# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_address ; Laboratory of Molecular Catalysis and Innovative Material Fudan University Department of Chemistry Shanghai 200433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Route to Multicluster Containing Ancillary ortho-Carborane-1,2-Dithiolato Ligands ; loop_ _publ_author_name 'Guo-Xin Jin' 'Chun-Xia Ren' 'Jianqiang Wang' data_f41110b _database_code_depnum_ccdc_archive 'CCDC 267768' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H57 Cl6 Ir3 N6' _chemical_formula_weight 1507.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRIGONAL _symmetry_space_group_name_H-M R3m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+1/3' '-x+y+2/3, y+1/3, z+1/3' 'x+2/3, x-y+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+2/3' '-x+y+1/3, y+2/3, z+2/3' 'x+1/3, x-y+2/3, z+2/3' _cell_length_a 24.096(7) _cell_length_b 24.096(7) _cell_length_c 7.479(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3761(2) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 720 _cell_measurement_theta_min 2.893 _cell_measurement_theta_max 26.056 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 8.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4907 _exptl_absorpt_correction_T_max 0.6816 _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 5271 _diffrn_reflns_av_R_equivalents 0.1157 _diffrn_reflns_av_sigmaI/netI 0.1421 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.01 _reflns_number_total 1572 _reflns_number_gt 1066 _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. The C2 C4 C5 C6 atoms of the Cp ring is disordered in some way. The C2 C4 C5 C6 atoms were refined with anisotropic restraints. The 25 restraints refer to anisotropical B parameters of C2 C4 C5 C6. The Cp ring was not modelled as disordered. ; _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^)+(0.0365P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 1572 _refine_ls_number_parameters 106 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 0.900 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 -0.03599(4) 0.48200(2) 0.1669 0.0383(3) Uani 1 2 d S . . Cl1 Cl -0.0442(3) 0.4080(3) -0.0605(7) 0.0586(15) Uani 1 1 d . . . C1 C -0.0238(11) 0.4881(6) 0.458(3) 0.048(7) Uani 1 2 d S . . C2 C -0.0599(9) 0.4218(8) 0.406(2) 0.051(5) Uani 1 1 d U . . C3 C -0.1178(7) 0.4156(8) 0.314(3) 0.054(6) Uani 1 1 d . . . C4 C 0.0369(14) 0.5184(7) 0.554(4) 0.066(7) Uani 1 2 d SU . . H4A H 0.0508 0.5630 0.5718 0.099 Uiso 0.50 1 calc PR . . H4B H 0.0684 0.5145 0.4851 0.099 Uiso 0.50 1 calc PR . . H4C H 0.0314 0.4978 0.6673 0.099 Uiso 0.50 1 calc PR . . C5 C -0.0400(9) 0.3738(9) 0.443(3) 0.070(6) Uani 1 1 d U . . H5A H -0.0570 0.3538 0.5562 0.105 Uiso 1 1 calc R . . H5B H 0.0059 0.3947 0.4458 0.105 Uiso 1 1 calc R . . H5C H -0.0561 0.3419 0.3504 0.105 Uiso 1 1 calc R . . C6 C -0.1716(10) 0.3503(10) 0.250(3) 0.090(8) Uani 1 1 d U . . H6A H -0.2031 0.3308 0.3431 0.136 Uiso 1 1 calc R . . H6B H -0.1542 0.3232 0.2220 0.136 Uiso 1 1 calc R . . H6C H -0.1913 0.3560 0.1456 0.136 Uiso 1 1 calc R . . C7 C 0.0986(7) 0.5952(7) 0.104(2) 0.029(4) Uani 1 1 d . . . H7A H 0.0767 0.6179 0.1008 0.035 Uiso 1 1 calc R . . C8 C 0.1639(8) 0.6309(7) 0.094(2) 0.033(4) Uani 1 1 d . . . H8A H 0.1845 0.6754 0.0904 0.040 Uiso 1 1 calc R . . C9 C 0.1988(10) 0.5994(5) 0.091(3) 0.030(6) Uani 1 2 d S . . C10 C 0.2701(10) 0.6350(5) 0.079(3) 0.027(5) Uani 1 2 d S . . N1 N 0.0624(8) 0.5312(4) 0.117(2) 0.029(4) Uani 1 2 d S . . N2 N 0.3009(4) 0.6991(4) 0.074(2) 0.038(5) Uani 1 2 d S . . 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 0.0349(7) 0.0389(5) 0.0397(5) 0.0008(3) 0.0015(6) 0.0174(3) Cl1 0.054(3) 0.054(3) 0.054(4) -0.019(3) 0.001(3) 0.017(3) C1 0.048(17) 0.062(13) 0.030(14) 0.015(6) 0.029(13) 0.024(8) C2 0.062(9) 0.050(8) 0.034(8) 0.017(6) 0.013(7) 0.024(7) C3 0.019(9) 0.059(13) 0.068(13) -0.007(10) 0.013(9) 0.009(8) C4 0.067(10) 0.069(9) 0.061(11) -0.001(4) -0.002(8) 0.034(5) C5 0.082(10) 0.064(9) 0.066(9) 0.011(7) -0.001(8) 0.039(8) C6 0.088(11) 0.083(11) 0.083(11) -0.004(8) -0.006(8) 0.030(8) C7 0.022(9) 0.032(9) 0.034(10) 0.019(8) 0.009(7) 0.013(8) C8 0.045(11) 0.022(8) 0.037(10) 0.000(7) -0.017(8) 0.020(8) C9 0.030(14) 0.035(11) 0.023(13) 0.011(5) 0.021(11) 0.015(7) C10 0.036(14) 0.031(10) 0.014(12) -0.006(5) -0.013(10) 0.018(7) N1 0.058(12) 0.027(7) 0.011(9) 0.003(4) 0.007(8) 0.029(6) N2 0.042(9) 0.042(9) 0.028(12) -0.001(5) 0.001(5) 0.020(11) _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 2.086(17) . ? Ir1 C3 2.122(16) 6_565 ? Ir1 C3 2.122(16) . ? Ir1 C1 2.19(2) . ? Ir1 C2 2.191(16) 6_565 ? Ir1 C2 2.191(16) . ? Ir1 Cl1 2.400(5) 6_565 ? Ir1 Cl1 2.400(5) . ? C1 C2 1.44(2) 6_565 ? C1 C2 1.44(2) . ? C1 C4 1.46(3) . ? C2 C5 1.48(2) . ? C2 C3 1.49(2) . ? C3 C3 1.23(3) 6_565 ? C3 C6 1.53(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N1 1.344(17) . ? C7 C8 1.366(19) . ? C7 H7A 0.9300 . ? C8 C9 1.387(17) . ? C8 H8A 0.9300 . ? C9 C8 1.387(17) 6_565 ? C9 C10 1.49(3) . ? C10 N2 1.338(13) 2_665 ? C10 N2 1.338(13) . ? N1 C7 1.344(17) 6_565 ? N2 C10 1.338(13) 3_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C3 152.2(6) . 6_565 ? N1 Ir1 C3 152.2(6) . . ? C3 Ir1 C3 33.8(9) 6_565 . ? N1 Ir1 C1 93.7(8) . . ? C3 Ir1 C1 65.0(8) 6_565 . ? C3 Ir1 C1 65.0(8) . . ? N1 Ir1 C2 111.7(6) . 6_565 ? C3 Ir1 C2 40.5(7) 6_565 6_565 ? C3 Ir1 C2 63.1(7) . 6_565 ? C1 Ir1 C2 38.3(5) . 6_565 ? N1 Ir1 C2 111.7(6) . . ? C3 Ir1 C2 63.1(7) 6_565 . ? C3 Ir1 C2 40.5(7) . . ? C1 Ir1 C2 38.3(5) . . ? C2 Ir1 C2 64.1(10) 6_565 . ? N1 Ir1 Cl1 86.7(3) . 6_565 ? C3 Ir1 Cl1 96.1(5) 6_565 6_565 ? C3 Ir1 Cl1 120.9(5) . 6_565 ? C1 Ir1 Cl1 135.41(14) . 6_565 ? C2 Ir1 Cl1 100.9(5) 6_565 6_565 ? C2 Ir1 Cl1 159.2(5) . 6_565 ? N1 Ir1 Cl1 86.7(3) . . ? C3 Ir1 Cl1 120.9(5) 6_565 . ? C3 Ir1 Cl1 96.1(5) . . ? C1 Ir1 Cl1 135.41(14) . . ? C2 Ir1 Cl1 159.2(5) 6_565 . ? C2 Ir1 Cl1 100.9(5) . . ? Cl1 Ir1 Cl1 89.2(3) 6_565 . ? C2 C1 C2 108(2) 6_565 . ? C2 C1 C4 126.0(12) 6_565 . ? C2 C1 C4 126.0(12) . . ? C2 C1 Ir1 71.0(11) 6_565 . ? C2 C1 Ir1 71.0(11) . . ? C4 C1 Ir1 126.2(16) . . ? C1 C2 C5 124.5(18) . . ? C1 C2 C3 104.5(16) . . ? C5 C2 C3 131.1(16) . . ? C1 C2 Ir1 70.7(11) . . ? C5 C2 Ir1 126.0(13) . . ? C3 C2 Ir1 67.3(9) . . ? C3 C3 C2 111.5(9) 6_565 . ? C3 C3 C6 127.1(11) 6_565 . ? C2 C3 C6 121.1(16) . . ? C3 C3 Ir1 73.1(5) 6_565 . ? C2 C3 Ir1 72.3(8) . . ? C6 C3 Ir1 127.1(14) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 127.6(14) . . ? N1 C7 H7A 116.2 . . ? C8 C7 H7A 116.2 . . ? C7 C8 C9 118.6(15) . . ? C7 C8 H8A 120.7 . . ? C9 C8 H8A 120.7 . . ? C8 C9 C8 117(2) . 6_565 ? C8 C9 C10 121.7(10) . . ? C8 C9 C10 121.7(10) 6_565 . ? N2 C10 N2 122(2) 2_665 . ? N2 C10 C9 118.8(11) 2_665 . ? N2 C10 C9 118.8(11) . . ? C7 N1 C7 110.8(18) . 6_565 ? C7 N1 Ir1 124.5(9) . . ? C7 N1 Ir1 124.5(9) 6_565 . ? C10 N2 C10 117(2) 3_565 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.914 _refine_diff_density_min -0.899 _refine_diff_density_rms 0.191 data_f50124e _database_code_depnum_ccdc_archive 'CCDC 267769' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H87 B30 Ir3 N6 S6' _chemical_formula_weight 1913.56 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/ncm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z' 'y, x, z' _cell_length_a 35.258(6) _cell_length_b 35.258(6) _cell_length_c 16.150(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20076(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 938 _cell_measurement_theta_min 2.311 _cell_measurement_theta_max 16.756 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7440 _exptl_absorpt_coefficient_mu 4.124 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4926 _exptl_absorpt_correction_T_max 0.7338 _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 81696 _diffrn_reflns_av_R_equivalents 0.1202 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 0.82 _diffrn_reflns_theta_max 25.01 _reflns_number_total 9083 _reflns_number_gt 6216 _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.The C27 C28 C29 atoms of the Cp ring is disordered in some way and refined with anisotropic restraints. The 18 restraints refer to anisotropical B parameters of C27 C28 C29 (there are six anisotropical B parameters for each atom). ; _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^)+(0.1065P)^2^+71.6900P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9083 _refine_ls_number_parameters 474 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.2177 _refine_ls_wR_factor_gt 0.1930 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.155 _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 0.937097(14) 0.296670(12) 0.06301(3) 0.04378(18) Uani 1 1 d . . . Ir2 Ir 0.870055(17) 0.629945(17) -0.25839(6) 0.0727(3) Uani 1 2 d S . . S1 S 0.97025(10) 0.30606(9) 0.1879(2) 0.0554(8) Uani 1 1 d . . . S2 S 0.88498(9) 0.33181(9) 0.1136(2) 0.0511(8) Uani 1 1 d . . . S3 S 0.82734(11) 0.60563(12) -0.1599(3) 0.0831(12) Uani 1 1 d . . . N1 N 0.9606(3) 0.3474(2) 0.0162(5) 0.038(2) Uani 1 1 d . . . N2 N 0.9106(3) 0.5894(3) -0.2207(9) 0.056(4) Uani 1 2 d S . . B3 B 0.8999(5) 0.3125(4) 0.2910(10) 0.060(4) Uani 1 1 d . . . H3 H 0.8927 0.2825 0.2813 0.072 Uiso 1 1 calc R . . B4 B 0.9373(5) 0.3264(5) 0.3557(9) 0.062(4) Uani 1 1 d . . . H4 H 0.9549 0.3055 0.3884 0.074 Uiso 1 1 calc R . . B5 B 0.9568(5) 0.3686(4) 0.3145(10) 0.057(4) Uani 1 1 d . . . H5 H 0.9871 0.3753 0.3208 0.069 Uiso 1 1 calc R . . B6 B 0.9325(4) 0.3801(4) 0.2246(9) 0.047(3) Uani 1 1 d . . . H6 H 0.9466 0.3940 0.1720 0.057 Uiso 1 1 calc R . . B7 B 0.8646(5) 0.3475(5) 0.2930(10) 0.067(5) Uani 1 1 d . . . H7 H 0.8344 0.3407 0.2850 0.080 Uiso 1 1 calc R . . B8 B 0.8900(5) 0.3358(6) 0.3857(12) 0.080(6) Uani 1 1 d . . . H8 H 0.8764 0.3211 0.4381 0.096 Uiso 1 1 calc R . . B9 B 0.9247(5) 0.3712(5) 0.4017(11) 0.068(5) Uani 1 1 d . . . H9 H 0.9335 0.3796 0.4644 0.082 Uiso 1 1 calc R . . B10 B 0.9220(5) 0.4040(4) 0.3186(10) 0.065(5) Uani 1 1 d . . . H10 H 0.9293 0.4341 0.3276 0.078 Uiso 1 1 calc R . . B11 B 0.8846(4) 0.3898(4) 0.2523(10) 0.054(4) Uani 1 1 d . . . H11 H 0.8672 0.4104 0.2178 0.064 Uiso 1 1 calc R . . B12 B 0.8812(6) 0.3842(5) 0.3615(10) 0.071(5) Uani 1 1 d . . . H12 H 0.8616 0.4015 0.3986 0.085 Uiso 1 1 calc R . . B13 B 0.8337(6) 0.6096(7) 0.0265(15) 0.100(7) Uani 1 1 d . . . H13 H 0.8262 0.5796 0.0347 0.120 Uiso 1 1 calc R . . B14 B 0.8777(5) 0.6223(5) -0.016(2) 0.085(9) Uani 1 2 d S . . H14 H 0.8989 0.6011 -0.0349 0.102 Uiso 1 2 calc SR . . B15 B 0.7983(6) 0.6438(6) -0.0017(16) 0.096(7) Uani 1 1 d . . . H15 H 0.7685 0.6358 -0.0115 0.115 Uiso 1 1 calc R . . B16 B 0.8211(6) 0.6789(6) -0.064(2) 0.095(9) Uani 1 2 d S . . H16 H 0.8061 0.6939 -0.1138 0.114 Uiso 1 2 calc SR . . B17 B 0.8123(8) 0.6877(8) 0.040(3) 0.142(16) Uani 1 2 d S . . H17 H 0.7910 0.7090 0.0581 0.170 Uiso 1 2 calc SR . . B18 B 0.8684(7) 0.6316(7) 0.0895(16) 0.088(9) Uani 1 2 d S . . H18 H 0.8835 0.6165 0.1391 0.106 Uiso 1 2 calc SR . . B19 B 0.8181(8) 0.6455(7) 0.0998(17) 0.117(8) Uani 1 1 d . . . H19 H 0.8012 0.6392 0.1553 0.140 Uiso 1 1 calc R . . C1 C 0.9398(3) 0.3337(3) 0.2515(7) 0.046(3) Uani 1 1 d . . . C2 C 0.8971(3) 0.3458(3) 0.2136(8) 0.047(3) Uani 1 1 d . . . C3 C 0.8357(4) 0.6310(4) -0.0679(10) 0.072(4) Uani 1 1 d . . . C4 C 0.9060(4) 0.2439(4) 0.0485(9) 0.062(4) Uani 1 1 d . . . C5 C 0.9432(5) 0.2350(3) 0.0657(9) 0.066(4) Uani 1 1 d . . . C6 C 0.9665(4) 0.2509(4) 0.0028(11) 0.068(4) Uani 1 1 d . . . C7 C 0.9431(5) 0.2682(4) -0.0563(9) 0.065(4) Uani 1 1 d . . . C8 C 0.9054(5) 0.2643(4) -0.0277(10) 0.067(4) Uani 1 1 d . . . C9 C 0.8722(6) 0.2328(5) 0.0990(14) 0.145(10) Uani 1 1 d . . . H9A H 0.8597 0.2117 0.0733 0.217 Uiso 1 1 calc R . . H9B H 0.8550 0.2538 0.1025 0.217 Uiso 1 1 calc R . . H9C H 0.8803 0.2257 0.1537 0.217 Uiso 1 1 calc R . . C10 C 0.9552(7) 0.2120(5) 0.1410(14) 0.131(9) Uani 1 1 d . . . H10A H 0.9378 0.2165 0.1856 0.196 Uiso 1 1 calc R . . H10B H 0.9803 0.2194 0.1576 0.196 Uiso 1 1 calc R . . H10C H 0.9551 0.1855 0.1272 0.196 Uiso 1 1 calc R . . C11 C 1.0085(5) 0.2471(6) -0.0090(18) 0.173(14) Uani 1 1 d . . . H11A H 1.0170 0.2654 -0.0489 0.259 Uiso 1 1 calc R . . H11B H 1.0143 0.2220 -0.0285 0.259 Uiso 1 1 calc R . . H11C H 1.0211 0.2514 0.0428 0.259 Uiso 1 1 calc R . . C12 C 0.9572(9) 0.2855(5) -0.1324(11) 0.164(13) Uani 1 1 d . . . H12A H 0.9830 0.2934 -0.1246 0.246 Uiso 1 1 calc R . . H12B H 0.9419 0.3071 -0.1461 0.246 Uiso 1 1 calc R . . H12C H 0.9560 0.2674 -0.1766 0.246 Uiso 1 1 calc R . . C13 C 0.8696(6) 0.2780(6) -0.0724(14) 0.140(10) Uani 1 1 d . . . H13A H 0.8546 0.2565 -0.0886 0.210 Uiso 1 1 calc R . . H13B H 0.8767 0.2921 -0.1207 0.210 Uiso 1 1 calc R . . H13C H 0.8551 0.2938 -0.0360 0.210 Uiso 1 1 calc R . . C14 C 0.9393(4) 0.3701(4) -0.0298(8) 0.052(3) Uani 1 1 d . . . H14A H 0.9140 0.3639 -0.0383 0.062 Uiso 1 1 calc R . . C15 C 0.9535(3) 0.4028(3) -0.0654(8) 0.052(3) Uani 1 1 d . . . H15A H 0.9382 0.4174 -0.1000 0.063 Uiso 1 1 calc R . . C16 C 0.9900(3) 0.4139(3) -0.0501(7) 0.043(3) Uani 1 1 d . . . C17 C 1.0129(3) 0.3894(3) -0.0057(8) 0.049(3) Uani 1 1 d . . . H17A H 1.0385 0.3947 0.0020 0.059 Uiso 1 1 calc R . . C18 C 0.9972(3) 0.3568(3) 0.0270(8) 0.048(3) Uani 1 1 d . . . H18A H 1.0126 0.3408 0.0579 0.057 Uiso 1 1 calc R . . N3 N 1.0394(3) 0.4606(3) -0.0577(9) 0.055(4) Uani 1 2 d S . . C19 C 1.0042(3) 0.4511(3) -0.0786(7) 0.048(3) Uani 1 1 d . . . N4 N 0.9786(3) 0.4735(3) -0.1168(6) 0.047(2) Uani 1 1 d . . . C20 C 0.9917(3) 0.5083(3) -0.1335(10) 0.046(4) Uani 1 2 d S . . C21 C 0.9638(3) 0.5362(3) -0.1705(10) 0.045(4) Uani 1 2 d S . . C22 C 0.9263(3) 0.5261(4) -0.1838(8) 0.058(4) Uani 1 1 d . . . H22A H 0.9186 0.5011 -0.1762 0.070 Uiso 1 1 calc R . . C23 C 0.9007(3) 0.5535(3) -0.2084(6) 0.060(4) Uani 1 1 d . . . H23A H 0.8755 0.5465 -0.2167 0.072 Uiso 1 1 calc R . . C24 C 0.8895(3) 0.6386(3) -0.3835(6) 0.147(12) Uani 1 1 d R . . C25 C 0.8710(3) 0.6706(3) -0.3576(6) 0.190(18) Uani 1 1 d R . . C26 C 0.8359(3) 0.6641(3) -0.3445(6) 0.24(4) Uani 1 2 d SR . . C27 C 0.9274(3) 0.6338(3) -0.4086(6) 0.38(3) Uani 1 1 d RU . . H27A H 0.9283 0.6306 -0.4676 0.569 Uiso 1 1 calc R . . H27B H 0.9378 0.6118 -0.3821 0.569 Uiso 1 1 calc R . . H27C H 0.9419 0.6557 -0.3932 0.569 Uiso 1 1 calc R . . C28 C 0.8756(3) 0.7131(3) -0.3427(6) 0.41(3) Uani 1 1 d RU . . H28A H 0.8518 0.7256 -0.3518 0.611 Uiso 1 1 calc R . . H28B H 0.8942 0.7230 -0.3802 0.611 Uiso 1 1 calc R . . H28C H 0.8837 0.7173 -0.2867 0.611 Uiso 1 1 calc R . . C29 C 0.8059(10) 0.6941(10) -0.325(4) 0.33(4) Uani 1 2 d SU . . H29A H 0.7852 0.6917 -0.3635 0.491 Uiso 0.50 1 calc PR . . H29B H 0.8169 0.7189 -0.3302 0.491 Uiso 0.50 1 calc PR . . H29C H 0.7967 0.6906 -0.2698 0.491 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0529(3) 0.0367(3) 0.0417(3) -0.0013(2) 0.0093(2) -0.0027(2) Ir2 0.0662(4) 0.0662(4) 0.0856(7) 0.0130(3) -0.0130(3) 0.0115(4) S1 0.062(2) 0.059(2) 0.0455(19) -0.0007(16) 0.0018(16) 0.0159(16) S2 0.0487(18) 0.0564(19) 0.0483(19) -0.0064(15) 0.0033(15) 0.0023(14) S3 0.059(2) 0.084(3) 0.107(3) -0.013(3) -0.004(2) -0.008(2) N1 0.046(6) 0.036(5) 0.032(5) 0.000(4) 0.001(4) -0.008(4) N2 0.055(6) 0.055(6) 0.058(10) 0.018(5) -0.018(5) -0.002(7) B3 0.094(12) 0.033(7) 0.053(10) 0.009(7) 0.015(9) -0.005(8) B4 0.093(12) 0.057(9) 0.036(8) 0.012(7) 0.007(8) 0.005(9) B5 0.065(10) 0.039(8) 0.068(11) -0.004(8) -0.017(8) 0.005(7) B6 0.058(9) 0.034(7) 0.050(9) 0.006(6) 0.001(7) -0.007(6) B7 0.067(11) 0.076(11) 0.058(11) -0.006(9) 0.025(8) 0.010(9) B8 0.085(13) 0.096(14) 0.060(12) 0.003(10) 0.027(10) 0.004(11) B9 0.096(13) 0.066(11) 0.043(9) -0.006(8) 0.011(9) -0.003(9) B10 0.103(13) 0.041(8) 0.051(10) -0.020(7) -0.004(9) 0.011(8) B11 0.057(9) 0.041(8) 0.063(10) 0.001(7) 0.008(8) 0.011(6) B12 0.094(14) 0.070(11) 0.048(10) -0.013(9) 0.008(9) -0.007(9) B13 0.095(16) 0.096(16) 0.108(18) 0.004(14) 0.014(14) 0.006(13) B14 0.068(10) 0.068(10) 0.12(3) 0.001(11) -0.001(11) 0.010(13) B15 0.063(12) 0.109(17) 0.117(19) -0.012(15) 0.001(12) 0.007(11) B16 0.087(13) 0.087(13) 0.11(3) -0.013(13) 0.013(13) 0.008(16) B17 0.14(2) 0.14(2) 0.14(4) -0.041(18) 0.041(18) 0.06(3) B18 0.112(15) 0.112(15) 0.040(14) 0.001(11) -0.001(11) -0.005(19) B19 0.14(2) 0.108(19) 0.108(19) -0.013(15) 0.016(17) 0.004(16) C1 0.064(8) 0.040(6) 0.034(6) 0.011(5) 0.001(6) 0.008(6) C2 0.051(7) 0.043(7) 0.048(7) -0.005(6) 0.009(6) -0.002(6) C3 0.053(8) 0.073(10) 0.091(12) -0.002(9) 0.002(8) 0.001(7) C4 0.073(10) 0.036(7) 0.078(11) -0.013(7) 0.025(8) -0.022(7) C5 0.115(14) 0.033(7) 0.052(9) 0.001(6) -0.010(9) 0.002(7) C6 0.066(9) 0.050(8) 0.088(12) -0.039(8) 0.016(9) 0.000(7) C7 0.103(12) 0.047(8) 0.046(8) -0.013(7) 0.021(8) -0.013(8) C8 0.088(11) 0.039(7) 0.074(10) -0.020(7) -0.016(9) -0.004(7) C9 0.16(2) 0.098(14) 0.17(2) -0.039(14) 0.104(17) -0.082(14) C10 0.20(2) 0.046(10) 0.15(2) 0.010(11) -0.069(18) 0.012(12) C11 0.082(14) 0.15(2) 0.29(4) -0.14(2) -0.002(18) 0.045(13) C12 0.36(4) 0.072(12) 0.066(13) -0.008(10) 0.102(19) -0.018(17) C13 0.16(2) 0.091(14) 0.17(2) -0.045(14) -0.113(18) 0.024(14) C14 0.049(7) 0.056(8) 0.050(8) 0.005(6) -0.007(6) -0.013(6) C15 0.050(7) 0.053(7) 0.054(8) 0.017(6) -0.023(6) -0.008(6) C16 0.048(7) 0.038(6) 0.043(7) 0.000(5) 0.000(6) -0.011(5) C17 0.028(6) 0.041(6) 0.077(9) 0.014(6) -0.004(6) -0.002(5) C18 0.041(7) 0.045(7) 0.058(8) 0.011(6) -0.003(6) 0.006(5) N3 0.050(5) 0.050(5) 0.063(10) 0.011(6) -0.011(6) -0.005(7) C19 0.049(7) 0.045(7) 0.050(8) -0.001(6) -0.012(6) -0.010(6) N4 0.048(6) 0.046(6) 0.046(6) 0.008(5) -0.016(5) -0.014(5) C20 0.045(6) 0.045(6) 0.048(10) 0.004(6) -0.004(6) -0.019(8) C21 0.048(6) 0.048(6) 0.041(10) 0.006(6) -0.006(6) -0.003(8) C22 0.047(7) 0.055(8) 0.072(9) 0.010(7) -0.007(7) -0.019(6) C23 0.058(8) 0.046(7) 0.074(10) 0.003(7) -0.018(7) 0.001(6) C24 0.084(13) 0.27(3) 0.090(15) 0.083(17) 0.004(11) 0.035(18) C25 0.36(6) 0.089(17) 0.13(2) 0.044(15) -0.09(2) 0.06(2) C26 0.26(6) 0.26(6) 0.22(5) 0.045(18) -0.045(18) 0.21(6) C27 0.25(4) 0.75(8) 0.14(3) 0.19(4) 0.01(3) 0.16(5) C28 0.84(9) 0.15(3) 0.23(4) 0.12(3) -0.26(5) -0.18(4) C29 0.36(5) 0.36(5) 0.26(6) -0.04(3) 0.04(3) 0.22(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 N1 2.111(8) . ? Ir1 C6 2.150(12) . ? Ir1 C8 2.169(13) . ? Ir1 C4 2.172(11) . ? Ir1 C7 2.182(13) . ? Ir1 C5 2.185(12) . ? Ir1 S1 2.355(3) . ? Ir1 S2 2.362(3) . ? Ir2 N2 2.110(14) . ? Ir2 C25 2.150(8) . ? Ir2 C25 2.150(8) 15_775 ? Ir2 C24 2.156(10) . ? Ir2 C24 2.156(10) 15_775 ? Ir2 C26 2.198(8) . ? Ir2 S3 2.352(5) 15_775 ? Ir2 S3 2.352(5) . ? S1 C1 1.777(12) . ? S2 C2 1.741(13) . ? S3 C3 1.761(16) . ? N1 C14 1.325(15) . ? N1 C18 1.346(14) . ? N2 C23 1.331(12) 15_775 ? N2 C23 1.331(12) . ? B3 C1 1.71(2) . ? B3 C2 1.716(19) . ? B3 B4 1.75(2) . ? B3 B7 1.75(2) . ? B3 B8 1.77(2) . ? B3 H3 1.1000 . ? B4 C1 1.705(18) . ? B4 B8 1.77(2) . ? B4 B5 1.77(2) . ? B4 B9 1.80(2) . ? B4 H4 1.1000 . ? B5 C1 1.706(19) . ? B5 B6 1.73(2) . ? B5 B10 1.75(2) . ? B5 B9 1.81(2) . ? B5 H5 1.1000 . ? B6 C1 1.711(17) . ? B6 C2 1.746(17) . ? B6 B10 1.78(2) . ? B6 B11 1.78(2) . ? B6 H6 1.1000 . ? B7 C2 1.722(19) . ? B7 B11 1.78(2) . ? B7 B8 1.79(3) . ? B7 B12 1.80(2) . ? B7 H7 1.1000 . ? B8 B9 1.77(3) . ? B8 B12 1.78(3) . ? B8 H8 1.1000 . ? B9 B12 1.72(3) . ? B9 B10 1.77(2) . ? B9 H9 1.1000 . ? B10 B12 1.74(2) . ? B10 B11 1.77(2) . ? B10 H10 1.1000 . ? B11 C2 1.731(18) . ? B11 B12 1.78(2) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? B13 C3 1.70(3) . ? B13 B14 1.75(3) . ? B13 B18 1.77(3) . ? B13 B15 1.79(3) . ? B13 B19 1.82(3) . ? B13 H13 1.1000 . ? B14 C3 1.73(3) . ? B14 C3 1.73(3) 15_775 ? B14 B13 1.75(3) 15_775 ? B14 B18 1.76(4) . ? B14 H14 1.1000 . ? B15 C3 1.76(3) . ? B15 B17 1.76(3) . ? B15 B19 1.78(3) . ? B15 B16 1.79(3) . ? B15 H15 1.1000 . ? B16 B17 1.74(5) . ? B16 C3 1.77(3) 15_775 ? B16 C3 1.77(3) . ? B16 B15 1.79(3) 15_775 ? B16 H16 1.1000 . ? B17 B15 1.76(3) 15_775 ? B17 B19 1.78(4) 15_775 ? B17 B19 1.78(4) . ? B17 H17 1.1000 . ? B18 B13 1.77(3) 15_775 ? B18 B19 1.85(4) 15_775 ? B18 B19 1.85(4) . ? B18 H18 1.1000 . ? B19 B19 1.81(5) 15_775 ? B19 H19 1.1000 . ? C1 C2 1.678(17) . ? C3 C3 1.66(3) 15_775 ? C4 C5 1.38(2) . ? C4 C8 1.42(2) . ? C4 C9 1.50(2) . ? C5 C6 1.42(2) . ? C5 C10 1.52(2) . ? C6 C7 1.40(2) . ? C6 C11 1.50(2) . ? C7 C8 1.41(2) . ? C7 C12 1.46(2) . ? C8 C13 1.53(2) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.383(16) . ? C14 H14A 0.9300 . ? C15 C16 1.365(16) . ? C15 H15A 0.9300 . ? C16 C17 1.384(15) . ? C16 C19 1.478(16) . ? C17 C18 1.378(15) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? N3 C19 1.329(13) 15_775 ? N3 C19 1.329(13) . ? C19 N4 1.349(15) . ? N4 C20 1.336(11) . ? C20 N4 1.336(11) 15_775 ? C20 C21 1.52(2) . ? C21 C22 1.384(14) 15_775 ? C21 C22 1.384(14) . ? C22 C23 1.382(15) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C25 1.3683 . ? C24 C24 1.40(2) 15_775 ? C24 C27 1.4063 . ? C25 C26 1.2751 . ? C25 C28 1.5245 . ? C26 C25 1.275(17) 15_775 ? C26 C29 1.53(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C6 106.6(5) . . ? N1 Ir1 C8 114.0(5) . . ? C6 Ir1 C8 63.1(6) . . ? N1 Ir1 C4 152.2(5) . . ? C6 Ir1 C4 63.3(5) . . ? C8 Ir1 C4 38.3(5) . . ? N1 Ir1 C7 92.0(4) . . ? C6 Ir1 C7 37.8(6) . . ? C8 Ir1 C7 37.9(6) . . ? C4 Ir1 C7 63.9(5) . . ? N1 Ir1 C5 144.2(5) . . ? C6 Ir1 C5 38.2(6) . . ? C8 Ir1 C5 62.6(5) . . ? C4 Ir1 C5 36.9(5) . . ? C7 Ir1 C5 63.3(5) . . ? N1 Ir1 S1 89.6(3) . . ? C6 Ir1 S1 104.7(5) . . ? C8 Ir1 S1 155.4(4) . . ? C4 Ir1 S1 117.6(5) . . ? C7 Ir1 S1 140.6(5) . . ? C5 Ir1 S1 94.2(4) . . ? N1 Ir1 S2 89.1(3) . . ? C6 Ir1 S2 157.7(4) . . ? C8 Ir1 S2 96.2(4) . . ? C4 Ir1 S2 95.4(4) . . ? C7 Ir1 S2 128.4(5) . . ? C5 Ir1 S2 126.3(5) . . ? S1 Ir1 S2 90.91(11) . . ? N2 Ir2 C25 131.0(4) . . ? N2 Ir2 C25 131.0(4) . 15_775 ? C25 Ir2 C25 57.7(5) . 15_775 ? N2 Ir2 C24 98.7(5) . . ? C25 Ir2 C24 37.05(15) . . ? C25 Ir2 C24 61.0(4) 15_775 . ? N2 Ir2 C24 98.7(5) . 15_775 ? C25 Ir2 C24 61.0(4) . 15_775 ? C25 Ir2 C24 37.05(15) 15_775 15_775 ? C24 Ir2 C24 37.9(5) . 15_775 ? N2 Ir2 C26 157.5(5) . . ? C25 Ir2 C26 34.08(12) . . ? C25 Ir2 C26 34.1(5) 15_775 . ? C24 Ir2 C26 60.2(2) . . ? C24 Ir2 C26 60.2(3) 15_775 . ? N2 Ir2 S3 89.5(3) . 15_775 ? C25 Ir2 S3 94.1(3) . 15_775 ? C25 Ir2 S3 139.2(3) 15_775 15_775 ? C24 Ir2 S3 115.3(3) . 15_775 ? C24 Ir2 S3 152.8(3) 15_775 15_775 ? C26 Ir2 S3 106.1(3) . 15_775 ? N2 Ir2 S3 89.5(3) . . ? C25 Ir2 S3 139.2(3) . . ? C25 Ir2 S3 94.1(3) 15_775 . ? C24 Ir2 S3 152.8(3) . . ? C24 Ir2 S3 115.3(3) 15_775 . ? C26 Ir2 S3 106.1(3) . . ? S3 Ir2 S3 90.6(2) 15_775 . ? C1 S1 Ir1 105.7(4) . . ? C2 S2 Ir1 106.1(4) . . ? C3 S3 Ir2 106.1(5) . . ? C14 N1 C18 117.8(10) . . ? C14 N1 Ir1 119.4(8) . . ? C18 N1 Ir1 122.7(8) . . ? C23 N2 C23 118.5(14) 15_775 . ? C23 N2 Ir2 120.7(7) 15_775 . ? C23 N2 Ir2 120.7(7) . . ? C1 B3 C2 58.5(7) . . ? C1 B3 B4 58.9(8) . . ? C2 B3 B4 106.7(10) . . ? C1 B3 B7 106.4(10) . . ? C2 B3 B7 59.5(8) . . ? B4 B3 B7 109.1(12) . . ? C1 B3 B8 106.4(12) . . ? C2 B3 B8 107.6(11) . . ? B4 B3 B8 60.2(10) . . ? B7 B3 B8 61.2(10) . . ? C1 B3 H3 123.6 . . ? C2 B3 H3 122.8 . . ? B4 B3 H3 121.7 . . ? B7 B3 H3 121.2 . . ? B8 B3 H3 121.6 . . ? C1 B4 B3 59.5(8) . . ? C1 B4 B8 107.0(12) . . ? B3 B4 B8 60.4(10) . . ? C1 B4 B5 58.8(8) . . ? B3 B4 B5 107.6(11) . . ? B8 B4 B5 108.2(12) . . ? C1 B4 B9 106.7(11) . . ? B3 B4 B9 107.8(12) . . ? B8 B4 B9 59.3(10) . . ? B5 B4 B9 60.9(9) . . ? C1 B4 H4 123.1 . . ? B3 B4 H4 121.7 . . ? B8 B4 H4 121.8 . . ? B5 B4 H4 121.6 . . ? B9 B4 H4 122.0 . . ? C1 B5 B6 59.7(7) . . ? C1 B5 B10 106.9(11) . . ? B6 B5 B10 61.3(9) . . ? C1 B5 B4 58.7(8) . . ? B6 B5 B4 108.6(11) . . ? B10 B5 B4 108.3(12) . . ? C1 B5 B9 106.3(11) . . ? B6 B5 B9 109.3(12) . . ? B10 B5 B9 59.7(9) . . ? B4 B5 B9 60.5(9) . . ? C1 B5 H5 123.5 . . ? B6 B5 H5 120.5 . . ? B10 B5 H5 121.6 . . ? B4 B5 H5 121.6 . . ? B9 B5 H5 121.7 . . ? C1 B6 B5 59.4(8) . . ? C1 B6 C2 58.0(7) . . ? B5 B6 C2 106.0(10) . . ? C1 B6 B10 105.6(10) . . ? B5 B6 B10 59.9(9) . . ? C2 B6 B10 105.5(10) . . ? C1 B6 B11 105.2(9) . . ? B5 B6 B11 107.6(11) . . ? C2 B6 B11 58.8(8) . . ? B10 B6 B11 59.7(9) . . ? C1 B6 H6 123.7 . . ? B5 B6 H6 121.8 . . ? C2 B6 H6 123.6 . . ? B10 B6 H6 122.8 . . ? B11 B6 H6 122.5 . . ? C2 B7 B3 59.2(8) . . ? C2 B7 B11 59.3(8) . . ? B3 B7 B11 107.6(11) . . ? C2 B7 B8 106.3(12) . . ? B3 B7 B8 59.9(10) . . ? B11 B7 B8 107.8(13) . . ? C2 B7 B12 105.4(12) . . ? B3 B7 B12 106.6(13) . . ? B11 B7 B12 59.6(9) . . ? B8 B7 B12 59.4(11) . . ? C2 B7 H7 123.3 . . ? B3 B7 H7 122.1 . . ? B11 B7 H7 121.7 . . ? B8 B7 H7 122.1 . . ? B12 B7 H7 123.0 . . ? B4 B8 B9 61.3(10) . . ? B4 B8 B3 59.3(10) . . ? B9 B8 B3 108.5(12) . . ? B4 B8 B12 106.4(13) . . ? B9 B8 B12 58.2(10) . . ? B3 B8 B12 106.7(12) . . ? B4 B8 B7 106.5(12) . . ? B9 B8 B7 107.6(13) . . ? B3 B8 B7 58.9(9) . . ? B12 B8 B7 60.5(10) . . ? B4 B8 H8 122.3 . . ? B9 B8 H8 121.4 . . ? B3 B8 H8 122.2 . . ? B12 B8 H8 122.9 . . ? B7 B8 H8 122.2 . . ? B12 B9 B8 61.3(11) . . ? B12 B9 B10 59.7(10) . . ? B8 B9 B10 108.4(13) . . ? B12 B9 B4 107.3(12) . . ? B8 B9 B4 59.3(10) . . ? B10 B9 B4 105.9(11) . . ? B12 B9 B5 106.1(12) . . ? B8 B9 B5 106.5(11) . . ? B10 B9 B5 58.5(9) . . ? B4 B9 B5 58.7(8) . . ? B12 B9 H9 121.8 . . ? B8 B9 H9 121.3 . . ? B10 B9 H9 122.4 . . ? B4 B9 H9 123.0 . . ? B5 B9 H9 123.6 . . ? B12 B10 B5 107.8(12) . . ? B12 B10 B11 60.8(10) . . ? B5 B10 B11 107.3(10) . . ? B12 B10 B9 58.7(10) . . ? B5 B10 B9 61.7(10) . . ? B11 B10 B9 108.2(12) . . ? B12 B10 B6 108.7(11) . . ? B5 B10 B6 58.9(8) . . ? B11 B10 B6 60.3(8) . . ? B9 B10 B6 109.0(10) . . ? B12 B10 H10 121.8 . . ? B5 B10 H10 122.0 . . ? B11 B10 H10 121.7 . . ? B9 B10 H10 121.2 . . ? B6 B10 H10 121.5 . . ? C2 B11 B10 106.4(10) . . ? C2 B11 B7 58.8(8) . . ? B10 B11 B7 108.0(12) . . ? C2 B11 B12 106.0(11) . . ? B10 B11 B12 58.8(10) . . ? B7 B11 B12 60.9(9) . . ? C2 B11 B6 59.6(7) . . ? B10 B11 B6 60.0(9) . . ? B7 B11 B6 107.9(10) . . ? B12 B11 B6 106.9(12) . . ? C2 B11 H11 123.3 . . ? B10 B11 H11 122.3 . . ? B7 B11 H11 121.3 . . ? B12 B11 H11 122.6 . . ? B6 B11 H11 121.8 . . ? B9 B12 B10 61.6(10) . . ? B9 B12 B11 110.1(13) . . ? B10 B12 B11 60.4(9) . . ? B9 B12 B8 60.5(11) . . ? B10 B12 B8 109.2(13) . . ? B11 B12 B8 108.3(12) . . ? B9 B12 B7 109.2(13) . . ? B10 B12 B7 108.2(12) . . ? B11 B12 B7 59.5(9) . . ? B8 B12 B7 60.1(10) . . ? B9 B12 H12 120.1 . . ? B10 B12 H12 120.9 . . ? B11 B12 H12 121.4 . . ? B8 B12 H12 121.4 . . ? B7 B12 H12 121.9 . . ? C3 B13 B14 60.1(14) . . ? C3 B13 B18 106.9(16) . . ? B14 B13 B18 60.0(15) . . ? C3 B13 B15 60.3(12) . . ? B14 B13 B15 110.3(18) . . ? B18 B13 B15 109.4(19) . . ? C3 B13 B19 106.7(16) . . ? B14 B13 B19 110.1(18) . . ? B18 B13 B19 61.9(15) . . ? B15 B13 B19 59.2(13) . . ? C3 B13 H13 123.0 . . ? B14 B13 H13 120.2 . . ? B18 B13 H13 121.2 . . ? B15 B13 H13 120.7 . . ? B19 B13 H13 121.4 . . ? C3 B14 C3 57.2(14) . 15_775 ? C3 B14 B13 104.4(17) . 15_775 ? C3 B14 B13 58.5(11) 15_775 15_775 ? C3 B14 B13 58.5(11) . . ? C3 B14 B13 104.4(17) 15_775 . ? B13 B14 B13 107(2) 15_775 . ? C3 B14 B18 106.0(18) . . ? C3 B14 B18 106.0(18) 15_775 . ? B13 B14 B18 60.4(13) 15_775 . ? B13 B14 B18 60.5(13) . . ? C3 B14 H14 124.4 . . ? C3 B14 H14 124.4 15_775 . ? B13 B14 H14 122.5 15_775 . ? B13 B14 H14 122.5 . . ? B18 B14 H14 121.7 . . ? C3 B15 B17 104.3(16) . . ? C3 B15 B19 105.9(15) . . ? B17 B15 B19 60.4(18) . . ? C3 B15 B16 59.9(13) . . ? B17 B15 B16 58.6(16) . . ? B19 B15 B16 108.4(18) . . ? C3 B15 B13 57.3(11) . . ? B17 B15 B13 107(2) . . ? B19 B15 B13 61.1(13) . . ? B16 B15 B13 107.2(17) . . ? C3 B15 H15 124.5 . . ? B17 B15 H15 123.2 . . ? B19 B15 H15 121.1 . . ? B16 B15 H15 121.7 . . ? B13 B15 H15 122.2 . . ? B17 B16 C3 105(2) . 15_775 ? B17 B16 C3 105(2) . . ? C3 B16 C3 55.9(13) 15_775 . ? B17 B16 B15 60.0(13) . 15_775 ? C3 B16 B15 59.2(11) 15_775 15_775 ? C3 B16 B15 104.3(19) . 15_775 ? B17 B16 B15 60.0(13) . . ? C3 B16 B15 104.3(19) 15_775 . ? C3 B16 B15 59.2(11) . . ? B15 B16 B15 108(2) 15_775 . ? B17 B16 H16 122.8 . . ? C3 B16 H16 124.8 15_775 . ? C3 B16 H16 124.8 . . ? B15 B16 H16 122.0 15_775 . ? B15 B16 H16 122.0 . . ? B16 B17 B15 61.4(14) . 15_775 ? B16 B17 B15 61.4(14) . . ? B15 B17 B15 110(2) 15_775 . ? B16 B17 B19 111(2) . 15_775 ? B15 B17 B19 60.4(14) 15_775 15_775 ? B15 B17 B19 110(2) . 15_775 ? B16 B17 B19 111(2) . . ? B15 B17 B19 110(2) 15_775 . ? B15 B17 B19 60.4(14) . . ? B19 B17 B19 61(2) 15_775 . ? B16 B17 H17 119.7 . . ? B15 B17 H17 120.6 15_775 . ? B15 B17 H17 120.6 . . ? B19 B17 H17 120.4 15_775 . ? B19 B17 H17 120.4 . . ? B14 B18 B13 59.5(11) . 15_775 ? B14 B18 B13 59.5(11) . . ? B13 B18 B13 106(2) 15_775 . ? B14 B18 B19 108.4(18) . 15_775 ? B13 B18 B19 60.3(13) 15_775 15_775 ? B13 B18 B19 107(2) . 15_775 ? B14 B18 B19 108.4(18) . . ? B13 B18 B19 107(2) 15_775 . ? B13 B18 B19 60.3(13) . . ? B19 B18 B19 58.9(19) 15_775 . ? B14 B18 H18 121.3 . . ? B13 B18 H18 122.7 15_775 . ? B13 B18 H18 122.7 . . ? B19 B18 H18 121.9 15_775 . ? B19 B18 H18 121.9 . . ? B17 B19 B15 59.2(14) . . ? B17 B19 B19 59.4(12) . 15_775 ? B15 B19 B19 107.6(12) . 15_775 ? B17 B19 B13 105(2) . . ? B15 B19 B13 59.7(13) . . ? B19 B19 B13 106.2(12) 15_775 . ? B17 B19 B18 106.4(19) . . ? B15 B19 B18 106.6(17) . . ? B19 B19 B18 60.5(9) 15_775 . ? B13 B19 B18 57.8(12) . . ? B17 B19 H19 123.1 . . ? B15 B19 H19 122.0 . . ? B19 B19 H19 121.8 15_775 . ? B13 B19 H19 123.6 . . ? B18 B19 H19 122.7 . . ? C2 C1 B4 110.6(10) . . ? C2 C1 B5 110.5(9) . . ? B4 C1 B5 62.5(9) . . ? C2 C1 B6 62.0(7) . . ? B4 C1 B6 112.8(10) . . ? B5 C1 B6 61.0(8) . . ? C2 C1 B3 60.8(8) . . ? B4 C1 B3 61.6(9) . . ? B5 C1 B3 112.3(10) . . ? B6 C1 B3 112.8(10) . . ? C2 C1 S1 118.1(8) . . ? B4 C1 S1 121.2(9) . . ? B5 C1 S1 121.8(9) . . ? B6 C1 S1 117.9(8) . . ? B3 C1 S1 118.2(8) . . ? C1 C2 B3 60.7(8) . . ? C1 C2 B7 109.5(10) . . ? B3 C2 B7 61.3(9) . . ? C1 C2 B11 109.0(9) . . ? B3 C2 B11 111.3(10) . . ? B7 C2 B11 61.9(9) . . ? C1 C2 S2 119.1(8) . . ? B3 C2 S2 119.7(9) . . ? B7 C2 S2 122.5(10) . . ? B11 C2 S2 121.7(9) . . ? C1 C2 B6 59.9(7) . . ? B3 C2 B6 111.0(10) . . ? B7 C2 B6 112.0(10) . . ? B11 C2 B6 61.6(8) . . ? S2 C2 B6 117.8(8) . . ? C3 C3 B13 110.1(10) 15_775 . ? C3 C3 B14 61.4(7) 15_775 . ? B13 C3 B14 61.4(12) . . ? C3 C3 B15 110.5(9) 15_775 . ? B13 C3 B15 62.4(12) . . ? B14 C3 B15 113.1(16) . . ? C3 C3 S3 118.6(5) 15_775 . ? B13 C3 S3 121.5(12) . . ? B14 C3 S3 117.6(13) . . ? B15 C3 S3 121.2(11) . . ? C3 C3 B16 62.0(7) 15_775 . ? B13 C3 B16 112.2(16) . . ? B14 C3 B16 113.7(13) . . ? B15 C3 B16 60.9(12) . . ? S3 C3 B16 118.0(14) . . ? C5 C4 C8 107.7(13) . . ? C5 C4 C9 126.1(17) . . ? C8 C4 C9 126.1(18) . . ? C5 C4 Ir1 72.1(7) . . ? C8 C4 Ir1 70.7(7) . . ? C9 C4 Ir1 124.5(10) . . ? C4 C5 C6 108.4(13) . . ? C4 C5 C10 123.2(17) . . ? C6 C5 C10 128.5(18) . . ? C4 C5 Ir1 71.0(7) . . ? C6 C5 Ir1 69.5(7) . . ? C10 C5 Ir1 125.0(10) . . ? C7 C6 C5 108.6(13) . . ? C7 C6 C11 122.3(19) . . ? C5 C6 C11 129(2) . . ? C7 C6 Ir1 72.4(8) . . ? C5 C6 Ir1 72.2(8) . . ? C11 C6 Ir1 126.9(11) . . ? C6 C7 C8 106.7(13) . . ? C6 C7 C12 123.7(19) . . ? C8 C7 C12 130(2) . . ? C6 C7 Ir1 69.9(8) . . ? C8 C7 Ir1 70.5(8) . . ? C12 C7 Ir1 125.8(11) . . ? C7 C8 C4 108.4(14) . . ? C7 C8 C13 126.1(17) . . ? C4 C8 C13 125.4(17) . . ? C7 C8 Ir1 71.5(8) . . ? C4 C8 Ir1 70.9(8) . . ? C13 C8 Ir1 125.3(10) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 122.2(11) . . ? N1 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C16 C15 C14 120.2(11) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C17 117.8(10) . . ? C15 C16 C19 121.1(11) . . ? C17 C16 C19 121.1(10) . . ? C18 C17 C16 118.9(10) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? N1 C18 C17 122.8(10) . . ? N1 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C19 N3 C19 114.1(15) 15_775 . ? N3 C19 N4 126.2(11) . . ? N3 C19 C16 117.5(11) . . ? N4 C19 C16 115.9(10) . . ? C20 N4 C19 113.6(10) . . ? N4 C20 N4 126.3(15) . 15_775 ? N4 C20 C21 116.8(8) . . ? N4 C20 C21 116.8(8) 15_775 . ? C22 C21 C22 118.0(16) 15_775 . ? C22 C21 C20 120.8(8) 15_775 . ? C22 C21 C20 120.8(8) . . ? C23 C22 C21 119.2(12) . . ? C23 C22 H22A 120.4 . . ? C21 C22 H22A 120.4 . . ? N2 C23 C22 122.5(11) . . ? N2 C23 H23A 118.7 . . ? C22 C23 H23A 118.7 . . ? C25 C24 C24 104.3 . 15_775 ? C25 C24 C27 129.8 . . ? C24 C24 C27 125.9 15_775 . ? C25 C24 Ir2 71.3(3) . . ? C24 C24 Ir2 71.0(3) 15_775 . ? C27 C24 Ir2 123.7(3) . . ? C26 C25 C24 111.3 . . ? C26 C25 C28 104.8 . . ? C24 C25 C28 143.8 . . ? C26 C25 Ir2 75.0(3) . . ? C24 C25 Ir2 71.7(3) . . ? C28 C25 Ir2 122.6(3) . . ? C25 C26 C25 108.9(5) 15_775 . ? C25 C26 C29 125.4(9) 15_775 . ? C25 C26 C29 125.4(4) . . ? C25 C26 Ir2 70.92(15) 15_775 . ? C25 C26 Ir2 70.9(3) . . ? C29 C26 Ir2 129(2) . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.267 _refine_diff_density_min -0.851 _refine_diff_density_rms 0.181 data_f50222b _database_code_depnum_ccdc_archive 'CCDC 267770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H62 B20 Cl4 Ir2 N2 S4' _chemical_formula_weight 1393.52 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.223(2) _cell_length_b 11.336(2) _cell_length_c 13.688(3) _cell_angle_alpha 101.052(2) _cell_angle_beta 109.107(3) _cell_angle_gamma 94.826(3) _cell_volume 1452.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5155 _cell_measurement_theta_min 2.180 _cell_measurement_theta_max 28.198 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 678 _exptl_absorpt_coefficient_mu 4.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1917 _exptl_absorpt_correction_T_max 0.6382 _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 6144 _diffrn_reflns_av_R_equivalents 0.0154 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5042 _reflns_number_gt 4729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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. The solvent molecules were disordered. C18, Cl1, Cl2 atoms refined with anisotropic restraint. The 18 restraints refer to anisotropical B parameters of C18 Cl1 Cl2 (there are six anisotropical B parameters for each atom). ; _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^)+(0.0550P)^2^+3.0698P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5042 _refine_ls_number_parameters 317 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0920 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.127 _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 0.81041(2) 0.104482(18) 0.243200(15) 0.02937(10) Uani 1 1 d . . . S1 S 0.68362(16) -0.06774(13) 0.10789(12) 0.0374(3) Uani 1 1 d . . . S2 S 0.98234(15) -0.01060(14) 0.31852(12) 0.0376(3) Uani 1 1 d . . . N1 N 0.6946(5) 0.0535(4) 0.3359(4) 0.0331(10) Uani 1 1 d . . . C1 C 0.7750(6) -0.1914(5) 0.1375(5) 0.0352(13) Uani 1 1 d . . . C2 C 0.9234(6) -0.1628(6) 0.2416(5) 0.0368(13) Uani 1 1 d . . . C3 C 0.5541(7) 0.0303(7) 0.2978(5) 0.0453(16) Uani 1 1 d . . . H3A H 0.5078 0.0272 0.2262 0.054 Uiso 1 1 calc R . . C4 C 0.4758(7) 0.0110(8) 0.3587(5) 0.0517(18) Uani 1 1 d . . . H4A H 0.3784 -0.0021 0.3285 0.062 Uiso 1 1 calc R . . C5 C 0.5398(6) 0.0107(6) 0.4655(5) 0.0367(13) Uani 1 1 d . . . C6 C 0.6850(6) 0.0333(7) 0.5033(5) 0.0433(15) Uani 1 1 d . . . H6A H 0.7342 0.0349 0.5740 0.052 Uiso 1 1 calc R . . C7 C 0.7569(6) 0.0533(6) 0.4380(5) 0.0422(15) Uani 1 1 d . . . H7A H 0.8543 0.0675 0.4664 0.051 Uiso 1 1 calc R . . C8 C 0.7238(7) 0.2628(5) 0.1940(5) 0.0402(14) Uani 1 1 d . . . C9 C 0.8040(7) 0.2185(6) 0.1305(5) 0.0437(15) Uani 1 1 d . . . C10 C 0.9442(7) 0.2259(6) 0.1972(5) 0.0427(15) Uani 1 1 d . . . C11 C 0.9529(7) 0.2782(6) 0.3051(5) 0.0446(15) Uani 1 1 d . . . C12 C 0.8196(7) 0.3008(6) 0.3034(5) 0.0434(15) Uani 1 1 d . . . C13 C 0.5738(8) 0.2797(7) 0.1549(6) 0.0583(19) Uani 1 1 d . . . H13A H 0.5679 0.3592 0.1407 0.087 Uiso 1 1 calc R . . H13B H 0.5335 0.2718 0.2080 0.087 Uiso 1 1 calc R . . H13C H 0.5235 0.2190 0.0908 0.087 Uiso 1 1 calc R . . C14 C 0.7472(9) 0.1766(7) 0.0106(5) 0.059(2) Uani 1 1 d . . . H14A H 0.7585 0.2445 -0.0200 0.088 Uiso 1 1 calc R . . H14B H 0.6495 0.1436 -0.0130 0.088 Uiso 1 1 calc R . . H14C H 0.7975 0.1152 -0.0113 0.088 Uiso 1 1 calc R . . C15 C 1.0657(9) 0.1933(9) 0.1639(7) 0.070(2) Uani 1 1 d . . . H15A H 1.1066 0.2620 0.1463 0.105 Uiso 1 1 calc R . . H15B H 1.0331 0.1260 0.1028 0.105 Uiso 1 1 calc R . . H15C H 1.1349 0.1711 0.2212 0.105 Uiso 1 1 calc R . . C16 C 1.0880(9) 0.3083(8) 0.4003(6) 0.066(2) Uani 1 1 d . . . H16A H 1.1294 0.3911 0.4111 0.099 Uiso 1 1 calc R . . H16B H 1.1518 0.2549 0.3878 0.099 Uiso 1 1 calc R . . H16C H 1.0684 0.2980 0.4624 0.099 Uiso 1 1 calc R . . C17 C 0.7835(10) 0.3569(7) 0.3972(6) 0.064(2) Uani 1 1 d . . . H17A H 0.7986 0.4439 0.4082 0.097 Uiso 1 1 calc R . . H17B H 0.8419 0.3341 0.4592 0.097 Uiso 1 1 calc R . . H17C H 0.6869 0.3288 0.3846 0.097 Uiso 1 1 calc R . . B3 B 0.7764(8) -0.2408(7) 0.2489(6) 0.0433(17) Uani 1 1 d . . . H3 H 0.7201 -0.2041 0.3010 0.052 Uiso 1 1 calc R . . B4 B 0.6870(9) -0.3340(7) 0.1205(7) 0.0488(19) Uani 1 1 d . . . H4 H 0.5722 -0.3585 0.0895 0.059 Uiso 1 1 calc R . . B5 B 0.7836(9) -0.3046(7) 0.0378(7) 0.0478(18) Uani 1 1 d . . . H5 H 0.7306 -0.3101 -0.0474 0.057 Uiso 1 1 calc R . . B6 B 0.9319(8) -0.1929(7) 0.1156(6) 0.0448(17) Uani 1 1 d . . . H6 H 0.9755 -0.1251 0.0821 0.054 Uiso 1 1 calc R . . B7 B 0.9452(10) -0.2849(8) 0.2994(8) 0.059(2) Uani 1 1 d . . . H7 H 0.9985 -0.2775 0.3848 0.071 Uiso 1 1 calc R . . B8 B 0.7967(11) -0.3960(8) 0.2210(8) 0.065(3) Uani 1 1 d . . . H8 H 0.7532 -0.4623 0.2559 0.078 Uiso 1 1 calc R . . B9 B 0.7990(11) -0.4362(8) 0.0893(8) 0.065(2) Uani 1 1 d . . . H9 H 0.7566 -0.5281 0.0380 0.078 Uiso 1 1 calc R . . B10 B 0.9507(10) -0.3481(8) 0.0869(8) 0.061(2) Uani 1 1 d . . . H10 H 1.0072 -0.3826 0.0342 0.073 Uiso 1 1 calc R . . B11 B 1.0398(9) -0.2549(8) 0.2168(8) 0.055(2) Uani 1 1 d . . . H11 H 1.1544 -0.2277 0.2492 0.066 Uiso 1 1 calc R . . B12 B 0.9584(11) -0.4065(8) 0.2000(9) 0.068(3) Uani 1 1 d . . . H12 H 1.0194 -0.4793 0.2205 0.082 Uiso 1 1 calc R . . C18 C 0.424(3) 0.661(2) 0.277(2) 0.217(10) Uani 1 1 d U . . H18A H 0.4919 0.6700 0.2424 0.260 Uiso 1 1 calc R . . H18B H 0.3462 0.7048 0.2530 0.260 Uiso 1 1 calc R . . Cl1 Cl 0.3703(12) 0.4850(11) 0.2927(11) 0.368(6) Uani 1 1 d U . . Cl2 Cl 0.4974(17) 0.6716(14) 0.4239(13) 0.431(8) 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 Ir1 0.03158(14) 0.03102(14) 0.02520(14) 0.00670(9) 0.01065(9) 0.00019(9) S1 0.0393(8) 0.0335(8) 0.0314(7) 0.0037(6) 0.0045(6) 0.0039(6) S2 0.0328(7) 0.0433(8) 0.0327(7) 0.0074(6) 0.0071(6) 0.0056(6) N1 0.032(2) 0.039(3) 0.028(2) 0.006(2) 0.012(2) 0.004(2) C1 0.040(3) 0.032(3) 0.033(3) 0.008(2) 0.014(3) 0.001(2) C2 0.036(3) 0.038(3) 0.038(3) 0.011(3) 0.014(3) 0.010(3) C3 0.038(3) 0.067(5) 0.032(3) 0.018(3) 0.011(3) 0.005(3) C4 0.028(3) 0.094(6) 0.035(3) 0.023(4) 0.010(3) 0.005(3) C5 0.034(3) 0.045(4) 0.033(3) 0.012(3) 0.013(3) 0.004(3) C6 0.031(3) 0.072(5) 0.029(3) 0.016(3) 0.012(3) 0.003(3) C7 0.029(3) 0.063(4) 0.031(3) 0.010(3) 0.009(3) 0.001(3) C8 0.057(4) 0.028(3) 0.036(3) 0.014(2) 0.014(3) 0.004(3) C9 0.057(4) 0.036(3) 0.036(3) 0.012(3) 0.016(3) -0.007(3) C10 0.047(4) 0.042(4) 0.042(3) 0.019(3) 0.018(3) -0.011(3) C11 0.048(4) 0.038(3) 0.041(3) 0.007(3) 0.012(3) -0.011(3) C12 0.059(4) 0.032(3) 0.033(3) 0.005(3) 0.012(3) 0.000(3) C13 0.059(5) 0.047(4) 0.061(5) 0.014(4) 0.009(4) 0.011(3) C14 0.080(5) 0.061(5) 0.032(3) 0.018(3) 0.016(4) 0.000(4) C15 0.064(5) 0.085(6) 0.076(6) 0.024(5) 0.046(5) -0.004(4) C16 0.062(5) 0.070(5) 0.046(4) 0.008(4) 0.002(4) -0.020(4) C17 0.098(6) 0.047(4) 0.049(4) 0.004(3) 0.029(4) 0.019(4) B3 0.051(4) 0.044(4) 0.039(4) 0.020(3) 0.018(3) -0.001(3) B4 0.059(5) 0.033(4) 0.052(5) 0.011(3) 0.019(4) -0.004(3) B5 0.060(5) 0.033(4) 0.049(4) 0.000(3) 0.024(4) 0.002(3) B6 0.049(4) 0.046(4) 0.045(4) 0.009(3) 0.024(4) 0.011(3) B7 0.065(5) 0.054(5) 0.060(5) 0.030(4) 0.013(4) 0.017(4) B8 0.074(6) 0.048(5) 0.076(6) 0.028(5) 0.021(5) 0.009(5) B9 0.082(7) 0.031(4) 0.077(6) 0.005(4) 0.027(5) 0.006(4) B10 0.067(6) 0.045(5) 0.075(6) 0.004(4) 0.034(5) 0.012(4) B11 0.046(4) 0.048(5) 0.072(6) 0.013(4) 0.018(4) 0.022(4) B12 0.078(6) 0.043(5) 0.086(7) 0.024(5) 0.023(5) 0.024(5) C18 0.190(13) 0.249(14) 0.235(13) 0.069(10) 0.095(9) 0.045(9) Cl1 0.288(8) 0.348(9) 0.417(10) -0.075(7) 0.154(7) 0.035(7) Cl2 0.444(11) 0.410(11) 0.434(11) 0.062(9) 0.165(9) 0.071(9) _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 2.120(5) . ? Ir1 C10 2.178(6) . ? Ir1 C9 2.184(6) . ? Ir1 C11 2.188(6) . ? Ir1 C8 2.191(6) . ? Ir1 C12 2.202(6) . ? Ir1 S1 2.3534(15) . ? Ir1 S2 2.3600(15) . ? S1 C1 1.786(6) . ? S2 C2 1.778(6) . ? N1 C7 1.333(8) . ? N1 C3 1.341(8) . ? C1 C2 1.662(8) . ? C1 B5 1.716(9) . ? C1 B4 1.717(9) . ? C1 B3 1.718(9) . ? C1 B6 1.726(10) . ? C2 B7 1.716(10) . ? C2 B3 1.719(10) . ? C2 B11 1.720(9) . ? C2 B6 1.726(10) . ? C3 C4 1.365(9) . ? C3 H3A 0.9300 . ? C4 C5 1.394(9) . ? C4 H4A 0.9300 . ? C5 C6 1.385(9) . ? C5 C5 1.474(12) 2_656 ? C6 C7 1.367(9) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.431(10) . ? C8 C12 1.452(9) . ? C8 C13 1.492(10) . ? C9 C10 1.411(10) . ? C9 C14 1.513(9) . ? C10 C11 1.453(10) . ? C10 C15 1.507(11) . ? C11 C12 1.401(10) . ? C11 C16 1.514(10) . ? C12 C17 1.492(10) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? B3 B4 1.765(11) . ? B3 B8 1.772(12) . ? B3 B7 1.789(12) . ? B3 H3 1.1000 . ? B4 B8 1.772(12) . ? B4 B5 1.786(12) . ? B4 B9 1.786(13) . ? B4 H4 1.1000 . ? B5 B9 1.767(12) . ? B5 B10 1.770(13) . ? B5 B6 1.771(11) . ? B5 H5 1.1000 . ? B6 B10 1.770(11) . ? B6 B11 1.771(12) . ? B6 H6 1.1000 . ? B7 B8 1.771(14) . ? B7 B11 1.772(14) . ? B7 B12 1.789(14) . ? B7 H7 1.1000 . ? B8 B12 1.778(15) . ? B8 B9 1.781(15) . ? B8 H8 1.1000 . ? B9 B12 1.778(15) . ? B9 B10 1.786(14) . ? B9 H9 1.1000 . ? B10 B12 1.779(15) . ? B10 B11 1.779(13) . ? B10 H10 1.1000 . ? B11 B12 1.784(13) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C18 Cl2 1.88(3) . ? C18 Cl1 2.09(3) . ? C18 H18A 0.9700 . ? C18 H18B 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 C10 156.3(2) . . ? N1 Ir1 C9 140.2(2) . . ? C10 Ir1 C9 37.7(3) . . ? N1 Ir1 C11 118.0(2) . . ? C10 Ir1 C11 38.9(3) . . ? C9 Ir1 C11 63.6(2) . . ? N1 Ir1 C8 103.8(2) . . ? C10 Ir1 C8 64.0(3) . . ? C9 Ir1 C8 38.2(3) . . ? C11 Ir1 C8 63.6(3) . . ? N1 Ir1 C12 93.6(2) . . ? C10 Ir1 C12 63.9(3) . . ? C9 Ir1 C12 63.8(2) . . ? C11 Ir1 C12 37.2(3) . . ? C8 Ir1 C12 38.6(2) . . ? N1 Ir1 S1 88.33(14) . . ? C10 Ir1 S1 114.24(18) . . ? C9 Ir1 S1 92.94(17) . . ? C11 Ir1 S1 153.04(19) . . ? C8 Ir1 S1 106.88(17) . . ? C12 Ir1 S1 144.68(17) . . ? N1 Ir1 S2 89.56(13) . . ? C10 Ir1 S2 96.97(19) . . ? C9 Ir1 S2 130.2(2) . . ? C11 Ir1 S2 94.70(19) . . ? C8 Ir1 S2 157.94(18) . . ? C12 Ir1 S2 124.54(18) . . ? S1 Ir1 S2 90.71(5) . . ? C1 S1 Ir1 106.1(2) . . ? C2 S2 Ir1 106.4(2) . . ? C7 N1 C3 116.4(5) . . ? C7 N1 Ir1 121.7(4) . . ? C3 N1 Ir1 121.7(4) . . ? C2 C1 B5 110.4(5) . . ? C2 C1 B4 110.4(5) . . ? B5 C1 B4 62.7(4) . . ? C2 C1 B3 61.1(4) . . ? B5 C1 B3 113.3(5) . . ? B4 C1 B3 61.8(4) . . ? C2 C1 B6 61.2(4) . . ? B5 C1 B6 61.9(4) . . ? B4 C1 B6 113.6(5) . . ? B3 C1 B6 113.3(5) . . ? C2 C1 S1 118.5(4) . . ? B5 C1 S1 121.0(4) . . ? B4 C1 S1 121.5(5) . . ? B3 C1 S1 118.1(4) . . ? B6 C1 S1 116.8(4) . . ? C1 C2 B7 111.0(5) . . ? C1 C2 B3 61.1(4) . . ? B7 C2 B3 62.8(5) . . ? C1 C2 B11 110.6(5) . . ? B7 C2 B11 62.1(5) . . ? B3 C2 B11 113.7(5) . . ? C1 C2 B6 61.2(4) . . ? B7 C2 B6 113.1(5) . . ? B3 C2 B6 113.3(5) . . ? B11 C2 B6 61.8(5) . . ? C1 C2 S2 118.2(4) . . ? B7 C2 S2 121.6(5) . . ? B3 C2 S2 117.7(4) . . ? B11 C2 S2 121.1(5) . . ? B6 C2 S2 117.1(4) . . ? N1 C3 C4 123.3(6) . . ? N1 C3 H3A 118.4 . . ? C4 C3 H3A 118.4 . . ? C3 C4 C5 120.8(6) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 115.2(6) . . ? C6 C5 C5 121.8(7) . 2_656 ? C4 C5 C5 123.0(7) . 2_656 ? C7 C6 C5 121.0(6) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? N1 C7 C6 123.4(6) . . ? N1 C7 H7A 118.3 . . ? C6 C7 H7A 118.3 . . ? C9 C8 C12 107.1(6) . . ? C9 C8 C13 126.7(6) . . ? C12 C8 C13 125.9(6) . . ? C9 C8 Ir1 70.6(3) . . ? C12 C8 Ir1 71.1(3) . . ? C13 C8 Ir1 128.3(5) . . ? C10 C9 C8 109.1(6) . . ? C10 C9 C14 126.0(7) . . ? C8 C9 C14 124.8(7) . . ? C10 C9 Ir1 70.9(3) . . ? C8 C9 Ir1 71.2(3) . . ? C14 C9 Ir1 126.3(5) . . ? C9 C10 C11 107.2(6) . . ? C9 C10 C15 127.2(7) . . ? C11 C10 C15 125.5(7) . . ? C9 C10 Ir1 71.3(4) . . ? C11 C10 Ir1 70.9(3) . . ? C15 C10 Ir1 125.6(5) . . ? C12 C11 C10 108.7(6) . . ? C12 C11 C16 127.4(7) . . ? C10 C11 C16 123.9(7) . . ? C12 C11 Ir1 71.9(4) . . ? C10 C11 Ir1 70.2(3) . . ? C16 C11 Ir1 126.4(5) . . ? C11 C12 C8 108.0(6) . . ? C11 C12 C17 125.9(6) . . ? C8 C12 C17 126.1(7) . . ? C11 C12 Ir1 70.8(4) . . ? C8 C12 Ir1 70.3(3) . . ? C17 C12 Ir1 125.6(5) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C9 C14 H14A 109.5 . . ? C9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 . . ? C1 B3 C2 57.8(4) . . ? C1 B3 B4 59.1(4) . . ? C2 B3 B4 105.7(5) . . ? C1 B3 B8 105.1(6) . . ? C2 B3 B8 104.7(6) . . ? B4 B3 B8 60.1(5) . . ? C1 B3 B7 105.0(6) . . ? C2 B3 B7 58.5(4) . . ? B4 B3 B7 108.1(6) . . ? B8 B3 B7 59.6(5) . . ? C1 B3 H3 124.1 . . ? C2 B3 H3 124.1 . . ? B4 B3 H3 121.7 . . ? B8 B3 H3 123.1 . . ? B7 B3 H3 122.3 . . ? C1 B4 B3 59.1(4) . . ? C1 B4 B8 105.1(6) . . ? B3 B4 B8 60.1(5) . . ? C1 B4 B5 58.6(4) . . ? B3 B4 B5 107.8(6) . . ? B8 B4 B5 107.1(7) . . ? C1 B4 B9 104.9(6) . . ? B3 B4 B9 108.4(6) . . ? B8 B4 B9 60.1(6) . . ? B5 B4 B9 59.3(5) . . ? C1 B4 H4 124.4 . . ? B3 B4 H4 121.2 . . ? B8 B4 H4 122.5 . . ? B5 B4 H4 122.2 . . ? B9 B4 H4 122.3 . . ? C1 B5 B9 105.8(6) . . ? C1 B5 B10 106.0(6) . . ? B9 B5 B10 60.7(5) . . ? C1 B5 B6 59.3(4) . . ? B9 B5 B6 108.6(6) . . ? B10 B5 B6 60.0(5) . . ? C1 B5 B4 58.7(4) . . ? B9 B5 B4 60.4(5) . . ? B10 B5 B4 108.8(6) . . ? B6 B5 B4 108.2(6) . . ? C1 B5 H5 124.0 . . ? B9 B5 H5 121.7 . . ? B10 B5 H5 121.7 . . ? B6 B5 H5 121.4 . . ? B4 B5 H5 121.3 . . ? C2 B6 C1 57.6(4) . . ? C2 B6 B10 105.6(6) . . ? C1 B6 B10 105.5(6) . . ? C2 B6 B11 58.9(4) . . ? C1 B6 B11 105.3(6) . . ? B10 B6 B11 60.3(5) . . ? C2 B6 B5 105.0(5) . . ? C1 B6 B5 58.7(4) . . ? B10 B6 B5 60.0(5) . . ? B11 B6 B5 107.9(6) . . ? C2 B6 H6 124.1 . . ? C1 B6 H6 124.1 . . ? B10 B6 H6 122.4 . . ? B11 B6 H6 121.9 . . ? B5 B6 H6 122.3 . . ? C2 B7 B8 104.9(6) . . ? C2 B7 B11 59.1(4) . . ? B8 B7 B11 107.9(7) . . ? C2 B7 B3 58.7(4) . . ? B8 B7 B3 59.7(5) . . ? B11 B7 B3 107.9(6) . . ? C2 B7 B12 105.4(6) . . ? B8 B7 B12 59.9(6) . . ? B11 B7 B12 60.1(6) . . ? B3 B7 B12 107.8(6) . . ? C2 B7 H7 124.3 . . ? B8 B7 H7 122.5 . . ? B11 B7 H7 121.4 . . ? B3 B7 H7 121.8 . . ? B12 B7 H7 122.2 . . ? B7 B8 B3 60.7(5) . . ? B7 B8 B4 108.6(6) . . ? B3 B8 B4 59.7(4) . . ? B7 B8 B12 60.6(6) . . ? B3 B8 B12 109.1(7) . . ? B4 B8 B12 108.6(7) . . ? B7 B8 B9 108.5(7) . . ? B3 B8 B9 108.3(6) . . ? B4 B8 B9 60.4(5) . . ? B12 B8 B9 59.9(6) . . ? B7 B8 H8 121.2 . . ? B3 B8 H8 121.3 . . ? B4 B8 H8 121.5 . . ? B12 B8 H8 121.2 . . ? B9 B8 H8 121.6 . . ? B5 B9 B12 107.7(6) . . ? B5 B9 B8 107.5(6) . . ? B12 B9 B8 59.9(6) . . ? B5 B9 B10 59.7(5) . . ? B12 B9 B10 59.9(6) . . ? B8 B9 B10 107.5(7) . . ? B5 B9 B4 60.3(5) . . ? B12 B9 B4 108.0(7) . . ? B8 B9 B4 59.6(5) . . ? B10 B9 B4 108.1(6) . . ? B5 B9 H9 121.9 . . ? B12 B9 H9 121.8 . . ? B8 B9 H9 122.2 . . ? B10 B9 H9 121.9 . . ? B4 B9 H9 121.6 . . ? B6 B10 B5 60.1(5) . . ? B6 B10 B12 108.1(6) . . ? B5 B10 B12 107.6(7) . . ? B6 B10 B11 59.9(5) . . ? B5 B10 B11 107.6(6) . . ? B12 B10 B11 60.2(6) . . ? B6 B10 B9 107.8(6) . . ? B5 B10 B9 59.6(5) . . ? B12 B10 B9 59.8(6) . . ? B11 B10 B9 107.8(7) . . ? B6 B10 H10 121.6 . . ? B5 B10 H10 122.1 . . ? B12 B10 H10 121.7 . . ? B11 B10 H10 121.8 . . ? B9 B10 H10 122.0 . . ? C2 B11 B6 59.2(4) . . ? C2 B11 B7 58.8(4) . . ? B6 B11 B7 108.3(6) . . ? C2 B11 B10 105.5(6) . . ? B6 B11 B10 59.8(5) . . ? B7 B11 B10 108.4(7) . . ? C2 B11 B12 105.5(6) . . ? B6 B11 B12 107.8(6) . . ? B7 B11 B12 60.4(6) . . ? B10 B11 B12 59.9(6) . . ? C2 B11 H11 124.1 . . ? B6 B11 H11 121.5 . . ? B7 B11 H11 121.2 . . ? B10 B11 H11 122.2 . . ? B12 B11 H11 122.2 . . ? B9 B12 B8 60.1(6) . . ? B9 B12 B10 60.3(6) . . ? B8 B12 B10 108.0(7) . . ? B9 B12 B11 107.9(6) . . ? B8 B12 B11 107.0(6) . . ? B10 B12 B11 59.9(5) . . ? B9 B12 B7 107.8(7) . . ? B8 B12 B7 59.5(6) . . ? B10 B12 B7 107.6(6) . . ? B11 B12 B7 59.4(5) . . ? B9 B12 H12 121.5 . . ? B8 B12 H12 122.1 . . ? B10 B12 H12 121.6 . . ? B11 B12 H12 122.2 . . ? B7 B12 H12 122.2 . . ? Cl2 C18 Cl1 75.4(11) . . ? Cl2 C18 H18A 115.9 . . ? Cl1 C18 H18A 115.9 . . ? Cl2 C18 H18B 115.9 . . ? Cl1 C18 H18B 115.9 . . ? H18A C18 H18B 112.9 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.480 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.144