# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name K.Yoshida T.Nakashima S.Yamaguchi A.Osuka H.Shinokubo _publ_contact_author_name 'Shigeru YAMAGUCHI' _publ_contact_author_email s-yamaguchi@chem.s.u-tokyo.ac.jp data_01115ky _database_code_depnum_ccdc_archive 'CCDC 812768' #TrackingRef 'compd2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C149.50 H174 Cl5 Ir2 N12 Ni2 O4.50' _chemical_formula_weight 2890.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.4273(18) _cell_length_b 21.224(2) _cell_length_c 22.036(2) _cell_angle_alpha 73.917(2) _cell_angle_beta 67.416(2) _cell_angle_gamma 64.419(2) _cell_volume 7113.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7751 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.31 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2972 _exptl_absorpt_coefficient_mu 2.276 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.418 _exptl_absorpt_correction_T_max 0.634 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27308 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0734 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16098 _reflns_number_gt 12330 _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. Some tert-butyl substituents showed severe disorders. Thus, restrains by SIMU, ISOR, DFIXs and Free were incorporated to the tert-butyl groups in order to maintain the exact structures. The distance of the C-O bond of one of the MeOH molecules is rather long. Thus, restrains by DFIX were incorporated to the MeOH molecule. ; _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^)+(0.0824P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16098 _refine_ls_number_parameters 1612 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1A C 0.6264(4) 0.7634(4) 0.4163(3) 0.0176(15) Uani 1 1 d . . . C2A C 0.6128(5) 0.7105(5) 0.3974(4) 0.0220(17) Uani 1 1 d . . . C3A C 0.6305(5) 0.6527(4) 0.4400(3) 0.0197(15) Uani 1 1 d . . . H3A H 0.6248 0.6102 0.4402 0.024 Uiso 1 1 calc R . . C4A C 0.6599(5) 0.6645(4) 0.4857(3) 0.0203(16) Uani 1 1 d . . . C5A C 0.6765(4) 0.6191(4) 0.5420(3) 0.0199(15) Uani 1 1 d . . . C6A C 0.7202(5) 0.6298(4) 0.5755(3) 0.0215(16) Uani 1 1 d . . . C7A C 0.7404(5) 0.5877(5) 0.6337(4) 0.0263(17) Uani 1 1 d . . . H7A H 0.7208 0.5508 0.6592 0.032 Uiso 1 1 calc R . . C8A C 0.7913(5) 0.6084(4) 0.6466(4) 0.0256(17) Uani 1 1 d . . . H8A H 0.8158 0.5884 0.6816 0.031 Uiso 1 1 calc R . . C9A C 0.8015(5) 0.6672(4) 0.5967(3) 0.0219(16) Uani 1 1 d . . . C10A C 0.8534(5) 0.7017(4) 0.5895(3) 0.0218(16) Uani 1 1 d . . . C11A C 0.8589(5) 0.7588(4) 0.5427(3) 0.0197(15) Uani 1 1 d . . . C12A C 0.9198(5) 0.7907(5) 0.5286(4) 0.0305(19) Uani 1 1 d . . . H12A H 0.9649 0.7740 0.5469 0.037 Uiso 1 1 calc R . . C13A C 0.9000(5) 0.8494(5) 0.4840(4) 0.0285(18) Uani 1 1 d . . . H13A H 0.9293 0.8811 0.4646 0.034 Uiso 1 1 calc R . . C14A C 0.8267(5) 0.8544(4) 0.4716(3) 0.0210(16) Uani 1 1 d . . . C15A C 0.7787(5) 0.9129(4) 0.4390(3) 0.0232(17) Uani 1 1 d . . . C16A C 0.7047(5) 0.9152(4) 0.4309(3) 0.0204(15) Uani 1 1 d . . . C17A C 0.6437(5) 0.9754(4) 0.4107(3) 0.0235(17) Uani 1 1 d . . . H17A H 0.6410 1.0224 0.4040 0.028 Uiso 1 1 calc R . . C18A C 0.5882(5) 0.9546(4) 0.4021(3) 0.0222(16) Uani 1 1 d . . . C19A C 0.6187(5) 0.8804(4) 0.4157(3) 0.0202(16) Uani 1 1 d . . . C20A C 0.5947(5) 0.8357(4) 0.3972(3) 0.0186(16) Uani 1 1 d . . . C21A C 0.6409(5) 0.5629(4) 0.5679(3) 0.0222(16) Uani 1 1 d . . . C22A C 0.5532(5) 0.5835(5) 0.5812(3) 0.0255(17) Uani 1 1 d . . . H22A H 0.5196 0.6321 0.5746 0.031 Uiso 1 1 calc R . . C23A C 0.5152(5) 0.5334(5) 0.6041(4) 0.0269(18) Uani 1 1 d . . . C24A C 0.5645(6) 0.4645(5) 0.6144(4) 0.0302(19) Uani 1 1 d . . . H24A H 0.5386 0.4305 0.6305 0.036 Uiso 1 1 calc R . . C25A C 0.6513(6) 0.4413(5) 0.6026(4) 0.0302(19) Uani 1 1 d . . . C26A C 0.6882(5) 0.4925(4) 0.5789(3) 0.0231(16) Uani 1 1 d . . . H26A H 0.7473 0.4781 0.5703 0.028 Uiso 1 1 calc R . . C27A C 0.4189(5) 0.5558(5) 0.6195(4) 0.035(2) Uani 1 1 d . . . C28A C 0.4046(6) 0.5186(7) 0.5754(4) 0.048(3) Uani 1 1 d . . . H28A H 0.3533 0.5079 0.5993 0.072 Uiso 1 1 calc R . . H28B H 0.4532 0.4747 0.5651 0.072 Uiso 1 1 calc R . . H28C H 0.3984 0.5498 0.5341 0.072 Uiso 1 1 calc R . . C29A C 0.3827(6) 0.5286(6) 0.6925(4) 0.046(3) Uani 1 1 d . . . H29A H 0.3959 0.5479 0.7209 0.069 Uiso 1 1 calc R . . H29B H 0.4079 0.4770 0.6994 0.069 Uiso 1 1 calc R . . H29C H 0.3213 0.5436 0.7038 0.069 Uiso 1 1 calc R . . C30A C 0.3733(6) 0.6343(6) 0.6088(7) 0.063(3) Uani 1 1 d . . . H30A H 0.3819 0.6566 0.6376 0.095 Uiso 1 1 calc R . . H30B H 0.3128 0.6449 0.6194 0.095 Uiso 1 1 calc R . . H30C H 0.3956 0.6525 0.5623 0.095 Uiso 1 1 calc R . . C31A C 0.7061(6) 0.3635(5) 0.6165(5) 0.039(2) Uani 1 1 d . . . C32A C 0.6531(8) 0.3163(7) 0.6496(8) 0.090(5) Uani 1 1 d . . . H32A H 0.6521 0.2954 0.6155 0.135 Uiso 1 1 calc R . . H32B H 0.5952 0.3447 0.6729 0.135 Uiso 1 1 calc R . . H32C H 0.6783 0.2787 0.6813 0.135 Uiso 1 1 calc R . . C33A C 0.7757(9) 0.3385(7) 0.5530(6) 0.074(4) Uani 1 1 d . . . H33A H 0.8031 0.3730 0.5312 0.110 Uiso 1 1 calc R . . H33B H 0.7511 0.3335 0.5231 0.110 Uiso 1 1 calc R . . H33C H 0.8176 0.2928 0.5639 0.110 Uiso 1 1 calc R . . C34A C 0.7502(8) 0.3556(7) 0.6684(6) 0.065(3) Uani 1 1 d . . . H34A H 0.7895 0.3069 0.6742 0.097 Uiso 1 1 calc R . . H34B H 0.7072 0.3675 0.7111 0.097 Uiso 1 1 calc R . . H34C H 0.7813 0.3876 0.6523 0.097 Uiso 1 1 calc R . . C35A C 0.9071(5) 0.6760(4) 0.6360(3) 0.0221(16) Uani 1 1 d . . . C36A C 0.8845(5) 0.7205(5) 0.6821(4) 0.0291(18) Uani 1 1 d . . . H36A H 0.8354 0.7623 0.6860 0.035 Uiso 1 1 calc R . . C37A C 0.9355(5) 0.7023(5) 0.7225(4) 0.031(2) Uani 1 1 d . A . C38A C 1.0049(5) 0.6426(5) 0.7166(3) 0.0240(17) Uani 1 1 d . . . H38A H 1.0387 0.6312 0.7444 0.029 Uiso 1 1 calc R . . C39A C 1.0299(5) 0.5955(5) 0.6705(3) 0.0250(17) Uani 1 1 d . . . C40A C 0.9774(5) 0.6159(4) 0.6305(3) 0.0238(17) Uani 1 1 d . . . H40A H 0.9914 0.5868 0.5987 0.029 Uiso 1 1 calc R . . C41A C 0.9092(5) 0.7495(5) 0.7774(4) 0.042(2) Uani 1 1 d DU . . C42A C 0.8293(11) 0.7357(13) 0.8271(9) 0.031(6) Uani 0.316(18) 1 d PDU A 1 H42A H 0.8134 0.7543 0.8683 0.047 Uiso 0.316(18) 1 calc PR A 1 H42B H 0.8414 0.6849 0.8366 0.047 Uiso 0.316(18) 1 calc PR A 1 H42C H 0.7828 0.7593 0.8077 0.047 Uiso 0.316(18) 1 calc PR A 1 C43A C 0.9825(10) 0.7237(12) 0.8069(11) 0.039(6) Uani 0.316(18) 1 d PDU A 1 H43A H 0.9718 0.7578 0.8345 0.058 Uiso 0.316(18) 1 calc PR A 1 H43B H 1.0356 0.7191 0.7709 0.058 Uiso 0.316(18) 1 calc PR A 1 H43C H 0.9867 0.6778 0.8341 0.058 Uiso 0.316(18) 1 calc PR A 1 C44A C 0.8908(16) 0.8238(8) 0.7386(11) 0.041(6) Uani 0.316(18) 1 d PDU A 1 H44A H 0.8899 0.8557 0.7638 0.061 Uiso 0.316(18) 1 calc PR A 1 H44B H 0.8357 0.8406 0.7314 0.061 Uiso 0.316(18) 1 calc PR A 1 H44C H 0.9348 0.8227 0.6956 0.061 Uiso 0.316(18) 1 calc PR A 1 C45A C 1.1078(5) 0.5290(5) 0.6635(4) 0.0326(19) Uani 1 1 d . . . C46A C 1.1610(6) 0.5220(6) 0.7064(5) 0.042(2) Uani 1 1 d . . . H46A H 1.1781 0.5627 0.6936 0.063 Uiso 1 1 calc R . . H46B H 1.2114 0.4787 0.6997 0.063 Uiso 1 1 calc R . . H46C H 1.1272 0.5199 0.7533 0.063 Uiso 1 1 calc R . . C47A C 1.0809(7) 0.4633(6) 0.6878(6) 0.056(3) Uani 1 1 d . . . H47A H 1.0501 0.4617 0.7353 0.084 Uiso 1 1 calc R . . H47B H 1.1314 0.4202 0.6800 0.084 Uiso 1 1 calc R . . H47C H 1.0444 0.4668 0.6634 0.084 Uiso 1 1 calc R . . C48A C 1.1644(6) 0.5283(7) 0.5906(5) 0.057(3) Uani 1 1 d . . . H48A H 1.1314 0.5347 0.5621 0.086 Uiso 1 1 calc R . . H48B H 1.2121 0.4831 0.5859 0.086 Uiso 1 1 calc R . . H48C H 1.1857 0.5667 0.5776 0.086 Uiso 1 1 calc R . . C49A C 0.8017(5) 0.9765(4) 0.4096(4) 0.0237(17) Uani 1 1 d . . . C50A C 0.8125(5) 1.0127(5) 0.4476(4) 0.032(2) Uani 1 1 d . . . H50A H 0.8061 0.9968 0.4934 0.038 Uiso 1 1 calc R . . C51A C 0.8331(6) 1.0733(5) 0.4172(4) 0.034(2) Uani 1 1 d . . . C52A C 0.8419(6) 1.0950(5) 0.3512(4) 0.035(2) Uani 1 1 d . . . H52A H 0.8559 1.1357 0.3311 0.042 Uiso 1 1 calc R . . C53A C 0.8313(5) 1.0603(5) 0.3123(4) 0.0301(18) Uani 1 1 d . . . C54A C 0.8111(5) 1.0019(5) 0.3411(4) 0.0259(17) Uani 1 1 d . . . H54A H 0.8032 0.9778 0.3150 0.031 Uiso 1 1 calc R . . C55A C 0.8469(7) 1.1135(6) 0.4580(5) 0.047(3) Uani 1 1 d . . . C56A C 0.8231(7) 1.0878(6) 0.5322(4) 0.047(3) Uani 1 1 d . . . H56A H 0.7670 1.0851 0.5471 0.071 Uiso 1 1 calc R . . H56B H 0.8222 1.1209 0.5562 0.071 Uiso 1 1 calc R . . H56C H 0.8647 1.0411 0.5410 0.071 Uiso 1 1 calc R . . C57A C 0.9356(8) 1.1088(9) 0.4324(6) 0.092(6) Uani 1 1 d . . . H57A H 0.9733 1.0592 0.4320 0.138 Uiso 1 1 calc R . . H57B H 0.9457 1.1302 0.4610 0.138 Uiso 1 1 calc R . . H57C H 0.9466 1.1339 0.3872 0.138 Uiso 1 1 calc R . . C58A C 0.7866(9) 1.1914(7) 0.4504(6) 0.071(4) Uani 1 1 d . . . H58A H 0.8008 1.2117 0.4037 0.107 Uiso 1 1 calc R . . H58B H 0.7928 1.2180 0.4769 0.107 Uiso 1 1 calc R . . H58C H 0.7282 1.1937 0.4660 0.107 Uiso 1 1 calc R . . C59A C 0.8361(7) 1.0893(6) 0.2387(4) 0.044(2) Uani 1 1 d . . . C60A C 0.7541(7) 1.1478(7) 0.2348(5) 0.058(3) Uani 1 1 d . . . H60A H 0.7073 1.1313 0.2600 0.087 Uiso 1 1 calc R . . H60B H 0.7550 1.1625 0.1883 0.087 Uiso 1 1 calc R . . H60C H 0.7466 1.1879 0.2535 0.087 Uiso 1 1 calc R . . C61A C 0.9086(6) 1.1193(7) 0.2039(5) 0.053(3) Uani 1 1 d . . . H61A H 0.8937 1.1620 0.2223 0.080 Uiso 1 1 calc R . . H61B H 0.9162 1.1310 0.1561 0.080 Uiso 1 1 calc R . . H61C H 0.9613 1.0839 0.2115 0.080 Uiso 1 1 calc R . . C62A C 0.8527(11) 1.0322(7) 0.2010(5) 0.080(5) Uani 1 1 d . . . H62A H 0.9109 0.9986 0.1951 0.121 Uiso 1 1 calc R . . H62B H 0.8444 1.0536 0.1575 0.121 Uiso 1 1 calc R . . H62C H 0.8135 1.0075 0.2260 0.121 Uiso 1 1 calc R . . C63A C 0.5916(5) 0.7206(4) 0.3363(3) 0.0219(17) Uani 1 1 d . . . C64A C 0.6063(5) 0.6603(5) 0.3110(4) 0.0281(18) Uani 1 1 d . . . H64A H 0.6221 0.6150 0.3361 0.034 Uiso 1 1 calc R . . C65A C 0.5975(6) 0.6673(5) 0.2501(4) 0.035(2) Uani 1 1 d . . . H65A H 0.6046 0.6273 0.2338 0.042 Uiso 1 1 calc R . . C66A C 0.5787(6) 0.7321(5) 0.2129(4) 0.033(2) Uani 1 1 d . . . H66A H 0.5756 0.7375 0.1696 0.039 Uiso 1 1 calc R . . C67A C 0.5642(5) 0.7903(5) 0.2399(4) 0.0300(19) Uani 1 1 d . . . H67A H 0.5516 0.8353 0.2138 0.036 Uiso 1 1 calc R . . C68A C 0.5068(5) 0.9991(4) 0.3924(3) 0.0218(16) Uani 1 1 d . . . C69A C 0.4701(5) 1.0714(5) 0.4009(4) 0.0279(17) Uani 1 1 d . . . H69A H 0.5022 1.0925 0.4074 0.033 Uiso 1 1 calc R . . C70A C 0.3886(5) 1.1112(5) 0.3999(4) 0.0334(19) Uani 1 1 d . . . H70A H 0.3649 1.1601 0.4035 0.040 Uiso 1 1 calc R . . C71A C 0.3421(5) 1.0784(5) 0.3934(4) 0.0307(18) Uani 1 1 d . . . H71A H 0.2842 1.1034 0.3962 0.037 Uiso 1 1 calc R . . C72A C 0.3806(5) 1.0097(5) 0.3831(4) 0.0265(17) Uani 1 1 d . . . H72A H 0.3479 0.9879 0.3781 0.032 Uiso 1 1 calc R . . C1B C 0.3524(5) 0.2336(4) 1.0606(3) 0.0215(16) Uani 1 1 d . . . C2B C 0.3726(5) 0.2850(4) 1.0748(3) 0.0215(16) Uani 1 1 d . . . C3B C 0.3475(5) 0.3450(4) 1.0333(4) 0.0245(17) Uani 1 1 d . . . H3B H 0.3534 0.3880 1.0307 0.029 Uiso 1 1 calc R . . C4B C 0.3112(5) 0.3316(4) 0.9945(4) 0.0238(17) Uani 1 1 d . . . C5B C 0.2841(5) 0.3788(5) 0.9410(4) 0.0254(17) Uani 1 1 d . . . C6B C 0.2380(5) 0.3666(5) 0.9127(4) 0.0282(18) Uani 1 1 d . . . C7B C 0.2143(5) 0.4076(5) 0.8557(4) 0.0299(19) Uani 1 1 d . . . H7B H 0.2316 0.4452 0.8288 0.036 Uiso 1 1 calc R . . C8B C 0.1629(6) 0.3839(5) 0.8462(4) 0.0332(19) Uani 1 1 d . . . H8B H 0.1371 0.4016 0.8119 0.040 Uiso 1 1 calc R . . C9B C 0.1549(5) 0.3273(5) 0.8975(4) 0.0262(17) Uani 1 1 d . . . C10B C 0.0994(5) 0.2943(4) 0.9089(4) 0.0244(17) Uani 1 1 d . . . C11B C 0.0947(5) 0.2391(5) 0.9590(3) 0.0242(17) Uani 1 1 d . . . C12B C 0.0348(5) 0.2064(5) 0.9763(4) 0.033(2) Uani 1 1 d . . . H12B H -0.0112 0.2215 0.9594 0.039 Uiso 1 1 calc R . . C13B C 0.0566(6) 0.1487(5) 1.0223(4) 0.034(2) Uani 1 1 d . . . H13B H 0.0280 0.1166 1.0433 0.041 Uiso 1 1 calc R . . C14B C 0.1282(6) 0.1458(5) 1.0326(4) 0.0286(19) Uani 1 1 d . . . C15B C 0.1777(5) 0.0889(5) 1.0650(4) 0.0275(18) Uani 1 1 d . . . C16B C 0.2552(5) 0.0859(4) 1.0679(4) 0.0232(17) Uani 1 1 d . . . C17B C 0.3181(5) 0.0237(4) 1.0866(4) 0.0265(17) Uani 1 1 d . . . H17B H 0.3184 -0.0229 1.0965 0.032 Uiso 1 1 calc R . . C18B C 0.3784(5) 0.0444(4) 1.0875(3) 0.0219(16) Uani 1 1 d . . . C19B C 0.3490(5) 0.1190(4) 1.0726(3) 0.0216(16) Uani 1 1 d . . . C20B C 0.3816(5) 0.1626(4) 1.0826(3) 0.0210(16) Uani 1 1 d . . . C21B C 0.3091(5) 0.4412(4) 0.9153(4) 0.0251(16) Uani 1 1 d . . . C22B C 0.2490(5) 0.5091(5) 0.9119(4) 0.0303(18) Uani 1 1 d . . . H22B H 0.1911 0.5149 0.9262 0.036 Uiso 1 1 calc R . . C23B C 0.2700(5) 0.5691(5) 0.8885(4) 0.0297(18) Uani 1 1 d . . . C24B C 0.3583(6) 0.5556(5) 0.8687(4) 0.033(2) Uani 1 1 d . . . H24B H 0.3759 0.5948 0.8524 0.040 Uiso 1 1 calc R . . C25B C 0.4187(5) 0.4902(5) 0.8719(4) 0.033(2) Uani 1 1 d . . . C26B C 0.3948(5) 0.4324(4) 0.8947(3) 0.0246(17) Uani 1 1 d . . . H26B H 0.4366 0.3863 0.8966 0.030 Uiso 1 1 calc R . . C27B C 0.5127(6) 0.4809(5) 0.8497(4) 0.038(2) Uani 1 1 d . . . C28B C 0.5411(7) 0.5145(7) 0.7792(5) 0.058(3) Uani 1 1 d . . . H28D H 0.6002 0.5092 0.7676 0.087 Uiso 1 1 calc R . . H28E H 0.5057 0.5647 0.7751 0.087 Uiso 1 1 calc R . . H28F H 0.5358 0.4914 0.7491 0.087 Uiso 1 1 calc R . . C29B C 0.5232(8) 0.5149(8) 0.8979(5) 0.065(4) Uani 1 1 d . . . H29D H 0.4997 0.4958 0.9437 0.097 Uiso 1 1 calc R . . H29E H 0.4933 0.5661 0.8915 0.097 Uiso 1 1 calc R . . H29F H 0.5834 0.5045 0.8889 0.097 Uiso 1 1 calc R . . C30B C 0.5711(6) 0.4048(6) 0.8532(7) 0.063(3) Uani 1 1 d . . . H30D H 0.6293 0.4021 0.8412 0.095 Uiso 1 1 calc R . . H30E H 0.5672 0.3819 0.8222 0.095 Uiso 1 1 calc R . . H30F H 0.5549 0.3809 0.8984 0.095 Uiso 1 1 calc R . . C31B C 0.2061(6) 0.6425(5) 0.8821(4) 0.038(2) Uani 1 1 d . . . C32B C 0.2141(8) 0.6929(6) 0.9159(6) 0.058(3) Uani 1 1 d . . . H32D H 0.1704 0.7397 0.9115 0.087 Uiso 1 1 calc R . . H32E H 0.2700 0.6963 0.8946 0.087 Uiso 1 1 calc R . . H32F H 0.2070 0.6748 0.9630 0.087 Uiso 1 1 calc R . . C33B C 0.1144(7) 0.6459(6) 0.9144(6) 0.056(3) Uani 1 1 d . . . H33D H 0.1034 0.6191 0.8914 0.084 Uiso 1 1 calc R . . H33E H 0.0757 0.6951 0.9111 0.084 Uiso 1 1 calc R . . H33F H 0.1058 0.6257 0.9612 0.084 Uiso 1 1 calc R . . C34B C 0.2186(7) 0.6713(6) 0.8084(5) 0.054(3) Uani 1 1 d . . . H34D H 0.2258 0.6352 0.7846 0.081 Uiso 1 1 calc R . . H34E H 0.2689 0.6839 0.7900 0.081 Uiso 1 1 calc R . . H34F H 0.1689 0.7132 0.8034 0.081 Uiso 1 1 calc R . . C35B C 0.0466(5) 0.3150(5) 0.8650(4) 0.0264(18) Uani 1 1 d . . . C36B C 0.0765(5) 0.2763(5) 0.8124(4) 0.032(2) Uani 1 1 d . . . H36B H 0.1292 0.2378 0.8065 0.039 Uiso 1 1 calc R . . C37B C 0.0310(6) 0.2928(5) 0.7691(4) 0.033(2) Uani 1 1 d . . . C38B C -0.0455(5) 0.3496(5) 0.7800(4) 0.031(2) Uani 1 1 d . . . H38B H -0.0775 0.3616 0.7507 0.037 Uiso 1 1 calc R . . C39B C -0.0785(5) 0.3905(5) 0.8313(4) 0.0277(18) Uani 1 1 d . . . C40B C -0.0291(5) 0.3719(5) 0.8731(4) 0.0284(18) Uani 1 1 d . . . H40B H -0.0482 0.3990 0.9078 0.034 Uiso 1 1 calc R . . C41B C 0.0650(8) 0.2536(6) 0.7087(5) 0.049(3) Uani 1 1 d . . . C42B C 0.1146(9) 0.2902(8) 0.6521(6) 0.084(5) Uani 1 1 d . . . H42D H 0.1556 0.2964 0.6657 0.126 Uiso 1 1 calc R . . H42E H 0.0764 0.3365 0.6378 0.126 Uiso 1 1 calc R . . H42F H 0.1445 0.2621 0.6152 0.126 Uiso 1 1 calc R . . C43B C 0.1162(16) 0.1766(8) 0.7252(8) 0.151(10) Uani 1 1 d . . . H43D H 0.1227 0.1496 0.6927 0.227 Uiso 1 1 calc R . . H43E H 0.0870 0.1586 0.7697 0.227 Uiso 1 1 calc R . . H43F H 0.1720 0.1719 0.7240 0.227 Uiso 1 1 calc R . . C44B C -0.0069(11) 0.2523(11) 0.6928(6) 0.113(8) Uani 1 1 d . . . H44D H -0.0461 0.3006 0.6852 0.169 Uiso 1 1 calc R . . H44E H -0.0368 0.2256 0.7300 0.169 Uiso 1 1 calc R . . H44F H 0.0154 0.2297 0.6528 0.169 Uiso 1 1 calc R . . C45B C -0.1618(6) 0.4545(6) 0.8401(5) 0.044(2) Uani 1 1 d . . . C46B C -0.2089(7) 0.4638(7) 0.7931(5) 0.057(3) Uani 1 1 d . . . H46D H -0.2265 0.4237 0.8029 0.085 Uiso 1 1 calc R . . H46E H -0.1718 0.4664 0.7473 0.085 Uiso 1 1 calc R . . H46F H -0.2588 0.5075 0.7988 0.085 Uiso 1 1 calc R . . C47B C -0.2194(7) 0.4473(8) 0.9129(5) 0.068(3) Uani 1 1 d . . . H47D H -0.2773 0.4807 0.9160 0.102 Uiso 1 1 calc R . . H47E H -0.1983 0.4575 0.9422 0.102 Uiso 1 1 calc R . . H47F H -0.2192 0.3992 0.9263 0.102 Uiso 1 1 calc R . . C48B C -0.1452(7) 0.5224(6) 0.8262(7) 0.069(3) Uani 1 1 d . . . H48D H -0.1989 0.5627 0.8325 0.104 Uiso 1 1 calc R . . H48E H -0.1090 0.5278 0.7804 0.104 Uiso 1 1 calc R . . H48F H -0.1169 0.5203 0.8568 0.104 Uiso 1 1 calc R . . C49B C 0.1556(5) 0.0261(5) 1.0984(4) 0.0298(19) Uani 1 1 d . . . C50B C 0.1516(6) -0.0184(5) 1.0658(4) 0.037(2) Uani 1 1 d . . . H50B H 0.1571 -0.0053 1.0198 0.044 Uiso 1 1 calc R . . C51B C 0.1397(7) -0.0820(6) 1.0969(4) 0.045(3) Uani 1 1 d . . . C52B C 0.1265(6) -0.0966(5) 1.1659(4) 0.040(2) Uani 1 1 d . . . H52B H 0.1142 -0.1375 1.1892 0.047 Uiso 1 1 calc R . . C53B C 0.1307(5) -0.0537(5) 1.2018(4) 0.0318(19) Uani 1 1 d . . . C54B C 0.1445(5) 0.0073(4) 1.1673(4) 0.0243(17) Uani 1 1 d . . . H54B H 0.1466 0.0377 1.1907 0.029 Uiso 1 1 calc R . . C55B C 0.1386(9) -0.1299(7) 1.0575(6) 0.071(3) Uani 1 1 d U . . C56B C 0.2280(9) -0.1489(9) 0.9948(7) 0.123(5) Uani 1 1 d DU . . H56D H 0.2716 -0.1907 1.0095 0.185 Uiso 1 1 calc R . . H56E H 0.2468 -0.1089 0.9799 0.185 Uiso 1 1 calc R . . H56F H 0.2183 -0.1583 0.9580 0.185 Uiso 1 1 calc R . . C57B C 0.1370(9) -0.2037(7) 1.0982(6) 0.089(4) Uani 1 1 d DU . . H57D H 0.0950 -0.1967 1.1420 0.134 Uiso 1 1 calc R . . H57E H 0.1929 -0.2333 1.1034 0.134 Uiso 1 1 calc R . . H57F H 0.1222 -0.2269 1.0743 0.134 Uiso 1 1 calc R . . C58B C 0.0641(9) -0.0904(8) 1.0280(8) 0.118(5) Uani 1 1 d DU . . H76 H 0.0635 -0.1212 1.0024 0.177 Uiso 1 1 calc R . . H77 H 0.0710 -0.0478 0.9989 0.177 Uiso 1 1 calc R . . H78 H 0.0108 -0.0773 1.0640 0.177 Uiso 1 1 calc R . . C59B C 0.1205(6) -0.0735(5) 1.2752(4) 0.038(2) Uani 1 1 d . . . C60B C 0.1201(8) -0.0169(6) 1.3056(5) 0.057(3) Uani 1 1 d . . . H60D H 0.1739 -0.0098 1.2841 0.085 Uiso 1 1 calc R . . H60E H 0.1124 -0.0319 1.3531 0.085 Uiso 1 1 calc R . . H60F H 0.0737 0.0274 1.2990 0.085 Uiso 1 1 calc R . . C61B C 0.0401(8) -0.0873(9) 1.3118(6) 0.080(5) Uani 1 1 d . . . H61D H -0.0075 -0.0424 1.3194 0.119 Uiso 1 1 calc R . . H61E H 0.0440 -0.1162 1.3545 0.119 Uiso 1 1 calc R . . H61F H 0.0315 -0.1123 1.2854 0.119 Uiso 1 1 calc R . . C62B C 0.1941(7) -0.1383(6) 1.2830(5) 0.050(2) Uani 1 1 d . . . H62D H 0.1990 -0.1743 1.2602 0.075 Uiso 1 1 calc R . . H62E H 0.1863 -0.1560 1.3302 0.075 Uiso 1 1 calc R . . H62F H 0.2457 -0.1275 1.2637 0.075 Uiso 1 1 calc R . . C63B C 0.3963(5) 0.2777(5) 1.1337(4) 0.0264(18) Uani 1 1 d . . . C64B C 0.3847(6) 0.3385(5) 1.1555(4) 0.035(2) Uani 1 1 d . . . H64B H 0.3714 0.3827 1.1283 0.042 Uiso 1 1 calc R . . C65B C 0.3927(7) 0.3337(5) 1.2163(4) 0.043(2) Uani 1 1 d . . . H65B H 0.3862 0.3742 1.2314 0.051 Uiso 1 1 calc R . . C66B C 0.4105(7) 0.2680(5) 1.2550(4) 0.047(3) Uani 1 1 d . . . H66B H 0.4141 0.2634 1.2980 0.056 Uiso 1 1 calc R . . C67B C 0.4226(6) 0.2108(5) 1.2311(4) 0.037(2) Uani 1 1 d . . . H67B H 0.4327 0.1667 1.2588 0.044 Uiso 1 1 calc R . . C68B C 0.4614(5) -0.0018(4) 1.0925(3) 0.0218(16) Uani 1 1 d . . . C69B C 0.4939(5) -0.0738(4) 1.0841(3) 0.0266(17) Uani 1 1 d . . . H69B H 0.4584 -0.0932 1.0800 0.032 Uiso 1 1 calc R . . C70B C 0.5768(6) -0.1163(5) 1.0818(4) 0.036(2) Uani 1 1 d . . . H70B H 0.5982 -0.1648 1.0772 0.043 Uiso 1 1 calc R . . C71B C 0.6269(5) -0.0864(5) 1.0863(4) 0.0316(19) Uani 1 1 d . . . H71B H 0.6844 -0.1138 1.0835 0.038 Uiso 1 1 calc R . . C72B C 0.5933(5) -0.0163(5) 1.0950(4) 0.0276(17) Uani 1 1 d . . . H72B H 0.6294 0.0040 1.0967 0.033 Uiso 1 1 calc R . . C1M C 0.3674(6) 0.9077(5) 0.2792(5) 0.040(2) Uani 1 1 d . . . H1M1 H 0.3208 0.9232 0.3193 0.060 Uiso 1 1 calc R . . H1M2 H 0.3859 0.8565 0.2813 0.060 Uiso 1 1 calc R . . H1M3 H 0.3483 0.9314 0.2401 0.060 Uiso 1 1 calc R . . C2M C 0.6212(7) 0.0913(6) 1.1856(5) 0.054(3) Uani 1 1 d . . . H73 H 0.6484 0.0630 1.2198 0.081 Uiso 1 1 calc R . . H74 H 0.6023 0.1415 1.1886 0.081 Uiso 1 1 calc R . . H75 H 0.6616 0.0811 1.1417 0.081 Uiso 1 1 calc R . . Cl1 Cl 0.41620(12) 0.83600(12) 0.42328(9) 0.0317(4) Uani 1 1 d . . . Cl2 Cl 0.61571(12) 0.91912(11) 0.25488(8) 0.0268(4) Uani 1 1 d . . . Cl3 Cl 0.56527(13) 0.15492(12) 1.04419(10) 0.0361(5) Uani 1 1 d . . . Cl4 Cl 0.36886(13) 0.08240(11) 1.22650(9) 0.0308(4) Uani 1 1 d . . . Ir1 Ir 0.518366(17) 0.876561(16) 0.342120(13) 0.01961(10) Uani 1 1 d . . . Ir2 Ir 0.463214(19) 0.120886(16) 1.133312(13) 0.02287(10) Uani 1 1 d . . . N1 N 0.6636(4) 0.7316(3) 0.4673(3) 0.0183(13) Uani 1 1 d . . . N2 N 0.6877(4) 0.8554(4) 0.4390(3) 0.0189(13) Uani 1 1 d . . . N3 N 0.7556(4) 0.6818(4) 0.5535(3) 0.0202(13) Uani 1 1 d . . . N4 N 0.2761(4) 0.1447(4) 1.0541(3) 0.0216(14) Uani 1 1 d . . . N5 N 0.3091(4) 0.2645(4) 1.0142(3) 0.0207(13) Uani 1 1 d . . . N6 N 0.2052(4) 0.3135(4) 0.9368(3) 0.0228(14) Uani 1 1 d . . . N7 N 0.1517(4) 0.2026(4) 0.9945(3) 0.0231(14) Uani 1 1 d . . . N8 N 0.5114(4) 0.0249(4) 1.1011(3) 0.0258(15) Uani 1 1 d . . . N9 N 0.4211(4) 0.2135(4) 1.1692(3) 0.0286(16) Uani 1 1 d . . . N10 N 0.8057(4) 0.7958(3) 0.5047(3) 0.0202(13) Uani 1 1 d . . . N11 N 0.4622(4) 0.9703(4) 0.3794(3) 0.0251(14) Uani 1 1 d . . . N12 N 0.5671(4) 0.7856(4) 0.3011(3) 0.0221(14) Uani 1 1 d . . . Ni1 Ni 0.72855(5) 0.76597(5) 0.49092(4) 0.0168(2) Uani 1 1 d . . . Ni2 Ni 0.23468(6) 0.23183(5) 1.00018(4) 0.0194(2) Uani 1 1 d . . . O1 O 0.4367(3) 0.9250(3) 0.2747(3) 0.0283(12) Uani 1 1 d . . . H1 H 0.4493 0.9603 0.2398 0.034 Uiso 1 1 calc R . . O2 O 0.5512(4) 0.0746(3) 1.1952(3) 0.0351(14) Uani 1 1 d . . . H2 H 0.5400 0.0401 1.2317 0.042 Uiso 1 1 calc R . . C42T C 0.8910(13) 0.7014(9) 0.8458(6) 0.091(8) Uani 0.684(18) 1 d PD A 2 H42G H 0.8996 0.7177 0.8791 0.137 Uiso 0.684(18) 1 calc PR A 2 H42H H 0.9295 0.6525 0.8407 0.137 Uiso 0.684(18) 1 calc PR A 2 H42I H 0.8325 0.7042 0.8600 0.137 Uiso 0.684(18) 1 calc PR A 2 C44T C 0.8283(11) 0.8205(8) 0.7766(10) 0.121(13) Uani 0.684(18) 1 d PD A 2 H44G H 0.8164 0.8464 0.8120 0.182 Uiso 0.684(18) 1 calc PR A 2 H44H H 0.7795 0.8088 0.7836 0.182 Uiso 0.684(18) 1 calc PR A 2 H44I H 0.8396 0.8498 0.7337 0.182 Uiso 0.684(18) 1 calc PR A 2 C43T C 0.9887(8) 0.7660(10) 0.7661(8) 0.067(6) Uani 0.684(18) 1 d PD A 2 H43G H 1.0336 0.7225 0.7766 0.101 Uiso 0.684(18) 1 calc PR A 2 H43H H 0.9739 0.8003 0.7950 0.101 Uiso 0.684(18) 1 calc PR A 2 H43I H 1.0084 0.7855 0.7197 0.101 Uiso 0.684(18) 1 calc PR A 2 Cl5 Cl 0.0608(2) 0.5731(2) 0.44419(16) 0.0761(8) Uiso 1 1 d . . . O4 O 0.5177(5) 0.2381(5) 0.9064(4) 0.0622(19) Uiso 1 1 d . . . H4 H 0.5113 0.2101 0.9417 0.093 Uiso 1 1 d R . . C73 C 0.6023(8) 0.2138(7) 0.8682(6) 0.065(3) Uiso 1 1 d . . . H73A H 0.6310 0.2406 0.8734 0.097 Uiso 1 1 d R . . H73B H 0.6055 0.2207 0.8215 0.097 Uiso 1 1 d R . . H73C H 0.6298 0.1636 0.8824 0.097 Uiso 1 1 d R . . O5 O 0.5803(6) 0.1396(6) 0.4366(4) 0.086(3) Uiso 1 1 d . . . H5 H 0.5371 0.1301 0.4600 0.129 Uiso 1 1 d R . . C74 C 0.0443(11) 0.4964(11) 0.4801(8) 0.104(5) Uiso 1 1 d . . . H74A H 0.0630 0.4675 0.4447 0.125 Uiso 1 1 calc R . . H74B H 0.0807 0.4702 0.5092 0.125 Uiso 1 1 calc R . . C75 C 0.5643(13) 0.2051(11) 0.4061(9) 0.124(6) Uiso 1 1 d . . . H75A H 0.5132 0.2334 0.4371 0.186 Uiso 1 1 d R . . H75B H 0.5528 0.2091 0.3650 0.186 Uiso 1 1 d R . . H75C H 0.6098 0.2222 0.3961 0.186 Uiso 1 1 d R . . O7 O 0.0118(11) 0.4600(10) 0.0927(7) 0.075(4) Uiso 0.50 1 d PD . . H79 H 0.0511 0.4259 0.1045 0.112 Uiso 0.50 1 calc PR . . C77 C 0.030(2) 0.467(2) 0.0224(9) 0.104(10) Uiso 0.50 1 d PD . . H77A H 0.0006 0.4810 -0.0108 0.155 Uiso 0.50 1 d PR . . H77B H 0.0791 0.4231 0.0128 0.155 Uiso 0.50 1 d PR . . H77C H 0.0488 0.5040 0.0211 0.155 Uiso 0.50 1 d 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 C1A 0.018(4) 0.014(4) 0.017(3) 0.007(3) -0.011(3) -0.003(3) C2A 0.019(4) 0.023(5) 0.023(4) 0.003(4) -0.013(3) -0.006(4) C3A 0.023(4) 0.008(4) 0.031(4) 0.005(3) -0.019(3) -0.003(3) C4A 0.020(4) 0.017(4) 0.023(4) -0.001(3) -0.008(3) -0.006(4) C5A 0.021(4) 0.013(4) 0.025(4) 0.004(3) -0.012(3) -0.005(4) C6A 0.023(4) 0.016(4) 0.021(3) 0.004(3) -0.009(3) -0.005(4) C7A 0.034(5) 0.020(5) 0.027(4) 0.009(4) -0.020(3) -0.010(4) C8A 0.031(4) 0.021(5) 0.025(4) 0.005(4) -0.017(3) -0.008(4) C9A 0.021(4) 0.018(4) 0.021(3) 0.007(3) -0.013(3) -0.002(4) C10A 0.025(4) 0.018(4) 0.022(3) 0.007(3) -0.017(3) -0.006(4) C11A 0.020(4) 0.010(4) 0.028(4) 0.005(3) -0.018(3) 0.001(3) C12A 0.029(4) 0.028(5) 0.042(4) 0.006(4) -0.025(4) -0.011(4) C13A 0.032(5) 0.021(5) 0.033(4) 0.006(4) -0.018(4) -0.011(4) C14A 0.018(4) 0.017(4) 0.027(4) 0.004(3) -0.011(3) -0.007(4) C15A 0.027(4) 0.019(4) 0.020(3) 0.004(3) -0.009(3) -0.008(4) C16A 0.024(4) 0.014(4) 0.022(3) 0.003(3) -0.011(3) -0.006(4) C17A 0.026(4) 0.019(4) 0.026(4) 0.002(3) -0.011(3) -0.008(4) C18A 0.026(4) 0.022(4) 0.015(3) 0.002(3) -0.010(3) -0.005(4) C19A 0.024(4) 0.014(4) 0.022(3) 0.003(3) -0.017(3) 0.000(4) C20A 0.021(4) 0.019(4) 0.016(3) 0.003(3) -0.008(3) -0.009(4) C21A 0.027(4) 0.019(4) 0.023(3) 0.002(3) -0.016(3) -0.006(4) C22A 0.030(4) 0.017(4) 0.026(4) 0.008(3) -0.014(3) -0.007(4) C23A 0.031(5) 0.024(5) 0.029(4) 0.003(4) -0.016(3) -0.011(4) C24A 0.047(5) 0.022(5) 0.033(4) 0.016(4) -0.027(4) -0.021(5) C25A 0.036(5) 0.023(5) 0.033(4) 0.004(4) -0.019(4) -0.010(4) C26A 0.023(4) 0.017(4) 0.026(4) 0.007(3) -0.014(3) -0.005(4) C27A 0.031(5) 0.035(6) 0.043(5) 0.008(4) -0.019(4) -0.017(5) C28A 0.045(6) 0.066(8) 0.044(5) -0.001(5) -0.021(4) -0.027(6) C29A 0.042(6) 0.061(7) 0.043(5) -0.012(5) -0.009(4) -0.026(6) C30A 0.026(5) 0.044(7) 0.113(10) -0.008(7) -0.024(6) -0.006(6) C31A 0.044(5) 0.012(4) 0.057(5) 0.013(4) -0.025(4) -0.007(5) C32A 0.072(9) 0.033(7) 0.175(15) 0.027(9) -0.074(9) -0.021(7) C33A 0.082(10) 0.033(7) 0.096(10) -0.005(7) -0.042(8) -0.001(7) C34A 0.066(8) 0.049(8) 0.082(8) 0.030(7) -0.053(6) -0.020(7) C35A 0.023(4) 0.016(4) 0.029(4) 0.001(3) -0.014(3) -0.005(4) C36A 0.024(4) 0.022(5) 0.043(4) -0.004(4) -0.018(3) -0.003(4) C37A 0.027(4) 0.037(6) 0.035(4) -0.008(4) -0.014(3) -0.010(5) C38A 0.022(4) 0.029(5) 0.024(3) 0.005(4) -0.017(3) -0.007(4) C39A 0.027(4) 0.025(5) 0.027(4) 0.004(4) -0.016(3) -0.010(4) C40A 0.024(4) 0.022(5) 0.027(4) 0.001(4) -0.016(3) -0.005(4) C41A 0.037(4) 0.048(5) 0.042(4) -0.015(4) -0.018(3) -0.007(4) C42A 0.032(9) 0.036(10) 0.028(8) -0.014(7) -0.014(7) -0.004(7) C43A 0.046(10) 0.051(10) 0.038(9) -0.022(7) -0.027(7) -0.011(8) C44A 0.047(10) 0.040(10) 0.035(9) -0.018(8) -0.009(7) -0.011(8) C45A 0.030(5) 0.027(5) 0.036(4) -0.001(4) -0.022(4) 0.002(4) C46A 0.038(5) 0.040(6) 0.052(5) 0.004(5) -0.031(4) -0.008(5) C47A 0.052(7) 0.036(6) 0.094(8) -0.009(6) -0.039(6) -0.012(6) C48A 0.032(5) 0.072(9) 0.048(6) -0.014(6) -0.012(4) 0.003(6) C49A 0.024(4) 0.014(4) 0.034(4) -0.002(4) -0.014(3) -0.004(4) C50A 0.045(5) 0.027(5) 0.032(4) 0.009(4) -0.020(4) -0.022(5) C51A 0.038(5) 0.023(5) 0.044(5) -0.002(4) -0.015(4) -0.014(5) C52A 0.040(5) 0.025(5) 0.042(5) 0.001(4) -0.013(4) -0.017(5) C53A 0.034(5) 0.017(5) 0.038(4) 0.004(4) -0.017(4) -0.006(4) C54A 0.026(4) 0.020(4) 0.034(4) 0.009(4) -0.022(3) -0.007(4) C55A 0.063(7) 0.040(6) 0.057(6) -0.008(5) -0.021(5) -0.033(6) C56A 0.060(7) 0.053(7) 0.044(5) -0.012(5) -0.026(4) -0.022(6) C57A 0.057(8) 0.144(15) 0.110(10) -0.088(11) 0.014(7) -0.059(10) C58A 0.096(10) 0.045(7) 0.086(8) -0.011(7) -0.037(7) -0.028(8) C59A 0.066(7) 0.038(6) 0.031(4) 0.016(4) -0.020(4) -0.029(6) C60A 0.054(7) 0.066(9) 0.058(6) 0.035(6) -0.039(5) -0.033(7) C61A 0.045(6) 0.060(8) 0.041(5) 0.029(5) -0.020(4) -0.022(6) C62A 0.154(14) 0.058(9) 0.030(5) 0.009(6) -0.028(7) -0.049(10) C63A 0.029(4) 0.021(5) 0.019(3) 0.005(3) -0.010(3) -0.014(4) C64A 0.036(5) 0.019(5) 0.031(4) 0.007(4) -0.018(3) -0.011(4) C65A 0.043(5) 0.034(5) 0.036(4) -0.012(4) -0.015(4) -0.014(5) C66A 0.054(6) 0.025(5) 0.022(4) 0.008(4) -0.024(4) -0.013(5) C67A 0.040(5) 0.026(5) 0.026(4) 0.004(4) -0.018(3) -0.012(4) C68A 0.026(4) 0.019(4) 0.014(3) 0.007(3) -0.011(3) -0.003(4) C69A 0.030(4) 0.021(5) 0.026(4) -0.003(4) -0.012(3) 0.000(4) C70A 0.033(5) 0.023(5) 0.030(4) -0.006(4) -0.013(3) 0.006(4) C71A 0.024(4) 0.028(5) 0.027(4) -0.003(4) -0.012(3) 0.006(4) C72A 0.016(4) 0.029(5) 0.026(4) -0.006(4) -0.008(3) 0.003(4) C1B 0.025(4) 0.017(4) 0.019(3) 0.004(3) -0.013(3) -0.004(4) C2B 0.026(4) 0.014(4) 0.023(3) 0.003(3) -0.011(3) -0.006(4) C3B 0.035(4) 0.008(4) 0.033(4) 0.008(3) -0.023(3) -0.005(4) C4B 0.025(4) 0.015(4) 0.034(4) 0.002(4) -0.015(3) -0.008(4) C5B 0.027(4) 0.019(5) 0.026(4) 0.005(4) -0.011(3) -0.007(4) C6B 0.028(4) 0.017(4) 0.036(4) 0.003(4) -0.016(3) -0.005(4) C7B 0.034(5) 0.021(5) 0.036(4) 0.016(4) -0.023(4) -0.012(4) C8B 0.041(5) 0.024(5) 0.034(4) 0.010(4) -0.027(4) -0.007(5) C9B 0.032(4) 0.016(4) 0.030(4) 0.007(4) -0.021(3) -0.004(4) C10B 0.027(4) 0.016(4) 0.028(4) 0.003(4) -0.017(3) -0.003(4) C11B 0.023(4) 0.021(5) 0.025(4) 0.005(4) -0.017(3) -0.002(4) C12B 0.034(5) 0.029(5) 0.040(4) 0.011(4) -0.027(4) -0.011(5) C13B 0.035(5) 0.035(6) 0.036(4) 0.013(4) -0.017(4) -0.021(5) C14B 0.040(5) 0.022(5) 0.032(4) 0.009(4) -0.023(4) -0.016(5) C15B 0.037(5) 0.020(5) 0.030(4) 0.005(4) -0.018(3) -0.013(4) C16B 0.030(4) 0.014(4) 0.026(4) 0.004(3) -0.016(3) -0.005(4) C17B 0.035(5) 0.016(4) 0.029(4) 0.005(4) -0.018(3) -0.008(4) C18B 0.030(4) 0.011(4) 0.025(4) 0.001(3) -0.017(3) -0.002(4) C19B 0.028(4) 0.016(4) 0.020(3) 0.006(3) -0.012(3) -0.008(4) C20B 0.029(4) 0.014(4) 0.017(3) 0.001(3) -0.010(3) -0.003(4) C21B 0.030(4) 0.011(4) 0.032(4) 0.005(4) -0.019(3) -0.001(4) C22B 0.032(5) 0.026(5) 0.031(4) 0.008(4) -0.016(3) -0.009(4) C23B 0.041(5) 0.018(4) 0.031(4) 0.003(4) -0.019(3) -0.008(4) C24B 0.046(5) 0.025(5) 0.036(4) 0.005(4) -0.021(4) -0.016(5) C25B 0.037(5) 0.030(5) 0.038(4) 0.002(4) -0.022(4) -0.013(5) C26B 0.025(4) 0.019(4) 0.027(4) 0.011(3) -0.017(3) -0.007(4) C27B 0.043(5) 0.033(6) 0.047(5) -0.001(5) -0.022(4) -0.018(5) C28B 0.061(7) 0.061(8) 0.059(6) 0.007(6) -0.021(5) -0.035(7) C29B 0.063(8) 0.097(11) 0.064(7) -0.025(7) -0.021(5) -0.046(8) C30B 0.024(5) 0.049(7) 0.106(9) -0.003(7) -0.025(5) -0.004(6) C31B 0.048(6) 0.016(5) 0.049(5) 0.002(4) -0.031(4) -0.001(5) C32B 0.069(8) 0.019(5) 0.084(8) -0.011(6) -0.032(6) -0.005(6) C33B 0.055(7) 0.020(5) 0.070(7) 0.001(5) -0.019(5) 0.002(5) C34B 0.060(7) 0.024(6) 0.061(6) 0.010(5) -0.031(5) 0.002(6) C35B 0.028(4) 0.022(5) 0.031(4) 0.001(4) -0.015(3) -0.008(4) C36B 0.030(5) 0.029(5) 0.034(4) -0.007(4) -0.008(3) -0.006(4) C37B 0.047(5) 0.025(5) 0.034(4) -0.002(4) -0.019(4) -0.014(5) C38B 0.035(5) 0.034(6) 0.028(4) 0.007(4) -0.021(3) -0.013(5) C39B 0.025(4) 0.026(5) 0.027(4) 0.005(4) -0.013(3) -0.005(4) C40B 0.033(5) 0.024(5) 0.029(4) -0.002(4) -0.014(3) -0.008(4) C41B 0.083(8) 0.028(6) 0.040(5) -0.004(5) -0.024(5) -0.019(6) C42B 0.090(11) 0.092(12) 0.055(7) -0.046(8) 0.027(7) -0.041(10) C43B 0.28(3) 0.042(8) 0.106(12) -0.046(9) -0.125(15) 0.047(13) C44B 0.139(15) 0.18(2) 0.070(8) -0.068(11) 0.001(8) -0.104(16) C45B 0.037(5) 0.040(6) 0.051(5) -0.003(5) -0.021(4) -0.007(5) C46B 0.041(6) 0.055(8) 0.054(6) 0.010(6) -0.023(5) -0.002(6) C47B 0.040(6) 0.067(9) 0.050(6) -0.002(6) -0.015(5) 0.020(6) C48B 0.041(6) 0.026(6) 0.114(10) 0.001(7) -0.035(7) 0.015(6) C49B 0.028(4) 0.028(5) 0.033(4) 0.011(4) -0.018(3) -0.011(4) C50B 0.057(6) 0.035(6) 0.035(4) 0.021(4) -0.031(4) -0.032(5) C51B 0.067(7) 0.041(6) 0.048(5) 0.009(5) -0.026(5) -0.039(6) C52B 0.049(6) 0.030(6) 0.050(5) 0.020(5) -0.031(4) -0.025(5) C53B 0.028(4) 0.028(5) 0.035(4) 0.010(4) -0.016(3) -0.009(4) C54B 0.030(4) 0.014(4) 0.031(4) 0.012(4) -0.020(3) -0.009(4) C55B 0.103(6) 0.076(6) 0.080(6) -0.006(5) -0.045(5) -0.060(5) C56B 0.140(9) 0.122(9) 0.121(9) -0.043(7) -0.029(7) -0.054(7) C57B 0.115(8) 0.081(7) 0.095(7) -0.012(6) -0.046(6) -0.044(7) C58B 0.135(9) 0.112(9) 0.140(9) -0.016(7) -0.071(7) -0.049(7) C59B 0.039(5) 0.028(5) 0.038(5) 0.015(4) -0.020(4) -0.009(5) C60B 0.086(9) 0.037(6) 0.039(5) 0.005(5) -0.029(5) -0.014(7) C61B 0.069(9) 0.106(13) 0.057(7) 0.029(8) -0.020(6) -0.050(10) C62B 0.059(7) 0.033(6) 0.046(5) -0.001(5) -0.031(5) 0.003(6) C63B 0.026(4) 0.021(5) 0.033(4) -0.002(4) -0.012(3) -0.007(4) C64B 0.052(6) 0.027(5) 0.039(4) -0.001(4) -0.022(4) -0.022(5) C65B 0.070(7) 0.026(5) 0.042(5) -0.002(5) -0.030(5) -0.017(6) C66B 0.082(8) 0.026(6) 0.037(5) 0.003(4) -0.040(5) -0.010(6) C67B 0.063(6) 0.022(5) 0.030(4) 0.003(4) -0.029(4) -0.010(5) C68B 0.028(4) 0.014(4) 0.016(3) 0.006(3) -0.010(3) -0.004(4) C69B 0.032(4) 0.013(4) 0.024(4) 0.000(4) -0.008(3) -0.001(4) C70B 0.052(6) 0.027(5) 0.022(4) -0.001(4) -0.008(4) -0.013(5) C71B 0.025(4) 0.032(5) 0.026(4) -0.005(4) -0.012(3) 0.005(4) C72B 0.022(4) 0.025(5) 0.027(4) 0.002(4) -0.014(3) 0.001(4) C1M 0.039(5) 0.037(6) 0.056(5) 0.002(5) -0.033(4) -0.014(5) C2M 0.069(7) 0.045(7) 0.070(7) 0.023(6) -0.054(6) -0.030(7) Cl1 0.0261(10) 0.0325(12) 0.0338(10) 0.0057(9) -0.0131(8) -0.0113(10) Cl2 0.0327(10) 0.0191(10) 0.0249(9) 0.0043(8) -0.0138(7) -0.0063(9) Cl3 0.0359(11) 0.0304(12) 0.0432(11) 0.0075(10) -0.0212(9) -0.0127(11) Cl4 0.0396(11) 0.0197(11) 0.0270(9) 0.0032(9) -0.0160(8) -0.0042(10) Ir1 0.02113(16) 0.01481(17) 0.02136(15) 0.00340(13) -0.01388(11) -0.00232(14) Ir2 0.03005(18) 0.01432(18) 0.02601(16) 0.00282(13) -0.01929(12) -0.00368(15) N1 0.020(3) 0.013(3) 0.022(3) 0.005(3) -0.015(2) -0.003(3) N2 0.018(3) 0.016(4) 0.022(3) 0.005(3) -0.013(2) -0.005(3) N3 0.021(3) 0.016(4) 0.025(3) -0.001(3) -0.013(2) -0.005(3) N4 0.030(4) 0.015(4) 0.022(3) 0.008(3) -0.017(3) -0.010(3) N5 0.023(3) 0.014(3) 0.024(3) 0.004(3) -0.017(2) -0.001(3) N6 0.022(3) 0.017(4) 0.025(3) 0.002(3) -0.012(3) -0.001(3) N7 0.027(3) 0.015(4) 0.026(3) 0.005(3) -0.015(3) -0.005(3) N8 0.029(4) 0.019(4) 0.027(3) 0.003(3) -0.015(3) -0.005(3) N9 0.039(4) 0.025(4) 0.027(3) 0.001(3) -0.016(3) -0.013(4) N10 0.018(3) 0.015(4) 0.025(3) -0.001(3) -0.013(2) 0.000(3) N11 0.024(4) 0.022(4) 0.027(3) 0.000(3) -0.010(3) -0.007(3) N12 0.025(3) 0.020(4) 0.021(3) 0.002(3) -0.009(3) -0.009(3) Ni1 0.0185(5) 0.0116(5) 0.0201(4) 0.0038(4) -0.0123(3) -0.0035(4) Ni2 0.0220(5) 0.0125(5) 0.0237(4) 0.0034(4) -0.0139(4) -0.0038(4) O1 0.034(3) 0.021(3) 0.035(3) 0.005(3) -0.024(2) -0.007(3) O2 0.051(4) 0.023(3) 0.044(3) 0.006(3) -0.035(3) -0.014(3) C42T 0.100(19) 0.074(16) 0.055(11) -0.023(12) 0.002(11) -0.005(16) C44T 0.17(3) 0.064(14) 0.13(2) -0.075(16) -0.11(2) 0.052(16) C43T 0.067(12) 0.065(13) 0.091(14) -0.038(12) -0.044(10) -0.010(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1A C20A 1.389(11) . ? C1A N1 1.400(9) . ? C1A C2A 1.443(10) . ? C2A C3A 1.321(11) . ? C2A C63A 1.477(9) . ? C3A C4A 1.431(9) . ? C3A H3A 0.9500 . ? C4A C5A 1.391(11) . ? C4A N1 1.392(10) . ? C5A C6A 1.398(9) . ? C5A C21A 1.480(10) . ? C6A N3 1.400(9) . ? C6A C7A 1.424(11) . ? C7A C8A 1.335(10) . ? C7A H7A 0.9500 . ? C8A C9A 1.445(11) . ? C8A H8A 0.9500 . ? C9A C10A 1.378(9) . ? C9A N3 1.395(9) . ? C10A C11A 1.369(10) . ? C10A C35A 1.526(10) . ? C11A N10 1.372(9) . ? C11A C12A 1.445(9) . ? C12A C13A 1.363(12) . ? C12A H12A 0.9500 . ? C13A C14A 1.432(10) . ? C13A H13A 0.9500 . ? C14A C15A 1.374(12) . ? C14A N10 1.387(9) . ? C15A C16A 1.420(10) . ? C15A C49A 1.490(10) . ? C16A N2 1.384(9) . ? C16A C17A 1.388(12) . ? C17A C18A 1.365(10) . ? C17A H17A 0.9500 . ? C18A C19A 1.409(11) . ? C18A C68A 1.449(11) . ? C19A N2 1.389(9) . ? C19A C20A 1.407(9) . ? C20A Ir1 1.969(7) . ? C21A C26A 1.376(12) . ? C21A C22A 1.408(10) . ? C22A C23A 1.397(10) . ? C22A H22A 0.9500 . ? C23A C24A 1.358(13) . ? C23A C27A 1.545(11) . ? C24A C25A 1.392(12) . ? C24A H24A 0.9500 . ? C25A C26A 1.402(10) . ? C25A C31A 1.534(13) . ? C26A H26A 0.9500 . ? C27A C30A 1.504(15) . ? C27A C29A 1.536(12) . ? C27A C28A 1.562(12) . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C31A C33A 1.526(16) . ? C31A C32A 1.544(12) . ? C31A C34A 1.579(14) . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? C35A C40A 1.364(12) . ? C35A C36A 1.402(11) . ? C36A C37A 1.401(11) . ? C36A H36A 0.9500 . ? C37A C38A 1.350(13) . ? C37A C41A 1.582(11) . ? C38A C39A 1.430(11) . ? C38A H38A 0.9500 . ? C39A C40A 1.408(10) . ? C39A C45A 1.510(13) . ? C40A H40A 0.9500 . ? C41A C44A 1.533(7) . ? C41A C43A 1.544(8) . ? C41A C42A 1.551(9) . ? C41A C43T 1.563(9) . ? C41A C42T 1.574(9) . ? C41A C44T 1.599(15) . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C43A H43A 0.9800 . ? C43A H43B 0.9800 . ? C43A H43C 0.9800 . ? C44A H44A 0.9800 . ? C44A H44B 0.9800 . ? C44A H44C 0.9800 . ? C45A C48A 1.542(12) . ? C45A C46A 1.545(11) . ? C45A C47A 1.568(13) . ? C46A H46A 0.9800 . ? C46A H46B 0.9800 . ? C46A H46C 0.9800 . ? C47A H47A 0.9800 . ? C47A H47B 0.9800 . ? C47A H47C 0.9800 . ? C48A H48A 0.9800 . ? C48A H48B 0.9800 . ? C48A H48C 0.9800 . ? C49A C50A 1.397(10) . ? C49A C54A 1.425(10) . ? C50A C51A 1.412(11) . ? C50A H50A 0.9500 . ? C51A C52A 1.366(12) . ? C51A C55A 1.546(11) . ? C52A C53A 1.386(11) . ? C52A H52A 0.9500 . ? C53A C54A 1.365(11) . ? C53A C59A 1.548(12) . ? C54A H54A 0.9500 . ? C55A C57A 1.476(14) . ? C55A C56A 1.524(13) . ? C55A C58A 1.549(17) . ? C56A H56A 0.9800 . ? C56A H56B 0.9800 . ? C56A H56C 0.9800 . ? C57A H57A 0.9800 . ? C57A H57B 0.9800 . ? C57A H57C 0.9800 . ? C58A H58A 0.9800 . ? C58A H58B 0.9800 . ? C58A H58C 0.9800 . ? C59A C60A 1.501(16) . ? C59A C62A 1.514(15) . ? C59A C61A 1.569(12) . ? C60A H60A 0.9800 . ? C60A H60B 0.9800 . ? C60A H60C 0.9800 . ? C61A H61A 0.9800 . ? C61A H61B 0.9800 . ? C61A H61C 0.9800 . ? C62A H62A 0.9800 . ? C62A H62B 0.9800 . ? C62A H62C 0.9800 . ? C63A N12 1.360(11) . ? C63A C64A 1.415(11) . ? C64A C65A 1.372(11) . ? C64A H64A 0.9500 . ? C65A C66A 1.366(13) . ? C65A H65A 0.9500 . ? C66A C67A 1.396(12) . ? C66A H66A 0.9500 . ? C67A N12 1.344(10) . ? C67A H67A 0.9500 . ? C68A N11 1.357(9) . ? C68A C69A 1.418(11) . ? C69A C70A 1.375(12) . ? C69A H69A 0.9500 . ? C70A C71A 1.378(11) . ? C70A H70A 0.9500 . ? C71A C72A 1.361(12) . ? C71A H71A 0.9500 . ? C72A N11 1.351(10) . ? C72A H72A 0.9500 . ? C1B C20B 1.376(12) . ? C1B N5 1.383(9) . ? C1B C2B 1.435(10) . ? C2B C3B 1.357(12) . ? C2B C63B 1.471(10) . ? C3B C4B 1.413(10) . ? C3B H3B 0.9500 . ? C4B N5 1.381(10) . ? C4B C5B 1.418(11) . ? C5B C6B 1.365(10) . ? C5B C21B 1.480(10) . ? C6B N6 1.390(10) . ? C6B C7B 1.421(11) . ? C7B C8B 1.347(11) . ? C7B H7B 0.9500 . ? C8B C9B 1.420(11) . ? C8B H8B 0.9500 . ? C9B C10B 1.386(10) . ? C9B N6 1.390(10) . ? C10B C11B 1.379(11) . ? C10B C35B 1.481(10) . ? C11B N7 1.383(10) . ? C11B C12B 1.426(10) . ? C12B C13B 1.373(12) . ? C12B H12B 0.9500 . ? C13B C14B 1.395(11) . ? C13B H13B 0.9500 . ? C14B C15B 1.368(13) . ? C14B N7 1.400(10) . ? C15B C16B 1.427(10) . ? C15B C49B 1.476(11) . ? C16B N4 1.382(9) . ? C16B C17B 1.415(12) . ? C17B C18B 1.369(10) . ? C17B H17B 0.9500 . ? C18B C19B 1.420(11) . ? C18B C68B 1.445(12) . ? C19B N4 1.390(10) . ? C19B C20B 1.399(9) . ? C20B Ir2 1.972(7) . ? C21B C22B 1.391(12) . ? C21B C26B 1.407(10) . ? C22B C23B 1.396(11) . ? C22B H22B 0.9500 . ? C23B C24B 1.429(12) . ? C23B C31B 1.501(13) . ? C24B C25B 1.357(13) . ? C24B H24B 0.9500 . ? C25B C26B 1.380(11) . ? C25B C27B 1.545(11) . ? C26B H26B 0.9500 . ? C27B C30B 1.505(15) . ? C27B C28B 1.511(13) . ? C27B C29B 1.545(12) . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C31B C34B 1.534(13) . ? C31B C33B 1.538(13) . ? C31B C32B 1.543(12) . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34B H34D 0.9800 . ? C34B H34E 0.9800 . ? C34B H34F 0.9800 . ? C35B C40B 1.382(12) . ? C35B C36B 1.402(11) . ? C36B C37B 1.383(12) . ? C36B H36B 0.9500 . ? C37B C38B 1.389(13) . ? C37B C41B 1.543(12) . ? C38B C39B 1.400(11) . ? C38B H38B 0.9500 . ? C39B C40B 1.401(11) . ? C39B C45B 1.534(14) . ? C40B H40B 0.9500 . ? C41B C42B 1.482(14) . ? C41B C44B 1.508(17) . ? C41B C43B 1.515(18) . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C43B H43D 0.9800 . ? C43B H43E 0.9800 . ? C43B H43F 0.9800 . ? C44B H44D 0.9800 . ? C44B H44E 0.9800 . ? C44B H44F 0.9800 . ? C45B C46B 1.513(14) . ? C45B C48B 1.526(15) . ? C45B C47B 1.556(13) . ? C46B H46D 0.9800 . ? C46B H46E 0.9800 . ? C46B H46F 0.9800 . ? C47B H47D 0.9800 . ? C47B H47E 0.9800 . ? C47B H47F 0.9800 . ? C48B H48D 0.9800 . ? C48B H48E 0.9800 . ? C48B H48F 0.9800 . ? C49B C50B 1.375(12) . ? C49B C54B 1.416(10) . ? C50B C51B 1.404(12) . ? C50B H50B 0.9500 . ? C51B C52B 1.409(12) . ? C51B C55B 1.518(13) . ? C52B C53B 1.403(13) . ? C52B H52B 0.9500 . ? C53B C54B 1.382(11) . ? C53B C59B 1.511(12) . ? C54B H54B 0.9500 . ? C55B C58B 1.549(18) . ? C55B C57B 1.581(17) . ? C55B C56B 1.666(17) . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C57B H57D 0.9800 . ? C57B H57E 0.9800 . ? C57B H57F 0.9800 . ? C58B H76 0.9800 . ? C58B H77 0.9800 . ? C58B H78 0.9800 . ? C59B C62B 1.482(15) . ? C59B C61B 1.501(13) . ? C59B C60B 1.526(14) . ? C60B H60D 0.9800 . ? C60B H60E 0.9800 . ? C60B H60F 0.9800 . ? C61B H61D 0.9800 . ? C61B H61E 0.9800 . ? C61B H61F 0.9800 . ? C62B H62D 0.9800 . ? C62B H62E 0.9800 . ? C62B H62F 0.9800 . ? C63B N9 1.350(12) . ? C63B C64B 1.402(11) . ? C64B C65B 1.375(12) . ? C64B H64B 0.9500 . ? C65B C66B 1.393(14) . ? C65B H65B 0.9500 . ? C66B C67B 1.355(13) . ? C66B H66B 0.9500 . ? C67B N9 1.360(10) . ? C67B H67B 0.9500 . ? C68B N8 1.361(9) . ? C68B C69B 1.416(11) . ? C69B C70B 1.387(13) . ? C69B H69B 0.9500 . ? C70B C71B 1.370(11) . ? C70B H70B 0.9500 . ? C71B C72B 1.381(12) . ? C71B H71B 0.9500 . ? C72B N8 1.353(11) . ? C72B H72B 0.9500 . ? C1M O1 1.436(9) . ? C1M H1M1 0.9800 . ? C1M H1M2 0.9800 . ? C1M H1M3 0.9800 . ? C2M O2 1.407(10) . ? C2M H73 0.9800 . ? C2M H74 0.9800 . ? C2M H75 0.9800 . ? Cl1 Ir1 2.3333(17) . ? Cl2 Ir1 2.3490(17) . ? Cl3 Ir2 2.3380(19) . ? Cl4 Ir2 2.3370(19) . ? Ir1 N11 2.045(7) . ? Ir1 N12 2.049(6) . ? Ir1 O1 2.250(5) . ? Ir2 N9 2.040(7) . ? Ir2 N8 2.049(7) . ? Ir2 O2 2.243(6) . ? N1 Ni1 1.918(5) . ? N2 Ni1 1.924(7) . ? N3 Ni1 1.933(7) . ? N4 Ni2 1.917(7) . ? N5 Ni2 1.930(5) . ? N6 Ni2 1.918(7) . ? N7 Ni2 1.935(5) . ? N10 Ni1 1.931(5) . ? O1 H1 0.9500 . ? O2 H2 0.9500 . ? C42T H42G 0.9800 . ? C42T H42H 0.9800 . ? C42T H42I 0.9800 . ? C44T H44G 0.9800 . ? C44T H44H 0.9800 . ? C44T H44I 0.9800 . ? C43T H43G 0.9800 . ? C43T H43H 0.9800 . ? C43T H43I 0.9800 . ? Cl5 C74 1.702(17) . ? O4 C73 1.393(13) . ? O4 H4 0.8400 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? O5 C75 1.32(2) . ? O5 H5 0.8400 . ? C74 C74 1.49(3) 2_566 ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? O7 C77 1.431(10) . ? O7 H79 0.8400 . ? C77 C77 1.71(7) 2_565 ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 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 C20A C1A N1 124.2(6) . . ? C20A C1A C2A 126.6(6) . . ? N1 C1A C2A 108.2(6) . . ? C3A C2A C1A 107.9(6) . . ? C3A C2A C63A 128.5(7) . . ? C1A C2A C63A 123.4(7) . . ? C2A C3A C4A 108.8(6) . . ? C2A C3A H3A 125.6 . . ? C4A C3A H3A 125.6 . . ? C5A C4A N1 125.1(6) . . ? C5A C4A C3A 126.2(6) . . ? N1 C4A C3A 108.6(7) . . ? C4A C5A C6A 120.6(6) . . ? C4A C5A C21A 117.9(6) . . ? C6A C5A C21A 121.3(7) . . ? C5A C6A N3 124.0(7) . . ? C5A C6A C7A 126.0(6) . . ? N3 C6A C7A 109.8(6) . . ? C8A C7A C6A 108.9(6) . . ? C8A C7A H7A 125.5 . . ? C6A C7A H7A 125.5 . . ? C7A C8A C9A 106.4(7) . . ? C7A C8A H8A 126.8 . . ? C9A C8A H8A 126.8 . . ? C10A C9A N3 124.1(7) . . ? C10A C9A C8A 125.3(6) . . ? N3 C9A C8A 110.5(6) . . ? C11A C10A C9A 123.2(6) . . ? C11A C10A C35A 117.8(6) . . ? C9A C10A C35A 119.0(7) . . ? C10A C11A N10 125.4(6) . . ? C10A C11A C12A 124.4(6) . . ? N10 C11A C12A 110.2(6) . . ? C13A C12A C11A 106.6(7) . . ? C13A C12A H12A 126.7 . . ? C11A C12A H12A 126.7 . . ? C12A C13A C14A 107.2(6) . . ? C12A C13A H13A 126.4 . . ? C14A C13A H13A 126.4 . . ? C15A C14A N10 125.2(6) . . ? C15A C14A C13A 124.3(7) . . ? N10 C14A C13A 110.0(7) . . ? C14A C15A C16A 121.2(7) . . ? C14A C15A C49A 122.2(6) . . ? C16A C15A C49A 116.6(7) . . ? N2 C16A C17A 111.7(6) . . ? N2 C16A C15A 122.9(8) . . ? C17A C16A C15A 125.3(7) . . ? C18A C17A C16A 107.3(7) . . ? C18A C17A H17A 126.4 . . ? C16A C17A H17A 126.4 . . ? C17A C18A C19A 106.3(7) . . ? C17A C18A C68A 127.2(8) . . ? C19A C18A C68A 125.8(6) . . ? N2 C19A C20A 122.4(7) . . ? N2 C19A C18A 111.0(6) . . ? C20A C19A C18A 125.5(7) . . ? C1A C20A C19A 120.1(6) . . ? C1A C20A Ir1 120.7(5) . . ? C19A C20A Ir1 119.2(6) . . ? C26A C21A C22A 118.6(6) . . ? C26A C21A C5A 124.0(7) . . ? C22A C21A C5A 117.4(7) . . ? C23A C22A C21A 120.8(8) . . ? C23A C22A H22A 119.6 . . ? C21A C22A H22A 119.6 . . ? C24A C23A C22A 118.3(7) . . ? C24A C23A C27A 120.6(7) . . ? C22A C23A C27A 121.0(8) . . ? C23A C24A C25A 123.3(7) . . ? C23A C24A H24A 118.4 . . ? C25A C24A H24A 118.4 . . ? C24A C25A C26A 117.3(8) . . ? C24A C25A C31A 122.8(7) . . ? C26A C25A C31A 119.8(7) . . ? C21A C26A C25A 121.6(7) . . ? C21A C26A H26A 119.2 . . ? C25A C26A H26A 119.2 . . ? C30A C27A C29A 108.4(9) . . ? C30A C27A C23A 113.6(7) . . ? C29A C27A C23A 108.0(7) . . ? C30A C27A C28A 110.6(9) . . ? C29A C27A C28A 108.2(6) . . ? C23A C27A C28A 107.8(7) . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C27A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C27A C30A H30A 109.5 . . ? C27A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C27A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C33A C31A C25A 110.1(8) . . ? C33A C31A C32A 112.6(10) . . ? C25A C31A C32A 112.4(8) . . ? C33A C31A C34A 107.5(9) . . ? C25A C31A C34A 109.2(8) . . ? C32A C31A C34A 104.9(9) . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C31A C33A H33A 109.5 . . ? C31A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C31A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C31A C34A H34A 109.5 . . ? C31A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C31A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C40A C35A C36A 120.6(7) . . ? C40A C35A C10A 122.7(6) . . ? C36A C35A C10A 116.5(8) . . ? C37A C36A C35A 119.0(8) . . ? C37A C36A H36A 120.5 . . ? C35A C36A H36A 120.5 . . ? C38A C37A C36A 119.7(7) . . ? C38A C37A C41A 120.1(7) . . ? C36A C37A C41A 120.1(8) . . ? C37A C38A C39A 123.1(7) . . ? C37A C38A H38A 118.4 . . ? C39A C38A H38A 118.4 . . ? C40A C39A C38A 115.4(8) . . ? C40A C39A C45A 121.4(7) . . ? C38A C39A C45A 123.2(6) . . ? C35A C40A C39A 122.1(7) . . ? C35A C40A H40A 118.9 . . ? C39A C40A H40A 118.9 . . ? C44A C41A C43A 114.9(8) . . ? C44A C41A C42A 114.0(8) . . ? C43A C41A C42A 113.6(8) . . ? C44A C41A C43T 76.2(10) . . ? C43A C41A C43T 41.1(9) . . ? C42A C41A C43T 148.0(10) . . ? C44A C41A C42T 148.2(13) . . ? C43A C41A C42T 69.4(10) . . ? C42A C41A C42T 45.6(10) . . ? C43T C41A C42T 109.6(8) . . ? C44A C41A C37A 102.4(11) . . ? C43A C41A C37A 108.7(10) . . ? C42A C41A C37A 101.5(9) . . ? C43T C41A C37A 105.8(8) . . ? C42T C41A C37A 105.6(9) . . ? C44A C41A C44T 43.1(10) . . ? C43A C41A C44T 134.3(11) . . ? C42A C41A C44T 71.1(11) . . ? C43T C41A C44T 111.0(8) . . ? C42T C41A C44T 109.8(8) . . ? C37A C41A C44T 114.8(8) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? C41A C43A H43A 109.5 . . ? C41A C43A H43B 109.5 . . ? C41A C43A H43C 109.5 . . ? C41A C44A H44A 109.5 . . ? C41A C44A H44B 109.5 . . ? C41A C44A H44C 109.5 . . ? C39A C45A C48A 110.2(8) . . ? C39A C45A C46A 112.2(7) . . ? C48A C45A C46A 107.9(7) . . ? C39A C45A C47A 109.4(7) . . ? C48A C45A C47A 110.4(8) . . ? C46A C45A C47A 106.6(8) . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C45A C47A H47A 109.5 . . ? C45A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C45A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C45A C48A H48A 109.5 . . ? C45A C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C45A C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C50A C49A C54A 119.1(7) . . ? C50A C49A C15A 121.9(7) . . ? C54A C49A C15A 119.0(6) . . ? C49A C50A C51A 119.4(7) . . ? C49A C50A H50A 120.3 . . ? C51A C50A H50A 120.3 . . ? C52A C51A C50A 119.0(7) . . ? C52A C51A C55A 120.7(7) . . ? C50A C51A C55A 120.3(8) . . ? C51A C52A C53A 122.9(8) . . ? C51A C52A H52A 118.5 . . ? C53A C52A H52A 118.5 . . ? C54A C53A C52A 118.6(8) . . ? C54A C53A C59A 119.8(7) . . ? C52A C53A C59A 121.4(7) . . ? C53A C54A C49A 120.9(7) . . ? C53A C54A H54A 119.5 . . ? C49A C54A H54A 119.5 . . ? C57A C55A C56A 110.6(10) . . ? C57A C55A C51A 109.6(8) . . ? C56A C55A C51A 113.2(7) . . ? C57A C55A C58A 110.2(10) . . ? C56A C55A C58A 105.5(9) . . ? C51A C55A C58A 107.5(9) . . ? C55A C56A H56A 109.5 . . ? C55A C56A H56B 109.5 . . ? H56A C56A H56B 109.5 . . ? C55A C56A H56C 109.5 . . ? H56A C56A H56C 109.5 . . ? H56B C56A H56C 109.5 . . ? C55A C57A H57A 109.5 . . ? C55A C57A H57B 109.5 . . ? H57A C57A H57B 109.5 . . ? C55A C57A H57C 109.5 . . ? H57A C57A H57C 109.5 . . ? H57B C57A H57C 109.5 . . ? C55A C58A H58A 109.5 . . ? C55A C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? C55A C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? C60A C59A C62A 108.7(10) . . ? C60A C59A C53A 109.7(8) . . ? C62A C59A C53A 111.3(8) . . ? C60A C59A C61A 108.2(8) . . ? C62A C59A C61A 108.3(9) . . ? C53A C59A C61A 110.7(7) . . ? C59A C60A H60A 109.5 . . ? C59A C60A H60B 109.5 . . ? H60A C60A H60B 109.5 . . ? C59A C60A H60C 109.5 . . ? H60A C60A H60C 109.5 . . ? H60B C60A H60C 109.5 . . ? C59A C61A H61A 109.5 . . ? C59A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C59A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? C59A C62A H62A 109.5 . . ? C59A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C59A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? N12 C63A C64A 120.2(6) . . ? N12 C63A C2A 120.9(7) . . ? C64A C63A C2A 118.6(8) . . ? C65A C64A C63A 119.9(8) . . ? C65A C64A H64A 120.0 . . ? C63A C64A H64A 120.0 . . ? C66A C65A C64A 119.6(8) . . ? C66A C65A H65A 120.2 . . ? C64A C65A H65A 120.2 . . ? C65A C66A C67A 118.6(7) . . ? C65A C66A H66A 120.7 . . ? C67A C66A H66A 120.7 . . ? N12 C67A C66A 123.0(8) . . ? N12 C67A H67A 118.5 . . ? C66A C67A H67A 118.5 . . ? N11 C68A C69A 119.2(7) . . ? N11 C68A C18A 119.6(7) . . ? C69A C68A C18A 121.0(6) . . ? C70A C69A C68A 120.8(7) . . ? C70A C69A H69A 119.6 . . ? C68A C69A H69A 119.6 . . ? C69A C70A C71A 118.4(8) . . ? C69A C70A H70A 120.8 . . ? C71A C70A H70A 120.8 . . ? C72A C71A C70A 118.9(8) . . ? C72A C71A H71A 120.6 . . ? C70A C71A H71A 120.6 . . ? N11 C72A C71A 124.1(7) . . ? N11 C72A H72A 117.9 . . ? C71A C72A H72A 117.9 . . ? C20B C1B N5 124.8(6) . . ? C20B C1B C2B 124.9(7) . . ? N5 C1B C2B 109.7(7) . . ? C3B C2B C1B 106.8(6) . . ? C3B C2B C63B 127.1(7) . . ? C1B C2B C63B 124.6(7) . . ? C2B C3B C4B 107.5(6) . . ? C2B C3B H3B 126.3 . . ? C4B C3B H3B 126.3 . . ? N5 C4B C3B 110.4(7) . . ? N5 C4B C5B 124.5(6) . . ? C3B C4B C5B 125.0(6) . . ? C6B C5B C4B 121.2(7) . . ? C6B C5B C21B 120.6(8) . . ? C4B C5B C21B 118.2(6) . . ? C5B C6B N6 124.9(8) . . ? C5B C6B C7B 125.1(7) . . ? N6 C6B C7B 110.0(6) . . ? C8B C7B C6B 108.1(7) . . ? C8B C7B H7B 126.0 . . ? C6B C7B H7B 126.0 . . ? C7B C8B C9B 106.6(7) . . ? C7B C8B H8B 126.7 . . ? C9B C8B H8B 126.7 . . ? C10B C9B N6 125.4(7) . . ? C10B C9B C8B 123.6(7) . . ? N6 C9B C8B 110.9(6) . . ? C11B C10B C9B 121.3(7) . . ? C11B C10B C35B 117.8(6) . . ? C9B C10B C35B 120.8(7) . . ? C10B C11B N7 125.4(6) . . ? C10B C11B C12B 124.1(7) . . ? N7 C11B C12B 110.2(7) . . ? C13B C12B C11B 106.7(7) . . ? C13B C12B H12B 126.7 . . ? C11B C12B H12B 126.7 . . ? C12B C13B C14B 107.7(7) . . ? C12B C13B H13B 126.2 . . ? C14B C13B H13B 126.2 . . ? C15B C14B C13B 124.6(7) . . ? C15B C14B N7 123.7(7) . . ? C13B C14B N7 110.6(8) . . ? C14B C15B C16B 122.1(7) . . ? C14B C15B C49B 122.5(7) . . ? C16B C15B C49B 115.4(8) . . ? N4 C16B C17B 112.3(6) . . ? N4 C16B C15B 123.2(8) . . ? C17B C16B C15B 124.5(7) . . ? C18B C17B C16B 105.8(7) . . ? C18B C17B H17B 127.1 . . ? C16B C17B H17B 127.1 . . ? C17B C18B C19B 107.1(7) . . ? C17B C18B C68B 125.8(7) . . ? C19B C18B C68B 126.6(6) . . ? N4 C19B C20B 123.3(7) . . ? N4 C19B C18B 110.9(6) . . ? C20B C19B C18B 125.4(7) . . ? C1B C20B C19B 119.6(7) . . ? C1B C20B Ir2 121.7(5) . . ? C19B C20B Ir2 118.6(6) . . ? C22B C21B C26B 118.8(7) . . ? C22B C21B C5B 121.2(7) . . ? C26B C21B C5B 120.0(8) . . ? C21B C22B C23B 122.9(7) . . ? C21B C22B H22B 118.6 . . ? C23B C22B H22B 118.6 . . ? C22B C23B C24B 114.8(8) . . ? C22B C23B C31B 123.4(8) . . ? C24B C23B C31B 121.7(7) . . ? C25B C24B C23B 124.0(7) . . ? C25B C24B H24B 118.0 . . ? C23B C24B H24B 118.0 . . ? C24B C25B C26B 119.0(7) . . ? C24B C25B C27B 120.2(7) . . ? C26B C25B C27B 120.8(9) . . ? C25B C26B C21B 120.5(8) . . ? C25B C26B H26B 119.7 . . ? C21B C26B H26B 119.7 . . ? C30B C27B C28B 106.8(9) . . ? C30B C27B C25B 113.0(7) . . ? C28B C27B C25B 111.8(8) . . ? C30B C27B C29B 107.3(9) . . ? C28B C27B C29B 110.4(8) . . ? C25B C27B C29B 107.5(8) . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C27B C30B H30D 109.5 . . ? C27B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C27B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C23B C31B C34B 109.0(8) . . ? C23B C31B C33B 113.0(8) . . ? C34B C31B C33B 108.1(8) . . ? C23B C31B C32B 112.3(8) . . ? C34B C31B C32B 108.7(8) . . ? C33B C31B C32B 105.5(9) . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C31B C33B H33D 109.5 . . ? C31B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C31B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C31B C34B H34D 109.5 . . ? C31B C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C31B C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? C40B C35B C36B 119.5(7) . . ? C40B C35B C10B 122.3(7) . . ? C36B C35B C10B 118.2(8) . . ? C37B C36B C35B 121.4(9) . . ? C37B C36B H36B 119.3 . . ? C35B C36B H36B 119.3 . . ? C36B C37B C38B 116.9(7) . . ? C36B C37B C41B 122.3(9) . . ? C38B C37B C41B 120.7(8) . . ? C37B C38B C39B 124.4(7) . . ? C37B C38B H38B 117.8 . . ? C39B C38B H38B 117.8 . . ? C38B C39B C40B 116.2(8) . . ? C38B C39B C45B 122.7(7) . . ? C40B C39B C45B 121.0(7) . . ? C35B C40B C39B 121.5(7) . . ? C35B C40B H40B 119.2 . . ? C39B C40B H40B 119.2 . . ? C42B C41B C44B 111.1(10) . . ? C42B C41B C43B 112.8(13) . . ? C44B C41B C43B 104.3(12) . . ? C42B C41B C37B 107.9(7) . . ? C44B C41B C37B 110.5(9) . . ? C43B C41B C37B 110.2(9) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C46B C45B C48B 105.7(10) . . ? C46B C45B C39B 113.5(8) . . ? C48B C45B C39B 110.5(7) . . ? C46B C45B C47B 109.4(8) . . ? C48B C45B C47B 108.4(10) . . ? C39B C45B C47B 109.2(9) . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.5 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.5 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C45B C47B H47D 109.5 . . ? C45B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C45B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C45B C48B H48D 109.5 . . ? C45B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C45B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C50B C49B C54B 117.8(7) . . ? C50B C49B C15B 124.0(7) . . ? C54B C49B C15B 118.1(7) . . ? C49B C50B C51B 123.4(8) . . ? C49B C50B H50B 118.3 . . ? C51B C50B H50B 118.3 . . ? C50B C51B C52B 115.9(8) . . ? C50B C51B C55B 120.8(8) . . ? C52B C51B C55B 123.3(8) . . ? C53B C52B C51B 123.3(8) . . ? C53B C52B H52B 118.4 . . ? C51B C52B H52B 118.4 . . ? C54B C53B C52B 117.2(7) . . ? C54B C53B C59B 121.6(8) . . ? C52B C53B C59B 121.3(8) . . ? C53B C54B C49B 122.3(7) . . ? C53B C54B H54B 118.9 . . ? C49B C54B H54B 118.9 . . ? C51B C55B C58B 109.4(12) . . ? C51B C55B C57B 113.8(9) . . ? C58B C55B C57B 111.9(8) . . ? C51B C55B C56B 108.5(9) . . ? C58B C55B C56B 107.9(9) . . ? C57B C55B C56B 105.0(12) . . ? C55B C56B H56D 109.5 . . ? C55B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C55B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C55B C57B H57D 109.5 . . ? C55B C57B H57E 109.5 . . ? H57D C57B H57E 109.5 . . ? C55B C57B H57F 109.5 . . ? H57D C57B H57F 109.5 . . ? H57E C57B H57F 109.5 . . ? C55B C58B H76 109.5 . . ? C55B C58B H77 109.5 . . ? H76 C58B H77 109.5 . . ? C55B C58B H78 109.5 . . ? H76 C58B H78 109.5 . . ? H77 C58B H78 109.5 . . ? C62B C59B C61B 110.0(10) . . ? C62B C59B C53B 107.2(8) . . ? C61B C59B C53B 110.6(8) . . ? C62B C59B C60B 107.7(8) . . ? C61B C59B C60B 108.7(10) . . ? C53B C59B C60B 112.6(7) . . ? C59B C60B H60D 109.5 . . ? C59B C60B H60E 109.5 . . ? H60D C60B H60E 109.5 . . ? C59B C60B H60F 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? C59B C61B H61D 109.5 . . ? C59B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C59B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? C59B C62B H62D 109.5 . . ? C59B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C59B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? N9 C63B C64B 121.3(7) . . ? N9 C63B C2B 119.4(7) . . ? C64B C63B C2B 119.1(8) . . ? C65B C64B C63B 119.7(9) . . ? C65B C64B H64B 120.2 . . ? C63B C64B H64B 120.2 . . ? C64B C65B C66B 118.2(8) . . ? C64B C65B H65B 120.9 . . ? C66B C65B H65B 120.9 . . ? C67B C66B C65B 119.6(8) . . ? C67B C66B H66B 120.2 . . ? C65B C66B H66B 120.2 . . ? C66B C67B N9 123.0(9) . . ? C66B C67B H67B 118.5 . . ? N9 C67B H67B 118.5 . . ? N8 C68B C69B 119.2(7) . . ? N8 C68B C18B 119.7(7) . . ? C69B C68B C18B 120.9(6) . . ? C70B C69B C68B 120.9(7) . . ? C70B C69B H69B 119.5 . . ? C68B C69B H69B 119.5 . . ? C71B C70B C69B 118.2(8) . . ? C71B C70B H70B 120.9 . . ? C69B C70B H70B 120.9 . . ? C70B C71B C72B 119.7(8) . . ? C70B C71B H71B 120.2 . . ? C72B C71B H71B 120.2 . . ? N8 C72B C71B 122.9(7) . . ? N8 C72B H72B 118.6 . . ? C71B C72B H72B 118.6 . . ? O1 C1M H1M1 109.5 . . ? O1 C1M H1M2 109.5 . . ? H1M1 C1M H1M2 109.5 . . ? O1 C1M H1M3 109.5 . . ? H1M1 C1M H1M3 109.5 . . ? H1M2 C1M H1M3 109.5 . . ? O2 C2M H73 109.5 . . ? O2 C2M H74 109.5 . . ? H73 C2M H74 109.5 . . ? O2 C2M H75 109.5 . . ? H73 C2M H75 109.5 . . ? H74 C2M H75 109.5 . . ? C20A Ir1 N11 92.2(3) . . ? C20A Ir1 N12 92.4(3) . . ? N11 Ir1 N12 175.3(2) . . ? C20A Ir1 O1 176.9(2) . . ? N11 Ir1 O1 88.0(2) . . ? N12 Ir1 O1 87.4(2) . . ? C20A Ir1 Cl1 92.23(18) . . ? N11 Ir1 Cl1 90.50(17) . . ? N12 Ir1 Cl1 88.58(16) . . ? O1 Ir1 Cl1 90.87(14) . . ? C20A Ir1 Cl2 91.91(18) . . ? N11 Ir1 Cl2 90.32(17) . . ? N12 Ir1 Cl2 90.27(16) . . ? O1 Ir1 Cl2 84.99(14) . . ? Cl1 Ir1 Cl2 175.75(6) . . ? C20B Ir2 N9 91.3(3) . . ? C20B Ir2 N8 92.8(3) . . ? N9 Ir2 N8 176.0(3) . . ? C20B Ir2 O2 177.4(3) . . ? N9 Ir2 O2 87.4(2) . . ? N8 Ir2 O2 88.5(2) . . ? C20B Ir2 Cl4 92.7(2) . . ? N9 Ir2 Cl4 90.42(18) . . ? N8 Ir2 Cl4 89.33(17) . . ? O2 Ir2 Cl4 85.08(16) . . ? C20B Ir2 Cl3 91.5(2) . . ? N9 Ir2 Cl3 89.92(18) . . ? N8 Ir2 Cl3 90.03(18) . . ? O2 Ir2 Cl3 90.67(16) . . ? Cl4 Ir2 Cl3 175.71(7) . . ? C4A N1 C1A 105.7(5) . . ? C4A N1 Ni1 127.3(5) . . ? C1A N1 Ni1 125.6(5) . . ? C16A N2 C19A 103.2(7) . . ? C16A N2 Ni1 128.0(5) . . ? C19A N2 Ni1 127.0(5) . . ? C9A N3 C6A 104.2(6) . . ? C9A N3 Ni1 126.6(5) . . ? C6A N3 Ni1 128.0(5) . . ? C16B N4 C19B 103.2(7) . . ? C16B N4 Ni2 127.6(5) . . ? C19B N4 Ni2 127.1(5) . . ? C4B N5 C1B 105.2(5) . . ? C4B N5 Ni2 126.2(5) . . ? C1B N5 Ni2 126.2(5) . . ? C9B N6 C6B 104.1(7) . . ? C9B N6 Ni2 127.1(5) . . ? C6B N6 Ni2 128.2(5) . . ? C11B N7 C14B 104.9(6) . . ? C11B N7 Ni2 127.1(5) . . ? C14B N7 Ni2 127.4(5) . . ? C72B N8 C68B 118.8(7) . . ? C72B N8 Ir2 119.0(5) . . ? C68B N8 Ir2 121.8(6) . . ? C63B N9 C67B 117.5(7) . . ? C63B N9 Ir2 124.0(5) . . ? C67B N9 Ir2 118.4(6) . . ? C11A N10 C14A 105.7(5) . . ? C11A N10 Ni1 126.9(5) . . ? C14A N10 Ni1 126.9(5) . . ? C72A N11 C68A 118.1(7) . . ? C72A N11 Ir1 119.2(5) . . ? C68A N11 Ir1 122.1(5) . . ? C67A N12 C63A 118.4(7) . . ? C67A N12 Ir1 118.4(6) . . ? C63A N12 Ir1 122.5(5) . . ? N1 Ni1 N2 90.0(2) . . ? N1 Ni1 N10 172.6(3) . . ? N2 Ni1 N10 90.2(2) . . ? N1 Ni1 N3 90.0(2) . . ? N2 Ni1 N3 171.8(3) . . ? N10 Ni1 N3 90.9(2) . . ? N4 Ni2 N6 172.6(3) . . ? N4 Ni2 N5 89.2(3) . . ? N6 Ni2 N5 90.5(3) . . ? N4 Ni2 N7 90.4(3) . . ? N6 Ni2 N7 90.6(3) . . ? N5 Ni2 N7 174.1(3) . . ? C1M O1 Ir1 126.4(5) . . ? C1M O1 H1 116.8 . . ? Ir1 O1 H1 116.8 . . ? C2M O2 Ir2 126.8(5) . . ? C2M O2 H2 116.6 . . ? Ir2 O2 H2 116.6 . . ? C41A C42T H42G 109.5 . . ? C41A C42T H42H 109.5 . . ? H42G C42T H42H 109.5 . . ? C41A C42T H42I 109.5 . . ? H42G C42T H42I 109.5 . . ? H42H C42T H42I 109.5 . . ? C41A C44T H44G 109.5 . . ? C41A C44T H44H 109.5 . . ? H44G C44T H44H 109.5 . . ? C41A C44T H44I 109.5 . . ? H44G C44T H44I 109.5 . . ? H44H C44T H44I 109.5 . . ? C41A C43T H43G 109.5 . . ? C41A C43T H43H 109.5 . . ? H43G C43T H43H 109.5 . . ? C41A C43T H43I 109.5 . . ? H43G C43T H43I 109.5 . . ? H43H C43T H43I 109.5 . . ? C73 O4 H4 108.7 . . ? O4 C73 H73A 109.1 . . ? O4 C73 H73B 109.1 . . ? H73A C73 H73B 109.5 . . ? O4 C73 H73C 110.3 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C75 O5 H5 114.5 . . ? C74 C74 Cl5 116(2) 2_566 . ? C74 C74 H74A 108.3 2_566 . ? Cl5 C74 H74A 108.3 . . ? C74 C74 H74B 108.3 2_566 . ? Cl5 C74 H74B 108.3 . . ? H74A C74 H74B 107.4 . . ? O5 C75 H75A 104.7 . . ? O5 C75 H75B 110.0 . . ? H75A C75 H75B 109.5 . . ? O5 C75 H75C 113.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C77 O7 H79 109.5 . . ? O7 C77 C77 125(3) . 2_565 ? O7 C77 H77A 139.9 . . ? C77 C77 H77A 31.7 2_565 . ? O7 C77 H77B 100.0 . . ? C77 C77 H77B 135.2 2_565 . ? H77A C77 H77B 109.5 . . ? O7 C77 H77C 84.4 . . ? C77 C77 H77C 81.5 2_565 . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20A C1A C2A C3A -161.4(7) . . . . ? N1 C1A C2A C3A 7.5(8) . . . . ? C20A C1A C2A C63A 24.4(12) . . . . ? N1 C1A C2A C63A -166.6(7) . . . . ? C1A C2A C3A C4A -2.7(9) . . . . ? C63A C2A C3A C4A 171.1(7) . . . . ? C2A C3A C4A C5A 172.9(7) . . . . ? C2A C3A C4A N1 -3.1(9) . . . . ? N1 C4A C5A C6A -17.2(11) . . . . ? C3A C4A C5A C6A 167.4(7) . . . . ? N1 C4A C5A C21A 158.1(7) . . . . ? C3A C4A C5A C21A -17.3(11) . . . . ? C4A C5A C6A N3 -5.0(12) . . . . ? C21A C5A C6A N3 179.8(7) . . . . ? C4A C5A C6A C7A 179.3(8) . . . . ? C21A C5A C6A C7A 4.2(12) . . . . ? C5A C6A C7A C8A 172.3(8) . . . . ? N3 C6A C7A C8A -3.9(9) . . . . ? C6A C7A C8A C9A 2.1(9) . . . . ? C7A C8A C9A C10A -175.9(8) . . . . ? C7A C8A C9A N3 0.2(9) . . . . ? N3 C9A C10A C11A 6.7(13) . . . . ? C8A C9A C10A C11A -177.6(8) . . . . ? N3 C9A C10A C35A -174.0(7) . . . . ? C8A C9A C10A C35A 1.6(12) . . . . ? C9A C10A C11A N10 10.7(12) . . . . ? C35A C10A C11A N10 -168.5(7) . . . . ? C9A C10A C11A C12A -172.1(8) . . . . ? C35A C10A C11A C12A 8.6(11) . . . . ? C10A C11A C12A C13A -174.6(8) . . . . ? N10 C11A C12A C13A 2.9(9) . . . . ? C11A C12A C13A C14A 1.0(9) . . . . ? C12A C13A C14A C15A 167.5(8) . . . . ? C12A C13A C14A N10 -4.7(9) . . . . ? N10 C14A C15A C16A -6.4(12) . . . . ? C13A C14A C15A C16A -177.4(7) . . . . ? N10 C14A C15A C49A 174.5(7) . . . . ? C13A C14A C15A C49A 3.5(12) . . . . ? C14A C15A C16A N2 -17.0(11) . . . . ? C49A C15A C16A N2 162.1(6) . . . . ? C14A C15A C16A C17A 166.7(7) . . . . ? C49A C15A C16A C17A -14.1(11) . . . . ? N2 C16A C17A C18A -3.1(8) . . . . ? C15A C16A C17A C18A 173.5(6) . . . . ? C16A C17A C18A C19A -1.7(8) . . . . ? C16A C17A C18A C68A 168.5(7) . . . . ? C17A C18A C19A N2 6.0(8) . . . . ? C68A C18A C19A N2 -164.5(6) . . . . ? C17A C18A C19A C20A -162.8(7) . . . . ? C68A C18A C19A C20A 26.8(11) . . . . ? N1 C1A C20A C19A 17.6(10) . . . . ? C2A C1A C20A C19A -175.2(6) . . . . ? N1 C1A C20A Ir1 -164.1(5) . . . . ? C2A C1A C20A Ir1 3.2(10) . . . . ? N2 C19A C20A C1A 15.5(10) . . . . ? C18A C19A C20A C1A -177.0(7) . . . . ? N2 C19A C20A Ir1 -162.9(5) . . . . ? C18A C19A C20A Ir1 4.7(10) . . . . ? C4A C5A C21A C26A 125.6(8) . . . . ? C6A C5A C21A C26A -59.1(10) . . . . ? C4A C5A C21A C22A -53.8(9) . . . . ? C6A C5A C21A C22A 121.5(8) . . . . ? C26A C21A C22A C23A -1.1(10) . . . . ? C5A C21A C22A C23A 178.3(6) . . . . ? C21A C22A C23A C24A 1.3(11) . . . . ? C21A C22A C23A C27A 179.3(6) . . . . ? C22A C23A C24A C25A -0.8(12) . . . . ? C27A C23A C24A C25A -178.8(7) . . . . ? C23A C24A C25A C26A 0.1(12) . . . . ? C23A C24A C25A C31A 178.1(8) . . . . ? C22A C21A C26A C25A 0.3(10) . . . . ? C5A C21A C26A C25A -179.0(7) . . . . ? C24A C25A C26A C21A 0.2(11) . . . . ? C31A C25A C26A C21A -178.0(7) . . . . ? C24A C23A C27A C30A 176.8(9) . . . . ? C22A C23A C27A C30A -1.2(11) . . . . ? C24A C23A C27A C29A 56.5(10) . . . . ? C22A C23A C27A C29A -121.5(8) . . . . ? C24A C23A C27A C28A -60.3(10) . . . . ? C22A C23A C27A C28A 121.8(8) . . . . ? C24A C25A C31A C33A 121.8(9) . . . . ? C26A C25A C31A C33A -60.1(10) . . . . ? C24A C25A C31A C32A -4.5(13) . . . . ? C26A C25A C31A C32A 173.5(9) . . . . ? C24A C25A C31A C34A -120.4(9) . . . . ? C26A C25A C31A C34A 57.6(11) . . . . ? C11A C10A C35A C40A -106.5(9) . . . . ? C9A C10A C35A C40A 74.2(10) . . . . ? C11A C10A C35A C36A 68.6(9) . . . . ? C9A C10A C35A C36A -110.7(8) . . . . ? C40A C35A C36A C37A 0.2(11) . . . . ? C10A C35A C36A C37A -174.9(7) . . . . ? C35A C36A C37A C38A -0.3(11) . . . . ? C35A C36A C37A C41A -177.0(7) . . . . ? C36A C37A C38A C39A -0.1(12) . . . . ? C41A C37A C38A C39A 176.6(6) . . . . ? C37A C38A C39A C40A 0.5(10) . . . . ? C37A C38A C39A C45A 179.4(7) . . . . ? C36A C35A C40A C39A 0.3(11) . . . . ? C10A C35A C40A C39A 175.2(6) . . . . ? C38A C39A C40A C35A -0.7(10) . . . . ? C45A C39A C40A C35A -179.5(7) . . . . ? C38A C37A C41A C44A 133.5(11) . . . . ? C36A C37A C41A C44A -49.9(12) . . . . ? C38A C37A C41A C43A 11.5(12) . . . . ? C36A C37A C41A C43A -171.8(11) . . . . ? C38A C37A C41A C42A -108.4(11) . . . . ? C36A C37A C41A C42A 68.2(12) . . . . ? C38A C37A C41A C43T 54.6(11) . . . . ? C36A C37A C41A C43T -128.8(10) . . . . ? C38A C37A C41A C42T -61.6(11) . . . . ? C36A C37A C41A C42T 115.0(11) . . . . ? C38A C37A C41A C44T 177.3(10) . . . . ? C36A C37A C41A C44T -6.1(12) . . . . ? C40A C39A C45A C48A 53.0(10) . . . . ? C38A C39A C45A C48A -125.8(8) . . . . ? C40A C39A C45A C46A 173.3(7) . . . . ? C38A C39A C45A C46A -5.5(11) . . . . ? C40A C39A C45A C47A -68.6(9) . . . . ? C38A C39A C45A C47A 112.6(8) . . . . ? C14A C15A C49A C50A -56.9(11) . . . . ? C16A C15A C49A C50A 124.0(8) . . . . ? C14A C15A C49A C54A 124.6(8) . . . . ? C16A C15A C49A C54A -54.6(10) . . . . ? C54A C49A C50A C51A -0.5(13) . . . . ? C15A C49A C50A C51A -179.0(8) . . . . ? C49A C50A C51A C52A 0.0(14) . . . . ? C49A C50A C51A C55A -178.9(9) . . . . ? C50A C51A C52A C53A 0.2(15) . . . . ? C55A C51A C52A C53A 179.1(9) . . . . ? C51A C52A C53A C54A 0.1(14) . . . . ? C51A C52A C53A C59A 175.9(9) . . . . ? C52A C53A C54A C49A -0.5(13) . . . . ? C59A C53A C54A C49A -176.5(8) . . . . ? C50A C49A C54A C53A 0.8(13) . . . . ? C15A C49A C54A C53A 179.4(8) . . . . ? C52A C51A C55A C57A -63.7(14) . . . . ? C50A C51A C55A C57A 115.2(12) . . . . ? C52A C51A C55A C56A 172.3(9) . . . . ? C50A C51A C55A C56A -8.8(14) . . . . ? C52A C51A C55A C58A 56.1(12) . . . . ? C50A C51A C55A C58A -125.0(10) . . . . ? C54A C53A C59A C60A 96.5(10) . . . . ? C52A C53A C59A C60A -79.3(11) . . . . ? C54A C53A C59A C62A -23.7(14) . . . . ? C52A C53A C59A C62A 160.5(11) . . . . ? C54A C53A C59A C61A -144.2(9) . . . . ? C52A C53A C59A C61A 40.0(13) . . . . ? C3A C2A C63A N12 173.7(7) . . . . ? C1A C2A C63A N12 -13.3(11) . . . . ? C3A C2A C63A C64A -13.2(12) . . . . ? C1A C2A C63A C64A 159.7(7) . . . . ? N12 C63A C64A C65A 1.4(12) . . . . ? C2A C63A C64A C65A -171.6(7) . . . . ? C63A C64A C65A C66A 3.2(13) . . . . ? C64A C65A C66A C67A -3.6(13) . . . . ? C65A C66A C67A N12 -0.6(13) . . . . ? C17A C18A C68A N11 174.9(7) . . . . ? C19A C18A C68A N11 -16.7(10) . . . . ? C17A C18A C68A C69A -9.7(11) . . . . ? C19A C18A C68A C69A 158.7(7) . . . . ? N11 C68A C69A C70A 3.7(11) . . . . ? C18A C68A C69A C70A -171.8(7) . . . . ? C68A C69A C70A C71A 3.0(11) . . . . ? C69A C70A C71A C72A -5.2(11) . . . . ? C70A C71A C72A N11 0.9(12) . . . . ? C20B C1B C2B C3B 167.0(8) . . . . ? N5 C1B C2B C3B -4.8(9) . . . . ? C20B C1B C2B C63B -26.3(12) . . . . ? N5 C1B C2B C63B 161.9(7) . . . . ? C1B C2B C3B C4B 0.9(9) . . . . ? C63B C2B C3B C4B -165.4(7) . . . . ? C2B C3B C4B N5 3.3(9) . . . . ? C2B C3B C4B C5B -174.0(8) . . . . ? N5 C4B C5B C6B 13.3(12) . . . . ? C3B C4B C5B C6B -169.8(8) . . . . ? N5 C4B C5B C21B -165.2(7) . . . . ? C3B C4B C5B C21B 11.7(12) . . . . ? C4B C5B C6B N6 7.6(13) . . . . ? C21B C5B C6B N6 -173.9(8) . . . . ? C4B C5B C6B C7B -174.5(8) . . . . ? C21B C5B C6B C7B 4.0(13) . . . . ? C5B C6B C7B C8B -174.3(9) . . . . ? N6 C6B C7B C8B 3.9(10) . . . . ? C6B C7B C8B C9B -0.4(10) . . . . ? C7B C8B C9B C10B 172.5(8) . . . . ? C7B C8B C9B N6 -3.3(10) . . . . ? N6 C9B C10B C11B -5.5(13) . . . . ? C8B C9B C10B C11B 179.3(8) . . . . ? N6 C9B C10B C35B 177.9(8) . . . . ? C8B C9B C10B C35B 2.7(13) . . . . ? C9B C10B C11B N7 -12.2(12) . . . . ? C35B C10B C11B N7 164.6(7) . . . . ? C9B C10B C11B C12B 175.2(8) . . . . ? C35B C10B C11B C12B -8.1(12) . . . . ? C10B C11B C12B C13B 172.7(8) . . . . ? N7 C11B C12B C13B -0.9(10) . . . . ? C11B C12B C13B C14B -0.4(10) . . . . ? C12B C13B C14B C15B -167.0(8) . . . . ? C12B C13B C14B N7 1.5(10) . . . . ? C13B C14B C15B C16B 173.2(8) . . . . ? N7 C14B C15B C16B 6.2(13) . . . . ? C13B C14B C15B C49B -5.8(14) . . . . ? N7 C14B C15B C49B -172.8(7) . . . . ? C14B C15B C16B N4 17.0(12) . . . . ? C49B C15B C16B N4 -163.9(7) . . . . ? C14B C15B C16B C17B -164.6(8) . . . . ? C49B C15B C16B C17B 14.5(11) . . . . ? N4 C16B C17B C18B 2.8(9) . . . . ? C15B C16B C17B C18B -175.8(7) . . . . ? C16B C17B C18B C19B 2.9(8) . . . . ? C16B C17B C18B C68B -168.6(7) . . . . ? C17B C18B C19B N4 -7.6(8) . . . . ? C68B C18B C19B N4 163.8(6) . . . . ? C17B C18B C19B C20B 165.0(7) . . . . ? C68B C18B C19B C20B -23.6(12) . . . . ? N5 C1B C20B C19B -17.6(11) . . . . ? C2B C1B C20B C19B 171.8(7) . . . . ? N5 C1B C20B Ir2 166.4(5) . . . . ? C2B C1B C20B Ir2 -4.1(11) . . . . ? N4 C19B C20B C1B -14.0(10) . . . . ? C18B C19B C20B C1B 174.2(7) . . . . ? N4 C19B C20B Ir2 162.1(5) . . . . ? C18B C19B C20B Ir2 -9.7(10) . . . . ? C6B C5B C21B C22B 57.3(11) . . . . ? C4B C5B C21B C22B -124.2(8) . . . . ? C6B C5B C21B C26B -123.9(8) . . . . ? C4B C5B C21B C26B 54.7(10) . . . . ? C26B C21B C22B C23B 0.6(11) . . . . ? C5B C21B C22B C23B 179.5(7) . . . . ? C21B C22B C23B C24B -0.6(11) . . . . ? C21B C22B C23B C31B 177.5(7) . . . . ? C22B C23B C24B C25B 0.0(11) . . . . ? C31B C23B C24B C25B -178.2(8) . . . . ? C23B C24B C25B C26B 0.7(12) . . . . ? C23B C24B C25B C27B -179.5(7) . . . . ? C24B C25B C26B C21B -0.8(11) . . . . ? C27B C25B C26B C21B 179.5(7) . . . . ? C22B C21B C26B C25B 0.2(11) . . . . ? C5B C21B C26B C25B -178.7(7) . . . . ? C24B C25B C27B C30B -177.0(9) . . . . ? C26B C25B C27B C30B 2.7(12) . . . . ? C24B C25B C27B C28B -56.5(11) . . . . ? C26B C25B C27B C28B 123.3(9) . . . . ? C24B C25B C27B C29B 64.8(11) . . . . ? C26B C25B C27B C29B -115.4(10) . . . . ? C22B C23B C31B C34B -110.9(9) . . . . ? C24B C23B C31B C34B 67.1(10) . . . . ? C22B C23B C31B C33B 9.3(11) . . . . ? C24B C23B C31B C33B -172.6(8) . . . . ? C22B C23B C31B C32B 128.6(9) . . . . ? C24B C23B C31B C32B -53.4(11) . . . . ? C11B C10B C35B C40B 100.0(10) . . . . ? C9B C10B C35B C40B -83.3(10) . . . . ? C11B C10B C35B C36B -81.9(9) . . . . ? C9B C10B C35B C36B 94.8(10) . . . . ? C40B C35B C36B C37B -1.3(12) . . . . ? C10B C35B C36B C37B -179.5(7) . . . . ? C35B C36B C37B C38B 0.2(12) . . . . ? C35B C36B C37B C41B 176.5(8) . . . . ? C36B C37B C38B C39B 0.1(12) . . . . ? C41B C37B C38B C39B -176.3(7) . . . . ? C37B C38B C39B C40B 0.8(11) . . . . ? C37B C38B C39B C45B 177.7(8) . . . . ? C36B C35B C40B C39B 2.2(11) . . . . ? C10B C35B C40B C39B -179.7(7) . . . . ? C38B C39B C40B C35B -1.9(11) . . . . ? C45B C39B C40B C35B -179.0(7) . . . . ? C36B C37B C41B C42B -88.6(12) . . . . ? C38B C37B C41B C42B 87.6(12) . . . . ? C36B C37B C41B C44B 149.8(11) . . . . ? C38B C37B C41B C44B -34.0(14) . . . . ? C36B C37B C41B C43B 35.1(16) . . . . ? C38B C37B C41B C43B -148.8(13) . . . . ? C38B C39B C45B C46B 6.5(12) . . . . ? C40B C39B C45B C46B -176.6(8) . . . . ? C38B C39B C45B C48B -112.0(10) . . . . ? C40B C39B C45B C48B 64.8(11) . . . . ? C38B C39B C45B C47B 128.8(9) . . . . ? C40B C39B C45B C47B -54.3(10) . . . . ? C14B C15B C49B C50B 64.8(13) . . . . ? C16B C15B C49B C50B -114.2(10) . . . . ? C14B C15B C49B C54B -120.4(9) . . . . ? C16B C15B C49B C54B 60.6(11) . . . . ? C54B C49B C50B C51B -2.1(15) . . . . ? C15B C49B C50B C51B 172.7(9) . . . . ? C49B C50B C51B C52B 3.9(16) . . . . ? C49B C50B C51B C55B -178.1(10) . . . . ? C50B C51B C52B C53B -4.5(16) . . . . ? C55B C51B C52B C53B 177.6(11) . . . . ? C51B C52B C53B C54B 3.1(15) . . . . ? C51B C52B C53B C59B -176.8(9) . . . . ? C52B C53B C54B C49B -1.1(13) . . . . ? C59B C53B C54B C49B 178.8(8) . . . . ? C50B C49B C54B C53B 0.6(13) . . . . ? C15B C49B C54B C53B -174.5(8) . . . . ? C50B C51B C55B C58B -61.9(14) . . . . ? C52B C51B C55B C58B 116.0(13) . . . . ? C50B C51B C55B C57B 172.1(11) . . . . ? C52B C51B C55B C57B -10.0(17) . . . . ? C50B C51B C55B C56B 55.6(15) . . . . ? C52B C51B C55B C56B -126.5(12) . . . . ? C54B C53B C59B C62B -113.7(10) . . . . ? C52B C53B C59B C62B 66.3(11) . . . . ? C54B C53B C59B C61B 126.5(10) . . . . ? C52B C53B C59B C61B -53.6(14) . . . . ? C54B C53B C59B C60B 4.7(13) . . . . ? C52B C53B C59B C60B -175.4(10) . . . . ? C3B C2B C63B N9 -179.0(8) . . . . ? C1B C2B C63B N9 17.1(12) . . . . ? C3B C2B C63B C64B 7.1(12) . . . . ? C1B C2B C63B C64B -156.8(8) . . . . ? N9 C63B C64B C65B -4.8(13) . . . . ? C2B C63B C64B C65B 168.9(8) . . . . ? C63B C64B C65B C66B -1.3(14) . . . . ? C64B C65B C66B C67B 2.6(16) . . . . ? C65B C66B C67B N9 2.3(17) . . . . ? C17B C18B C68B N8 -171.8(7) . . . . ? C19B C18B C68B N8 18.3(11) . . . . ? C17B C18B C68B C69B 12.5(11) . . . . ? C19B C18B C68B C69B -157.3(7) . . . . ? N8 C68B C69B C70B -2.7(10) . . . . ? C18B C68B C69B C70B 172.9(7) . . . . ? C68B C69B C70B C71B -1.5(11) . . . . ? C69B C70B C71B C72B 2.0(11) . . . . ? C70B C71B C72B N8 1.8(12) . . . . ? C1A C20A Ir1 N11 152.7(6) . . . . ? C19A C20A Ir1 N11 -29.0(5) . . . . ? C1A C20A Ir1 N12 -26.6(6) . . . . ? C19A C20A Ir1 N12 151.8(5) . . . . ? C1A C20A Ir1 O1 -113(5) . . . . ? C19A C20A Ir1 O1 65(5) . . . . ? C1A C20A Ir1 Cl1 62.1(6) . . . . ? C19A C20A Ir1 Cl1 -119.6(5) . . . . ? C1A C20A Ir1 Cl2 -117.0(6) . . . . ? C19A C20A Ir1 Cl2 61.4(5) . . . . ? C1B C20B Ir2 N9 27.6(6) . . . . ? C19B C20B Ir2 N9 -148.4(6) . . . . ? C1B C20B Ir2 N8 -152.4(6) . . . . ? C19B C20B Ir2 N8 31.6(6) . . . . ? C1B C20B Ir2 O2 86(6) . . . . ? C19B C20B Ir2 O2 -90(6) . . . . ? C1B C20B Ir2 Cl4 118.1(6) . . . . ? C19B C20B Ir2 Cl4 -57.9(5) . . . . ? C1B C20B Ir2 Cl3 -62.3(6) . . . . ? C19B C20B Ir2 Cl3 121.7(5) . . . . ? C5A C4A N1 C1A -168.5(7) . . . . ? C3A C4A N1 C1A 7.6(8) . . . . ? C5A C4A N1 Ni1 24.7(10) . . . . ? C3A C4A N1 Ni1 -159.2(5) . . . . ? C20A C1A N1 C4A 160.1(7) . . . . ? C2A C1A N1 C4A -9.2(7) . . . . ? C20A C1A N1 Ni1 -32.8(10) . . . . ? C2A C1A N1 Ni1 157.9(5) . . . . ? C17A C16A N2 C19A 6.5(8) . . . . ? C15A C16A N2 C19A -170.2(6) . . . . ? C17A C16A N2 Ni1 -158.7(5) . . . . ? C15A C16A N2 Ni1 24.6(10) . . . . ? C20A C19A N2 C16A 161.6(6) . . . . ? C18A C19A N2 C16A -7.6(8) . . . . ? C20A C19A N2 Ni1 -32.9(9) . . . . ? C18A C19A N2 Ni1 157.9(5) . . . . ? C10A C9A N3 C6A 173.7(7) . . . . ? C8A C9A N3 C6A -2.5(8) . . . . ? C10A C9A N3 Ni1 -18.0(11) . . . . ? C8A C9A N3 Ni1 165.8(5) . . . . ? C5A C6A N3 C9A -172.5(7) . . . . ? C7A C6A N3 C9A 3.8(8) . . . . ? C5A C6A N3 Ni1 19.4(11) . . . . ? C7A C6A N3 Ni1 -164.3(5) . . . . ? C17B C16B N4 C19B -7.2(8) . . . . ? C15B C16B N4 C19B 171.4(7) . . . . ? C17B C16B N4 Ni2 157.2(5) . . . . ? C15B C16B N4 Ni2 -24.2(10) . . . . ? C20B C19B N4 C16B -163.9(6) . . . . ? C18B C19B N4 C16B 8.9(8) . . . . ? C20B C19B N4 Ni2 31.6(10) . . . . ? C18B C19B N4 Ni2 -155.6(5) . . . . ? C3B C4B N5 C1B -6.1(8) . . . . ? C5B C4B N5 C1B 171.2(7) . . . . ? C3B C4B N5 Ni2 157.5(5) . . . . ? C5B C4B N5 Ni2 -25.2(11) . . . . ? C20B C1B N5 C4B -165.2(7) . . . . ? C2B C1B N5 C4B 6.6(8) . . . . ? C20B C1B N5 Ni2 31.2(11) . . . . ? C2B C1B N5 Ni2 -157.0(5) . . . . ? C10B C9B N6 C6B -170.3(8) . . . . ? C8B C9B N6 C6B 5.5(9) . . . . ? C10B C9B N6 Ni2 17.9(12) . . . . ? C8B C9B N6 Ni2 -166.4(6) . . . . ? C5B C6B N6 C9B 172.6(8) . . . . ? C7B C6B N6 C9B -5.6(9) . . . . ? C5B C6B N6 Ni2 -15.7(12) . . . . ? C7B C6B N6 Ni2 166.1(6) . . . . ? C10B C11B N7 C14B -171.8(8) . . . . ? C12B C11B N7 C14B 1.7(9) . . . . ? C10B C11B N7 Ni2 16.6(11) . . . . ? C12B C11B N7 Ni2 -169.9(5) . . . . ? C15B C14B N7 C11B 166.6(8) . . . . ? C13B C14B N7 C11B -2.0(9) . . . . ? C15B C14B N7 Ni2 -21.8(12) . . . . ? C13B C14B N7 Ni2 169.6(6) . . . . ? C71B C72B N8 C68B -6.0(11) . . . . ? C71B C72B N8 Ir2 167.1(6) . . . . ? C69B C68B N8 C72B 6.3(10) . . . . ? C18B C68B N8 C72B -169.4(7) . . . . ? C69B C68B N8 Ir2 -166.6(5) . . . . ? C18B C68B N8 Ir2 17.7(9) . . . . ? C20B Ir2 N8 C72B 150.0(6) . . . . ? N9 Ir2 N8 C72B -31(4) . . . . ? O2 Ir2 N8 C72B -32.2(6) . . . . ? Cl4 Ir2 N8 C72B -117.3(5) . . . . ? Cl3 Ir2 N8 C72B 58.4(5) . . . . ? C20B Ir2 N8 C68B -37.2(6) . . . . ? N9 Ir2 N8 C68B 142(3) . . . . ? O2 Ir2 N8 C68B 140.7(6) . . . . ? Cl4 Ir2 N8 C68B 55.6(5) . . . . ? Cl3 Ir2 N8 C68B -128.7(5) . . . . ? C64B C63B N9 C67B 9.4(12) . . . . ? C2B C63B N9 C67B -164.4(7) . . . . ? C64B C63B N9 Ir2 -166.6(6) . . . . ? C2B C63B N9 Ir2 19.6(10) . . . . ? C66B C67B N9 C63B -8.2(14) . . . . ? C66B C67B N9 Ir2 168.0(8) . . . . ? C20B Ir2 N9 C63B -36.5(6) . . . . ? N8 Ir2 N9 C63B 144(3) . . . . ? O2 Ir2 N9 C63B 145.7(6) . . . . ? Cl4 Ir2 N9 C63B -129.3(6) . . . . ? Cl3 Ir2 N9 C63B 55.0(6) . . . . ? C20B Ir2 N9 C67B 147.5(6) . . . . ? N8 Ir2 N9 C67B -32(4) . . . . ? O2 Ir2 N9 C67B -30.3(6) . . . . ? Cl4 Ir2 N9 C67B 54.8(6) . . . . ? Cl3 Ir2 N9 C67B -121.0(6) . . . . ? C10A C11A N10 C14A 171.8(7) . . . . ? C12A C11A N10 C14A -5.7(8) . . . . ? C10A C11A N10 Ni1 -15.8(11) . . . . ? C12A C11A N10 Ni1 166.7(5) . . . . ? C15A C14A N10 C11A -165.8(7) . . . . ? C13A C14A N10 C11A 6.4(8) . . . . ? C15A C14A N10 Ni1 21.8(11) . . . . ? C13A C14A N10 Ni1 -166.1(5) . . . . ? C71A C72A N11 C68A 5.8(11) . . . . ? C71A C72A N11 Ir1 -165.5(6) . . . . ? C69A C68A N11 C72A -7.9(10) . . . . ? C18A C68A N11 C72A 167.6(6) . . . . ? C69A C68A N11 Ir1 163.2(5) . . . . ? C18A C68A N11 Ir1 -21.3(9) . . . . ? C20A Ir1 N11 C72A -150.3(6) . . . . ? N12 Ir1 N11 C72A 21(3) . . . . ? O1 Ir1 N11 C72A 32.8(6) . . . . ? Cl1 Ir1 N11 C72A -58.1(5) . . . . ? Cl2 Ir1 N11 C72A 117.7(5) . . . . ? C20A Ir1 N11 C68A 38.7(6) . . . . ? N12 Ir1 N11 C68A -150(2) . . . . ? O1 Ir1 N11 C68A -138.2(6) . . . . ? Cl1 Ir1 N11 C68A 130.9(5) . . . . ? Cl2 Ir1 N11 C68A -53.2(5) . . . . ? C66A C67A N12 C63A 5.1(12) . . . . ? C66A C67A N12 Ir1 -166.1(7) . . . . ? C64A C63A N12 C67A -5.4(11) . . . . ? C2A C63A N12 C67A 167.5(7) . . . . ? C64A C63A N12 Ir1 165.4(5) . . . . ? C2A C63A N12 Ir1 -21.7(9) . . . . ? C20A Ir1 N12 C67A -152.4(5) . . . . ? N11 Ir1 N12 C67A 37(3) . . . . ? O1 Ir1 N12 C67A 24.5(5) . . . . ? Cl1 Ir1 N12 C67A 115.5(5) . . . . ? Cl2 Ir1 N12 C67A -60.4(5) . . . . ? C20A Ir1 N12 C63A 36.8(5) . . . . ? N11 Ir1 N12 C63A -134(3) . . . . ? O1 Ir1 N12 C63A -146.3(5) . . . . ? Cl1 Ir1 N12 C63A -55.4(5) . . . . ? Cl2 Ir1 N12 C63A 128.7(5) . . . . ? C4A N1 Ni1 N2 178.7(6) . . . . ? C1A N1 Ni1 N2 14.3(6) . . . . ? C4A N1 Ni1 N10 88(2) . . . . ? C1A N1 Ni1 N10 -77(2) . . . . ? C4A N1 Ni1 N3 -9.6(6) . . . . ? C1A N1 Ni1 N3 -173.9(6) . . . . ? C16A N2 Ni1 N1 178.1(6) . . . . ? C19A N2 Ni1 N1 16.2(6) . . . . ? C16A N2 Ni1 N10 -9.3(6) . . . . ? C19A N2 Ni1 N10 -171.2(6) . . . . ? C16A N2 Ni1 N3 88.4(16) . . . . ? C19A N2 Ni1 N3 -73.6(17) . . . . ? C11A N10 Ni1 N1 -92(2) . . . . ? C14A N10 Ni1 N1 78(2) . . . . ? C11A N10 Ni1 N2 176.6(6) . . . . ? C14A N10 Ni1 N2 -12.5(6) . . . . ? C11A N10 Ni1 N3 4.8(6) . . . . ? C14A N10 Ni1 N3 175.7(6) . . . . ? C9A N3 Ni1 N1 -176.5(6) . . . . ? C6A N3 Ni1 N1 -10.9(6) . . . . ? C9A N3 Ni1 N2 -86.7(16) . . . . ? C6A N3 Ni1 N2 78.9(16) . . . . ? C9A N3 Ni1 N10 10.9(6) . . . . ? C6A N3 Ni1 N10 176.5(6) . . . . ? C16B N4 Ni2 N6 -88.9(19) . . . . ? C19B N4 Ni2 N6 71.9(19) . . . . ? C16B N4 Ni2 N5 -176.9(6) . . . . ? C19B N4 Ni2 N5 -16.1(6) . . . . ? C16B N4 Ni2 N7 8.9(6) . . . . ? C19B N4 Ni2 N7 169.7(6) . . . . ? C9B N6 Ni2 N4 86.6(19) . . . . ? C6B N6 Ni2 N4 -83.3(19) . . . . ? C9B N6 Ni2 N5 174.5(7) . . . . ? C6B N6 Ni2 N5 4.6(7) . . . . ? C9B N6 Ni2 N7 -11.2(7) . . . . ? C6B N6 Ni2 N7 178.9(7) . . . . ? C4B N5 Ni2 N4 -173.1(6) . . . . ? C1B N5 Ni2 N4 -12.8(6) . . . . ? C4B N5 Ni2 N6 14.4(6) . . . . ? C1B N5 Ni2 N6 174.6(6) . . . . ? C4B N5 Ni2 N7 -87(3) . . . . ? C1B N5 Ni2 N7 73(3) . . . . ? C11B N7 Ni2 N4 -177.3(6) . . . . ? C14B N7 Ni2 N4 12.9(7) . . . . ? C11B N7 Ni2 N6 -4.7(6) . . . . ? C14B N7 Ni2 N6 -174.5(7) . . . . ? C11B N7 Ni2 N5 97(3) . . . . ? C14B N7 Ni2 N5 -73(3) . . . . ? C20A Ir1 O1 C1M 156(5) . . . . ? N11 Ir1 O1 C1M -109.6(7) . . . . ? N12 Ir1 O1 C1M 69.4(7) . . . . ? Cl1 Ir1 O1 C1M -19.1(6) . . . . ? Cl2 Ir1 O1 C1M 159.9(6) . . . . ? C20B Ir2 O2 C2M -127(5) . . . . ? N9 Ir2 O2 C2M -68.4(8) . . . . ? N8 Ir2 O2 C2M 111.5(8) . . . . ? Cl4 Ir2 O2 C2M -159.0(8) . . . . ? Cl3 Ir2 O2 C2M 21.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.643 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.643 _refine_diff_density_max 2.037 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.149 data_90724naka _database_code_depnum_ccdc_archive 'CCDC 812769' #TrackingRef '- compd3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C80 H87 Ir N6 Ni O), 14(C2 H3 N)' _chemical_formula_sum 'C188 H216 Ir2 N26 Ni2 O2' _chemical_formula_weight 3373.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.195(5) _cell_length_b 17.790(5) _cell_length_c 35.311(5) _cell_angle_alpha 86.438(5) _cell_angle_beta 84.753(5) _cell_angle_gamma 81.444(5) _cell_volume 8152(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7121 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.24 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 1.919 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.301 _exptl_absorpt_correction_T_max 0.466 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _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 60148 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.28 _reflns_number_total 39751 _reflns_number_gt 28598 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Some tert-butyl substituents showed severe disorders. Thus, restrains by SIMUs, ISORs, DFIXs and Free were incorporated to the tert-butyl groups in order to maintain the exact structures. The distance of the C-N bond of some acetonitrile molecules is rather long. Thus, restrains by DFIX were incorporated to the acetonitrile molecule. ; _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^)+(0.0806P)^2^+67.7304P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 39751 _refine_ls_number_parameters 1806 _refine_ls_number_restraints 224 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2166 _refine_ls_wR_factor_gt 0.2072 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C36B C 0.0152(6) 0.8461(5) 0.4759(2) 0.0316(16) Uani 1 1 d . . . H36B H -0.0136 0.8951 0.4685 0.038 Uiso 1 1 calc R . . C1A C 0.3583(5) 0.3247(4) 0.17631(18) 0.0220(13) Uani 1 1 d . . . C2A C 0.2913(5) 0.2687(4) 0.17565(19) 0.0236(14) Uani 1 1 d . . . C3A C 0.2050(5) 0.3040(4) 0.15889(18) 0.0217(13) Uani 1 1 d . . . H3A H 0.1467 0.2823 0.1555 0.026 Uiso 1 1 calc R . . C4A C 0.2219(5) 0.3791(4) 0.14787(19) 0.0216(13) Uani 1 1 d . . . C5A C 0.1610(5) 0.4309(4) 0.12440(18) 0.0219(13) Uani 1 1 d . . . C6A C 0.1978(5) 0.4950(4) 0.10795(18) 0.0207(13) Uani 1 1 d . . . C7A C 0.1566(6) 0.5389(4) 0.0755(2) 0.0294(15) Uani 1 1 d . . . H7A H 0.0961 0.5343 0.0648 0.035 Uiso 1 1 calc R . . C8A C 0.2238(6) 0.5880(4) 0.0637(2) 0.0306(16) Uani 1 1 d . . . H8A H 0.2197 0.6215 0.0425 0.037 Uiso 1 1 calc R . . C9A C 0.3013(5) 0.5794(4) 0.0897(2) 0.0248(14) Uani 1 1 d . . . C10A C 0.3730(5) 0.6289(4) 0.0914(2) 0.0254(14) Uani 1 1 d . . . C11A C 0.4200(5) 0.6326(4) 0.1245(2) 0.0273(15) Uani 1 1 d . . . C12A C 0.4670(6) 0.6964(4) 0.1338(3) 0.0348(18) Uani 1 1 d . . . H12A H 0.4804 0.7377 0.1177 0.042 Uiso 1 1 calc R . . C13A C 0.4875(6) 0.6847(4) 0.1705(3) 0.0351(18) Uani 1 1 d . . . H13A H 0.5142 0.7181 0.1848 0.042 Uiso 1 1 calc R . . C14A C 0.4610(5) 0.6116(4) 0.1837(2) 0.0262(15) Uani 1 1 d . . . C15A C 0.4862(5) 0.5737(4) 0.2182(2) 0.0277(15) Uani 1 1 d . . . C16A C 0.4855(5) 0.4951(4) 0.2232(2) 0.0266(15) Uani 1 1 d . . . C17A C 0.5277(5) 0.4473(4) 0.2532(2) 0.0272(15) Uani 1 1 d . . . H17A H 0.5509 0.4634 0.2750 0.033 Uiso 1 1 calc R . . C18A C 0.5284(5) 0.3730(4) 0.2443(2) 0.0261(15) Uani 1 1 d . . . C19A C 0.4776(6) 0.3787(4) 0.2096(2) 0.0254(14) Uani 1 1 d . . . C20A C 0.4488(6) 0.3138(4) 0.1946(2) 0.0263(15) Uani 1 1 d . . . C21A C 0.0610(5) 0.4132(4) 0.11304(19) 0.0229(14) Uani 1 1 d . . . C22A C 0.0564(5) 0.3653(4) 0.0843(2) 0.0266(15) Uani 1 1 d . . . H22A H 0.1174 0.3389 0.0736 0.032 Uiso 1 1 calc R . . C23A C -0.0354(6) 0.3549(4) 0.0706(2) 0.0292(16) Uani 1 1 d . . . C24A C -0.1259(6) 0.3957(4) 0.0870(2) 0.0307(16) Uani 1 1 d . . . H24A H -0.1884 0.3900 0.0781 0.037 Uiso 1 1 calc R . . C25A C -0.1252(6) 0.4446(4) 0.1163(2) 0.0300(16) Uani 1 1 d . . . C26A C -0.0307(5) 0.4522(4) 0.1288(2) 0.0250(14) Uani 1 1 d . . . H26A H -0.0288 0.4844 0.1484 0.030 Uiso 1 1 calc R . . C27A C -0.0362(7) 0.3047(5) 0.0365(2) 0.0368(18) Uani 1 1 d . . . C28A C -0.1431(9) 0.2848(8) 0.0327(3) 0.069(3) Uani 1 1 d . . . H28A H -0.1408 0.2536 0.0113 0.103 Uiso 1 1 calc R . . H28B H -0.1902 0.3308 0.0289 0.103 Uiso 1 1 calc R . . H28C H -0.1658 0.2576 0.0555 0.103 Uiso 1 1 calc R . . C29A C -0.0044(9) 0.3524(7) 0.0008(3) 0.059(3) Uani 1 1 d . . . H29A H 0.0622 0.3664 0.0030 0.088 Uiso 1 1 calc R . . H29B H -0.0537 0.3975 -0.0017 0.088 Uiso 1 1 calc R . . H29C H -0.0019 0.3230 -0.0213 0.088 Uiso 1 1 calc R . . C30A C 0.0376(11) 0.2326(6) 0.0404(3) 0.072(4) Uani 1 1 d . . . H30A H 0.0361 0.2024 0.0188 0.108 Uiso 1 1 calc R . . H30B H 0.0182 0.2044 0.0633 0.108 Uiso 1 1 calc R . . H30C H 0.1058 0.2446 0.0414 0.108 Uiso 1 1 calc R . . C31A C -0.2243(6) 0.4909(5) 0.1338(3) 0.049(2) Uani 1 1 d . . . C32A C -0.2163(10) 0.5749(7) 0.1281(5) 0.082(4) Uani 1 1 d U . . H32A H -0.2751 0.6038 0.1411 0.123 Uiso 1 1 calc R . . H32B H -0.2139 0.5892 0.1014 0.123 Uiso 1 1 calc R . . H32C H -0.1548 0.5849 0.1382 0.123 Uiso 1 1 calc R . . C33A C -0.3216(7) 0.4774(7) 0.1159(4) 0.078(4) Uani 1 1 d . . . H33A H -0.3806 0.5074 0.1281 0.117 Uiso 1 1 calc R . . H33B H -0.3292 0.4245 0.1192 0.117 Uiso 1 1 calc R . . H33C H -0.3157 0.4918 0.0892 0.117 Uiso 1 1 calc R . . C34A C -0.2364(9) 0.4677(9) 0.1765(4) 0.088(5) Uani 1 1 d . . . H34A H -0.1856 0.4872 0.1894 0.131 Uiso 1 1 calc R . . H34B H -0.2273 0.4132 0.1798 0.131 Uiso 1 1 calc R . . H34C H -0.3039 0.4881 0.1870 0.131 Uiso 1 1 calc R . . C35A C 0.3994(6) 0.6794(4) 0.0575(2) 0.0282(15) Uani 1 1 d . . . C36A C 0.4715(6) 0.6456(4) 0.0301(2) 0.0316(16) Uani 1 1 d . . . H36A H 0.4965 0.5940 0.0329 0.038 Uiso 1 1 calc R . . C37A C 0.5067(6) 0.6883(4) -0.0016(2) 0.0349(18) Uani 1 1 d . . . C38A C 0.4649(6) 0.7656(4) -0.0051(2) 0.0328(17) Uani 1 1 d . . . H38A H 0.4886 0.7951 -0.0258 0.039 Uiso 1 1 calc R . . C39A C 0.3900(6) 0.7998(4) 0.0211(2) 0.0333(17) Uani 1 1 d . . . C40A C 0.3583(6) 0.7554(4) 0.0526(2) 0.0345(17) Uani 1 1 d . . . H40A H 0.3088 0.7772 0.0707 0.041 Uiso 1 1 calc R . . C41A C 0.5876(8) 0.6484(6) -0.0309(3) 0.055(3) Uani 1 1 d . . . C42A C 0.6279(8) 0.7044(6) -0.0602(3) 0.054(3) Uani 1 1 d . . . H42A H 0.5712 0.7344 -0.0718 0.082 Uiso 1 1 calc R . . H42B H 0.6726 0.6772 -0.0794 0.082 Uiso 1 1 calc R . . H42C H 0.6654 0.7371 -0.0481 0.082 Uiso 1 1 calc R . . C43A C 0.6776(10) 0.6059(8) -0.0103(4) 0.097(6) Uani 1 1 d . . . H43A H 0.7323 0.5873 -0.0287 0.145 Uiso 1 1 calc R . . H43B H 0.6553 0.5638 0.0049 0.145 Uiso 1 1 calc R . . H43C H 0.7017 0.6398 0.0058 0.145 Uiso 1 1 calc R . . C44A C 0.5349(12) 0.5927(6) -0.0498(4) 0.083(5) Uani 1 1 d . . . H44A H 0.4747 0.6192 -0.0606 0.124 Uiso 1 1 calc R . . H44B H 0.5152 0.5546 -0.0312 0.124 Uiso 1 1 calc R . . H44C H 0.5811 0.5687 -0.0695 0.124 Uiso 1 1 calc R . . C45A C 0.3500(9) 0.8846(5) 0.0161(3) 0.058(3) Uani 1 1 d U . . C46A C 0.3499(17) 0.9088(9) -0.0255(5) 0.141(7) Uani 1 1 d U . . H46A H 0.3156 0.9601 -0.0283 0.212 Uiso 1 1 calc R . . H46B H 0.3146 0.8756 -0.0383 0.212 Uiso 1 1 calc R . . H46C H 0.4195 0.9062 -0.0366 0.212 Uiso 1 1 calc R . . C47A C 0.2411(11) 0.9022(7) 0.0334(5) 0.094(5) Uani 1 1 d U . . H47A H 0.2383 0.8870 0.0600 0.141 Uiso 1 1 calc R . . H47B H 0.1974 0.8748 0.0208 0.141 Uiso 1 1 calc R . . H47C H 0.2181 0.9558 0.0304 0.141 Uiso 1 1 calc R . . C48A C 0.4180(12) 0.9299(7) 0.0333(6) 0.115(5) Uani 1 1 d U . . H48A H 0.3822 0.9802 0.0373 0.172 Uiso 1 1 calc R . . H48B H 0.4788 0.9330 0.0164 0.172 Uiso 1 1 calc R . . H48C H 0.4369 0.9058 0.0572 0.172 Uiso 1 1 calc R . . C49A C 0.5163(5) 0.6195(5) 0.2479(2) 0.0310(16) Uani 1 1 d . . . C50A C 0.6087(6) 0.6019(5) 0.2644(2) 0.0333(17) Uani 1 1 d . . . H50A H 0.6554 0.5605 0.2563 0.040 Uiso 1 1 calc R . . C51A C 0.6332(6) 0.6450(5) 0.2931(3) 0.0381(19) Uani 1 1 d . . . C52A C 0.5612(7) 0.7075(6) 0.3038(3) 0.046(2) Uani 1 1 d . . . H52A H 0.5757 0.7368 0.3230 0.055 Uiso 1 1 calc R . . C53A C 0.4684(6) 0.7282(5) 0.2870(3) 0.047(2) Uani 1 1 d . . . C54A C 0.4473(6) 0.6817(5) 0.2600(3) 0.042(2) Uani 1 1 d . . . H54A H 0.3844 0.6923 0.2495 0.051 Uiso 1 1 calc R . . C55A C 0.7321(7) 0.6230(5) 0.3129(3) 0.044(2) Uani 1 1 d . . . C56A C 0.8209(7) 0.5896(8) 0.2848(3) 0.074(4) Uani 1 1 d . . . H56A H 0.7988 0.5509 0.2710 0.112 Uiso 1 1 calc R . . H56B H 0.8784 0.5677 0.2986 0.112 Uiso 1 1 calc R . . H56C H 0.8407 0.6292 0.2673 0.112 Uiso 1 1 calc R . . C57A C 0.7647(10) 0.6912(7) 0.3303(5) 0.103(6) Uani 1 1 d . . . H57A H 0.7727 0.7305 0.3108 0.154 Uiso 1 1 calc R . . H57B H 0.8288 0.6759 0.3414 0.154 Uiso 1 1 calc R . . H57C H 0.7129 0.7103 0.3496 0.154 Uiso 1 1 calc R . . C58A C 0.7116(9) 0.5642(7) 0.3445(3) 0.065(3) Uani 1 1 d . . . H58A H 0.6600 0.5867 0.3630 0.098 Uiso 1 1 calc R . . H58B H 0.7738 0.5466 0.3565 0.098 Uiso 1 1 calc R . . H58C H 0.6879 0.5221 0.3340 0.098 Uiso 1 1 calc R . . C59A C 0.3908(7) 0.7957(6) 0.3011(3) 0.057(3) Uani 1 1 d . . . C60A C 0.3413(16) 0.7735(12) 0.3385(6) 0.135(7) Uani 1 1 d U . . H60A H 0.3922 0.7630 0.3566 0.202 Uiso 1 1 calc R . . H60B H 0.3099 0.7289 0.3363 0.202 Uiso 1 1 calc R . . H60C H 0.2897 0.8144 0.3469 0.202 Uiso 1 1 calc R . . C61A C 0.4425(9) 0.8635(7) 0.3053(5) 0.096(6) Uani 1 1 d . . . H61A H 0.3915 0.9066 0.3109 0.145 Uiso 1 1 calc R . . H61B H 0.4826 0.8741 0.2820 0.145 Uiso 1 1 calc R . . H61C H 0.4867 0.8533 0.3257 0.145 Uiso 1 1 calc R . . C62A C 0.3101(11) 0.8225(8) 0.2735(5) 0.093(4) Uani 1 1 d U . . H62A H 0.2601 0.7881 0.2754 0.139 Uiso 1 1 calc R . . H62B H 0.3424 0.8239 0.2480 0.139 Uiso 1 1 calc R . . H62C H 0.2767 0.8726 0.2795 0.139 Uiso 1 1 calc R . . C63A C 0.3033(6) 0.1916(4) 0.1937(2) 0.0287(15) Uani 1 1 d . . . C64A C 0.2252(6) 0.1477(4) 0.1938(2) 0.0330(17) Uani 1 1 d . . . H64A H 0.1665 0.1662 0.1815 0.040 Uiso 1 1 calc R . . C65A C 0.2342(7) 0.0759(4) 0.2122(3) 0.040(2) Uani 1 1 d . . . H65A H 0.1830 0.0455 0.2114 0.048 Uiso 1 1 calc R . . C66A C 0.3185(8) 0.0505(5) 0.2314(3) 0.049(2) Uani 1 1 d . . . H66A H 0.3242 0.0039 0.2451 0.059 Uiso 1 1 calc R . . C67A C 0.3950(9) 0.0958(5) 0.2299(3) 0.052(3) Uani 1 1 d . . . H67A H 0.4533 0.0775 0.2424 0.063 Uiso 1 1 calc R . . C68A C 0.5456(5) 0.3071(5) 0.2703(2) 0.0306(16) Uani 1 1 d . . . C69A C 0.5612(6) 0.3182(5) 0.3083(2) 0.0361(18) Uani 1 1 d . . . H69A H 0.5638 0.3671 0.3158 0.043 Uiso 1 1 calc R . . C70A C 0.5725(6) 0.2579(5) 0.3347(2) 0.0354(18) Uani 1 1 d . . . H70A H 0.5791 0.2657 0.3601 0.043 Uiso 1 1 calc R . . C71A C 0.5740(6) 0.1849(6) 0.3223(2) 0.042(2) Uani 1 1 d . . . H71A H 0.5837 0.1425 0.3391 0.050 Uiso 1 1 calc R . . C72A C 0.5608(6) 0.1771(5) 0.2848(2) 0.0362(18) Uani 1 1 d . . . H72A H 0.5624 0.1282 0.2767 0.043 Uiso 1 1 calc R . . C73A C 0.5258(6) 0.1942(5) 0.1433(2) 0.0377(18) Uani 1 1 d . . . H73A H 0.4552 0.2103 0.1365 0.045 Uiso 1 1 d R . . C74A C 0.5516(9) 0.1136(6) 0.1394(3) 0.060(3) Uani 1 1 d . . . C75A C 0.6513(11) 0.0773(7) 0.1553(5) 0.089(5) Uani 1 1 d . . . H75A H 0.6562 0.0223 0.1556 0.106 Uiso 1 1 d R . . H75B H 0.7095 0.0922 0.1393 0.106 Uiso 1 1 d R . . C76A C 0.6537(10) 0.1013(7) 0.1940(3) 0.073(4) Uani 1 1 d . . . H76A H 0.6514 0.0617 0.2145 0.087 Uiso 1 1 d R . . C77A C 0.6986(8) 0.1720(6) 0.2030(3) 0.057(3) Uani 1 1 d . . . H77A H 0.7286 0.1719 0.2273 0.068 Uiso 1 1 d R . . C78A C 0.6804(6) 0.2406(5) 0.1817(2) 0.0395(19) Uani 1 1 d . . . H78A H 0.6979 0.2843 0.1940 0.047 Uiso 1 1 d R . . C79A C 0.6950(7) 0.2469(6) 0.1381(3) 0.046(2) Uani 1 1 d . . . H79A H 0.7213 0.2940 0.1302 0.055 Uiso 1 1 d R . . H79B H 0.7458 0.2051 0.1293 0.055 Uiso 1 1 d R . . C80A C 0.5978(8) 0.2452(7) 0.1199(3) 0.058(3) Uani 1 1 d . . . H80A H 0.6144 0.2260 0.0947 0.069 Uiso 1 1 d R . . H80B H 0.5617 0.2967 0.1172 0.069 Uiso 1 1 d R . . C1B C 0.1550(5) 1.1285(4) 0.31534(19) 0.0223(13) Uani 1 1 d . . . C2B C 0.2233(5) 1.1845(4) 0.31351(19) 0.0245(14) Uani 1 1 d . . . C3B C 0.3072(5) 1.1510(4) 0.3316(2) 0.0262(14) Uani 1 1 d . . . H3B H 0.3659 1.1726 0.3343 0.031 Uiso 1 1 calc R . . C4B C 0.2883(5) 1.0771(4) 0.34542(19) 0.0215(13) Uani 1 1 d . . . C5B C 0.3453(5) 1.0306(4) 0.37175(19) 0.0230(13) Uani 1 1 d . . . C6B C 0.3045(5) 0.9710(4) 0.39141(18) 0.0197(13) Uani 1 1 d . . . C7B C 0.3406(6) 0.9337(4) 0.4263(2) 0.0282(15) Uani 1 1 d . . . H7B H 0.4012 0.9389 0.4367 0.034 Uiso 1 1 calc R . . C8B C 0.2701(6) 0.8902(4) 0.44071(19) 0.0261(14) Uani 1 1 d . . . H8B H 0.2699 0.8628 0.4640 0.031 Uiso 1 1 calc R . . C9B C 0.1952(5) 0.8940(4) 0.41352(18) 0.0206(13) Uani 1 1 d . . . C10B C 0.1194(5) 0.8465(4) 0.41493(18) 0.0222(13) Uani 1 1 d . . . C11B C 0.0722(5) 0.8361(4) 0.38206(19) 0.0223(13) Uani 1 1 d . . . C12B C 0.0212(5) 0.7731(4) 0.3765(2) 0.0279(15) Uani 1 1 d . . . H12B H 0.0035 0.7367 0.3950 0.034 Uiso 1 1 calc R . . C13B C 0.0032(5) 0.7760(4) 0.3395(2) 0.0277(15) Uani 1 1 d . . . H13B H -0.0248 0.7401 0.3272 0.033 Uiso 1 1 calc R . . C14B C 0.0353(5) 0.8452(4) 0.3224(2) 0.0222(13) Uani 1 1 d . . . C15B C 0.0154(5) 0.8758(4) 0.28622(19) 0.0229(13) Uani 1 1 d . . . C16B C 0.0212(5) 0.9519(4) 0.27657(19) 0.0229(14) Uani 1 1 d . . . C17B C -0.0178(5) 0.9951(4) 0.2442(2) 0.0274(15) Uani 1 1 d . . . H17B H -0.0425 0.9757 0.2235 0.033 Uiso 1 1 calc R . . C18B C -0.0123(6) 1.0695(4) 0.24901(19) 0.0246(14) Uani 1 1 d . . . C19B C 0.0344(5) 1.0723(4) 0.28362(18) 0.0223(13) Uani 1 1 d . . . C20B C 0.0645(5) 1.1386(4) 0.29586(19) 0.0231(14) Uani 1 1 d . . . C21B C 0.4450(5) 1.0482(4) 0.38306(19) 0.0231(14) Uani 1 1 d . . . C22B C 0.4484(5) 1.1048(4) 0.4079(2) 0.0257(14) Uani 1 1 d . . . H22B H 0.3878 1.1362 0.4152 0.031 Uiso 1 1 calc R . . C23B C 0.5393(6) 1.1164(4) 0.4224(2) 0.0274(15) Uani 1 1 d . . . C24B C 0.6293(6) 1.0701(4) 0.4097(2) 0.0297(16) Uani 1 1 d . . . H24B H 0.6911 1.0776 0.4186 0.036 Uiso 1 1 calc R . . C25B C 0.6303(6) 1.0130(5) 0.3842(2) 0.0315(16) Uani 1 1 d . A . C26B C 0.5360(5) 1.0032(4) 0.3714(2) 0.0284(15) Uani 1 1 d . . . H26B H 0.5345 0.9653 0.3545 0.034 Uiso 1 1 calc R . . C27B C 0.5395(7) 1.1718(5) 0.4530(2) 0.0370(18) Uani 1 1 d . . . C28B C 0.5167(10) 1.1297(7) 0.4916(3) 0.061(3) Uani 1 1 d . . . H28D H 0.4511 1.1123 0.4922 0.091 Uiso 1 1 calc R . . H28E H 0.5156 1.1637 0.5118 0.091 Uiso 1 1 calc R . . H28F H 0.5692 1.0869 0.4950 0.091 Uiso 1 1 calc R . . C29B C 0.6417(9) 1.2020(7) 0.4530(3) 0.066(3) Uani 1 1 d . . . H29D H 0.6929 1.1621 0.4617 0.099 Uiso 1 1 calc R . . H29E H 0.6338 1.2435 0.4697 0.099 Uiso 1 1 calc R . . H29F H 0.6629 1.2195 0.4277 0.099 Uiso 1 1 calc R . . C30B C 0.4569(9) 1.2400(6) 0.4494(3) 0.055(3) Uani 1 1 d . . . H30D H 0.4645 1.2639 0.4244 0.083 Uiso 1 1 calc R . . H30E H 0.4634 1.2757 0.4681 0.083 Uiso 1 1 calc R . . H30F H 0.3904 1.2238 0.4536 0.083 Uiso 1 1 calc R . . C31B C 0.7310(6) 0.9630(5) 0.3711(3) 0.0444(19) Uani 1 1 d U . . C32B C 0.8235(11) 0.9794(10) 0.3902(5) 0.053(4) Uani 0.641(13) 1 d PU A 3 H32D H 0.8829 0.9442 0.3822 0.080 Uiso 0.641(13) 1 calc PR A 3 H32E H 0.8101 0.9738 0.4174 0.080 Uiso 0.641(13) 1 calc PR A 3 H32F H 0.8360 1.0304 0.3833 0.080 Uiso 0.641(13) 1 calc PR A 3 C33B C 0.7149(15) 0.8817(11) 0.3824(7) 0.075(5) Uani 0.641(13) 1 d PU A 3 H33D H 0.6530 0.8714 0.3728 0.113 Uiso 0.641(13) 1 calc PR A 3 H33E H 0.7093 0.8749 0.4097 0.113 Uiso 0.641(13) 1 calc PR A 3 H33F H 0.7723 0.8473 0.3720 0.113 Uiso 0.641(13) 1 calc PR A 3 C34B C 0.7505(14) 0.9766(12) 0.3290(5) 0.070(5) Uani 0.641(13) 1 d PU A 3 H34D H 0.7639 1.0279 0.3235 0.105 Uiso 0.641(13) 1 calc PR A 3 H34E H 0.6912 0.9688 0.3167 0.105 Uiso 0.641(13) 1 calc PR A 3 H34F H 0.8090 0.9419 0.3197 0.105 Uiso 0.641(13) 1 calc PR A 3 C35B C 0.0899(5) 0.8061(4) 0.45158(18) 0.0227(13) Uani 1 1 d . . . C37B C -0.0179(6) 0.8143(4) 0.5114(2) 0.0328(17) Uani 1 1 d . . . C38B C 0.0269(6) 0.7407(4) 0.5213(2) 0.0320(16) Uani 1 1 d . . . H38B H 0.0053 0.7181 0.5445 0.038 Uiso 1 1 calc R . . C39B C 0.1024(6) 0.7000(4) 0.4979(2) 0.0299(16) Uani 1 1 d . . . C40B C 0.1331(6) 0.7334(4) 0.4629(2) 0.0283(15) Uani 1 1 d . . . H40B H 0.1835 0.7064 0.4469 0.034 Uiso 1 1 calc R . . C41B C -0.0990(7) 0.8622(6) 0.5375(2) 0.048(2) Uani 1 1 d . . . C42B C -0.0460(11) 0.9222(6) 0.5532(3) 0.075(4) Uani 1 1 d . . . H42D H -0.0165 0.9517 0.5325 0.113 Uiso 1 1 calc R . . H42E H 0.0073 0.8979 0.5684 0.113 Uiso 1 1 calc R . . H42F H -0.0953 0.9551 0.5686 0.113 Uiso 1 1 calc R . . C43B C -0.1891(9) 0.8981(8) 0.5158(3) 0.082(4) Uani 1 1 d . . . H43D H -0.1677 0.9368 0.4979 0.122 Uiso 1 1 calc R . . H43E H -0.2436 0.9205 0.5333 0.122 Uiso 1 1 calc R . . H43F H -0.2131 0.8599 0.5023 0.122 Uiso 1 1 calc R . . C44B C -0.1413(8) 0.8142(7) 0.5709(3) 0.055(3) Uani 1 1 d . . . H44D H -0.1852 0.8468 0.5881 0.083 Uiso 1 1 calc R . . H44E H -0.0853 0.7870 0.5839 0.083 Uiso 1 1 calc R . . H44F H -0.1800 0.7787 0.5616 0.083 Uiso 1 1 calc R . . C45B C 0.1500(8) 0.6192(5) 0.5103(3) 0.047(2) Uani 1 1 d U . . C46B C 0.0832(13) 0.5647(10) 0.5025(5) 0.106(5) Uani 1 1 d U . . H46D H 0.1071 0.5159 0.5142 0.159 Uiso 1 1 d R . . H46E H 0.0851 0.5605 0.4754 0.159 Uiso 1 1 d R . . H46F H 0.0140 0.5816 0.5124 0.159 Uiso 1 1 d R . . C47B C 0.2567(12) 0.5963(9) 0.4903(5) 0.101(4) Uani 1 1 d U . . H47D H 0.2800 0.5436 0.4965 0.151 Uiso 1 1 calc R . . H47E H 0.3038 0.6269 0.4986 0.151 Uiso 1 1 calc R . . H47F H 0.2535 0.6039 0.4633 0.151 Uiso 1 1 calc R . . C48B C 0.1758(14) 0.6162(9) 0.5516(4) 0.101(5) Uani 1 1 d U . . H48D H 0.1144 0.6317 0.5676 0.152 Uiso 1 1 calc R . . H48E H 0.2251 0.6498 0.5541 0.152 Uiso 1 1 calc R . . H48F H 0.2041 0.5651 0.5591 0.152 Uiso 1 1 calc R . . C49B C -0.0203(5) 0.8273(4) 0.2588(2) 0.0248(14) Uani 1 1 d . . . C50B C -0.1141(5) 0.8451(4) 0.2439(2) 0.0284(15) Uani 1 1 d . . . H50B H -0.1591 0.8870 0.2525 0.034 Uiso 1 1 calc R . . C51B C -0.1435(5) 0.8021(4) 0.2163(2) 0.0280(15) Uani 1 1 d . . . C52B C -0.0754(6) 0.7387(5) 0.2049(2) 0.0317(16) Uani 1 1 d . . . H52B H -0.0938 0.7088 0.1867 0.038 Uiso 1 1 calc R . . C53B C 0.0193(6) 0.7184(4) 0.2199(2) 0.0295(16) Uani 1 1 d . . . C54B C 0.0460(5) 0.7626(4) 0.2471(2) 0.0290(15) Uani 1 1 d . . . H54B H 0.1086 0.7494 0.2576 0.035 Uiso 1 1 calc R . . C55B C -0.2432(7) 0.8266(5) 0.1972(3) 0.044(2) Uani 1 1 d U . . C56B C -0.3265(11) 0.8587(10) 0.2246(4) 0.098(4) Uani 1 1 d U . . H56D H -0.3876 0.8749 0.2117 0.148 Uiso 1 1 calc R . . H56E H -0.3067 0.9015 0.2358 0.148 Uiso 1 1 calc R . . H56F H -0.3398 0.8206 0.2442 0.148 Uiso 1 1 calc R . . C57B C -0.2196(11) 0.8840(8) 0.1641(4) 0.080(4) Uani 1 1 d U . . H57D H -0.2761 0.8930 0.1483 0.120 Uiso 1 1 calc R . . H57E H -0.1582 0.8636 0.1492 0.120 Uiso 1 1 calc R . . H57F H -0.2097 0.9310 0.1742 0.120 Uiso 1 1 calc R . . C58B C -0.2760(10) 0.7613(7) 0.1777(4) 0.075(3) Uani 1 1 d U . . H58D H -0.2845 0.7201 0.1960 0.113 Uiso 1 1 calc R . . H58E H -0.2243 0.7443 0.1579 0.113 Uiso 1 1 calc R . . H58F H -0.3400 0.7785 0.1667 0.113 Uiso 1 1 calc R . . C59B C 0.0944(7) 0.6504(5) 0.2038(3) 0.041(2) Uani 1 1 d . . . C60B C 0.1199(12) 0.6689(7) 0.1613(3) 0.088(5) Uani 1 1 d . . . H60D H 0.1643 0.7073 0.1583 0.133 Uiso 1 1 calc R . . H60E H 0.0575 0.6872 0.1495 0.133 Uiso 1 1 calc R . . H60F H 0.1537 0.6238 0.1494 0.133 Uiso 1 1 calc R . . C61B C 0.1902(7) 0.6338(7) 0.2241(4) 0.069(4) Uani 1 1 d . . . H61D H 0.2349 0.5922 0.2127 0.103 Uiso 1 1 calc R . . H61E H 0.1730 0.6206 0.2504 0.103 Uiso 1 1 calc R . . H61F H 0.2244 0.6781 0.2222 0.103 Uiso 1 1 calc R . . C62B C 0.0422(8) 0.5791(6) 0.2077(4) 0.062(3) Uani 1 1 d . . . H62D H 0.0862 0.5384 0.1954 0.094 Uiso 1 1 calc R . . H62E H -0.0216 0.5892 0.1960 0.094 Uiso 1 1 calc R . . H62F H 0.0291 0.5650 0.2342 0.094 Uiso 1 1 calc R . . C63B C 0.2109(6) 1.2597(4) 0.2932(2) 0.0276(15) Uani 1 1 d . . . C64B C 0.2891(6) 1.3047(4) 0.2928(2) 0.0369(18) Uani 1 1 d . . . H64B H 0.3471 1.2869 0.3056 0.044 Uiso 1 1 calc R . . C65B C 0.2820(7) 1.3753(5) 0.2736(2) 0.0387(19) Uani 1 1 d . . . H65B H 0.3327 1.4063 0.2742 0.046 Uiso 1 1 calc R . . C66B C 0.1966(7) 1.3978(4) 0.2537(2) 0.039(2) Uani 1 1 d . . . H66B H 0.1902 1.4439 0.2395 0.047 Uiso 1 1 calc R . . C67B C 0.1227(8) 1.3530(5) 0.2548(2) 0.040(2) Uani 1 1 d . . . H67B H 0.0657 1.3696 0.2412 0.048 Uiso 1 1 calc R . . C68B C -0.0307(5) 1.1340(4) 0.2206(2) 0.0266(15) Uani 1 1 d . . . C69B C -0.0444(6) 1.1176(5) 0.1832(2) 0.0319(16) Uani 1 1 d . . . H69B H -0.0464 1.0675 0.1775 0.038 Uiso 1 1 calc R . . C70B C -0.0549(6) 1.1730(5) 0.1553(2) 0.0363(18) Uani 1 1 d . . . H70B H -0.0618 1.1614 0.1305 0.044 Uiso 1 1 calc R . . C71B C -0.0553(6) 1.2481(5) 0.1647(2) 0.0328(17) Uani 1 1 d . . . H71B H -0.0638 1.2878 0.1463 0.039 Uiso 1 1 calc R . . C72B C -0.0428(5) 1.2622(5) 0.2016(2) 0.0303(16) Uani 1 1 d . . . H72B H -0.0438 1.3124 0.2077 0.036 Uiso 1 1 calc R . . C73B C -0.0110(6) 1.2639(5) 0.3431(2) 0.0358(18) Uani 1 1 d . . . H73B H 0.0596 1.2484 0.3500 0.043 Uiso 1 1 d R . . C74B C -0.0329(8) 1.3431(6) 0.3445(3) 0.058(3) Uani 1 1 d . . . C75B C -0.1298(11) 1.3835(7) 0.3279(3) 0.071(3) Uani 1 1 d . . . H75C H -0.1897 1.3751 0.3448 0.085 Uiso 1 1 d R . . H75D H -0.1277 1.4378 0.3249 0.085 Uiso 1 1 d R . . C76B C -0.1363(9) 1.3511(5) 0.2897(3) 0.058(3) Uani 1 1 d . . . H76B H -0.1315 1.3874 0.2678 0.070 Uiso 1 1 d R . . C77B C -0.1820(7) 1.2825(6) 0.2827(2) 0.047(2) Uani 1 1 d . . . H77B H -0.2117 1.2805 0.2584 0.056 Uiso 1 1 d R . . C78B C -0.1641(6) 1.2138(5) 0.3060(3) 0.040(2) Uani 1 1 d . . . H78B H -0.1829 1.1688 0.2954 0.048 Uiso 1 1 d R . . C79B C -0.1822(7) 1.2160(6) 0.3503(3) 0.050(2) Uani 1 1 d . . . H79C H -0.2285 1.2617 0.3570 0.060 Uiso 1 1 d R . . H79D H -0.2145 1.1724 0.3602 0.060 Uiso 1 1 d R . . C80B C -0.0815(7) 1.2148(6) 0.3681(3) 0.045(2) Uani 1 1 d . . . H80C H -0.0471 1.1628 0.3705 0.054 Uiso 1 1 d R . . H80D H -0.0953 1.2344 0.3934 0.054 Uiso 1 1 d R . . C1S C 0.1899(16) 0.0729(9) 0.1030(5) 0.096(5) Uani 1 1 d . . . C2S C 0.2716(14) 0.1123(11) 0.0912(5) 0.106(5) Uani 1 1 d . . . H2S1 H 0.3305 0.0910 0.1044 0.159 Uiso 1 1 d R . . H2S2 H 0.2525 0.1648 0.0969 0.159 Uiso 1 1 d R . . H2S3 H 0.2879 0.1084 0.0643 0.159 Uiso 1 1 d R . . C3S C 0.6984(11) 0.8339(10) 0.0345(4) 0.089(5) Uani 1 1 d . . . C4S C 0.6569(13) 0.7895(11) 0.0663(4) 0.105(6) Uani 1 1 d . . . H4S1 H 0.6282 0.8226 0.0863 0.157 Uiso 1 1 d R . . H4S2 H 0.7106 0.7524 0.0757 0.157 Uiso 1 1 d R . . H4S3 H 0.6041 0.7640 0.0581 0.157 Uiso 1 1 d R . . C5S C 0.236(2) 0.3825(12) 0.4194(4) 0.143(9) Uani 1 1 d D . . C6S C 0.269(3) 0.3672(16) 0.3819(6) 0.207(14) Uani 1 1 d . . . H6S1 H 0.3199 0.3991 0.3727 0.310 Uiso 1 1 d R . . H6S2 H 0.2120 0.3772 0.3666 0.310 Uiso 1 1 d R . . H6S3 H 0.2994 0.3147 0.3804 0.310 Uiso 1 1 d R . . C7S C 0.5346(18) 0.4355(10) 0.4139(5) 0.124(7) Uani 1 1 d D . . C8S C 0.4922(18) 0.4672(16) 0.4480(8) 0.186(13) Uani 1 1 d . . . H8S1 H 0.4484 0.4341 0.4615 0.279 Uiso 1 1 d R . . H8S2 H 0.4526 0.5158 0.4426 0.279 Uiso 1 1 d R . . H8S3 H 0.5463 0.4736 0.4634 0.279 Uiso 1 1 d R . . C9S C 0.241(4) 0.8805(12) 0.1625(10) 0.173(17) Uani 1 1 d . . . C10S C 0.109(3) 0.8865(13) 0.1575(7) 0.187(14) Uani 1 1 d . . . H10A H 0.0831 0.9371 0.1487 0.280 Uiso 1 1 d R . . H10B H 0.0741 0.8747 0.1817 0.280 Uiso 1 1 d R . . H10C H 0.0986 0.8509 0.1395 0.280 Uiso 1 1 d R . . C32T C 0.812(2) 1.0091(17) 0.3554(9) 0.054(6) Uani 0.359(13) 1 d PU A 4 H32G H 0.8720 0.9759 0.3457 0.081 Uiso 0.359(13) 1 calc PR A 4 H32H H 0.8308 1.0379 0.3752 0.081 Uiso 0.359(13) 1 calc PR A 4 H32I H 0.7869 1.0433 0.3352 0.081 Uiso 0.359(13) 1 calc PR A 4 C33T C 0.775(2) 0.9164(18) 0.4049(9) 0.059(7) Uani 0.359(13) 1 d PU A 4 H33G H 0.8364 0.8841 0.3965 0.089 Uiso 0.359(13) 1 calc PR A 4 H33H H 0.7251 0.8857 0.4165 0.089 Uiso 0.359(13) 1 calc PR A 4 H33I H 0.7900 0.9500 0.4232 0.089 Uiso 0.359(13) 1 calc PR A 4 C34T C 0.7205(19) 0.9063(15) 0.3410(8) 0.045(6) Uani 0.359(13) 1 d PU A 4 H34G H 0.6917 0.9335 0.3192 0.067 Uiso 0.359(13) 1 calc PR A 4 H34H H 0.6761 0.8708 0.3516 0.067 Uiso 0.359(13) 1 calc PR A 4 H34I H 0.7870 0.8793 0.3334 0.067 Uiso 0.359(13) 1 calc PR A 4 Ir1 Ir 0.53186(2) 0.211356(17) 0.200944(9) 0.03350(9) Uani 1 1 d . . . Ir2 Ir -0.01590(2) 1.239769(17) 0.286138(8) 0.02917(8) Uani 1 1 d . . . N1A N 0.3137(4) 0.3930(3) 0.16004(15) 0.0207(11) Uani 1 1 d . . . N2A N 0.2856(4) 0.5216(3) 0.11640(15) 0.0215(11) Uani 1 1 d . . . N3A N 0.4180(4) 0.5804(3) 0.15488(17) 0.0234(12) Uani 1 1 d . . . N4A N 0.4497(4) 0.4516(3) 0.19779(16) 0.0249(12) Uani 1 1 d . . . N5A N 0.3911(6) 0.1651(4) 0.21140(19) 0.0348(15) Uani 1 1 d . . . N6A N 0.5456(5) 0.2363(4) 0.25875(17) 0.0295(13) Uani 1 1 d . . . N1B N 0.1961(4) 1.0628(3) 0.33394(15) 0.0194(11) Uani 1 1 d . . . N2B N 0.2158(4) 0.9444(3) 0.38388(15) 0.0190(11) Uani 1 1 d . . . N3B N 0.0796(4) 0.8807(3) 0.34901(15) 0.0199(11) Uani 1 1 d . . . N4B N 0.0587(4) 1.0001(3) 0.29939(15) 0.0195(11) Uani 1 1 d . . . N5B N 0.1265(5) 1.2849(4) 0.27460(16) 0.0291(13) Uani 1 1 d . . . N6B N -0.0292(4) 1.2077(3) 0.22928(16) 0.0253(13) Uani 1 1 d . . . N1S N 0.1235(16) 0.0408(12) 0.1123(6) 0.157(8) Uani 1 1 d . . . N2S N 0.7275(12) 0.8681(9) 0.0092(4) 0.109(5) Uani 1 1 d . . . N3S N 0.2280(16) 0.3899(10) 0.4515(4) 0.155(8) Uani 1 1 d D . . N4S N 0.566(2) 0.4099(11) 0.3864(5) 0.214(14) Uani 1 1 d D . . N5S N 0.309(5) 0.874(2) 0.1615(18) 0.35(4) Uani 1 1 d . . . Ni1 Ni 0.36801(6) 0.48633(5) 0.15692(2) 0.01926(17) Uani 1 1 d . . . Ni2 Ni 0.13686(6) 0.97238(5) 0.34191(2) 0.01710(16) Uani 1 1 d . . . O1 O 0.4924(8) 0.0755(5) 0.1268(3) 0.091(3) Uani 1 1 d . . . O2 O 0.0241(10) 1.3828(5) 0.3561(4) 0.115(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C36B 0.029(4) 0.036(4) 0.027(4) 0.004(3) 0.002(3) 0.000(3) C1A 0.028(3) 0.018(3) 0.019(3) 0.000(2) 0.003(3) -0.001(3) C2A 0.024(3) 0.020(3) 0.025(3) -0.001(3) 0.004(3) -0.005(3) C3A 0.021(3) 0.022(3) 0.022(3) -0.001(2) 0.003(3) -0.002(3) C4A 0.018(3) 0.024(3) 0.022(3) -0.001(3) 0.002(2) -0.001(3) C5A 0.021(3) 0.024(3) 0.020(3) -0.002(2) 0.001(2) 0.001(3) C6A 0.017(3) 0.021(3) 0.022(3) -0.002(2) 0.004(2) 0.000(2) C7A 0.026(4) 0.030(4) 0.030(4) 0.001(3) -0.005(3) 0.002(3) C8A 0.038(4) 0.030(4) 0.022(3) 0.006(3) -0.002(3) -0.004(3) C9A 0.025(3) 0.021(3) 0.026(3) -0.001(3) 0.006(3) -0.001(3) C10A 0.024(3) 0.019(3) 0.031(4) 0.002(3) 0.006(3) 0.000(3) C11A 0.020(3) 0.022(3) 0.037(4) 0.002(3) 0.006(3) 0.000(3) C12A 0.027(4) 0.021(4) 0.055(5) 0.006(3) -0.004(3) -0.001(3) C13A 0.022(4) 0.023(4) 0.062(5) -0.010(4) -0.003(3) -0.005(3) C14A 0.017(3) 0.024(3) 0.037(4) -0.010(3) 0.004(3) -0.002(3) C15A 0.017(3) 0.026(4) 0.039(4) -0.009(3) 0.001(3) 0.000(3) C16A 0.016(3) 0.036(4) 0.027(3) -0.003(3) 0.006(3) -0.005(3) C17A 0.022(3) 0.036(4) 0.024(3) -0.004(3) -0.003(3) -0.002(3) C18A 0.020(3) 0.030(4) 0.024(3) 0.001(3) 0.002(3) 0.008(3) C19A 0.031(4) 0.015(3) 0.029(3) 0.009(3) -0.009(3) 0.003(3) C20A 0.030(4) 0.024(3) 0.023(3) 0.002(3) 0.003(3) -0.003(3) C21A 0.023(3) 0.018(3) 0.025(3) 0.003(3) 0.001(3) 0.000(3) C22A 0.023(3) 0.028(4) 0.027(3) 0.002(3) -0.003(3) 0.002(3) C23A 0.032(4) 0.030(4) 0.025(3) 0.009(3) -0.006(3) -0.005(3) C24A 0.026(4) 0.031(4) 0.035(4) 0.007(3) -0.009(3) -0.001(3) C25A 0.025(4) 0.025(4) 0.040(4) -0.001(3) -0.001(3) -0.001(3) C26A 0.026(3) 0.017(3) 0.033(4) -0.006(3) -0.001(3) -0.004(3) C27A 0.044(5) 0.036(4) 0.033(4) 0.001(3) -0.010(4) -0.009(4) C28A 0.071(8) 0.095(9) 0.050(6) -0.032(6) 0.002(5) -0.037(7) C29A 0.074(7) 0.080(8) 0.026(4) 0.003(4) -0.005(4) -0.027(6) C30A 0.115(11) 0.050(6) 0.053(6) -0.029(5) -0.030(7) 0.008(6) C31A 0.023(4) 0.041(5) 0.084(7) -0.026(5) -0.004(4) 0.003(4) C32A 0.054(6) 0.063(6) 0.124(8) -0.029(6) -0.003(6) 0.014(5) C33A 0.022(5) 0.072(8) 0.142(12) -0.051(8) -0.014(6) 0.011(5) C34A 0.042(6) 0.136(13) 0.083(9) -0.047(9) 0.017(6) -0.001(7) C35A 0.027(4) 0.025(4) 0.032(4) 0.002(3) 0.004(3) -0.006(3) C36A 0.029(4) 0.029(4) 0.035(4) -0.002(3) 0.008(3) -0.003(3) C37A 0.038(4) 0.027(4) 0.036(4) 0.005(3) 0.008(3) 0.000(3) C38A 0.038(4) 0.024(4) 0.034(4) 0.004(3) 0.005(3) -0.006(3) C39A 0.039(4) 0.020(3) 0.040(4) 0.003(3) 0.001(3) -0.004(3) C40A 0.030(4) 0.030(4) 0.039(4) 0.005(3) 0.004(3) 0.006(3) C41A 0.062(6) 0.047(6) 0.044(5) 0.005(4) 0.026(5) 0.010(5) C42A 0.055(6) 0.066(7) 0.034(5) 0.009(4) 0.016(4) 0.001(5) C43A 0.079(9) 0.101(10) 0.074(8) 0.039(7) 0.045(7) 0.058(8) C44A 0.132(12) 0.037(6) 0.069(8) -0.018(5) 0.047(8) -0.007(7) C45A 0.072(6) 0.016(4) 0.078(6) 0.013(4) 0.012(5) 0.007(4) C46A 0.200(15) 0.080(9) 0.101(10) 0.044(8) 0.033(11) 0.071(10) C47A 0.079(8) 0.043(6) 0.143(12) 0.010(7) 0.029(8) 0.016(6) C48A 0.094(10) 0.034(6) 0.219(15) -0.014(8) -0.047(10) 0.003(6) C49A 0.016(3) 0.036(4) 0.042(4) -0.012(3) -0.003(3) -0.003(3) C50A 0.022(4) 0.034(4) 0.045(4) -0.007(3) -0.004(3) -0.002(3) C51A 0.023(4) 0.044(5) 0.049(5) -0.010(4) -0.004(3) -0.007(3) C52A 0.030(4) 0.057(6) 0.055(6) -0.024(5) -0.008(4) -0.008(4) C53A 0.019(4) 0.050(5) 0.072(6) -0.029(5) -0.003(4) 0.001(4) C54A 0.020(4) 0.042(5) 0.068(6) -0.025(4) -0.010(4) -0.002(3) C55A 0.034(5) 0.044(5) 0.057(6) -0.005(4) -0.013(4) -0.008(4) C56A 0.020(4) 0.124(11) 0.074(8) 0.013(7) -0.010(5) 0.003(5) C57A 0.071(9) 0.059(8) 0.195(18) -0.002(9) -0.090(10) -0.015(6) C58A 0.053(6) 0.084(8) 0.058(6) 0.014(6) -0.012(5) -0.009(6) C59A 0.026(4) 0.066(7) 0.078(7) -0.039(6) 0.001(4) 0.008(4) C60A 0.127(10) 0.124(10) 0.135(10) -0.011(8) 0.035(8) 0.015(8) C61A 0.049(7) 0.073(8) 0.171(15) -0.077(10) -0.034(8) 0.025(6) C62A 0.071(7) 0.086(7) 0.118(8) -0.047(7) -0.030(6) 0.029(6) C63A 0.035(4) 0.021(3) 0.028(4) 0.003(3) 0.004(3) -0.003(3) C64A 0.032(4) 0.025(4) 0.038(4) 0.003(3) 0.006(3) 0.000(3) C65A 0.038(5) 0.023(4) 0.056(5) 0.000(4) 0.007(4) -0.006(3) C66A 0.070(7) 0.031(4) 0.051(5) 0.015(4) -0.016(5) -0.019(4) C67A 0.074(7) 0.034(5) 0.053(6) 0.018(4) -0.035(5) -0.011(5) C68A 0.019(3) 0.040(4) 0.028(4) 0.009(3) 0.001(3) 0.004(3) C69A 0.028(4) 0.052(5) 0.029(4) 0.000(3) -0.006(3) -0.006(4) C70A 0.027(4) 0.052(5) 0.029(4) 0.009(3) -0.010(3) -0.009(4) C71A 0.021(4) 0.066(6) 0.039(4) 0.030(4) -0.011(3) -0.018(4) C72A 0.026(4) 0.038(4) 0.045(5) 0.018(4) -0.005(3) -0.011(3) C73A 0.026(4) 0.046(5) 0.039(4) -0.009(4) 0.003(3) 0.002(3) C74A 0.072(7) 0.033(5) 0.072(7) -0.011(5) 0.005(6) -0.001(5) C75A 0.070(9) 0.048(7) 0.139(14) 0.006(8) -0.016(9) 0.018(6) C76A 0.090(9) 0.061(7) 0.051(6) -0.002(5) -0.017(6) 0.047(7) C77A 0.052(6) 0.056(6) 0.048(5) 0.005(5) 0.004(4) 0.030(5) C78A 0.034(4) 0.040(5) 0.041(5) 0.004(4) -0.001(4) 0.002(4) C79A 0.046(5) 0.047(5) 0.041(5) 0.006(4) 0.000(4) -0.003(4) C80A 0.045(6) 0.087(8) 0.044(5) 0.000(5) -0.002(4) -0.020(5) C1B 0.016(3) 0.026(3) 0.021(3) -0.004(3) 0.006(2) 0.002(3) C2B 0.020(3) 0.027(3) 0.024(3) 0.003(3) 0.006(3) 0.000(3) C3B 0.017(3) 0.027(4) 0.034(4) 0.000(3) 0.001(3) -0.006(3) C4B 0.015(3) 0.025(3) 0.023(3) -0.003(3) 0.004(2) -0.001(3) C5B 0.021(3) 0.025(3) 0.022(3) -0.005(3) 0.003(3) 0.000(3) C6B 0.017(3) 0.024(3) 0.017(3) -0.003(2) -0.001(2) 0.002(2) C7B 0.027(4) 0.031(4) 0.026(3) 0.002(3) -0.007(3) 0.001(3) C8B 0.035(4) 0.030(4) 0.015(3) 0.000(3) -0.006(3) -0.007(3) C9B 0.022(3) 0.020(3) 0.017(3) -0.002(2) 0.001(2) 0.003(3) C10B 0.018(3) 0.026(3) 0.019(3) 0.002(3) 0.002(2) 0.004(3) C11B 0.015(3) 0.024(3) 0.025(3) -0.001(3) 0.001(2) 0.004(2) C12B 0.020(3) 0.028(4) 0.036(4) 0.003(3) -0.003(3) -0.008(3) C13B 0.023(3) 0.027(4) 0.035(4) -0.006(3) -0.001(3) -0.007(3) C14B 0.014(3) 0.020(3) 0.032(4) -0.007(3) 0.000(3) 0.003(2) C15B 0.016(3) 0.027(3) 0.024(3) -0.004(3) 0.000(2) 0.001(3) C16B 0.015(3) 0.031(4) 0.020(3) -0.006(3) -0.002(2) 0.009(3) C17B 0.024(3) 0.035(4) 0.021(3) 0.002(3) -0.005(3) 0.001(3) C18B 0.031(4) 0.023(3) 0.019(3) 0.004(3) 0.000(3) -0.001(3) C19B 0.017(3) 0.032(4) 0.017(3) -0.002(3) 0.005(2) -0.001(3) C20B 0.019(3) 0.025(3) 0.022(3) 0.005(3) 0.000(3) 0.001(3) C21B 0.022(3) 0.025(3) 0.024(3) 0.002(3) -0.003(3) -0.007(3) C22B 0.021(3) 0.026(4) 0.028(3) 0.004(3) -0.003(3) 0.000(3) C23B 0.030(4) 0.030(4) 0.024(3) 0.001(3) -0.007(3) -0.008(3) C24B 0.021(3) 0.029(4) 0.038(4) 0.016(3) -0.011(3) -0.002(3) C25B 0.025(4) 0.036(4) 0.032(4) 0.000(3) -0.001(3) -0.004(3) C26B 0.022(3) 0.030(4) 0.033(4) 0.000(3) -0.001(3) -0.005(3) C27B 0.046(5) 0.042(5) 0.026(4) -0.007(3) -0.009(3) -0.008(4) C28B 0.093(9) 0.066(7) 0.027(4) -0.005(4) -0.014(5) -0.015(6) C29B 0.061(7) 0.079(8) 0.067(7) -0.037(6) 0.000(6) -0.031(6) C30B 0.069(7) 0.051(6) 0.050(6) -0.021(5) -0.014(5) -0.009(5) C31B 0.025(3) 0.042(4) 0.065(5) -0.016(4) -0.001(3) 0.007(3) C32B 0.035(6) 0.055(7) 0.068(7) -0.012(6) -0.004(6) 0.006(5) C33B 0.058(8) 0.061(8) 0.103(9) -0.011(7) -0.007(7) 0.006(6) C34B 0.049(7) 0.084(8) 0.070(8) -0.022(7) 0.004(6) 0.014(6) C35B 0.019(3) 0.028(3) 0.020(3) 0.004(3) 0.001(2) 0.000(3) C37B 0.035(4) 0.031(4) 0.026(4) 0.006(3) 0.007(3) 0.007(3) C38B 0.034(4) 0.030(4) 0.032(4) 0.006(3) -0.001(3) -0.008(3) C39B 0.037(4) 0.017(3) 0.034(4) 0.004(3) -0.004(3) -0.003(3) C40B 0.030(4) 0.022(3) 0.032(4) -0.004(3) 0.002(3) -0.002(3) C41B 0.047(5) 0.056(6) 0.026(4) 0.007(4) 0.016(4) 0.021(4) C42B 0.117(11) 0.040(6) 0.055(6) -0.009(5) 0.032(7) 0.012(6) C43B 0.068(8) 0.102(10) 0.049(6) 0.016(6) 0.024(6) 0.044(7) C44B 0.044(5) 0.078(7) 0.034(5) 0.007(5) 0.012(4) 0.013(5) C45B 0.053(4) 0.035(4) 0.052(4) 0.002(3) -0.002(4) -0.001(3) C46B 0.101(7) 0.092(7) 0.126(7) 0.000(6) -0.018(6) -0.012(6) C47B 0.095(7) 0.085(6) 0.114(7) 0.013(5) -0.002(6) 0.004(5) C48B 0.113(7) 0.090(7) 0.095(7) 0.000(5) -0.017(6) 0.007(5) C49B 0.022(3) 0.027(3) 0.025(3) -0.007(3) -0.003(3) 0.000(3) C50B 0.015(3) 0.034(4) 0.035(4) -0.002(3) -0.003(3) 0.001(3) C51B 0.021(3) 0.031(4) 0.033(4) -0.003(3) -0.007(3) 0.000(3) C52B 0.027(4) 0.036(4) 0.033(4) -0.009(3) -0.006(3) -0.002(3) C53B 0.021(3) 0.030(4) 0.037(4) -0.008(3) 0.001(3) -0.001(3) C54B 0.018(3) 0.032(4) 0.036(4) -0.003(3) -0.005(3) 0.001(3) C55B 0.035(4) 0.049(4) 0.049(4) -0.010(4) -0.018(3) 0.000(3) C56B 0.072(7) 0.126(8) 0.092(7) -0.025(7) -0.010(6) 0.010(6) C57B 0.074(6) 0.074(6) 0.093(7) 0.018(6) -0.035(6) -0.007(5) C58B 0.062(6) 0.067(6) 0.105(7) -0.008(5) -0.048(5) -0.012(5) C59B 0.033(4) 0.038(5) 0.049(5) -0.018(4) 0.001(4) 0.007(4) C60B 0.123(12) 0.070(8) 0.052(7) -0.016(6) 0.033(7) 0.036(8) C61B 0.032(5) 0.062(7) 0.114(10) -0.053(7) -0.016(6) 0.013(5) C62B 0.045(6) 0.047(6) 0.098(9) -0.037(6) -0.025(6) 0.009(4) C63B 0.028(4) 0.026(4) 0.025(3) 0.000(3) 0.011(3) -0.001(3) C64B 0.030(4) 0.028(4) 0.047(5) 0.005(3) 0.007(3) 0.004(3) C65B 0.038(4) 0.031(4) 0.045(5) 0.002(3) 0.017(4) -0.009(3) C66B 0.060(6) 0.022(4) 0.031(4) 0.009(3) 0.002(4) 0.000(4) C67B 0.059(6) 0.032(4) 0.027(4) 0.004(3) -0.007(4) -0.003(4) C68B 0.022(3) 0.034(4) 0.022(3) 0.008(3) -0.003(3) -0.002(3) C69B 0.027(4) 0.036(4) 0.032(4) -0.001(3) -0.009(3) 0.000(3) C70B 0.034(4) 0.053(5) 0.023(4) 0.008(3) -0.012(3) -0.006(4) C71B 0.024(4) 0.043(5) 0.030(4) 0.014(3) -0.004(3) -0.008(3) C72B 0.019(3) 0.034(4) 0.037(4) 0.011(3) -0.005(3) -0.005(3) C73B 0.030(4) 0.053(5) 0.024(4) 0.000(3) -0.002(3) -0.005(4) C74B 0.049(6) 0.045(6) 0.077(7) -0.014(5) 0.002(5) 0.008(5) C75B 0.092(9) 0.049(6) 0.066(7) -0.017(5) -0.010(7) 0.016(6) C76B 0.088(8) 0.032(5) 0.045(5) 0.002(4) -0.005(5) 0.022(5) C77B 0.038(5) 0.056(6) 0.033(4) 0.007(4) 0.001(4) 0.030(4) C78B 0.027(4) 0.044(5) 0.046(5) 0.010(4) -0.007(3) 0.003(3) C79B 0.043(5) 0.068(7) 0.040(5) 0.013(4) -0.003(4) -0.015(5) C80B 0.036(5) 0.054(6) 0.041(5) -0.001(4) 0.004(4) 0.001(4) C1S 0.112(14) 0.069(10) 0.097(12) -0.019(8) 0.020(10) 0.005(9) C2S 0.111(13) 0.135(15) 0.077(10) -0.010(10) -0.005(9) -0.035(12) C3S 0.067(9) 0.120(13) 0.070(9) -0.010(9) 0.017(7) 0.005(8) C4S 0.100(12) 0.141(15) 0.085(10) 0.030(10) -0.026(9) -0.056(11) C5S 0.24(3) 0.123(16) 0.070(11) -0.034(11) 0.019(14) -0.054(17) C6S 0.32(4) 0.21(3) 0.078(14) 0.029(16) -0.072(19) 0.00(3) C7S 0.21(2) 0.076(11) 0.093(13) -0.017(10) -0.029(14) -0.032(13) C8S 0.13(2) 0.22(3) 0.21(3) -0.13(2) -0.050(19) 0.024(18) C9S 0.32(6) 0.037(9) 0.15(2) -0.009(11) 0.00(3) 0.013(19) C10S 0.29(4) 0.104(17) 0.126(18) -0.006(13) 0.09(2) 0.02(2) C32T 0.044(9) 0.050(9) 0.067(10) -0.010(8) 0.004(8) -0.007(7) C33T 0.053(9) 0.060(10) 0.061(10) -0.010(8) -0.009(8) 0.007(8) C34T 0.032(8) 0.049(9) 0.052(9) -0.019(7) -0.006(7) 0.007(7) Ir1 0.03543(17) 0.02757(16) 0.03275(16) 0.00593(12) -0.00330(12) 0.00827(12) Ir2 0.03040(16) 0.02826(15) 0.02412(14) 0.00472(11) -0.00059(11) 0.00776(11) N1A 0.019(3) 0.024(3) 0.017(2) 0.004(2) 0.004(2) -0.002(2) N2A 0.027(3) 0.017(3) 0.019(3) -0.001(2) 0.001(2) 0.001(2) N3A 0.024(3) 0.017(3) 0.029(3) 0.000(2) -0.002(2) -0.003(2) N4A 0.020(3) 0.030(3) 0.025(3) -0.004(2) -0.001(2) -0.005(2) N5A 0.048(4) 0.020(3) 0.035(3) 0.004(3) -0.011(3) 0.001(3) N6A 0.024(3) 0.036(4) 0.027(3) 0.008(3) 0.000(2) -0.005(3) N1B 0.019(3) 0.015(3) 0.024(3) -0.001(2) -0.003(2) 0.000(2) N2B 0.020(3) 0.018(3) 0.018(3) -0.006(2) 0.000(2) -0.001(2) N3B 0.018(3) 0.022(3) 0.019(3) 0.000(2) -0.001(2) -0.002(2) N4B 0.020(3) 0.014(2) 0.022(3) 0.000(2) 0.000(2) 0.004(2) N5B 0.040(4) 0.027(3) 0.018(3) 0.005(2) 0.002(3) -0.003(3) N6B 0.016(3) 0.030(3) 0.025(3) 0.004(2) 0.003(2) 0.008(2) N1S 0.153(18) 0.143(17) 0.173(18) -0.081(14) 0.052(15) -0.023(13) N2S 0.107(11) 0.113(11) 0.094(10) 0.004(8) 0.019(8) 0.012(9) N3S 0.20(2) 0.142(15) 0.114(13) -0.066(12) -0.017(13) 0.036(13) N4S 0.45(4) 0.138(16) 0.076(10) -0.042(10) 0.055(17) -0.15(2) N5S 0.43(8) 0.17(3) 0.39(6) 0.00(3) -0.05(5) 0.16(4) Ni1 0.0165(4) 0.0173(4) 0.0228(4) 0.0002(3) 0.0008(3) -0.0009(3) Ni2 0.0134(4) 0.0188(4) 0.0185(4) 0.0000(3) -0.0005(3) -0.0012(3) O1 0.109(8) 0.045(5) 0.120(8) -0.025(5) -0.028(6) 0.007(5) O2 0.153(11) 0.056(6) 0.147(10) -0.026(6) -0.079(9) -0.003(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 C36B C35B 1.389(10) . ? C36B C37B 1.403(10) . ? C36B H36B 0.9300 . ? C1A N1A 1.385(8) . ? C1A C20A 1.391(10) . ? C1A C2A 1.428(10) . ? C2A C3A 1.381(10) . ? C2A C63A 1.469(9) . ? C3A C4A 1.413(9) . ? C3A H3A 0.9300 . ? C4A N1A 1.383(9) . ? C4A C5A 1.410(9) . ? C5A C6A 1.380(9) . ? C5A C21A 1.496(10) . ? C6A N2A 1.377(9) . ? C6A C7A 1.446(9) . ? C7A C8A 1.356(11) . ? C7A H7A 0.9300 . ? C8A C9A 1.420(10) . ? C8A H8A 0.9300 . ? C9A N2A 1.377(8) . ? C9A C10A 1.393(10) . ? C10A C11A 1.382(11) . ? C10A C35A 1.500(9) . ? C11A N3A 1.374(9) . ? C11A C12A 1.441(11) . ? C12A C13A 1.343(12) . ? C12A H12A 0.9300 . ? C13A C14A 1.435(10) . ? C13A H13A 0.9300 . ? C14A N3A 1.391(9) . ? C14A C15A 1.397(11) . ? C15A C16A 1.401(10) . ? C15A C49A 1.482(10) . ? C16A N4A 1.377(9) . ? C16A C17A 1.418(10) . ? C17A C18A 1.375(10) . ? C17A H17A 0.9300 . ? C18A C19A 1.442(10) . ? C18A C68A 1.446(10) . ? C19A N4A 1.346(9) . ? C19A C20A 1.415(10) . ? C20A Ir1 1.994(7) . ? C21A C22A 1.377(10) . ? C21A C26A 1.390(9) . ? C22A C23A 1.387(10) . ? C22A H22A 0.9300 . ? C23A C24A 1.398(11) . ? C23A C27A 1.543(11) . ? C24A C25A 1.393(11) . ? C24A H24A 0.9300 . ? C25A C26A 1.388(10) . ? C25A C31A 1.539(11) . ? C26A H26A 0.9300 . ? C27A C30A 1.498(14) . ? C27A C28A 1.524(14) . ? C27A C29A 1.538(12) . ? C28A H28A 0.9600 . ? C28A H28B 0.9600 . ? C28A H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C30A H30A 0.9600 . ? C30A H30B 0.9600 . ? C30A H30C 0.9600 . ? C31A C32A 1.514(16) . ? C31A C34A 1.538(18) . ? C31A C33A 1.538(13) . ? C32A H32A 0.9600 . ? C32A H32B 0.9600 . ? C32A H32C 0.9600 . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C34A H34A 0.9600 . ? C34A H34B 0.9600 . ? C34A H34C 0.9600 . ? C35A C40A 1.386(10) . ? C35A C36A 1.391(10) . ? C36A C37A 1.396(10) . ? C36A H36A 0.9300 . ? C37A C38A 1.405(11) . ? C37A C41A 1.543(11) . ? C38A C39A 1.387(11) . ? C38A H38A 0.9300 . ? C39A C40A 1.393(11) . ? C39A C45A 1.528(11) . ? C40A H40A 0.9300 . ? C41A C42A 1.508(13) . ? C41A C44A 1.512(18) . ? C41A C43A 1.527(16) . ? C42A H42A 0.9600 . ? C42A H42B 0.9600 . ? C42A H42C 0.9600 . ? C43A H43A 0.9600 . ? C43A H43B 0.9600 . ? C43A H43C 0.9600 . ? C44A H44A 0.9600 . ? C44A H44B 0.9600 . ? C44A H44C 0.9600 . ? C45A C48A 1.482(18) . ? C45A C47A 1.506(16) . ? C45A C46A 1.505(18) . ? C46A H46A 0.9600 . ? C46A H46B 0.9600 . ? C46A H46C 0.9600 . ? C47A H47A 0.9600 . ? C47A H47B 0.9600 . ? C47A H47C 0.9600 . ? C48A H48A 0.9600 . ? C48A H48B 0.9600 . ? C48A H48C 0.9600 . ? C49A C50A 1.386(10) . ? C49A C54A 1.388(11) . ? C50A C51A 1.396(11) . ? C50A H50A 0.9300 . ? C51A C52A 1.398(12) . ? C51A C55A 1.526(12) . ? C52A C53A 1.400(12) . ? C52A H52A 0.9300 . ? C53A C54A 1.371(12) . ? C53A C59A 1.535(12) . ? C54A H54A 0.9300 . ? C55A C58A 1.515(14) . ? C55A C57A 1.526(15) . ? C55A C56A 1.537(15) . ? C56A H56A 0.9600 . ? C56A H56B 0.9600 . ? C56A H56C 0.9600 . ? C57A H57A 0.9600 . ? C57A H57B 0.9600 . ? C57A H57C 0.9600 . ? C58A H58A 0.9600 . ? C58A H58B 0.9600 . ? C58A H58C 0.9600 . ? C59A C60A 1.48(2) . ? C59A C61A 1.493(16) . ? C59A C62A 1.515(17) . ? C60A H60A 0.9600 . ? C60A H60B 0.9600 . ? C60A H60C 0.9600 . ? C61A H61A 0.9600 . ? C61A H61B 0.9600 . ? C61A H61C 0.9600 . ? C62A H62A 0.9600 . ? C62A H62B 0.9600 . ? C62A H62C 0.9600 . ? C63A N5A 1.374(10) . ? C63A C64A 1.383(11) . ? C64A C65A 1.390(11) . ? C64A H64A 0.9300 . ? C65A C66A 1.360(13) . ? C65A H65A 0.9300 . ? C66A C67A 1.377(13) . ? C66A H66A 0.9300 . ? C67A N5A 1.356(10) . ? C67A H67A 0.9300 . ? C68A N6A 1.348(11) . ? C68A C69A 1.408(11) . ? C69A C70A 1.378(11) . ? C69A H69A 0.9300 . ? C70A C71A 1.392(13) . ? C70A H70A 0.9300 . ? C71A C72A 1.371(12) . ? C71A H71A 0.9300 . ? C72A N6A 1.359(9) . ? C72A H72A 0.9300 . ? C73A C74A 1.437(13) . ? C73A C80A 1.558(13) . ? C73A Ir1 2.087(8) . ? C73A H73A 0.9800 . ? C74A O1 1.235(14) . ? C74A C75A 1.516(17) . ? C75A C76A 1.464(19) . ? C75A H75A 0.9700 . ? C75A H75B 0.9700 . ? C76A C77A 1.528(18) . ? C76A Ir1 2.351(10) . ? C76A H76A 0.9800 . ? C77A C78A 1.393(13) . ? C77A Ir1 2.213(10) . ? C77A H77A 0.9800 . ? C78A C79A 1.533(12) . ? C78A Ir1 2.143(9) . ? C78A H78A 0.9800 . ? C79A C80A 1.491(14) . ? C79A H79A 0.9700 . ? C79A H79B 0.9700 . ? C80A H80A 0.9700 . ? C80A H80B 0.9700 . ? C1B N1B 1.368(8) . ? C1B C20B 1.416(9) . ? C1B C2B 1.434(10) . ? C2B C3B 1.368(10) . ? C2B C63B 1.473(10) . ? C3B C4B 1.423(10) . ? C3B H3B 0.9300 . ? C4B N1B 1.380(8) . ? C4B C5B 1.400(10) . ? C5B C6B 1.380(9) . ? C5B C21B 1.491(10) . ? C6B N2B 1.379(8) . ? C6B C7B 1.447(9) . ? C7B C8B 1.343(10) . ? C7B H7B 0.9300 . ? C8B C9B 1.431(9) . ? C8B H8B 0.9300 . ? C9B N2B 1.370(8) . ? C9B C10B 1.398(10) . ? C10B C11B 1.401(10) . ? C10B C35B 1.489(9) . ? C11B N3B 1.374(8) . ? C11B C12B 1.422(10) . ? C12B C13B 1.346(11) . ? C12B H12B 0.9300 . ? C13B C14B 1.441(10) . ? C13B H13B 0.9300 . ? C14B N3B 1.381(9) . ? C14B C15B 1.388(10) . ? C15B C16B 1.386(10) . ? C15B C49B 1.488(10) . ? C16B N4B 1.384(9) . ? C16B C17B 1.429(9) . ? C17B C18B 1.358(10) . ? C17B H17B 0.9300 . ? C18B C19B 1.425(9) . ? C18B C68B 1.485(9) . ? C19B N4B 1.372(8) . ? C19B C20B 1.403(10) . ? C20B Ir2 1.976(7) . ? C21B C26B 1.385(10) . ? C21B C22B 1.385(10) . ? C22B C23B 1.394(10) . ? C22B H22B 0.9300 . ? C23B C24B 1.396(11) . ? C23B C27B 1.506(11) . ? C24B C25B 1.397(11) . ? C24B H24B 0.9300 . ? C25B C26B 1.400(10) . ? C25B C31B 1.536(11) . ? C26B H26B 0.9300 . ? C27B C30B 1.513(13) . ? C27B C29B 1.525(13) . ? C27B C28B 1.541(12) . ? C28B H28D 0.9600 . ? C28B H28E 0.9600 . ? C28B H28F 0.9600 . ? C29B H29D 0.9600 . ? C29B H29E 0.9600 . ? C29B H29F 0.9600 . ? C30B H30D 0.9600 . ? C30B H30E 0.9600 . ? C30B H30F 0.9600 . ? C31B C32T 1.49(3) . ? C31B C34B 1.50(2) . ? C31B C33B 1.52(2) . ? C31B C33T 1.52(3) . ? C31B C32B 1.521(18) . ? C31B C34T 1.54(3) . ? C32B H32D 0.9600 . ? C32B H32E 0.9600 . ? C32B H32F 0.9600 . ? C33B H33D 0.9600 . ? C33B H33E 0.9600 . ? C33B H33F 0.9600 . ? C34B H34D 0.9600 . ? C34B H34E 0.9600 . ? C34B H34F 0.9600 . ? C35B C40B 1.384(10) . ? C37B C38B 1.390(10) . ? C37B C41B 1.539(11) . ? C38B C39B 1.380(11) . ? C38B H38B 0.9300 . ? C39B C40B 1.390(10) . ? C39B C45B 1.536(11) . ? C40B H40B 0.9300 . ? C41B C43B 1.513(14) . ? C41B C42B 1.517(17) . ? C41B C44B 1.525(12) . ? C42B H42D 0.9600 . ? C42B H42E 0.9600 . ? C42B H42F 0.9600 . ? C43B H43D 0.9600 . ? C43B H43E 0.9600 . ? C43B H43F 0.9600 . ? C44B H44D 0.9600 . ? C44B H44E 0.9600 . ? C44B H44F 0.9600 . ? C45B C46B 1.459(18) . ? C45B C48B 1.521(18) . ? C45B C47B 1.527(18) . ? C46B H46D 0.9600 . ? C46B H46E 0.9600 . ? C46B H46F 0.9600 . ? C47B H47D 0.9600 . ? C47B H47E 0.9600 . ? C47B H47F 0.9600 . ? C48B H48D 0.9600 . ? C48B H48E 0.9600 . ? C48B H48F 0.9600 . ? C49B C50B 1.376(9) . ? C49B C54B 1.397(10) . ? C50B C51B 1.389(10) . ? C50B H50B 0.9300 . ? C51B C52B 1.390(10) . ? C51B C55B 1.527(11) . ? C52B C53B 1.391(10) . ? C52B H52B 0.9300 . ? C53B C54B 1.378(11) . ? C53B C59B 1.548(10) . ? C54B H54B 0.9300 . ? C55B C56B 1.468(16) . ? C55B C58B 1.522(14) . ? C55B C57B 1.545(16) . ? C56B H56D 0.9600 . ? C56B H56E 0.9600 . ? C56B H56F 0.9600 . ? C57B H57D 0.9600 . ? C57B H57E 0.9600 . ? C57B H57F 0.9600 . ? C58B H58D 0.9600 . ? C58B H58E 0.9600 . ? C58B H58F 0.9600 . ? C59B C61B 1.492(13) . ? C59B C62B 1.523(14) . ? C59B C60B 1.535(14) . ? C60B H60D 0.9600 . ? C60B H60E 0.9600 . ? C60B H60F 0.9600 . ? C61B H61D 0.9600 . ? C61B H61E 0.9600 . ? C61B H61F 0.9600 . ? C62B H62D 0.9600 . ? C62B H62E 0.9600 . ? C62B H62F 0.9600 . ? C63B N5B 1.349(10) . ? C63B C64B 1.396(11) . ? C64B C65B 1.385(11) . ? C64B H64B 0.9300 . ? C65B C66B 1.380(13) . ? C65B H65B 0.9300 . ? C66B C67B 1.345(13) . ? C66B H66B 0.9300 . ? C67B N5B 1.359(10) . ? C67B H67B 0.9300 . ? C68B N6B 1.368(10) . ? C68B C69B 1.402(10) . ? C69B C70B 1.350(11) . ? C69B H69B 0.9300 . ? C70B C71B 1.396(12) . ? C70B H70B 0.9300 . ? C71B C72B 1.369(11) . ? C71B H71B 0.9300 . ? C72B N6B 1.339(9) . ? C72B H72B 0.9300 . ? C73B C74B 1.398(13) . ? C73B C80B 1.551(12) . ? C73B Ir2 2.092(8) . ? C73B H73B 0.9800 . ? C74B O2 1.217(14) . ? C74B C75B 1.518(16) . ? C75B C76B 1.515(15) . ? C75B H75C 0.9700 . ? C75B H75D 0.9700 . ? C76B C77B 1.482(16) . ? C76B Ir2 2.349(9) . ? C76B H76B 0.9800 . ? C77B C78B 1.431(12) . ? C77B Ir2 2.222(8) . ? C77B H77B 0.9800 . ? C78B C79B 1.559(13) . ? C78B Ir2 2.124(8) . ? C78B H78B 0.9800 . ? C79B C80B 1.519(13) . ? C79B H79C 0.9700 . ? C79B H79D 0.9700 . ? C80B H80C 0.9700 . ? C80B H80D 0.9700 . ? C1S N1S 1.13(2) . ? C1S C2S 1.39(2) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? C3S N2S 1.121(18) . ? C3S C4S 1.45(2) . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C5S N3S 1.143(9) . ? C5S C6S 1.39(3) . ? C6S H6S1 0.9600 . ? C6S H6S2 0.9600 . ? C6S H6S3 0.9600 . ? C7S N4S 1.116(9) . ? C7S C8S 1.40(3) . ? C8S H8S1 0.9600 . ? C8S H8S2 0.9600 . ? C8S H8S3 0.9600 . ? C9S N5S 0.88(9) . ? C9S C10S 1.75(5) . ? C10S H10A 0.9600 . ? C10S H10B 0.9600 . ? C10S H10C 0.9600 . ? C32T H32G 0.9600 . ? C32T H32H 0.9600 . ? C32T H32I 0.9600 . ? C33T H33G 0.9600 . ? C33T H33H 0.9600 . ? C33T H33I 0.9600 . ? C34T H34G 0.9600 . ? C34T H34H 0.9600 . ? C34T H34I 0.9600 . ? Ir1 N5A 2.134(7) . ? Ir1 N6A 2.145(6) . ? Ir2 N5B 2.146(7) . ? Ir2 N6B 2.151(6) . ? N1A Ni1 1.897(6) . ? N2A Ni1 1.896(6) . ? N3A Ni1 1.883(6) . ? N4A Ni1 1.898(6) . ? N1B Ni2 1.886(5) . ? N2B Ni2 1.888(5) . ? N3B Ni2 1.891(6) . ? N4B Ni2 1.898(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C35B C36B C37B 121.6(7) . . ? C35B C36B H36B 119.2 . . ? C37B C36B H36B 119.2 . . ? N1A C1A C20A 125.4(6) . . ? N1A C1A C2A 109.8(6) . . ? C20A C1A C2A 124.5(6) . . ? C3A C2A C1A 106.8(6) . . ? C3A C2A C63A 125.2(7) . . ? C1A C2A C63A 127.5(7) . . ? C2A C3A C4A 107.1(6) . . ? C2A C3A H3A 126.5 . . ? C4A C3A H3A 126.5 . . ? N1A C4A C5A 123.5(6) . . ? N1A C4A C3A 110.3(6) . . ? C5A C4A C3A 125.9(6) . . ? C6A C5A C4A 120.5(6) . . ? C6A C5A C21A 118.3(6) . . ? C4A C5A C21A 120.8(6) . . ? N2A C6A C5A 125.9(6) . . ? N2A C6A C7A 109.4(6) . . ? C5A C6A C7A 124.3(7) . . ? C8A C7A C6A 106.4(7) . . ? C8A C7A H7A 126.8 . . ? C6A C7A H7A 126.8 . . ? C7A C8A C9A 107.9(6) . . ? C7A C8A H8A 126.0 . . ? C9A C8A H8A 126.0 . . ? N2A C9A C10A 124.5(7) . . ? N2A C9A C8A 109.8(6) . . ? C10A C9A C8A 125.0(7) . . ? C11A C10A C9A 120.5(6) . . ? C11A C10A C35A 119.2(6) . . ? C9A C10A C35A 120.4(7) . . ? N3A C11A C10A 124.8(7) . . ? N3A C11A C12A 110.4(7) . . ? C10A C11A C12A 124.3(7) . . ? C13A C12A C11A 106.5(7) . . ? C13A C12A H12A 126.7 . . ? C11A C12A H12A 126.7 . . ? C12A C13A C14A 108.1(7) . . ? C12A C13A H13A 125.9 . . ? C14A C13A H13A 125.9 . . ? N3A C14A C15A 125.1(6) . . ? N3A C14A C13A 109.2(7) . . ? C15A C14A C13A 125.2(7) . . ? C14A C15A C16A 120.0(7) . . ? C14A C15A C49A 117.4(7) . . ? C16A C15A C49A 122.6(7) . . ? N4A C16A C15A 124.4(7) . . ? N4A C16A C17A 109.6(6) . . ? C15A C16A C17A 125.9(7) . . ? C18A C17A C16A 108.0(6) . . ? C18A C17A H17A 126.0 . . ? C16A C17A H17A 126.0 . . ? C17A C18A C19A 104.4(6) . . ? C17A C18A C68A 125.7(7) . . ? C19A C18A C68A 127.2(7) . . ? N4A C19A C20A 126.3(6) . . ? N4A C19A C18A 111.8(6) . . ? C20A C19A C18A 121.2(6) . . ? C1A C20A C19A 116.8(6) . . ? C1A C20A Ir1 121.9(5) . . ? C19A C20A Ir1 121.3(5) . . ? C22A C21A C26A 118.1(7) . . ? C22A C21A C5A 122.0(6) . . ? C26A C21A C5A 119.5(6) . . ? C21A C22A C23A 122.7(7) . . ? C21A C22A H22A 118.7 . . ? C23A C22A H22A 118.7 . . ? C22A C23A C24A 117.4(7) . . ? C22A C23A C27A 120.8(7) . . ? C24A C23A C27A 121.6(7) . . ? C25A C24A C23A 121.9(7) . . ? C25A C24A H24A 119.0 . . ? C23A C24A H24A 119.0 . . ? C26A C25A C24A 117.8(7) . . ? C26A C25A C31A 120.1(7) . . ? C24A C25A C31A 122.1(7) . . ? C25A C26A C21A 122.0(7) . . ? C25A C26A H26A 119.0 . . ? C21A C26A H26A 119.0 . . ? C30A C27A C28A 109.0(9) . . ? C30A C27A C29A 110.5(9) . . ? C28A C27A C29A 108.5(8) . . ? C30A C27A C23A 110.9(7) . . ? C28A C27A C23A 111.7(7) . . ? C29A C27A C23A 106.2(7) . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C27A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C27A C30A H30A 109.5 . . ? C27A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C27A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C32A C31A C34A 110.5(10) . . ? C32A C31A C33A 107.4(9) . . ? C34A C31A C33A 108.2(10) . . ? C32A C31A C25A 109.2(8) . . ? C34A C31A C25A 108.1(8) . . ? C33A C31A C25A 113.4(8) . . ? C31A C32A H32A 109.5 . . ? C31A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C31A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C31A C33A H33A 109.5 . . ? C31A C33A H33B 109.5 . . ? H33A C33A H33B 109.5 . . ? C31A C33A H33C 109.5 . . ? H33A C33A H33C 109.5 . . ? H33B C33A H33C 109.5 . . ? C31A C34A H34A 109.5 . . ? C31A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C31A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C40A C35A C36A 120.0(7) . . ? C40A C35A C10A 124.4(7) . . ? C36A C35A C10A 115.6(6) . . ? C35A C36A C37A 120.6(7) . . ? C35A C36A H36A 119.7 . . ? C37A C36A H36A 119.7 . . ? C36A C37A C38A 117.7(7) . . ? C36A C37A C41A 118.6(7) . . ? C38A C37A C41A 123.7(7) . . ? C39A C38A C37A 122.7(7) . . ? C39A C38A H38A 118.7 . . ? C37A C38A H38A 118.7 . . ? C38A C39A C40A 117.8(7) . . ? C38A C39A C45A 119.9(7) . . ? C40A C39A C45A 122.2(8) . . ? C35A C40A C39A 121.2(7) . . ? C35A C40A H40A 119.4 . . ? C39A C40A H40A 119.4 . . ? C42A C41A C44A 110.3(9) . . ? C42A C41A C43A 108.8(10) . . ? C44A C41A C43A 109.9(11) . . ? C42A C41A C37A 111.8(8) . . ? C44A C41A C37A 106.5(9) . . ? C43A C41A C37A 109.4(8) . . ? C41A C42A H42A 109.5 . . ? C41A C42A H42B 109.5 . . ? H42A C42A H42B 109.5 . . ? C41A C42A H42C 109.5 . . ? H42A C42A H42C 109.5 . . ? H42B C42A H42C 109.5 . . ? C41A C43A H43A 109.5 . . ? C41A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C41A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? C41A C44A H44A 109.5 . . ? C41A C44A H44B 109.5 . . ? H44A C44A H44B 109.5 . . ? C41A C44A H44C 109.5 . . ? H44A C44A H44C 109.5 . . ? H44B C44A H44C 109.5 . . ? C48A C45A C47A 110.6(12) . . ? C48A C45A C46A 107.4(14) . . ? C47A C45A C46A 107.3(13) . . ? C48A C45A C39A 110.1(10) . . ? C47A C45A C39A 110.9(8) . . ? C46A C45A C39A 110.5(10) . . ? C45A C46A H46A 109.5 . . ? C45A C46A H46B 109.5 . . ? H46A C46A H46B 109.5 . . ? C45A C46A H46C 109.5 . . ? H46A C46A H46C 109.5 . . ? H46B C46A H46C 109.5 . . ? C45A C47A H47A 109.5 . . ? C45A C47A H47B 109.5 . . ? H47A C47A H47B 109.5 . . ? C45A C47A H47C 109.5 . . ? H47A C47A H47C 109.5 . . ? H47B C47A H47C 109.5 . . ? C45A C48A H48A 109.5 . . ? C45A C48A H48B 109.5 . . ? H48A C48A H48B 109.5 . . ? C45A C48A H48C 109.5 . . ? H48A C48A H48C 109.5 . . ? H48B C48A H48C 109.5 . . ? C50A C49A C54A 118.9(7) . . ? C50A C49A C15A 123.0(7) . . ? C54A C49A C15A 118.1(7) . . ? C49A C50A C51A 121.5(7) . . ? C49A C50A H50A 119.2 . . ? C51A C50A H50A 119.2 . . ? C50A C51A C52A 116.9(8) . . ? C50A C51A C55A 121.4(8) . . ? C52A C51A C55A 121.6(8) . . ? C51A C52A C53A 123.1(8) . . ? C51A C52A H52A 118.4 . . ? C53A C52A H52A 118.4 . . ? C54A C53A C52A 116.9(8) . . ? C54A C53A C59A 122.3(8) . . ? C52A C53A C59A 120.5(8) . . ? C53A C54A C49A 122.5(8) . . ? C53A C54A H54A 118.7 . . ? C49A C54A H54A 118.7 . . ? C58A C55A C51A 107.4(8) . . ? C58A C55A C57A 108.8(10) . . ? C51A C55A C57A 111.7(8) . . ? C58A C55A C56A 109.9(9) . . ? C51A C55A C56A 110.9(8) . . ? C57A C55A C56A 108.0(10) . . ? C55A C56A H56A 109.5 . . ? C55A C56A H56B 109.5 . . ? H56A C56A H56B 109.5 . . ? C55A C56A H56C 109.5 . . ? H56A C56A H56C 109.5 . . ? H56B C56A H56C 109.5 . . ? C55A C57A H57A 109.5 . . ? C55A C57A H57B 109.5 . . ? H57A C57A H57B 109.5 . . ? C55A C57A H57C 109.5 . . ? H57A C57A H57C 109.5 . . ? H57B C57A H57C 109.5 . . ? C55A C58A H58A 109.5 . . ? C55A C58A H58B 109.5 . . ? H58A C58A H58B 109.5 . . ? C55A C58A H58C 109.5 . . ? H58A C58A H58C 109.5 . . ? H58B C58A H58C 109.5 . . ? C60A C59A C61A 108.9(13) . . ? C60A C59A C62A 110.2(12) . . ? C61A C59A C62A 104.9(11) . . ? C60A C59A C53A 108.9(12) . . ? C61A C59A C53A 111.2(8) . . ? C62A C59A C53A 112.7(9) . . ? C59A C60A H60A 109.5 . . ? C59A C60A H60B 109.5 . . ? H60A C60A H60B 109.5 . . ? C59A C60A H60C 109.5 . . ? H60A C60A H60C 109.5 . . ? H60B C60A H60C 109.5 . . ? C59A C61A H61A 109.5 . . ? C59A C61A H61B 109.5 . . ? H61A C61A H61B 109.5 . . ? C59A C61A H61C 109.5 . . ? H61A C61A H61C 109.5 . . ? H61B C61A H61C 109.5 . . ? C59A C62A H62A 109.5 . . ? C59A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C59A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? N5A C63A C64A 120.9(7) . . ? N5A C63A C2A 119.2(7) . . ? C64A C63A C2A 119.9(7) . . ? C63A C64A C65A 120.2(8) . . ? C63A C64A H64A 119.9 . . ? C65A C64A H64A 119.9 . . ? C66A C65A C64A 119.6(8) . . ? C66A C65A H65A 120.2 . . ? C64A C65A H65A 120.2 . . ? C65A C66A C67A 118.0(8) . . ? C65A C66A H66A 121.0 . . ? C67A C66A H66A 121.0 . . ? N5A C67A C66A 124.5(9) . . ? N5A C67A H67A 117.7 . . ? C66A C67A H67A 117.7 . . ? N6A C68A C69A 120.2(7) . . ? N6A C68A C18A 121.2(7) . . ? C69A C68A C18A 118.6(8) . . ? C70A C69A C68A 121.0(8) . . ? C70A C69A H69A 119.5 . . ? C68A C69A H69A 119.5 . . ? C69A C70A C71A 118.2(8) . . ? C69A C70A H70A 120.9 . . ? C71A C70A H70A 120.9 . . ? C72A C71A C70A 118.4(7) . . ? C72A C71A H71A 120.8 . . ? C70A C71A H71A 120.8 . . ? N6A C72A C71A 124.1(9) . . ? N6A C72A H72A 118.0 . . ? C71A C72A H72A 118.0 . . ? C74A C73A C80A 116.3(8) . . ? C74A C73A Ir1 105.8(7) . . ? C80A C73A Ir1 108.0(6) . . ? C74A C73A H73A 109.0 . . ? C80A C73A H73A 108.7 . . ? Ir1 C73A H73A 108.7 . . ? O1 C74A C73A 122.0(11) . . ? O1 C74A C75A 122.2(10) . . ? C73A C74A C75A 115.5(11) . . ? C76A C75A C74A 109.5(11) . . ? C76A C75A H75A 109.6 . . ? C74A C75A H75A 109.6 . . ? C76A C75A H75B 109.9 . . ? C74A C75A H75B 110.1 . . ? H75A C75A H75B 108.2 . . ? C75A C76A C77A 123.1(12) . . ? C75A C76A Ir1 106.9(7) . . ? C77A C76A Ir1 65.6(5) . . ? C75A C76A H76A 116.6 . . ? C77A C76A H76A 116.3 . . ? Ir1 C76A H76A 116.3 . . ? C78A C77A C76A 122.3(10) . . ? C78A C77A Ir1 68.6(5) . . ? C76A C77A Ir1 75.4(6) . . ? C78A C77A H77A 118.6 . . ? C76A C77A H77A 117.9 . . ? Ir1 C77A H77A 118.4 . . ? C77A C78A C79A 123.3(9) . . ? C77A C78A Ir1 74.1(6) . . ? C79A C78A Ir1 111.1(6) . . ? C77A C78A H78A 113.9 . . ? C79A C78A H78A 113.9 . . ? Ir1 C78A H78A 113.9 . . ? C80A C79A C78A 112.8(8) . . ? C80A C79A H79A 109.0 . . ? C78A C79A H79A 109.1 . . ? C80A C79A H79B 109.1 . . ? C78A C79A H79B 108.9 . . ? H79A C79A H79B 107.8 . . ? C79A C80A C73A 112.4(8) . . ? C79A C80A H80A 109.1 . . ? C73A C80A H80A 108.9 . . ? C79A C80A H80B 109.2 . . ? C73A C80A H80B 109.3 . . ? H80A C80A H80B 107.9 . . ? N1B C1B C20B 125.9(6) . . ? N1B C1B C2B 110.9(6) . . ? C20B C1B C2B 122.8(6) . . ? C3B C2B C1B 105.8(6) . . ? C3B C2B C63B 126.7(7) . . ? C1B C2B C63B 127.2(7) . . ? C2B C3B C4B 107.6(6) . . ? C2B C3B H3B 126.2 . . ? C4B C3B H3B 126.2 . . ? N1B C4B C5B 124.2(6) . . ? N1B C4B C3B 109.8(6) . . ? C5B C4B C3B 125.3(6) . . ? C6B C5B C4B 120.2(6) . . ? C6B C5B C21B 117.3(6) . . ? C4B C5B C21B 122.1(6) . . ? N2B C6B C5B 125.4(6) . . ? N2B C6B C7B 109.3(6) . . ? C5B C6B C7B 124.8(6) . . ? C8B C7B C6B 107.1(6) . . ? C8B C7B H7B 126.5 . . ? C6B C7B H7B 126.5 . . ? C7B C8B C9B 107.1(6) . . ? C7B C8B H8B 126.4 . . ? C9B C8B H8B 126.4 . . ? N2B C9B C10B 124.9(6) . . ? N2B C9B C8B 110.3(6) . . ? C10B C9B C8B 124.4(6) . . ? C9B C10B C11B 120.4(6) . . ? C9B C10B C35B 119.5(6) . . ? C11B C10B C35B 120.1(6) . . ? N3B C11B C10B 124.3(6) . . ? N3B C11B C12B 110.3(6) . . ? C10B C11B C12B 125.0(6) . . ? C13B C12B C11B 107.3(6) . . ? C13B C12B H12B 126.4 . . ? C11B C12B H12B 126.4 . . ? C12B C13B C14B 107.2(6) . . ? C12B C13B H13B 126.4 . . ? C14B C13B H13B 126.4 . . ? N3B C14B C15B 124.9(6) . . ? N3B C14B C13B 109.2(6) . . ? C15B C14B C13B 125.5(6) . . ? C16B C15B C14B 120.8(6) . . ? C16B C15B C49B 120.1(6) . . ? C14B C15B C49B 119.0(6) . . ? N4B C16B C15B 124.0(6) . . ? N4B C16B C17B 108.8(6) . . ? C15B C16B C17B 127.0(7) . . ? C18B C17B C16B 107.7(6) . . ? C18B C17B H17B 126.1 . . ? C16B C17B H17B 126.1 . . ? C17B C18B C19B 106.8(6) . . ? C17B C18B C68B 127.0(7) . . ? C19B C18B C68B 125.1(7) . . ? N4B C19B C20B 125.8(6) . . ? N4B C19B C18B 110.0(6) . . ? C20B C19B C18B 123.5(6) . . ? C19B C20B C1B 116.2(6) . . ? C19B C20B Ir2 121.4(5) . . ? C1B C20B Ir2 122.4(5) . . ? C26B C21B C22B 118.5(6) . . ? C26B C21B C5B 119.9(6) . . ? C22B C21B C5B 121.3(6) . . ? C21B C22B C23B 122.4(7) . . ? C21B C22B H22B 118.8 . . ? C23B C22B H22B 118.8 . . ? C22B C23B C24B 117.1(7) . . ? C22B C23B C27B 121.6(7) . . ? C24B C23B C27B 121.1(7) . . ? C23B C24B C25B 122.7(7) . . ? C23B C24B H24B 118.7 . . ? C25B C24B H24B 118.7 . . ? C24B C25B C26B 117.3(7) . . ? C24B C25B C31B 121.0(7) . . ? C26B C25B C31B 121.7(7) . . ? C21B C26B C25B 122.0(7) . . ? C21B C26B H26B 119.0 . . ? C25B C26B H26B 119.0 . . ? C23B C27B C30B 112.2(7) . . ? C23B C27B C29B 113.1(7) . . ? C30B C27B C29B 107.2(8) . . ? C23B C27B C28B 107.4(7) . . ? C30B C27B C28B 107.7(8) . . ? C29B C27B C28B 109.1(8) . . ? C27B C28B H28D 109.5 . . ? C27B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C27B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C27B C30B H30D 109.5 . . ? C27B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C27B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C32T C31B C34B 59.7(15) . . ? C32T C31B C33B 141.5(15) . . ? C34B C31B C33B 113.0(13) . . ? C32T C31B C33T 105.6(19) . . ? C34B C31B C33T 142.2(15) . . ? C33B C31B C33T 54.8(15) . . ? C32T C31B C32B 52.0(14) . . ? C34B C31B C32B 108.8(12) . . ? C33B C31B C32B 107.7(12) . . ? C33T C31B C32B 55.8(15) . . ? C32T C31B C34T 107.3(17) . . ? C34B C31B C34T 54.8(13) . . ? C33B C31B C34T 58.8(14) . . ? C33T C31B C34T 106.8(17) . . ? C32B C31B C34T 131.8(12) . . ? C32T C31B C25B 112.2(13) . . ? C34B C31B C25B 108.0(9) . . ? C33B C31B C25B 105.9(10) . . ? C33T C31B C25B 109.7(13) . . ? C32B C31B C25B 113.5(9) . . ? C34T C31B C25B 114.7(11) . . ? C31B C32B H32D 109.5 . . ? C31B C32B H32E 109.5 . . ? C31B C32B H32F 109.5 . . ? C31B C33B H33D 109.5 . . ? C31B C33B H33E 109.5 . . ? C31B C33B H33F 109.5 . . ? C31B C34B H34D 109.5 . . ? C31B C34B H34E 109.5 . . ? C31B C34B H34F 109.5 . . ? C40B C35B C36B 118.9(6) . . ? C40B C35B C10B 124.6(6) . . ? C36B C35B C10B 116.5(6) . . ? C38B C37B C36B 117.2(7) . . ? C38B C37B C41B 123.7(7) . . ? C36B C37B C41B 119.0(7) . . ? C39B C38B C37B 122.5(7) . . ? C39B C38B H38B 118.8 . . ? C37B C38B H38B 118.8 . . ? C38B C39B C40B 118.6(7) . . ? C38B C39B C45B 120.3(7) . . ? C40B C39B C45B 121.1(7) . . ? C35B C40B C39B 121.2(7) . . ? C35B C40B H40B 119.4 . . ? C39B C40B H40B 119.4 . . ? C43B C41B C42B 111.3(10) . . ? C43B C41B C44B 107.5(9) . . ? C42B C41B C44B 108.4(8) . . ? C43B C41B C37B 110.8(8) . . ? C42B C41B C37B 107.1(8) . . ? C44B C41B C37B 111.7(8) . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C41B C43B H43D 109.5 . . ? C41B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C41B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C41B C44B H44D 109.5 . . ? C41B C44B H44E 109.5 . . ? H44D C44B H44E 109.5 . . ? C41B C44B H44F 109.5 . . ? H44D C44B H44F 109.5 . . ? H44E C44B H44F 109.5 . . ? C46B C45B C48B 114.1(12) . . ? C46B C45B C47B 109.1(12) . . ? C48B C45B C47B 100.7(11) . . ? C46B C45B C39B 109.9(10) . . ? C48B C45B C39B 110.5(9) . . ? C47B C45B C39B 112.3(9) . . ? C45B C46B H46D 109.5 . . ? C45B C46B H46E 109.0 . . ? H46D C46B H46E 109.5 . . ? C45B C46B H46F 109.9 . . ? H46D C46B H46F 109.5 . . ? H46E C46B H46F 109.5 . . ? C45B C47B H47D 109.5 . . ? C45B C47B H47E 109.5 . . ? H47D C47B H47E 109.5 . . ? C45B C47B H47F 109.5 . . ? H47D C47B H47F 109.5 . . ? H47E C47B H47F 109.5 . . ? C45B C48B H48D 109.5 . . ? C45B C48B H48E 109.5 . . ? H48D C48B H48E 109.5 . . ? C45B C48B H48F 109.5 . . ? H48D C48B H48F 109.5 . . ? H48E C48B H48F 109.5 . . ? C50B C49B C54B 119.4(7) . . ? C50B C49B C15B 122.4(6) . . ? C54B C49B C15B 118.2(6) . . ? C49B C50B C51B 121.8(7) . . ? C49B C50B H50B 119.1 . . ? C51B C50B H50B 119.1 . . ? C50B C51B C52B 117.5(7) . . ? C50B C51B C55B 121.4(7) . . ? C52B C51B C55B 121.0(7) . . ? C51B C52B C53B 122.1(7) . . ? C51B C52B H52B 118.9 . . ? C53B C52B H52B 118.9 . . ? C54B C53B C52B 118.7(7) . . ? C54B C53B C59B 122.0(7) . . ? C52B C53B C59B 119.2(7) . . ? C53B C54B C49B 120.5(7) . . ? C53B C54B H54B 119.7 . . ? C49B C54B H54B 119.7 . . ? C56B C55B C58B 110.0(11) . . ? C56B C55B C51B 111.3(9) . . ? C58B C55B C51B 112.0(8) . . ? C56B C55B C57B 112.4(11) . . ? C58B C55B C57B 103.9(9) . . ? C51B C55B C57B 107.0(8) . . ? C55B C56B H56D 109.5 . . ? C55B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C55B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? C55B C57B H57D 109.5 . . ? C55B C57B H57E 109.5 . . ? H57D C57B H57E 109.5 . . ? C55B C57B H57F 109.5 . . ? H57D C57B H57F 109.5 . . ? H57E C57B H57F 109.5 . . ? C55B C58B H58D 109.5 . . ? C55B C58B H58E 109.5 . . ? H58D C58B H58E 109.5 . . ? C55B C58B H58F 109.5 . . ? H58D C58B H58F 109.5 . . ? H58E C58B H58F 109.5 . . ? C61B C59B C62B 107.8(9) . . ? C61B C59B C60B 110.7(10) . . ? C62B C59B C60B 108.2(9) . . ? C61B C59B C53B 112.6(7) . . ? C62B C59B C53B 109.6(7) . . ? C60B C59B C53B 107.8(8) . . ? C59B C60B H60D 109.5 . . ? C59B C60B H60E 109.5 . . ? H60D C60B H60E 109.5 . . ? C59B C60B H60F 109.5 . . ? H60D C60B H60F 109.5 . . ? H60E C60B H60F 109.5 . . ? C59B C61B H61D 109.5 . . ? C59B C61B H61E 109.5 . . ? H61D C61B H61E 109.5 . . ? C59B C61B H61F 109.5 . . ? H61D C61B H61F 109.5 . . ? H61E C61B H61F 109.5 . . ? C59B C62B H62D 109.5 . . ? C59B C62B H62E 109.5 . . ? H62D C62B H62E 109.5 . . ? C59B C62B H62F 109.5 . . ? H62D C62B H62F 109.5 . . ? H62E C62B H62F 109.5 . . ? N5B C63B C64B 119.9(7) . . ? N5B C63B C2B 121.2(7) . . ? C64B C63B C2B 118.9(7) . . ? C65B C64B C63B 121.2(8) . . ? C65B C64B H64B 119.4 . . ? C63B C64B H64B 119.4 . . ? C66B C65B C64B 117.2(8) . . ? C66B C65B H65B 121.4 . . ? C64B C65B H65B 121.4 . . ? C67B C66B C65B 119.9(7) . . ? C67B C66B H66B 120.1 . . ? C65B C66B H66B 120.1 . . ? C66B C67B N5B 123.7(8) . . ? C66B C67B H67B 118.1 . . ? N5B C67B H67B 118.1 . . ? N6B C68B C69B 119.6(6) . . ? N6B C68B C18B 122.1(6) . . ? C69B C68B C18B 118.2(7) . . ? C70B C69B C68B 121.3(8) . . ? C70B C69B H69B 119.3 . . ? C68B C69B H69B 119.3 . . ? C69B C70B C71B 118.5(7) . . ? C69B C70B H70B 120.7 . . ? C71B C70B H70B 120.7 . . ? C72B C71B C70B 118.6(7) . . ? C72B C71B H71B 120.7 . . ? C70B C71B H71B 120.7 . . ? N6B C72B C71B 123.7(8) . . ? N6B C72B H72B 118.2 . . ? C71B C72B H72B 118.2 . . ? C74B C73B C80B 118.4(8) . . ? C74B C73B Ir2 105.9(7) . . ? C80B C73B Ir2 108.3(6) . . ? C74B C73B H73B 107.9 . . ? C80B C73B H73B 108.0 . . ? Ir2 C73B H73B 107.9 . . ? O2 C74B C73B 124.2(11) . . ? O2 C74B C75B 117.1(10) . . ? C73B C74B C75B 118.6(10) . . ? C76B C75B C74B 107.9(9) . . ? C76B C75B H75C 109.8 . . ? C74B C75B H75C 110.0 . . ? C76B C75B H75D 110.3 . . ? C74B C75B H75D 110.3 . . ? H75C C75B H75D 108.5 . . ? C77B C76B C75B 126.7(10) . . ? C77B C76B Ir2 66.5(4) . . ? C75B C76B Ir2 107.0(7) . . ? C77B C76B H76B 115.1 . . ? C75B C76B H76B 114.8 . . ? Ir2 C76B H76B 115.0 . . ? C78B C77B C76B 121.8(9) . . ? C78B C77B Ir2 67.1(4) . . ? C76B C77B Ir2 75.8(6) . . ? C78B C77B H77B 118.6 . . ? C76B C77B H77B 118.2 . . ? Ir2 C77B H77B 118.5 . . ? C77B C78B C79B 120.3(9) . . ? C77B C78B Ir2 74.5(5) . . ? C79B C78B Ir2 111.5(6) . . ? C77B C78B H78B 114.7 . . ? C79B C78B H78B 114.7 . . ? Ir2 C78B H78B 114.6 . . ? C80B C79B C78B 111.0(7) . . ? C80B C79B H79C 109.4 . . ? C78B C79B H79C 109.4 . . ? C80B C79B H79D 109.5 . . ? C78B C79B H79D 109.4 . . ? H79C C79B H79D 108.0 . . ? C79B C80B C73B 110.2(7) . . ? C79B C80B H80C 109.6 . . ? C73B C80B H80C 109.6 . . ? C79B C80B H80D 109.6 . . ? C73B C80B H80D 109.7 . . ? H80C C80B H80D 108.2 . . ? N1S C1S C2S 179(2) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.8 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? N2S C3S C4S 177.4(19) . . ? C3S C4S H4S1 109.4 . . ? C3S C4S H4S2 109.7 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.3 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? N3S C5S C6S 166(3) . . ? C5S C6S H6S1 109.6 . . ? C5S C6S H6S2 109.1 . . ? H6S1 C6S H6S2 109.5 . . ? C5S C6S H6S3 109.7 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? N4S C7S C8S 178(3) . . ? C7S C8S H8S1 109.7 . . ? C7S C8S H8S2 109.2 . . ? H8S1 C8S H8S2 109.5 . . ? C7S C8S H8S3 109.5 . . ? H8S1 C8S H8S3 109.5 . . ? H8S2 C8S H8S3 109.5 . . ? N5S C9S C10S 171(6) . . ? C9S C10S H10A 109.3 . . ? C9S C10S H10B 109.6 . . ? H10A C10S H10B 109.5 . . ? C9S C10S H10C 109.4 . . ? H10A C10S H10C 109.5 . . ? H10B C10S H10C 109.5 . . ? C31B C32T H32G 109.5 . . ? C31B C32T H32H 109.5 . . ? C31B C32T H32I 109.5 . . ? C31B C33T H33G 109.5 . . ? C31B C33T H33H 109.5 . . ? C31B C33T H33I 109.5 . . ? C31B C34T H34G 109.5 . . ? C31B C34T H34H 109.5 . . ? C31B C34T H34I 109.5 . . ? C20A Ir1 C73A 90.0(3) . . ? C20A Ir1 N5A 88.1(3) . . ? C73A Ir1 N5A 87.7(3) . . ? C20A Ir1 C78A 98.8(3) . . ? C73A Ir1 C78A 82.8(3) . . ? N5A Ir1 C78A 168.2(3) . . ? C20A Ir1 N6A 88.1(3) . . ? C73A Ir1 N6A 175.3(3) . . ? N5A Ir1 N6A 96.6(2) . . ? C78A Ir1 N6A 93.2(3) . . ? C20A Ir1 C77A 133.3(4) . . ? C73A Ir1 C77A 96.5(4) . . ? N5A Ir1 C77A 138.1(3) . . ? C78A Ir1 C77A 37.3(3) . . ? N6A Ir1 C77A 81.7(3) . . ? C20A Ir1 C76A 165.1(4) . . ? C73A Ir1 C76A 79.8(4) . . ? N5A Ir1 C76A 102.2(4) . . ? C78A Ir1 C76A 69.3(4) . . ? N6A Ir1 C76A 101.2(3) . . ? C77A Ir1 C76A 39.0(5) . . ? C20B Ir2 C73B 89.8(3) . . ? C20B Ir2 C78B 98.7(3) . . ? C73B Ir2 C78B 82.7(3) . . ? C20B Ir2 N5B 88.5(3) . . ? C73B Ir2 N5B 87.4(3) . . ? C78B Ir2 N5B 167.7(3) . . ? C20B Ir2 N6B 88.4(3) . . ? C73B Ir2 N6B 175.1(3) . . ? C78B Ir2 N6B 93.1(3) . . ? N5B Ir2 N6B 97.2(2) . . ? C20B Ir2 C77B 134.5(3) . . ? C73B Ir2 C77B 96.2(3) . . ? C78B Ir2 C77B 38.4(3) . . ? N5B Ir2 C77B 136.7(3) . . ? N6B Ir2 C77B 81.9(3) . . ? C20B Ir2 C76B 164.7(3) . . ? C73B Ir2 C76B 79.7(3) . . ? C78B Ir2 C76B 69.2(4) . . ? N5B Ir2 C76B 102.0(4) . . ? N6B Ir2 C76B 101.2(3) . . ? C77B Ir2 C76B 37.7(4) . . ? C4A N1A C1A 105.9(6) . . ? C4A N1A Ni1 128.0(5) . . ? C1A N1A Ni1 126.1(5) . . ? C9A N2A C6A 106.3(6) . . ? C9A N2A Ni1 126.7(5) . . ? C6A N2A Ni1 127.0(4) . . ? C11A N3A C14A 105.5(6) . . ? C11A N3A Ni1 127.2(5) . . ? C14A N3A Ni1 127.3(5) . . ? C19A N4A C16A 105.9(6) . . ? C19A N4A Ni1 126.4(5) . . ? C16A N4A Ni1 127.5(5) . . ? C67A N5A C63A 116.7(7) . . ? C67A N5A Ir1 117.2(6) . . ? C63A N5A Ir1 124.3(5) . . ? C68A N6A C72A 118.1(7) . . ? C68A N6A Ir1 123.7(5) . . ? C72A N6A Ir1 118.2(6) . . ? C1B N1B C4B 105.7(5) . . ? C1B N1B Ni2 126.3(5) . . ? C4B N1B Ni2 127.9(4) . . ? C9B N2B C6B 105.9(5) . . ? C9B N2B Ni2 126.6(5) . . ? C6B N2B Ni2 127.5(4) . . ? C11B N3B C14B 105.7(6) . . ? C11B N3B Ni2 126.9(5) . . ? C14B N3B Ni2 127.4(4) . . ? C19B N4B C16B 106.3(5) . . ? C19B N4B Ni2 126.2(5) . . ? C16B N4B Ni2 127.3(4) . . ? C63B N5B C67B 118.0(7) . . ? C63B N5B Ir2 123.3(5) . . ? C67B N5B Ir2 116.7(6) . . ? C72B N6B C68B 118.2(6) . . ? C72B N6B Ir2 119.0(5) . . ? C68B N6B Ir2 122.7(4) . . ? N3A Ni1 N2A 90.1(2) . . ? N3A Ni1 N1A 178.1(2) . . ? N2A Ni1 N1A 89.7(2) . . ? N3A Ni1 N4A 89.8(3) . . ? N2A Ni1 N4A 179.5(3) . . ? N1A Ni1 N4A 90.4(2) . . ? N1B Ni2 N2B 89.6(2) . . ? N1B Ni2 N3B 178.7(2) . . ? N2B Ni2 N3B 90.6(2) . . ? N1B Ni2 N4B 90.3(2) . . ? N2B Ni2 N4B 179.4(2) . . ? N3B Ni2 N4B 89.5(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.639 _refine_diff_density_min -7.020 _refine_diff_density_rms 0.189 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 367 138 ' ' 2 -0.008 0.622 0.400 369 126 ' ' 3 0.011 0.378 0.600 369 127 ' ' 4 0.139 0.469 0.966 10 3 ' ' 5 0.498 0.919 0.153 25 11 ' ' 6 0.502 0.081 0.846 26 9 ' ' 7 0.860 0.531 0.034 10 3 ' ' _platon_squeeze_details ; ;