# 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 ; Shanghai 200433 CHINA ; _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Pophyrin-carborane organometallic assemblies based on 1, 2-dicarba-closo-dodecaborane (12) ligands ; loop_ _publ_author_name 'Guo-Xin Jin' 'Chun-Xia Ren' 'Jian-Qiang Wang' 'Lin-Hong Weng' data_f50520e _database_code_depnum_ccdc_archive 'CCDC 282857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H132 B40 Ir4 N8 O2 S8 Zn' _chemical_formula_weight 2953.15 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' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.785(6) _cell_length_b 27.191(13) _cell_length_c 20.552(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.947(7) _cell_angle_gamma 90.00 _cell_volume 7443(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2892 _exptl_absorpt_coefficient_mu 3.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6980 _exptl_absorpt_correction_T_max 0.8299 _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 31138 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.1368 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13112 _reflns_number_gt 6830 _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 coordinate molecular THF was disorder in some way. O1, C45, C46, C47, C48 bond length and bond angle were refined with distance restraints. B8 B9 B11 B12 B13 B14 B15 B16 B17 B18 B19 B20 B21 B22 atoms were refined with anisotropic restraints. ; _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^)+(0.0996P)^2^+72.1886P] 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 13112 _refine_ls_number_parameters 723 _refine_ls_number_restraints 93 _refine_ls_R_factor_all 0.1604 _refine_ls_R_factor_gt 0.0882 _refine_ls_wR_factor_ref 0.2572 _refine_ls_wR_factor_gt 0.2160 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.21813(5) 0.25729(3) 0.16774(3) 0.0464(2) Uani 1 1 d . . . Ir2 Ir 0.81374(5) 0.25748(3) 0.82243(3) 0.0473(2) Uani 1 1 d . . . Zn1 Zn 0.5000 0.0000 0.5000 0.0513(8) Uani 1 2 d S . . S1 S 0.1495(4) 0.29461(18) 0.2494(2) 0.0575(12) Uani 1 1 d . . . S2 S 0.3698(4) 0.30014(17) 0.2092(2) 0.0577(12) Uani 1 1 d . . . S3 S 0.6678(4) 0.30552(19) 0.7819(2) 0.0623(13) Uani 1 1 d . . . S4 S 0.8872(4) 0.29263(17) 0.7421(2) 0.0553(12) Uani 1 1 d . . . N1 N 0.2743(11) 0.1996(5) 0.2382(7) 0.048(4) Uani 1 1 d . . . N2 N 0.5066(10) 0.0752(4) 0.4971(7) 0.046(3) Uani 1 1 d . . . N3 N 0.6012(10) 0.0003(4) 0.5926(6) 0.038(3) Uani 1 1 d . . . N4 N 0.7525(11) 0.2024(5) 0.7491(7) 0.051(4) Uani 1 1 d . . . B3 B 0.287(2) 0.3819(8) 0.2704(14) 0.078(8) Uani 1 1 d . . . H3 H 0.2521 0.3968 0.2201 0.094 Uiso 1 1 calc R . . B4 B 0.233(3) 0.3830(9) 0.3391(14) 0.098(10) Uani 1 1 d . . . H4 H 0.1587 0.4000 0.3335 0.118 Uiso 1 1 calc R . . B5 B 0.272(2) 0.3294(9) 0.3882(11) 0.075(7) Uani 1 1 d . . . H5 H 0.2239 0.3100 0.4146 0.090 Uiso 1 1 calc R . . B6 B 0.3506(16) 0.2972(10) 0.3514(10) 0.061(6) Uani 1 1 d . . . H6 H 0.3561 0.2569 0.3531 0.073 Uiso 1 1 calc R . . B7 B 0.415(2) 0.3853(9) 0.3055(12) 0.087(9) Uani 1 1 d . . . H7 H 0.4639 0.4034 0.2779 0.104 Uiso 1 1 calc R . . B8 B 0.334(2) 0.4191(12) 0.3433(16) 0.096(9) Uani 1 1 d U . . H8 H 0.3282 0.4594 0.3414 0.115 Uiso 1 1 calc R . . B9 B 0.326(2) 0.3849(11) 0.4161(16) 0.097(9) Uani 1 1 d U . . H9 H 0.3149 0.4028 0.4616 0.117 Uiso 1 1 calc R . . B10 B 0.397(2) 0.3336(10) 0.4226(13) 0.085(8) Uani 1 1 d . . . H10 H 0.4324 0.3179 0.4724 0.102 Uiso 1 1 calc R . . B11 B 0.455(2) 0.3331(9) 0.3542(13) 0.076(7) Uani 1 1 d U . . H11 H 0.5292 0.3169 0.3581 0.091 Uiso 1 1 calc R . . B12 B 0.440(2) 0.3878(10) 0.3938(15) 0.091(9) Uani 1 1 d U . . H12 H 0.5053 0.4080 0.4242 0.110 Uiso 1 1 calc R . . B13 B 0.6865(17) 0.3018(9) 0.6410(11) 0.064(6) Uani 1 1 d U . . H13 H 0.6732 0.2619 0.6366 0.077 Uiso 1 1 calc R . . B14 B 0.591(2) 0.3469(10) 0.6408(14) 0.084(8) Uani 1 1 d U . . H14 H 0.5130 0.3350 0.6355 0.101 Uiso 1 1 calc R . . B15 B 0.639(2) 0.3953(10) 0.6913(16) 0.094(9) Uani 1 1 d U . . H15 H 0.5930 0.4149 0.7193 0.112 Uiso 1 1 calc R . . B16 B 0.763(2) 0.3853(10) 0.7237(15) 0.088(8) Uani 1 1 d U . . H16 H 0.8005 0.3983 0.7747 0.106 Uiso 1 1 calc R . . B17 B 0.776(2) 0.3337(10) 0.6054(13) 0.080(8) Uani 1 1 d U . . H17 H 0.8201 0.3127 0.5776 0.097 Uiso 1 1 calc R . . B18 B 0.649(2) 0.3456(10) 0.5718(15) 0.087(8) Uani 1 1 d U . . H18 H 0.6103 0.3330 0.5210 0.104 Uiso 1 1 calc R . . B19 B 0.620(3) 0.4014(13) 0.6047(19) 0.118(12) Uani 1 1 d U . . H19 H 0.5607 0.4251 0.5748 0.142 Uiso 1 1 calc R . . B20 B 0.730(2) 0.4271(13) 0.6581(17) 0.111(11) Uani 1 1 d U . . H20 H 0.7452 0.4668 0.6646 0.134 Uiso 1 1 calc R . . B21 B 0.826(2) 0.3848(10) 0.6580(15) 0.092(9) Uani 1 1 d U . . H21 H 0.9041 0.3967 0.6646 0.110 Uiso 1 1 calc R . . B22 B 0.735(2) 0.3957(11) 0.5833(17) 0.105(10) Uani 1 1 d U . . H22 H 0.7528 0.4154 0.5409 0.126 Uiso 1 1 calc R . . C1 C 0.2499(15) 0.3295(7) 0.3033(9) 0.062(5) Uani 1 1 d . . . C2 C 0.3564(16) 0.3308(7) 0.2841(10) 0.066(6) Uani 1 1 d . . . C3 C 0.6839(15) 0.3381(8) 0.7107(9) 0.068(6) Uani 1 1 d . . . C4 C 0.7919(14) 0.3310(6) 0.6919(9) 0.057(5) Uani 1 1 d . . . C5 C 0.2163(14) 0.1777(6) 0.2713(9) 0.055(5) Uani 1 1 d . . . H5A H 0.1492 0.1870 0.2621 0.066 Uiso 1 1 calc R . . C6 C 0.2507(13) 0.1416(6) 0.3190(9) 0.055(5) Uani 1 1 d . . . H6A H 0.2072 0.1275 0.3415 0.066 Uiso 1 1 calc R . . C7 C 0.3477(13) 0.1267(5) 0.3330(8) 0.042(4) Uani 1 1 d . . . C8 C 0.4093(14) 0.1479(6) 0.2979(8) 0.053(5) Uani 1 1 d . . . H8A H 0.4758 0.1380 0.3053 0.064 Uiso 1 1 calc R . . C9 C 0.3705(14) 0.1842(6) 0.2513(9) 0.057(5) Uani 1 1 d . . . H9A H 0.4126 0.1987 0.2279 0.069 Uiso 1 1 calc R . . C10 C 0.3906(12) 0.0888(5) 0.3854(8) 0.036(4) Uani 1 1 d . . . C11 C 0.4557(12) 0.1054(6) 0.4463(8) 0.045(4) Uani 1 1 d . . . C12 C 0.4814(13) 0.1556(6) 0.4639(9) 0.054(5) Uani 1 1 d . . . H12A H 0.4574 0.1830 0.4376 0.064 Uiso 1 1 calc R . . C13 C 0.5450(14) 0.1561(5) 0.5241(8) 0.051(5) Uani 1 1 d . . . H13A H 0.5741 0.1837 0.5479 0.061 Uiso 1 1 calc R . . C14 C 0.5611(12) 0.1055(6) 0.5461(8) 0.041(4) Uani 1 1 d . . . C15 C 0.6221(12) 0.0898(6) 0.6074(8) 0.046(4) Uani 1 1 d . . . C16 C 0.6409(13) 0.0398(6) 0.6284(8) 0.049(5) Uani 1 1 d . . . C17 C 0.7054(14) 0.0258(6) 0.6926(9) 0.063(5) Uani 1 1 d . . . H17A H 0.7426 0.0466 0.7257 0.075 Uiso 1 1 calc R . . C18 C 0.7008(13) -0.0227(7) 0.6949(8) 0.059(5) Uani 1 1 d . . . H18A H 0.7345 -0.0426 0.7303 0.071 Uiso 1 1 calc R . . C19 C 0.6341(13) -0.0392(6) 0.6326(8) 0.052(5) Uani 1 1 d . . . C20 C 0.8088(14) 0.1780(5) 0.7170(8) 0.050(5) Uani 1 1 d . . . H20A H 0.8763 0.1863 0.7249 0.060 Uiso 1 1 calc R . . C21 C 0.7702(14) 0.1401(6) 0.6714(9) 0.057(5) Uani 1 1 d . . . H21A H 0.8121 0.1225 0.6509 0.069 Uiso 1 1 calc R . . C22 C 0.6697(12) 0.1295(6) 0.6575(8) 0.042(4) Uani 1 1 d . . . C23 C 0.6108(14) 0.1551(6) 0.6911(9) 0.056(5) Uani 1 1 d . . . H23A H 0.5423 0.1489 0.6828 0.067 Uiso 1 1 calc R . . C24 C 0.6575(14) 0.1907(6) 0.7377(9) 0.055(5) Uani 1 1 d . . . H24A H 0.6190 0.2069 0.7621 0.065 Uiso 1 1 calc R . . C25 C 0.2326(15) 0.2619(8) 0.0644(9) 0.065(5) Uani 1 1 d . . . C26 C 0.2067(15) 0.2130(6) 0.0754(9) 0.055(5) Uani 1 1 d . . . C27 C 0.1085(15) 0.2148(7) 0.0920(10) 0.063(6) Uani 1 1 d . . . C28 C 0.0748(14) 0.2654(7) 0.0901(8) 0.053(5) Uani 1 1 d . . . C29 C 0.1541(15) 0.2966(6) 0.0751(7) 0.059(6) Uani 1 1 d . . . C30 C 0.3217(17) 0.2777(8) 0.0418(10) 0.084(7) Uani 1 1 d . . . H30A H 0.3790 0.2586 0.0646 0.125 Uiso 1 1 calc R . . H30B H 0.3346 0.3119 0.0521 0.125 Uiso 1 1 calc R . . H30C H 0.3091 0.2728 -0.0059 0.125 Uiso 1 1 calc R . . C31 C 0.2597(18) 0.1677(8) 0.0690(11) 0.086(7) Uani 1 1 d . . . H31A H 0.3247 0.1754 0.0629 0.129 Uiso 1 1 calc R . . H31B H 0.2221 0.1494 0.0309 0.129 Uiso 1 1 calc R . . H31C H 0.2674 0.1483 0.1091 0.129 Uiso 1 1 calc R . . C32 C 0.0529(16) 0.1717(7) 0.1019(11) 0.079(7) Uani 1 1 d . . . H32A H 0.0166 0.1786 0.1349 0.118 Uiso 1 1 calc R . . H32B H 0.0985 0.1449 0.1172 0.118 Uiso 1 1 calc R . . H32C H 0.0065 0.1628 0.0601 0.118 Uiso 1 1 calc R . . C33 C -0.0201(14) 0.2834(8) 0.1004(9) 0.070(6) Uani 1 1 d . . . H33A H -0.0744 0.2735 0.0632 0.105 Uiso 1 1 calc R . . H33B H -0.0183 0.3187 0.1034 0.105 Uiso 1 1 calc R . . H33C H -0.0300 0.2699 0.1414 0.105 Uiso 1 1 calc R . . C34 C 0.1512(18) 0.3506(7) 0.0650(11) 0.091(8) Uani 1 1 d . . . H34A H 0.0864 0.3600 0.0377 0.137 Uiso 1 1 calc R . . H34B H 0.2019 0.3600 0.0429 0.137 Uiso 1 1 calc R . . H34C H 0.1636 0.3667 0.1079 0.137 Uiso 1 1 calc R . . C35 C 0.8261(15) 0.2108(7) 0.9107(9) 0.058(5) Uani 1 1 d . . . C36 C 0.9223(14) 0.2140(7) 0.8974(9) 0.057(5) Uani 1 1 d . . . C37 C 0.9543(14) 0.2654(7) 0.8997(8) 0.059(5) Uani 1 1 d . . . C38 C 0.8740(18) 0.2932(7) 0.9166(9) 0.066(6) Uani 1 1 d . . . C39 C 0.7967(16) 0.2595(8) 0.9258(8) 0.062(5) Uani 1 1 d . . . C40 C 0.7721(18) 0.1635(7) 0.9153(12) 0.091(7) Uani 1 1 d . . . H40A H 0.7794 0.1416 0.8801 0.136 Uiso 1 1 calc R . . H40B H 0.7021 0.1701 0.9103 0.136 Uiso 1 1 calc R . . H40C H 0.8002 0.1485 0.9583 0.136 Uiso 1 1 calc R . . C41 C 0.9827(16) 0.1708(7) 0.8846(10) 0.080(7) Uani 1 1 d . . . H41A H 1.0220 0.1581 0.9268 0.120 Uiso 1 1 calc R . . H41B H 1.0265 0.1811 0.8577 0.120 Uiso 1 1 calc R . . H41C H 0.9383 0.1457 0.8613 0.120 Uiso 1 1 calc R . . C42 C 1.0520(13) 0.2850(7) 0.8915(10) 0.073(6) Uani 1 1 d . . . H42A H 1.0732 0.2658 0.8585 0.110 Uiso 1 1 calc R . . H42B H 1.1018 0.2831 0.9338 0.110 Uiso 1 1 calc R . . H42C H 1.0436 0.3186 0.8770 0.110 Uiso 1 1 calc R . . C43 C 0.8752(19) 0.3475(7) 0.9303(10) 0.090(7) Uani 1 1 d . . . H43A H 0.8083 0.3603 0.9151 0.134 Uiso 1 1 calc R . . H43B H 0.9181 0.3636 0.9069 0.134 Uiso 1 1 calc R . . H43C H 0.8999 0.3532 0.9778 0.134 Uiso 1 1 calc R . . C44 C 0.7037(18) 0.2732(11) 0.9481(10) 0.106(9) Uani 1 1 d . . . H44A H 0.6607 0.2449 0.9444 0.158 Uiso 1 1 calc R . . H44B H 0.6685 0.2991 0.9200 0.158 Uiso 1 1 calc R . . H44C H 0.7229 0.2841 0.9941 0.158 Uiso 1 1 calc R . . O1 O 0.6357(13) -0.0056(6) 0.4439(9) 0.112(6) Uiso 1 1 d D . . C48 C 0.637(3) -0.0370(10) 0.3868(15) 0.219(19) Uiso 1 1 d D . . H48 H 0.6147 -0.0694 0.3807 0.262 Uiso 1 1 calc R . . C45 C 0.693(3) 0.0387(9) 0.4373(17) 0.209(18) Uiso 1 1 d D . . H45 H 0.7296 0.0586 0.4717 0.250 Uiso 1 1 calc R . . C46 C 0.678(4) 0.0451(14) 0.362(2) 0.34(3) Uiso 1 1 d D . . H46 H 0.6696 0.0739 0.3368 0.411 Uiso 1 1 calc R . . C47 C 0.683(4) -0.0076(18) 0.3390(17) 0.34(4) Uiso 1 1 d D . . H47 H 0.7071 -0.0193 0.3038 0.408 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0483(4) 0.0533(4) 0.0328(4) 0.0062(3) 0.0019(3) 0.0019(3) Ir2 0.0489(4) 0.0537(4) 0.0333(4) -0.0081(3) 0.0000(3) 0.0021(3) Zn1 0.065(2) 0.0366(13) 0.0398(14) 0.0016(12) -0.0101(14) -0.0034(13) S1 0.057(3) 0.070(3) 0.040(2) -0.003(2) 0.003(2) 0.010(2) S2 0.060(3) 0.059(3) 0.051(3) 0.003(2) 0.007(2) -0.010(2) S3 0.059(3) 0.079(3) 0.046(3) -0.008(2) 0.009(3) 0.016(2) S4 0.054(3) 0.058(3) 0.047(3) 0.001(2) 0.001(2) 0.003(2) N1 0.049(9) 0.061(9) 0.038(8) 0.008(7) 0.018(8) 0.009(7) N2 0.052(9) 0.037(7) 0.038(7) 0.006(6) -0.008(6) -0.002(6) N3 0.053(9) 0.034(6) 0.027(6) -0.001(6) 0.013(6) -0.003(6) N4 0.057(10) 0.045(8) 0.038(8) -0.009(6) -0.010(8) 0.000(7) B3 0.11(2) 0.041(13) 0.084(18) 0.007(12) 0.015(17) 0.004(13) B4 0.16(3) 0.046(14) 0.078(19) -0.009(13) 0.02(2) -0.011(16) B5 0.09(2) 0.080(17) 0.043(13) -0.013(11) 0.000(14) -0.020(14) B6 0.053(14) 0.098(17) 0.032(11) 0.009(11) 0.014(11) -0.013(12) B7 0.13(3) 0.072(17) 0.054(15) -0.007(12) 0.017(17) -0.040(16) B8 0.102(12) 0.093(12) 0.096(12) -0.003(9) 0.033(9) -0.010(9) B9 0.102(12) 0.098(12) 0.090(12) -0.008(9) 0.022(9) -0.014(9) B10 0.10(2) 0.10(2) 0.048(14) -0.011(13) 0.005(15) -0.031(16) B11 0.074(10) 0.075(10) 0.074(10) 0.005(8) 0.010(8) -0.009(8) B12 0.095(12) 0.094(11) 0.084(11) -0.010(9) 0.020(9) -0.014(9) B13 0.062(9) 0.072(9) 0.053(9) -0.002(8) 0.005(8) 0.005(8) B14 0.079(11) 0.090(11) 0.082(11) 0.005(8) 0.020(9) 0.012(8) B15 0.097(12) 0.092(11) 0.092(12) 0.000(9) 0.022(9) 0.023(9) B16 0.100(12) 0.086(11) 0.080(11) 0.003(8) 0.026(9) 0.003(9) B17 0.084(11) 0.084(11) 0.073(11) 0.000(8) 0.019(8) 0.010(8) B18 0.084(11) 0.092(11) 0.081(11) 0.006(8) 0.015(9) 0.013(8) B19 0.119(12) 0.119(12) 0.118(12) 0.003(5) 0.032(6) 0.006(5) B20 0.113(12) 0.110(11) 0.111(12) 0.001(5) 0.028(5) 0.005(5) B21 0.093(10) 0.091(9) 0.092(10) 0.001(5) 0.024(5) 0.001(5) B22 0.105(11) 0.106(11) 0.104(11) 0.003(5) 0.026(5) 0.003(5) C1 0.064(13) 0.062(12) 0.051(12) -0.010(9) 0.002(10) -0.019(10) C2 0.083(15) 0.053(11) 0.055(12) 0.004(9) 0.007(11) -0.015(10) C3 0.071(14) 0.095(15) 0.039(11) -0.005(10) 0.016(10) 0.042(12) C4 0.070(13) 0.053(11) 0.043(11) -0.002(8) 0.005(10) 0.004(9) C5 0.057(12) 0.054(11) 0.047(11) 0.013(9) 0.001(10) 0.003(9) C6 0.047(11) 0.059(12) 0.063(12) 0.013(9) 0.020(10) 0.001(9) C7 0.053(11) 0.036(9) 0.035(9) 0.005(7) 0.010(9) 0.003(8) C8 0.049(11) 0.063(11) 0.044(10) 0.012(9) 0.006(9) 0.016(9) C9 0.060(13) 0.054(11) 0.055(12) 0.000(9) 0.009(10) 0.002(9) C10 0.044(10) 0.031(8) 0.040(9) 0.005(6) 0.022(8) 0.000(7) C11 0.044(10) 0.044(10) 0.043(10) 0.005(7) 0.007(8) -0.009(7) C12 0.067(12) 0.032(9) 0.050(11) 0.004(8) -0.005(10) 0.000(8) C13 0.081(13) 0.025(9) 0.044(10) 0.003(7) 0.011(10) -0.010(8) C14 0.038(9) 0.047(10) 0.035(9) -0.009(7) 0.005(8) -0.006(7) C15 0.047(10) 0.048(10) 0.044(10) -0.011(8) 0.012(9) -0.006(8) C16 0.056(11) 0.034(9) 0.044(10) 0.004(7) -0.011(9) 0.004(8) C17 0.081(14) 0.038(11) 0.050(11) -0.002(9) -0.017(10) -0.006(9) C18 0.057(12) 0.072(13) 0.035(9) -0.007(9) -0.012(9) 0.011(9) C19 0.056(11) 0.052(11) 0.037(9) 0.001(8) -0.008(9) 0.005(8) C20 0.057(11) 0.037(9) 0.053(11) -0.020(8) 0.008(10) 0.003(8) C21 0.062(13) 0.055(11) 0.053(12) -0.011(9) 0.010(10) 0.014(9) C22 0.043(11) 0.045(10) 0.031(8) 0.004(7) -0.003(8) 0.000(8) C23 0.052(11) 0.060(11) 0.051(11) -0.008(9) 0.005(10) 0.010(9) C24 0.058(12) 0.056(11) 0.047(11) -0.030(9) 0.009(10) 0.004(9) C25 0.054(12) 0.095(16) 0.038(10) 0.006(10) -0.004(10) 0.000(11) C26 0.077(14) 0.049(11) 0.039(10) -0.009(8) 0.015(10) 0.002(10) C27 0.059(13) 0.060(13) 0.055(12) -0.004(9) -0.013(11) -0.006(10) C28 0.053(11) 0.079(14) 0.031(9) -0.001(9) 0.017(9) -0.009(10) C29 0.088(15) 0.052(11) 0.019(8) 0.019(7) -0.021(9) -0.001(10) C30 0.088(17) 0.115(18) 0.045(12) 0.004(12) 0.013(12) -0.021(14) C31 0.108(19) 0.088(16) 0.062(14) -0.012(12) 0.021(14) 0.015(14) C32 0.082(16) 0.065(14) 0.080(15) -0.015(11) 0.004(13) -0.023(11) C33 0.066(14) 0.100(16) 0.036(10) 0.015(10) -0.001(10) 0.019(11) C34 0.12(2) 0.070(14) 0.065(14) 0.034(11) -0.009(14) -0.011(13) C35 0.054(13) 0.082(14) 0.033(10) -0.012(9) 0.001(9) 0.001(10) C36 0.059(13) 0.062(13) 0.039(10) 0.006(8) -0.008(9) 0.015(10) C37 0.057(12) 0.073(13) 0.028(9) -0.008(8) -0.024(9) -0.010(10) C38 0.098(17) 0.065(13) 0.033(10) -0.008(9) 0.012(11) 0.015(12) C39 0.081(15) 0.082(14) 0.015(7) 0.000(8) -0.002(9) 0.003(12) C40 0.104(19) 0.071(15) 0.100(19) 0.015(13) 0.030(16) -0.023(13) C41 0.091(17) 0.076(15) 0.060(13) 0.009(11) -0.004(13) 0.016(12) C42 0.044(12) 0.089(15) 0.066(14) 0.012(11) -0.023(10) -0.016(10) C43 0.14(2) 0.068(14) 0.057(13) -0.011(11) 0.017(15) 0.005(14) C44 0.090(18) 0.20(3) 0.037(11) -0.004(15) 0.030(13) 0.025(18) _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 2.140(13) . ? Ir1 C29 2.164(14) . ? Ir1 C25 2.19(2) . ? Ir1 C27 2.198(17) . ? Ir1 C28 2.207(17) . ? Ir1 C26 2.220(16) . ? Ir1 S2 2.353(5) . ? Ir1 S1 2.359(5) . ? Ir2 C38 2.133(18) . ? Ir2 N4 2.139(13) . ? Ir2 C37 2.176(15) . ? Ir2 C35 2.185(19) . ? Ir2 C39 2.197(17) . ? Ir2 C36 2.196(16) . ? Ir2 S4 2.351(5) . ? Ir2 S3 2.362(5) . ? Zn1 N2 2.047(11) 3_656 ? Zn1 N2 2.047(11) . ? Zn1 N3 2.049(11) 3_656 ? Zn1 N3 2.049(11) . ? Zn1 O1 2.443(18) . ? Zn1 O1 2.443(18) 3_656 ? S1 C1 1.803(17) . ? S2 C2 1.80(2) . ? S3 C3 1.77(2) . ? S4 C4 1.782(18) . ? N1 C5 1.32(2) . ? N1 C9 1.35(2) . ? N2 C14 1.366(18) . ? N2 C11 1.373(19) . ? N3 C16 1.338(18) . ? N3 C19 1.356(19) . ? N4 C24 1.31(2) . ? N4 C20 1.32(2) . ? B3 C2 1.67(3) . ? B3 C1 1.71(3) . ? B3 B7 1.73(4) . ? B3 B4 1.76(4) . ? B3 B8 1.78(4) . ? B4 C1 1.68(3) . ? B4 B8 1.69(4) . ? B4 B9 1.76(4) . ? B4 B5 1.78(4) . ? B5 B10 1.68(4) . ? B5 C1 1.69(3) . ? B5 B6 1.71(4) . ? B5 B9 1.71(4) . ? B6 C2 1.68(3) . ? B6 C1 1.72(3) . ? B6 B11 1.73(3) . ? B6 B10 1.75(3) . ? B7 C2 1.69(3) . ? B7 B11 1.74(3) . ? B7 B12 1.76(4) . ? B7 B8 1.77(4) . ? B8 B12 1.77(4) . ? B8 B9 1.79(4) . ? B9 B10 1.69(4) . ? B9 B12 1.75(4) . ? B10 B12 1.75(4) . ? B10 B11 1.79(4) . ? B11 C2 1.71(3) . ? B11 B12 1.73(4) . ? B13 C4 1.75(3) . ? B13 C3 1.75(3) . ? B13 B14 1.80(3) . ? B13 B17 1.81(4) . ? B13 B18 1.82(3) . ? B14 C3 1.68(3) . ? B14 B15 1.70(4) . ? B14 B19 1.75(4) . ? B14 B18 1.80(4) . ? B15 C3 1.68(3) . ? B15 B16 1.69(4) . ? B15 B19 1.74(4) . ? B15 B20 1.80(5) . ? B16 C3 1.66(4) . ? B16 C4 1.70(3) . ? B16 B20 1.73(4) . ? B16 B21 1.78(4) . ? B17 B18 1.73(4) . ? B17 C4 1.74(3) . ? B17 B21 1.79(4) . ? B17 B22 1.79(4) . ? B18 B19 1.75(4) . ? B18 B22 1.78(4) . ? B19 B22 1.76(5) . ? B19 B20 1.77(5) . ? B20 B21 1.75(4) . ? B20 B22 1.78(5) . ? B21 C4 1.74(3) . ? B21 B22 1.74(4) . ? C1 C2 1.61(3) . ? C3 C4 1.64(3) . ? C5 C6 1.38(2) . ? C6 C7 1.36(2) . ? C7 C8 1.38(2) . ? C7 C10 1.50(2) . ? C8 C9 1.38(2) . ? C10 C11 1.41(2) . ? C10 C19 1.42(2) 3_656 ? C11 C12 1.43(2) . ? C12 C13 1.32(2) . ? C13 C14 1.45(2) . ? C14 C15 1.39(2) . ? C15 C16 1.43(2) . ? C15 C22 1.52(2) . ? C16 C17 1.44(2) . ? C17 C18 1.32(2) . ? C18 C19 1.44(2) . ? C19 C10 1.42(2) 3_656 ? C20 C21 1.40(2) . ? C21 C22 1.37(2) . ? C22 C23 1.38(2) . ? C23 C24 1.40(2) . ? C25 C26 1.41(3) . ? C25 C30 1.48(3) . ? C25 C29 1.49(3) . ? C26 C31 1.45(2) . ? C26 C27 1.48(3) . ? C27 C32 1.44(3) . ? C27 C28 1.45(3) . ? C28 C33 1.46(2) . ? C28 C29 1.48(3) . ? C29 C34 1.48(2) . ? C35 C36 1.42(3) . ? C35 C39 1.44(3) . ? C35 C40 1.50(3) . ? C36 C37 1.46(2) . ? C36 C41 1.50(3) . ? C37 C38 1.45(3) . ? C37 C42 1.50(3) . ? C38 C39 1.45(3) . ? C38 C43 1.50(3) . ? C39 C44 1.52(3) . ? O1 C48 1.455(10) . ? O1 C45 1.464(10) . ? C48 C47 1.520(10) . ? C45 C46 1.516(10) . ? C46 C47 1.517(10) . ? 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 C29 162.2(6) . . ? N1 Ir1 C25 126.2(7) . . ? C29 Ir1 C25 40.2(7) . . ? N1 Ir1 C27 99.0(6) . . ? C29 Ir1 C27 65.6(7) . . ? C25 Ir1 C27 63.9(8) . . ? N1 Ir1 C28 131.5(6) . . ? C29 Ir1 C28 39.5(7) . . ? C25 Ir1 C28 65.2(7) . . ? C27 Ir1 C28 38.5(7) . . ? N1 Ir1 C26 96.5(6) . . ? C29 Ir1 C26 66.0(7) . . ? C25 Ir1 C26 37.3(7) . . ? C27 Ir1 C26 39.1(7) . . ? C28 Ir1 C26 65.4(7) . . ? N1 Ir1 S2 89.2(4) . . ? C29 Ir1 S2 101.4(5) . . ? C25 Ir1 S2 91.6(5) . . ? C27 Ir1 S2 154.3(6) . . ? C28 Ir1 S2 139.3(5) . . ? C26 Ir1 S2 116.1(6) . . ? N1 Ir1 S1 88.6(4) . . ? C29 Ir1 S1 105.5(6) . . ? C25 Ir1 S1 145.1(6) . . ? C27 Ir1 S1 113.7(6) . . ? C28 Ir1 S1 91.3(5) . . ? C26 Ir1 S1 152.8(6) . . ? S2 Ir1 S1 90.64(18) . . ? C38 Ir2 N4 161.6(7) . . ? C38 Ir2 C37 39.4(7) . . ? N4 Ir2 C37 134.4(6) . . ? C38 Ir2 C35 65.3(7) . . ? N4 Ir2 C35 96.3(6) . . ? C37 Ir2 C35 65.7(7) . . ? C38 Ir2 C39 39.2(7) . . ? N4 Ir2 C39 125.3(7) . . ? C37 Ir2 C39 65.8(8) . . ? C35 Ir2 C39 38.4(7) . . ? C38 Ir2 C36 64.7(7) . . ? N4 Ir2 C36 101.0(6) . . ? C37 Ir2 C36 39.1(7) . . ? C35 Ir2 C36 37.9(7) . . ? C39 Ir2 C36 63.8(7) . . ? C38 Ir2 S4 108.4(6) . . ? N4 Ir2 S4 87.3(4) . . ? C37 Ir2 S4 90.5(6) . . ? C35 Ir2 S4 149.8(5) . . ? C39 Ir2 S4 147.3(6) . . ? C36 Ir2 S4 111.9(6) . . ? C38 Ir2 S3 99.5(6) . . ? N4 Ir2 S3 89.6(4) . . ? C37 Ir2 S3 136.0(5) . . ? C35 Ir2 S3 119.4(6) . . ? C39 Ir2 S3 91.9(5) . . ? C36 Ir2 S3 155.4(6) . . ? S4 Ir2 S3 90.53(18) . . ? N2 Zn1 N2 180.000(1) 3_656 . ? N2 Zn1 N3 89.9(5) 3_656 3_656 ? N2 Zn1 N3 90.1(5) . 3_656 ? N2 Zn1 N3 90.1(5) 3_656 . ? N2 Zn1 N3 89.9(5) . . ? N3 Zn1 N3 180.0(4) 3_656 . ? N2 Zn1 O1 89.8(6) 3_656 . ? N2 Zn1 O1 90.2(6) . . ? N3 Zn1 O1 89.0(6) 3_656 . ? N3 Zn1 O1 91.0(6) . . ? N2 Zn1 O1 90.2(6) 3_656 3_656 ? N2 Zn1 O1 89.8(6) . 3_656 ? N3 Zn1 O1 91.0(6) 3_656 3_656 ? N3 Zn1 O1 89.0(6) . 3_656 ? O1 Zn1 O1 180.000(2) . 3_656 ? C1 S1 Ir1 106.1(7) . . ? C2 S2 Ir1 105.1(7) . . ? C3 S3 Ir2 106.9(6) . . ? C4 S4 Ir2 104.9(7) . . ? C5 N1 C9 117.0(16) . . ? C5 N1 Ir1 121.2(12) . . ? C9 N1 Ir1 121.8(12) . . ? C14 N2 C11 105.9(12) . . ? C14 N2 Zn1 127.0(10) . . ? C11 N2 Zn1 127.1(10) . . ? C16 N3 C19 106.1(12) . . ? C16 N3 Zn1 126.7(10) . . ? C19 N3 Zn1 127.0(10) . . ? C24 N4 C20 118.7(15) . . ? C24 N4 Ir2 119.4(12) . . ? C20 N4 Ir2 121.9(12) . . ? C2 B3 C1 57.1(12) . . ? C2 B3 B7 59.8(14) . . ? C1 B3 B7 105.0(17) . . ? C2 B3 B4 102.9(18) . . ? C1 B3 B4 57.7(13) . . ? B7 B3 B4 105(2) . . ? C2 B3 B8 105.2(19) . . ? C1 B3 B8 102.8(19) . . ? B7 B3 B8 60.6(16) . . ? B4 B3 B8 57.0(16) . . ? C1 B4 B8 109(2) . . ? C1 B4 B3 59.7(14) . . ? B8 B4 B3 62.2(18) . . ? C1 B4 B9 105(2) . . ? B8 B4 B9 62.3(18) . . ? B3 B4 B9 111(2) . . ? C1 B4 B5 58.6(13) . . ? B8 B4 B5 109(2) . . ? B3 B4 B5 108(2) . . ? B9 B4 B5 57.9(15) . . ? B10 B5 C1 109(2) . . ? B10 B5 B6 61.9(15) . . ? C1 B5 B6 60.8(13) . . ? B10 B5 B9 59.6(16) . . ? C1 B5 B9 107.0(19) . . ? B6 B5 B9 109(2) . . ? B10 B5 B4 108(2) . . ? C1 B5 B4 57.7(13) . . ? B6 B5 B4 108(2) . . ? B9 B5 B4 60.7(16) . . ? C2 B6 B5 104.8(18) . . ? C2 B6 C1 56.7(12) . . ? B5 B6 C1 59.1(13) . . ? C2 B6 B11 60.2(13) . . ? B5 B6 B11 108.0(19) . . ? C1 B6 B11 105.8(17) . . ? C2 B6 B10 107.4(17) . . ? B5 B6 B10 58.3(15) . . ? C1 B6 B10 105.0(19) . . ? B11 B6 B10 62.0(14) . . ? C2 B7 B3 58.3(13) . . ? C2 B7 B11 59.6(13) . . ? B3 B7 B11 109.3(18) . . ? C2 B7 B12 104.8(18) . . ? B3 B7 B12 110(2) . . ? B11 B7 B12 59.3(15) . . ? C2 B7 B8 105(2) . . ? B3 B7 B8 61.3(17) . . ? B11 B7 B8 108(2) . . ? B12 B7 B8 60.3(17) . . ? B4 B8 B7 106(2) . . ? B4 B8 B12 107(2) . . ? B7 B8 B12 59.5(16) . . ? B4 B8 B3 60.8(16) . . ? B7 B8 B3 58.1(16) . . ? B12 B8 B3 107(2) . . ? B4 B8 B9 60.9(17) . . ? B7 B8 B9 106(2) . . ? B12 B8 B9 58.7(17) . . ? B3 B8 B9 109(2) . . ? B10 B9 B5 59.3(16) . . ? B10 B9 B12 61.2(17) . . ? B5 B9 B12 107(2) . . ? B10 B9 B4 109(2) . . ? B5 B9 B4 61.4(15) . . ? B12 B9 B4 105(2) . . ? B10 B9 B8 110(2) . . ? B5 B9 B8 107(2) . . ? B12 B9 B8 60.2(17) . . ? B4 B9 B8 56.8(16) . . ? B5 B10 B9 61.1(17) . . ? B5 B10 B6 59.7(13) . . ? B9 B10 B6 109(2) . . ? B5 B10 B12 108(2) . . ? B9 B10 B12 61.1(17) . . ? B6 B10 B12 106.1(18) . . ? B5 B10 B11 106.4(18) . . ? B9 B10 B11 108(2) . . ? B6 B10 B11 58.5(13) . . ? B12 B10 B11 58.7(15) . . ? C2 B11 B6 58.4(12) . . ? C2 B11 B12 105.4(19) . . ? B6 B11 B12 108(2) . . ? C2 B11 B7 58.8(13) . . ? B6 B11 B7 107.9(19) . . ? B12 B11 B7 60.9(15) . . ? C2 B11 B10 104.2(18) . . ? B6 B11 B10 59.6(13) . . ? B12 B11 B10 59.6(16) . . ? B7 B11 B10 108(2) . . ? B11 B12 B9 108(2) . . ? B11 B12 B10 61.7(15) . . ? B9 B12 B10 57.7(16) . . ? B11 B12 B7 59.8(15) . . ? B9 B12 B7 109(2) . . ? B10 B12 B7 108.9(19) . . ? B11 B12 B8 108(2) . . ? B9 B12 B8 61.1(17) . . ? B10 B12 B8 108(2) . . ? B7 B12 B8 60.1(17) . . ? C4 B13 C3 56.1(11) . . ? C4 B13 B14 100.8(16) . . ? C3 B13 B14 56.5(13) . . ? C4 B13 B17 58.5(13) . . ? C3 B13 B17 102.7(17) . . ? B14 B13 B17 104.3(18) . . ? C4 B13 B18 101.2(17) . . ? C3 B13 B18 102.1(17) . . ? B14 B13 B18 59.7(14) . . ? B17 B13 B18 57.0(14) . . ? C3 B14 B15 59.6(15) . . ? C3 B14 B19 106(2) . . ? B15 B14 B19 60.5(18) . . ? C3 B14 B13 60.3(13) . . ? B15 B14 B13 111(2) . . ? B19 B14 B13 109(2) . . ? C3 B14 B18 105.9(19) . . ? B15 B14 B18 108(2) . . ? B19 B14 B18 59.0(17) . . ? B13 B14 B18 60.8(14) . . ? C3 B15 B16 59.1(15) . . ? C3 B15 B14 59.5(15) . . ? B16 B15 B14 108(2) . . ? C3 B15 B19 106(2) . . ? B16 B15 B19 107(2) . . ? B14 B15 B19 61.1(18) . . ? C3 B15 B20 107(2) . . ? B16 B15 B20 59.4(17) . . ? B14 B15 B20 110(2) . . ? B19 B15 B20 60.1(19) . . ? C3 B16 B15 60.3(16) . . ? C3 B16 C4 58.4(13) . . ? B15 B16 C4 107(2) . . ? C3 B16 B20 111(2) . . ? B15 B16 B20 63.5(18) . . ? C4 B16 B20 108(2) . . ? C3 B16 B21 107(2) . . ? B15 B16 B21 110(2) . . ? C4 B16 B21 59.8(15) . . ? B20 B16 B21 59.7(17) . . ? B18 B17 C4 105(2) . . ? B18 B17 B21 107(2) . . ? C4 B17 B21 59.1(14) . . ? B18 B17 B22 60.7(16) . . ? C4 B17 B22 104.5(19) . . ? B21 B17 B22 58.0(16) . . ? B18 B17 B13 62.0(15) . . ? C4 B17 B13 59.1(13) . . ? B21 B17 B13 109(2) . . ? B22 B17 B13 111(2) . . ? B17 B18 B19 108(2) . . ? B17 B18 B22 61.4(16) . . ? B19 B18 B22 59.8(18) . . ? B17 B18 B14 107(2) . . ? B19 B18 B14 59.0(17) . . ? B22 B18 B14 107(2) . . ? B17 B18 B13 61.0(14) . . ? B19 B18 B13 108(2) . . ? B22 B18 B13 111(2) . . ? B14 B18 B13 59.5(14) . . ? B15 B19 B14 58.4(18) . . ? B15 B19 B18 109(2) . . ? B14 B19 B18 62.0(17) . . ? B15 B19 B22 110(3) . . ? B14 B19 B22 111(2) . . ? B18 B19 B22 61.1(18) . . ? B15 B19 B20 62(2) . . ? B14 B19 B20 109(3) . . ? B18 B19 B20 110(3) . . ? B22 B19 B20 60.4(19) . . ? B16 B20 B21 61.6(18) . . ? B16 B20 B19 103(2) . . ? B21 B20 B19 105(2) . . ? B16 B20 B22 107(2) . . ? B21 B20 B22 59.0(18) . . ? B19 B20 B22 59.5(19) . . ? B16 B20 B15 57.1(17) . . ? B21 B20 B15 107(2) . . ? B19 B20 B15 58.3(18) . . ? B22 B20 B15 107(2) . . ? C4 B21 B22 107(2) . . ? C4 B21 B20 106(2) . . ? B22 B21 B20 61.3(18) . . ? C4 B21 B16 57.9(15) . . ? B22 B21 B16 107(2) . . ? B20 B21 B16 58.7(17) . . ? C4 B21 B17 59.0(14) . . ? B22 B21 B17 61.3(16) . . ? B20 B21 B17 110(2) . . ? B16 B21 B17 106(2) . . ? B21 B22 B19 106(3) . . ? B21 B22 B20 59.7(18) . . ? B19 B22 B20 60.1(19) . . ? B21 B22 B18 107(2) . . ? B19 B22 B18 59.1(18) . . ? B20 B22 B18 108(2) . . ? B21 B22 B17 60.8(16) . . ? B19 B22 B17 105(2) . . ? B20 B22 B17 108(2) . . ? B18 B22 B17 57.8(15) . . ? C2 C1 B4 109.1(17) . . ? C2 C1 B5 108.4(16) . . ? B4 C1 B5 63.7(14) . . ? C2 C1 B3 60.1(13) . . ? B4 C1 B3 62.6(14) . . ? B5 C1 B3 114.4(16) . . ? C2 C1 B6 60.2(11) . . ? B4 C1 B6 112.0(17) . . ? B5 C1 B6 60.0(13) . . ? B3 C1 B6 111.8(16) . . ? C2 C1 S1 117.7(13) . . ? B4 C1 S1 123.6(17) . . ? B5 C1 S1 122.7(15) . . ? B3 C1 S1 117.2(14) . . ? B6 C1 S1 117.5(13) . . ? C1 C2 B3 62.8(14) . . ? C1 C2 B6 63.1(13) . . ? B3 C2 B6 116.5(19) . . ? C1 C2 B7 111.1(17) . . ? B3 C2 B7 61.9(15) . . ? B6 C2 B7 112.6(16) . . ? C1 C2 B11 111.7(16) . . ? B3 C2 B11 114.0(17) . . ? B6 C2 B11 61.4(13) . . ? B7 C2 B11 61.6(13) . . ? C1 C2 S2 119.9(13) . . ? B3 C2 S2 114.9(15) . . ? B6 C2 S2 119.4(14) . . ? B7 C2 S2 118.6(15) . . ? B11 C2 S2 120.3(16) . . ? C4 C3 B16 62.1(14) . . ? C4 C3 B14 110.7(16) . . ? B16 C3 B14 110.7(18) . . ? C4 C3 B15 110.7(19) . . ? B16 C3 B15 60.6(16) . . ? B14 C3 B15 60.9(15) . . ? C4 C3 B13 61.9(11) . . ? B16 C3 B13 114.6(18) . . ? B14 C3 B13 63.3(13) . . ? B15 C3 B13 114.3(17) . . ? C4 C3 S3 116.7(12) . . ? B16 C3 S3 118.1(15) . . ? B14 C3 S3 123.2(17) . . ? B15 C3 S3 122.8(16) . . ? B13 C3 S3 115.3(15) . . ? C3 C4 B16 59.5(14) . . ? C3 C4 B17 110.5(15) . . ? B16 C4 B17 111.9(16) . . ? C3 C4 B21 110.4(16) . . ? B16 C4 B21 62.3(14) . . ? B17 C4 B21 61.9(14) . . ? C3 C4 B13 62.0(12) . . ? B16 C4 B13 112.6(17) . . ? B17 C4 B13 62.5(13) . . ? B21 C4 B13 114.2(16) . . ? C3 C4 S4 120.7(13) . . ? B16 C4 S4 119.7(14) . . ? B17 C4 S4 119.9(14) . . ? B21 C4 S4 119.3(15) . . ? B13 C4 S4 117.2(13) . . ? N1 C5 C6 122.9(18) . . ? C7 C6 C5 120.2(18) . . ? C6 C7 C8 118.1(16) . . ? C6 C7 C10 123.0(16) . . ? C8 C7 C10 118.9(15) . . ? C7 C8 C9 118.8(17) . . ? N1 C9 C8 122.9(19) . . ? C11 C10 C19 126.3(14) . 3_656 ? C11 C10 C7 117.2(13) . . ? C19 C10 C7 116.4(14) 3_656 . ? N2 C11 C10 124.4(14) . . ? N2 C11 C12 109.5(14) . . ? C10 C11 C12 126.1(14) . . ? C13 C12 C11 108.0(15) . . ? C12 C13 C14 107.1(14) . . ? N2 C14 C15 124.9(14) . . ? N2 C14 C13 109.4(13) . . ? C15 C14 C13 125.7(14) . . ? C14 C15 C16 125.8(14) . . ? C14 C15 C22 116.9(14) . . ? C16 C15 C22 117.2(14) . . ? N3 C16 C15 125.6(14) . . ? N3 C16 C17 111.0(13) . . ? C15 C16 C17 123.4(14) . . ? C18 C17 C16 105.8(15) . . ? C17 C18 C19 107.7(16) . . ? N3 C19 C10 125.1(14) . 3_656 ? N3 C19 C18 109.2(14) . . ? C10 C19 C18 125.7(15) 3_656 . ? N4 C20 C21 122.2(17) . . ? C22 C21 C20 118.8(17) . . ? C21 C22 C23 118.9(16) . . ? C21 C22 C15 121.8(16) . . ? C23 C22 C15 119.3(15) . . ? C22 C23 C24 117.8(17) . . ? N4 C24 C23 123.6(17) . . ? C26 C25 C30 126(2) . . ? C26 C25 C29 110.5(18) . . ? C30 C25 C29 123(2) . . ? C26 C25 Ir1 72.6(11) . . ? C30 C25 Ir1 127.6(13) . . ? C29 C25 Ir1 69.0(10) . . ? C25 C26 C31 129(2) . . ? C25 C26 C27 106.9(16) . . ? C31 C26 C27 124.0(18) . . ? C25 C26 Ir1 70.1(10) . . ? C31 C26 Ir1 127.6(13) . . ? C27 C26 Ir1 69.7(10) . . ? C32 C27 C28 126.6(19) . . ? C32 C27 C26 123.8(18) . . ? C28 C27 C26 109.3(16) . . ? C32 C27 Ir1 128.3(14) . . ? C28 C27 Ir1 71.1(10) . . ? C26 C27 Ir1 71.2(9) . . ? C27 C28 C33 127.3(18) . . ? C27 C28 C29 107.5(17) . . ? C33 C28 C29 125.2(19) . . ? C27 C28 Ir1 70.4(10) . . ? C33 C28 Ir1 126.6(12) . . ? C29 C28 Ir1 68.7(9) . . ? C28 C29 C34 127(2) . . ? C28 C29 C25 105.7(16) . . ? C34 C29 C25 127(2) . . ? C28 C29 Ir1 71.8(9) . . ? C34 C29 Ir1 127.0(12) . . ? C25 C29 Ir1 70.8(9) . . ? C36 C35 C39 108.2(17) . . ? C36 C35 C40 124.5(18) . . ? C39 C35 C40 127(2) . . ? C36 C35 Ir2 71.5(10) . . ? C39 C35 Ir2 71.3(10) . . ? C40 C35 Ir2 128.0(13) . . ? C35 C36 C37 110.0(16) . . ? C35 C36 C41 124.9(18) . . ? C37 C36 C41 125.2(19) . . ? C35 C36 Ir2 70.6(10) . . ? C37 C36 Ir2 69.7(9) . . ? C41 C36 Ir2 127.3(13) . . ? C38 C37 C36 105.1(18) . . ? C38 C37 C42 127.2(19) . . ? C36 C37 C42 127.5(19) . . ? C38 C37 Ir2 68.7(10) . . ? C36 C37 Ir2 71.2(9) . . ? C42 C37 Ir2 127.7(13) . . ? C39 C38 C37 109.5(18) . . ? C39 C38 C43 125(2) . . ? C37 C38 C43 126(2) . . ? C39 C38 Ir2 72.8(10) . . ? C37 C38 Ir2 71.9(9) . . ? C43 C38 Ir2 126.9(13) . . ? C35 C39 C38 107.1(18) . . ? C35 C39 C44 127(2) . . ? C38 C39 C44 126(2) . . ? C35 C39 Ir2 70.3(10) . . ? C38 C39 Ir2 68.0(10) . . ? C44 C39 Ir2 127.5(12) . . ? C48 O1 C45 106.8(13) . . ? C48 O1 Zn1 126.1(19) . . ? C45 O1 Zn1 119.1(17) . . ? O1 C48 C47 107.9(11) . . ? O1 C45 C46 104.9(12) . . ? C45 C46 C47 101.8(12) . . ? C46 C47 C48 103.9(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.453 _refine_diff_density_min -3.065 _refine_diff_density_rms 0.208 data_f50629c _database_code_depnum_ccdc_archive 'CCDC 282858' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H132 B40 Cu Ir4 N8 O2 S8' _chemical_formula_weight 2951.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.822(5) _cell_length_b 27.187(9) _cell_length_c 20.635(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.145(5) _cell_angle_gamma 90.00 _cell_volume 7485(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1012 _cell_measurement_theta_min 2.669 _cell_measurement_theta_max 24.550 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2890 _exptl_absorpt_coefficient_mu 3.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3925 _exptl_absorpt_correction_T_max 0.5143 _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 31125 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.01 _reflns_number_total 13194 _reflns_number_gt 7408 _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 coordinate molecular THF was disorder in some way. O1, C45, C46, C47, C48 refined with anisotropic restraints. B4 B9 B10 B11 B12 B15 B16 B17 B18 B19 B20 B22 atoms were refined with anisotropic restraints. ; _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^)+(0.0805P)^2^+76.0414P] 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 13194 _refine_ls_number_parameters 748 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1416 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2410 _refine_ls_wR_factor_gt 0.2142 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.197 _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 0.21843(5) 0.24323(3) 0.16705(3) 0.0394(2) Uani 1 1 d . . . Ir2 Ir 0.81374(5) 0.24251(3) 0.82085(3) 0.0406(2) Uani 1 1 d . . . Cu3 Cu 0.5000 0.5000 0.5000 0.0361(7) Uani 1 2 d S . . S1 S 0.1488(4) 0.20611(17) 0.2485(2) 0.0488(11) Uani 1 1 d . . . S2 S 0.3696(4) 0.20043(17) 0.2096(2) 0.0493(11) Uani 1 1 d . . . S3 S 0.8874(3) 0.20751(17) 0.7406(2) 0.0463(11) Uani 1 1 d . . . S4 S 0.6680(4) 0.19484(18) 0.7794(2) 0.0531(12) Uani 1 1 d . . . B3 B 0.3475(16) 0.2038(9) 0.3502(9) 0.049(5) Uani 1 1 d . . . H3 H 0.3514 0.2442 0.3515 0.059 Uiso 1 1 calc R . . B4 B 0.269(2) 0.1716(10) 0.3877(13) 0.073(7) Uani 1 1 d U . . H4 H 0.2206 0.1910 0.4141 0.087 Uiso 1 1 calc R . . B5 B 0.229(2) 0.1179(9) 0.3380(12) 0.074(8) Uani 1 1 d . . . H5 H 0.1535 0.1020 0.3313 0.089 Uiso 1 1 calc R . . B6 B 0.287(2) 0.1187(8) 0.2724(12) 0.067(7) Uani 1 1 d . . . H6 H 0.2516 0.1029 0.2228 0.081 Uiso 1 1 calc R . . B7 B 0.454(2) 0.1684(9) 0.3538(10) 0.067(7) Uani 1 1 d . . . H7 H 0.5279 0.1851 0.3575 0.080 Uiso 1 1 calc R . . B8 B 0.397(2) 0.1673(11) 0.4236(11) 0.078(9) Uani 1 1 d . . . H8 H 0.4332 0.1826 0.4734 0.094 Uiso 1 1 calc R . . B9 B 0.322(2) 0.1142(10) 0.4151(14) 0.081(8) Uani 1 1 d U . . H9 H 0.3095 0.0951 0.4591 0.097 Uiso 1 1 calc R . . B10 B 0.332(2) 0.0805(12) 0.3429(15) 0.090(9) Uani 1 1 d U . . H10 H 0.3257 0.0401 0.3408 0.108 Uiso 1 1 calc R . . B11 B 0.416(2) 0.1161(9) 0.3053(12) 0.067(7) Uani 1 1 d U . . H11 H 0.4651 0.0985 0.2781 0.080 Uiso 1 1 calc R . . B12 B 0.439(3) 0.1140(11) 0.3944(15) 0.095(9) Uani 1 1 d U . . H12 H 0.5047 0.0947 0.4257 0.114 Uiso 1 1 calc R . . B13 B 0.6876(18) 0.1987(11) 0.6378(10) 0.071(8) Uani 1 1 d . . . H13 H 0.6757 0.2387 0.6333 0.085 Uiso 1 1 calc R . . B14 B 0.7748(19) 0.1673(9) 0.6034(10) 0.064(7) Uani 1 1 d . . . H14 H 0.8195 0.1883 0.5760 0.076 Uiso 1 1 calc R . . B15 B 0.826(2) 0.1159(10) 0.6555(13) 0.080(8) Uani 1 1 d U . . H15 H 0.9045 0.1038 0.6626 0.096 Uiso 1 1 calc R . . B16 B 0.764(2) 0.1158(10) 0.7198(13) 0.073(7) Uani 1 1 d U . . H16 H 0.8010 0.1029 0.7707 0.088 Uiso 1 1 calc R . . B17 B 0.590(2) 0.1564(10) 0.6365(13) 0.082(8) Uani 1 1 d U . . H17 H 0.5132 0.1695 0.6308 0.098 Uiso 1 1 calc R . . B18 B 0.650(2) 0.1556(10) 0.5702(14) 0.081(8) Uani 1 1 d U . . H18 H 0.6114 0.1683 0.5194 0.097 Uiso 1 1 calc R . . B19 B 0.733(2) 0.1060(11) 0.5802(16) 0.095(9) Uani 1 1 d U . . H19 H 0.7491 0.0868 0.5372 0.114 Uiso 1 1 calc R . . B20 B 0.729(2) 0.0737(12) 0.6527(15) 0.096(9) Uani 1 1 d U . . H20 H 0.7425 0.0338 0.6575 0.115 Uiso 1 1 calc R . . B21 B 0.644(3) 0.1062(12) 0.6870(16) 0.097(9) Uani 1 1 d U . . H21 H 0.5999 0.0860 0.7157 0.116 Uiso 1 1 calc R . . B22 B 0.620(3) 0.0998(14) 0.6008(19) 0.120(12) Uani 1 1 d U . . H22 H 0.5595 0.0761 0.5714 0.144 Uiso 1 1 calc R . . N1 N 0.2745(9) 0.3013(4) 0.2375(6) 0.034(3) Uani 1 1 d . . . N2 N 0.4045(10) 0.5005(4) 0.4081(6) 0.038(3) Uani 1 1 d . . . N3 N 0.5065(10) 0.4264(4) 0.4962(6) 0.037(3) Uani 1 1 d . . . N4 N 0.7501(11) 0.2977(5) 0.7489(6) 0.040(3) Uani 1 1 d . . . C1 C 0.2501(15) 0.1721(7) 0.3026(9) 0.053(5) Uani 1 1 d . . . C2 C 0.3563(14) 0.1696(6) 0.2837(8) 0.050(5) Uani 1 1 d . . . C3 C 0.7913(15) 0.1699(6) 0.6893(8) 0.054(5) Uani 1 1 d . . . C4 C 0.6831(15) 0.1630(8) 0.7065(9) 0.065(6) Uani 1 1 d . . . C5 C 0.2159(14) 0.3229(6) 0.2715(8) 0.046(4) Uani 1 1 d . . . H5A H 0.1491 0.3135 0.2635 0.056 Uiso 1 1 calc R . . C6 C 0.2535(13) 0.3590(6) 0.3184(9) 0.048(5) Uani 1 1 d . . . H6A H 0.2116 0.3736 0.3416 0.057 Uiso 1 1 calc R . . C7 C 0.3519(12) 0.3739(6) 0.3314(7) 0.036(4) Uani 1 1 d . . . C8 C 0.4091(14) 0.3522(6) 0.2956(8) 0.047(4) Uani 1 1 d . . . H8A H 0.4757 0.3616 0.3025 0.056 Uiso 1 1 calc R . . C9 C 0.3699(13) 0.3161(6) 0.2488(8) 0.043(4) Uani 1 1 d . . . H9A H 0.4108 0.3017 0.2248 0.052 Uiso 1 1 calc R . . C10 C 0.3628(12) 0.5402(6) 0.3723(7) 0.040(4) Uani 1 1 d . . . C11 C 0.3007(14) 0.5252(7) 0.3074(8) 0.056(5) Uani 1 1 d . . . H11A H 0.2647 0.5457 0.2735 0.067 Uiso 1 1 calc R . . C12 C 0.3052(14) 0.4768(7) 0.3056(8) 0.055(5) Uani 1 1 d . . . H12A H 0.2729 0.4567 0.2700 0.066 Uiso 1 1 calc R . . C13 C 0.3680(13) 0.4611(6) 0.3677(8) 0.041(4) Uani 1 1 d . . . C14 C 0.3942(12) 0.4122(6) 0.3834(7) 0.036(4) Uani 1 1 d . . . C15 C 0.4575(12) 0.3965(5) 0.4446(7) 0.037(4) Uani 1 1 d . . . C16 C 0.4832(13) 0.3457(6) 0.4625(8) 0.044(4) Uani 1 1 d . . . H16A H 0.4611 0.3183 0.4358 0.052 Uiso 1 1 calc R . . C17 C 0.5429(15) 0.3453(6) 0.5228(8) 0.050(5) Uani 1 1 d . . . H17A H 0.5694 0.3175 0.5472 0.060 Uiso 1 1 calc R . . C18 C 0.5607(12) 0.3952(6) 0.5451(7) 0.038(4) Uani 1 1 d . . . C19 C 0.6211(12) 0.4100(6) 0.6077(8) 0.038(4) Uani 1 1 d . . . C20 C 0.8071(12) 0.3219(6) 0.7165(8) 0.042(4) Uani 1 1 d . . . H20A H 0.8748 0.3141 0.7257 0.050 Uiso 1 1 calc R . . C21 C 0.7693(14) 0.3584(6) 0.6693(8) 0.051(5) Uani 1 1 d . . . H21A H 0.8106 0.3742 0.6468 0.061 Uiso 1 1 calc R . . C22 C 0.6679(14) 0.3706(6) 0.6566(8) 0.045(5) Uani 1 1 d . . . C23 C 0.6110(13) 0.3457(6) 0.6912(8) 0.044(4) Uani 1 1 d . . . H23A H 0.5431 0.3527 0.6838 0.053 Uiso 1 1 calc R . . C24 C 0.6554(13) 0.3105(6) 0.7369(9) 0.049(5) Uani 1 1 d . . . H24A H 0.6161 0.2946 0.7608 0.059 Uiso 1 1 calc R . . C25 C 0.1086(14) 0.2857(6) 0.0920(8) 0.047(5) Uani 1 1 d . . . C26 C 0.2062(15) 0.2874(7) 0.0754(8) 0.051(5) Uani 1 1 d . . . C27 C 0.2323(14) 0.2381(8) 0.0651(9) 0.056(5) Uani 1 1 d . . . C28 C 0.1545(15) 0.2045(7) 0.0750(8) 0.054(5) Uani 1 1 d . . . C29 C 0.0771(13) 0.2350(7) 0.0883(7) 0.043(4) Uani 1 1 d . . . C30 C 0.0528(15) 0.3295(7) 0.1015(10) 0.066(6) Uani 1 1 d . . . H30A H 0.0092 0.3394 0.0592 0.100 Uiso 1 1 calc R . . H30B H 0.0988 0.3556 0.1191 0.100 Uiso 1 1 calc R . . H30C H 0.0135 0.3223 0.1325 0.100 Uiso 1 1 calc R . . C31 C 0.2631(17) 0.3332(8) 0.0689(10) 0.082(7) Uani 1 1 d . . . H31A H 0.3311 0.3248 0.0703 0.124 Uiso 1 1 calc R . . H31B H 0.2624 0.3552 0.1052 0.124 Uiso 1 1 calc R . . H31C H 0.2323 0.3490 0.0269 0.124 Uiso 1 1 calc R . . C32 C 0.3237(17) 0.2220(9) 0.0436(10) 0.081(7) Uani 1 1 d . . . H32A H 0.3767 0.2454 0.0592 0.122 Uiso 1 1 calc R . . H32B H 0.3076 0.2201 -0.0045 0.122 Uiso 1 1 calc R . . H32C H 0.3450 0.1903 0.0624 0.122 Uiso 1 1 calc R . . C33 C 0.1482(18) 0.1503(7) 0.0644(10) 0.084(7) Uani 1 1 d . . . H33A H 0.1151 0.1357 0.0952 0.126 Uiso 1 1 calc R . . H33B H 0.2145 0.1370 0.0721 0.126 Uiso 1 1 calc R . . H33C H 0.1109 0.1434 0.0192 0.126 Uiso 1 1 calc R . . C34 C -0.0183(15) 0.2167(8) 0.1006(9) 0.067(6) Uani 1 1 d . . . H34A H -0.0136 0.1819 0.1086 0.101 Uiso 1 1 calc R . . H34B H -0.0729 0.2234 0.0620 0.101 Uiso 1 1 calc R . . H34C H -0.0299 0.2331 0.1391 0.101 Uiso 1 1 calc R . . C35 C 0.9237(14) 0.2846(7) 0.8953(8) 0.049(5) Uani 1 1 d . . . C36 C 0.8277(16) 0.2891(7) 0.9095(9) 0.056(5) Uani 1 1 d . . . C37 C 0.7989(17) 0.2404(8) 0.9246(7) 0.066(6) Uani 1 1 d . . . C38 C 0.8755(16) 0.2060(7) 0.9158(8) 0.057(5) Uani 1 1 d . . . C39 C 0.9525(14) 0.2344(7) 0.8989(8) 0.048(5) Uani 1 1 d . . . C40 C 0.9855(17) 0.3278(8) 0.8838(10) 0.076(7) Uani 1 1 d . . . H40A H 1.0285 0.3384 0.9259 0.114 Uiso 1 1 calc R . . H40B H 0.9418 0.3543 0.8639 0.114 Uiso 1 1 calc R . . H40C H 1.0254 0.3183 0.8541 0.114 Uiso 1 1 calc R . . C41 C 0.7726(16) 0.3353(8) 0.9129(11) 0.074(6) Uani 1 1 d . . . H41A H 0.7870 0.3588 0.8819 0.111 Uiso 1 1 calc R . . H41B H 0.7931 0.3484 0.9576 0.111 Uiso 1 1 calc R . . H41C H 0.7019 0.3288 0.9014 0.111 Uiso 1 1 calc R . . C42 C 0.7044(17) 0.2264(9) 0.9465(9) 0.084(8) Uani 1 1 d . . . H42A H 0.7231 0.2164 0.9927 0.126 Uiso 1 1 calc R . . H42B H 0.6706 0.1999 0.9192 0.126 Uiso 1 1 calc R . . H42C H 0.6606 0.2544 0.9414 0.126 Uiso 1 1 calc R . . C43 C 0.879(2) 0.1512(7) 0.9277(10) 0.089(8) Uani 1 1 d . . . H43A H 0.9096 0.1354 0.8964 0.133 Uiso 1 1 calc R . . H43B H 0.8122 0.1389 0.9216 0.133 Uiso 1 1 calc R . . H43C H 0.9177 0.1444 0.9727 0.133 Uiso 1 1 calc R . . C44 C 1.0512(14) 0.2159(8) 0.8907(9) 0.068(6) Uani 1 1 d . . . H44A H 1.0698 0.2346 0.8563 0.102 Uiso 1 1 calc R . . H44B H 1.0451 0.1818 0.8782 0.102 Uiso 1 1 calc R . . H44C H 1.1017 0.2197 0.9323 0.102 Uiso 1 1 calc R . . C45 C 0.714(4) 0.4675(17) 0.435(2) 0.190(17) Uani 1 1 d U . . H45A H 0.7651 0.4512 0.4655 0.228 Uiso 1 1 calc R . . C46 C 0.669(4) 0.455(2) 0.371(3) 0.22(2) Uani 1 1 d U . . H46A H 0.6591 0.4235 0.3539 0.263 Uiso 1 1 calc R . . C47 C 0.636(4) 0.5022(18) 0.334(3) 0.21(2) Uani 1 1 d U . . H47A H 0.6142 0.5062 0.2874 0.253 Uiso 1 1 calc R . . C48 C 0.646(3) 0.5409(15) 0.386(2) 0.166(15) Uani 1 1 d U . . H48A H 0.6425 0.5749 0.3810 0.199 Uiso 1 1 calc R . . O1 O 0.663(2) 0.5123(12) 0.4435(15) 0.190(11) 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 0.0403(4) 0.0471(4) 0.0287(3) -0.0058(3) 0.0053(3) -0.0010(3) Ir2 0.0407(4) 0.0489(4) 0.0295(3) 0.0076(3) 0.0043(3) -0.0028(3) Cu3 0.0431(18) 0.0292(13) 0.0309(13) -0.0009(11) 0.0006(13) 0.0006(12) S1 0.048(3) 0.056(3) 0.039(2) 0.0020(19) 0.005(2) -0.006(2) S2 0.050(3) 0.054(3) 0.042(2) -0.003(2) 0.010(2) 0.006(2) S3 0.046(3) 0.057(3) 0.034(2) 0.0005(19) 0.007(2) -0.003(2) S4 0.050(3) 0.068(3) 0.041(2) 0.008(2) 0.012(2) -0.019(2) B3 0.047(13) 0.072(15) 0.030(10) -0.006(9) 0.015(10) 0.011(11) B4 0.076(11) 0.076(10) 0.064(10) -0.001(8) 0.016(8) 0.011(8) B5 0.10(2) 0.057(15) 0.068(16) 0.018(12) 0.033(16) 0.009(14) B6 0.11(2) 0.035(12) 0.062(15) -0.002(10) 0.033(15) -0.006(13) B7 0.074(17) 0.080(17) 0.039(12) -0.006(11) 0.000(12) 0.031(14) B8 0.075(18) 0.12(2) 0.032(12) 0.005(12) 0.002(12) 0.055(17) B9 0.088(11) 0.084(11) 0.074(11) 0.011(8) 0.023(9) 0.015(9) B10 0.098(12) 0.083(12) 0.091(12) 0.003(9) 0.027(9) 0.008(9) B11 0.074(10) 0.060(10) 0.064(10) 0.002(8) 0.015(8) 0.013(8) B12 0.100(12) 0.093(12) 0.088(12) 0.003(9) 0.019(9) 0.012(9) B13 0.059(16) 0.10(2) 0.038(12) 0.010(12) -0.015(12) -0.029(14) B14 0.069(16) 0.085(17) 0.034(11) -0.006(11) 0.007(11) -0.025(14) B15 0.086(11) 0.079(11) 0.078(11) -0.004(8) 0.025(9) -0.006(8) B16 0.081(11) 0.074(10) 0.067(10) 0.002(8) 0.023(8) -0.008(8) B17 0.084(11) 0.087(11) 0.075(11) 0.000(8) 0.020(9) -0.009(9) B18 0.080(11) 0.088(11) 0.074(11) -0.001(8) 0.019(9) -0.014(9) B19 0.103(13) 0.094(12) 0.088(12) -0.011(9) 0.024(9) -0.011(9) B20 0.102(13) 0.088(12) 0.098(12) -0.002(9) 0.025(9) -0.014(9) B21 0.101(13) 0.094(12) 0.093(12) -0.002(9) 0.023(9) -0.017(9) B22 0.123(15) 0.123(15) 0.117(15) -0.005(9) 0.035(10) -0.015(9) N1 0.027(7) 0.040(8) 0.034(7) -0.005(6) 0.007(6) -0.007(6) N2 0.050(9) 0.025(6) 0.033(7) 0.002(6) 0.002(6) 0.001(6) N3 0.048(8) 0.031(6) 0.029(6) 0.004(6) 0.008(6) 0.005(6) N4 0.047(9) 0.044(8) 0.031(7) 0.015(6) 0.014(7) -0.004(7) C1 0.066(13) 0.056(12) 0.040(10) 0.002(8) 0.022(10) 0.008(10) C2 0.065(13) 0.050(11) 0.034(9) 0.000(7) 0.011(9) 0.018(9) C3 0.070(14) 0.050(11) 0.038(10) 0.004(8) 0.005(10) -0.006(10) C4 0.060(14) 0.088(15) 0.043(11) 0.011(10) 0.009(10) -0.037(12) C5 0.046(11) 0.048(11) 0.051(11) -0.019(8) 0.023(9) 0.000(9) C6 0.037(10) 0.063(12) 0.047(10) -0.014(9) 0.018(9) 0.004(9) C7 0.039(10) 0.034(9) 0.030(8) 0.001(6) 0.003(8) -0.002(7) C8 0.041(11) 0.059(12) 0.044(10) 0.000(8) 0.018(9) 0.006(9) C9 0.050(11) 0.048(10) 0.035(9) -0.010(7) 0.016(9) -0.006(9) C10 0.046(10) 0.039(10) 0.030(8) -0.001(7) 0.001(8) 0.003(8) C11 0.071(14) 0.048(12) 0.040(10) 0.002(8) 0.001(10) 0.006(10) C12 0.064(13) 0.052(12) 0.037(9) 0.000(8) -0.009(9) 0.006(9) C13 0.044(10) 0.042(10) 0.037(9) -0.004(7) 0.008(8) -0.006(8) C14 0.040(10) 0.041(10) 0.029(8) -0.005(6) 0.013(8) -0.002(7) C15 0.044(10) 0.033(9) 0.032(9) -0.007(6) 0.008(8) -0.001(7) C16 0.061(12) 0.029(9) 0.039(10) -0.003(7) 0.008(9) -0.007(8) C17 0.085(14) 0.023(9) 0.040(10) 0.003(7) 0.015(10) 0.010(9) C18 0.047(10) 0.036(9) 0.029(8) -0.003(6) 0.008(8) 0.000(7) C19 0.036(9) 0.039(10) 0.037(9) 0.006(7) 0.005(8) 0.002(7) C20 0.027(9) 0.053(11) 0.039(9) 0.007(8) -0.002(8) 0.005(8) C21 0.059(13) 0.048(11) 0.042(10) 0.013(8) 0.007(10) -0.011(9) C22 0.050(12) 0.040(10) 0.037(9) 0.003(7) -0.004(9) 0.008(8) C23 0.029(9) 0.055(11) 0.048(10) 0.018(8) 0.010(8) 0.003(8) C24 0.040(11) 0.055(11) 0.048(11) 0.017(8) 0.002(9) -0.002(9) C25 0.059(13) 0.048(12) 0.033(9) -0.002(7) 0.005(9) -0.001(9) C26 0.065(13) 0.051(12) 0.030(9) 0.004(8) 0.001(9) -0.001(10) C27 0.038(10) 0.095(16) 0.041(10) 0.012(10) 0.020(9) 0.013(11) C28 0.068(13) 0.057(12) 0.027(9) -0.020(8) -0.006(9) -0.003(10) C29 0.042(10) 0.069(13) 0.019(7) -0.008(7) 0.009(7) 0.008(9) C30 0.066(14) 0.063(14) 0.073(14) 0.010(10) 0.023(12) 0.021(11) C31 0.088(18) 0.094(18) 0.059(13) 0.017(12) 0.008(13) -0.023(14) C32 0.088(18) 0.105(18) 0.056(13) 0.008(12) 0.031(13) 0.017(15) C33 0.11(2) 0.061(14) 0.063(13) -0.029(11) -0.006(14) 0.003(13) C34 0.073(15) 0.073(14) 0.048(12) -0.016(10) 0.000(11) -0.011(12) C35 0.045(11) 0.061(13) 0.032(9) -0.007(8) -0.005(9) -0.012(9) C36 0.068(15) 0.057(13) 0.043(11) -0.005(9) 0.013(11) -0.001(11) C37 0.082(16) 0.094(16) 0.007(7) 0.006(8) -0.015(9) -0.007(13) C38 0.070(14) 0.065(14) 0.032(10) 0.008(8) 0.004(10) -0.020(11) C39 0.049(11) 0.059(12) 0.026(8) 0.002(8) -0.007(8) 0.008(9) C40 0.082(16) 0.076(15) 0.061(13) -0.020(11) -0.001(12) -0.013(13) C41 0.067(15) 0.075(15) 0.078(15) -0.012(11) 0.015(13) 0.009(12) C42 0.089(18) 0.14(2) 0.038(11) 0.005(12) 0.040(12) -0.034(16) C43 0.13(2) 0.063(15) 0.054(13) 0.009(10) -0.005(14) -0.029(14) C44 0.050(12) 0.087(16) 0.053(12) -0.004(10) -0.010(10) 0.009(11) C45 0.190(19) 0.189(19) 0.187(19) 0.005(10) 0.042(10) 0.013(10) C46 0.23(2) 0.21(2) 0.22(2) -0.009(10) 0.050(11) 0.005(10) C47 0.22(2) 0.21(2) 0.20(2) 0.003(10) 0.049(11) 0.001(10) C48 0.176(17) 0.159(17) 0.165(17) 0.008(10) 0.047(10) 0.000(10) O1 0.204(14) 0.196(14) 0.174(13) -0.014(9) 0.057(9) 0.016(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 2.148(12) . ? Ir1 C28 2.150(15) . ? Ir1 C27 2.167(17) . ? Ir1 C25 2.192(17) . ? Ir1 C29 2.202(16) . ? Ir1 C26 2.209(16) . ? Ir1 S2 2.352(5) . ? Ir1 S1 2.369(5) . ? Ir2 N4 2.132(12) . ? Ir2 C38 2.162(17) . ? Ir2 C39 2.169(16) . ? Ir2 C35 2.181(16) . ? Ir2 C36 2.191(18) . ? Ir2 C37 2.204(17) . ? Ir2 S3 2.358(5) . ? Ir2 S4 2.360(5) . ? Cu3 N3 2.006(11) 3_666 ? Cu3 N3 2.006(11) . ? Cu3 N2 2.008(11) . ? Cu3 N2 2.008(11) 3_666 ? Cu3 O1 2.82(3) . ? S1 C1 1.802(19) . ? S2 C2 1.795(17) . ? S3 C3 1.787(18) . ? S4 C4 1.79(2) . ? B3 C1 1.68(3) . ? B3 C2 1.69(2) . ? B3 B4 1.73(3) . ? B3 B7 1.75(3) . ? B3 B8 1.79(3) . ? B3 H3 1.1000 . ? B4 C1 1.71(3) . ? B4 B8 1.74(4) . ? B4 B9 1.76(4) . ? B4 B5 1.79(4) . ? B4 H4 1.1000 . ? B5 C1 1.70(3) . ? B5 B10 1.73(4) . ? B5 B6 1.75(3) . ? B5 B9 1.77(4) . ? B5 H5 1.1000 . ? B6 C2 1.67(3) . ? B6 C1 1.71(3) . ? B6 B11 1.73(4) . ? B6 B10 1.76(4) . ? B6 H6 1.1000 . ? B7 C2 1.70(3) . ? B7 B12 1.74(4) . ? B7 B11 1.74(3) . ? B7 B8 1.81(3) . ? B7 H7 1.1000 . ? B8 B12 1.73(4) . ? B8 B9 1.76(4) . ? B8 H8 1.1000 . ? B9 B12 1.77(4) . ? B9 B10 1.78(4) . ? B9 H9 1.1000 . ? B10 B12 1.83(4) . ? B10 B11 1.83(4) . ? B10 H10 1.1000 . ? B11 C2 1.67(3) . ? B11 B12 1.78(4) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? B13 C4 1.73(3) . ? B13 C3 1.73(3) . ? B13 B17 1.77(4) . ? B13 B14 1.77(4) . ? B13 B18 1.79(4) . ? B13 H13 1.1000 . ? B14 B18 1.71(4) . ? B14 C3 1.73(3) . ? B14 B19 1.79(4) . ? B14 B15 1.79(4) . ? B14 H14 1.1000 . ? B15 C3 1.75(3) . ? B15 B20 1.76(4) . ? B15 B19 1.76(4) . ? B15 B16 1.77(4) . ? B15 H15 1.1000 . ? B16 B21 1.64(4) . ? B16 C4 1.67(3) . ? B16 C3 1.68(3) . ? B16 B20 1.76(4) . ? B16 H16 1.1000 . ? B17 C4 1.67(3) . ? B17 B21 1.76(4) . ? B17 B18 1.77(4) . ? B17 B22 1.80(5) . ? B17 H17 1.1000 . ? B18 B22 1.74(4) . ? B18 B19 1.75(4) . ? B18 H18 1.1000 . ? B19 B22 1.74(5) . ? B19 B20 1.75(4) . ? B19 H19 1.1000 . ? B20 B22 1.76(5) . ? B20 B21 1.76(5) . ? B20 H20 1.1000 . ? B21 C4 1.65(4) . ? B21 B22 1.73(4) . ? B21 H21 1.1000 . ? B22 H22 1.1000 . ? N1 C5 1.339(19) . ? N1 C9 1.34(2) . ? N2 C10 1.348(18) . ? N2 C13 1.371(18) . ? N3 C15 1.368(18) . ? N3 C18 1.379(19) . ? N4 C24 1.31(2) . ? N4 C20 1.332(19) . ? C1 C2 1.62(3) . ? C3 C4 1.64(3) . ? C5 C6 1.38(2) . ? C5 H5A 0.9300 . ? C6 C7 1.38(2) . ? C6 H6A 0.9300 . ? C7 C8 1.35(2) . ? C7 C14 1.50(2) . ? C8 C9 1.38(2) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C19 1.42(2) 3_666 ? C10 C11 1.45(2) . ? C11 C12 1.32(2) . ? C11 H11A 0.9300 . ? C12 C13 1.41(2) . ? C12 H12A 0.9300 . ? C13 C14 1.39(2) . ? C14 C15 1.40(2) . ? C15 C16 1.45(2) . ? C16 C17 1.30(2) . ? C16 H16A 0.9300 . ? C17 C18 1.43(2) . ? C17 H17A 0.9300 . ? C18 C19 1.40(2) . ? C19 C10 1.42(2) 3_666 ? C19 C22 1.50(2) . ? C20 C21 1.39(2) . ? C20 H20A 0.9300 . ? C21 C22 1.40(2) . ? C21 H21A 0.9300 . ? C22 C23 1.37(2) . ? C23 C24 1.37(2) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C29 1.44(2) . ? C25 C30 1.46(2) . ? C25 C26 1.48(3) . ? C26 C27 1.42(3) . ? C26 C31 1.50(3) . ? C27 C28 1.47(3) . ? C27 C32 1.51(3) . ? C28 C29 1.43(2) . ? C28 C33 1.49(3) . ? C29 C34 1.49(2) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C39 1.42(2) . ? C35 C36 1.44(3) . ? C35 C40 1.51(3) . ? C36 C37 1.44(3) . ? C36 C41 1.48(3) . ? C37 C38 1.46(3) . ? C37 C42 1.54(3) . ? C38 C39 1.43(3) . ? C38 C43 1.51(3) . ? C39 C44 1.50(2) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.34(5) . ? C45 O1 1.44(5) . ? C45 H45A 0.9300 . ? C46 C47 1.50(6) . ? C46 H46A 0.9300 . ? C47 C48 1.48(5) . ? C47 H47A 0.9300 . ? C48 O1 1.39(4) . ? C48 H48A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ir1 C28 161.9(6) . . ? N1 Ir1 C27 126.6(7) . . ? C28 Ir1 C27 39.7(7) . . ? N1 Ir1 C25 98.8(5) . . ? C28 Ir1 C25 65.5(7) . . ? C27 Ir1 C25 64.4(7) . . ? N1 Ir1 C29 131.9(6) . . ? C28 Ir1 C29 38.5(6) . . ? C27 Ir1 C29 64.1(6) . . ? C25 Ir1 C29 38.3(6) . . ? N1 Ir1 C26 96.5(6) . . ? C28 Ir1 C26 65.7(7) . . ? C27 Ir1 C26 37.9(7) . . ? C25 Ir1 C26 39.2(7) . . ? C29 Ir1 C26 64.5(7) . . ? N1 Ir1 S2 89.0(4) . . ? C28 Ir1 S2 101.9(5) . . ? C27 Ir1 S2 92.0(5) . . ? C25 Ir1 S2 155.2(5) . . ? C29 Ir1 S2 139.0(5) . . ? C26 Ir1 S2 116.8(5) . . ? N1 Ir1 S1 88.5(3) . . ? C28 Ir1 S1 105.6(6) . . ? C27 Ir1 S1 144.7(6) . . ? C25 Ir1 S1 113.0(5) . . ? C29 Ir1 S1 91.9(5) . . ? C26 Ir1 S1 152.2(5) . . ? S2 Ir1 S1 90.62(16) . . ? N4 Ir2 C38 161.2(7) . . ? N4 Ir2 C39 135.4(6) . . ? C38 Ir2 C39 38.5(7) . . ? N4 Ir2 C35 101.9(6) . . ? C38 Ir2 C35 64.2(7) . . ? C39 Ir2 C35 38.0(6) . . ? N4 Ir2 C36 96.0(6) . . ? C38 Ir2 C36 65.2(7) . . ? C39 Ir2 C36 64.6(7) . . ? C35 Ir2 C36 38.4(7) . . ? N4 Ir2 C37 124.7(7) . . ? C38 Ir2 C37 39.0(7) . . ? C39 Ir2 C37 64.2(7) . . ? C35 Ir2 C37 63.5(7) . . ? C36 Ir2 C37 38.2(7) . . ? N4 Ir2 S3 88.3(4) . . ? C38 Ir2 S3 108.1(6) . . ? C39 Ir2 S3 91.1(5) . . ? C35 Ir2 S3 110.9(5) . . ? C36 Ir2 S3 149.2(6) . . ? C37 Ir2 S3 146.9(6) . . ? N4 Ir2 S4 88.7(4) . . ? C38 Ir2 S4 100.0(5) . . ? C39 Ir2 S4 135.9(5) . . ? C35 Ir2 S4 156.2(5) . . ? C36 Ir2 S4 120.0(6) . . ? C37 Ir2 S4 92.9(6) . . ? S3 Ir2 S4 90.47(17) . . ? N3 Cu3 N3 180.000(2) 3_666 . ? N3 Cu3 N2 90.3(5) 3_666 . ? N3 Cu3 N2 89.7(5) . . ? N3 Cu3 N2 89.7(5) 3_666 3_666 ? N3 Cu3 N2 90.3(5) . 3_666 ? N2 Cu3 N2 180.000(3) . 3_666 ? N3 Cu3 O1 86.9(7) 3_666 . ? N3 Cu3 O1 93.1(7) . . ? N2 Cu3 O1 90.5(7) . . ? N2 Cu3 O1 89.5(7) 3_666 . ? C1 S1 Ir1 105.3(6) . . ? C2 S2 Ir1 105.6(6) . . ? C3 S3 Ir2 104.9(7) . . ? C4 S4 Ir2 107.0(6) . . ? C1 B3 C2 57.3(11) . . ? C1 B3 B4 60.1(13) . . ? C2 B3 B4 105.9(17) . . ? C1 B3 B7 106.3(16) . . ? C2 B3 B7 59.5(11) . . ? B4 B3 B7 109.0(18) . . ? C1 B3 B8 106.3(17) . . ? C2 B3 B8 106.9(15) . . ? B4 B3 B8 59.1(14) . . ? B7 B3 B8 61.8(13) . . ? C1 B3 H3 123.5 . . ? C2 B3 H3 123.7 . . ? B4 B3 H3 121.9 . . ? B7 B3 H3 120.9 . . ? B8 B3 H3 121.9 . . ? C1 B4 B3 58.7(12) . . ? C1 B4 B8 107.7(18) . . ? B3 B4 B8 62.3(14) . . ? C1 B4 B9 106.0(18) . . ? B3 B4 B9 110(2) . . ? B8 B4 B9 60.5(16) . . ? C1 B4 B5 58.3(12) . . ? B3 B4 B5 107.2(18) . . ? B8 B4 B5 109(2) . . ? B9 B4 B5 60.0(15) . . ? C1 B4 H4 123.8 . . ? B3 B4 H4 120.9 . . ? B8 B4 H4 120.4 . . ? B9 B4 H4 121.6 . . ? B5 B4 H4 122.3 . . ? C1 B5 B10 108(2) . . ? C1 B5 B6 59.4(12) . . ? B10 B5 B6 60.9(16) . . ? C1 B5 B9 105(2) . . ? B10 B5 B9 61.1(16) . . ? B6 B5 B9 109(2) . . ? C1 B5 B4 58.5(13) . . ? B10 B5 B4 108(2) . . ? B6 B5 B4 107.3(19) . . ? B9 B5 B4 59.1(15) . . ? C1 B5 H5 123.5 . . ? B10 B5 H5 120.7 . . ? B6 B5 H5 121.4 . . ? B9 B5 H5 122.2 . . ? B4 B5 H5 122.4 . . ? C2 B6 C1 57.2(11) . . ? C2 B6 B11 59.0(13) . . ? C1 B6 B11 105.4(17) . . ? C2 B6 B5 105.5(16) . . ? C1 B6 B5 59.0(12) . . ? B11 B6 B5 109.4(19) . . ? C2 B6 B10 108.1(19) . . ? C1 B6 B10 105.8(17) . . ? B11 B6 B10 63.3(16) . . ? B5 B6 B10 59.2(14) . . ? C2 B6 H6 123.5 . . ? C1 B6 H6 124.5 . . ? B11 B6 H6 120.7 . . ? B5 B6 H6 122.2 . . ? B10 B6 H6 121.0 . . ? C2 B7 B12 105(2) . . ? C2 B7 B11 58.2(12) . . ? B12 B7 B11 61.7(15) . . ? C2 B7 B3 58.6(11) . . ? B12 B7 B3 106(2) . . ? B11 B7 B3 107.4(19) . . ? C2 B7 B8 105.1(18) . . ? B12 B7 B8 58.1(15) . . ? B11 B7 B8 108(2) . . ? B3 B7 B8 60.3(12) . . ? C2 B7 H7 124.6 . . ? B12 B7 H7 122.9 . . ? B11 B7 H7 121.0 . . ? B3 B7 H7 122.2 . . ? B8 B7 H7 122.6 . . ? B12 B8 B4 108(2) . . ? B12 B8 B9 61.2(17) . . ? B4 B8 B9 60.3(16) . . ? B12 B8 B3 105.0(17) . . ? B4 B8 B3 58.6(13) . . ? B9 B8 B3 106.6(18) . . ? B12 B8 B7 58.8(14) . . ? B4 B8 B7 105.5(17) . . ? B9 B8 B7 107.5(19) . . ? B3 B8 B7 57.9(12) . . ? B12 B8 H8 122.2 . . ? B4 B8 H8 122.4 . . ? B9 B8 H8 121.1 . . ? B3 B8 H8 124.0 . . ? B7 B8 H8 123.4 . . ? B4 B9 B8 59.2(15) . . ? B4 B9 B5 60.9(14) . . ? B8 B9 B5 108.4(19) . . ? B4 B9 B12 105(2) . . ? B8 B9 B12 58.5(15) . . ? B5 B9 B12 106(2) . . ? B4 B9 B10 107.8(19) . . ? B8 B9 B10 110(2) . . ? B5 B9 B10 58.4(15) . . ? B12 B9 B10 61.9(16) . . ? B4 B9 H9 122.8 . . ? B8 B9 H9 121.4 . . ? B5 B9 H9 122.2 . . ? B12 B9 H9 123.3 . . ? B10 B9 H9 120.7 . . ? B5 B10 B6 60.0(15) . . ? B5 B10 B9 60.6(16) . . ? B6 B10 B9 107(2) . . ? B5 B10 B12 106(2) . . ? B6 B10 B12 104(2) . . ? B9 B10 B12 58.9(17) . . ? B5 B10 B11 105(2) . . ? B6 B10 B11 57.5(15) . . ? B9 B10 B11 106(2) . . ? B12 B10 B11 58.3(15) . . ? B5 B10 H10 122.2 . . ? B6 B10 H10 123.3 . . ? B9 B10 H10 121.7 . . ? B12 B10 H10 124.1 . . ? B11 B10 H10 123.9 . . ? C2 B11 B6 58.5(13) . . ? C2 B11 B7 59.8(12) . . ? B6 B11 B7 108.6(18) . . ? C2 B11 B12 104.2(17) . . ? B6 B11 B12 107(2) . . ? B7 B11 B12 59.1(15) . . ? C2 B11 B10 104.5(18) . . ? B6 B11 B10 59.1(15) . . ? B7 B11 B10 108.7(19) . . ? B12 B11 B10 60.7(16) . . ? C2 B11 H11 124.7 . . ? B6 B11 H11 121.9 . . ? B7 B11 H11 120.8 . . ? B12 B11 H11 123.0 . . ? B10 B11 H11 122.2 . . ? B8 B12 B7 63.2(16) . . ? B8 B12 B9 60.3(17) . . ? B7 B12 B9 110(2) . . ? B8 B12 B11 110(2) . . ? B7 B12 B11 59.2(14) . . ? B9 B12 B11 108(2) . . ? B8 B12 B10 109(2) . . ? B7 B12 B10 109(2) . . ? B9 B12 B10 59.3(17) . . ? B11 B12 B10 61.1(16) . . ? B8 B12 H12 119.8 . . ? B7 B12 H12 120.2 . . ? B9 B12 H12 121.6 . . ? B11 B12 H12 121.3 . . ? B10 B12 H12 121.6 . . ? C4 B13 C3 56.4(12) . . ? C4 B13 B17 57.1(13) . . ? C3 B13 B17 102.7(18) . . ? C4 B13 B14 103.3(19) . . ? C3 B13 B14 59.1(13) . . ? B17 B13 B14 106(2) . . ? C4 B13 B18 101.9(18) . . ? C3 B13 B18 102(2) . . ? B17 B13 B18 59.9(15) . . ? B14 B13 B18 57.3(14) . . ? C4 B13 H13 125.9 . . ? C3 B13 H13 125.4 . . ? B17 B13 H13 123.1 . . ? B14 B13 H13 123.1 . . ? B18 B13 H13 125.1 . . ? B18 B14 C3 105.5(18) . . ? B18 B14 B13 61.9(15) . . ? C3 B14 B13 59.4(12) . . ? B18 B14 B19 59.9(16) . . ? C3 B14 B19 105.2(17) . . ? B13 B14 B19 110.6(19) . . ? B18 B14 B15 107.3(19) . . ? C3 B14 B15 59.6(12) . . ? B13 B14 B15 110.1(17) . . ? B19 B14 B15 59.0(15) . . ? B18 B14 H14 122.2 . . ? C3 B14 H14 124.3 . . ? B13 B14 H14 119.2 . . ? B19 B14 H14 122.1 . . ? B15 B14 H14 121.6 . . ? C3 B15 B20 106(2) . . ? C3 B15 B19 105(2) . . ? B20 B15 B19 59.6(17) . . ? C3 B15 B16 57.2(13) . . ? B20 B15 B16 60.1(16) . . ? B19 B15 B16 106(2) . . ? C3 B15 B14 58.3(13) . . ? B20 B15 B14 108(2) . . ? B19 B15 B14 60.3(15) . . ? B16 B15 B14 105(2) . . ? C3 B15 H15 124.3 . . ? B20 B15 H15 121.6 . . ? B19 B15 H15 122.6 . . ? B16 B15 H15 123.9 . . ? B14 B15 H15 122.4 . . ? B21 B16 C4 59.8(16) . . ? B21 B16 C3 107(2) . . ? C4 B16 C3 58.3(13) . . ? B21 B16 B20 62.3(18) . . ? C4 B16 B20 110(2) . . ? C3 B16 B20 108.4(18) . . ? B21 B16 B15 109(2) . . ? C4 B16 B15 108.2(19) . . ? C3 B16 B15 60.9(14) . . ? B20 B16 B15 59.7(16) . . ? B21 B16 H16 121.1 . . ? C4 B16 H16 121.9 . . ? C3 B16 H16 122.7 . . ? B20 B16 H16 120.3 . . ? B15 B16 H16 121.1 . . ? C4 B17 B21 57.5(15) . . ? C4 B17 B13 60.4(13) . . ? B21 B17 B13 107(2) . . ? C4 B17 B18 105(2) . . ? B21 B17 B18 104(2) . . ? B13 B17 B18 60.8(15) . . ? C4 B17 B22 104(2) . . ? B21 B17 B22 58.2(18) . . ? B13 B17 B22 108(2) . . ? B18 B17 B22 58.2(17) . . ? C4 B17 H17 124.1 . . ? B21 B17 H17 124.1 . . ? B13 B17 H17 120.2 . . ? B18 B17 H17 123.8 . . ? B22 B17 H17 123.4 . . ? B14 B18 B22 109(2) . . ? B14 B18 B19 62.2(16) . . ? B22 B18 B19 59.8(19) . . ? B14 B18 B17 108(2) . . ? B22 B18 B17 61.6(17) . . ? B19 B18 B17 110(2) . . ? B14 B18 B13 60.8(15) . . ? B22 B18 B13 110(2) . . ? B19 B18 B13 112(2) . . ? B17 B18 B13 59.4(15) . . ? B14 B18 H18 120.9 . . ? B22 B18 H18 120.9 . . ? B19 B18 H18 119.6 . . ? B17 B18 H18 121.4 . . ? B13 B18 H18 120.5 . . ? B22 B19 B18 59.8(18) . . ? B22 B19 B20 60.6(19) . . ? B18 B19 B20 109(2) . . ? B22 B19 B15 107(2) . . ? B18 B19 B15 107(2) . . ? B20 B19 B15 60.1(17) . . ? B22 B19 B14 106(2) . . ? B18 B19 B14 57.8(15) . . ? B20 B19 B14 109(2) . . ? B15 B19 B14 60.7(15) . . ? B22 B19 H19 122.4 . . ? B18 B19 H19 122.4 . . ? B20 B19 H19 120.6 . . ? B15 B19 H19 121.8 . . ? B14 B19 H19 122.7 . . ? B19 B20 B15 60.3(17) . . ? B19 B20 B22 59.3(19) . . ? B15 B20 B22 107(2) . . ? B19 B20 B21 105(2) . . ? B15 B20 B21 104(2) . . ? B22 B20 B21 58.8(19) . . ? B19 B20 B16 106(2) . . ? B15 B20 B16 60.2(16) . . ? B22 B20 B16 103(2) . . ? B21 B20 B16 55.3(16) . . ? B19 B20 H20 122.1 . . ? B15 B20 H20 122.1 . . ? B22 B20 H20 123.4 . . ? B21 B20 H20 125.0 . . ? B16 B20 H20 124.4 . . ? B16 B21 C4 61.2(16) . . ? B16 B21 B22 110(3) . . ? C4 B21 B22 108(2) . . ? B16 B21 B17 110(2) . . ? C4 B21 B17 58.7(15) . . ? B22 B21 B17 62.1(19) . . ? B16 B21 B20 62.3(18) . . ? C4 B21 B20 111(2) . . ? B22 B21 B20 60.4(19) . . ? B17 B21 B20 112(2) . . ? B16 B21 H21 119.8 . . ? C4 B21 H21 122.0 . . ? B22 B21 H21 121.2 . . ? B17 B21 H21 120.1 . . ? B20 B21 H21 119.0 . . ? B21 B22 B19 107(3) . . ? B21 B22 B18 107(3) . . ? B19 B22 B18 60.4(18) . . ? B21 B22 B20 61(2) . . ? B19 B22 B20 60.1(19) . . ? B18 B22 B20 109(3) . . ? B21 B22 B17 59.7(18) . . ? B19 B22 B17 109(3) . . ? B18 B22 B17 60.2(18) . . ? B20 B22 B17 110(3) . . ? B21 B22 H22 122.8 . . ? B19 B22 H22 121.5 . . ? B18 B22 H22 122.1 . . ? B20 B22 H22 120.4 . . ? B17 B22 H22 120.5 . . ? C5 N1 C9 118.7(14) . . ? C5 N1 Ir1 121.1(11) . . ? C9 N1 Ir1 120.2(11) . . ? C10 N2 C13 104.8(12) . . ? C10 N2 Cu3 127.2(10) . . ? C13 N2 Cu3 128.0(10) . . ? C15 N3 C18 105.5(11) . . ? C15 N3 Cu3 127.2(10) . . ? C18 N3 Cu3 127.3(10) . . ? C24 N4 C20 117.7(14) . . ? C24 N4 Ir2 121.8(11) . . ? C20 N4 Ir2 120.5(11) . . ? C2 C1 B3 61.5(11) . . ? C2 C1 B5 109.9(15) . . ? B3 C1 B5 113.3(16) . . ? C2 C1 B4 110.1(16) . . ? B3 C1 B4 61.2(13) . . ? B5 C1 B4 63.3(14) . . ? C2 C1 B6 60.0(12) . . ? B3 C1 B6 112.2(16) . . ? B5 C1 B6 61.6(13) . . ? B4 C1 B6 112.9(16) . . ? C2 C1 S1 118.6(12) . . ? B3 C1 S1 118.2(13) . . ? B5 C1 S1 121.0(16) . . ? B4 C1 S1 121.8(14) . . ? B6 C1 S1 117.9(14) . . ? C1 C2 B6 62.8(13) . . ? C1 C2 B11 112.6(15) . . ? B6 C2 B11 62.5(14) . . ? C1 C2 B3 61.2(11) . . ? B6 C2 B3 114.2(15) . . ? B11 C2 B3 113.3(15) . . ? C1 C2 B7 111.4(14) . . ? B6 C2 B7 113.7(16) . . ? B11 C2 B7 62.0(13) . . ? B3 C2 B7 61.9(11) . . ? C1 C2 S2 119.3(12) . . ? B6 C2 S2 116.9(13) . . ? B11 C2 S2 118.7(13) . . ? B3 C2 S2 118.8(13) . . ? B7 C2 S2 119.8(15) . . ? C4 C3 B16 60.5(13) . . ? C4 C3 B14 109.5(15) . . ? B16 C3 B14 111.4(16) . . ? C4 C3 B13 61.8(12) . . ? B16 C3 B13 113.0(17) . . ? B14 C3 B13 61.6(13) . . ? C4 C3 B15 110.8(16) . . ? B16 C3 B15 61.9(14) . . ? B14 C3 B15 62.1(14) . . ? B13 C3 B15 114.0(16) . . ? C4 C3 S3 121.1(13) . . ? B16 C3 S3 118.9(14) . . ? B14 C3 S3 120.7(13) . . ? B13 C3 S3 118.2(13) . . ? B15 C3 S3 118.4(15) . . ? C3 C4 B21 108.4(19) . . ? C3 C4 B17 111.3(16) . . ? B21 C4 B17 63.9(16) . . ? C3 C4 B16 61.1(13) . . ? B21 C4 B16 59.0(16) . . ? B17 C4 B16 112.7(19) . . ? C3 C4 B13 61.8(12) . . ? B21 C4 B13 113.8(18) . . ? B17 C4 B13 62.4(13) . . ? B16 C4 B13 113.6(18) . . ? C3 C4 S4 116.1(12) . . ? B21 C4 S4 123.5(16) . . ? B17 C4 S4 123.0(17) . . ? B16 C4 S4 116.7(14) . . ? B13 C4 S4 116.9(16) . . ? N1 C5 C6 120.7(16) . . ? N1 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C7 C6 C5 121.1(16) . . ? C7 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C6 117.0(16) . . ? C8 C7 C14 121.4(15) . . ? C6 C7 C14 121.6(15) . . ? C7 C8 C9 120.9(17) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? N1 C9 C8 121.5(16) . . ? N1 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? N2 C10 C19 126.4(14) . 3_666 ? N2 C10 C11 110.3(14) . . ? C19 C10 C11 123.3(14) 3_666 . ? C12 C11 C10 106.7(16) . . ? C12 C11 H11A 126.7 . . ? C10 C11 H11A 126.7 . . ? C11 C12 C13 107.4(17) . . ? C11 C12 H12A 126.3 . . ? C13 C12 H12A 126.3 . . ? N2 C13 C14 124.9(14) . . ? N2 C13 C12 110.8(14) . . ? C14 C13 C12 124.1(15) . . ? C13 C14 C15 124.3(14) . . ? C13 C14 C7 117.8(13) . . ? C15 C14 C7 117.9(13) . . ? N3 C15 C14 125.8(14) . . ? N3 C15 C16 109.2(13) . . ? C14 C15 C16 124.9(14) . . ? C17 C16 C15 107.6(15) . . ? C17 C16 H16A 126.2 . . ? C15 C16 H16A 126.2 . . ? C16 C17 C18 108.2(15) . . ? C16 C17 H17A 125.9 . . ? C18 C17 H17A 125.9 . . ? N3 C18 C19 125.2(14) . . ? N3 C18 C17 109.4(13) . . ? C19 C18 C17 125.3(15) . . ? C18 C19 C10 123.6(14) . 3_666 ? C18 C19 C22 117.7(14) . . ? C10 C19 C22 118.7(14) 3_666 . ? N4 C20 C21 122.7(16) . . ? N4 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? C20 C21 C22 118.3(17) . . ? C20 C21 H21A 120.8 . . ? C22 C21 H21A 120.8 . . ? C23 C22 C21 118.1(15) . . ? C23 C22 C19 119.8(16) . . ? C21 C22 C19 122.1(16) . . ? C22 C23 C24 119.1(16) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? N4 C24 C23 124.0(17) . . ? N4 C24 H24A 118.0 . . ? C23 C24 H24A 118.0 . . ? C29 C25 C30 128.6(18) . . ? C29 C25 C26 107.5(15) . . ? C30 C25 C26 123.5(17) . . ? C29 C25 Ir1 71.2(9) . . ? C30 C25 Ir1 128.8(13) . . ? C26 C25 Ir1 71.0(10) . . ? C27 C26 C25 106.7(15) . . ? C27 C26 C31 127.7(19) . . ? C25 C26 C31 125.5(18) . . ? C27 C26 Ir1 69.5(10) . . ? C25 C26 Ir1 69.8(9) . . ? C31 C26 Ir1 127.2(12) . . ? C26 C27 C28 110.1(16) . . ? C26 C27 C32 125.7(19) . . ? C28 C27 C32 124(2) . . ? C26 C27 Ir1 72.7(10) . . ? C28 C27 Ir1 69.5(9) . . ? C32 C27 Ir1 126.7(13) . . ? C29 C28 C27 106.1(17) . . ? C29 C28 C33 126(2) . . ? C27 C28 C33 128(2) . . ? C29 C28 Ir1 72.7(9) . . ? C27 C28 Ir1 70.8(10) . . ? C33 C28 Ir1 127.6(13) . . ? C28 C29 C25 109.4(16) . . ? C28 C29 C34 125.2(18) . . ? C25 C29 C34 125.2(16) . . ? C28 C29 Ir1 68.8(9) . . ? C25 C29 Ir1 70.5(9) . . ? C34 C29 Ir1 124.2(11) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C39 C35 C36 109.4(16) . . ? C39 C35 C40 126.6(18) . . ? C36 C35 C40 123.8(18) . . ? C39 C35 Ir2 70.5(9) . . ? C36 C35 Ir2 71.2(10) . . ? C40 C35 Ir2 128.1(12) . . ? C35 C36 C37 106.7(17) . . ? C35 C36 C41 126.5(18) . . ? C37 C36 C41 127(2) . . ? C35 C36 Ir2 70.4(9) . . ? C37 C36 Ir2 71.4(10) . . ? C41 C36 Ir2 126.5(14) . . ? C36 C37 C38 108.1(19) . . ? C36 C37 C42 126(2) . . ? C38 C37 C42 125(2) . . ? C36 C37 Ir2 70.4(10) . . ? C38 C37 Ir2 68.9(10) . . ? C42 C37 Ir2 126.4(12) . . ? C39 C38 C37 107.3(18) . . ? C39 C38 C43 125(2) . . ? C37 C38 C43 127(2) . . ? C39 C38 Ir2 71.0(9) . . ? C37 C38 Ir2 72.1(10) . . ? C43 C38 Ir2 126.1(13) . . ? C35 C39 C38 108.4(17) . . ? C35 C39 C44 124.4(18) . . ? C38 C39 C44 127.1(19) . . ? C35 C39 Ir2 71.4(9) . . ? C38 C39 Ir2 70.5(10) . . ? C44 C39 Ir2 127.1(12) . . ? C35 C40 H40A 109.5 . . ? C35 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C35 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C37 C42 H42A 109.5 . . ? C37 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C37 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C39 C44 H44A 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C39 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 O1 102(4) . . ? C46 C45 H45A 128.8 . . ? O1 C45 H45A 128.8 . . ? C45 C46 C47 107(5) . . ? C45 C46 H46A 126.5 . . ? C47 C46 H46A 126.5 . . ? C48 C47 C46 106(4) . . ? C48 C47 H47A 127.2 . . ? C46 C47 H47A 127.2 . . ? O1 C48 C47 101(4) . . ? O1 C48 H48A 129.6 . . ? C47 C48 H48A 129.6 . . ? C48 O1 C45 110(3) . . ? C48 O1 Cu3 117(3) . . ? C45 O1 Cu3 115(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.631 _refine_diff_density_min -2.393 _refine_diff_density_rms 0.209 data_f50521a _database_code_depnum_ccdc_archive 'CCDC 282859' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H79 B20 Cl15 Ir2 N8 S4 Zn' _chemical_formula_weight 2346.36 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' Zn Zn 0.2839 1.4301 '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 24.852(8) _cell_length_b 13.702(5) _cell_length_c 15.216(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.958(5) _cell_angle_gamma 90.00 _cell_volume 5029(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2534 _cell_measurement_theta_min 2.326 _cell_measurement_theta_max 20.922 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2304 _exptl_absorpt_coefficient_mu 3.400 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7273 _exptl_absorpt_correction_T_max 0.7273 _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 20672 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8866 _reflns_number_gt 5403 _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. C35, Cl7, Cl8, Cl9 atoms bond lengths were refined with distance restraints. C34, Cl1 to Cl6 atoms were refined with anisotropic refinement. ; _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^)+(0.0875P)^2^+19.0063P] 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 8866 _refine_ls_number_parameters 551 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1218 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2016 _refine_ls_wR_factor_gt 0.1753 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.403113(18) 1.02583(4) 0.24289(3) 0.0494(2) Uani 1 1 d . . . Zn1 Zn 0.0000 1.0000 0.0000 0.0409(5) Uani 1 2 d S . . S1 S 0.39726(15) 0.8645(3) 0.1916(2) 0.0711(11) Uani 1 1 d . . . S2 S 0.37970(13) 0.9774(3) 0.37809(19) 0.0539(8) Uani 1 1 d . . . N1 N 0.3160(3) 1.0437(7) 0.1805(6) 0.045(2) Uani 1 1 d . . . N2 N 0.0606(3) 0.9362(6) 0.0986(5) 0.0317(19) Uani 1 1 d . . . N3 N -0.0583(3) 0.9133(6) 0.0377(5) 0.0298(19) Uani 1 1 d . . . N4 N 0.0042(4) 0.6218(7) 0.3810(6) 0.044(2) Uani 1 1 d . . . B3 B 0.3044(6) 0.8196(13) 0.2810(11) 0.067(5) Uani 1 1 d . . . H3 H 0.2769 0.8726 0.2378 0.080 Uiso 1 1 calc R . . B4 B 0.3194(11) 0.7083(15) 0.2396(16) 0.117(9) Uani 1 1 d . . . H4 H 0.3016 0.6867 0.1689 0.140 Uiso 1 1 calc R . . B5 B 0.3887(11) 0.6787(15) 0.2951(16) 0.122(10) Uani 1 1 d . . . H5 H 0.4161 0.6377 0.2615 0.146 Uiso 1 1 calc R . . B6 B 0.4155(8) 0.7718(14) 0.3745(13) 0.092(7) Uani 1 1 d . . . H6 H 0.4597 0.7914 0.3920 0.111 Uiso 1 1 calc R . . B7 B 0.3045(8) 0.8059(16) 0.3967(14) 0.095(7) Uani 1 1 d . . . H7 H 0.2773 0.8481 0.4298 0.113 Uiso 1 1 calc R . . B8 B 0.2786(11) 0.7111(17) 0.3163(16) 0.118(9) Uani 1 1 d . . . H8 H 0.2344 0.6916 0.2971 0.141 Uiso 1 1 calc R . . B9 B 0.3306(13) 0.6249(18) 0.3275(18) 0.137(11) Uani 1 1 d . . . H9 H 0.3206 0.5471 0.3151 0.164 Uiso 1 1 calc R . . B10 B 0.3870(13) 0.6638(17) 0.4137(17) 0.147(12) Uani 1 1 d . . . H10 H 0.4134 0.6111 0.4591 0.176 Uiso 1 1 calc R . . B11 B 0.3742(9) 0.7735(17) 0.4540(14) 0.101(7) Uani 1 1 d . . . H11 H 0.3923 0.7955 0.5244 0.121 Uiso 1 1 calc R . . B12 B 0.3234(11) 0.684(2) 0.423(2) 0.144(12) Uani 1 1 d . . . H12 H 0.3076 0.6446 0.4742 0.172 Uiso 1 1 calc R . . C1 C 0.3713(6) 0.7969(10) 0.2716(9) 0.073(4) Uani 1 1 d . . . C2 C 0.3617(5) 0.8535(11) 0.3636(8) 0.064(4) Uani 1 1 d . . . C3 C 0.2930(5) 1.0080(9) 0.0995(7) 0.050(3) Uani 1 1 d . . . H3A H 0.3162 0.9835 0.0650 0.060 Uiso 1 1 calc R . . C4 C 0.2379(5) 1.0051(9) 0.0640(7) 0.046(3) Uani 1 1 d . . . H4A H 0.2240 0.9771 0.0074 0.056 Uiso 1 1 calc R . . C5 C 0.2017(4) 1.0435(8) 0.1111(6) 0.037(3) Uani 1 1 d . . . C6 C 0.2263(4) 1.0878(9) 0.1926(8) 0.053(3) Uani 1 1 d . . . H6A H 0.2042 1.1192 0.2252 0.063 Uiso 1 1 calc R . . C7 C 0.2821(4) 1.0862(9) 0.2257(7) 0.045(3) Uani 1 1 d . . . H7A H 0.2973 1.1153 0.2813 0.054 Uiso 1 1 calc R . . C8 C 0.1397(4) 1.0319(8) 0.0774(6) 0.036(2) Uani 1 1 d . . . C9 C 0.1150(4) 0.9615(8) 0.1217(7) 0.039(3) Uani 1 1 d . . . C10 C 0.1433(4) 0.9060(10) 0.1999(8) 0.057(4) Uani 1 1 d . . . H10A H 0.1808 0.9091 0.2287 0.068 Uiso 1 1 calc R . . C11 C 0.1057(5) 0.8502(10) 0.2224(8) 0.059(4) Uani 1 1 d . . . H11A H 0.1121 0.8073 0.2711 0.071 Uiso 1 1 calc R . . C12 C 0.0530(4) 0.8661(8) 0.1597(7) 0.040(3) Uani 1 1 d . . . C13 C 0.0023(4) 0.8244(8) 0.1633(6) 0.038(3) Uani 1 1 d . . . C14 C -0.0486(4) 0.8425(7) 0.1032(7) 0.034(2) Uani 1 1 d . . . C15 C -0.1000(4) 0.7923(9) 0.1001(7) 0.045(3) Uani 1 1 d . . . H15A H -0.1048 0.7407 0.1372 0.054 Uiso 1 1 calc R . . C16 C -0.1395(4) 0.8326(8) 0.0348(7) 0.045(3) Uani 1 1 d . . . H16A H -0.1767 0.8148 0.0184 0.055 Uiso 1 1 calc R . . C17 C -0.1133(4) 0.9095(8) -0.0057(6) 0.035(2) Uani 1 1 d . . . C18 C 0.0286(7) 0.6010(11) 0.3162(10) 0.080(5) Uani 1 1 d . . . H18A H 0.0471 0.5417 0.3185 0.096 Uiso 1 1 calc R . . C19 C 0.0280(7) 0.6638(10) 0.2433(9) 0.076(4) Uani 1 1 d . . . H19A H 0.0451 0.6444 0.1981 0.091 Uiso 1 1 calc R . . C20 C 0.0032(4) 0.7519(9) 0.2373(6) 0.040(3) Uani 1 1 d . . . C21 C -0.0226(6) 0.7714(10) 0.3040(9) 0.071(4) Uani 1 1 d . . . H21A H -0.0424 0.8292 0.3027 0.085 Uiso 1 1 calc R . . C22 C -0.0199(6) 0.7058(11) 0.3745(9) 0.068(4) Uani 1 1 d . . . H22 H -0.0368 0.7237 0.4204 0.082 Uiso 1 1 calc R . . C23 C 0.4407(6) 1.1132(14) 0.1583(9) 0.080(5) Uani 1 1 d . . . C24 C 0.4270(5) 1.1741(12) 0.2273(11) 0.071(4) Uani 1 1 d . . . C25 C 0.4599(5) 1.1395(11) 0.3123(9) 0.064(4) Uani 1 1 d . . . C26 C 0.4896(5) 1.0583(13) 0.2943(9) 0.071(4) Uani 1 1 d . . . C27 C 0.4800(6) 1.0409(14) 0.1983(10) 0.082(5) Uani 1 1 d . . . C28 C 0.4202(8) 1.1283(16) 0.0543(10) 0.126(8) Uani 1 1 d . . . H28A H 0.3953 1.1829 0.0424 0.190 Uiso 1 1 calc R . . H28B H 0.4013 1.0707 0.0272 0.190 Uiso 1 1 calc R . . H28C H 0.4515 1.1406 0.0291 0.190 Uiso 1 1 calc R . . C29 C 0.3917(8) 1.2595(14) 0.2135(14) 0.130(8) Uani 1 1 d . . . H29A H 0.4115 1.3137 0.1964 0.196 Uiso 1 1 calc R . . H29B H 0.3812 1.2747 0.2687 0.196 Uiso 1 1 calc R . . H29C H 0.3591 1.2466 0.1664 0.196 Uiso 1 1 calc R . . C30 C 0.4638(6) 1.1793(13) 0.4049(10) 0.094(5) Uani 1 1 d . . . H30A H 0.4737 1.1278 0.4486 0.141 Uiso 1 1 calc R . . H30B H 0.4285 1.2061 0.4079 0.141 Uiso 1 1 calc R . . H30C H 0.4915 1.2295 0.4177 0.141 Uiso 1 1 calc R . . C31 C 0.5308(6) 0.9992(14) 0.3676(13) 0.112(7) Uani 1 1 d . . . H31A H 0.5681 1.0182 0.3680 0.167 Uiso 1 1 calc R . . H31B H 0.5261 0.9308 0.3544 0.167 Uiso 1 1 calc R . . H31C H 0.5238 1.0121 0.4259 0.167 Uiso 1 1 calc R . . C32 C 0.5082(8) 0.9692(15) 0.1502(14) 0.124(7) Uani 1 1 d . . . H32A H 0.5113 0.9075 0.1809 0.186 Uiso 1 1 calc R . . H32B H 0.5445 0.9928 0.1498 0.186 Uiso 1 1 calc R . . H32C H 0.4868 0.9613 0.0891 0.186 Uiso 1 1 calc R . . C33 C 0.2754(8) 0.4304(16) 0.9790(13) 0.112(6) Uani 1 1 d . . . H33 H 0.2948 0.4687 0.9417 0.135 Uiso 1 1 calc R . . C34 C 0.1950(14) 0.060(3) 0.726(2) 0.206(13) Uani 1 1 d U . . H34 H 0.2147 0.0151 0.6941 0.247 Uiso 1 1 calc R . . Cl1 Cl 0.2916(4) 0.3066(6) 0.9690(6) 0.206(3) Uani 1 1 d U . . Cl2 Cl 0.2985(3) 0.4679(6) 1.0896(5) 0.164(3) Uani 1 1 d U . . Cl3 Cl 0.2061(3) 0.4427(7) 0.9352(5) 0.179(3) Uani 1 1 d U . . Cl4 Cl 0.2439(6) 0.1337(10) 0.8101(9) 0.300(6) Uani 1 1 d U . . Cl5 Cl 0.1630(5) 0.1540(9) 0.6546(8) 0.267(5) Uani 1 1 d U . . Cl6 Cl 0.1565(5) 0.0018(7) 0.7786(8) 0.223(4) Uani 1 1 d U . . Cl9 Cl 0.1586(8) 0.7817(14) -0.0541(13) 0.216(7) Uiso 0.50 1 d PD . . Cl7 Cl 0.0954(8) 0.6321(15) -0.0070(12) 0.212(7) Uiso 0.50 1 d PD . . Cl8 Cl 0.1874(11) 0.686(2) 0.0947(18) 0.294(11) Uiso 0.50 1 d PD . . C35 C 0.1256(12) 0.7466(17) 0.0334(18) 0.24(3) Uiso 0.50 1 d PD . . H35A H 0.1061 0.7940 0.0626 0.284 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 0.0321(3) 0.0780(4) 0.0335(3) 0.0009(3) -0.00109(17) -0.0057(2) Zn1 0.0276(9) 0.0520(13) 0.0393(9) 0.0189(8) 0.0004(7) -0.0040(8) S1 0.064(2) 0.091(3) 0.0513(19) -0.0113(19) -0.0010(16) 0.015(2) S2 0.0520(18) 0.069(2) 0.0369(15) -0.0011(16) 0.0045(13) -0.0093(17) N1 0.032(5) 0.060(7) 0.039(5) 0.004(5) -0.001(4) -0.007(5) N2 0.027(4) 0.034(5) 0.032(4) 0.006(4) 0.004(3) 0.004(4) N3 0.035(5) 0.031(5) 0.023(4) 0.008(4) 0.006(3) 0.005(4) N4 0.042(5) 0.053(7) 0.041(5) 0.004(5) 0.015(4) 0.004(5) B3 0.057(10) 0.073(12) 0.062(10) 0.000(9) -0.002(8) -0.007(8) B4 0.15(2) 0.058(13) 0.100(16) -0.005(12) -0.047(16) 0.000(14) B5 0.17(2) 0.053(13) 0.106(16) -0.020(12) -0.041(16) 0.037(14) B6 0.089(14) 0.064(13) 0.096(14) 0.008(11) -0.033(11) 0.019(11) B7 0.092(14) 0.092(16) 0.091(14) 0.024(12) 0.005(11) -0.035(12) B8 0.13(2) 0.090(18) 0.111(18) 0.032(14) -0.016(15) -0.046(16) B9 0.19(3) 0.072(16) 0.11(2) 0.044(15) -0.022(18) -0.053(18) B10 0.20(3) 0.073(16) 0.119(19) 0.028(15) -0.066(19) 0.020(18) B11 0.115(17) 0.101(18) 0.070(12) 0.034(12) -0.010(11) -0.009(14) B12 0.13(2) 0.13(2) 0.14(2) 0.10(2) -0.027(17) -0.045(18) C1 0.074(9) 0.057(9) 0.069(9) 0.004(7) -0.022(7) 0.003(8) C2 0.056(8) 0.080(11) 0.043(7) 0.005(7) -0.015(6) 0.000(7) C3 0.040(6) 0.073(10) 0.033(6) 0.000(6) 0.001(5) 0.000(6) C4 0.043(7) 0.057(9) 0.033(6) 0.000(5) -0.005(5) -0.004(5) C5 0.034(6) 0.043(8) 0.032(5) 0.004(5) 0.002(4) -0.001(5) C6 0.040(7) 0.064(9) 0.048(7) -0.009(6) -0.002(5) 0.009(6) C7 0.037(6) 0.050(8) 0.042(6) -0.005(6) 0.000(5) -0.006(6) C8 0.031(5) 0.042(7) 0.033(5) 0.004(5) 0.002(4) -0.002(5) C9 0.027(5) 0.051(8) 0.038(6) 0.011(5) 0.005(4) -0.006(5) C10 0.028(6) 0.082(10) 0.052(7) 0.025(7) -0.007(5) -0.002(6) C11 0.041(7) 0.082(10) 0.049(7) 0.030(7) 0.001(5) -0.003(7) C12 0.030(6) 0.049(7) 0.038(6) 0.009(5) 0.004(4) 0.002(5) C13 0.042(6) 0.046(7) 0.026(5) 0.012(5) 0.006(4) -0.003(5) C14 0.037(6) 0.027(6) 0.041(6) 0.002(5) 0.012(5) 0.001(5) C15 0.050(7) 0.049(8) 0.035(6) 0.017(5) 0.007(5) -0.012(6) C16 0.035(6) 0.047(8) 0.050(7) 0.014(6) 0.002(5) -0.010(5) C17 0.030(5) 0.044(7) 0.028(5) 0.001(5) 0.005(4) 0.006(5) C18 0.116(13) 0.063(10) 0.075(10) 0.033(8) 0.048(9) 0.044(9) C19 0.122(13) 0.057(10) 0.064(9) 0.014(8) 0.055(9) 0.024(9) C20 0.038(6) 0.051(8) 0.032(6) 0.019(5) 0.011(5) -0.001(6) C21 0.111(12) 0.041(8) 0.072(9) 0.023(7) 0.046(9) 0.033(8) C22 0.101(11) 0.062(10) 0.058(8) 0.009(7) 0.050(8) 0.019(9) C23 0.046(8) 0.131(16) 0.060(9) 0.016(10) 0.006(7) -0.023(9) C24 0.041(8) 0.068(11) 0.101(12) 0.001(9) 0.009(8) -0.007(7) C25 0.040(7) 0.089(11) 0.054(8) -0.002(8) -0.006(6) -0.019(7) C26 0.045(8) 0.113(14) 0.054(8) -0.008(8) 0.009(6) -0.017(8) C27 0.055(9) 0.131(16) 0.062(9) -0.012(10) 0.017(7) -0.016(9) C28 0.131(16) 0.18(2) 0.062(10) 0.034(12) 0.009(10) -0.046(15) C29 0.109(15) 0.095(16) 0.162(19) 0.034(14) -0.017(14) -0.049(13) C30 0.081(11) 0.117(15) 0.083(11) -0.038(10) 0.018(9) -0.030(10) C31 0.043(9) 0.159(19) 0.118(15) 0.002(13) -0.010(9) 0.016(10) C32 0.107(15) 0.16(2) 0.112(15) -0.043(14) 0.050(13) 0.001(14) C33 0.111(15) 0.126(18) 0.107(15) -0.011(13) 0.042(12) 0.003(13) C34 0.210(15) 0.203(16) 0.204(15) 0.012(10) 0.050(10) 0.001(10) Cl1 0.250(7) 0.165(6) 0.204(6) 0.016(5) 0.055(6) 0.023(6) Cl2 0.156(5) 0.194(6) 0.145(5) -0.014(4) 0.040(4) 0.006(4) Cl3 0.139(5) 0.227(7) 0.171(6) 0.017(5) 0.035(4) 0.001(5) Cl4 0.295(9) 0.302(10) 0.309(9) -0.026(8) 0.083(8) -0.016(8) Cl5 0.269(8) 0.262(9) 0.272(8) 0.042(7) 0.071(7) 0.028(7) Cl6 0.237(8) 0.201(7) 0.250(8) 0.003(6) 0.096(7) -0.022(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 C23 2.131(14) . ? Ir1 C24 2.147(15) . ? Ir1 C26 2.149(13) . ? Ir1 N1 2.159(8) . ? Ir1 C27 2.187(14) . ? Ir1 C25 2.194(13) . ? Ir1 S1 2.337(4) . ? Ir1 S2 2.364(3) . ? Zn1 N2 2.048(7) . ? Zn1 N2 2.048(7) 3_575 ? Zn1 N3 2.060(8) 3_575 ? Zn1 N3 2.060(8) . ? Zn1 N4 2.483(9) 4_575 ? Zn1 N4 2.483(9) 2 ? S1 C1 1.771(16) . ? S2 C2 1.755(15) . ? N1 C3 1.321(14) . ? N1 C7 1.342(14) . ? N2 C9 1.357(12) . ? N2 C12 1.381(13) . ? N3 C17 1.368(12) . ? N3 C14 1.370(12) . ? N4 C22 1.291(15) . ? N4 C18 1.307(15) . ? N4 Zn1 2.483(9) 2_545 ? B3 C2 1.722(18) . ? B3 B4 1.72(3) . ? B3 C1 1.73(2) . ? B3 B8 1.75(3) . ? B3 B7 1.77(3) . ? B3 H3 1.1000 . ? B4 B8 1.72(4) . ? B4 B9 1.73(3) . ? B4 C1 1.75(3) . ? B4 B5 1.77(3) . ? B4 H4 1.1000 . ? B5 C1 1.69(2) . ? B5 B6 1.77(3) . ? B5 B9 1.79(4) . ? B5 B10 1.83(4) . ? B5 H5 1.1000 . ? B6 C1 1.72(2) . ? B6 C2 1.72(2) . ? B6 B11 1.77(3) . ? B6 B10 1.80(3) . ? B6 H6 1.1000 . ? B7 C2 1.75(2) . ? B7 B12 1.76(3) . ? B7 B8 1.79(3) . ? B7 B11 1.80(3) . ? B7 H7 1.1000 . ? B8 B9 1.73(4) . ? B8 B12 1.77(3) . ? B8 H8 1.1000 . ? B9 B12 1.70(4) . ? B9 B10 1.76(3) . ? B9 H9 1.1000 . ? B10 B12 1.64(4) . ? B10 B11 1.68(3) . ? B10 H10 1.1000 . ? B11 C2 1.73(2) . ? B11 B12 1.74(3) . ? B11 H11 1.1000 . ? B12 H12 1.1000 . ? C1 C2 1.67(2) . ? C3 C4 1.347(15) . ? C3 H3A 0.9300 . ? C4 C5 1.380(15) . ? C4 H4A 0.9300 . ? C5 C6 1.384(14) . ? C5 C8 1.511(13) . ? C6 C7 1.356(14) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C17 1.386(13) 3_575 ? C8 C9 1.401(14) . ? C9 C10 1.443(14) . ? C10 C11 1.316(16) . ? C10 H10A 0.9300 . ? C11 C12 1.438(14) . ? C11 H11A 0.9300 . ? C12 C13 1.397(14) . ? C13 C14 1.394(14) . ? C13 C20 1.498(14) . ? C14 C15 1.441(14) . ? C15 C16 1.337(14) . ? C15 H15A 0.9300 . ? C16 C17 1.451(14) . ? C16 H16A 0.9300 . ? C17 C8 1.386(13) 3_575 ? C18 C19 1.402(17) . ? C18 H18A 0.9300 . ? C19 C20 1.349(16) . ? C19 H19A 0.9300 . ? C20 C21 1.352(15) . ? C21 C22 1.388(17) . ? C21 H21A 0.9300 . ? C22 H22 0.9300 . ? C23 C27 1.42(2) . ? C23 C24 1.44(2) . ? C23 C28 1.555(19) . ? C24 C25 1.434(18) . ? C24 C29 1.45(2) . ? C25 C26 1.40(2) . ? C25 C30 1.493(18) . ? C26 C27 1.442(19) . ? C26 C31 1.55(2) . ? C27 C32 1.50(2) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 Cl3 1.700(19) . ? C33 Cl2 1.72(2) . ? C33 Cl1 1.76(2) . ? C33 H33 0.9800 . ? C34 Cl6 1.60(3) . ? C34 Cl5 1.75(3) . ? C34 Cl4 1.84(3) . ? C34 H34 0.9800 . ? Cl9 C35 1.790(10) . ? Cl7 C35 1.784(10) . ? Cl8 C35 1.795(10) . ? C35 H35A 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 C23 Ir1 C24 39.5(6) . . ? C23 Ir1 C26 63.8(5) . . ? C24 Ir1 C26 64.2(6) . . ? C23 Ir1 N1 102.1(5) . . ? C24 Ir1 N1 96.9(4) . . ? C26 Ir1 N1 161.1(5) . . ? C23 Ir1 C27 38.4(6) . . ? C24 Ir1 C27 65.8(6) . . ? C26 Ir1 C27 38.8(5) . . ? N1 Ir1 C27 135.4(5) . . ? C23 Ir1 C25 64.3(5) . . ? C24 Ir1 C25 38.6(5) . . ? C26 Ir1 C25 37.5(5) . . ? N1 Ir1 C25 126.3(5) . . ? C27 Ir1 C25 64.7(6) . . ? C23 Ir1 S1 109.3(5) . . ? C24 Ir1 S1 148.8(5) . . ? C26 Ir1 S1 107.1(5) . . ? N1 Ir1 S1 89.1(3) . . ? C27 Ir1 S1 88.5(5) . . ? C25 Ir1 S1 144.4(4) . . ? C23 Ir1 S2 156.8(4) . . ? C24 Ir1 S2 119.7(5) . . ? C26 Ir1 S2 100.1(4) . . ? N1 Ir1 S2 89.0(2) . . ? C27 Ir1 S2 135.5(4) . . ? C25 Ir1 S2 92.6(4) . . ? S1 Ir1 S2 90.95(13) . . ? N2 Zn1 N2 180.0(4) . 3_575 ? N2 Zn1 N3 90.4(3) . 3_575 ? N2 Zn1 N3 89.6(3) 3_575 3_575 ? N2 Zn1 N3 89.6(3) . . ? N2 Zn1 N3 90.4(3) 3_575 . ? N3 Zn1 N3 180.0(3) 3_575 . ? N2 Zn1 N4 95.4(3) . 4_575 ? N2 Zn1 N4 84.6(3) 3_575 4_575 ? N3 Zn1 N4 91.6(3) 3_575 4_575 ? N3 Zn1 N4 88.4(3) . 4_575 ? N2 Zn1 N4 84.6(3) . 2 ? N2 Zn1 N4 95.4(3) 3_575 2 ? N3 Zn1 N4 88.4(3) 3_575 2 ? N3 Zn1 N4 91.6(3) . 2 ? N4 Zn1 N4 180.0(4) 4_575 2 ? C1 S1 Ir1 105.6(5) . . ? C2 S2 Ir1 105.7(4) . . ? C3 N1 C7 117.1(9) . . ? C3 N1 Ir1 122.0(8) . . ? C7 N1 Ir1 120.7(7) . . ? C9 N2 C12 107.0(8) . . ? C9 N2 Zn1 126.3(7) . . ? C12 N2 Zn1 126.4(6) . . ? C17 N3 C14 107.7(8) . . ? C17 N3 Zn1 125.2(6) . . ? C14 N3 Zn1 126.8(6) . . ? C22 N4 C18 115.4(11) . . ? C22 N4 Zn1 123.7(8) . 2_545 ? C18 N4 Zn1 120.8(9) . 2_545 ? C2 B3 B4 106.9(12) . . ? C2 B3 C1 57.7(8) . . ? B4 B3 C1 60.9(11) . . ? C2 B3 B8 107.8(12) . . ? B4 B3 B8 59.3(13) . . ? C1 B3 B8 107.6(15) . . ? C2 B3 B7 60.0(9) . . ? B4 B3 B7 108.8(15) . . ? C1 B3 B7 107.0(12) . . ? B8 B3 B7 61.2(12) . . ? C2 B3 H3 122.9 . . ? B4 B3 H3 121.5 . . ? C1 B3 H3 122.6 . . ? B8 B3 H3 121.5 . . ? B7 B3 H3 121.1 . . ? B8 B4 B3 61.1(13) . . ? B8 B4 B9 60.1(17) . . ? B3 B4 B9 108.0(19) . . ? B8 B4 C1 108.1(15) . . ? B3 B4 C1 59.8(10) . . ? B9 B4 C1 105.8(14) . . ? B8 B4 B5 110.2(18) . . ? B3 B4 B5 107.4(13) . . ? B9 B4 B5 61.6(14) . . ? C1 B4 B5 57.3(11) . . ? B8 B4 H4 120.2 . . ? B3 B4 H4 121.6 . . ? B9 B4 H4 122.0 . . ? C1 B4 H4 123.7 . . ? B5 B4 H4 121.4 . . ? C1 B5 B4 60.8(10) . . ? C1 B5 B6 59.3(9) . . ? B4 B5 B6 108.8(15) . . ? C1 B5 B9 105.7(18) . . ? B4 B5 B9 58.1(14) . . ? B6 B5 B9 107.7(19) . . ? C1 B5 B10 104.5(15) . . ? B4 B5 B10 104(2) . . ? B6 B5 B10 60.1(13) . . ? B9 B5 B10 58.0(15) . . ? C1 B5 H5 123.1 . . ? B4 B5 H5 122.4 . . ? B6 B5 H5 120.7 . . ? B9 B5 H5 123.2 . . ? B10 B5 H5 124.5 . . ? C1 B6 C2 58.0(8) . . ? C1 B6 B11 105.8(14) . . ? C2 B6 B11 59.4(11) . . ? C1 B6 B5 58.0(10) . . ? C2 B6 B5 104.3(13) . . ? B11 B6 B5 106.9(18) . . ? C1 B6 B10 104.5(13) . . ? C2 B6 B10 102.0(16) . . ? B11 B6 B10 56.3(14) . . ? B5 B6 B10 61.4(14) . . ? C1 B6 H6 123.7 . . ? C2 B6 H6 124.9 . . ? B11 B6 H6 122.9 . . ? B5 B6 H6 122.1 . . ? B10 B6 H6 124.7 . . ? C2 B7 B12 103.2(16) . . ? C2 B7 B3 58.6(9) . . ? B12 B7 B3 105.1(18) . . ? C2 B7 B8 104.9(16) . . ? B12 B7 B8 59.7(14) . . ? B3 B7 B8 58.9(11) . . ? C2 B7 B11 58.3(10) . . ? B12 B7 B11 58.8(13) . . ? B3 B7 B11 106.2(15) . . ? B8 B7 B11 107.3(18) . . ? C2 B7 H7 124.7 . . ? B12 B7 H7 124.0 . . ? B3 B7 H7 123.1 . . ? B8 B7 H7 122.3 . . ? B11 B7 H7 122.3 . . ? B4 B8 B9 60.2(16) . . ? B4 B8 B3 59.6(12) . . ? B9 B8 B3 106.9(18) . . ? B4 B8 B12 106(2) . . ? B9 B8 B12 58.3(16) . . ? B3 B8 B12 105.3(15) . . ? B4 B8 B7 107.8(16) . . ? B9 B8 B7 106.9(17) . . ? B3 B8 B7 59.8(11) . . ? B12 B8 B7 59.1(14) . . ? B4 B8 H8 122.0 . . ? B9 B8 H8 122.4 . . ? B3 B8 H8 122.7 . . ? B12 B8 H8 124.0 . . ? B7 B8 H8 121.8 . . ? B12 B9 B8 62.0(17) . . ? B12 B9 B4 108.2(19) . . ? B8 B9 B4 59.7(14) . . ? B12 B9 B10 56.7(16) . . ? B8 B9 B10 108(2) . . ? B4 B9 B10 109.1(17) . . ? B12 B9 B5 107.2(17) . . ? B8 B9 B5 108.9(15) . . ? B4 B9 B5 60.3(13) . . ? B10 B9 B5 62.0(16) . . ? B12 B9 H9 122.6 . . ? B8 B9 H9 120.8 . . ? B4 B9 H9 121.3 . . ? B10 B9 H9 121.9 . . ? B5 B9 H9 121.0 . . ? B12 B10 B11 63.2(18) . . ? B12 B10 B9 60.0(18) . . ? B11 B10 B9 111(2) . . ? B12 B10 B6 110.6(17) . . ? B11 B10 B6 60.8(13) . . ? B9 B10 B6 108.0(15) . . ? B12 B10 B5 108.3(17) . . ? B11 B10 B5 108.1(15) . . ? B9 B10 B5 60.0(14) . . ? B6 B10 B5 58.5(13) . . ? B12 B10 H10 119.9 . . ? B11 B10 H10 119.6 . . ? B9 B10 H10 121.2 . . ? B6 B10 H10 121.6 . . ? B5 B10 H10 122.9 . . ? B10 B11 C2 106.9(16) . . ? B10 B11 B12 57.2(17) . . ? C2 B11 B12 104.5(13) . . ? B10 B11 B6 63.0(16) . . ? C2 B11 B6 59.0(10) . . ? B12 B11 B6 107.7(19) . . ? B10 B11 B7 106.8(16) . . ? C2 B11 B7 59.4(9) . . ? B12 B11 B7 59.4(13) . . ? B6 B11 B7 108.8(13) . . ? B10 B11 H11 122.0 . . ? C2 B11 H11 123.7 . . ? B12 B11 H11 124.0 . . ? B6 B11 H11 120.2 . . ? B7 B11 H11 121.7 . . ? B10 B12 B9 63.3(19) . . ? B10 B12 B11 59.6(14) . . ? B9 B12 B11 111(2) . . ? B10 B12 B7 110.6(17) . . ? B9 B12 B7 109.8(16) . . ? B11 B12 B7 61.8(13) . . ? B10 B12 B8 112(2) . . ? B9 B12 B8 59.7(16) . . ? B11 B12 B8 110.9(15) . . ? B7 B12 B8 61.2(12) . . ? B10 B12 H12 119.5 . . ? B9 B12 H12 120.2 . . ? B11 B12 H12 120.5 . . ? B7 B12 H12 120.2 . . ? B8 B12 H12 120.2 . . ? C2 C1 B5 110.5(13) . . ? C2 C1 B6 61.1(9) . . ? B5 C1 B6 62.7(10) . . ? C2 C1 B3 60.8(9) . . ? B5 C1 B3 110.8(15) . . ? B6 C1 B3 112.1(13) . . ? C2 C1 B4 108.1(14) . . ? B5 C1 B4 61.9(12) . . ? B6 C1 B4 112.4(13) . . ? B3 C1 B4 59.3(11) . . ? C2 C1 S1 118.9(10) . . ? B5 C1 S1 122.0(14) . . ? B6 C1 S1 118.2(12) . . ? B3 C1 S1 118.6(9) . . ? B4 C1 S1 122.4(12) . . ? C1 C2 B6 60.8(9) . . ? C1 C2 B3 61.5(8) . . ? B6 C2 B3 112.4(12) . . ? C1 C2 B11 109.8(13) . . ? B6 C2 B11 61.7(11) . . ? B3 C2 B11 111.5(12) . . ? C1 C2 B7 111.1(12) . . ? B6 C2 B7 113.4(14) . . ? B3 C2 B7 61.3(9) . . ? B11 C2 B7 62.3(11) . . ? C1 C2 S2 118.2(10) . . ? B6 C2 S2 116.7(10) . . ? B3 C2 S2 119.6(9) . . ? B11 C2 S2 121.5(10) . . ? B7 C2 S2 121.7(12) . . ? N1 C3 C4 123.6(11) . . ? N1 C3 H3A 118.2 . . ? C4 C3 H3A 118.2 . . ? C3 C4 C5 120.5(10) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C4 C5 C6 115.5(9) . . ? C4 C5 C8 121.5(9) . . ? C6 C5 C8 122.9(9) . . ? C7 C6 C5 121.1(11) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? N1 C7 C6 121.9(10) . . ? N1 C7 H7A 119.1 . . ? C6 C7 H7A 119.1 . . ? C17 C8 C9 126.8(9) 3_575 . ? C17 C8 C5 117.2(9) 3_575 . ? C9 C8 C5 116.0(9) . . ? N2 C9 C8 125.1(9) . . ? N2 C9 C10 109.6(9) . . ? C8 C9 C10 125.2(9) . . ? C11 C10 C9 106.5(9) . . ? C11 C10 H10A 126.7 . . ? C9 C10 H10A 126.7 . . ? C10 C11 C12 109.3(10) . . ? C10 C11 H11A 125.4 . . ? C12 C11 H11A 125.4 . . ? N2 C12 C13 125.6(9) . . ? N2 C12 C11 107.5(9) . . ? C13 C12 C11 126.7(10) . . ? C14 C13 C12 125.9(9) . . ? C14 C13 C20 117.3(9) . . ? C12 C13 C20 116.8(9) . . ? N3 C14 C13 125.2(9) . . ? N3 C14 C15 108.4(8) . . ? C13 C14 C15 126.4(9) . . ? C16 C15 C14 108.2(9) . . ? C16 C15 H15A 125.9 . . ? C14 C15 H15A 125.9 . . ? C15 C16 C17 106.9(9) . . ? C15 C16 H16A 126.5 . . ? C17 C16 H16A 126.5 . . ? N3 C17 C8 125.9(9) . 3_575 ? N3 C17 C16 108.8(8) . . ? C8 C17 C16 125.4(9) 3_575 . ? N4 C18 C19 123.0(13) . . ? N4 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C20 C19 C18 121.3(12) . . ? C20 C19 H19A 119.3 . . ? C18 C19 H19A 119.3 . . ? C19 C20 C21 114.7(11) . . ? C19 C20 C13 124.6(10) . . ? C21 C20 C13 120.7(11) . . ? C20 C21 C22 120.6(12) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? N4 C22 C21 124.8(12) . . ? N4 C22 H22 117.6 . . ? C21 C22 H22 117.6 . . ? C27 C23 C24 110.5(13) . . ? C27 C23 C28 123.4(16) . . ? C24 C23 C28 125.9(17) . . ? C27 C23 Ir1 72.9(9) . . ? C24 C23 Ir1 70.9(8) . . ? C28 C23 Ir1 127.3(10) . . ? C25 C24 C23 106.3(13) . . ? C25 C24 C29 126.3(17) . . ? C23 C24 C29 127.1(17) . . ? C25 C24 Ir1 72.5(9) . . ? C23 C24 Ir1 69.7(9) . . ? C29 C24 Ir1 127.3(11) . . ? C26 C25 C24 107.5(13) . . ? C26 C25 C30 124.0(13) . . ? C24 C25 C30 128.5(15) . . ? C26 C25 Ir1 69.5(8) . . ? C24 C25 Ir1 68.9(8) . . ? C30 C25 Ir1 126.9(10) . . ? C25 C26 C27 111.3(14) . . ? C25 C26 C31 124.3(13) . . ? C27 C26 C31 124.2(16) . . ? C25 C26 Ir1 73.0(8) . . ? C27 C26 Ir1 72.0(8) . . ? C31 C26 Ir1 125.7(11) . . ? C23 C27 C26 104.3(14) . . ? C23 C27 C32 127.1(16) . . ? C26 C27 C32 128.5(17) . . ? C23 C27 Ir1 68.6(8) . . ? C26 C27 Ir1 69.1(8) . . ? C32 C27 Ir1 129.5(13) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl3 C33 Cl2 114.9(11) . . ? Cl3 C33 Cl1 107.0(12) . . ? Cl2 C33 Cl1 110.1(12) . . ? Cl3 C33 H33 108.2 . . ? Cl2 C33 H33 108.2 . . ? Cl1 C33 H33 108.2 . . ? Cl6 C34 Cl5 116(2) . . ? Cl6 C34 Cl4 107(2) . . ? Cl5 C34 Cl4 98.8(19) . . ? Cl6 C34 H34 111.3 . . ? Cl5 C34 H34 111.3 . . ? Cl4 C34 H34 111.3 . . ? Cl7 C35 Cl9 102.2(15) . . ? Cl7 C35 Cl8 90.6(15) . . ? Cl9 C35 Cl8 91.3(16) . . ? Cl7 C35 H35A 121.7 . . ? Cl9 C35 H35A 121.7 . . ? Cl8 C35 H35A 121.7 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.047 _refine_diff_density_min -1.238 _refine_diff_density_rms 0.161