) Uani 1 1 d . . . B3 B 0.8416(10) 1.1964(9) 0.6279(8) 0.066(3) Uani 1 1 d . . . H3 H 0.9211 1.1345 0.5992 0.079 Uiso 1 1 calc R . . B4 B 0.7665(10) 1.3060(8) 0.5448(8) 0.066(3) Uani 1 1 d . . . H4 H 0.7974 1.3156 0.4613 0.079 Uiso 1 1 calc R . . B5 B 0.5966(11) 1.3248(8) 0.6097(7) 0.063(3) Uani 1 1 d . . . H5 H 0.5172 1.3464 0.5687 0.076 Uiso 1 1 calc R . . B6 B 0.5639(10) 1.2248(8) 0.7351(7) 0.054(2) Uani 1 1 d . . . H6 H 0.4639 1.1810 0.7754 0.065 Uiso 1 1 calc R . . B7 B 0.8387(11) 1.2561(10) 0.7356(9) 0.077(3) Uani 1 1 d . . . H7 H 0.9175 1.2329 0.7771 0.092 Uiso 1 1 calc R . . B8 B 0.8702(12) 1.3548(10) 0.6114(10) 0.091(4) Uani 1 1 d . . . H8 H 0.9704 1.3981 0.5708 0.109 Uiso 1 1 calc R . . B9 B 0.7197(11) 1.4335(9) 0.6001(9) 0.080(3) Uani 1 1 d . . . H9 H 0.7210 1.5278 0.5524 0.096 Uiso 1 1 calc R . . B10 B 0.5972(12) 1.3841(8) 0.7176(8) 0.074(3) Uani 1 1 d . . . H10 H 0.5182 1.4461 0.7467 0.088 Uiso 1 1 calc R . . B11 B 0.6696(11) 1.2730(9) 0.8012(8) 0.071(3) Uani 1 1 d . . . H11 H 0.6379 1.2602 0.8850 0.085 Uiso 1 1 calc R . . B12 B 0.7654(12) 1.4031(9) 0.7197(10) 0.086(4) Uani 1 1 d . . . H12 H 0.7966 1.4768 0.7499 0.103 Uiso 1 1 calc R . . C1 C 0.6748(8) 1.1830(7) 0.6301(5) 0.0533(19) Uani 1 1 d . . . C2 C 0.7167(7) 1.1556(6) 0.7397(6) 0.0524(19) Uani 1 1 d . . . C3 C 0.7803(9) 0.7847(7) 0.6839(7) 0.063(2) Uani 1 1 d . . . C4 C 0.6935(9) 0.7825(6) 0.6212(6) 0.058(2) Uani 1 1 d . . . C5 C 0.5655(8) 0.7355(6) 0.6837(5) 0.0515(19) Uani 1 1 d . . . C6 C 0.5746(10) 0.7032(6) 0.7875(6) 0.059(2) Uani 1 1 d . . . C7 C 0.7021(10) 0.7328(7) 0.7881(7) 0.067(2) Uani 1 1 d . . . C8 C 0.9250(9) 0.8219(10) 0.6508(9) 0.103(4) Uani 1 1 d . . . H8A H 0.9788 0.7541 0.6325 0.155 Uiso 1 1 calc R . . H8B H 0.9501 0.8448 0.7059 0.155 Uiso 1 1 calc R . . H8C H 0.9401 0.8910 0.5925 0.155 Uiso 1 1 calc R . . C9 C 0.7324(10) 0.8194(7) 0.5061(6) 0.079(3) Uani 1 1 d . . . H9A H 0.7823 0.7543 0.4794 0.119 Uiso 1 1 calc R . . H9B H 0.7877 0.8934 0.4832 0.119 Uiso 1 1 calc R . . H9C H 0.6521 0.8341 0.4821 0.119 Uiso 1 1 calc R . . C10 C 0.4458(9) 0.7140(7) 0.6482(7) 0.073(2) Uani 1 1 d . . . H10A H 0.4395 0.7805 0.5915 0.110 Uiso 1 1 calc R . . H10B H 0.3653 0.7101 0.7033 0.110 Uiso 1 1 calc R . . H10C H 0.4553 0.6375 0.6270 0.110 Uiso 1 1 calc R . . C11 C 0.4670(11) 0.6423(7) 0.8791(6) 0.092(3) Uani 1 1 d . . . H11A H 0.4691 0.5546 0.8859 0.138 Uiso 1 1 calc R . . H11B H 0.3802 0.6721 0.8712 0.138 Uiso 1 1 calc R . . H11C H 0.4821 0.6609 0.9392 0.138 Uiso 1 1 calc R . . C12 C 0.7597(12) 0.7100(9) 0.8797(8) 0.107(4) Uani 1 1 d . . . H12A H 0.6968 0.7366 0.9349 0.161 Uiso 1 1 calc R . . H12B H 0.8436 0.7555 0.8617 0.161 Uiso 1 1 calc R . . H12C H 0.7755 0.6235 0.9009 0.161 Uiso 1 1 calc R . . C13 C 0.3280(7) 0.9574(6) 0.7466(5) 0.0502(18) Uani 1 1 d . . . H13 H 0.3500 0.9609 0.6766 0.060 Uiso 1 1 calc R . . C14 C 0.1988(8) 0.9792(7) 0.7934(6) 0.059(2) Uani 1 1 d . . . H14 H 0.1355 0.9979 0.7552 0.071 Uiso 1 1 calc R . . C15 C 0.1591(8) 0.9738(7) 0.8989(6) 0.0544(19) Uani 1 1 d . . . C16 C 0.2628(8) 0.9472(7) 0.9479(6) 0.059(2) Uani 1 1 d . . . H16 H 0.2443 0.9437 1.0177 0.071 Uiso 1 1 calc R . . C17 C 0.3911(8) 0.9263(6) 0.8952(5) 0.0513(18) Uani 1 1 d . . . H17 H 0.4573 0.9077 0.9307 0.062 Uiso 1 1 calc R . . C18 C 0.0218(8) 0.9960(7) 0.9522(6) 0.063(2) Uani 1 1 d . . . H18 H -0.0422 1.0057 0.9146 0.075 Uiso 1 1 calc R . . O1 O 0.1107(12) 0.5399(12) 0.8282(11) 0.203(5) Uiso 1 1 d D . . C19 C 0.077(3) 0.4155(15) 0.8979(13) 0.399(19) Uiso 1 1 d D . . H19A H -0.0155 0.3931 0.9031 0.479 Uiso 1 1 calc R . . H19B H 0.0827 0.4185 0.9658 0.479 Uiso 1 1 calc R . . C20 C 0.1765(14) 0.3114(12) 0.8589(10) 0.149(5) Uiso 1 1 d D . . H20A H 0.2576 0.3066 0.8829 0.178 Uiso 1 1 calc R . . H20B H 0.1315 0.2309 0.8811 0.178 Uiso 1 1 calc R . . C21 C 0.2093(17) 0.3591(14) 0.7413(10) 0.184(7) Uiso 1 1 d D . . H21A H 0.1682 0.3069 0.7101 0.221 Uiso 1 1 calc R . . H21B H 0.3061 0.3663 0.7101 0.221 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 Co1 0.0634(7) 0.0331(5) 0.0381(6) -0.0099(4) -0.0144(5) 0.0113(4) S1 0.0833(14) 0.0382(10) 0.0382(10) -0.0090(8) -0.0163(10) 0.0120(9) S2 0.0689(13) 0.0430(11) 0.0492(11) -0.0102(8) -0.0258(10) 0.0089(9) N1 0.065(4) 0.039(3) 0.038(3) -0.008(3) -0.013(3) 0.006(3) B3 0.063(6) 0.057(6) 0.066(6) 0.003(5) -0.012(5) -0.003(5) B4 0.082(7) 0.042(5) 0.061(6) 0.002(4) -0.010(6) 0.000(5) B5 0.093(7) 0.036(5) 0.059(6) -0.012(4) -0.020(6) 0.019(5) B6 0.075(6) 0.045(5) 0.047(5) -0.020(4) -0.018(5) 0.014(4) B7 0.086(8) 0.056(6) 0.096(8) -0.012(6) -0.041(7) -0.007(5) B8 0.081(8) 0.065(7) 0.112(10) 0.004(7) -0.020(8) -0.018(6) B9 0.102(8) 0.035(5) 0.102(9) -0.006(5) -0.032(7) 0.001(5) B10 0.113(9) 0.043(5) 0.074(7) -0.021(5) -0.037(7) 0.026(6) B11 0.109(9) 0.046(6) 0.074(7) -0.023(5) -0.043(7) 0.010(5) B12 0.118(10) 0.045(6) 0.114(10) -0.027(6) -0.057(8) 0.004(6) C1 0.067(5) 0.045(4) 0.043(4) -0.011(3) -0.006(4) 0.010(4) C2 0.063(5) 0.044(4) 0.055(5) -0.013(4) -0.023(4) 0.009(4) C3 0.073(6) 0.047(5) 0.074(6) -0.019(4) -0.027(5) 0.029(4) C4 0.089(6) 0.029(4) 0.051(5) -0.012(3) -0.007(5) 0.012(4) C5 0.084(6) 0.031(4) 0.042(4) -0.011(3) -0.020(4) 0.014(4) C6 0.095(7) 0.031(4) 0.047(5) -0.008(3) -0.011(5) 0.003(4) C7 0.113(8) 0.029(4) 0.067(6) -0.013(4) -0.041(6) 0.028(5) C8 0.073(7) 0.104(9) 0.130(10) -0.048(8) -0.010(7) 0.026(6) C9 0.127(8) 0.046(5) 0.052(5) -0.016(4) 0.001(5) 0.011(5) C10 0.102(7) 0.051(5) 0.076(6) -0.022(4) -0.033(6) 0.000(5) C11 0.170(10) 0.043(5) 0.048(5) -0.001(4) -0.008(6) -0.005(6) C12 0.177(11) 0.067(7) 0.108(8) -0.021(6) -0.095(8) 0.040(7) C13 0.061(5) 0.053(5) 0.037(4) -0.013(3) -0.013(4) 0.012(4) C14 0.067(6) 0.063(5) 0.050(5) -0.014(4) -0.023(4) 0.010(4) C15 0.055(5) 0.059(5) 0.050(5) -0.016(4) -0.013(4) 0.010(4) C16 0.071(5) 0.072(6) 0.034(4) -0.012(4) -0.015(4) 0.013(4) C17 0.058(5) 0.050(5) 0.042(4) -0.003(3) -0.015(4) 0.009(4) C18 0.064(5) 0.066(5) 0.060(5) -0.015(4) -0.022(5) 0.011(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 C22 O1 1.484(9) . ? C22 C21 1.597(9) . ? Co1 N1 2.000(6) . ? Co1 C7 2.070(7) . ? Co1 C3 2.073(7) . ? Co1 C5 2.078(7) . ? Co1 C4 2.089(7) . ? Co1 C6 2.091(7) . ? Co1 S1 2.255(2) . ? Co1 S2 2.256(2) . ? S1 C1 1.774(7) . ? S2 C2 1.784(7) . ? N1 C13 1.327(8) . ? N1 C17 1.338(8) . ? B3 C2 1.709(12) . ? B3 C1 1.712(12) . ? B3 B8 1.753(15) . ? B3 B7 1.770(15) . ? B3 B4 1.772(13) . ? B4 C1 1.708(12) . ? B4 B8 1.759(16) . ? B4 B9 1.763(13) . ? B4 B5 1.764(14) . ? B5 C1 1.738(10) . ? B5 B9 1.744(15) . ? B5 B10 1.778(13) . ? B5 B6 1.788(12) . ? B6 C2 1.725(11) . ? B6 C1 1.743(11) . ? B6 B11 1.765(13) . ? B6 B10 1.769(13) . ? B7 C2 1.693(12) . ? B7 B11 1.756(16) . ? B7 B12 1.764(14) . ? B7 B8 1.770(16) . ? B8 B9 1.765(16) . ? B8 B12 1.786(17) . ? B9 B10 1.758(16) . ? B9 B12 1.797(16) . ? B10 B12 1.753(16) . ? B10 B11 1.770(13) . ? B11 C2 1.713(11) . ? B11 B12 1.762(16) . ? C1 C2 1.648(10) . ? C3 C4 1.406(11) . ? C3 C7 1.451(12) . ? C3 C8 1.476(12) . ? C4 C5 1.409(11) . ? C4 C9 1.501(10) . ? C5 C6 1.431(10) . ? C5 C10 1.485(11) . ? C6 C7 1.363(12) . ? C6 C11 1.485(11) . ? C7 C12 1.505(11) . ? C13 C14 1.351(10) . ? C14 C15 1.403(10) . ? C15 C16 1.393(10) . ? C15 C18 1.447(10) . ? C16 C17 1.365(10) . ? C18 C18 1.309(14) 2_577 ? O1 C19 1.486(10) . ? C19 C20 1.608(9) . ? C20 C21 1.543(9) . ? 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 O1 C22 C21 116.7(10) . . ? N1 Co1 C7 119.5(3) . . ? N1 Co1 C3 157.9(3) . . ? C7 Co1 C3 41.0(3) . . ? N1 Co1 C5 97.2(3) . . ? C7 Co1 C5 66.1(3) . . ? C3 Co1 C5 67.0(3) . . ? N1 Co1 C4 133.5(3) . . ? C7 Co1 C4 66.5(3) . . ? C3 Co1 C4 39.5(3) . . ? C5 Co1 C4 39.5(3) . . ? N1 Co1 C6 91.0(3) . . ? C7 Co1 C6 38.2(3) . . ? C3 Co1 C6 67.0(3) . . ? C5 Co1 C6 40.1(3) . . ? C4 Co1 C6 66.5(3) . . ? N1 Co1 S1 93.09(17) . . ? C7 Co1 S1 147.1(3) . . ? C3 Co1 S1 106.2(3) . . ? C5 Co1 S1 108.2(2) . . ? C4 Co1 S1 88.5(2) . . ? C6 Co1 S1 148.4(2) . . ? N1 Co1 S2 94.50(17) . . ? C7 Co1 S2 89.0(2) . . ? C3 Co1 S2 95.1(2) . . ? C5 Co1 S2 155.1(2) . . ? C4 Co1 S2 131.9(3) . . ? C6 Co1 S2 118.0(2) . . ? S1 Co1 S2 92.91(8) . . ? C1 S1 Co1 105.3(2) . . ? C2 S2 Co1 105.7(2) . . ? C13 N1 C17 116.9(6) . . ? C13 N1 Co1 123.0(5) . . ? C17 N1 Co1 120.0(5) . . ? C2 B3 C1 57.6(5) . . ? C2 B3 B8 104.7(7) . . ? C1 B3 B8 105.0(7) . . ? C2 B3 B7 58.2(5) . . ? C1 B3 B7 104.8(7) . . ? B8 B3 B7 60.3(6) . . ? C2 B3 B4 104.8(6) . . ? C1 B3 B4 58.7(5) . . ? B8 B3 B4 59.8(6) . . ? B7 B3 B4 107.9(7) . . ? C1 B4 B8 104.9(7) . . ? C1 B4 B9 105.5(7) . . ? B8 B4 B9 60.2(6) . . ? C1 B4 B5 60.0(5) . . ? B8 B4 B5 107.6(7) . . ? B9 B4 B5 59.3(6) . . ? C1 B4 B3 58.9(5) . . ? B8 B4 B3 59.5(6) . . ? B9 B4 B3 108.0(7) . . ? B5 B4 B3 108.8(7) . . ? C1 B5 B9 105.1(7) . . ? C1 B5 B4 58.4(5) . . ? B9 B5 B4 60.3(6) . . ? C1 B5 B10 104.8(6) . . ? B9 B5 B10 59.9(6) . . ? B4 B5 B10 107.8(8) . . ? C1 B5 B6 59.2(4) . . ? B9 B5 B6 107.8(7) . . ? B4 B5 B6 107.9(6) . . ? B10 B5 B6 59.5(5) . . ? C2 B6 C1 56.7(4) . . ? C2 B6 B11 58.8(5) . . ? C1 B6 B11 104.8(7) . . ? C2 B6 B10 104.5(7) . . ? C1 B6 B10 105.0(7) . . ? B11 B6 B10 60.1(5) . . ? C2 B6 B5 104.3(6) . . ? C1 B6 B5 59.0(4) . . ? B11 B6 B5 108.1(7) . . ? B10 B6 B5 60.0(5) . . ? C2 B7 B11 59.5(5) . . ? C2 B7 B12 105.9(7) . . ? B11 B7 B12 60.1(6) . . ? C2 B7 B8 104.7(7) . . ? B11 B7 B8 108.3(8) . . ? B12 B7 B8 60.7(7) . . ? C2 B7 B3 59.1(5) . . ? B11 B7 B3 109.0(7) . . ? B12 B7 B3 108.9(8) . . ? B8 B7 B3 59.4(6) . . ? B3 B8 B4 60.6(6) . . ? B3 B8 B9 108.8(8) . . ? B4 B8 B9 60.0(6) . . ? B3 B8 B7 60.3(6) . . ? B4 B8 B7 108.5(8) . . ? B9 B8 B7 108.1(9) . . ? B3 B8 B12 108.6(8) . . ? B4 B8 B12 109.0(8) . . ? B9 B8 B12 60.8(7) . . ? B7 B8 B12 59.5(6) . . ? B5 B9 B10 61.0(6) . . ? B5 B9 B4 60.4(5) . . ? B10 B9 B4 108.7(7) . . ? B5 B9 B8 108.2(7) . . ? B10 B9 B8 107.4(8) . . ? B4 B9 B8 59.8(6) . . ? B5 B9 B12 108.4(8) . . ? B10 B9 B12 59.1(6) . . ? B4 B9 B12 108.3(7) . . ? B8 B9 B12 60.2(6) . . ? B12 B10 B9 61.6(7) . . ? B12 B10 B6 108.5(7) . . ? B9 B10 B6 108.0(7) . . ? B12 B10 B11 60.0(6) . . ? B9 B10 B11 108.8(8) . . ? B6 B10 B11 59.8(5) . . ? B12 B10 B5 108.9(8) . . ? B9 B10 B5 59.1(6) . . ? B6 B10 B5 60.5(5) . . ? B11 B10 B5 108.3(6) . . ? C2 B11 B7 58.4(5) . . ? C2 B11 B12 105.2(8) . . ? B7 B11 B12 60.2(6) . . ? C2 B11 B6 59.4(5) . . ? B7 B11 B6 108.2(7) . . ? B12 B11 B6 108.3(7) . . ? C2 B11 B10 105.0(6) . . ? B7 B11 B10 107.4(8) . . ? B12 B11 B10 59.5(6) . . ? B6 B11 B10 60.1(5) . . ? B10 B12 B11 60.5(6) . . ? B10 B12 B7 107.8(7) . . ? B11 B12 B7 59.7(6) . . ? B10 B12 B8 106.7(8) . . ? B11 B12 B8 107.3(7) . . ? B7 B12 B8 59.8(6) . . ? B10 B12 B9 59.4(6) . . ? B11 B12 B9 107.4(7) . . ? B7 B12 B9 106.9(7) . . ? B8 B12 B9 59.0(6) . . ? C2 C1 B4 110.5(6) . . ? C2 C1 B3 61.1(5) . . ? B4 C1 B3 62.4(5) . . ? C2 C1 B5 110.1(5) . . ? B4 C1 B5 61.6(5) . . ? B3 C1 B5 112.8(6) . . ? C2 C1 B6 61.1(4) . . ? B4 C1 B6 112.6(6) . . ? B3 C1 B6 113.1(6) . . ? B5 C1 B6 61.8(5) . . ? C2 C1 S1 117.9(5) . . ? B4 C1 S1 121.7(5) . . ? B3 C1 S1 116.7(5) . . ? B5 C1 S1 122.7(6) . . ? B6 C1 S1 118.1(5) . . ? C1 C2 B7 111.4(7) . . ? C1 C2 B3 61.3(5) . . ? B7 C2 B3 62.7(6) . . ? C1 C2 B11 111.7(6) . . ? B7 C2 B11 62.1(6) . . ? B3 C2 B11 114.0(7) . . ? C1 C2 B6 62.2(4) . . ? B7 C2 B6 113.1(6) . . ? B3 C2 B6 114.2(6) . . ? B11 C2 B6 61.8(5) . . ? C1 C2 S2 116.4(5) . . ? B7 C2 S2 121.5(5) . . ? B3 C2 S2 115.5(5) . . ? B11 C2 S2 122.6(6) . . ? B6 C2 S2 117.9(5) . . ? C4 C3 C7 106.0(8) . . ? C4 C3 C8 127.4(9) . . ? C7 C3 C8 126.4(9) . . ? C4 C3 Co1 70.9(4) . . ? C7 C3 Co1 69.4(4) . . ? C8 C3 Co1 128.1(6) . . ? C3 C4 C5 108.9(7) . . ? C3 C4 C9 125.5(8) . . ? C5 C4 C9 125.5(8) . . ? C3 C4 Co1 69.6(4) . . ? C5 C4 Co1 69.8(4) . . ? C9 C4 Co1 128.4(5) . . ? C4 C5 C6 107.5(7) . . ? C4 C5 C10 126.5(7) . . ? C6 C5 C10 125.8(8) . . ? C4 C5 Co1 70.6(4) . . ? C6 C5 Co1 70.4(4) . . ? C10 C5 Co1 127.9(5) . . ? C7 C6 C5 108.2(8) . . ? C7 C6 C11 125.3(8) . . ? C5 C6 C11 126.5(9) . . ? C7 C6 Co1 70.0(4) . . ? C5 C6 Co1 69.5(4) . . ? C11 C6 Co1 128.4(5) . . ? C6 C7 C3 109.4(7) . . ? C6 C7 C12 126.9(9) . . ? C3 C7 C12 123.6(9) . . ? C6 C7 Co1 71.7(4) . . ? C3 C7 Co1 69.6(4) . . ? C12 C7 Co1 127.7(5) . . ? N1 C13 C14 123.8(7) . . ? C13 C14 C15 120.7(7) . . ? C16 C15 C14 114.7(7) . . ? C16 C15 C18 122.7(7) . . ? C14 C15 C18 122.6(7) . . ? C17 C16 C15 121.0(7) . . ? N1 C17 C16 122.7(7) . . ? C18 C18 C15 126.9(10) 2_577 . ? C22 O1 C19 93.2(11) . . ? O1 C19 C20 112.5(12) . . ? C21 C20 C19 101.9(7) . . ? C20 C21 C22 99.9(7) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.327 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.102