# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Chi, Yun' 'Chou, Pi-Tai' _publ_contact_author_name 'Chi, Yun' _publ_contact_author_email ychi@mx.nthu.edu.tw _publ_section_title ; Heteroleptic Ir(III) Complexes Containing both Azolate Chromophoric Chelate and Diphenylphosphinoaryl Cyclometalates; Reactivities, Electronic Properties and Applications ; # Attachment '- xray-1_3_6a_6b_7a-NEW.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 787571' #TrackingRef '- xray-1_3_6a_6b_7a-NEW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H32 Cl2 Ir P S2' _chemical_formula_weight 750.75 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.4024(1) _cell_length_b 15.6941(2) _cell_length_c 18.7797(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2771.17(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13480 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 5.239 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.441 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13480 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6254 _reflns_number_gt 5553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(4) _refine_ls_number_reflns 6254 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0461 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.005 _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 Ir Ir 0.295550(13) 0.495692(9) 0.870757(6) 0.01756(4) Uani 1 1 d . . . Cl1 Cl 0.18512(11) 0.41341(6) 0.77241(5) 0.0264(2) Uani 1 1 d . . . Cl2 Cl 0.18088(11) 0.39639(6) 0.95143(5) 0.0272(2) Uani 1 1 d . . . S1 S 0.11011(10) 0.59572(6) 0.88085(5) 0.0228(2) Uani 1 1 d . . . S2 S 0.49515(10) 0.40573(6) 0.87100(5) 0.0235(2) Uani 1 1 d . . . P1 P 0.40718(11) 0.58755(6) 0.79783(5) 0.0176(2) Uani 1 1 d . . . C1 C 0.3901(4) 0.5654(2) 0.95023(18) 0.0211(9) Uani 1 1 d . . . C2 C 0.3698(4) 0.5506(2) 1.02270(17) 0.0223(9) Uani 1 1 d . . . H2 H 0.3047 0.5077 1.0373 0.027 Uiso 1 1 calc R . . C3 C 0.4441(4) 0.5979(2) 1.07516(19) 0.0266(9) Uani 1 1 d . . . H3 H 0.4297 0.5851 1.1241 0.032 Uiso 1 1 calc R . . C4 C 0.5351(4) 0.6612(2) 1.05692(19) 0.0259(9) Uani 1 1 d . . . H4 H 0.5835 0.6922 1.0929 0.031 Uiso 1 1 calc R . . C5 C 0.5581(4) 0.6811(2) 0.9844(2) 0.0218(9) Uani 1 1 d . . . C6 C 0.4850(4) 0.6336(2) 0.93139(18) 0.0174(8) Uani 1 1 d . . . C7 C 0.5024(4) 0.6564(2) 0.85874(18) 0.0192(8) Uani 1 1 d . . . C8 C 0.5859(4) 0.7258(2) 0.84035(19) 0.0253(9) Uani 1 1 d . . . H8 H 0.5917 0.7433 0.7920 0.030 Uiso 1 1 calc R . . C9 C 0.6615(4) 0.7702(2) 0.8925(2) 0.0298(10) Uani 1 1 d . . . H9 H 0.7209 0.8166 0.8793 0.036 Uiso 1 1 calc R . . C10 C 0.6503(5) 0.7471(3) 0.9625(2) 0.0289(10) Uani 1 1 d . . . H10 H 0.7059 0.7761 0.9971 0.035 Uiso 1 1 calc R . . C11 C 0.5337(4) 0.5464(2) 0.73217(18) 0.0205(9) Uani 1 1 d . . . C12 C 0.5046(5) 0.4708(2) 0.69688(19) 0.0295(10) Uani 1 1 d . . . H12 H 0.4223 0.4389 0.7093 0.035 Uiso 1 1 calc R . . C13 C 0.5938(5) 0.4411(2) 0.6436(2) 0.0335(10) Uani 1 1 d . . . H13 H 0.5720 0.3892 0.6199 0.040 Uiso 1 1 calc R . . C14 C 0.7136(4) 0.4859(3) 0.62477(19) 0.0318(10) Uani 1 1 d . . . H14 H 0.7740 0.4657 0.5879 0.038 Uiso 1 1 calc R . . C15 C 0.7452(4) 0.5610(3) 0.6602(2) 0.0371(12) Uani 1 1 d . . . H15 H 0.8282 0.5922 0.6478 0.045 Uiso 1 1 calc R . . C16 C 0.6568(4) 0.5909(2) 0.71340(19) 0.0271(9) Uani 1 1 d . . . H16 H 0.6800 0.6423 0.7375 0.032 Uiso 1 1 calc R . . C17 C 0.2917(4) 0.6564(2) 0.74491(17) 0.0198(8) Uani 1 1 d . . . C18 C 0.2374(4) 0.6269(3) 0.68037(19) 0.0252(10) Uani 1 1 d . . . H18 H 0.2689 0.5740 0.6615 0.030 Uiso 1 1 calc R . . C19 C 0.1383(4) 0.6745(3) 0.6440(2) 0.0314(10) Uani 1 1 d . . . H19 H 0.1021 0.6542 0.6000 0.038 Uiso 1 1 calc R . . C20 C 0.0905(5) 0.7515(3) 0.6707(2) 0.0322(11) Uani 1 1 d . . . H20 H 0.0206 0.7833 0.6456 0.039 Uiso 1 1 calc R . . C21 C 0.1452(5) 0.7819(3) 0.7342(2) 0.0311(10) Uani 1 1 d . . . H21 H 0.1142 0.8352 0.7525 0.037 Uiso 1 1 calc R . . C22 C 0.2452(4) 0.7344(3) 0.7711(2) 0.0244(10) Uani 1 1 d . . . H22 H 0.2824 0.7554 0.8147 0.029 Uiso 1 1 calc R . . C23 C -0.0326(4) 0.5718(3) 0.8195(2) 0.0317(10) Uani 1 1 d . . . H23A H -0.0926 0.6226 0.8113 0.038 Uiso 1 1 calc R . . H23B H 0.0056 0.5518 0.7733 0.038 Uiso 1 1 calc R . . C24 C -0.1169(4) 0.5019(3) 0.8558(2) 0.0422(10) Uani 1 1 d . . . H24A H -0.2125 0.4973 0.8340 0.051 Uiso 1 1 calc R . . H24B H -0.0678 0.4465 0.8500 0.051 Uiso 1 1 calc R . . C25 C -0.1305(5) 0.5232(3) 0.9338(2) 0.0407(12) Uani 1 1 d . . . H25A H -0.1388 0.4700 0.9618 0.049 Uiso 1 1 calc R . . H25B H -0.2175 0.5574 0.9417 0.049 Uiso 1 1 calc R . . C26 C -0.0018(5) 0.5729(3) 0.95848(19) 0.0282(10) Uani 1 1 d . . . H26A H 0.0524 0.5393 0.9938 0.034 Uiso 1 1 calc R . . H26B H -0.0322 0.6268 0.9812 0.034 Uiso 1 1 calc R . . C27 C 0.4460(5) 0.2933(2) 0.8580(2) 0.0358(11) Uani 1 1 d . . . H27A H 0.3443 0.2887 0.8450 0.043 Uiso 1 1 calc R . . H27B H 0.5037 0.2679 0.8194 0.043 Uiso 1 1 calc R . . C28 C 0.4740(5) 0.2474(2) 0.9280(2) 0.0363(11) Uani 1 1 d . . . H28A H 0.5023 0.1876 0.9190 0.044 Uiso 1 1 calc R . . H28B H 0.3872 0.2473 0.9579 0.044 Uiso 1 1 calc R . . C29 C 0.5936(5) 0.2951(2) 0.9657(2) 0.0303(10) Uani 1 1 d . . . H29A H 0.6031 0.2757 1.0156 0.036 Uiso 1 1 calc R . . H29B H 0.6853 0.2862 0.9409 0.036 Uiso 1 1 calc R . . C30 C 0.5499(4) 0.3875(2) 0.96275(19) 0.0274(10) Uani 1 1 d . . . H30A H 0.6307 0.4250 0.9755 0.033 Uiso 1 1 calc R . . H30B H 0.4703 0.3987 0.9959 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.01761(7) 0.01688(7) 0.01820(7) 0.00054(8) 0.00044(6) -0.00173(9) Cl1 0.0261(6) 0.0261(5) 0.0271(5) -0.0042(4) -0.0024(5) -0.0069(5) Cl2 0.0281(6) 0.0226(5) 0.0308(5) 0.0059(4) 0.0050(5) -0.0039(5) S1 0.0195(5) 0.0229(5) 0.0259(5) 0.0013(4) 0.0021(5) 0.0008(4) S2 0.0234(5) 0.0231(5) 0.0240(5) 0.0041(5) 0.0030(5) 0.0040(4) P1 0.0178(5) 0.0174(5) 0.0177(5) 0.0002(4) -0.0004(4) 0.0002(4) C1 0.022(2) 0.022(2) 0.0201(19) -0.0035(16) 0.0014(18) 0.0130(19) C2 0.023(2) 0.019(2) 0.024(2) 0.0023(16) 0.0026(18) 0.0031(18) C3 0.032(2) 0.030(2) 0.0185(19) -0.0017(18) -0.0007(18) 0.012(2) C4 0.025(2) 0.030(2) 0.022(2) -0.0099(17) -0.0093(19) 0.011(2) C5 0.019(2) 0.021(2) 0.026(2) -0.0030(17) -0.0008(18) 0.0052(18) C6 0.017(2) 0.014(2) 0.0210(19) 0.0006(16) -0.0025(18) -0.0003(17) C7 0.021(2) 0.0158(19) 0.021(2) -0.0005(16) -0.0035(18) 0.0000(16) C8 0.027(2) 0.025(2) 0.024(2) 0.0007(17) -0.0018(19) -0.0001(19) C9 0.028(2) 0.022(2) 0.039(2) -0.0015(19) -0.003(2) -0.0088(18) C10 0.026(2) 0.028(2) 0.033(2) -0.0111(19) -0.011(2) 0.004(2) C11 0.026(2) 0.018(2) 0.0178(19) 0.0000(16) -0.0022(18) 0.0016(18) C12 0.032(2) 0.026(2) 0.031(2) -0.0010(18) 0.007(2) -0.0009(19) C13 0.041(3) 0.028(2) 0.031(2) -0.0063(19) 0.003(2) 0.004(2) C14 0.027(2) 0.039(3) 0.030(2) 0.000(2) 0.009(2) 0.011(2) C15 0.024(3) 0.050(3) 0.037(3) 0.003(2) 0.009(2) -0.0013(19) C16 0.022(2) 0.027(2) 0.032(2) 0.0010(18) -0.0011(19) -0.0041(18) C17 0.0182(19) 0.019(2) 0.0223(19) 0.0028(15) 0.0034(19) -0.0042(19) C18 0.027(2) 0.024(2) 0.025(2) 0.0001(17) -0.0051(18) 0.0018(17) C19 0.035(3) 0.032(2) 0.028(2) -0.0020(19) -0.006(2) 0.000(2) C20 0.028(2) 0.037(3) 0.032(2) 0.012(2) -0.009(2) 0.005(2) C21 0.030(3) 0.031(2) 0.031(2) -0.0003(19) -0.001(2) 0.006(2) C22 0.024(2) 0.025(2) 0.024(2) 0.0020(17) 0.0023(17) -0.0001(16) C23 0.026(2) 0.036(3) 0.033(2) 0.0045(19) -0.003(2) 0.004(2) C24 0.025(2) 0.048(3) 0.053(2) 0.001(3) -0.0077(19) -0.020(3) C25 0.034(3) 0.047(3) 0.041(2) -0.001(2) 0.008(2) -0.005(2) C26 0.029(2) 0.029(2) 0.027(2) -0.0024(18) 0.008(2) 0.000(2) C27 0.047(3) 0.022(2) 0.038(2) -0.009(2) -0.005(2) 0.008(2) C28 0.045(3) 0.023(2) 0.041(2) 0.007(2) 0.001(2) 0.005(2) C29 0.035(3) 0.027(2) 0.029(2) 0.0030(18) 0.002(2) 0.011(2) C30 0.029(2) 0.027(2) 0.026(2) -0.0010(18) -0.0058(19) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir C1 2.053(4) . ? Ir P1 2.2485(10) . ? Ir S2 2.3485(9) . ? Ir S1 2.3538(9) . ? Ir Cl2 2.4263(9) . ? Ir Cl1 2.4813(9) . ? S1 C23 1.808(4) . ? S1 C26 1.833(4) . ? S2 C30 1.821(4) . ? S2 C27 1.840(4) . ? P1 C7 1.810(4) . ? P1 C17 1.825(4) . ? P1 C11 1.831(4) . ? C1 C2 1.394(5) . ? C1 C6 1.438(5) . ? C2 C3 1.418(5) . ? C3 C4 1.354(5) . ? C4 C5 1.413(5) . ? C5 C10 1.412(5) . ? C5 C6 1.422(5) . ? C6 C7 1.420(5) . ? C7 C8 1.387(5) . ? C8 C9 1.396(5) . ? C9 C10 1.367(5) . ? C11 C12 1.386(5) . ? C11 C16 1.398(5) . ? C12 C13 1.386(5) . ? C13 C14 1.374(5) . ? C14 C15 1.386(6) . ? C15 C16 1.381(5) . ? C17 C22 1.391(5) . ? C17 C18 1.394(5) . ? C18 C19 1.376(5) . ? C19 C20 1.382(5) . ? C20 C21 1.384(5) . ? C21 C22 1.386(5) . ? C23 C24 1.516(5) . ? C24 C25 1.508(5) . ? C25 C26 1.512(6) . ? C27 C28 1.522(5) . ? C28 C29 1.524(6) . ? C29 C30 1.509(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 C1 Ir P1 84.20(11) . . ? C1 Ir S2 88.45(10) . . ? P1 Ir S2 90.78(4) . . ? C1 Ir S1 84.65(10) . . ? P1 Ir S1 88.12(3) . . ? S2 Ir S1 173.09(3) . . ? C1 Ir Cl2 94.63(11) . . ? P1 Ir Cl2 178.44(4) . . ? S2 Ir Cl2 88.15(3) . . ? S1 Ir Cl2 92.81(3) . . ? C1 Ir Cl1 178.52(11) . . ? P1 Ir Cl1 94.34(3) . . ? S2 Ir Cl1 91.32(3) . . ? S1 Ir Cl1 95.57(3) . . ? Cl2 Ir Cl1 86.82(3) . . ? C23 S1 C26 92.30(19) . . ? C23 S1 Ir 111.09(14) . . ? C26 S1 Ir 111.04(14) . . ? C30 S2 C27 92.62(18) . . ? C30 S2 Ir 108.80(13) . . ? C27 S2 Ir 112.05(15) . . ? C7 P1 C17 106.57(16) . . ? C7 P1 C11 108.36(18) . . ? C17 P1 C11 103.21(16) . . ? C7 P1 Ir 103.21(12) . . ? C17 P1 Ir 115.67(13) . . ? C11 P1 Ir 119.14(12) . . ? C2 C1 C6 116.7(3) . . ? C2 C1 Ir 124.2(3) . . ? C6 C1 Ir 119.1(3) . . ? C1 C2 C3 121.6(4) . . ? C4 C3 C2 121.3(3) . . ? C3 C4 C5 120.2(4) . . ? C10 C5 C4 122.5(4) . . ? C10 C5 C6 118.5(3) . . ? C4 C5 C6 119.0(4) . . ? C7 C6 C5 119.1(3) . . ? C7 C6 C1 119.7(3) . . ? C5 C6 C1 121.2(3) . . ? C8 C7 C6 120.1(3) . . ? C8 C7 P1 126.3(3) . . ? C6 C7 P1 113.6(3) . . ? C7 C8 C9 120.4(3) . . ? C10 C9 C8 120.2(4) . . ? C9 C10 C5 121.5(4) . . ? C12 C11 C16 118.1(4) . . ? C12 C11 P1 119.7(3) . . ? C16 C11 P1 122.1(3) . . ? C11 C12 C13 120.9(4) . . ? C14 C13 C12 120.7(4) . . ? C13 C14 C15 119.2(4) . . ? C16 C15 C14 120.5(4) . . ? C15 C16 C11 120.7(4) . . ? C22 C17 C18 119.0(3) . . ? C22 C17 P1 121.0(3) . . ? C18 C17 P1 119.7(3) . . ? C19 C18 C17 119.9(4) . . ? C18 C19 C20 121.0(4) . . ? C19 C20 C21 119.5(4) . . ? C20 C21 C22 119.8(4) . . ? C21 C22 C17 120.7(4) . . ? C24 C23 S1 104.6(3) . . ? C25 C24 C23 108.7(4) . . ? C24 C25 C26 110.1(3) . . ? C25 C26 S1 108.4(3) . . ? C28 C27 S2 107.2(3) . . ? C27 C28 C29 107.2(3) . . ? C30 C29 C28 104.7(3) . . ? C29 C30 S2 105.2(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.117 _refine_diff_density_min -1.229 _refine_diff_density_rms 0.114 data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 787572' #TrackingRef '- xray-1_3_6a_6b_7a-NEW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C89 H72 Cl14 Ir2 N4 P4' _chemical_formula_weight 2202.09 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.5529(4) _cell_length_b 14.1688(3) _cell_length_c 29.0378(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.3146(12) _cell_angle_gamma 90.00 _cell_volume 8663.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 55017 _cell_measurement_theta_min 1.44 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4344 _exptl_absorpt_coefficient_mu 3.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.489 _exptl_absorpt_correction_T_max 0.777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55017 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 27.50 _reflns_number_total 19863 _reflns_number_gt 13220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^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 19863 _refine_ls_number_parameters 1002 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1337 _refine_ls_wR_factor_gt 0.1208 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.181861(11) 0.596760(18) 0.332851(8) 0.02011(7) Uani 1 1 d . . . Cl1 Cl 0.11336(7) 0.49141(11) 0.28016(6) 0.0260(4) Uani 1 1 d . . . Cl2 Cl 0.24287(8) 0.46086(11) 0.37069(5) 0.0271(4) Uani 1 1 d . . . P1 P 0.11571(8) 0.61259(12) 0.38287(6) 0.0221(4) Uani 1 1 d . . . P2 P 0.25973(8) 0.70330(12) 0.36053(6) 0.0237(4) Uani 1 1 d . . . N1 N 0.0236(3) 0.7521(4) 0.3788(2) 0.0288(13) Uani 1 1 d . . . N2 N 0.2498(2) 0.6026(4) 0.28942(18) 0.0212(12) Uani 1 1 d . . . C1 C 0.1287(3) 0.7035(4) 0.2967(2) 0.0219(14) Uani 1 1 d . . . C2 C 0.1362(3) 0.7343(4) 0.2531(2) 0.0280(16) Uani 1 1 d . . . H2 H 0.1683 0.7067 0.2395 0.034 Uiso 1 1 calc R . . C3 C 0.0968(3) 0.8069(5) 0.2277(2) 0.0345(18) Uani 1 1 d . . . H3 H 0.1030 0.8264 0.1977 0.041 Uiso 1 1 calc R . . C4 C 0.0495(3) 0.8492(5) 0.2467(2) 0.0311(16) Uani 1 1 d . . . H4 H 0.0232 0.8970 0.2298 0.037 Uiso 1 1 calc R . . C5 C 0.0413(3) 0.8195(5) 0.2916(2) 0.0261(15) Uani 1 1 d . . . C6 C 0.0793(3) 0.7456(4) 0.3144(2) 0.0235(14) Uani 1 1 d . . . C7 C 0.0665(3) 0.7139(5) 0.3578(2) 0.0251(15) Uani 1 1 d . . . C8 C -0.0105(3) 0.8248(5) 0.3560(2) 0.0355(18) Uani 1 1 d . . . H8 H -0.0411 0.8539 0.3705 0.043 Uiso 1 1 calc R . . C9 C -0.0037(3) 0.8594(5) 0.3130(2) 0.0302(16) Uani 1 1 d . . . H9 H -0.0296 0.9099 0.2983 0.036 Uiso 1 1 calc R . . C10 C 0.1493(3) 0.6392(5) 0.4446(2) 0.0262(15) Uani 1 1 d . . . C11 C 0.2087(3) 0.6035(5) 0.4656(2) 0.0288(16) Uani 1 1 d . . . H11 H 0.2324 0.5681 0.4474 0.035 Uiso 1 1 calc R . . C12 C 0.2331(3) 0.6195(5) 0.5124(2) 0.0331(17) Uani 1 1 d . . . H12 H 0.2744 0.5972 0.5263 0.040 Uiso 1 1 calc R . . C13 C 0.1981(4) 0.6680(5) 0.5397(3) 0.0369(18) Uani 1 1 d . . . H13 H 0.2151 0.6770 0.5724 0.044 Uiso 1 1 calc R . . C14 C 0.1394(4) 0.7028(5) 0.5199(3) 0.043(2) Uani 1 1 d . . . H14 H 0.1156 0.7358 0.5389 0.052 Uiso 1 1 calc R . . C15 C 0.1145(3) 0.6901(5) 0.4724(2) 0.0358(18) Uani 1 1 d . . . H15 H 0.0740 0.7155 0.4585 0.043 Uiso 1 1 calc R . . C16 C 0.0625(3) 0.5146(5) 0.3883(2) 0.0252(15) Uani 1 1 d . . . C17 C 0.0814(3) 0.4241(5) 0.3812(2) 0.0326(17) Uani 1 1 d . . . H17 H 0.1211 0.4131 0.3729 0.039 Uiso 1 1 calc R . . C18 C 0.0417(4) 0.3480(5) 0.3864(2) 0.0373(18) Uani 1 1 d . . . H18 H 0.0550 0.2855 0.3816 0.045 Uiso 1 1 calc R . . C19 C -0.0163(3) 0.3625(5) 0.3983(2) 0.0343(17) Uani 1 1 d . . . H19 H -0.0430 0.3107 0.4015 0.041 Uiso 1 1 calc R . . C20 C -0.0346(3) 0.4534(5) 0.4055(3) 0.0371(18) Uani 1 1 d . . . H20 H -0.0742 0.4641 0.4140 0.045 Uiso 1 1 calc R . . C21 C 0.0042(3) 0.5304(5) 0.4003(2) 0.0326(17) Uani 1 1 d . . . H21 H -0.0093 0.5929 0.4050 0.039 Uiso 1 1 calc R . . C22 C 0.3939(3) 0.7544(5) 0.3142(2) 0.0329(17) Uani 1 1 d . . . H22 H 0.3902 0.7854 0.3425 0.040 Uiso 1 1 calc R . . C23 C 0.4441(3) 0.7726(5) 0.2936(3) 0.0388(19) Uani 1 1 d . . . H23 H 0.4753 0.8174 0.3076 0.047 Uiso 1 1 calc R . . C24 C 0.4504(3) 0.7263(5) 0.2523(3) 0.0387(19) Uani 1 1 d . . . H24 H 0.4857 0.7401 0.2387 0.046 Uiso 1 1 calc R . . C25 C 0.4067(3) 0.6618(5) 0.2312(2) 0.0334(17) Uani 1 1 d . . . H25 H 0.4118 0.6315 0.2031 0.040 Uiso 1 1 calc R . . C26 C 0.3539(3) 0.6396(5) 0.2509(2) 0.0276(16) Uani 1 1 d . . . C27 C 0.3469(3) 0.6874(5) 0.2921(2) 0.0268(15) Uani 1 1 d . . . C28 C 0.2916(3) 0.6670(4) 0.3095(2) 0.0241(15) Uani 1 1 d . . . C29 C 0.2578(3) 0.5537(5) 0.2515(2) 0.0253(15) Uani 1 1 d . . . H29 H 0.2284 0.5059 0.2385 0.030 Uiso 1 1 calc R . . C30 C 0.3085(3) 0.5728(5) 0.2316(2) 0.0282(16) Uani 1 1 d . . . H30 H 0.3128 0.5397 0.2040 0.034 Uiso 1 1 calc R . . C31 C 0.3239(3) 0.6918(5) 0.4127(2) 0.0289(16) Uani 1 1 d . . . C32 C 0.3345(3) 0.7600(5) 0.4477(3) 0.0377(18) Uani 1 1 d . . . H32 H 0.3087 0.8150 0.4443 0.045 Uiso 1 1 calc R . . C33 C 0.3830(4) 0.7486(6) 0.4881(3) 0.055(2) Uani 1 1 d . . . H33 H 0.3909 0.7957 0.5119 0.066 Uiso 1 1 calc R . . C34 C 0.4188(4) 0.6673(7) 0.4923(3) 0.053(2) Uani 1 1 d . . . H34 H 0.4515 0.6581 0.5196 0.064 Uiso 1 1 calc R . . C35 C 0.4081(4) 0.5995(6) 0.4580(3) 0.048(2) Uani 1 1 d . . . H35 H 0.4336 0.5442 0.4615 0.058 Uiso 1 1 calc R . . C36 C 0.3607(3) 0.6108(5) 0.4183(3) 0.0396(19) Uani 1 1 d . . . H36 H 0.3532 0.5630 0.3948 0.047 Uiso 1 1 calc R . . C37 C 0.2383(3) 0.8262(5) 0.3563(2) 0.0296(16) Uani 1 1 d . . . C38 C 0.2571(4) 0.8875(5) 0.3246(3) 0.044(2) Uani 1 1 d . . . H38 H 0.2834 0.8646 0.3046 0.053 Uiso 1 1 calc R . . C39 C 0.2386(5) 0.9805(6) 0.3212(3) 0.060(3) Uani 1 1 d . . . H39 H 0.2535 1.0217 0.3001 0.072 Uiso 1 1 calc R . . C40 C 0.1986(5) 1.0135(6) 0.3482(3) 0.062(3) Uani 1 1 d . . . H40 H 0.1842 1.0770 0.3450 0.075 Uiso 1 1 calc R . . C41 C 0.1793(4) 0.9543(6) 0.3802(3) 0.052(2) Uani 1 1 d . . . H41 H 0.1522 0.9771 0.3996 0.063 Uiso 1 1 calc R . . C42 C 0.1996(3) 0.8613(5) 0.3838(3) 0.0359(18) Uani 1 1 d . . . H42 H 0.1862 0.8209 0.4059 0.043 Uiso 1 1 calc R . . Ir2 Ir 0.315706(12) 0.255072(17) 0.177584(9) 0.02022(7) Uani 1 1 d . . . Cl3 Cl 0.24773(8) 0.39242(11) 0.14603(6) 0.0284(4) Uani 1 1 d . . . Cl4 Cl 0.38856(8) 0.36012(11) 0.22694(6) 0.0274(4) Uani 1 1 d . . . P3 P 0.37271(8) 0.24290(12) 0.12129(6) 0.0231(4) Uani 1 1 d . . . P4 P 0.23731(8) 0.14868(12) 0.15264(6) 0.0210(4) Uani 1 1 d . . . N3 N 0.4677(3) 0.1133(4) 0.1180(2) 0.0357(15) Uani 1 1 d . . . N4 N 0.2534(2) 0.2445(4) 0.22565(17) 0.0227(12) Uani 1 1 d . . . C43 C 0.3741(3) 0.1490(4) 0.2101(2) 0.0207(14) Uani 1 1 d . . . C44 C 0.3718(3) 0.1128(5) 0.2536(2) 0.0267(15) Uani 1 1 d . . . H44 H 0.3410 0.1365 0.2696 0.032 Uiso 1 1 calc R . . C45 C 0.4132(3) 0.0422(5) 0.2749(2) 0.0347(17) Uani 1 1 d . . . H45 H 0.4098 0.0190 0.3049 0.042 Uiso 1 1 calc R . . C46 C 0.4585(3) 0.0059(5) 0.2537(3) 0.0364(18) Uani 1 1 d . . . H46 H 0.4866 -0.0416 0.2691 0.044 Uiso 1 1 calc R . . C47 C 0.4637(3) 0.0395(5) 0.2081(2) 0.0287(16) Uani 1 1 d . . . C48 C 0.4211(3) 0.1122(4) 0.1873(2) 0.0223(14) Uani 1 1 d . . . C49 C 0.4265(3) 0.1452(5) 0.1423(2) 0.0271(15) Uani 1 1 d . . . C50 C 0.5074(3) 0.0421(5) 0.1388(3) 0.0389(19) Uani 1 1 d . . . H50 H 0.5362 0.0158 0.1217 0.047 Uiso 1 1 calc R . . C51 C 0.5077(3) 0.0076(5) 0.1822(3) 0.0370(18) Uani 1 1 d . . . H51 H 0.5381 -0.0389 0.1953 0.044 Uiso 1 1 calc R . . C52 C 0.4223(3) 0.3416(5) 0.1098(2) 0.0285(16) Uani 1 1 d . . . C53 C 0.4750(4) 0.3267(6) 0.0910(3) 0.042(2) Uani 1 1 d . . . H53 H 0.4858 0.2644 0.0836 0.050 Uiso 1 1 calc R . . C54 C 0.5121(4) 0.4011(7) 0.0829(3) 0.056(2) Uani 1 1 d . . . H54 H 0.5481 0.3898 0.0696 0.067 Uiso 1 1 calc R . . C55 C 0.4977(4) 0.4907(7) 0.0937(3) 0.066(3) Uani 1 1 d . . . H55 H 0.5243 0.5415 0.0888 0.079 Uiso 1 1 calc R . . C56 C 0.4440(5) 0.5088(6) 0.1121(3) 0.064(3) Uani 1 1 d . . . H56 H 0.4332 0.5712 0.1194 0.077 Uiso 1 1 calc R . . C57 C 0.4065(4) 0.4315(5) 0.1194(3) 0.044(2) Uani 1 1 d . . . H57 H 0.3694 0.4420 0.1313 0.053 Uiso 1 1 calc R . . C58 C 0.3293(3) 0.2146(5) 0.0619(2) 0.0263(15) Uani 1 1 d . . . C59 C 0.3463(3) 0.1430(5) 0.0341(2) 0.0347(17) Uani 1 1 d . . . H59 H 0.3824 0.1046 0.0457 0.042 Uiso 1 1 calc R . . C60 C 0.3096(4) 0.1285(6) -0.0113(3) 0.046(2) Uani 1 1 d . . . H60 H 0.3207 0.0794 -0.0303 0.056 Uiso 1 1 calc R . . C61 C 0.2571(4) 0.1847(6) -0.0289(3) 0.0415(19) Uani 1 1 d . . . H61 H 0.2330 0.1748 -0.0599 0.050 Uiso 1 1 calc R . . C62 C 0.2402(4) 0.2542(5) -0.0015(3) 0.045(2) Uani 1 1 d . . . H62 H 0.2038 0.2917 -0.0134 0.054 Uiso 1 1 calc R . . C63 C 0.2754(3) 0.2708(5) 0.0435(2) 0.0301(16) Uani 1 1 d . . . H63 H 0.2634 0.3200 0.0621 0.036 Uiso 1 1 calc R . . C64 C 0.1009(3) 0.1107(5) 0.2006(2) 0.0285(16) Uani 1 1 d . . . H64 H 0.1027 0.0799 0.1718 0.034 Uiso 1 1 calc R . . C65 C 0.0496(3) 0.0971(5) 0.2203(3) 0.0315(16) Uani 1 1 d . . . H65 H 0.0162 0.0559 0.2060 0.038 Uiso 1 1 calc R . . C66 C 0.0468(3) 0.1456(5) 0.2625(3) 0.0360(18) Uani 1 1 d . . . H66 H 0.0108 0.1372 0.2760 0.043 Uiso 1 1 calc R . . C67 C 0.0932(3) 0.2027(5) 0.2836(2) 0.0306(16) Uani 1 1 d . . . H67 H 0.0897 0.2336 0.3120 0.037 Uiso 1 1 calc R . . C68 C 0.1479(3) 0.2186(5) 0.2647(2) 0.0273(16) Uani 1 1 d . . . C69 C 0.1521(3) 0.1703(4) 0.2225(2) 0.0237(15) Uani 1 1 d . . . C70 C 0.2067(3) 0.1862(4) 0.2048(2) 0.0235(14) Uani 1 1 d . . . C71 C 0.2488(3) 0.2912(5) 0.2658(2) 0.0276(15) Uani 1 1 d . . . H71 H 0.2817 0.3330 0.2801 0.033 Uiso 1 1 calc R . . C72 C 0.1981(3) 0.2790(5) 0.2853(2) 0.0281(16) Uani 1 1 d . . . H72 H 0.1962 0.3116 0.3136 0.034 Uiso 1 1 calc R . . C73 C 0.1750(3) 0.1572(5) 0.1003(2) 0.0265(15) Uani 1 1 d . . . C74 C 0.1339(3) 0.2340(5) 0.0944(3) 0.0358(18) Uani 1 1 d . . . H74 H 0.1379 0.2811 0.1182 0.043 Uiso 1 1 calc R . . C75 C 0.0872(3) 0.2415(6) 0.0536(3) 0.0374(18) Uani 1 1 d . . . H75 H 0.0590 0.2938 0.0496 0.045 Uiso 1 1 calc R . . C76 C 0.0811(3) 0.1738(6) 0.0189(3) 0.045(2) Uani 1 1 d . . . H76 H 0.0483 0.1792 -0.0086 0.053 Uiso 1 1 calc R . . C77 C 0.1224(4) 0.0985(6) 0.0239(3) 0.045(2) Uani 1 1 d . . . H77 H 0.1189 0.0528 -0.0004 0.054 Uiso 1 1 calc R . . C78 C 0.1686(4) 0.0896(5) 0.0642(2) 0.0349(18) Uani 1 1 d . . . H78 H 0.1966 0.0371 0.0677 0.042 Uiso 1 1 calc R . . C79 C 0.2581(3) 0.0242(5) 0.1593(2) 0.0262(15) Uani 1 1 d . . . C80 C 0.2339(3) -0.0349(4) 0.1897(2) 0.0275(15) Uani 1 1 d . . . H80 H 0.2043 -0.0114 0.2068 0.033 Uiso 1 1 calc R . . C81 C 0.2533(3) -0.1274(5) 0.1945(3) 0.0351(18) Uani 1 1 d . . . H81 H 0.2361 -0.1684 0.2144 0.042 Uiso 1 1 calc R . . C82 C 0.2980(4) -0.1617(5) 0.1703(3) 0.0392(19) Uani 1 1 d . . . H82 H 0.3117 -0.2255 0.1745 0.047 Uiso 1 1 calc R . . C83 C 0.3231(3) -0.1036(5) 0.1399(3) 0.0342(17) Uani 1 1 d . . . H83 H 0.3534 -0.1269 0.1233 0.041 Uiso 1 1 calc R . . C84 C 0.3022(3) -0.0109(5) 0.1346(2) 0.0289(16) Uani 1 1 d . . . H84 H 0.3182 0.0297 0.1138 0.035 Uiso 1 1 calc R . . C85 C 0.4336(4) 0.2577(5) 0.3494(3) 0.043(2) Uani 1 1 d . . . H85A H 0.4209 0.1938 0.3576 0.052 Uiso 1 1 calc R . . H85B H 0.4275 0.2611 0.3147 0.052 Uiso 1 1 calc R . . Cl5 Cl 0.38408(10) 0.34237(16) 0.36853(8) 0.0528(5) Uani 1 1 d . . . Cl6 Cl 0.51468(10) 0.27516(15) 0.37509(8) 0.0527(6) Uani 1 1 d . . . C86 C 0.3842(4) 0.1078(8) 0.4807(3) 0.078(4) Uani 1 1 d . . . H86A H 0.4045 0.0552 0.5008 0.094 Uiso 1 1 calc R . . H86B H 0.3550 0.1409 0.4974 0.094 Uiso 1 1 calc R . . Cl7 Cl 0.44441(14) 0.1891(2) 0.46969(9) 0.0805(8) Uani 1 1 d . . . Cl8 Cl 0.34202(14) 0.0640(3) 0.42717(11) 0.1052(11) Uani 1 1 d . . . C87 C 0.1173(4) 0.5710(6) 0.1532(3) 0.053(2) Uani 1 1 d . . . H87A H 0.1222 0.5676 0.1879 0.063 Uiso 1 1 calc R . . H87B H 0.1320 0.5103 0.1424 0.063 Uiso 1 1 calc R . . Cl9 Cl 0.03680(14) 0.5867(2) 0.12710(11) 0.0890(9) Uani 1 1 d . . . Cl10 Cl 0.16467(11) 0.66225(16) 0.13946(7) 0.0570(6) Uani 1 1 d . . . C88 C 0.2507(7) 0.9291(11) 0.5577(5) 0.162(7) Uiso 1 1 d D . . H88A H 0.2110 0.8923 0.5485 0.194 Uiso 1 1 d R . . H88B H 0.2435 0.9863 0.5755 0.194 Uiso 1 1 d R . . Cl11 Cl 0.3151(2) 0.8477(3) 0.59063(15) 0.1342(14) Uani 1 1 d D . . Cl12 Cl 0.2636(2) 0.9613(3) 0.50753(12) 0.1376(15) Uani 1 1 d D . . C89 C 0.1238(7) 1.0000(12) 0.5138(6) 0.175(7) Uiso 1 1 d D . . Cl13 Cl 0.0956(7) 1.0872(10) 0.4622(5) 0.348(9) Uiso 1 1 d D A . Cl1A Cl 0.0508(9) 0.9514(14) 0.5159(8) 0.373(12) Uiso 0.50 1 d PD A 1 Cl1B Cl 0.0648(9) 0.9205(12) 0.4772(8) 0.360(11) Uiso 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01843(14) 0.02237(14) 0.01938(14) -0.00035(10) 0.00371(10) -0.00010(11) Cl1 0.0242(9) 0.0266(9) 0.0265(9) -0.0029(7) 0.0040(7) -0.0036(7) Cl2 0.0258(9) 0.0279(9) 0.0264(9) 0.0000(7) 0.0030(7) 0.0050(7) P1 0.0195(9) 0.0265(9) 0.0208(9) 0.0012(7) 0.0051(7) 0.0014(7) P2 0.0221(10) 0.0252(9) 0.0228(9) -0.0026(7) 0.0025(7) -0.0047(8) N1 0.027(3) 0.028(3) 0.033(3) 0.002(3) 0.010(3) 0.007(3) N2 0.020(3) 0.020(3) 0.025(3) 0.000(2) 0.006(2) 0.000(2) C1 0.022(4) 0.026(4) 0.015(3) 0.005(3) -0.001(3) 0.001(3) C2 0.025(4) 0.027(4) 0.031(4) -0.003(3) 0.003(3) 0.000(3) C3 0.038(5) 0.038(4) 0.023(4) 0.007(3) -0.001(3) -0.006(4) C4 0.032(4) 0.024(4) 0.037(4) 0.008(3) 0.006(3) 0.007(3) C5 0.022(4) 0.028(4) 0.026(4) 0.003(3) -0.001(3) -0.002(3) C6 0.020(4) 0.025(4) 0.025(4) 0.000(3) 0.002(3) 0.002(3) C7 0.022(4) 0.024(4) 0.029(4) 0.002(3) 0.005(3) -0.001(3) C8 0.028(4) 0.039(5) 0.038(4) 0.000(3) 0.003(3) 0.007(3) C9 0.026(4) 0.023(4) 0.039(4) 0.004(3) 0.004(3) 0.005(3) C10 0.027(4) 0.027(4) 0.024(4) 0.002(3) 0.005(3) -0.001(3) C11 0.030(4) 0.033(4) 0.024(4) 0.002(3) 0.007(3) 0.002(3) C12 0.026(4) 0.045(5) 0.028(4) 0.005(3) 0.005(3) -0.003(3) C13 0.045(5) 0.037(4) 0.027(4) -0.003(3) 0.006(4) -0.003(4) C14 0.058(6) 0.043(5) 0.030(4) -0.007(4) 0.013(4) 0.010(4) C15 0.029(4) 0.047(5) 0.032(4) -0.006(3) 0.006(3) 0.005(4) C16 0.029(4) 0.028(4) 0.018(3) 0.002(3) 0.004(3) 0.001(3) C17 0.037(4) 0.032(4) 0.031(4) 0.000(3) 0.012(3) -0.008(3) C18 0.050(5) 0.031(4) 0.034(4) -0.002(3) 0.016(4) -0.005(4) C19 0.029(4) 0.042(5) 0.029(4) 0.004(3) 0.001(3) -0.010(3) C20 0.020(4) 0.050(5) 0.044(5) 0.011(4) 0.014(3) 0.005(4) C21 0.030(4) 0.031(4) 0.039(4) 0.006(3) 0.011(3) 0.004(3) C22 0.028(4) 0.041(4) 0.028(4) 0.005(3) 0.003(3) -0.003(3) C23 0.024(4) 0.044(5) 0.043(5) 0.011(4) -0.004(3) -0.010(3) C24 0.022(4) 0.054(5) 0.040(5) 0.015(4) 0.009(3) 0.007(4) C25 0.024(4) 0.046(5) 0.033(4) 0.008(3) 0.013(3) 0.008(3) C26 0.022(4) 0.034(4) 0.029(4) 0.006(3) 0.010(3) 0.004(3) C27 0.022(4) 0.032(4) 0.026(4) 0.005(3) 0.004(3) -0.001(3) C28 0.022(4) 0.023(4) 0.026(4) 0.003(3) 0.000(3) 0.000(3) C29 0.026(4) 0.027(4) 0.023(4) 0.002(3) 0.006(3) 0.005(3) C30 0.031(4) 0.030(4) 0.025(4) 0.007(3) 0.010(3) 0.010(3) C31 0.021(4) 0.038(4) 0.027(4) 0.001(3) 0.004(3) -0.006(3) C32 0.033(4) 0.047(5) 0.032(4) -0.007(3) 0.003(3) -0.001(4) C33 0.063(6) 0.066(6) 0.030(5) -0.016(4) -0.003(4) -0.002(5) C34 0.033(5) 0.077(7) 0.042(5) -0.006(5) -0.011(4) -0.004(5) C35 0.043(5) 0.050(5) 0.049(5) 0.010(4) 0.004(4) 0.007(4) C36 0.031(4) 0.043(5) 0.044(5) -0.001(4) 0.004(4) 0.000(4) C37 0.029(4) 0.028(4) 0.029(4) -0.006(3) -0.001(3) -0.001(3) C38 0.070(6) 0.032(4) 0.030(4) 0.001(3) 0.009(4) 0.002(4) C39 0.105(8) 0.031(5) 0.040(5) 0.002(4) 0.009(5) -0.003(5) C40 0.082(7) 0.036(5) 0.063(6) -0.006(5) 0.001(5) 0.021(5) C41 0.051(6) 0.041(5) 0.063(6) -0.019(4) 0.009(5) 0.002(4) C42 0.036(5) 0.028(4) 0.041(5) -0.003(3) 0.002(4) 0.006(3) Ir2 0.01858(14) 0.02046(14) 0.02122(14) -0.00079(10) 0.00337(10) -0.00138(10) Cl3 0.0273(10) 0.0252(9) 0.0310(9) 0.0010(7) 0.0024(7) 0.0030(7) Cl4 0.0234(9) 0.0252(9) 0.0319(9) -0.0055(7) 0.0023(7) -0.0043(7) P3 0.0209(9) 0.0256(9) 0.0231(9) -0.0005(7) 0.0049(7) -0.0019(7) P4 0.0192(9) 0.0217(9) 0.0220(9) -0.0028(7) 0.0041(7) -0.0024(7) N3 0.026(4) 0.039(4) 0.044(4) -0.002(3) 0.012(3) 0.005(3) N4 0.022(3) 0.029(3) 0.017(3) 0.002(2) 0.004(2) -0.002(2) C43 0.016(3) 0.023(3) 0.018(3) 0.000(3) -0.008(3) -0.002(3) C44 0.024(4) 0.027(4) 0.026(4) 0.002(3) -0.001(3) 0.001(3) C45 0.035(4) 0.041(5) 0.027(4) 0.006(3) 0.004(3) -0.001(4) C46 0.039(5) 0.029(4) 0.039(5) 0.007(3) 0.004(4) 0.004(3) C47 0.020(4) 0.029(4) 0.034(4) 0.000(3) -0.002(3) -0.001(3) C48 0.016(3) 0.025(4) 0.025(4) -0.001(3) 0.002(3) -0.001(3) C49 0.018(4) 0.026(4) 0.037(4) -0.007(3) 0.003(3) -0.002(3) C50 0.028(4) 0.045(5) 0.045(5) 0.003(4) 0.010(4) 0.015(4) C51 0.023(4) 0.034(4) 0.052(5) -0.002(4) 0.005(4) 0.010(3) C52 0.031(4) 0.032(4) 0.022(4) -0.001(3) 0.003(3) -0.011(3) C53 0.039(5) 0.048(5) 0.043(5) 0.000(4) 0.019(4) -0.004(4) C54 0.047(6) 0.075(7) 0.052(6) 0.000(5) 0.024(4) -0.026(5) C55 0.076(7) 0.073(7) 0.057(6) -0.010(5) 0.032(5) -0.053(6) C56 0.097(8) 0.034(5) 0.069(6) -0.007(4) 0.037(6) -0.027(5) C57 0.059(6) 0.035(5) 0.043(5) 0.001(4) 0.024(4) -0.021(4) C58 0.031(4) 0.027(4) 0.022(4) -0.004(3) 0.010(3) -0.011(3) C59 0.031(4) 0.040(4) 0.036(4) -0.007(3) 0.011(3) -0.001(3) C60 0.066(6) 0.047(5) 0.028(4) -0.017(4) 0.015(4) -0.007(4) C61 0.043(5) 0.052(5) 0.028(4) -0.003(4) 0.002(4) 0.003(4) C62 0.052(6) 0.045(5) 0.037(5) -0.002(4) 0.005(4) 0.016(4) C63 0.035(4) 0.037(4) 0.018(4) -0.005(3) 0.006(3) 0.000(3) C64 0.028(4) 0.024(4) 0.033(4) -0.001(3) 0.006(3) -0.001(3) C65 0.019(4) 0.031(4) 0.043(4) 0.006(3) 0.005(3) 0.001(3) C66 0.031(4) 0.042(5) 0.042(5) 0.013(4) 0.022(4) 0.003(4) C67 0.029(4) 0.034(4) 0.032(4) -0.003(3) 0.014(3) 0.001(3) C68 0.031(4) 0.028(4) 0.023(4) 0.004(3) 0.004(3) 0.008(3) C69 0.025(4) 0.026(4) 0.021(3) -0.003(3) 0.005(3) 0.003(3) C70 0.022(4) 0.021(4) 0.027(4) -0.003(3) 0.004(3) 0.002(3) C71 0.029(4) 0.027(4) 0.025(4) -0.002(3) 0.002(3) 0.001(3) C72 0.030(4) 0.031(4) 0.023(4) -0.002(3) 0.006(3) 0.006(3) C73 0.022(4) 0.027(4) 0.030(4) 0.001(3) 0.005(3) -0.009(3) C74 0.026(4) 0.044(5) 0.036(4) -0.001(3) 0.004(3) 0.002(3) C75 0.018(4) 0.058(5) 0.034(4) -0.002(4) 0.001(3) 0.002(4) C76 0.022(4) 0.073(6) 0.035(5) -0.002(4) -0.004(3) -0.002(4) C77 0.052(6) 0.056(6) 0.028(4) -0.015(4) 0.008(4) -0.005(4) C78 0.039(5) 0.037(4) 0.026(4) -0.010(3) 0.001(3) -0.001(3) C79 0.027(4) 0.025(4) 0.025(4) -0.006(3) 0.001(3) -0.002(3) C80 0.028(4) 0.024(4) 0.031(4) -0.001(3) 0.008(3) -0.005(3) C81 0.038(5) 0.025(4) 0.038(4) 0.009(3) 0.000(4) -0.006(3) C82 0.041(5) 0.026(4) 0.044(5) -0.002(3) -0.007(4) 0.006(3) C83 0.028(4) 0.034(4) 0.040(4) 0.004(3) 0.004(3) 0.006(3) C84 0.023(4) 0.032(4) 0.030(4) -0.005(3) 0.002(3) -0.004(3) C85 0.050(5) 0.042(5) 0.034(4) -0.006(4) 0.002(4) -0.003(4) Cl5 0.0436(13) 0.0556(14) 0.0613(14) -0.0024(11) 0.0158(11) 0.0040(10) Cl6 0.0418(13) 0.0550(14) 0.0617(14) 0.0034(10) 0.0120(11) 0.0057(10) C86 0.033(5) 0.160(11) 0.044(6) -0.030(6) 0.015(4) -0.018(6) Cl7 0.104(2) 0.080(2) 0.0590(16) -0.0079(14) 0.0207(15) -0.0120(16) Cl8 0.071(2) 0.155(3) 0.090(2) -0.046(2) 0.0162(17) -0.024(2) C87 0.060(6) 0.044(5) 0.050(5) 0.006(4) 0.001(4) -0.007(4) Cl9 0.082(2) 0.073(2) 0.100(2) 0.0231(16) -0.0090(17) -0.0168(15) Cl10 0.0698(16) 0.0617(15) 0.0430(13) 0.0086(10) 0.0203(11) -0.0022(12) Cl11 0.148(4) 0.112(3) 0.142(3) 0.004(3) 0.031(3) -0.027(3) Cl12 0.244(5) 0.102(3) 0.080(2) 0.000(2) 0.067(3) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.047(6) . ? Ir1 N2 2.127(5) . ? Ir1 P1 2.2530(16) . ? Ir1 P2 2.2729(17) . ? Ir1 Cl1 2.4053(16) . ? Ir1 Cl2 2.4552(16) . ? P1 C10 1.823(7) . ? P1 C16 1.829(7) . ? P1 C7 1.841(7) . ? P2 C37 1.799(7) . ? P2 C31 1.827(7) . ? P2 C28 1.835(7) . ? N1 C7 1.327(8) . ? N1 C8 1.353(8) . ? N2 C28 1.327(8) . ? N2 C29 1.344(7) . ? C1 C2 1.381(9) . ? C1 C6 1.410(9) . ? C2 C3 1.433(9) . ? C3 C4 1.394(9) . ? C4 C5 1.415(9) . ? C5 C9 1.381(9) . ? C5 C6 1.404(9) . ? C6 C7 1.420(9) . ? C8 C9 1.377(9) . ? C10 C11 1.391(9) . ? C10 C15 1.413(9) . ? C11 C12 1.367(9) . ? C12 C13 1.387(10) . ? C13 C14 1.366(10) . ? C14 C15 1.381(10) . ? C16 C17 1.375(9) . ? C16 C21 1.392(9) . ? C17 C18 1.404(9) . ? C18 C19 1.381(10) . ? C19 C20 1.376(10) . ? C20 C21 1.402(9) . ? C22 C23 1.370(10) . ? C22 C27 1.436(9) . ? C23 C24 1.398(10) . ? C24 C25 1.359(10) . ? C25 C26 1.412(9) . ? C26 C30 1.391(9) . ? C26 C27 1.413(9) . ? C27 C28 1.419(9) . ? C29 C30 1.366(8) . ? C31 C36 1.385(10) . ? C31 C32 1.386(10) . ? C32 C33 1.405(10) . ? C33 C34 1.377(11) . ? C34 C35 1.369(11) . ? C35 C36 1.376(10) . ? C37 C42 1.365(9) . ? C37 C38 1.389(10) . ? C38 C39 1.374(10) . ? C39 C40 1.366(12) . ? C40 C41 1.380(12) . ? C41 C42 1.386(10) . ? Ir2 C43 2.056(6) . ? Ir2 N4 2.139(5) . ? Ir2 P3 2.2513(17) . ? Ir2 P4 2.2649(16) . ? Ir2 Cl4 2.4032(16) . ? Ir2 Cl3 2.4901(16) . ? P3 C58 1.822(7) . ? P3 C49 1.825(7) . ? P3 C52 1.834(7) . ? P4 C73 1.805(7) . ? P4 C79 1.821(7) . ? P4 C70 1.853(6) . ? N3 C49 1.328(8) . ? N3 C50 1.375(9) . ? N4 C70 1.343(8) . ? N4 C71 1.362(8) . ? C43 C44 1.375(8) . ? C43 C48 1.420(9) . ? C44 C45 1.395(9) . ? C45 C46 1.361(10) . ? C46 C47 1.434(9) . ? C47 C51 1.406(9) . ? C47 C48 1.426(9) . ? C48 C49 1.415(9) . ? C50 C51 1.350(10) . ? C52 C57 1.363(10) . ? C52 C53 1.376(9) . ? C53 C54 1.373(10) . ? C54 C55 1.361(12) . ? C55 C56 1.397(12) . ? C56 C57 1.403(10) . ? C58 C59 1.395(9) . ? C58 C63 1.415(9) . ? C59 C60 1.399(10) . ? C60 C61 1.390(10) . ? C61 C62 1.362(10) . ? C62 C63 1.384(10) . ? C64 C65 1.365(9) . ? C64 C69 1.426(9) . ? C65 C66 1.416(10) . ? C66 C67 1.331(10) . ? C67 C68 1.419(9) . ? C68 C72 1.409(9) . ? C68 C69 1.424(8) . ? C69 C70 1.400(8) . ? C71 C72 1.345(9) . ? C73 C74 1.390(9) . ? C73 C78 1.405(9) . ? C74 C75 1.385(10) . ? C75 C76 1.378(10) . ? C76 C77 1.379(11) . ? C77 C78 1.369(10) . ? C79 C80 1.394(9) . ? C79 C84 1.399(9) . ? C80 C81 1.374(9) . ? C81 C82 1.396(10) . ? C82 C83 1.396(10) . ? C83 C84 1.387(9) . ? C85 Cl6 1.765(8) . ? C85 Cl5 1.772(8) . ? C86 Cl8 1.739(9) . ? C86 Cl7 1.814(10) . ? C87 Cl10 1.746(8) . ? C87 Cl9 1.753(8) . ? C88 Cl12 1.607(12) . ? C88 Cl11 1.898(12) . ? C89 Cl1A 1.731(15) . ? C89 Cl1B 1.854(16) . ? C89 Cl13 1.937(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 N2 92.7(2) . . ? C1 Ir1 P1 84.00(18) . . ? N2 Ir1 P1 171.17(14) . . ? C1 Ir1 P2 88.89(18) . . ? N2 Ir1 P2 68.55(14) . . ? P1 Ir1 P2 103.12(6) . . ? C1 Ir1 Cl1 86.11(18) . . ? N2 Ir1 Cl1 93.07(14) . . ? P1 Ir1 Cl1 94.88(6) . . ? P2 Ir1 Cl1 160.71(6) . . ? C1 Ir1 Cl2 175.48(18) . . ? N2 Ir1 Cl2 85.72(14) . . ? P1 Ir1 Cl2 98.14(6) . . ? P2 Ir1 Cl2 94.47(6) . . ? Cl1 Ir1 Cl2 89.74(6) . . ? C10 P1 C16 101.3(3) . . ? C10 P1 C7 107.6(3) . . ? C16 P1 C7 107.9(3) . . ? C10 P1 Ir1 118.7(2) . . ? C16 P1 Ir1 118.4(2) . . ? C7 P1 Ir1 102.3(2) . . ? C37 P2 C31 106.3(3) . . ? C37 P2 C28 110.6(3) . . ? C31 P2 C28 107.3(3) . . ? C37 P2 Ir1 117.4(2) . . ? C31 P2 Ir1 127.3(2) . . ? C28 P2 Ir1 84.5(2) . . ? C7 N1 C8 116.2(6) . . ? C28 N2 C29 121.3(6) . . ? C28 N2 Ir1 104.8(4) . . ? C29 N2 Ir1 133.8(4) . . ? C2 C1 C6 116.4(6) . . ? C2 C1 Ir1 122.8(5) . . ? C6 C1 Ir1 120.6(4) . . ? C1 C2 C3 121.8(6) . . ? C4 C3 C2 120.5(6) . . ? C3 C4 C5 118.8(6) . . ? C9 C5 C6 119.2(6) . . ? C9 C5 C4 122.0(6) . . ? C6 C5 C4 118.7(6) . . ? C5 C6 C1 123.6(6) . . ? C5 C6 C7 116.7(6) . . ? C1 C6 C7 119.6(6) . . ? N1 C7 C6 124.5(6) . . ? N1 C7 P1 122.4(5) . . ? C6 C7 P1 113.1(5) . . ? N1 C8 C9 124.4(7) . . ? C8 C9 C5 118.8(6) . . ? C11 C10 C15 119.1(6) . . ? C11 C10 P1 119.4(5) . . ? C15 C10 P1 121.3(5) . . ? C12 C11 C10 119.8(7) . . ? C11 C12 C13 120.7(7) . . ? C14 C13 C12 120.4(7) . . ? C13 C14 C15 120.0(7) . . ? C14 C15 C10 119.8(7) . . ? C17 C16 C21 120.0(6) . . ? C17 C16 P1 118.9(5) . . ? C21 C16 P1 121.1(5) . . ? C16 C17 C18 119.6(7) . . ? C19 C18 C17 121.1(7) . . ? C20 C19 C18 118.8(7) . . ? C19 C20 C21 121.1(7) . . ? C16 C21 C20 119.4(7) . . ? C23 C22 C27 118.5(7) . . ? C22 C23 C24 121.1(7) . . ? C25 C24 C23 121.1(7) . . ? C24 C25 C26 120.6(7) . . ? C30 C26 C25 123.3(6) . . ? C30 C26 C27 118.2(6) . . ? C25 C26 C27 118.5(6) . . ? C26 C27 C28 117.0(6) . . ? C26 C27 C22 120.2(6) . . ? C28 C27 C22 122.8(6) . . ? N2 C28 C27 121.8(6) . . ? N2 C28 P2 102.2(4) . . ? C27 C28 P2 135.8(5) . . ? N2 C29 C30 119.9(6) . . ? C29 C30 C26 121.5(6) . . ? C36 C31 C32 119.4(7) . . ? C36 C31 P2 119.0(6) . . ? C32 C31 P2 121.5(6) . . ? C31 C32 C33 120.6(7) . . ? C34 C33 C32 118.3(8) . . ? C35 C34 C33 121.2(8) . . ? C34 C35 C36 120.5(8) . . ? C35 C36 C31 120.0(7) . . ? C42 C37 C38 117.5(7) . . ? C42 C37 P2 119.5(6) . . ? C38 C37 P2 122.9(6) . . ? C39 C38 C37 121.7(8) . . ? C40 C39 C38 119.8(9) . . ? C39 C40 C41 119.8(8) . . ? C40 C41 C42 119.5(8) . . ? C37 C42 C41 121.6(8) . . ? C43 Ir2 N4 93.3(2) . . ? C43 Ir2 P3 84.33(18) . . ? N4 Ir2 P3 169.88(15) . . ? C43 Ir2 P4 90.13(17) . . ? N4 Ir2 P4 68.44(14) . . ? P3 Ir2 P4 101.67(6) . . ? C43 Ir2 Cl4 85.46(17) . . ? N4 Ir2 Cl4 94.33(14) . . ? P3 Ir2 Cl4 95.29(6) . . ? P4 Ir2 Cl4 161.97(6) . . ? C43 Ir2 Cl3 174.15(17) . . ? N4 Ir2 Cl3 83.85(14) . . ? P3 Ir2 Cl3 99.33(6) . . ? P4 Ir2 Cl3 93.57(6) . . ? Cl4 Ir2 Cl3 89.64(5) . . ? C58 P3 C49 108.1(3) . . ? C58 P3 C52 101.4(3) . . ? C49 P3 C52 106.6(3) . . ? C58 P3 Ir2 117.0(2) . . ? C49 P3 Ir2 102.8(2) . . ? C52 P3 Ir2 120.3(2) . . ? C73 P4 C79 106.1(3) . . ? C73 P4 C70 109.8(3) . . ? C79 P4 C70 108.2(3) . . ? C73 P4 Ir2 126.5(2) . . ? C79 P4 Ir2 117.5(2) . . ? C70 P4 Ir2 85.4(2) . . ? C49 N3 C50 116.1(6) . . ? C70 N4 C71 120.0(6) . . ? C70 N4 Ir2 105.3(4) . . ? C71 N4 Ir2 134.0(4) . . ? C44 C43 C48 117.4(6) . . ? C44 C43 Ir2 123.7(5) . . ? C48 C43 Ir2 118.8(4) . . ? C43 C44 C45 121.9(6) . . ? C46 C45 C44 121.6(7) . . ? C45 C46 C47 119.7(7) . . ? C51 C47 C48 116.9(6) . . ? C51 C47 C46 125.6(6) . . ? C48 C47 C46 117.5(6) . . ? C49 C48 C43 121.0(6) . . ? C49 C48 C47 117.2(6) . . ? C43 C48 C47 121.8(6) . . ? N3 C49 C48 125.1(6) . . ? N3 C49 P3 122.0(5) . . ? C48 C49 P3 112.8(5) . . ? C51 C50 N3 123.7(7) . . ? C50 C51 C47 120.9(7) . . ? C57 C52 C53 119.2(7) . . ? C57 C52 P3 119.6(5) . . ? C53 C52 P3 121.2(6) . . ? C54 C53 C52 120.7(8) . . ? C55 C54 C53 120.5(8) . . ? C54 C55 C56 120.5(8) . . ? C55 C56 C57 117.7(8) . . ? C52 C57 C56 121.5(8) . . ? C59 C58 C63 119.1(6) . . ? C59 C58 P3 124.3(6) . . ? C63 C58 P3 116.6(5) . . ? C58 C59 C60 119.1(7) . . ? C61 C60 C59 120.9(7) . . ? C62 C61 C60 119.8(7) . . ? C61 C62 C63 120.9(7) . . ? C62 C63 C58 120.1(6) . . ? C65 C64 C69 121.0(6) . . ? C64 C65 C66 118.8(7) . . ? C67 C66 C65 121.9(6) . . ? C66 C67 C68 121.5(6) . . ? C72 C68 C67 123.9(6) . . ? C72 C68 C69 118.3(6) . . ? C67 C68 C69 117.8(6) . . ? C70 C69 C68 116.8(6) . . ? C70 C69 C64 124.1(6) . . ? C68 C69 C64 119.0(6) . . ? N4 C70 C69 122.8(6) . . ? N4 C70 P4 100.5(4) . . ? C69 C70 P4 136.7(5) . . ? C72 C71 N4 120.9(6) . . ? C71 C72 C68 121.2(6) . . ? C74 C73 C78 118.9(6) . . ? C74 C73 P4 119.7(5) . . ? C78 C73 P4 121.4(5) . . ? C75 C74 C73 119.5(7) . . ? C76 C75 C74 120.8(7) . . ? C75 C76 C77 120.1(7) . . ? C78 C77 C76 119.8(7) . . ? C77 C78 C73 120.8(7) . . ? C80 C79 C84 119.9(6) . . ? C80 C79 P4 122.2(5) . . ? C84 C79 P4 117.9(5) . . ? C81 C80 C79 119.3(6) . . ? C80 C81 C82 120.6(7) . . ? C83 C82 C81 121.0(7) . . ? C84 C83 C82 117.9(7) . . ? C83 C84 C79 121.3(7) . . ? Cl6 C85 Cl5 112.4(4) . . ? Cl8 C86 Cl7 109.1(5) . . ? Cl10 C87 Cl9 112.4(5) . . ? Cl12 C88 Cl11 112.3(8) . . ? Cl1A C89 Cl1B 42.4(10) . . ? Cl1A C89 Cl13 98.2(9) . . ? Cl1B C89 Cl13 83.1(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.549 _refine_diff_density_min -1.679 _refine_diff_density_rms 0.224 data_complex_6a _database_code_depnum_ccdc_archive 'CCDC 787573' #TrackingRef '- xray-1_3_6a_6b_7a-NEW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H54 Ir N4 P2' _chemical_formula_weight 1109.23 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 23.3005(5) _cell_length_b 12.3608(3) _cell_length_c 33.9148(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9767.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12518 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4488 _exptl_absorpt_coefficient_mu 2.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.588 _exptl_absorpt_correction_T_max 0.871 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39338 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0758 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20536 _reflns_number_gt 15932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.389(7) _refine_ls_number_reflns 20536 _refine_ls_number_parameters 1203 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1393 _refine_ls_wR_factor_gt 0.1260 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.016025(12) 0.20118(2) 0.528403(9) 0.01721(8) Uani 1 1 d . . . P1 P -0.04590(10) 0.33349(18) 0.50867(7) 0.0207(5) Uani 1 1 d . . . P2 P -0.03763(10) 0.13131(19) 0.58072(7) 0.0208(5) Uani 1 1 d . . . N1 N 0.0765(3) 0.0743(5) 0.5383(2) 0.0184(15) Uani 1 1 d . . . N2 N 0.0800(3) 0.2715(6) 0.5646(2) 0.0243(17) Uani 1 1 d . . . N3 N 0.0895(3) 0.3713(6) 0.5805(2) 0.0227(16) Uani 1 1 d . . . N4 N 0.1622(3) 0.2591(6) 0.5984(2) 0.0262(17) Uani 1 1 d . . . C1 C 0.0711(4) -0.0265(7) 0.5220(3) 0.025(2) Uani 1 1 d . . . H1 H 0.0399 -0.0394 0.5046 0.030 Uiso 1 1 calc R . . C2 C 0.1082(4) -0.1089(6) 0.5294(3) 0.0277(19) Uani 1 1 d . . . H2 H 0.1025 -0.1780 0.5178 0.033 Uiso 1 1 calc R . . C3 C 0.1557(4) -0.0901(7) 0.5547(3) 0.030(2) Uani 1 1 d . . . C4 C 0.1966(5) -0.1710(8) 0.5631(3) 0.039(3) Uani 1 1 d . . . H4 H 0.1926 -0.2407 0.5516 0.047 Uiso 1 1 calc R . . C5 C 0.2418(5) -0.1497(9) 0.5874(4) 0.053(3) Uani 1 1 d . . . H5 H 0.2686 -0.2054 0.5932 0.064 Uiso 1 1 calc R . . C6 C 0.2492(5) -0.0476(9) 0.6038(4) 0.047(3) Uani 1 1 d . . . H6 H 0.2808 -0.0343 0.6209 0.057 Uiso 1 1 calc R . . C7 C 0.2110(4) 0.0347(8) 0.5956(3) 0.040(3) Uani 1 1 d . . . H7 H 0.2165 0.1049 0.6064 0.048 Uiso 1 1 calc R . . C8 C 0.1631(4) 0.0124(8) 0.5706(3) 0.027(2) Uani 1 1 d . . . C9 C 0.1222(4) 0.0967(7) 0.5619(3) 0.0210(19) Uani 1 1 d . . . C10 C 0.1233(4) 0.2063(7) 0.5760(3) 0.0194(18) Uani 1 1 d . . . C11 C 0.1401(4) 0.3594(8) 0.5997(3) 0.027(2) Uani 1 1 d . . . C12 C 0.1684(4) 0.4507(7) 0.6225(3) 0.027(2) Uani 1 1 d . . . C13 C 0.1289(5) 0.5520(8) 0.6220(4) 0.050(3) Uani 1 1 d . . . H13A H 0.1209 0.5729 0.5947 0.075 Uiso 1 1 calc R . . H13B H 0.1481 0.6119 0.6356 0.075 Uiso 1 1 calc R . . H13C H 0.0927 0.5352 0.6355 0.075 Uiso 1 1 calc R . . C14 C 0.1801(5) 0.4174(9) 0.6644(3) 0.051(3) Uani 1 1 d . . . H14A H 0.1448 0.3896 0.6764 0.076 Uiso 1 1 calc R . . H14B H 0.1936 0.4802 0.6795 0.076 Uiso 1 1 calc R . . H14C H 0.2096 0.3609 0.6648 0.076 Uiso 1 1 calc R . . C15 C 0.2240(5) 0.4800(10) 0.6018(4) 0.055(3) Uani 1 1 d . . . H15A H 0.2518 0.4212 0.6052 0.083 Uiso 1 1 calc R . . H15B H 0.2395 0.5467 0.6132 0.083 Uiso 1 1 calc R . . H15C H 0.2166 0.4909 0.5736 0.083 Uiso 1 1 calc R . . C16 C 0.0621(4) 0.2521(8) 0.4791(3) 0.023(2) Uani 1 1 d . . . C17 C 0.1164(4) 0.2129(7) 0.4695(3) 0.024(2) Uani 1 1 d . . . H17 H 0.1343 0.1623 0.4867 0.029 Uiso 1 1 calc R . . C18 C 0.1459(4) 0.2467(8) 0.4346(3) 0.028(2) Uani 1 1 d . . . H18 H 0.1823 0.2166 0.4284 0.033 Uiso 1 1 calc R . . C19 C 0.1218(4) 0.3219(7) 0.4103(3) 0.027(2) Uani 1 1 d . . . H19 H 0.1422 0.3462 0.3877 0.032 Uiso 1 1 calc R . . C20 C 0.0662(4) 0.3644(6) 0.4185(3) 0.0211(18) Uani 1 1 d . . . C21 C 0.0376(4) 0.4366(7) 0.3927(3) 0.031(2) Uani 1 1 d . . . H21 H 0.0564 0.4594 0.3693 0.037 Uiso 1 1 calc R . . C22 C -0.0158(4) 0.4740(8) 0.4005(3) 0.031(2) Uani 1 1 d . . . H22 H -0.0340 0.5217 0.3824 0.037 Uiso 1 1 calc R . . C23 C -0.0442(4) 0.4436(7) 0.4345(3) 0.025(2) Uani 1 1 d . . . H23 H -0.0815 0.4706 0.4400 0.030 Uiso 1 1 calc R . . C24 C -0.0169(4) 0.3716(7) 0.4609(3) 0.025(2) Uani 1 1 d . . . C25 C 0.0377(4) 0.3298(7) 0.4527(3) 0.0180(18) Uani 1 1 d . . . C26 C -0.1202(4) 0.2901(6) 0.5011(3) 0.0202(18) Uani 1 1 d . . . C27 C -0.1605(4) 0.2945(6) 0.5331(3) 0.030(2) Uani 1 1 d . . . H27 H -0.1486 0.3250 0.5575 0.036 Uiso 1 1 calc R . . C28 C -0.2141(4) 0.2573(7) 0.5299(3) 0.0302(19) Uiso 1 1 d . . . H28 H -0.2397 0.2624 0.5516 0.036 Uiso 1 1 calc R . . C29 C -0.2325(4) 0.2105(8) 0.4944(4) 0.042(3) Uani 1 1 d . . . H29 H -0.2704 0.1831 0.4919 0.050 Uiso 1 1 calc R . . C30 C -0.1949(5) 0.2050(7) 0.4632(3) 0.032(2) Uani 1 1 d . . . H30 H -0.2072 0.1732 0.4392 0.039 Uiso 1 1 calc R . . C31 C -0.1390(4) 0.2449(7) 0.4661(3) 0.026(2) Uani 1 1 d . . . H31 H -0.1139 0.2411 0.4440 0.031 Uiso 1 1 calc R . . C32 C -0.0572(3) 0.4649(7) 0.5327(3) 0.0239(18) Uani 1 1 d . . . C33 C -0.1066(4) 0.5269(7) 0.5224(3) 0.030(2) Uani 1 1 d . . . H33 H -0.1345 0.4989 0.5046 0.036 Uiso 1 1 calc R . . C34 C -0.1131(4) 0.6286(7) 0.5387(3) 0.030(2) Uani 1 1 d . . . H34 H -0.1449 0.6715 0.5310 0.036 Uiso 1 1 calc R . . C35 C -0.0747(4) 0.6701(7) 0.5659(3) 0.034(2) Uani 1 1 d . . . H35 H -0.0814 0.7382 0.5781 0.040 Uiso 1 1 calc R . . C36 C -0.0263(4) 0.6098(8) 0.5751(3) 0.029(2) Uani 1 1 d . . . H36 H 0.0018 0.6389 0.5923 0.035 Uiso 1 1 calc R . . C37 C -0.0187(4) 0.5075(7) 0.5592(3) 0.027(2) Uani 1 1 d . . . H37 H 0.0138 0.4661 0.5668 0.032 Uiso 1 1 calc R . . C38 C -0.0357(3) 0.1015(7) 0.4946(3) 0.0195(18) Uani 1 1 d . . . C39 C -0.0303(4) 0.0871(7) 0.4546(3) 0.0236(19) Uani 1 1 d . . . H39 H 0.0000 0.1229 0.4411 0.028 Uiso 1 1 calc R . . C40 C -0.0682(4) 0.0207(7) 0.4325(3) 0.028(2) Uani 1 1 d . . . H40 H -0.0629 0.0139 0.4048 0.034 Uiso 1 1 calc R . . C41 C -0.1120(4) -0.0335(7) 0.4503(3) 0.023(2) Uani 1 1 d . . . H41 H -0.1384 -0.0745 0.4351 0.028 Uiso 1 1 calc R . . C42 C -0.1176(4) -0.0278(7) 0.4919(3) 0.024(2) Uani 1 1 d . . . C43 C -0.1605(4) -0.0889(8) 0.5119(3) 0.030(2) Uani 1 1 d . . . H43 H -0.1875 -0.1295 0.4971 0.036 Uiso 1 1 calc R . . C44 C -0.1634(4) -0.0899(7) 0.5517(3) 0.028(2) Uani 1 1 d . . . H44 H -0.1908 -0.1346 0.5645 0.034 Uiso 1 1 calc R . . C45 C -0.1262(4) -0.0255(8) 0.5744(3) 0.030(2) Uani 1 1 d . . . H45 H -0.1288 -0.0268 0.6023 0.036 Uiso 1 1 calc R . . C46 C -0.0864(4) 0.0393(7) 0.5564(3) 0.0208(19) Uani 1 1 d . . . C47 C -0.0805(4) 0.0376(6) 0.5144(3) 0.0221(19) Uani 1 1 d . . . C48 C 0.0036(5) 0.0495(9) 0.6155(3) 0.032(2) Uani 1 1 d . . . C49 C 0.0118(4) -0.0595(9) 0.6113(4) 0.038(3) Uani 1 1 d . . . H49 H -0.0067 -0.0966 0.5903 0.046 Uiso 1 1 calc R . . C50 C 0.0463(5) -0.1164(10) 0.6368(4) 0.048(3) Uani 1 1 d . . . H50 H 0.0509 -0.1923 0.6336 0.058 Uiso 1 1 calc R . . C51 C 0.0742(5) -0.0640(11) 0.6670(4) 0.058(4) Uani 1 1 d . . . H51 H 0.0976 -0.1036 0.6848 0.070 Uiso 1 1 calc R . . C52 C 0.0682(5) 0.0439(11) 0.6712(4) 0.055(3) Uani 1 1 d . . . H52 H 0.0889 0.0797 0.6914 0.066 Uiso 1 1 calc R . . C53 C 0.0330(5) 0.1039(9) 0.6470(3) 0.039(2) Uani 1 1 d . . . H53 H 0.0283 0.1794 0.6511 0.047 Uiso 1 1 calc R . . C54 C -0.0786(4) 0.2228(7) 0.6126(3) 0.027(2) Uani 1 1 d . . . C55 C -0.1330(4) 0.2010(8) 0.6273(3) 0.035(2) Uani 1 1 d . . . H55 H -0.1507 0.1335 0.6216 0.042 Uiso 1 1 calc R . . C56 C -0.1614(5) 0.2753(8) 0.6500(3) 0.038(3) Uani 1 1 d . . . H56 H -0.1987 0.2592 0.6597 0.046 Uiso 1 1 calc R . . C57 C -0.1357(5) 0.3761(9) 0.6590(4) 0.045(3) Uani 1 1 d . . . H57 H -0.1550 0.4282 0.6748 0.054 Uiso 1 1 calc R . . C58 C -0.0803(5) 0.3967(9) 0.6440(3) 0.039(3) Uani 1 1 d . . . H58 H -0.0618 0.4633 0.6498 0.047 Uiso 1 1 calc R . . C59 C -0.0532(4) 0.3213(7) 0.6211(3) 0.029(2) Uani 1 1 d . . . H59 H -0.0162 0.3369 0.6109 0.035 Uiso 1 1 calc R . . Ir2 Ir 0.136197(12) 0.79734(2) 0.358527(9) 0.01687(8) Uani 1 1 d . . . P3 P 0.19739(9) 0.66477(18) 0.37907(7) 0.0196(5) Uani 1 1 d . . . P4 P 0.19040(10) 0.86443(19) 0.30682(7) 0.0220(5) Uani 1 1 d . . . N5 N 0.0752(3) 0.9252(5) 0.3498(2) 0.0198(16) Uani 1 1 d . . . N6 N 0.0722(3) 0.7286(6) 0.3220(2) 0.0205(16) Uani 1 1 d . . . N7 N 0.0628(3) 0.6316(5) 0.3054(2) 0.0222(16) Uani 1 1 d . . . N8 N -0.0096(3) 0.7446(7) 0.2887(2) 0.0250(17) Uani 1 1 d . . . C60 C 0.0808(4) 1.0245(7) 0.3672(3) 0.026(2) Uani 1 1 d . . . H60 H 0.1123 1.0367 0.3844 0.031 Uiso 1 1 calc R . . C61 C 0.0431(4) 1.1061(7) 0.3608(3) 0.0286(19) Uani 1 1 d . . . H61 H 0.0489 1.1746 0.3728 0.034 Uiso 1 1 calc R . . C62 C -0.0043(4) 1.0895(8) 0.3366(3) 0.028(2) Uani 1 1 d . . . C63 C -0.0455(5) 1.1706(8) 0.3288(4) 0.043(3) Uani 1 1 d . . . H63 H -0.0407 1.2410 0.3396 0.051 Uiso 1 1 calc R . . C64 C -0.0925(5) 1.1480(9) 0.3056(4) 0.049(3) Uani 1 1 d . . . H64 H -0.1208 1.2021 0.3013 0.059 Uiso 1 1 calc R . . C65 C -0.0989(5) 1.0455(10) 0.2882(4) 0.054(3) Uani 1 1 d . . . H65 H -0.1309 1.0320 0.2716 0.065 Uiso 1 1 calc R . . C66 C -0.0602(4) 0.9658(8) 0.2947(3) 0.032(2) Uani 1 1 d . . . H66 H -0.0656 0.8968 0.2829 0.038 Uiso 1 1 calc R . . C67 C -0.0121(4) 0.9847(8) 0.3187(3) 0.029(2) Uani 1 1 d . . . C68 C 0.0308(4) 0.9060(7) 0.3265(3) 0.0212(18) Uani 1 1 d . . . C69 C 0.0287(4) 0.7947(7) 0.3119(3) 0.022(2) Uani 1 1 d . . . C70 C 0.0126(4) 0.6444(8) 0.2862(3) 0.025(2) Uani 1 1 d . A . C71 C -0.0136(4) 0.5544(8) 0.2620(3) 0.040(3) Uani 1 1 d D . . C72 C -0.0661(7) 0.5168(16) 0.2831(6) 0.070(6) Uiso 0.769(19) 1 d PD A 1 H72A H -0.0553 0.4880 0.3090 0.105 Uiso 0.769(19) 1 calc PR A 1 H72B H -0.0850 0.4600 0.2677 0.105 Uiso 0.769(19) 1 calc PR A 1 H72C H -0.0925 0.5777 0.2866 0.105 Uiso 0.769(19) 1 calc PR A 1 C73 C -0.0306(8) 0.6002(14) 0.2218(4) 0.055(5) Uiso 0.769(19) 1 d PD A 1 H73A H 0.0041 0.6144 0.2063 0.083 Uiso 0.769(19) 1 calc PR A 1 H73B H -0.0519 0.6678 0.2255 0.083 Uiso 0.769(19) 1 calc PR A 1 H73C H -0.0548 0.5478 0.2079 0.083 Uiso 0.769(19) 1 calc PR A 1 C74 C 0.0289(7) 0.4643(12) 0.2557(5) 0.053(5) Uiso 0.769(19) 1 d PD A 1 H74A H 0.0405 0.4344 0.2812 0.080 Uiso 0.769(19) 1 calc PR A 1 H74B H 0.0627 0.4925 0.2419 0.080 Uiso 0.769(19) 1 calc PR A 1 H74C H 0.0112 0.4072 0.2397 0.080 Uiso 0.769(19) 1 calc PR A 1 C72' C -0.004(2) 0.449(3) 0.2838(14) 0.049(11) Uiso 0.231(19) 1 d PD A 2 H72D H 0.0113 0.4647 0.3101 0.073 Uiso 0.231(19) 1 calc PR A 2 H72E H 0.0233 0.4046 0.2691 0.073 Uiso 0.231(19) 1 calc PR A 2 H72F H -0.0406 0.4107 0.2863 0.073 Uiso 0.231(19) 1 calc PR A 2 C73' C -0.0783(9) 0.558(4) 0.2635(17) 0.049(11) Uiso 0.231(19) 1 d PD A 2 H73D H -0.0914 0.5309 0.2892 0.073 Uiso 0.231(19) 1 calc PR A 2 H73E H -0.0941 0.5120 0.2426 0.073 Uiso 0.231(19) 1 calc PR A 2 H73F H -0.0915 0.6323 0.2599 0.073 Uiso 0.231(19) 1 calc PR A 2 C74' C 0.007(2) 0.555(4) 0.2205(8) 0.050(15) Uiso 0.231(19) 1 d PD A 2 H74D H 0.0431 0.5154 0.2187 0.076 Uiso 0.231(19) 1 calc PR A 2 H74E H 0.0126 0.6299 0.2119 0.076 Uiso 0.231(19) 1 calc PR A 2 H74F H -0.0219 0.5202 0.2036 0.076 Uiso 0.231(19) 1 calc PR A 2 C75 C 0.0892(4) 0.7484(7) 0.4087(2) 0.0210(18) Uani 1 1 d . . . C76 C 0.0360(4) 0.7872(7) 0.4190(3) 0.025(2) Uani 1 1 d . . . H76 H 0.0183 0.8398 0.4025 0.030 Uiso 1 1 calc R . . C77 C 0.0068(4) 0.7524(8) 0.4526(3) 0.026(2) Uani 1 1 d . . . H77 H -0.0302 0.7809 0.4580 0.031 Uiso 1 1 calc R . . C78 C 0.0300(4) 0.6783(7) 0.4782(3) 0.027(2) Uani 1 1 d . . . H78 H 0.0098 0.6567 0.5012 0.032 Uiso 1 1 calc R . . C79 C 0.0841(4) 0.6353(7) 0.4696(3) 0.025(2) Uani 1 1 d . . . C80 C 0.1113(4) 0.5609(7) 0.4953(3) 0.031(2) Uani 1 1 d . . . H80 H 0.0917 0.5362 0.5181 0.037 Uiso 1 1 calc R . . C81 C 0.1659(5) 0.5241(8) 0.4874(3) 0.035(2) Uani 1 1 d . . . H81 H 0.1846 0.4782 0.5059 0.042 Uiso 1 1 calc R . . C82 C 0.1943(4) 0.5535(8) 0.4523(3) 0.031(2) Uani 1 1 d . . . H82 H 0.2306 0.5225 0.4465 0.037 Uiso 1 1 calc R . . C83 C 0.1705(4) 0.6256(7) 0.4267(3) 0.026(2) Uani 1 1 d . . . C84 C 0.1144(4) 0.6700(7) 0.4346(3) 0.0214(19) Uani 1 1 d . . . C85 C 0.2086(3) 0.5333(6) 0.3547(3) 0.0211(17) Uani 1 1 d . . . C86 C 0.1688(4) 0.4919(7) 0.3285(3) 0.026(2) Uani 1 1 d . . . H86 H 0.1356 0.5325 0.3218 0.031 Uiso 1 1 calc R . . C87 C 0.1779(4) 0.3891(8) 0.3119(3) 0.031(2) Uani 1 1 d . . . H87 H 0.1519 0.3630 0.2926 0.037 Uiso 1 1 calc R . . C88 C 0.2241(5) 0.3247(8) 0.3232(3) 0.034(2) Uani 1 1 d . . . H88 H 0.2284 0.2538 0.3128 0.040 Uiso 1 1 calc R . . C89 C 0.2630(4) 0.3646(8) 0.3492(3) 0.036(3) Uani 1 1 d . . . H89 H 0.2952 0.3220 0.3566 0.043 Uiso 1 1 calc R . . C90 C 0.2559(4) 0.4697(7) 0.3654(3) 0.024(2) Uani 1 1 d . . . H90 H 0.2832 0.4970 0.3836 0.029 Uiso 1 1 calc R . . C91 C 0.2728(4) 0.7063(6) 0.3859(3) 0.0235(19) Uani 1 1 d D . . C92 C 0.3174(3) 0.7009(6) 0.3565(3) 0.0188(16) Uiso 1 1 d D . . H92A H 0.3096 0.6621 0.3329 0.023 Uiso 1 1 calc R . . C93 C 0.3668(4) 0.7452(8) 0.3602(4) 0.038(2) Uani 1 1 d D . . H93A H 0.3924 0.7474 0.3384 0.045 Uiso 1 1 calc R . . C94 C 0.3823(5) 0.7882(8) 0.3947(4) 0.045(3) Uani 1 1 d . . . H94 H 0.4202 0.8154 0.3978 0.053 Uiso 1 1 calc R . . C95 C 0.3453(4) 0.7940(7) 0.4251(4) 0.036(3) Uani 1 1 d . . . H95 H 0.3569 0.8268 0.4492 0.044 Uiso 1 1 calc R . . C96 C 0.2896(5) 0.7517(7) 0.4216(3) 0.030(2) Uani 1 1 d . . . H96 H 0.2638 0.7540 0.4432 0.037 Uiso 1 1 calc R . . C97 C 0.1895(3) 0.8969(7) 0.3924(2) 0.0183(17) Uani 1 1 d . . . C98 C 0.1828(4) 0.9131(6) 0.4325(2) 0.0205(18) Uani 1 1 d . . . H98 H 0.1517 0.8787 0.4456 0.025 Uiso 1 1 calc R . . C99 C 0.2204(4) 0.9789(7) 0.4545(3) 0.025(2) Uani 1 1 d . . . H99 H 0.2151 0.9864 0.4821 0.030 Uiso 1 1 calc R . . C100 C 0.2645(4) 1.0319(7) 0.4363(3) 0.029(2) Uani 1 1 d . . . H10A H 0.2906 1.0733 0.4516 0.035 Uiso 1 1 calc R . . C101 C 0.2716(4) 1.0260(7) 0.3950(3) 0.0225(19) Uani 1 1 d . . . C102 C 0.3139(4) 1.0848(7) 0.3753(3) 0.030(2) Uani 1 1 d . . . H10B H 0.3408 1.1258 0.3901 0.036 Uiso 1 1 calc R . . C103 C 0.3173(4) 1.0844(8) 0.3347(3) 0.033(2) Uani 1 1 d . . . H10C H 0.3449 1.1285 0.3219 0.039 Uiso 1 1 calc R . . C104 C 0.2799(4) 1.0186(7) 0.3120(3) 0.029(2) Uani 1 1 d . . . H10D H 0.2823 1.0188 0.2840 0.035 Uiso 1 1 calc R . . C105 C 0.2396(4) 0.9539(7) 0.3310(3) 0.0205(19) Uani 1 1 d . . . C106 C 0.2336(4) 0.9573(6) 0.3729(3) 0.0200(19) Uani 1 1 d . . . C107 C 0.1489(4) 0.9468(9) 0.2714(3) 0.030(2) Uani 1 1 d . . . C108 C 0.1386(4) 1.0556(9) 0.2798(4) 0.035(3) Uani 1 1 d . . . H10E H 0.1591 1.0907 0.3003 0.042 Uiso 1 1 calc R . . C109 C 0.0986(5) 1.1117(9) 0.2581(4) 0.046(3) Uani 1 1 d . . . H10F H 0.0902 1.1848 0.2646 0.056 Uiso 1 1 calc R . . C110 C 0.0705(6) 1.0629(13) 0.2270(4) 0.070(4) Uani 1 1 d . . . H11A H 0.0434 1.1024 0.2117 0.083 Uiso 1 1 calc R . . C111 C 0.0821(6) 0.9571(11) 0.2183(4) 0.062(4) Uani 1 1 d . . . H11B H 0.0634 0.9233 0.1966 0.075 Uiso 1 1 calc R . . C112 C 0.1213(5) 0.8982(10) 0.2410(3) 0.044(3) Uani 1 1 d . . . H11C H 0.1285 0.8243 0.2352 0.053 Uiso 1 1 calc R . . C113 C 0.2297(4) 0.7706(7) 0.2750(3) 0.024(2) Uani 1 1 d . . . C114 C 0.2857(4) 0.7872(8) 0.2610(3) 0.035(2) Uani 1 1 d . . . H11D H 0.3055 0.8516 0.2680 0.042 Uiso 1 1 calc R . . C115 C 0.3121(5) 0.7126(8) 0.2377(4) 0.044(3) Uani 1 1 d . . . H11E H 0.3498 0.7259 0.2281 0.053 Uiso 1 1 calc R . . C116 C 0.2837(4) 0.6158(8) 0.2278(3) 0.035(2) Uani 1 1 d . . . H11F H 0.3019 0.5640 0.2112 0.042 Uiso 1 1 calc R . . C117 C 0.2306(4) 0.5974(8) 0.2419(3) 0.034(2) Uani 1 1 d . . . H11G H 0.2118 0.5310 0.2362 0.041 Uiso 1 1 calc R . . C118 C 0.2027(4) 0.6753(7) 0.2650(3) 0.028(2) Uani 1 1 d . . . H11H H 0.1647 0.6623 0.2739 0.033 Uiso 1 1 calc R . . C119 C 0.1005(12) 0.2921(17) 0.1717(9) 0.161(11) Uiso 1 1 d . . . H11I H 0.0705 0.2583 0.1556 0.241 Uiso 1 1 calc R . . H11J H 0.1057 0.3674 0.1634 0.241 Uiso 1 1 calc R . . H11K H 0.0891 0.2901 0.1995 0.241 Uiso 1 1 calc R . . C120 C 0.1547(8) 0.2327(15) 0.1666(6) 0.095(5) Uiso 1 1 d . . . H12A H 0.1681 0.2351 0.1389 0.114 Uiso 1 1 calc R . . H12B H 0.1510 0.1564 0.1750 0.114 Uiso 1 1 calc R . . C121 C 0.1944(7) 0.2953(11) 0.1935(5) 0.075(4) Uiso 1 1 d . . . H12C H 0.1761 0.3090 0.2194 0.090 Uiso 1 1 calc R . . H12D H 0.2054 0.3654 0.1816 0.090 Uiso 1 1 calc R . . C122 C 0.2471(10) 0.2203(17) 0.1979(8) 0.130(8) Uiso 1 1 d . . . H12E H 0.2358 0.1543 0.2126 0.156 Uiso 1 1 calc R . . H12F H 0.2607 0.1980 0.1715 0.156 Uiso 1 1 calc R . . C123 C 0.2899(8) 0.2708(14) 0.2173(6) 0.087(5) Uiso 1 1 d D . . H12G H 0.2761 0.2926 0.2437 0.104 Uiso 1 1 calc R . . H12H H 0.3005 0.3373 0.2027 0.104 Uiso 1 1 calc R . . C124 C 0.3402(9) 0.2033(15) 0.2217(7) 0.133(9) Uiso 1 1 d D . . H12I H 0.3702 0.2437 0.2356 0.199 Uiso 1 1 calc R . . H12J H 0.3543 0.1820 0.1956 0.199 Uiso 1 1 calc R . . H12K H 0.3302 0.1384 0.2368 0.199 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01348(15) 0.01581(15) 0.02233(16) 0.0003(2) -0.00024(13) -0.00047(12) P1 0.0166(11) 0.0179(10) 0.0275(13) -0.0006(9) -0.0012(9) -0.0002(9) P2 0.0173(11) 0.0219(12) 0.0232(12) 0.0015(9) -0.0002(9) -0.0007(9) N1 0.014(3) 0.016(3) 0.025(4) -0.001(3) -0.003(3) 0.001(3) N2 0.017(4) 0.025(4) 0.030(4) -0.004(3) -0.004(3) -0.004(3) N3 0.015(3) 0.023(4) 0.030(4) -0.007(3) -0.002(3) -0.006(3) N4 0.023(4) 0.028(4) 0.028(4) -0.001(3) -0.001(3) -0.006(3) C1 0.024(4) 0.024(4) 0.028(6) 0.001(4) 0.000(4) -0.006(4) C2 0.034(5) 0.017(4) 0.032(5) -0.009(4) 0.002(5) 0.007(4) C3 0.029(5) 0.020(5) 0.039(6) 0.001(4) 0.005(5) 0.008(4) C4 0.043(6) 0.030(5) 0.045(7) -0.004(5) -0.010(5) 0.016(5) C5 0.052(7) 0.034(6) 0.074(9) -0.007(6) -0.026(7) 0.019(6) C6 0.044(7) 0.034(6) 0.064(8) -0.001(5) -0.027(6) 0.010(5) C7 0.030(5) 0.031(5) 0.060(7) -0.003(5) -0.019(5) 0.007(5) C8 0.020(5) 0.035(5) 0.027(5) 0.008(4) -0.007(4) -0.006(4) C9 0.013(4) 0.018(4) 0.032(5) 0.001(4) 0.000(4) 0.000(4) C10 0.017(4) 0.020(4) 0.021(5) 0.003(4) -0.005(4) 0.002(4) C11 0.023(5) 0.022(5) 0.036(6) -0.003(4) -0.009(4) -0.002(4) C12 0.027(5) 0.028(5) 0.025(5) -0.003(4) -0.005(4) -0.004(4) C13 0.052(7) 0.024(5) 0.074(9) -0.020(5) -0.031(6) 0.002(5) C14 0.063(8) 0.048(7) 0.042(7) -0.012(5) -0.008(6) -0.002(6) C15 0.043(7) 0.062(8) 0.060(8) -0.020(6) 0.012(6) -0.032(6) C16 0.015(4) 0.027(5) 0.027(5) -0.004(4) 0.004(4) -0.003(4) C17 0.022(5) 0.028(5) 0.023(5) -0.003(4) 0.003(4) 0.002(4) C18 0.018(4) 0.031(5) 0.034(6) -0.007(5) 0.010(4) 0.001(4) C19 0.031(5) 0.026(5) 0.023(5) 0.000(4) 0.007(4) -0.011(4) C20 0.020(4) 0.016(4) 0.027(5) -0.009(3) -0.001(4) 0.001(3) C21 0.040(6) 0.027(5) 0.026(5) -0.001(4) 0.006(4) -0.003(5) C22 0.035(5) 0.031(5) 0.027(5) 0.005(4) -0.001(4) 0.008(5) C23 0.024(5) 0.024(5) 0.027(5) -0.003(4) 0.001(4) 0.012(4) C24 0.019(4) 0.028(5) 0.029(5) 0.006(4) -0.001(4) 0.002(4) C25 0.017(4) 0.016(4) 0.021(4) 0.001(3) -0.003(4) -0.002(4) C26 0.014(4) 0.014(4) 0.032(5) 0.001(4) -0.001(3) 0.002(3) C27 0.050(6) 0.011(4) 0.030(5) 0.010(4) 0.009(5) -0.006(4) C29 0.021(5) 0.030(6) 0.074(9) 0.021(6) -0.012(5) -0.007(4) C30 0.038(6) 0.020(5) 0.039(6) 0.002(4) -0.018(5) -0.001(5) C31 0.025(5) 0.016(4) 0.036(6) 0.001(4) -0.011(4) 0.001(4) C32 0.019(4) 0.025(4) 0.028(5) 0.002(4) 0.003(4) 0.004(3) C33 0.024(5) 0.022(4) 0.043(6) 0.003(4) -0.001(4) 0.007(4) C34 0.026(5) 0.026(5) 0.040(6) -0.001(4) -0.002(4) 0.010(4) C35 0.039(6) 0.018(4) 0.045(6) -0.007(4) 0.005(5) 0.006(4) C36 0.025(5) 0.028(5) 0.035(6) -0.001(4) 0.000(4) -0.003(4) C37 0.029(5) 0.023(5) 0.029(5) 0.001(4) 0.007(4) -0.002(4) C38 0.013(4) 0.016(4) 0.030(5) -0.002(4) -0.003(4) 0.002(3) C39 0.021(4) 0.025(5) 0.025(5) -0.005(4) 0.002(4) 0.003(4) C40 0.030(5) 0.028(5) 0.027(5) -0.007(4) -0.006(4) 0.002(4) C41 0.027(5) 0.019(4) 0.022(5) 0.001(4) -0.003(4) 0.001(4) C42 0.023(5) 0.015(4) 0.034(5) 0.000(4) -0.001(4) -0.001(4) C43 0.019(5) 0.026(5) 0.046(6) 0.004(4) -0.004(4) -0.006(4) C44 0.027(5) 0.014(5) 0.044(7) 0.000(4) 0.010(5) -0.006(4) C45 0.020(5) 0.026(5) 0.043(6) 0.002(5) 0.011(4) -0.002(4) C46 0.018(4) 0.015(4) 0.030(5) 0.000(4) -0.007(4) 0.002(4) C47 0.021(4) 0.013(4) 0.032(5) 0.001(3) -0.002(4) 0.000(4) C48 0.026(5) 0.035(6) 0.034(6) 0.006(5) -0.001(4) -0.007(5) C49 0.026(6) 0.040(7) 0.049(8) 0.003(6) 0.004(5) 0.005(5) C50 0.045(7) 0.043(7) 0.056(8) 0.024(6) -0.009(6) 0.004(6) C51 0.046(7) 0.060(8) 0.069(9) 0.027(7) -0.016(7) 0.007(6) C52 0.049(7) 0.070(9) 0.046(7) 0.002(6) -0.022(6) 0.005(7) C53 0.033(6) 0.045(6) 0.038(6) 0.005(5) 0.001(5) 0.003(5) C54 0.018(4) 0.028(5) 0.034(5) 0.005(4) 0.001(4) 0.003(4) C55 0.027(5) 0.040(6) 0.040(6) -0.007(5) 0.009(4) -0.007(5) C56 0.027(5) 0.045(6) 0.043(6) 0.001(5) 0.010(5) 0.000(5) C57 0.043(7) 0.046(7) 0.046(7) -0.004(5) 0.008(5) 0.019(6) C58 0.050(7) 0.034(6) 0.034(6) 0.000(5) 0.004(5) -0.008(5) C59 0.028(5) 0.034(5) 0.026(5) 0.000(4) 0.006(4) -0.002(4) Ir2 0.01342(15) 0.01555(15) 0.02165(16) -0.0007(2) -0.00164(13) -0.00035(12) P3 0.0146(11) 0.0192(10) 0.0250(12) 0.0007(9) -0.0012(9) -0.0004(9) P4 0.0197(11) 0.0222(12) 0.0242(12) 0.0005(10) -0.0021(10) -0.0008(10) N5 0.017(3) 0.016(3) 0.027(4) 0.002(3) 0.000(3) 0.004(3) N6 0.022(4) 0.020(4) 0.020(4) 0.003(3) -0.008(3) -0.003(3) N7 0.014(3) 0.020(4) 0.033(4) -0.006(3) -0.006(3) 0.002(3) N8 0.020(4) 0.025(4) 0.030(5) -0.006(3) -0.004(3) 0.004(3) C60 0.022(4) 0.021(4) 0.034(6) -0.003(4) 0.001(4) -0.001(4) C61 0.024(4) 0.017(4) 0.045(6) -0.009(5) -0.004(5) 0.003(4) C62 0.026(5) 0.021(5) 0.037(6) 0.004(4) -0.003(4) 0.007(4) C63 0.037(6) 0.029(5) 0.062(8) -0.004(5) -0.008(6) 0.015(5) C64 0.031(6) 0.037(6) 0.079(9) -0.003(6) -0.020(6) 0.015(5) C65 0.040(7) 0.049(7) 0.073(9) -0.013(6) -0.024(6) 0.022(6) C66 0.022(5) 0.032(5) 0.041(6) -0.002(4) -0.007(4) 0.009(4) C67 0.025(5) 0.025(5) 0.036(6) -0.003(4) 0.002(4) 0.000(4) C68 0.022(4) 0.021(5) 0.021(5) 0.003(4) -0.003(4) 0.005(4) C69 0.016(4) 0.021(5) 0.031(5) -0.002(4) 0.001(4) 0.001(4) C70 0.018(5) 0.027(5) 0.030(6) -0.004(4) -0.008(4) 0.002(4) C71 0.020(5) 0.033(6) 0.067(8) -0.018(5) -0.012(5) 0.002(4) C75 0.027(5) 0.024(4) 0.013(4) -0.004(4) 0.002(4) -0.004(4) C76 0.021(5) 0.021(5) 0.034(6) -0.001(4) 0.005(4) 0.002(4) C77 0.018(4) 0.027(5) 0.033(6) -0.001(4) 0.005(4) -0.007(4) C78 0.022(4) 0.022(5) 0.036(6) 0.002(4) 0.002(4) -0.001(4) C79 0.029(5) 0.017(4) 0.029(5) 0.001(4) 0.004(4) -0.005(4) C80 0.038(6) 0.029(5) 0.026(5) 0.003(4) 0.000(4) 0.014(5) C81 0.046(6) 0.028(5) 0.031(6) 0.006(4) 0.003(5) 0.009(5) C82 0.030(5) 0.030(5) 0.033(6) 0.005(4) -0.007(4) 0.009(4) C83 0.026(5) 0.019(4) 0.032(5) -0.005(4) 0.000(4) 0.002(4) C84 0.022(5) 0.018(4) 0.023(5) -0.001(3) -0.001(4) -0.001(4) C85 0.020(4) 0.022(4) 0.022(5) -0.001(4) 0.003(4) -0.001(3) C86 0.026(5) 0.024(5) 0.028(5) -0.003(4) 0.004(4) 0.009(4) C87 0.032(5) 0.031(5) 0.030(5) -0.001(4) 0.008(4) -0.008(5) C88 0.042(6) 0.025(5) 0.034(6) -0.008(4) 0.003(5) 0.007(4) C89 0.031(5) 0.031(5) 0.045(7) -0.003(4) -0.001(5) 0.012(4) C90 0.021(4) 0.022(4) 0.028(6) 0.003(4) 0.000(4) 0.002(4) C91 0.027(5) 0.014(4) 0.029(5) 0.007(4) 0.000(4) 0.002(4) C93 0.014(4) 0.040(5) 0.060(7) 0.021(6) 0.005(5) -0.006(4) C94 0.030(6) 0.031(6) 0.073(9) -0.006(6) -0.012(6) -0.007(5) C95 0.027(5) 0.016(5) 0.066(8) 0.002(5) -0.025(5) -0.005(4) C96 0.027(5) 0.020(5) 0.045(6) 0.006(4) -0.005(5) 0.004(5) C97 0.016(4) 0.016(4) 0.023(4) -0.004(3) -0.003(3) -0.006(3) C98 0.021(4) 0.019(4) 0.022(4) -0.001(3) -0.001(4) -0.004(4) C99 0.025(5) 0.029(5) 0.020(5) -0.007(4) -0.008(4) 0.006(4) C100 0.024(5) 0.014(4) 0.048(6) -0.006(4) -0.009(4) 0.004(4) C101 0.012(4) 0.022(5) 0.033(5) -0.001(4) -0.002(4) 0.005(4) C102 0.024(5) 0.017(5) 0.049(6) -0.003(4) -0.014(4) 0.001(4) C103 0.025(5) 0.026(5) 0.048(7) 0.001(4) -0.006(5) -0.011(4) C104 0.028(5) 0.022(5) 0.038(6) 0.000(4) 0.001(4) -0.009(4) C105 0.018(4) 0.014(4) 0.030(5) 0.009(3) -0.003(4) -0.001(4) C106 0.014(4) 0.015(4) 0.031(5) -0.001(3) -0.001(3) -0.003(3) C107 0.020(5) 0.041(6) 0.029(6) 0.008(4) 0.005(4) 0.006(5) C108 0.032(6) 0.033(6) 0.039(7) 0.008(5) -0.001(5) -0.001(4) C109 0.047(7) 0.035(6) 0.057(7) 0.015(5) -0.014(6) 0.010(5) C110 0.070(9) 0.091(11) 0.048(8) -0.005(7) -0.021(7) 0.030(8) C111 0.072(10) 0.062(8) 0.054(8) -0.010(7) -0.031(7) 0.012(8) C112 0.041(6) 0.048(7) 0.043(7) -0.009(5) -0.020(5) 0.008(6) C113 0.023(5) 0.026(5) 0.021(5) 0.007(3) 0.006(4) 0.001(4) C114 0.028(5) 0.029(5) 0.049(6) -0.006(5) 0.016(5) -0.001(4) C115 0.036(6) 0.040(6) 0.057(7) 0.006(5) 0.025(5) 0.009(5) C116 0.036(6) 0.037(6) 0.032(6) -0.003(4) 0.019(5) 0.007(5) C117 0.046(6) 0.020(5) 0.037(6) -0.002(4) -0.006(5) 0.002(5) C118 0.030(5) 0.025(5) 0.028(5) 0.003(4) 0.000(4) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C38 2.071(8) . ? Ir1 C16 2.084(9) . ? Ir1 N2 2.117(7) . ? Ir1 N1 2.134(6) . ? Ir1 P1 2.281(2) . ? Ir1 P2 2.336(2) . ? P1 C24 1.817(10) . ? P1 C26 1.831(9) . ? P1 C32 1.836(9) . ? P2 C46 1.808(9) . ? P2 C48 1.827(11) . ? P2 C54 1.834(10) . ? N1 C9 1.359(11) . ? N1 C1 1.369(10) . ? N2 C10 1.349(11) . ? N2 N3 1.365(10) . ? N3 C11 1.353(11) . ? N4 C11 1.344(12) . ? N4 C10 1.350(12) . ? C1 C2 1.359(12) . ? C2 C3 1.420(14) . ? C3 C8 1.388(13) . ? C3 C4 1.410(13) . ? C4 C5 1.365(15) . ? C5 C6 1.390(15) . ? C6 C7 1.379(14) . ? C7 C8 1.428(13) . ? C8 C9 1.444(13) . ? C9 C10 1.437(12) . ? C11 C12 1.518(13) . ? C12 C14 1.507(14) . ? C12 C15 1.517(14) . ? C12 C13 1.554(14) . ? C16 C17 1.393(13) . ? C16 C25 1.431(13) . ? C17 C18 1.433(13) . ? C18 C19 1.364(14) . ? C19 C20 1.425(13) . ? C20 C25 1.404(12) . ? C20 C21 1.418(13) . ? C21 C22 1.353(14) . ? C22 C23 1.381(13) . ? C23 C24 1.415(12) . ? C24 C25 1.399(12) . ? C26 C31 1.384(13) . ? C26 C27 1.435(13) . ? C27 C28 1.334(13) . ? C28 C29 1.404(16) . ? C29 C30 1.374(17) . ? C30 C31 1.396(14) . ? C32 C37 1.374(13) . ? C32 C33 1.429(11) . ? C33 C34 1.381(12) . ? C34 C35 1.383(14) . ? C35 C36 1.386(13) . ? C36 C37 1.386(13) . ? C38 C39 1.375(13) . ? C38 C47 1.472(12) . ? C39 C40 1.418(13) . ? C40 C41 1.362(13) . ? C41 C42 1.417(13) . ? C42 C47 1.409(12) . ? C42 C43 1.425(13) . ? C43 C44 1.350(13) . ? C44 C45 1.405(14) . ? C45 C46 1.369(13) . ? C46 C47 1.429(13) . ? C48 C49 1.369(14) . ? C48 C53 1.437(15) . ? C49 C50 1.376(15) . ? C50 C51 1.374(17) . ? C51 C52 1.348(17) . ? C52 C53 1.375(15) . ? C54 C59 1.385(13) . ? C54 C55 1.386(13) . ? C55 C56 1.370(14) . ? C56 C57 1.417(15) . ? C57 C58 1.410(15) . ? C58 C59 1.367(14) . ? Ir2 C97 2.092(8) . ? Ir2 C75 2.112(9) . ? Ir2 N6 2.116(7) . ? Ir2 N5 2.147(6) . ? Ir2 P3 2.281(2) . ? Ir2 P4 2.315(2) . ? P3 C83 1.799(10) . ? P3 C85 1.842(8) . ? P3 C91 1.846(9) . ? P4 C105 1.793(9) . ? P4 C113 1.830(9) . ? P4 C107 1.846(10) . ? N5 C68 1.324(11) . ? N5 C60 1.369(10) . ? N6 N7 1.343(10) . ? N6 C69 1.345(11) . ? N7 C70 1.348(11) . ? N8 C69 1.341(12) . ? N8 C70 1.345(12) . ? C60 C61 1.356(11) . ? C61 C62 1.391(14) . ? C62 C63 1.414(13) . ? C62 C67 1.440(14) . ? C63 C64 1.377(15) . ? C64 C65 1.405(16) . ? C65 C66 1.352(14) . ? C66 C67 1.407(13) . ? C67 C68 1.419(13) . ? C68 C69 1.462(12) . ? C70 C71 1.511(13) . ? C71 C74' 1.484(19) . ? C71 C72 1.491(15) . ? C71 C74 1.507(14) . ? C71 C73' 1.508(19) . ? C71 C72' 1.510(19) . ? C71 C73 1.527(15) . ? C75 C76 1.374(13) . ? C75 C84 1.436(13) . ? C76 C77 1.396(14) . ? C77 C78 1.371(14) . ? C78 C79 1.398(13) . ? C79 C80 1.415(13) . ? C79 C84 1.447(12) . ? C80 C81 1.376(14) . ? C81 C82 1.410(14) . ? C82 C83 1.363(13) . ? C83 C84 1.443(13) . ? C85 C86 1.383(12) . ? C85 C90 1.401(11) . ? C86 C87 1.405(13) . ? C87 C88 1.393(14) . ? C88 C89 1.359(14) . ? C89 C90 1.421(12) . ? C91 C96 1.389(13) . ? C91 C92 1.440(11) . ? C92 C93 1.282(10) . ? C93 C94 1.336(17) . ? C94 C95 1.347(18) . ? C95 C96 1.404(14) . ? C97 C98 1.382(12) . ? C97 C106 1.433(11) . ? C98 C99 1.410(12) . ? C99 C100 1.365(13) . ? C100 C101 1.412(14) . ? C101 C102 1.395(13) . ? C101 C106 1.436(12) . ? C102 C103 1.377(14) . ? C103 C104 1.419(13) . ? C104 C105 1.392(12) . ? C105 C106 1.428(13) . ? C107 C112 1.356(15) . ? C107 C108 1.396(14) . ? C108 C109 1.375(14) . ? C109 C110 1.381(17) . ? C110 C111 1.367(18) . ? C111 C112 1.401(16) . ? C113 C118 1.377(13) . ? C113 C114 1.403(13) . ? C114 C115 1.362(13) . ? C115 C116 1.408(15) . ? C116 C117 1.348(14) . ? C117 C118 1.400(13) . ? C119 C120 1.47(3) . ? C120 C121 1.51(2) . ? C121 C122 1.55(2) . ? C122 C123 1.35(3) . ? C123 C124 1.447(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 Ir1 C16 92.0(4) . . ? C38 Ir1 N2 167.2(3) . . ? C16 Ir1 N2 88.8(4) . . ? C38 Ir1 N1 92.0(3) . . ? C16 Ir1 N1 90.5(3) . . ? N2 Ir1 N1 75.3(3) . . ? C38 Ir1 P1 84.0(2) . . ? C16 Ir1 P1 82.8(3) . . ? N2 Ir1 P1 108.7(2) . . ? N1 Ir1 P1 172.01(19) . . ? C38 Ir1 P2 83.6(3) . . ? C16 Ir1 P2 175.3(3) . . ? N2 Ir1 P2 95.0(2) . . ? N1 Ir1 P2 87.80(19) . . ? P1 Ir1 P2 98.59(8) . . ? C24 P1 C26 107.7(4) . . ? C24 P1 C32 102.7(4) . . ? C26 P1 C32 100.7(4) . . ? C24 P1 Ir1 102.2(3) . . ? C26 P1 Ir1 115.4(3) . . ? C32 P1 Ir1 126.4(3) . . ? C46 P2 C48 106.1(4) . . ? C46 P2 C54 109.3(4) . . ? C48 P2 C54 103.5(5) . . ? C46 P2 Ir1 102.8(3) . . ? C48 P2 Ir1 114.4(3) . . ? C54 P2 Ir1 120.0(3) . . ? C9 N1 C1 119.6(7) . . ? C9 N1 Ir1 117.4(5) . . ? C1 N1 Ir1 123.0(6) . . ? C10 N2 N3 107.7(7) . . ? C10 N2 Ir1 116.6(6) . . ? N3 N2 Ir1 135.6(6) . . ? C11 N3 N2 103.5(7) . . ? C11 N4 C10 101.9(7) . . ? C2 C1 N1 123.4(8) . . ? C1 C2 C3 118.9(8) . . ? C8 C3 C4 119.0(10) . . ? C8 C3 C2 118.8(8) . . ? C4 C3 C2 122.1(9) . . ? C5 C4 C3 120.5(10) . . ? C4 C5 C6 120.8(10) . . ? C7 C6 C5 120.6(10) . . ? C6 C7 C8 118.8(10) . . ? C3 C8 C7 120.3(9) . . ? C3 C8 C9 119.7(8) . . ? C7 C8 C9 120.0(9) . . ? N1 C9 C10 113.7(7) . . ? N1 C9 C8 119.5(8) . . ? C10 C9 C8 126.8(8) . . ? N2 C10 N4 112.0(8) . . ? N2 C10 C9 117.0(8) . . ? N4 C10 C9 131.0(8) . . ? N4 C11 N3 114.8(8) . . ? N4 C11 C12 122.4(8) . . ? N3 C11 C12 122.8(8) . . ? C14 C12 C15 110.3(9) . . ? C14 C12 C11 110.9(8) . . ? C15 C12 C11 108.2(8) . . ? C14 C12 C13 109.7(9) . . ? C15 C12 C13 108.0(9) . . ? C11 C12 C13 109.7(8) . . ? C17 C16 C25 116.7(9) . . ? C17 C16 Ir1 123.3(7) . . ? C25 C16 Ir1 120.0(6) . . ? C16 C17 C18 121.9(9) . . ? C19 C18 C17 120.1(9) . . ? C18 C19 C20 120.5(9) . . ? C25 C20 C21 118.6(8) . . ? C25 C20 C19 118.7(8) . . ? C21 C20 C19 122.6(9) . . ? C22 C21 C20 121.8(9) . . ? C21 C22 C23 120.6(9) . . ? C22 C23 C24 119.1(8) . . ? C25 C24 C23 120.9(8) . . ? C25 C24 P1 114.8(6) . . ? C23 C24 P1 124.1(7) . . ? C24 C25 C20 118.8(8) . . ? C24 C25 C16 119.0(8) . . ? C20 C25 C16 122.2(8) . . ? C31 C26 C27 117.2(9) . . ? C31 C26 P1 122.4(7) . . ? C27 C26 P1 120.2(7) . . ? C28 C27 C26 122.5(10) . . ? C27 C28 C29 119.8(10) . . ? C30 C29 C28 119.0(9) . . ? C29 C30 C31 121.6(10) . . ? C26 C31 C30 119.8(10) . . ? C37 C32 C33 118.8(8) . . ? C37 C32 P1 122.5(6) . . ? C33 C32 P1 118.7(7) . . ? C34 C33 C32 118.5(9) . . ? C33 C34 C35 122.4(9) . . ? C34 C35 C36 118.4(9) . . ? C37 C36 C35 120.6(9) . . ? C32 C37 C36 121.3(9) . . ? C39 C38 C47 116.5(8) . . ? C39 C38 Ir1 124.8(7) . . ? C47 C38 Ir1 118.6(6) . . ? C38 C39 C40 122.7(9) . . ? C41 C40 C39 121.0(9) . . ? C40 C41 C42 119.2(9) . . ? C47 C42 C41 120.7(8) . . ? C47 C42 C43 118.4(9) . . ? C41 C42 C43 120.9(9) . . ? C44 C43 C42 121.1(10) . . ? C43 C44 C45 120.7(10) . . ? C46 C45 C44 120.3(10) . . ? C45 C46 C47 120.1(9) . . ? C45 C46 P2 126.1(8) . . ? C47 C46 P2 113.8(7) . . ? C42 C47 C46 119.3(8) . . ? C42 C47 C38 119.6(8) . . ? C46 C47 C38 121.1(8) . . ? C49 C48 C53 118.2(11) . . ? C49 C48 P2 123.4(9) . . ? C53 C48 P2 118.2(8) . . ? C48 C49 C50 121.3(12) . . ? C51 C50 C49 120.3(12) . . ? C52 C51 C50 119.7(11) . . ? C51 C52 C53 122.2(12) . . ? C52 C53 C48 118.4(11) . . ? C59 C54 C55 119.2(9) . . ? C59 C54 P2 116.2(7) . . ? C55 C54 P2 124.6(7) . . ? C56 C55 C54 120.9(9) . . ? C55 C56 C57 120.5(10) . . ? C58 C57 C56 117.9(10) . . ? C59 C58 C57 120.4(10) . . ? C58 C59 C54 121.2(9) . . ? C97 Ir2 C75 91.9(3) . . ? C97 Ir2 N6 167.3(3) . . ? C75 Ir2 N6 89.5(3) . . ? C97 Ir2 N5 92.0(3) . . ? C75 Ir2 N5 88.8(3) . . ? N6 Ir2 N5 75.4(3) . . ? C97 Ir2 P3 83.3(2) . . ? C75 Ir2 P3 82.7(3) . . ? N6 Ir2 P3 109.3(2) . . ? N5 Ir2 P3 170.11(19) . . ? C97 Ir2 P4 83.2(2) . . ? C75 Ir2 P4 174.8(2) . . ? N6 Ir2 P4 94.9(2) . . ? N5 Ir2 P4 89.60(19) . . ? P3 Ir2 P4 98.50(8) . . ? C83 P3 C85 102.4(4) . . ? C83 P3 C91 107.1(4) . . ? C85 P3 C91 99.6(4) . . ? C83 P3 Ir2 104.5(3) . . ? C85 P3 Ir2 125.8(3) . . ? C91 P3 Ir2 115.7(3) . . ? C105 P4 C113 109.9(4) . . ? C105 P4 C107 107.0(4) . . ? C113 P4 C107 103.2(4) . . ? C105 P4 Ir2 102.9(3) . . ? C113 P4 Ir2 119.5(3) . . ? C107 P4 Ir2 113.9(3) . . ? C68 N5 C60 119.6(7) . . ? C68 N5 Ir2 117.9(5) . . ? C60 N5 Ir2 122.5(6) . . ? N7 N6 C69 108.3(7) . . ? N7 N6 Ir2 135.9(6) . . ? C69 N6 Ir2 115.8(6) . . ? N6 N7 C70 103.9(7) . . ? C69 N8 C70 102.0(7) . . ? C61 C60 N5 122.3(8) . . ? C60 C61 C62 120.0(8) . . ? C61 C62 C63 123.0(9) . . ? C61 C62 C67 118.8(8) . . ? C63 C62 C67 118.3(9) . . ? C64 C63 C62 120.2(10) . . ? C63 C64 C65 120.4(10) . . ? C66 C65 C64 121.2(11) . . ? C65 C66 C67 120.3(10) . . ? C66 C67 C68 123.7(9) . . ? C66 C67 C62 119.6(9) . . ? C68 C67 C62 116.7(9) . . ? N5 C68 C67 122.5(8) . . ? N5 C68 C69 113.3(8) . . ? C67 C68 C69 124.1(9) . . ? N8 C69 N6 111.7(8) . . ? N8 C69 C68 130.8(8) . . ? N6 C69 C68 117.5(8) . . ? N8 C70 N7 114.2(8) . . ? N8 C70 C71 123.8(8) . . ? N7 C70 C71 121.8(8) . . ? C74' C71 C72 136(2) . . ? C74' C71 C74 70(2) . . ? C72 C71 C74 112.2(12) . . ? C74' C71 C73' 111(3) . . ? C72 C71 C73' 34(2) . . ? C74 C71 C73' 133(2) . . ? C74' C71 C72' 115(3) . . ? C72 C71 C72' 68(2) . . ? C74 C71 C72' 48(2) . . ? C73' C71 C72' 99(3) . . ? C74' C71 C70 112(2) . . ? C72 C71 C70 107.5(11) . . ? C74 C71 C70 110.8(9) . . ? C73' C71 C70 111(2) . . ? C72' C71 C70 108(2) . . ? C74' C71 C73 40(2) . . ? C72 C71 C73 109.4(12) . . ? C74 C71 C73 108.5(12) . . ? C73' C71 C73 76(2) . . ? C72' C71 C73 142(2) . . ? C70 C71 C73 108.4(10) . . ? C76 C75 C84 116.8(8) . . ? C76 C75 Ir2 124.9(7) . . ? C84 C75 Ir2 118.3(6) . . ? C75 C76 C77 122.6(9) . . ? C78 C77 C76 122.1(9) . . ? C77 C78 C79 118.6(9) . . ? C78 C79 C80 121.6(9) . . ? C78 C79 C84 119.8(8) . . ? C80 C79 C84 118.6(8) . . ? C81 C80 C79 120.7(9) . . ? C80 C81 C82 120.8(9) . . ? C83 C82 C81 121.0(9) . . ? C82 C83 C84 119.9(9) . . ? C82 C83 P3 127.4(8) . . ? C84 C83 P3 112.3(7) . . ? C75 C84 C83 121.0(8) . . ? C75 C84 C79 120.2(8) . . ? C83 C84 C79 118.8(8) . . ? C86 C85 C90 119.1(8) . . ? C86 C85 P3 121.3(6) . . ? C90 C85 P3 119.3(7) . . ? C85 C86 C87 119.4(9) . . ? C88 C87 C86 121.6(9) . . ? C89 C88 C87 119.1(9) . . ? C88 C89 C90 120.3(9) . . ? C85 C90 C89 120.3(9) . . ? C96 C91 C92 114.8(9) . . ? C96 C91 P3 119.3(7) . . ? C92 C91 P3 125.9(7) . . ? C93 C92 C91 124.1(10) . . ? C92 C93 C94 119.9(12) . . ? C93 C94 C95 121.3(11) . . ? C94 C95 C96 120.4(11) . . ? C91 C96 C95 119.0(10) . . ? C98 C97 C106 117.3(7) . . ? C98 C97 Ir2 123.9(6) . . ? C106 C97 Ir2 118.6(6) . . ? C97 C98 C99 122.2(8) . . ? C100 C99 C98 120.4(9) . . ? C99 C100 C101 120.8(9) . . ? C102 C101 C100 122.1(9) . . ? C102 C101 C106 119.6(9) . . ? C100 C101 C106 118.3(8) . . ? C103 C102 C101 121.1(9) . . ? C102 C103 C104 120.6(10) . . ? C105 C104 C103 119.4(10) . . ? C104 C105 C106 120.7(9) . . ? C104 C105 P4 125.0(8) . . ? C106 C105 P4 114.3(6) . . ? C105 C106 C97 120.9(8) . . ? C105 C106 C101 118.4(8) . . ? C97 C106 C101 120.7(8) . . ? C112 C107 C108 119.9(10) . . ? C112 C107 P4 119.9(8) . . ? C108 C107 P4 119.4(9) . . ? C109 C108 C107 119.7(11) . . ? C108 C109 C110 120.6(12) . . ? C111 C110 C109 119.3(12) . . ? C110 C111 C112 120.5(12) . . ? C107 C112 C111 119.9(11) . . ? C118 C113 C114 117.8(8) . . ? C118 C113 P4 117.3(7) . . ? C114 C113 P4 124.9(7) . . ? C115 C114 C113 121.1(10) . . ? C114 C115 C116 120.2(10) . . ? C117 C116 C115 119.3(9) . . ? C116 C117 C118 120.6(9) . . ? C113 C118 C117 120.9(9) . . ? C119 C120 C121 101.4(16) . . ? C120 C121 C122 103.7(13) . . ? C123 C122 C121 110.9(16) . . ? C122 C123 C124 112.5(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 4.895 _refine_diff_density_min -2.061 _refine_diff_density_rms 0.182 data_complex_6b _database_code_depnum_ccdc_archive 'CCDC 787574' #TrackingRef '- xray-1_3_6a_6b_7a-NEW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H49 Cl2 Ir N4 P2' _chemical_formula_weight 1151.07 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6136(5) _cell_length_b 13.8180(6) _cell_length_c 17.5871(8) _cell_angle_alpha 83.412(1) _cell_angle_beta 74.040(1) _cell_angle_gamma 82.624(1) _cell_volume 2450.81(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5187 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.73 _exptl_crystal_description needle _exptl_crystal_colour orange-yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 2.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3207 _exptl_absorpt_correction_T_max 0.9169 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31716 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0679 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11214 _reflns_number_gt 9908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0344P)^2^+2.1715P] 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 11214 _refine_ls_number_parameters 621 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0840 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.066 _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 Ir Ir 0.480021(16) 0.234888(12) 0.206995(10) 0.01337(6) Uani 1 1 d . . . P1 P 0.49875(12) 0.14192(8) 0.32304(7) 0.0172(2) Uani 1 1 d . . . P2 P 0.65830(11) 0.17069(8) 0.11471(7) 0.0166(2) Uani 1 1 d . . . N1 N 0.5394(3) 0.3705(3) 0.2352(2) 0.0154(8) Uani 1 1 d . . . N2 N 0.3118(4) 0.3022(3) 0.2780(2) 0.0187(8) Uani 1 1 d . . . N3 N 0.1887(4) 0.2744(3) 0.3098(2) 0.0188(8) Uani 1 1 d . . . N4 N 0.1990(4) 0.4220(3) 0.3516(2) 0.0195(8) Uani 1 1 d . . . C1 C 0.3678(4) 0.1277(3) 0.1993(3) 0.0176(9) Uani 1 1 d . . . C2 C 0.3150(4) 0.1224(3) 0.1360(3) 0.0202(10) Uani 1 1 d . . . H2 H 0.3394 0.1661 0.0898 0.024 Uiso 1 1 calc R . . C3 C 0.2256(5) 0.0532(3) 0.1385(3) 0.0250(11) Uani 1 1 d . . . H3 H 0.1932 0.0510 0.0935 0.030 Uiso 1 1 calc R . . C4 C 0.1851(5) -0.0099(3) 0.2032(3) 0.0229(10) Uani 1 1 d . . . H4 H 0.1242 -0.0548 0.2037 0.028 Uiso 1 1 calc R . . C5 C 0.2344(4) -0.0080(3) 0.2701(3) 0.0228(10) Uani 1 1 d . . . C6 C 0.1973(5) -0.0721(3) 0.3392(3) 0.0262(11) Uani 1 1 d . . . H6 H 0.1373 -0.1182 0.3407 0.031 Uiso 1 1 calc R . . C7 C 0.2443(5) -0.0705(3) 0.4042(3) 0.0282(11) Uani 1 1 d . . . H7 H 0.2159 -0.1138 0.4501 0.034 Uiso 1 1 calc R . . C8 C 0.3358(5) -0.0036(3) 0.4021(3) 0.0244(10) Uani 1 1 d . . . H8 H 0.3702 -0.0026 0.4464 0.029 Uiso 1 1 calc R . . C9 C 0.3750(4) 0.0600(3) 0.3359(3) 0.0183(9) Uani 1 1 d . . . C10 C 0.3256(4) 0.0606(3) 0.2682(3) 0.0171(9) Uani 1 1 d . . . C11 C 0.6400(4) 0.0555(3) 0.3352(3) 0.0202(10) Uani 1 1 d . . . C12 C 0.7234(5) 0.0697(4) 0.3804(3) 0.0250(11) Uani 1 1 d . . . H12 H 0.7081 0.1272 0.4079 0.030 Uiso 1 1 calc R . . C13 C 0.8282(5) 0.0016(4) 0.3861(3) 0.0305(12) Uani 1 1 d . . . H13 H 0.8851 0.0125 0.4168 0.037 Uiso 1 1 calc R . . C14 C 0.8502(5) -0.0826(4) 0.3468(3) 0.0332(13) Uani 1 1 d . . . H14 H 0.9217 -0.1299 0.3511 0.040 Uiso 1 1 calc R . . C15 C 0.7684(5) -0.0980(4) 0.3014(3) 0.0309(12) Uani 1 1 d . . . H15 H 0.7844 -0.1556 0.2741 0.037 Uiso 1 1 calc R . . C16 C 0.6633(5) -0.0299(3) 0.2954(3) 0.0246(11) Uani 1 1 d . . . H16 H 0.6070 -0.0411 0.2644 0.029 Uiso 1 1 calc R . . C17 C 0.4601(5) 0.2167(3) 0.4068(3) 0.0215(9) Uani 1 1 d U . . C18 C 0.3416(5) 0.2182(4) 0.4653(3) 0.0269(10) Uani 1 1 d U . . H18 H 0.2809 0.1726 0.4671 0.032 Uiso 1 1 calc R . . C19 C 0.3121(5) 0.2873(4) 0.5215(3) 0.0322(11) Uani 1 1 d U . . H19 H 0.2310 0.2879 0.5615 0.039 Uiso 1 1 calc R . . C20 C 0.3985(6) 0.3545(4) 0.5199(3) 0.0325(11) Uani 1 1 d U . . H20 H 0.3766 0.4016 0.5579 0.039 Uiso 1 1 calc R . . C21 C 0.5172(5) 0.3523(4) 0.4623(3) 0.0294(11) Uani 1 1 d U . . H21 H 0.5778 0.3980 0.4605 0.035 Uiso 1 1 calc R . . C22 C 0.5466(5) 0.2843(4) 0.4083(3) 0.0277(10) Uani 1 1 d U . . H22 H 0.6294 0.2828 0.3698 0.033 Uiso 1 1 calc R . . C23 C 0.4411(4) 0.3180(3) 0.1075(3) 0.0179(9) Uani 1 1 d . . . C24 C 0.3464(4) 0.3959(3) 0.1086(3) 0.0202(10) Uani 1 1 d . . . H24 H 0.2929 0.4148 0.1586 0.024 Uiso 1 1 calc R . . C25 C 0.3247(5) 0.4496(4) 0.0389(3) 0.0265(11) Uani 1 1 d . . . H25 H 0.2594 0.5041 0.0434 0.032 Uiso 1 1 calc R . . C26 C 0.3957(5) 0.4245(3) -0.0345(3) 0.0262(11) Uani 1 1 d . . . H26 H 0.3777 0.4596 -0.0807 0.031 Uiso 1 1 calc R . . C27 C 0.4969(5) 0.3452(3) -0.0415(3) 0.0200(10) Uani 1 1 d . . . C28 C 0.5718(5) 0.3141(4) -0.1156(3) 0.0249(11) Uani 1 1 d . . . H28 H 0.5558 0.3478 -0.1628 0.030 Uiso 1 1 calc R . . C29 C 0.6677(5) 0.2360(4) -0.1211(3) 0.0277(11) Uani 1 1 d . . . H29 H 0.7153 0.2151 -0.1716 0.033 Uiso 1 1 calc R . . C30 C 0.6948(5) 0.1875(4) -0.0520(3) 0.0237(10) Uani 1 1 d . . . H30 H 0.7615 0.1341 -0.0555 0.028 Uiso 1 1 calc R . . C31 C 0.6238(4) 0.2177(3) 0.0213(3) 0.0195(10) Uani 1 1 d . . . C32 C 0.5205(4) 0.2947(3) 0.0294(3) 0.0178(9) Uani 1 1 d . . . C33 C 0.7072(4) 0.0399(3) 0.1023(3) 0.0196(10) Uani 1 1 d . . . C34 C 0.8376(5) -0.0011(4) 0.0909(3) 0.0279(11) Uani 1 1 d . . . H34 H 0.9039 0.0386 0.0917 0.033 Uiso 1 1 calc R . . C35 C 0.8707(6) -0.0994(4) 0.0785(3) 0.0372(13) Uani 1 1 d . . . H35 H 0.9597 -0.1265 0.0713 0.045 Uiso 1 1 calc R . . C36 C 0.7778(6) -0.1582(4) 0.0766(3) 0.0367(13) Uani 1 1 d . . . H36 H 0.8016 -0.2255 0.0682 0.044 Uiso 1 1 calc R . . C37 C 0.6486(6) -0.1183(4) 0.0870(4) 0.0383(14) Uani 1 1 d . . . H37 H 0.5831 -0.1586 0.0858 0.046 Uiso 1 1 calc R . . C38 C 0.6138(5) -0.0203(4) 0.0991(3) 0.0294(12) Uani 1 1 d . . . H38 H 0.5248 0.0063 0.1053 0.035 Uiso 1 1 calc R . . C39 C 0.8144(4) 0.2164(3) 0.1108(3) 0.0193(9) Uani 1 1 d . . . C40 C 0.8730(5) 0.1887(4) 0.1723(3) 0.0234(10) Uani 1 1 d . . . H40 H 0.8364 0.1409 0.2128 0.028 Uiso 1 1 calc R . . C41 C 0.9834(5) 0.2290(4) 0.1760(3) 0.0309(12) Uani 1 1 d . . . H41 H 1.0228 0.2087 0.2184 0.037 Uiso 1 1 calc R . . C42 C 1.0362(5) 0.2995(4) 0.1171(4) 0.0365(14) Uani 1 1 d . . . H42 H 1.1122 0.3276 0.1192 0.044 Uiso 1 1 calc R . . C43 C 0.9790(5) 0.3290(4) 0.0554(3) 0.0352(13) Uani 1 1 d . . . H43 H 1.0147 0.3781 0.0158 0.042 Uiso 1 1 calc R . . C44 C 0.8688(5) 0.2869(4) 0.0514(3) 0.0259(11) Uani 1 1 d . . . H44 H 0.8307 0.3061 0.0084 0.031 Uiso 1 1 calc R . . C45 C 0.6631(4) 0.4018(3) 0.2116(3) 0.0222(10) Uani 1 1 d . . . H45 H 0.7340 0.3587 0.1844 0.027 Uiso 1 1 calc R . . C46 C 0.6897(5) 0.4908(3) 0.2252(3) 0.0225(10) Uani 1 1 d . . . H46 H 0.7772 0.5088 0.2071 0.027 Uiso 1 1 calc R . . C47 C 0.5878(5) 0.5564(3) 0.2659(3) 0.0203(10) Uani 1 1 d . . . C48 C 0.6079(5) 0.6534(4) 0.2765(3) 0.0268(11) Uani 1 1 d . . . H48 H 0.6932 0.6751 0.2573 0.032 Uiso 1 1 calc R . . C49 C 0.5056(5) 0.7145(4) 0.3140(3) 0.0302(12) Uani 1 1 d . . . H49 H 0.5188 0.7800 0.3190 0.036 Uiso 1 1 calc R . . C50 C 0.3795(5) 0.6824(3) 0.3458(3) 0.0276(11) Uani 1 1 d . . . H50 H 0.3093 0.7255 0.3736 0.033 Uiso 1 1 calc R . . C51 C 0.3575(5) 0.5902(3) 0.3369(3) 0.0228(10) Uani 1 1 d . . . H51 H 0.2723 0.5691 0.3592 0.027 Uiso 1 1 calc R . . C52 C 0.4609(4) 0.5251(3) 0.2948(3) 0.0181(9) Uani 1 1 d . . . C53 C 0.4414(4) 0.4302(3) 0.2784(3) 0.0162(9) Uani 1 1 d . . . C54 C 0.3150(4) 0.3889(3) 0.3045(3) 0.0156(9) Uani 1 1 d . . . C55 C 0.1249(4) 0.3480(3) 0.3534(3) 0.0197(10) Uani 1 1 d . A . C56 C -0.0160(5) 0.3475(4) 0.4034(3) 0.0264(11) Uani 1 1 d . . . C57 C -0.0952(9) 0.4422(7) 0.3918(6) 0.037(3) Uiso 0.615(13) 1 d P A 1 H57A H -0.0971 0.4841 0.4335 0.055 Uiso 0.615(13) 1 calc PR A 1 H57B H -0.1853 0.4301 0.3943 0.055 Uiso 0.615(13) 1 calc PR A 1 H57C H -0.0554 0.4750 0.3398 0.055 Uiso 0.615(13) 1 calc PR A 1 C58 C -0.0111(10) 0.3351(8) 0.4933(6) 0.037(3) Uiso 0.615(13) 1 d P A 1 H58A H 0.0594 0.2843 0.4999 0.056 Uiso 0.615(13) 1 calc PR A 1 H58B H -0.0957 0.3161 0.5272 0.056 Uiso 0.615(13) 1 calc PR A 1 H58C H 0.0059 0.3973 0.5085 0.056 Uiso 0.615(13) 1 calc PR A 1 C59 C -0.0804(9) 0.2631(7) 0.3894(6) 0.032(2) Uiso 0.615(13) 1 d P A 1 H59A H -0.0245 0.2020 0.3953 0.048 Uiso 0.615(13) 1 calc PR A 1 H59B H -0.0925 0.2722 0.3357 0.048 Uiso 0.615(13) 1 calc PR A 1 H59C H -0.1664 0.2600 0.4282 0.048 Uiso 0.615(13) 1 calc PR A 1 C57' C -0.1051(15) 0.4135(11) 0.3485(10) 0.039(4) Uiso 0.385(13) 1 d P A 2 H57D H -0.0726 0.3959 0.2935 0.059 Uiso 0.385(13) 1 calc PR A 2 H57E H -0.0980 0.4832 0.3501 0.059 Uiso 0.385(13) 1 calc PR A 2 H57F H -0.1975 0.4005 0.3693 0.059 Uiso 0.385(13) 1 calc PR A 2 C58' C -0.0405(18) 0.3951(14) 0.4757(10) 0.052(5) Uiso 0.385(13) 1 d P A 2 H58D H 0.0096 0.3575 0.5104 0.077 Uiso 0.385(13) 1 calc PR A 2 H58E H -0.1347 0.3987 0.5028 0.077 Uiso 0.385(13) 1 calc PR A 2 H58F H -0.0130 0.4614 0.4630 0.077 Uiso 0.385(13) 1 calc PR A 2 C59' C -0.0589(15) 0.2444(11) 0.4161(10) 0.029(4) Uiso 0.385(13) 1 d P A 2 H59D H -0.0080 0.2024 0.4483 0.044 Uiso 0.385(13) 1 calc PR A 2 H59E H -0.0435 0.2179 0.3647 0.044 Uiso 0.385(13) 1 calc PR A 2 H59F H -0.1529 0.2467 0.4437 0.044 Uiso 0.385(13) 1 calc PR A 2 C60 C 0.1030(5) 0.6006(4) 0.2251(3) 0.0360(13) Uani 1 1 d . . . H60A H 0.1038 0.5352 0.2548 0.043 Uiso 1 1 calc R . . H60B H 0.1953 0.6127 0.1984 0.043 Uiso 1 1 calc R . . Cl1 Cl 0.01574(18) 0.6019(2) 0.15401(11) 0.0795(7) Uani 1 1 d . . . Cl2 Cl 0.0322(2) 0.68966(15) 0.29145(13) 0.0719(6) 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 Ir 0.01227(9) 0.01274(9) 0.01493(9) -0.00230(6) -0.00268(6) -0.00165(6) P1 0.0185(6) 0.0161(6) 0.0172(6) -0.0015(5) -0.0042(5) -0.0034(5) P2 0.0153(6) 0.0157(6) 0.0177(6) -0.0024(4) -0.0025(5) -0.0007(4) N1 0.0123(18) 0.0183(19) 0.0151(18) -0.0047(15) -0.0020(15) -0.0010(14) N2 0.020(2) 0.021(2) 0.0147(19) -0.0034(15) -0.0032(16) -0.0019(16) N3 0.0150(19) 0.021(2) 0.020(2) -0.0044(16) -0.0012(16) -0.0031(15) N4 0.0167(19) 0.0187(19) 0.022(2) -0.0046(16) -0.0016(16) -0.0016(15) C1 0.013(2) 0.015(2) 0.021(2) -0.0077(18) 0.0024(18) -0.0001(17) C2 0.018(2) 0.021(2) 0.024(2) -0.0032(19) -0.0094(19) -0.0006(18) C3 0.018(2) 0.025(3) 0.035(3) -0.014(2) -0.008(2) 0.001(2) C4 0.019(2) 0.020(2) 0.032(3) -0.010(2) -0.005(2) -0.0060(19) C5 0.017(2) 0.016(2) 0.035(3) -0.010(2) -0.003(2) -0.0012(18) C6 0.024(3) 0.021(2) 0.034(3) -0.004(2) -0.004(2) -0.007(2) C7 0.029(3) 0.017(2) 0.033(3) 0.003(2) 0.001(2) -0.006(2) C8 0.028(3) 0.023(2) 0.021(2) -0.001(2) -0.004(2) -0.005(2) C9 0.017(2) 0.013(2) 0.021(2) -0.0004(18) -0.0004(19) -0.0014(17) C10 0.012(2) 0.016(2) 0.022(2) -0.0085(18) -0.0002(18) -0.0019(17) C11 0.018(2) 0.017(2) 0.022(2) 0.0034(18) -0.0025(19) -0.0022(18) C12 0.024(3) 0.024(3) 0.029(3) -0.005(2) -0.009(2) 0.000(2) C13 0.023(3) 0.033(3) 0.040(3) -0.004(2) -0.017(2) -0.001(2) C14 0.021(3) 0.025(3) 0.051(4) -0.001(2) -0.008(2) 0.003(2) C15 0.028(3) 0.022(3) 0.039(3) -0.005(2) -0.003(2) -0.002(2) C16 0.025(3) 0.024(3) 0.028(3) -0.004(2) -0.010(2) -0.002(2) C17 0.026(2) 0.020(2) 0.019(2) -0.0004(17) -0.0069(18) -0.0006(18) C18 0.033(2) 0.026(2) 0.020(2) -0.0020(19) -0.0038(19) -0.005(2) C19 0.036(3) 0.033(2) 0.023(2) -0.005(2) -0.001(2) 0.003(2) C20 0.047(3) 0.029(2) 0.021(2) -0.010(2) -0.009(2) 0.004(2) C21 0.037(3) 0.026(2) 0.028(2) -0.0040(19) -0.013(2) -0.003(2) C22 0.042(3) 0.031(2) 0.0086(19) 0.0069(18) -0.0047(19) -0.007(2) C23 0.018(2) 0.018(2) 0.020(2) -0.0011(18) -0.0053(18) -0.0058(18) C24 0.018(2) 0.021(2) 0.022(2) -0.0010(19) -0.0059(19) -0.0015(18) C25 0.027(3) 0.021(2) 0.031(3) 0.003(2) -0.010(2) 0.001(2) C26 0.030(3) 0.021(2) 0.027(3) 0.008(2) -0.011(2) -0.003(2) C27 0.023(2) 0.019(2) 0.020(2) 0.0013(19) -0.0071(19) -0.0079(19) C28 0.027(3) 0.028(3) 0.020(2) 0.000(2) -0.007(2) -0.005(2) C29 0.032(3) 0.030(3) 0.020(3) -0.002(2) -0.004(2) -0.007(2) C30 0.022(2) 0.025(3) 0.024(3) -0.007(2) -0.003(2) -0.001(2) C31 0.020(2) 0.017(2) 0.022(2) -0.0002(18) -0.0049(19) -0.0069(18) C32 0.018(2) 0.017(2) 0.021(2) -0.0009(18) -0.0065(19) -0.0077(18) C33 0.021(2) 0.016(2) 0.017(2) -0.0032(18) -0.0003(19) 0.0039(18) C34 0.022(3) 0.024(3) 0.036(3) -0.006(2) -0.005(2) 0.001(2) C35 0.033(3) 0.027(3) 0.048(4) -0.009(3) -0.009(3) 0.011(2) C36 0.046(3) 0.017(3) 0.042(3) -0.008(2) -0.002(3) 0.000(2) C37 0.033(3) 0.026(3) 0.054(4) -0.016(3) -0.001(3) -0.011(2) C38 0.022(3) 0.024(3) 0.042(3) -0.013(2) -0.004(2) 0.000(2) C39 0.016(2) 0.020(2) 0.020(2) -0.0043(19) -0.0013(19) -0.0022(18) C40 0.020(2) 0.027(3) 0.025(3) -0.008(2) -0.008(2) 0.001(2) C41 0.021(3) 0.035(3) 0.039(3) -0.011(2) -0.012(2) 0.004(2) C42 0.021(3) 0.042(3) 0.048(4) -0.019(3) -0.003(2) -0.011(2) C43 0.029(3) 0.037(3) 0.038(3) -0.004(3) 0.002(2) -0.017(2) C44 0.025(3) 0.027(3) 0.025(3) -0.005(2) -0.003(2) -0.006(2) C45 0.015(2) 0.027(3) 0.025(3) -0.003(2) -0.0067(19) 0.0007(19) C46 0.017(2) 0.025(2) 0.026(3) -0.002(2) -0.004(2) -0.0078(19) C47 0.021(2) 0.021(2) 0.021(2) -0.0019(19) -0.0079(19) -0.0062(19) C48 0.027(3) 0.028(3) 0.030(3) -0.002(2) -0.011(2) -0.012(2) C49 0.038(3) 0.021(3) 0.034(3) -0.009(2) -0.011(2) -0.006(2) C50 0.029(3) 0.019(2) 0.032(3) -0.009(2) -0.004(2) 0.003(2) C51 0.021(2) 0.022(2) 0.025(3) -0.008(2) -0.005(2) -0.0033(19) C52 0.022(2) 0.014(2) 0.020(2) 0.0000(18) -0.0087(19) -0.0009(18) C53 0.015(2) 0.017(2) 0.016(2) 0.0002(17) -0.0043(18) -0.0013(17) C54 0.015(2) 0.015(2) 0.018(2) -0.0021(17) -0.0048(18) 0.0001(17) C55 0.016(2) 0.022(2) 0.019(2) -0.0030(19) -0.0023(18) -0.0011(18) C56 0.017(2) 0.028(3) 0.032(3) -0.009(2) 0.003(2) -0.008(2) C60 0.033(3) 0.034(3) 0.039(3) -0.004(3) -0.006(3) 0.002(2) Cl1 0.0437(10) 0.152(2) 0.0462(10) -0.0144(12) -0.0056(8) -0.0314(12) Cl2 0.0639(12) 0.0643(12) 0.0845(14) -0.0399(11) -0.0077(11) 0.0085(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir C1 2.054(4) . ? Ir N2 2.056(4) . ? Ir C23 2.090(4) . ? Ir N1 2.201(4) . ? Ir P2 2.2830(11) . ? Ir P1 2.3261(12) . ? P1 C9 1.794(5) . ? P1 C17 1.820(5) . ? P1 C11 1.838(5) . ? P2 C31 1.811(5) . ? P2 C39 1.829(5) . ? P2 C33 1.836(4) . ? N1 C53 1.352(5) . ? N1 C45 1.374(6) . ? N2 C54 1.342(5) . ? N2 N3 1.359(5) . ? N3 C55 1.341(6) . ? N4 C54 1.339(5) . ? N4 C55 1.359(6) . ? C1 C2 1.391(6) . ? C1 C10 1.441(6) . ? C2 C3 1.420(6) . ? C3 C4 1.356(7) . ? C4 C5 1.417(7) . ? C5 C6 1.413(7) . ? C5 C10 1.430(6) . ? C6 C7 1.370(7) . ? C7 C8 1.414(7) . ? C8 C9 1.376(6) . ? C9 C10 1.426(6) . ? C11 C12 1.387(6) . ? C11 C16 1.400(6) . ? C12 C13 1.380(7) . ? C13 C14 1.381(7) . ? C14 C15 1.380(7) . ? C15 C16 1.383(7) . ? C17 C18 1.388(7) . ? C17 C22 1.398(7) . ? C18 C19 1.398(7) . ? C19 C20 1.379(8) . ? C20 C21 1.381(7) . ? C21 C22 1.361(7) . ? C23 C24 1.373(6) . ? C23 C32 1.447(6) . ? C24 C25 1.418(6) . ? C25 C26 1.362(7) . ? C26 C27 1.423(7) . ? C27 C28 1.409(7) . ? C27 C32 1.426(6) . ? C28 C29 1.378(7) . ? C29 C30 1.402(7) . ? C30 C31 1.383(6) . ? C31 C32 1.416(6) . ? C33 C38 1.389(7) . ? C33 C34 1.396(6) . ? C34 C35 1.385(7) . ? C35 C36 1.365(8) . ? C36 C37 1.382(8) . ? C37 C38 1.382(7) . ? C39 C40 1.384(6) . ? C39 C44 1.397(6) . ? C40 C41 1.380(7) . ? C41 C42 1.388(8) . ? C42 C43 1.381(8) . ? C43 C44 1.393(7) . ? C45 C46 1.358(6) . ? C46 C47 1.405(6) . ? C47 C52 1.408(6) . ? C47 C48 1.424(6) . ? C48 C49 1.352(7) . ? C49 C50 1.409(7) . ? C50 C51 1.356(6) . ? C51 C52 1.420(6) . ? C52 C53 1.426(6) . ? C53 C54 1.461(6) . ? C55 C56 1.512(6) . ? C56 C58' 1.443(17) . ? C56 C57 1.488(10) . ? C56 C59 1.500(10) . ? C56 C59' 1.524(15) . ? C56 C58 1.586(10) . ? C56 C57' 1.655(16) . ? C60 Cl2 1.746(6) . ? C60 Cl1 1.747(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir N2 87.17(15) . . ? C1 Ir C23 92.71(17) . . ? N2 Ir C23 89.97(16) . . ? C1 Ir N1 162.00(14) . . ? N2 Ir N1 74.91(14) . . ? C23 Ir N1 85.68(15) . . ? C1 Ir P2 92.38(12) . . ? N2 Ir P2 172.65(11) . . ? C23 Ir P2 82.72(13) . . ? N1 Ir P2 105.17(10) . . ? C1 Ir P1 83.42(13) . . ? N2 Ir P1 84.99(11) . . ? C23 Ir P1 173.78(12) . . ? N1 Ir P1 96.49(10) . . ? P2 Ir P1 102.25(4) . . ? C9 P1 C17 110.3(2) . . ? C9 P1 C11 101.0(2) . . ? C17 P1 C11 105.0(2) . . ? C9 P1 Ir 101.31(15) . . ? C17 P1 Ir 111.72(15) . . ? C11 P1 Ir 126.32(15) . . ? C31 P2 C39 104.7(2) . . ? C31 P2 C33 103.3(2) . . ? C39 P2 C33 102.4(2) . . ? C31 P2 Ir 103.31(15) . . ? C39 P2 Ir 114.99(15) . . ? C33 P2 Ir 125.86(15) . . ? C53 N1 C45 117.3(4) . . ? C53 N1 Ir 115.6(3) . . ? C45 N1 Ir 127.1(3) . . ? C54 N2 N3 107.6(3) . . ? C54 N2 Ir 119.8(3) . . ? N3 N2 Ir 132.5(3) . . ? C55 N3 N2 103.9(4) . . ? C54 N4 C55 101.4(4) . . ? C2 C1 C10 116.7(4) . . ? C2 C1 Ir 124.6(3) . . ? C10 C1 Ir 118.2(3) . . ? C1 C2 C3 121.7(4) . . ? C4 C3 C2 121.9(5) . . ? C3 C4 C5 119.4(4) . . ? C6 C5 C4 122.4(4) . . ? C6 C5 C10 118.3(4) . . ? C4 C5 C10 119.4(4) . . ? C7 C6 C5 122.7(4) . . ? C6 C7 C8 119.2(5) . . ? C9 C8 C7 120.1(5) . . ? C8 C9 C10 121.6(4) . . ? C8 C9 P1 124.3(4) . . ? C10 C9 P1 114.0(3) . . ? C9 C10 C5 118.2(4) . . ? C9 C10 C1 120.8(4) . . ? C5 C10 C1 121.0(4) . . ? C12 C11 C16 118.8(4) . . ? C12 C11 P1 124.4(4) . . ? C16 C11 P1 116.8(4) . . ? C13 C12 C11 120.9(5) . . ? C12 C13 C14 119.9(5) . . ? C15 C14 C13 120.1(5) . . ? C14 C15 C16 120.4(5) . . ? C15 C16 C11 120.0(5) . . ? C18 C17 C22 117.4(4) . . ? C18 C17 P1 123.2(4) . . ? C22 C17 P1 118.9(4) . . ? C17 C18 C19 119.7(5) . . ? C20 C19 C18 121.2(5) . . ? C19 C20 C21 119.2(5) . . ? C22 C21 C20 119.5(5) . . ? C21 C22 C17 122.9(5) . . ? C24 C23 C32 115.3(4) . . ? C24 C23 Ir 125.8(3) . . ? C32 C23 Ir 118.9(3) . . ? C23 C24 C25 123.2(4) . . ? C26 C25 C24 121.2(4) . . ? C25 C26 C27 119.5(4) . . ? C28 C27 C26 122.3(4) . . ? C28 C27 C32 119.4(4) . . ? C26 C27 C32 118.2(4) . . ? C29 C28 C27 121.4(5) . . ? C28 C29 C30 119.8(5) . . ? C31 C30 C29 119.7(5) . . ? C30 C31 C32 122.0(4) . . ? C30 C31 P2 124.7(4) . . ? C32 C31 P2 113.2(3) . . ? C31 C32 C27 117.5(4) . . ? C31 C32 C23 120.1(4) . . ? C27 C32 C23 122.4(4) . . ? C38 C33 C34 118.0(4) . . ? C38 C33 P2 119.5(3) . . ? C34 C33 P2 122.4(4) . . ? C35 C34 C33 120.3(5) . . ? C36 C35 C34 121.2(5) . . ? C35 C36 C37 119.1(5) . . ? C36 C37 C38 120.5(5) . . ? C37 C38 C33 120.9(5) . . ? C40 C39 C44 118.9(4) . . ? C40 C39 P2 119.5(4) . . ? C44 C39 P2 121.3(4) . . ? C41 C40 C39 121.5(5) . . ? C40 C41 C42 119.2(5) . . ? C43 C42 C41 120.4(5) . . ? C42 C43 C44 120.0(5) . . ? C43 C44 C39 120.0(5) . . ? C46 C45 N1 123.7(4) . . ? C45 C46 C47 120.0(4) . . ? C46 C47 C52 118.1(4) . . ? C46 C47 C48 122.4(4) . . ? C52 C47 C48 119.5(4) . . ? C49 C48 C47 120.0(5) . . ? C48 C49 C50 120.8(5) . . ? C51 C50 C49 120.5(5) . . ? C50 C51 C52 120.5(4) . . ? C47 C52 C51 118.6(4) . . ? C47 C52 C53 118.3(4) . . ? C51 C52 C53 123.0(4) . . ? N1 C53 C52 122.5(4) . . ? N1 C53 C54 113.6(4) . . ? C52 C53 C54 124.0(4) . . ? N4 C54 N2 112.7(4) . . ? N4 C54 C53 131.4(4) . . ? N2 C54 C53 116.0(4) . . ? N3 C55 N4 114.4(4) . . ? N3 C55 C56 123.1(4) . . ? N4 C55 C56 122.4(4) . . ? C58' C56 C57 73.7(9) . . ? C58' C56 C59 127.9(9) . . ? C57 C56 C59 111.1(6) . . ? C58' C56 C55 113.0(8) . . ? C57 C56 C55 111.6(5) . . ? C59 C56 C55 112.2(5) . . ? C58' C56 C59' 113.9(10) . . ? C57 C56 C59' 128.4(8) . . ? C59 C56 C59' 22.7(6) . . ? C55 C56 C59' 110.8(7) . . ? C58' C56 C58 34.1(7) . . ? C57 C56 C58 107.0(6) . . ? C59 C56 C58 107.7(6) . . ? C55 C56 C58 106.7(5) . . ? C59' C56 C58 87.2(7) . . ? C58' C56 C57' 106.9(10) . . ? C57 C56 C57' 34.0(6) . . ? C59 C56 C57' 84.7(7) . . ? C55 C56 C57' 104.9(6) . . ? C59' C56 C57' 106.6(9) . . ? C58 C56 C57' 137.9(7) . . ? Cl2 C60 Cl1 111.2(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.593 _refine_diff_density_min -1.345 _refine_diff_density_rms 0.141 data_complxe_7a _database_code_depnum_ccdc_archive 'CCDC 787575' #TrackingRef '- xray-1_3_6a_6b_7a-NEW.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H35 F3 Ir N5 P2' _chemical_formula_weight 1028.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8887(6) _cell_length_b 18.6773(10) _cell_length_c 18.6889(11) _cell_angle_alpha 90.00 _cell_angle_beta 91.080(1) _cell_angle_gamma 90.00 _cell_volume 4149.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5889 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.33 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 3.353 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5000 _exptl_absorpt_correction_T_max 0.7303 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31752 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9539 _reflns_number_gt 8554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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. ; _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^)+(0.0296P)^2^+1.8547P] 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 9539 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0331 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0634 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.474100(9) 0.264326(6) 0.254743(5) 0.01571(4) Uani 1 1 d . . . P1 P 0.44485(6) 0.35818(4) 0.17488(4) 0.01904(15) Uani 1 1 d . . . P2 P 0.66436(6) 0.25616(4) 0.24237(4) 0.01706(15) Uani 1 1 d . . . N1 N 0.3011(2) 0.27266(12) 0.28387(12) 0.0185(5) Uani 1 1 d . . . N2 N 0.39245(19) 0.18484(13) 0.19008(12) 0.0193(5) Uani 1 1 d . . . N3 N 0.4258(2) 0.13320(13) 0.14513(13) 0.0235(5) Uani 1 1 d . . . N4 N 0.4915(2) 0.50029(14) 0.19965(14) 0.0294(6) Uani 1 1 d . . . N5 N 0.8136(2) 0.18721(14) 0.33284(13) 0.0261(6) Uani 1 1 d . . . C1 C 0.5170(2) 0.34532(15) 0.32505(15) 0.0189(6) Uani 1 1 d . . . C2 C 0.5407(2) 0.33610(16) 0.39761(15) 0.0228(6) Uani 1 1 d . . . H2 H 0.5376 0.2893 0.4173 0.027 Uiso 1 1 calc R . . C3 C 0.5693(3) 0.39416(18) 0.44314(16) 0.0278(7) Uani 1 1 d . . . H3 H 0.5851 0.3852 0.4923 0.033 Uiso 1 1 calc R . . C4 C 0.5746(3) 0.46246(17) 0.41825(17) 0.0297(7) Uani 1 1 d . . . H4 H 0.5951 0.5006 0.4495 0.036 Uiso 1 1 calc R . . C5 C 0.5493(2) 0.47615(16) 0.34548(16) 0.0245(6) Uani 1 1 d . . . C6 C 0.5529(3) 0.54497(17) 0.31362(19) 0.0313(7) Uani 1 1 d . . . H6 H 0.5750 0.5851 0.3417 0.038 Uiso 1 1 calc R . . C7 C 0.5252(3) 0.55413(18) 0.24381(18) 0.0343(8) Uani 1 1 d . . . H7 H 0.5295 0.6011 0.2245 0.041 Uiso 1 1 calc R . . C8 C 0.4905(2) 0.43519(16) 0.22788(16) 0.0229(6) Uani 1 1 d . . . C9 C 0.5193(2) 0.41820(15) 0.29992(15) 0.0206(6) Uani 1 1 d . . . C10 C 0.5159(2) 0.35884(16) 0.08917(15) 0.0214(6) Uani 1 1 d . . . C11 C 0.5365(3) 0.29305(18) 0.05785(16) 0.0276(7) Uani 1 1 d . . . H11 H 0.5119 0.2504 0.0804 0.033 Uiso 1 1 calc R . . C12 C 0.5929(3) 0.2892(2) -0.00597(17) 0.0374(8) Uani 1 1 d . . . H12 H 0.6074 0.2439 -0.0269 0.045 Uiso 1 1 calc R . . C13 C 0.6281(3) 0.3508(2) -0.03937(17) 0.0364(8) Uani 1 1 d . . . H13 H 0.6670 0.3479 -0.0832 0.044 Uiso 1 1 calc R . . C14 C 0.6069(3) 0.4166(2) -0.00918(17) 0.0351(8) Uani 1 1 d . . . H14 H 0.6310 0.4590 -0.0324 0.042 Uiso 1 1 calc R . . C15 C 0.5503(3) 0.42113(18) 0.05500(16) 0.0283(7) Uani 1 1 d . . . H15 H 0.5352 0.4666 0.0755 0.034 Uiso 1 1 calc R . . C16 C 0.2986(3) 0.37597(17) 0.15087(16) 0.0261(7) Uani 1 1 d . . . C17 C 0.2455(3) 0.33219(19) 0.10028(18) 0.0345(8) Uani 1 1 d . . . H17 H 0.2879 0.2977 0.0749 0.041 Uiso 1 1 calc R . . C18 C 0.1312(3) 0.3389(2) 0.0869(2) 0.0476(10) Uani 1 1 d . . . H18 H 0.0957 0.3087 0.0524 0.057 Uiso 1 1 calc R . . C19 C 0.0687(3) 0.3883(2) 0.1225(2) 0.0525(12) Uani 1 1 d . . . H19 H -0.0098 0.3923 0.1129 0.063 Uiso 1 1 calc R . . C20 C 0.1198(3) 0.4319(2) 0.1718(2) 0.0512(11) Uani 1 1 d . . . H20 H 0.0762 0.4665 0.1962 0.061 Uiso 1 1 calc R . . C21 C 0.2348(3) 0.4266(2) 0.18726(19) 0.0380(8) Uani 1 1 d . . . H21 H 0.2692 0.4570 0.2220 0.046 Uiso 1 1 calc R . . C22 C 0.5011(2) 0.18434(15) 0.33120(14) 0.0188(6) Uani 1 1 d . . . C23 C 0.4187(3) 0.14621(17) 0.36487(17) 0.0277(7) Uani 1 1 d . . . H23 H 0.3423 0.1555 0.3523 0.033 Uiso 1 1 calc R . . C24 C 0.4428(3) 0.09347(18) 0.41764(18) 0.0331(8) Uani 1 1 d . . . H24 H 0.3825 0.0686 0.4392 0.040 Uiso 1 1 calc R . . C25 C 0.5504(3) 0.07775(18) 0.43802(17) 0.0308(7) Uani 1 1 d . . . H25 H 0.5650 0.0426 0.4737 0.037 Uiso 1 1 calc R . . C26 C 0.6403(3) 0.11418(16) 0.40556(15) 0.0255(7) Uani 1 1 d . . . C27 C 0.7551(3) 0.10406(17) 0.42336(16) 0.0287(7) Uani 1 1 d . . . H27 H 0.7761 0.0715 0.4603 0.034 Uiso 1 1 calc R . . C28 C 0.8358(3) 0.14058(18) 0.38804(17) 0.0303(7) Uani 1 1 d . . . H28 H 0.9120 0.1334 0.4024 0.036 Uiso 1 1 calc R . . C29 C 0.7061(2) 0.19761(15) 0.31714(14) 0.0196(6) Uani 1 1 d . . . C30 C 0.6147(2) 0.16556(15) 0.35135(14) 0.0197(6) Uani 1 1 d . . . C31 C 0.7434(2) 0.33909(16) 0.25490(16) 0.0215(6) Uani 1 1 d . . . C32 C 0.7501(3) 0.38760(17) 0.19855(18) 0.0280(7) Uani 1 1 d . . . H32 H 0.7187 0.3753 0.1531 0.034 Uiso 1 1 calc R . . C33 C 0.8019(3) 0.45334(18) 0.2077(2) 0.0382(9) Uani 1 1 d . . . H33 H 0.8050 0.4862 0.1690 0.046 Uiso 1 1 calc R . . C34 C 0.8490(3) 0.47102(19) 0.2734(2) 0.0453(10) Uani 1 1 d . . . H34 H 0.8853 0.5160 0.2796 0.054 Uiso 1 1 calc R . . C35 C 0.8437(3) 0.4244(2) 0.3296(2) 0.0387(9) Uani 1 1 d . . . H35 H 0.8762 0.4372 0.3747 0.046 Uiso 1 1 calc R . . C36 C 0.7910(2) 0.35802(18) 0.32117(17) 0.0277(7) Uani 1 1 d . . . H36 H 0.7874 0.3258 0.3604 0.033 Uiso 1 1 calc R . . C37 C 0.7308(2) 0.21462(16) 0.16498(14) 0.0194(6) Uani 1 1 d . . . C38 C 0.6788(2) 0.15498(16) 0.13517(16) 0.0245(6) Uani 1 1 d . . . H38 H 0.6141 0.1355 0.1570 0.029 Uiso 1 1 calc R . . C39 C 0.7199(3) 0.12332(18) 0.07391(17) 0.0305(7) Uani 1 1 d . . . H39 H 0.6834 0.0824 0.0542 0.037 Uiso 1 1 calc R . . C40 C 0.8138(3) 0.15111(18) 0.04138(17) 0.0314(7) Uani 1 1 d . . . H40 H 0.8400 0.1309 -0.0019 0.038 Uiso 1 1 calc R . . C41 C 0.8690(3) 0.20853(19) 0.07248(18) 0.0350(8) Uani 1 1 d . . . H41 H 0.9352 0.2267 0.0513 0.042 Uiso 1 1 calc R . . C42 C 0.8291(3) 0.24006(17) 0.13425(18) 0.0287(7) Uani 1 1 d . . . H42 H 0.8687 0.2790 0.1556 0.034 Uiso 1 1 calc R . . C43 C 0.2602(2) 0.31940(16) 0.33139(15) 0.0230(6) Uani 1 1 d . . . H43 H 0.3112 0.3494 0.3572 0.028 Uiso 1 1 calc R . . C44 C 0.1470(3) 0.32526(17) 0.34391(16) 0.0276(7) Uani 1 1 d . . . H44 H 0.1206 0.3590 0.3778 0.033 Uiso 1 1 calc R . . C45 C 0.0714(3) 0.28169(17) 0.30690(18) 0.0295(7) Uani 1 1 d . . . H45 H -0.0071 0.2848 0.3151 0.035 Uiso 1 1 calc R . . C46 C 0.1129(3) 0.23402(16) 0.25815(18) 0.0263(7) Uani 1 1 d . . . H46 H 0.0628 0.2040 0.2316 0.032 Uiso 1 1 calc R . . C47 C 0.2277(2) 0.22957(15) 0.24757(15) 0.0206(6) Uani 1 1 d . . . C48 C 0.2792(2) 0.18014(16) 0.19895(15) 0.0207(6) Uani 1 1 d . . . C49 C 0.2368(3) 0.12386(17) 0.15771(16) 0.0266(7) Uani 1 1 d . . . H49 H 0.1612 0.1079 0.1526 0.032 Uiso 1 1 calc R . . C50 C 0.3321(3) 0.09691(17) 0.12602(16) 0.0261(7) Uani 1 1 d . . . C51 C 0.3404(3) 0.03678(19) 0.07524(19) 0.0364(8) Uani 1 1 d . . . F1 F 0.4278(2) -0.00570(13) 0.08773(14) 0.0649(8) Uani 1 1 d . . . F2 F 0.2490(2) -0.00472(14) 0.07538(15) 0.0723(8) Uani 1 1 d . . . F3 F 0.3504(3) 0.05740(15) 0.00777(13) 0.0780(9) 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 Ir 0.01324(6) 0.01573(6) 0.01822(6) -0.00048(4) 0.00182(4) -0.00030(4) P1 0.0163(4) 0.0193(4) 0.0215(3) 0.0014(3) 0.0029(3) 0.0012(3) P2 0.0145(4) 0.0170(4) 0.0198(3) -0.0001(3) 0.0026(3) -0.0004(3) N1 0.0179(12) 0.0156(12) 0.0221(11) 0.0045(9) 0.0038(9) 0.0006(9) N2 0.0154(12) 0.0201(13) 0.0224(11) -0.0032(10) -0.0001(9) 0.0000(10) N3 0.0213(13) 0.0227(13) 0.0264(12) -0.0054(10) 0.0003(10) 0.0003(10) N4 0.0319(15) 0.0199(14) 0.0369(15) 0.0010(11) 0.0111(12) 0.0041(12) N5 0.0213(13) 0.0287(15) 0.0281(13) -0.0001(11) -0.0016(10) 0.0031(11) C1 0.0119(13) 0.0187(14) 0.0263(14) -0.0031(11) 0.0058(11) 0.0001(11) C2 0.0223(15) 0.0223(16) 0.0240(14) -0.0008(12) 0.0047(12) -0.0025(12) C3 0.0229(16) 0.0360(19) 0.0246(15) -0.0072(13) 0.0022(12) -0.0048(14) C4 0.0261(17) 0.0281(18) 0.0352(17) -0.0146(14) 0.0063(13) -0.0059(14) C5 0.0188(15) 0.0205(15) 0.0344(16) -0.0067(13) 0.0085(12) -0.0021(12) C6 0.0280(17) 0.0182(16) 0.048(2) -0.0102(14) 0.0112(15) -0.0021(13) C7 0.039(2) 0.0152(16) 0.049(2) 0.0002(14) 0.0174(16) 0.0025(14) C8 0.0209(15) 0.0196(15) 0.0286(15) -0.0025(12) 0.0098(12) 0.0021(12) C9 0.0149(14) 0.0189(15) 0.0282(15) -0.0040(12) 0.0065(11) -0.0003(11) C10 0.0180(14) 0.0261(16) 0.0201(13) 0.0032(12) 0.0003(11) 0.0027(12) C11 0.0283(17) 0.0277(17) 0.0268(15) 0.0019(13) -0.0005(13) 0.0036(14) C12 0.041(2) 0.043(2) 0.0289(17) -0.0040(15) 0.0027(15) 0.0145(17) C13 0.0245(17) 0.061(3) 0.0244(16) 0.0011(16) 0.0069(13) 0.0037(16) C14 0.0284(18) 0.045(2) 0.0324(17) 0.0094(15) 0.0027(14) -0.0099(16) C15 0.0293(17) 0.0277(17) 0.0279(15) 0.0010(13) 0.0009(13) -0.0017(14) C16 0.0190(15) 0.0308(18) 0.0287(15) 0.0138(13) 0.0021(12) 0.0021(13) C17 0.0245(17) 0.042(2) 0.0373(18) 0.0124(16) -0.0040(14) -0.0058(15) C18 0.028(2) 0.063(3) 0.051(2) 0.025(2) -0.0087(17) -0.0135(19) C19 0.0180(18) 0.076(3) 0.063(3) 0.037(2) 0.0027(18) 0.0068(19) C20 0.033(2) 0.061(3) 0.060(3) 0.025(2) 0.0140(19) 0.023(2) C21 0.0287(18) 0.044(2) 0.0413(19) 0.0129(16) 0.0063(15) 0.0129(16) C22 0.0196(14) 0.0167(14) 0.0202(13) -0.0009(11) 0.0006(11) -0.0021(11) C23 0.0212(16) 0.0267(17) 0.0351(17) 0.0082(13) -0.0005(13) -0.0023(13) C24 0.0295(18) 0.0308(18) 0.0393(18) 0.0128(15) 0.0049(14) -0.0081(15) C25 0.0368(19) 0.0260(17) 0.0296(16) 0.0104(13) -0.0006(14) -0.0012(14) C26 0.0306(17) 0.0230(16) 0.0229(14) -0.0014(12) -0.0024(12) 0.0020(13) C27 0.0327(18) 0.0255(17) 0.0277(15) 0.0030(13) -0.0049(13) 0.0080(14) C28 0.0235(17) 0.0351(19) 0.0321(16) 0.0019(14) -0.0072(13) 0.0061(14) C29 0.0190(14) 0.0188(15) 0.0210(13) -0.0026(11) -0.0020(11) 0.0030(11) C30 0.0185(14) 0.0205(15) 0.0201(13) -0.0041(11) 0.0009(11) -0.0006(12) C31 0.0121(13) 0.0199(15) 0.0327(15) -0.0060(12) 0.0053(11) -0.0003(11) C32 0.0199(15) 0.0236(16) 0.0408(18) 0.0030(14) 0.0043(13) 0.0000(13) C33 0.0283(18) 0.0226(17) 0.064(2) 0.0052(17) 0.0160(17) -0.0008(14) C34 0.032(2) 0.0251(19) 0.080(3) -0.0181(19) 0.0202(19) -0.0099(15) C35 0.0233(17) 0.042(2) 0.051(2) -0.0251(18) 0.0076(15) -0.0078(15) C36 0.0160(15) 0.0287(17) 0.0384(17) -0.0099(14) 0.0046(13) -0.0002(13) C37 0.0167(14) 0.0206(14) 0.0208(13) -0.0005(11) 0.0010(11) 0.0044(11) C38 0.0154(14) 0.0259(16) 0.0324(16) -0.0050(13) 0.0040(12) 0.0007(12) C39 0.0287(17) 0.0276(18) 0.0350(17) -0.0108(14) -0.0019(14) 0.0027(14) C40 0.0363(19) 0.0314(18) 0.0268(16) -0.0032(13) 0.0080(14) 0.0114(15) C41 0.0338(19) 0.0331(19) 0.0387(18) 0.0003(15) 0.0202(15) -0.0009(16) C42 0.0247(17) 0.0271(17) 0.0347(17) -0.0050(13) 0.0091(13) -0.0051(13) C43 0.0198(15) 0.0259(16) 0.0234(14) -0.0013(12) 0.0042(11) 0.0014(12) C44 0.0249(16) 0.0261(17) 0.0320(16) 0.0007(13) 0.0105(13) 0.0041(13) C45 0.0175(15) 0.0303(18) 0.0410(18) 0.0047(14) 0.0092(13) 0.0040(13) C46 0.0162(15) 0.0251(16) 0.0378(17) 0.0026(13) 0.0006(13) -0.0026(12) C47 0.0159(14) 0.0212(15) 0.0247(14) 0.0034(11) 0.0026(11) -0.0004(11) C48 0.0146(14) 0.0209(15) 0.0265(14) 0.0007(12) -0.0002(11) -0.0007(11) C49 0.0182(15) 0.0269(17) 0.0346(16) -0.0045(13) -0.0018(12) -0.0036(13) C50 0.0238(16) 0.0249(17) 0.0297(15) -0.0056(13) -0.0021(12) 0.0003(13) C51 0.0308(19) 0.035(2) 0.043(2) -0.0145(16) -0.0077(15) -0.0020(15) F1 0.0511(15) 0.0490(15) 0.0937(19) -0.0385(14) -0.0230(13) 0.0235(12) F2 0.0465(15) 0.0629(17) 0.108(2) -0.0544(16) 0.0062(14) -0.0206(13) F3 0.131(3) 0.0645(18) 0.0388(13) -0.0209(12) 0.0039(15) 0.0019(17) _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 Ir C1 2.062(3) . ? Ir C22 2.088(3) . ? Ir N2 2.136(2) . ? Ir N1 2.143(2) . ? Ir P2 2.2831(8) . ? Ir P1 2.3243(7) . ? P1 C16 1.818(3) . ? P1 C10 1.825(3) . ? P1 C8 1.823(3) . ? P2 C31 1.825(3) . ? P2 C37 1.833(3) . ? P2 C29 1.836(3) . ? N1 C43 1.343(4) . ? N1 C47 1.359(4) . ? N2 N3 1.344(3) . ? N2 C48 1.363(4) . ? N3 C50 1.346(4) . ? N4 C8 1.325(4) . ? N4 C7 1.357(4) . ? N5 C29 1.320(4) . ? N5 C28 1.372(4) . ? C1 C2 1.390(4) . ? C1 C9 1.440(4) . ? C2 C3 1.416(4) . ? C3 C4 1.360(5) . ? C4 C5 1.411(4) . ? C5 C6 1.418(4) . ? C5 C9 1.419(4) . ? C6 C7 1.351(5) . ? C8 C9 1.419(4) . ? C10 C11 1.385(4) . ? C10 C15 1.393(4) . ? C11 C12 1.381(4) . ? C12 C13 1.378(5) . ? C13 C14 1.377(5) . ? C14 C15 1.388(4) . ? C16 C17 1.392(5) . ? C16 C21 1.397(5) . ? C17 C18 1.383(5) . ? C18 C19 1.365(6) . ? C19 C20 1.365(6) . ? C20 C21 1.395(5) . ? C22 C23 1.374(4) . ? C22 C30 1.438(4) . ? C23 C24 1.419(4) . ? C24 C25 1.360(5) . ? C25 C26 1.414(4) . ? C26 C27 1.411(4) . ? C26 C30 1.424(4) . ? C27 C28 1.358(5) . ? C29 C30 1.405(4) . ? C31 C32 1.393(4) . ? C31 C36 1.397(4) . ? C32 C33 1.383(4) . ? C33 C34 1.379(5) . ? C34 C35 1.368(5) . ? C35 C36 1.397(5) . ? C37 C38 1.386(4) . ? C37 C42 1.396(4) . ? C38 C39 1.386(4) . ? C39 C40 1.382(5) . ? C40 C41 1.380(5) . ? C41 C42 1.388(4) . ? C43 C44 1.375(4) . ? C44 C45 1.387(4) . ? C45 C46 1.372(4) . ? C46 C47 1.386(4) . ? C47 C48 1.440(4) . ? C48 C49 1.392(4) . ? C49 C50 1.384(4) . ? C50 C51 1.475(4) . ? C51 F1 1.325(4) . ? C51 F3 1.326(4) . ? C51 F2 1.335(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir C22 93.20(11) . . ? C1 Ir N2 167.15(10) . . ? C22 Ir N2 87.27(10) . . ? C1 Ir N1 90.68(10) . . ? C22 Ir N1 90.82(10) . . ? N2 Ir N1 76.47(9) . . ? C1 Ir P2 83.10(8) . . ? C22 Ir P2 83.20(8) . . ? N2 Ir P2 109.68(6) . . ? N1 Ir P2 171.09(6) . . ? C1 Ir P1 83.58(8) . . ? C22 Ir P1 176.71(8) . . ? N2 Ir P1 95.74(7) . . ? N1 Ir P1 88.60(6) . . ? P2 Ir P1 97.00(3) . . ? C16 P1 C10 103.79(13) . . ? C16 P1 C8 105.28(15) . . ? C10 P1 C8 109.49(13) . . ? C16 P1 Ir 115.29(10) . . ? C10 P1 Ir 120.17(10) . . ? C8 P1 Ir 101.92(10) . . ? C31 P2 C37 103.41(13) . . ? C31 P2 C29 106.06(13) . . ? C37 P2 C29 103.54(13) . . ? C31 P2 Ir 116.06(9) . . ? C37 P2 Ir 123.40(9) . . ? C29 P2 Ir 102.53(9) . . ? C43 N1 C47 118.6(3) . . ? C43 N1 Ir 125.2(2) . . ? C47 N1 Ir 116.12(19) . . ? N3 N2 C48 109.5(2) . . ? N3 N2 Ir 135.73(18) . . ? C48 N2 Ir 114.56(18) . . ? N2 N3 C50 105.9(2) . . ? C8 N4 C7 116.3(3) . . ? C29 N5 C28 115.6(3) . . ? C2 C1 C9 115.5(3) . . ? C2 C1 Ir 125.0(2) . . ? C9 C1 Ir 119.5(2) . . ? C1 C2 C3 122.2(3) . . ? C4 C3 C2 121.7(3) . . ? C3 C4 C5 119.3(3) . . ? C4 C5 C6 124.2(3) . . ? C4 C5 C9 119.1(3) . . ? C6 C5 C9 116.7(3) . . ? C7 C6 C5 120.8(3) . . ? C6 C7 N4 123.9(3) . . ? N4 C8 C9 125.4(3) . . ? N4 C8 P1 120.8(2) . . ? C9 C8 P1 113.8(2) . . ? C8 C9 C5 116.9(3) . . ? C8 C9 C1 121.0(3) . . ? C5 C9 C1 122.1(3) . . ? C11 C10 C15 119.4(3) . . ? C11 C10 P1 117.0(2) . . ? C15 C10 P1 123.6(2) . . ? C12 C11 C10 120.3(3) . . ? C13 C12 C11 120.3(3) . . ? C14 C13 C12 120.0(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C10 119.8(3) . . ? C17 C16 C21 119.0(3) . . ? C17 C16 P1 118.7(3) . . ? C21 C16 P1 122.0(3) . . ? C18 C17 C16 120.1(4) . . ? C19 C18 C17 121.0(4) . . ? C20 C19 C18 119.5(4) . . ? C19 C20 C21 121.3(4) . . ? C20 C21 C16 119.1(4) . . ? C23 C22 C30 115.3(3) . . ? C23 C22 Ir 125.6(2) . . ? C30 C22 Ir 119.0(2) . . ? C22 C23 C24 122.8(3) . . ? C25 C24 C23 121.4(3) . . ? C24 C25 C26 119.4(3) . . ? C27 C26 C25 124.8(3) . . ? C27 C26 C30 116.8(3) . . ? C25 C26 C30 118.4(3) . . ? C28 C27 C26 120.4(3) . . ? C27 C28 N5 123.9(3) . . ? N5 C29 C30 126.2(3) . . ? N5 C29 P2 120.2(2) . . ? C30 C29 P2 113.5(2) . . ? C29 C30 C26 117.0(3) . . ? C29 C30 C22 120.5(3) . . ? C26 C30 C22 122.5(3) . . ? C32 C31 C36 118.5(3) . . ? C32 C31 P2 119.5(2) . . ? C36 C31 P2 121.8(2) . . ? C33 C32 C31 121.0(3) . . ? C34 C33 C32 119.7(3) . . ? C35 C34 C33 120.5(3) . . ? C34 C35 C36 120.3(3) . . ? C35 C36 C31 119.9(3) . . ? C38 C37 C42 118.6(3) . . ? C38 C37 P2 117.5(2) . . ? C42 C37 P2 123.9(2) . . ? C37 C38 C39 120.9(3) . . ? C40 C39 C38 120.2(3) . . ? C41 C40 C39 119.2(3) . . ? C40 C41 C42 120.8(3) . . ? C41 C42 C37 120.0(3) . . ? N1 C43 C44 122.1(3) . . ? C43 C44 C45 119.7(3) . . ? C46 C45 C44 118.3(3) . . ? C45 C46 C47 120.1(3) . . ? N1 C47 C46 121.2(3) . . ? N1 C47 C48 114.8(3) . . ? C46 C47 C48 124.0(3) . . ? N2 C48 C49 109.3(3) . . ? N2 C48 C47 117.9(2) . . ? C49 C48 C47 132.8(3) . . ? C50 C49 C48 102.7(3) . . ? N3 C50 C49 112.6(3) . . ? N3 C50 C51 119.3(3) . . ? C49 C50 C51 128.1(3) . . ? F1 C51 F3 104.9(3) . . ? F1 C51 F2 106.7(3) . . ? F3 C51 F2 105.0(3) . . ? F1 C51 C50 113.9(3) . . ? F3 C51 C50 113.5(3) . . ? F2 C51 C50 112.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.283 _refine_diff_density_min -0.596 _refine_diff_density_rms 0.096