# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Jose Mata' 'Eduardo Peris' 'Alessandro Zanardi' _publ_contact_author_name 'Jose A. Mata' _publ_contact_author_address ; Inorganic and Organic University Jaume I Avd. Vicent Sos Baynat s/n Castellon Castellon 12071 SPAIN ; _publ_contact_author_email JMATA@QIO.UJI.ES _publ_section_title ;Alkenyl-functionalized NHC Iridium-based catalysts for hydrosilylation. ; data_str871m _database_code_depnum_ccdc_archive 'CCDC 656989' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H32 Cl Ir N2' _chemical_formula_weight 540.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0233(11) _cell_length_b 13.9740(14) _cell_length_c 14.7666(15) _cell_angle_alpha 64.168(2) _cell_angle_beta 85.560(3) _cell_angle_gamma 89.213(2) _cell_volume 2225.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.612 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 6.124 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12840 _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7842 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Hydrogen atoms could not be found in the difference maps and had been added in 'idealized' positions. No reliance should be placed on the reported ethylenic H-atom coordinates ; _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^)+(0.0504P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7842 _refine_ls_number_parameters 451 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.002 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 0.62645(3) 0.90041(3) 0.27258(3) 0.05867(15) Uani 1 1 d . . . N1 N 0.4286(7) 0.7822(7) 0.2443(7) 0.068(2) Uani 1 1 d . . . C1 C 0.4851(8) 0.8767(8) 0.2176(8) 0.059(3) Uani 1 1 d . . . N2 N 0.4281(7) 0.9483(7) 0.1456(6) 0.065(2) Uani 1 1 d . . . C2 C 0.3410(8) 0.7986(10) 0.1860(9) 0.080(3) Uani 1 1 d . . . H2 H 0.2912 0.7469 0.1888 0.096 Uiso 1 1 calc R . . C3 C 0.3396(8) 0.9017(10) 0.1247(9) 0.079(3) Uani 1 1 d . . . H3 H 0.2887 0.9358 0.0769 0.095 Uiso 1 1 calc R . . C4 C 0.4654(9) 0.6777(8) 0.3179(8) 0.073(3) Uani 1 1 d D . . H4A H 0.4024 0.6391 0.3640 0.088 Uiso 1 1 calc R . . H4B H 0.5211 0.6883 0.3570 0.088 Uiso 1 1 calc R . . Cl1 Cl 0.7255(2) 0.8874(2) 0.1343(2) 0.0798(8) Uani 1 1 d . . . C5 C 0.5140(9) 0.6128(8) 0.2662(8) 0.083(3) Uani 1 1 d D . . H5A H 0.5816 0.6483 0.2257 0.100 Uiso 1 1 calc R . . H5B H 0.4614 0.6098 0.2209 0.100 Uiso 1 1 calc R . . Cl31 Cl 0.7897(2) 0.4681(2) 0.6803(2) 0.0852(9) Uani 1 1 d . . . C6 C 0.5416(11) 0.4987(8) 0.3398(11) 0.114(5) Uani 1 1 d DU . . H6A H 0.5983 0.5017 0.3819 0.136 Uiso 1 1 calc R . . H6B H 0.4753 0.4650 0.3836 0.136 Uiso 1 1 calc R . . C7 C 0.580(2) 0.4347(15) 0.291(2) 0.219(13) Uani 1 1 d DU . . H7 H 0.5207 0.4173 0.2641 0.263 Uiso 1 1 calc R . . C8 C 0.650(2) 0.402(2) 0.275(2) 0.252(15) Uani 1 1 d DU . . H8A H 0.7179 0.4116 0.2966 0.302 Uiso 1 1 calc R . . H8B H 0.6464 0.3617 0.2390 0.302 Uiso 1 1 calc R . . C9 C 0.4578(9) 1.0587(8) 0.0899(8) 0.075(3) Uani 1 1 d . . . H9A H 0.4605 1.0768 0.0185 0.090 Uiso 1 1 calc R . . H9B H 0.5323 1.0698 0.1050 0.090 Uiso 1 1 calc R . . C10 C 0.3813(13) 1.1330(10) 0.1104(12) 0.130(6) Uani 1 1 d . . . H10A H 0.3841 1.1204 0.1802 0.155 Uiso 1 1 calc R . . H10B H 0.3055 1.1181 0.1012 0.155 Uiso 1 1 calc R . . C11 C 0.4107(18) 1.2499(13) 0.0418(15) 0.181(10) Uani 1 1 d D . . H11A H 0.4258 1.2589 -0.0270 0.217 Uiso 1 1 calc R . . H11B H 0.3471 1.2928 0.0432 0.217 Uiso 1 1 calc R . . C12 C 0.512(3) 1.2895(17) 0.073(3) 0.238(16) Uani 1 1 d D . . H12 H 0.5361 1.2403 0.1338 0.286 Uiso 1 1 calc R . . C13 C 0.556(5) 1.355(4) 0.043(4) 0.62(3) Uani 1 1 d . . . H13A H 0.5387 1.4097 -0.0183 0.738 Uiso 1 1 calc R . . H13B H 0.6160 1.3633 0.0753 0.738 Uiso 1 1 calc R . . C14 C 0.5409(10) 0.9661(11) 0.3618(10) 0.089(4) Uani 1 1 d . . . H14 H 0.4892 0.9904 0.3134 0.107 Uiso 1 1 calc R . . C15 C 0.5486(9) 0.8562(10) 0.4185(8) 0.077(3) Uani 1 1 d . . . H15 H 0.5006 0.8115 0.4073 0.093 Uiso 1 1 calc R . . C16 C 0.6325(11) 0.8063(11) 0.4983(9) 0.105(4) Uani 1 1 d . . . H16A H 0.6203 0.8356 0.5468 0.126 Uiso 1 1 calc R . . H16B H 0.6150 0.7307 0.5340 0.126 Uiso 1 1 calc R . . C17 C 0.7481(11) 0.8185(14) 0.4657(11) 0.127(5) Uani 1 1 d . . . H17A H 0.7807 0.7486 0.4919 0.152 Uiso 1 1 calc R . . H17B H 0.7835 0.8588 0.4953 0.152 Uiso 1 1 calc R . . C18 C 0.7751(9) 0.8720(10) 0.3546(9) 0.078(3) Uani 1 1 d . . . H18 H 0.7976 0.8298 0.3225 0.094 Uiso 1 1 calc R . . C19 C 0.7688(10) 0.9811(11) 0.2956(11) 0.097(4) Uani 1 1 d . . . H19 H 0.7914 1.0069 0.2273 0.116 Uiso 1 1 calc R . . C20 C 0.7275(15) 1.0626(14) 0.3343(16) 0.163(8) Uani 1 1 d . . . H20A H 0.7738 1.0584 0.3868 0.196 Uiso 1 1 calc R . . H20B H 0.7379 1.1334 0.2793 0.196 Uiso 1 1 calc R . . C21 C 0.6118(16) 1.0487(13) 0.3740(13) 0.151(7) Uani 1 1 d . . . H21A H 0.5762 1.1169 0.3420 0.181 Uiso 1 1 calc R . . H21B H 0.6102 1.0303 0.4455 0.181 Uiso 1 1 calc R . . Ir31 Ir 0.91060(3) 0.55893(3) 0.73648(3) 0.05774(15) Uani 1 1 d . . . N31 N 1.0920(7) 0.5273(7) 0.5939(6) 0.067(2) Uani 1 1 d . . . C31 C 1.0397(8) 0.4933(7) 0.6895(8) 0.061(3) Uani 1 1 d . . . N32 N 1.0907(6) 0.4013(6) 0.7443(6) 0.060(2) Uani 1 1 d . . . C32 C 1.1706(8) 0.4566(10) 0.5919(10) 0.080(3) Uani 1 1 d . . . H32 H 1.2163 0.4626 0.5359 0.096 Uiso 1 1 calc R . . C33 C 1.1702(9) 0.3781(10) 0.6840(10) 0.078(3) Uani 1 1 d . . . H33 H 1.2148 0.3185 0.7044 0.094 Uiso 1 1 calc R . . C44 C 1.0064(10) 0.6072(9) 0.8260(9) 0.082(3) Uani 1 1 d . . . H44 H 1.0472 0.5460 0.8401 0.098 Uiso 1 1 calc R . . C45 C 1.0108(10) 0.6871(8) 0.7234(9) 0.078(3) Uani 1 1 d . . . H45 H 1.0575 0.6771 0.6752 0.093 Uiso 1 1 calc R . . C46 C 0.9427(12) 0.7870(9) 0.6899(9) 0.098(4) Uani 1 1 d . . . H46A H 0.9454 0.8206 0.6168 0.117 Uiso 1 1 calc R . . H46B H 0.9773 0.8360 0.7104 0.117 Uiso 1 1 calc R . . C47 C 0.8205(12) 0.7695(10) 0.7316(9) 0.099(4) Uani 1 1 d . . . H47A H 0.8134 0.7746 0.7952 0.119 Uiso 1 1 calc R . . H47B H 0.7759 0.8246 0.6847 0.119 Uiso 1 1 calc R . . C48 C 0.7778(9) 0.6621(9) 0.7475(8) 0.075(3) Uani 1 1 d . . . H48 H 0.7515 0.6571 0.6921 0.090 Uiso 1 1 calc R . . C49 C 0.7742(9) 0.5699(10) 0.8375(8) 0.080(3) Uani 1 1 d . . . H49 H 0.7405 0.5095 0.8393 0.096 Uiso 1 1 calc R . . C50 C 0.8219(12) 0.5613(11) 0.9337(9) 0.106(5) Uani 1 1 d . . . H50A H 0.8274 0.4868 0.9803 0.128 Uiso 1 1 calc R . . H50B H 0.7716 0.5942 0.9658 0.128 Uiso 1 1 calc R . . C51 C 0.9406(12) 0.6167(10) 0.9110(9) 0.096(4) Uani 1 1 d . . . H51A H 0.9318 0.6914 0.8948 0.115 Uiso 1 1 calc R . . H51B H 0.9813 0.5847 0.9710 0.115 Uiso 1 1 calc R . . C34 C 1.0613(9) 0.6232(9) 0.5092(8) 0.085(3) Uani 1 1 d DU . . H34A H 0.9947 0.6516 0.5292 0.102 Uiso 1 1 calc R . . H34B H 1.0443 0.6064 0.4545 0.102 Uiso 1 1 calc R . . C35 C 1.1535(12) 0.7054(9) 0.4731(10) 0.119(5) Uani 1 1 d DU . . H35A H 1.2192 0.6789 0.4497 0.143 Uiso 1 1 calc R . . H35B H 1.1729 0.7205 0.5282 0.143 Uiso 1 1 calc R . . C36 C 1.1147(18) 0.8107(12) 0.3841(12) 0.187(9) Uani 1 1 d DU . . H36A H 1.1269 0.8042 0.3213 0.224 Uiso 1 1 calc R . . H36B H 1.0353 0.8184 0.3957 0.224 Uiso 1 1 calc R . . C37 C 1.171(3) 0.9025(16) 0.3741(17) 0.251(15) Uani 1 1 d DU . . H37 H 1.2167 0.9407 0.3155 0.301 Uiso 1 1 calc R . . C38 C 1.164(5) 0.929(3) 0.429(3) 0.61(6) Uani 1 1 d DU . . H38A H 1.1186 0.8918 0.4878 0.733 Uiso 1 1 calc R . . H38B H 1.2025 0.9901 0.4195 0.733 Uiso 1 1 calc R . . C39 C 1.0592(9) 0.3313(8) 0.8495(8) 0.073(3) Uani 1 1 d D . . H39A H 1.0225 0.3723 0.8814 0.087 Uiso 1 1 calc R . . H39B H 1.1260 0.3020 0.8837 0.087 Uiso 1 1 calc R . . C40 C 0.9832(10) 0.2424(9) 0.8615(9) 0.090(4) Uani 1 1 d D . . H40A H 1.0248 0.1904 0.8465 0.108 Uiso 1 1 calc R . . H40B H 0.9253 0.2695 0.8150 0.108 Uiso 1 1 calc R . . C41 C 0.9268(18) 0.1864(19) 0.9780(13) 0.41(3) Uani 1 1 d D . . H41A H 0.9036 0.2395 1.0010 0.491 Uiso 1 1 calc R . . H41B H 0.8628 0.1418 0.9841 0.491 Uiso 1 1 calc R . . C42 C 1.016(2) 0.124(2) 1.0344(18) 0.40(3) Uani 1 1 d D . . H42 H 1.0794 0.1114 1.0012 0.476 Uiso 1 1 calc R . . C43 C 1.008(3) 0.092(5) 1.112(2) 0.87(7) Uani 1 1 d D . . H43A H 0.9438 0.1049 1.1450 1.049 Uiso 1 1 calc R . . H43B H 1.0642 0.0517 1.1499 1.049 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 0.0541(2) 0.0610(3) 0.0553(3) -0.0197(2) -0.00889(19) 0.00751(19) N1 0.060(5) 0.065(6) 0.072(6) -0.021(5) -0.011(5) 0.003(4) C1 0.054(6) 0.069(7) 0.057(7) -0.030(6) -0.002(5) 0.017(5) N2 0.057(5) 0.069(6) 0.059(6) -0.019(5) -0.011(4) 0.015(4) C2 0.050(6) 0.098(9) 0.087(9) -0.031(8) -0.028(6) 0.008(6) C3 0.056(7) 0.099(9) 0.079(8) -0.034(8) -0.027(6) 0.021(6) C4 0.075(7) 0.063(7) 0.072(8) -0.019(6) -0.007(6) -0.006(5) Cl1 0.0676(16) 0.103(2) 0.0621(18) -0.0302(16) -0.0080(13) 0.0263(15) C5 0.076(7) 0.083(8) 0.085(9) -0.029(7) -0.018(6) 0.010(6) Cl31 0.0684(17) 0.102(2) 0.086(2) -0.0411(18) -0.0071(15) -0.0156(16) C6 0.102(10) 0.061(8) 0.145(14) -0.015(8) -0.006(9) 0.012(7) C7 0.21(2) 0.124(15) 0.34(4) -0.117(19) 0.02(2) 0.057(16) C8 0.20(3) 0.34(4) 0.30(4) -0.21(3) -0.04(2) 0.11(2) C9 0.076(7) 0.073(7) 0.062(7) -0.019(6) 0.006(6) 0.014(6) C10 0.159(14) 0.090(10) 0.111(13) -0.022(9) 0.019(11) 0.031(9) C11 0.24(2) 0.101(14) 0.144(19) -0.013(12) 0.025(17) 0.094(14) C12 0.35(4) 0.097(15) 0.26(4) -0.053(18) -0.12(3) 0.02(2) C13 0.79(7) 0.65(6) 0.34(6) -0.17(6) 0.16(6) -0.546 C14 0.098(9) 0.111(10) 0.082(9) -0.065(9) -0.001(7) 0.020(8) C15 0.085(8) 0.090(9) 0.060(7) -0.037(7) -0.001(6) 0.012(6) C16 0.096(10) 0.138(12) 0.062(8) -0.025(8) -0.017(7) 0.009(8) C17 0.090(10) 0.190(16) 0.094(12) -0.054(11) -0.034(8) 0.036(10) C18 0.079(8) 0.099(9) 0.070(8) -0.045(7) -0.032(6) 0.013(7) C19 0.081(8) 0.109(11) 0.103(11) -0.046(9) -0.016(7) -0.011(8) C20 0.136(15) 0.155(15) 0.26(3) -0.153(18) 0.011(15) -0.036(12) C21 0.189(19) 0.138(14) 0.170(18) -0.114(14) 0.036(14) -0.032(13) Ir31 0.0616(3) 0.0630(3) 0.0479(3) -0.0233(2) -0.00749(19) 0.0125(2) N31 0.060(5) 0.080(6) 0.055(6) -0.026(5) 0.000(4) 0.008(4) C31 0.064(6) 0.056(6) 0.071(7) -0.033(6) -0.032(6) 0.013(5) N32 0.057(5) 0.065(5) 0.062(6) -0.032(5) -0.008(4) 0.005(4) C32 0.061(7) 0.104(9) 0.088(9) -0.056(8) -0.003(6) 0.032(6) C33 0.073(7) 0.083(8) 0.090(9) -0.048(8) -0.014(7) 0.027(6) C44 0.101(9) 0.079(8) 0.086(9) -0.051(8) -0.031(7) 0.023(7) C45 0.098(8) 0.064(7) 0.085(9) -0.046(7) -0.006(7) -0.001(6) C46 0.150(13) 0.059(7) 0.066(8) -0.012(6) -0.002(8) 0.011(8) C47 0.147(12) 0.092(9) 0.072(9) -0.045(8) -0.035(8) 0.058(9) C48 0.093(8) 0.092(8) 0.050(7) -0.039(6) -0.016(6) 0.052(6) C49 0.087(8) 0.100(9) 0.043(7) -0.023(6) 0.000(6) 0.023(7) C50 0.147(12) 0.105(10) 0.053(8) -0.023(7) -0.003(8) 0.060(9) C51 0.147(12) 0.088(9) 0.064(8) -0.042(7) -0.030(8) 0.036(8) C34 0.085(8) 0.100(8) 0.067(8) -0.034(7) -0.011(6) 0.019(6) C35 0.164(13) 0.095(8) 0.102(11) -0.044(7) -0.023(10) -0.008(8) C36 0.27(2) 0.140(12) 0.089(13) 0.011(9) -0.025(13) -0.032(14) C37 0.49(5) 0.112(12) 0.13(2) -0.042(14) 0.01(3) -0.031(19) C38 1.43(18) 0.27(4) 0.20(4) -0.15(3) -0.12(6) -0.05(6) C39 0.085(7) 0.071(7) 0.061(7) -0.025(6) -0.022(6) 0.025(6) C40 0.101(9) 0.075(8) 0.080(9) -0.018(7) -0.024(7) 0.008(7) C41 0.50(5) 0.22(2) 0.27(3) 0.17(2) -0.33(4) -0.25(3) C42 0.47(6) 0.33(4) 0.47(6) -0.30(5) 0.37(5) -0.26(4) C43 0.74(8) 0.82(9) 0.88(15) -0.29(8) 0.59(11) -0.556 _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 2.030(10) . ? Ir1 C15 2.109(10) . ? Ir1 C14 2.111(11) . ? Ir1 C18 2.171(10) . ? Ir1 C19 2.189(12) . ? Ir1 Cl1 2.358(3) . ? N1 C2 1.365(12) . ? N1 C1 1.376(12) . ? N1 C4 1.477(12) . ? C1 N2 1.330(12) . ? N2 C3 1.377(13) . ? N2 C9 1.431(12) . ? C2 C3 1.326(14) . ? C4 C5 1.505(12) . ? C5 C6 1.538(12) . ? Cl31 Ir31 2.360(3) . ? C6 C7 1.428(19) . ? C7 C8 1.010(19) . ? C9 C10 1.490(15) . ? C10 C11 1.53(2) . ? C11 C12 1.522(10) . ? C12 C13 0.97(3) . ? C14 C15 1.399(15) . ? C14 C21 1.524(18) . ? C15 C16 1.529(15) . ? C16 C17 1.423(15) . ? C17 C18 1.486(16) . ? C18 C19 1.392(16) . ? C19 C20 1.543(19) . ? C20 C21 1.449(19) . ? Ir31 C31 2.020(10) . ? Ir31 C45 2.102(10) . ? Ir31 C44 2.137(11) . ? Ir31 C49 2.180(10) . ? Ir31 C48 2.181(9) . ? N31 C32 1.366(12) . ? N31 C31 1.378(12) . ? N31 C34 1.448(13) . ? C31 N32 1.353(11) . ? N32 C33 1.387(12) . ? N32 C39 1.452(12) . ? C32 C33 1.324(14) . ? C44 C45 1.435(15) . ? C44 C51 1.485(15) . ? C45 C46 1.514(15) . ? C46 C47 1.528(16) . ? C47 C48 1.505(15) . ? C48 C49 1.388(14) . ? C49 C50 1.529(16) . ? C50 C51 1.574(17) . ? C34 C35 1.498(12) . ? C35 C36 1.581(15) . ? C36 C37 1.40(2) . ? C37 C38 1.02(2) . ? C39 C40 1.491(12) . ? C40 C41 1.641(18) . ? C41 C42 1.44(2) . ? C42 C43 1.04(2) . ? 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 C15 93.4(4) . . ? C1 Ir1 C14 93.6(4) . . ? C15 Ir1 C14 38.7(4) . . ? C1 Ir1 C18 162.1(4) . . ? C15 Ir1 C18 81.4(4) . . ? C14 Ir1 C18 92.9(5) . . ? C1 Ir1 C19 160.6(5) . . ? C15 Ir1 C19 94.6(5) . . ? C14 Ir1 C19 81.8(5) . . ? C18 Ir1 C19 37.2(4) . . ? C1 Ir1 Cl1 87.1(3) . . ? C15 Ir1 Cl1 160.4(3) . . ? C14 Ir1 Cl1 160.8(4) . . ? C18 Ir1 Cl1 92.2(3) . . ? C19 Ir1 Cl1 91.3(4) . . ? C2 N1 C1 109.8(9) . . ? C2 N1 C4 125.7(9) . . ? C1 N1 C4 124.2(8) . . ? N2 C1 N1 104.4(9) . . ? N2 C1 Ir1 127.9(8) . . ? N1 C1 Ir1 127.7(7) . . ? C1 N2 C3 111.4(9) . . ? C1 N2 C9 125.5(10) . . ? C3 N2 C9 123.0(9) . . ? C3 C2 N1 107.7(10) . . ? C2 C3 N2 106.7(10) . . ? N1 C4 C5 111.5(9) . . ? C4 C5 C6 113.5(10) . . ? C7 C6 C5 113.6(14) . . ? C8 C7 C6 142(3) . . ? N2 C9 C10 115.3(9) . . ? C9 C10 C11 112.9(12) . . ? C12 C11 C10 112.7(18) . . ? C13 C12 C11 134(5) . . ? C15 C14 C21 124.3(14) . . ? C15 C14 Ir1 70.6(6) . . ? C21 C14 Ir1 112.4(8) . . ? C14 C15 C16 122.8(12) . . ? C14 C15 Ir1 70.7(6) . . ? C16 C15 Ir1 110.6(8) . . ? C17 C16 C15 118.2(11) . . ? C16 C17 C18 115.7(11) . . ? C19 C18 C17 124.3(13) . . ? C19 C18 Ir1 72.1(7) . . ? C17 C18 Ir1 111.9(8) . . ? C18 C19 C20 125.3(14) . . ? C18 C19 Ir1 70.7(6) . . ? C20 C19 Ir1 110.1(9) . . ? C21 C20 C19 115.0(12) . . ? C20 C21 C14 117.8(12) . . ? C31 Ir31 C45 92.3(4) . . ? C31 Ir31 C44 95.1(4) . . ? C45 Ir31 C44 39.6(4) . . ? C31 Ir31 C49 157.6(4) . . ? C45 Ir31 C49 98.9(5) . . ? C44 Ir31 C49 81.8(5) . . ? C31 Ir31 C48 165.2(4) . . ? C45 Ir31 C48 81.7(4) . . ? C44 Ir31 C48 88.9(4) . . ? C49 Ir31 C48 37.1(4) . . ? C31 Ir31 Cl31 88.0(3) . . ? C45 Ir31 Cl31 155.6(4) . . ? C44 Ir31 Cl31 164.6(3) . . ? C49 Ir31 Cl31 89.6(3) . . ? C48 Ir31 Cl31 91.9(3) . . ? C32 N31 C31 110.6(9) . . ? C32 N31 C34 126.8(9) . . ? C31 N31 C34 122.6(9) . . ? N32 C31 N31 103.8(9) . . ? N32 C31 Ir31 127.5(8) . . ? N31 C31 Ir31 128.6(7) . . ? C31 N32 C33 110.7(9) . . ? C31 N32 C39 124.6(9) . . ? C33 N32 C39 124.4(9) . . ? C33 C32 N31 107.8(10) . . ? C32 C33 N32 107.1(10) . . ? C45 C44 C51 123.8(10) . . ? C45 C44 Ir31 68.9(6) . . ? C51 C44 Ir31 114.3(8) . . ? C44 C45 C46 123.0(11) . . ? C44 C45 Ir31 71.5(6) . . ? C46 C45 Ir31 109.8(8) . . ? C45 C46 C47 115.0(9) . . ? C48 C47 C46 110.9(9) . . ? C49 C48 C47 125.8(11) . . ? C49 C48 Ir31 71.4(6) . . ? C47 C48 Ir31 112.9(8) . . ? C48 C49 C50 124.3(12) . . ? C48 C49 Ir31 71.5(6) . . ? C50 C49 Ir31 108.6(8) . . ? C49 C50 C51 111.7(10) . . ? C44 C51 C50 112.4(10) . . ? N31 C34 C35 111.1(9) . . ? C34 C35 C36 109.6(11) . . ? C37 C36 C35 113.3(17) . . ? C38 C37 C36 122(3) . . ? N32 C39 C40 112.4(9) . . ? C39 C40 C41 109.0(11) . . ? C42 C41 C40 103.3(18) . . ? C43 C42 C41 119(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 1.6(11) . . . . ? C4 N1 C1 N2 175.8(9) . . . . ? C2 N1 C1 Ir1 -176.6(7) . . . . ? C4 N1 C1 Ir1 -2.4(14) . . . . ? C15 Ir1 C1 N2 116.5(9) . . . . ? C14 Ir1 C1 N2 77.7(9) . . . . ? C18 Ir1 C1 N2 -171.2(11) . . . . ? C19 Ir1 C1 N2 2.3(19) . . . . ? Cl1 Ir1 C1 N2 -83.1(9) . . . . ? C15 Ir1 C1 N1 -65.7(9) . . . . ? C14 Ir1 C1 N1 -104.5(9) . . . . ? C18 Ir1 C1 N1 6.6(18) . . . . ? C19 Ir1 C1 N1 -179.9(12) . . . . ? Cl1 Ir1 C1 N1 94.7(8) . . . . ? N1 C1 N2 C3 -1.4(11) . . . . ? Ir1 C1 N2 C3 176.8(7) . . . . ? N1 C1 N2 C9 -176.8(9) . . . . ? Ir1 C1 N2 C9 1.5(15) . . . . ? C1 N1 C2 C3 -1.3(13) . . . . ? C4 N1 C2 C3 -175.4(10) . . . . ? N1 C2 C3 N2 0.4(13) . . . . ? C1 N2 C3 C2 0.6(13) . . . . ? C9 N2 C3 C2 176.1(9) . . . . ? C2 N1 C4 C5 68.3(13) . . . . ? C1 N1 C4 C5 -105.0(11) . . . . ? N1 C4 C5 C6 -173.6(9) . . . . ? C4 C5 C6 C7 175.9(14) . . . . ? C5 C6 C7 C8 107(5) . . . . ? C1 N2 C9 C10 -111.9(13) . . . . ? C3 N2 C9 C10 73.2(15) . . . . ? N2 C9 C10 C11 -174.5(14) . . . . ? C9 C10 C11 C12 -76(3) . . . . ? C10 C11 C12 C13 173(7) . . . . ? C1 Ir1 C14 C15 91.0(8) . . . . ? C18 Ir1 C14 C15 -72.3(8) . . . . ? C19 Ir1 C14 C15 -107.9(8) . . . . ? Cl1 Ir1 C14 C15 -177.7(8) . . . . ? C1 Ir1 C14 C21 -148.9(11) . . . . ? C15 Ir1 C14 C21 120.1(15) . . . . ? C18 Ir1 C14 C21 47.8(12) . . . . ? C19 Ir1 C14 C21 12.2(11) . . . . ? Cl1 Ir1 C14 C21 -57.6(18) . . . . ? C21 C14 C15 C16 -1.7(18) . . . . ? Ir1 C14 C15 C16 102.6(10) . . . . ? C21 C14 C15 Ir1 -104.3(11) . . . . ? C1 Ir1 C15 C14 -91.5(8) . . . . ? C18 Ir1 C15 C14 105.8(8) . . . . ? C19 Ir1 C15 C14 70.8(8) . . . . ? Cl1 Ir1 C15 C14 177.8(8) . . . . ? C1 Ir1 C15 C16 149.7(9) . . . . ? C14 Ir1 C15 C16 -118.8(13) . . . . ? C18 Ir1 C15 C16 -13.0(9) . . . . ? C19 Ir1 C15 C16 -48.0(10) . . . . ? Cl1 Ir1 C15 C16 58.9(15) . . . . ? C14 C15 C16 C17 -65.8(18) . . . . ? Ir1 C15 C16 C17 14.0(17) . . . . ? C15 C16 C17 C18 -5(2) . . . . ? C16 C17 C18 C19 76.1(18) . . . . ? C16 C17 C18 Ir1 -6.6(18) . . . . ? C1 Ir1 C18 C19 176.4(12) . . . . ? C15 Ir1 C18 C19 -109.4(8) . . . . ? C14 Ir1 C18 C19 -72.3(8) . . . . ? Cl1 Ir1 C18 C19 89.2(8) . . . . ? C1 Ir1 C18 C17 -63.0(18) . . . . ? C15 Ir1 C18 C17 11.1(10) . . . . ? C14 Ir1 C18 C17 48.2(11) . . . . ? C19 Ir1 C18 C17 120.5(14) . . . . ? Cl1 Ir1 C18 C17 -150.3(10) . . . . ? C17 C18 C19 C20 -3.3(19) . . . . ? Ir1 C18 C19 C20 101.4(13) . . . . ? C17 C18 C19 Ir1 -104.7(11) . . . . ? C1 Ir1 C19 C18 -176.7(11) . . . . ? C15 Ir1 C19 C18 69.3(8) . . . . ? C14 Ir1 C19 C18 106.0(8) . . . . ? Cl1 Ir1 C19 C18 -92.0(7) . . . . ? C1 Ir1 C19 C20 62(2) . . . . ? C15 Ir1 C19 C20 -52.3(12) . . . . ? C14 Ir1 C19 C20 -15.6(12) . . . . ? C18 Ir1 C19 C20 -121.6(15) . . . . ? Cl1 Ir1 C19 C20 146.4(11) . . . . ? C18 C19 C20 C21 -63(2) . . . . ? Ir1 C19 C20 C21 17(2) . . . . ? C19 C20 C21 C14 -7(3) . . . . ? C15 C14 C21 C20 75(2) . . . . ? Ir1 C14 C21 C20 -6(2) . . . . ? C32 N31 C31 N32 0.9(10) . . . . ? C34 N31 C31 N32 178.6(9) . . . . ? C32 N31 C31 Ir31 -175.6(7) . . . . ? C34 N31 C31 Ir31 2.1(14) . . . . ? C45 Ir31 C31 N32 112.2(8) . . . . ? C44 Ir31 C31 N32 72.6(9) . . . . ? C49 Ir31 C31 N32 -8.2(16) . . . . ? C48 Ir31 C31 N32 177.9(13) . . . . ? Cl31 Ir31 C31 N32 -92.2(8) . . . . ? C45 Ir31 C31 N31 -72.1(9) . . . . ? C44 Ir31 C31 N31 -111.7(9) . . . . ? C49 Ir31 C31 N31 167.6(10) . . . . ? C48 Ir31 C31 N31 -6(2) . . . . ? Cl31 Ir31 C31 N31 83.5(8) . . . . ? N31 C31 N32 C33 -1.3(10) . . . . ? Ir31 C31 N32 C33 175.2(7) . . . . ? N31 C31 N32 C39 -175.8(8) . . . . ? Ir31 C31 N32 C39 0.8(13) . . . . ? C31 N31 C32 C33 -0.1(12) . . . . ? C34 N31 C32 C33 -177.7(10) . . . . ? N31 C32 C33 N32 -0.7(13) . . . . ? C31 N32 C33 C32 1.3(12) . . . . ? C39 N32 C33 C32 175.8(9) . . . . ? C31 Ir31 C44 C45 87.4(7) . . . . ? C49 Ir31 C44 C45 -114.9(7) . . . . ? C48 Ir31 C44 C45 -78.3(7) . . . . ? Cl31 Ir31 C44 C45 -171.6(9) . . . . ? C31 Ir31 C44 C51 -153.9(9) . . . . ? C45 Ir31 C44 C51 118.7(12) . . . . ? C49 Ir31 C44 C51 3.8(9) . . . . ? C48 Ir31 C44 C51 40.4(9) . . . . ? Cl31 Ir31 C44 C51 -52.9(17) . . . . ? C51 C44 C45 C46 -3.8(18) . . . . ? Ir31 C44 C45 C46 102.0(11) . . . . ? C51 C44 C45 Ir31 -105.8(11) . . . . ? C31 Ir31 C45 C44 -95.2(7) . . . . ? C49 Ir31 C45 C44 65.4(7) . . . . ? C48 Ir31 C45 C44 98.4(7) . . . . ? Cl31 Ir31 C45 C44 174.6(6) . . . . ? C31 Ir31 C45 C46 145.4(8) . . . . ? C44 Ir31 C45 C46 -119.4(11) . . . . ? C49 Ir31 C45 C46 -54.0(9) . . . . ? C48 Ir31 C45 C46 -21.0(8) . . . . ? Cl31 Ir31 C45 C46 55.2(13) . . . . ? C44 C45 C46 C47 -45.3(16) . . . . ? Ir31 C45 C46 C47 35.0(13) . . . . ? C45 C46 C47 C48 -31.0(15) . . . . ? C46 C47 C48 C49 95.0(13) . . . . ? C46 C47 C48 Ir31 12.0(12) . . . . ? C31 Ir31 C48 C49 176.2(14) . . . . ? C45 Ir31 C48 C49 -116.8(8) . . . . ? C44 Ir31 C48 C49 -77.8(8) . . . . ? Cl31 Ir31 C48 C49 86.8(7) . . . . ? C31 Ir31 C48 C47 -61.9(19) . . . . ? C45 Ir31 C48 C47 5.1(8) . . . . ? C44 Ir31 C48 C47 44.1(8) . . . . ? C49 Ir31 C48 C47 121.9(11) . . . . ? Cl31 Ir31 C48 C47 -151.3(7) . . . . ? C47 C48 C49 C50 -4.9(17) . . . . ? Ir31 C48 C49 C50 100.4(11) . . . . ? C47 C48 C49 Ir31 -105.3(11) . . . . ? C31 Ir31 C49 C48 -177.4(9) . . . . ? C45 Ir31 C49 C48 63.4(8) . . . . ? C44 Ir31 C49 C48 99.2(8) . . . . ? Cl31 Ir31 C49 C48 -93.7(7) . . . . ? C31 Ir31 C49 C50 61.7(16) . . . . ? C45 Ir31 C49 C50 -57.6(9) . . . . ? C44 Ir31 C49 C50 -21.7(9) . . . . ? C48 Ir31 C49 C50 -120.9(12) . . . . ? Cl31 Ir31 C49 C50 145.4(8) . . . . ? C48 C49 C50 C51 -44.2(15) . . . . ? Ir31 C49 C50 C51 35.6(12) . . . . ? C45 C44 C51 C50 94.9(13) . . . . ? Ir31 C44 C51 C50 14.8(13) . . . . ? C49 C50 C51 C44 -33.9(14) . . . . ? C32 N31 C34 C35 -69.1(15) . . . . ? C31 N31 C34 C35 113.6(11) . . . . ? N31 C34 C35 C36 -177.4(12) . . . . ? C34 C35 C36 C37 154.5(18) . . . . ? C35 C36 C37 C38 -65(7) . . . . ? C31 N32 C39 C40 96.1(11) . . . . ? C33 N32 C39 C40 -77.6(12) . . . . ? N32 C39 C40 C41 -165.6(12) . . . . ? C39 C40 C41 C42 -76(2) . . . . ? C40 C41 C42 C43 167(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.104 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.126 data_str861m _database_code_depnum_ccdc_archive 'CCDC 656990' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H24 Ir N2, B F4' _chemical_formula_sum 'C17 H24 B F4 Ir N2' _chemical_formula_weight 535.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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_Int_Tables_number 14 _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 8.1277(4) _cell_length_b 36.568(2) _cell_length_c 12.0502(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.5350(10) _cell_angle_gamma 90.00 _cell_volume 3532.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8122 _cell_measurement_theta_min 1.11 _cell_measurement_theta_max 27.50 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.191 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 7.602 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _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 24448 _diffrn_reflns_av_R_equivalents 0.0742 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8122 _reflns_number_gt 5136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms could not be found in the difference maps and had been added in 'idealized' positions. No reliance should be placed on the reported ethylenic H-atom coordinates ; _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^)+(0.0215P)^2^+13.2770P] 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 8122 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.79187(4) 0.186750(9) 0.84328(3) 0.02683(9) Uani 1 1 d . . . C1 C 0.6167(11) 0.2164(3) 0.7597(7) 0.037(2) Uani 1 1 d . . . F1 F 0.0629(9) 0.19871(18) 0.4414(6) 0.079(2) Uani 1 1 d . . . B1 B 0.1435(15) 0.1777(3) 0.3719(10) 0.039(3) Uani 1 1 d . . . N1 N 0.5031(9) 0.20367(19) 0.6728(6) 0.0332(17) Uani 1 1 d . . . F2 F 0.1321(9) 0.14166(17) 0.3938(6) 0.081(2) Uani 1 1 d . . . N2 N 0.5695(9) 0.24972(19) 0.7815(6) 0.0338(18) Uani 1 1 d . . . C2 C 0.3839(11) 0.2301(3) 0.6380(8) 0.040(2) Uani 1 1 d . . . H2 H 0.2933 0.2284 0.5799 0.048 Uiso 1 1 calc R . . F3 F 0.0773(10) 0.1852(2) 0.2618(6) 0.096(2) Uani 1 1 d . . . C3 C 0.4277(12) 0.2596(2) 0.7074(8) 0.040(2) Uani 1 1 d . . . H3 H 0.3725 0.2819 0.7051 0.048 Uiso 1 1 calc R . . F4 F 0.3087(8) 0.18844(18) 0.3905(6) 0.076(2) Uani 1 1 d . . . C4 C 0.5250(12) 0.1657(2) 0.6382(8) 0.042(2) Uani 1 1 d . . . H4A H 0.5757 0.1651 0.5708 0.050 Uiso 1 1 calc R . . H4B H 0.4178 0.1534 0.6222 0.050 Uiso 1 1 calc R . . C5 C 0.6380(11) 0.1464(2) 0.7350(8) 0.036(2) Uani 1 1 d . . . H5 H 0.7370 0.1357 0.7221 0.044 Uiso 1 1 calc R . . C6 C 0.5946(12) 0.1446(3) 0.8429(9) 0.050(3) Uani 1 1 d . . . H6A H 0.4958 0.1552 0.8565 0.060 Uiso 1 1 calc R . . H6B H 0.6646 0.1328 0.9008 0.060 Uiso 1 1 calc R . . C7 C 0.6770(12) 0.2675(3) 0.8776(9) 0.048(3) Uani 1 1 d . . . H7A H 0.6088 0.2813 0.9216 0.058 Uiso 1 1 calc R . . H7B H 0.7536 0.2842 0.8502 0.058 Uiso 1 1 calc R . . C8 C 0.7738(12) 0.2385(3) 0.9503(8) 0.043(3) Uani 1 1 d . . . H8 H 0.8896 0.2400 0.9655 0.052 Uiso 1 1 calc R . . C9 C 0.6966(13) 0.2099(3) 0.9947(8) 0.055(3) Uani 1 1 d . . . H9A H 0.5810 0.2079 0.9804 0.066 Uiso 1 1 calc R . . H9B H 0.7600 0.1925 1.0392 0.066 Uiso 1 1 calc R . . C10 C 0.9804(11) 0.1403(2) 0.8853(8) 0.036(2) Uani 1 1 d . . . H10 H 0.8888 0.1250 0.8848 0.043 Uiso 1 1 calc R . . C11 C 1.0109(11) 0.1659(2) 0.9690(8) 0.039(2) Uani 1 1 d . . . H11 H 0.9382 0.1664 1.0210 0.047 Uiso 1 1 calc R . . C12 C 1.1492(11) 0.1927(3) 0.9844(8) 0.045(3) Uani 1 1 d . . . H12A H 1.2527 0.1802 1.0127 0.054 Uiso 1 1 calc R . . H12B H 1.1298 0.2106 1.0404 0.054 Uiso 1 1 calc R . . C13 C 1.1682(11) 0.2132(3) 0.8730(8) 0.042(2) Uani 1 1 d . . . H13A H 1.2155 0.2372 0.8923 0.050 Uiso 1 1 calc R . . H13B H 1.2466 0.1999 0.8358 0.050 Uiso 1 1 calc R . . C14 C 1.0080(10) 0.2179(2) 0.7915(7) 0.032(2) Uani 1 1 d . . . H14 H 0.9456 0.2389 0.7973 0.038 Uiso 1 1 calc R . . C15 C 0.9473(11) 0.1929(2) 0.7083(7) 0.035(2) Uani 1 1 d . . . H15 H 0.8468 0.1985 0.6625 0.042 Uiso 1 1 calc R . . C16 C 1.0292(13) 0.1576(3) 0.6856(8) 0.048(3) Uani 1 1 d . . . H16A H 1.1256 0.1629 0.6504 0.058 Uiso 1 1 calc R . . H16B H 0.9518 0.1433 0.6331 0.058 Uiso 1 1 calc R . . C17 C 1.0853(12) 0.1349(3) 0.7934(9) 0.049(3) Uani 1 1 d . . . H17A H 1.0829 0.1093 0.7731 0.059 Uiso 1 1 calc R . . H17B H 1.2000 0.1412 0.8234 0.059 Uiso 1 1 calc R . . Ir31 Ir 0.60380(4) 0.083178(9) 0.24527(3) 0.02916(10) Uani 1 1 d . . . N31 N 0.3907(9) 0.0648(2) 0.0337(6) 0.041(2) Uani 1 1 d . . . C31 C 0.5423(11) 0.0620(2) 0.0969(8) 0.036(2) Uani 1 1 d . . . F31 F -0.0040(8) -0.0475(2) 0.1225(5) 0.084(2) Uani 1 1 d . . . B31 B 0.0788(15) -0.0343(4) 0.2234(10) 0.046(3) Uani 1 1 d . . . N32 N 0.6426(9) 0.0474(2) 0.0319(6) 0.0361(18) Uani 1 1 d . . . C32 C 0.3976(12) 0.0515(3) -0.0737(8) 0.045(3) Uani 1 1 d . . . H32 H 0.3096 0.0503 -0.1337 0.054 Uiso 1 1 calc R . . F32 F -0.0403(10) -0.0326(3) 0.2914(6) 0.115(3) Uani 1 1 d . . . C33 C 0.5557(13) 0.0407(3) -0.0744(8) 0.045(2) Uani 1 1 d . . . H33 H 0.5980 0.0307 -0.1347 0.054 Uiso 1 1 calc R . . F33 F 0.2008(8) -0.0583(2) 0.2658(6) 0.085(2) Uani 1 1 d . . . C34 C 0.2632(12) 0.0813(3) 0.0877(9) 0.051(3) Uani 1 1 d . . . H34A H 0.1947 0.0625 0.1142 0.061 Uiso 1 1 calc R . . H34B H 0.1920 0.0969 0.0350 0.061 Uiso 1 1 calc R . . F34 F 0.1418(10) -0.00190(19) 0.2026(9) 0.132(4) Uani 1 1 d . . . C35 C 0.3523(12) 0.1041(3) 0.1878(9) 0.050(3) Uani 1 1 d . . . H35 H 0.3294 0.1002 0.2600 0.060 Uiso 1 1 calc R . . C36 C 0.4671(14) 0.1305(3) 0.1685(9) 0.059(3) Uani 1 1 d . . . H36A H 0.4894 0.1343 0.0962 0.071 Uiso 1 1 calc R . . H36B H 0.5216 0.1445 0.2280 0.071 Uiso 1 1 calc R . . C37 C 0.8156(12) 0.0415(3) 0.0842(8) 0.054(3) Uani 1 1 d . . . H37A H 0.8902 0.0463 0.0308 0.065 Uiso 1 1 calc R . . H37B H 0.8320 0.0165 0.1105 0.065 Uiso 1 1 calc R . . C38 C 0.8487(11) 0.0681(4) 0.1826(9) 0.054(3) Uani 1 1 d . . . H38 H 0.8867 0.0588 0.2541 0.065 Uiso 1 1 calc R . . C39 C 0.8253(13) 0.1046(3) 0.1708(9) 0.059(3) Uani 1 1 d . . . H39A H 0.7874 0.1145 0.1001 0.071 Uiso 1 1 calc R . . H39B H 0.8472 0.1198 0.2334 0.071 Uiso 1 1 calc R . . C40 C 0.7459(13) 0.1054(2) 0.4109(8) 0.046(3) Uani 1 1 d . . . H40 H 0.7910 0.1236 0.3711 0.055 Uiso 1 1 calc R . . C41 C 0.5776(13) 0.1071(2) 0.4175(7) 0.041(2) Uani 1 1 d . . . H41 H 0.5161 0.1255 0.3768 0.049 Uiso 1 1 calc R . . C42 C 0.4846(14) 0.0819(3) 0.4842(9) 0.057(3) Uani 1 1 d . . . H42A H 0.3982 0.0958 0.5119 0.069 Uiso 1 1 calc R . . H42B H 0.5614 0.0732 0.5491 0.069 Uiso 1 1 calc R . . C43 C 0.4045(13) 0.0490(3) 0.4195(8) 0.048(3) Uani 1 1 d . . . H43A H 0.3967 0.0292 0.4718 0.058 Uiso 1 1 calc R . . H43B H 0.2920 0.0554 0.3844 0.058 Uiso 1 1 calc R . . C44 C 0.5003(13) 0.0361(2) 0.3304(8) 0.041(2) Uani 1 1 d . . . H44 H 0.4387 0.0313 0.2598 0.049 Uiso 1 1 calc R . . C45 C 0.6717(12) 0.0306(2) 0.3430(8) 0.039(2) Uani 1 1 d . . . H45 H 0.7157 0.0224 0.2810 0.047 Uiso 1 1 calc R . . C46 C 0.7904(12) 0.0373(3) 0.4514(7) 0.045(3) Uani 1 1 d . . . H46A H 0.7328 0.0320 0.5139 0.054 Uiso 1 1 calc R . . H46B H 0.8828 0.0203 0.4555 0.054 Uiso 1 1 calc R . . C47 C 0.8597(13) 0.0756(3) 0.4653(8) 0.058(3) Uani 1 1 d . . . H47A H 0.9624 0.0764 0.4343 0.069 Uiso 1 1 calc R . . H47B H 0.8877 0.0808 0.5451 0.069 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 0.02439(17) 0.02369(18) 0.0313(2) -0.00095(14) 0.00133(14) -0.00012(15) C1 0.037(5) 0.035(6) 0.038(6) -0.006(4) 0.004(4) 0.000(4) F1 0.087(5) 0.069(5) 0.088(5) -0.005(4) 0.037(4) 0.029(4) B1 0.049(7) 0.030(6) 0.040(7) 0.004(5) 0.008(6) -0.001(5) N1 0.032(4) 0.021(4) 0.044(5) -0.008(3) 0.000(4) -0.001(3) F2 0.102(6) 0.037(4) 0.112(6) 0.009(4) 0.037(5) -0.007(4) N2 0.029(4) 0.031(4) 0.038(5) -0.011(3) -0.003(3) 0.011(3) C2 0.028(5) 0.045(6) 0.045(6) 0.006(5) 0.000(4) 0.007(4) F3 0.130(7) 0.087(6) 0.059(5) -0.005(4) -0.022(4) -0.010(5) C3 0.050(6) 0.024(5) 0.046(6) 0.015(4) 0.011(5) 0.008(4) F4 0.053(4) 0.069(5) 0.103(5) 0.003(4) 0.004(4) -0.015(4) C4 0.049(6) 0.026(5) 0.046(6) -0.011(4) -0.004(5) 0.001(4) C5 0.028(5) 0.030(5) 0.049(6) -0.001(4) -0.001(4) -0.002(4) C6 0.026(5) 0.057(7) 0.064(7) 0.010(5) -0.004(5) -0.008(5) C7 0.050(6) 0.027(6) 0.065(7) -0.015(5) 0.005(5) 0.002(5) C8 0.038(6) 0.056(7) 0.035(6) -0.028(5) 0.007(5) 0.010(5) C9 0.048(7) 0.069(8) 0.050(7) 0.003(6) 0.016(5) 0.010(6) C10 0.028(5) 0.026(5) 0.052(6) 0.009(4) 0.001(4) 0.006(4) C11 0.031(5) 0.034(6) 0.053(7) 0.014(5) 0.007(5) 0.004(4) C12 0.029(5) 0.053(7) 0.048(6) -0.006(5) -0.014(4) -0.009(5) C13 0.033(5) 0.032(6) 0.061(7) -0.002(5) 0.009(5) -0.009(4) C14 0.029(5) 0.028(5) 0.040(5) -0.002(4) 0.013(4) 0.004(4) C15 0.032(5) 0.047(6) 0.030(5) -0.007(4) 0.016(4) 0.002(4) C16 0.052(7) 0.033(6) 0.063(7) -0.012(5) 0.024(6) 0.002(5) C17 0.037(6) 0.026(6) 0.085(8) -0.006(5) 0.012(6) 0.002(4) Ir31 0.0328(2) 0.02353(18) 0.0301(2) -0.00141(15) 0.00220(15) -0.00008(16) N31 0.036(5) 0.047(5) 0.037(5) -0.013(4) -0.002(4) -0.004(4) C31 0.027(5) 0.036(6) 0.045(6) 0.003(4) 0.009(4) -0.002(4) F31 0.080(5) 0.109(6) 0.058(5) -0.005(4) -0.006(4) -0.011(4) B31 0.038(7) 0.063(9) 0.034(7) -0.003(6) -0.002(5) 0.025(6) N32 0.032(4) 0.045(5) 0.030(4) -0.008(3) -0.002(3) 0.000(4) C32 0.045(6) 0.057(7) 0.030(6) -0.008(5) -0.008(5) -0.004(5) F32 0.098(6) 0.188(10) 0.062(5) 0.011(5) 0.021(4) 0.078(6) C33 0.057(7) 0.043(6) 0.037(6) 0.000(4) 0.014(5) -0.006(5) F33 0.070(5) 0.110(6) 0.075(5) 0.024(4) 0.011(4) 0.049(4) C34 0.039(6) 0.048(7) 0.063(7) -0.003(5) 0.000(5) 0.016(5) F34 0.078(5) 0.034(4) 0.264(12) 0.014(6) -0.033(6) -0.011(4) C35 0.045(6) 0.055(7) 0.047(7) 0.009(5) 0.000(5) 0.015(5) C36 0.076(8) 0.040(7) 0.051(7) -0.002(5) -0.015(6) 0.022(6) C37 0.038(6) 0.080(8) 0.046(7) -0.022(6) 0.009(5) -0.002(6) C38 0.021(5) 0.093(10) 0.047(7) 0.000(6) 0.004(5) -0.017(6) C39 0.051(7) 0.083(10) 0.044(7) -0.003(6) 0.009(5) -0.039(7) C40 0.069(8) 0.027(5) 0.034(6) -0.001(4) -0.009(5) -0.015(5) C41 0.064(7) 0.032(6) 0.027(5) -0.007(4) 0.007(5) 0.001(5) C42 0.071(8) 0.050(7) 0.059(7) -0.018(6) 0.035(6) -0.003(6) C43 0.060(7) 0.046(7) 0.045(6) 0.004(5) 0.025(5) -0.003(5) C44 0.056(6) 0.028(5) 0.039(6) 0.014(4) 0.006(5) -0.003(5) C45 0.052(6) 0.025(5) 0.038(6) 0.009(4) 0.003(5) 0.001(4) C46 0.054(6) 0.046(6) 0.032(6) 0.019(4) -0.002(5) -0.002(5) C47 0.051(7) 0.085(9) 0.033(6) 0.004(5) -0.006(5) -0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.934(9) . ? Ir1 C5 2.214(8) . ? Ir1 C6 2.225(9) . ? Ir1 C15 2.230(8) . ? Ir1 C9 2.261(9) . ? Ir1 C14 2.266(8) . ? Ir1 C11 2.270(9) . ? Ir1 C10 2.289(8) . ? Ir1 C8 2.308(8) . ? C1 N2 1.318(10) . ? C1 N1 1.358(11) . ? F1 B1 1.380(12) . ? B1 F2 1.350(12) . ? B1 F3 1.374(12) . ? B1 F4 1.381(13) . ? N1 C2 1.385(11) . ? N1 C4 1.470(10) . ? N2 C3 1.383(11) . ? N2 C7 1.481(11) . ? C2 C3 1.374(13) . ? C4 C5 1.531(12) . ? C5 C6 1.404(12) . ? C7 C8 1.511(13) . ? C8 C9 1.373(13) . ? C10 C11 1.368(12) . ? C10 C17 1.519(13) . ? C11 C12 1.481(12) . ? C12 C13 1.567(13) . ? C13 C14 1.505(12) . ? C14 C15 1.386(11) . ? C15 C16 1.496(12) . ? C16 C17 1.545(13) . ? Ir31 C31 1.936(9) . ? Ir31 C36 2.179(9) . ? Ir31 C35 2.185(9) . ? Ir31 C44 2.239(8) . ? Ir31 C45 2.274(8) . ? Ir31 C39 2.279(9) . ? Ir31 C40 2.284(9) . ? Ir31 C41 2.294(8) . ? Ir31 C38 2.309(10) . ? N31 C31 1.341(11) . ? N31 C32 1.392(11) . ? N31 C34 1.444(11) . ? C31 N32 1.333(11) . ? F31 B31 1.376(12) . ? B31 F34 1.330(14) . ? B31 F33 1.360(12) . ? B31 F32 1.370(13) . ? N32 C33 1.378(11) . ? N32 C37 1.458(11) . ? C32 C33 1.345(13) . ? C34 C35 1.544(14) . ? C35 C36 1.389(14) . ? C37 C38 1.523(14) . ? C38 C39 1.352(15) . ? C40 C41 1.384(13) . ? C40 C47 1.508(14) . ? C41 C42 1.506(13) . ? C42 C43 1.520(13) . ? C43 C44 1.503(12) . ? C44 C45 1.391(13) . ? C45 C46 1.510(12) . ? C46 C47 1.507(14) . ? 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 C5 76.8(3) . . ? C1 Ir1 C6 85.4(4) . . ? C5 Ir1 C6 36.9(3) . . ? C1 Ir1 C15 91.2(4) . . ? C5 Ir1 C15 88.3(3) . . ? C6 Ir1 C15 124.3(4) . . ? C1 Ir1 C9 83.7(4) . . ? C5 Ir1 C9 119.3(4) . . ? C6 Ir1 C9 85.3(4) . . ? C15 Ir1 C9 149.5(4) . . ? C1 Ir1 C14 96.4(3) . . ? C5 Ir1 C14 124.1(3) . . ? C6 Ir1 C14 160.0(3) . . ? C15 Ir1 C14 35.9(3) . . ? C9 Ir1 C14 114.7(4) . . ? C1 Ir1 C11 164.6(4) . . ? C5 Ir1 C11 118.2(3) . . ? C6 Ir1 C11 104.7(3) . . ? C15 Ir1 C11 92.5(3) . . ? C9 Ir1 C11 85.6(4) . . ? C14 Ir1 C11 78.2(3) . . ? C1 Ir1 C10 160.0(3) . . ? C5 Ir1 C10 85.9(3) . . ? C6 Ir1 C10 86.6(4) . . ? C15 Ir1 C10 78.3(3) . . ? C9 Ir1 C10 113.9(4) . . ? C14 Ir1 C10 85.0(3) . . ? C11 Ir1 C10 34.9(3) . . ? C1 Ir1 C8 73.9(4) . . ? C5 Ir1 C8 142.5(3) . . ? C6 Ir1 C8 117.2(4) . . ? C15 Ir1 C8 114.9(4) . . ? C9 Ir1 C8 35.0(3) . . ? C14 Ir1 C8 82.3(3) . . ? C11 Ir1 C8 91.1(4) . . ? C10 Ir1 C8 126.0(3) . . ? N2 C1 N1 106.7(8) . . ? N2 C1 Ir1 128.9(7) . . ? N1 C1 Ir1 123.9(7) . . ? F2 B1 F3 110.8(9) . . ? F2 B1 F1 111.7(9) . . ? F3 B1 F1 109.0(9) . . ? F2 B1 F4 110.0(9) . . ? F3 B1 F4 108.4(9) . . ? F1 B1 F4 106.8(9) . . ? C1 N1 C2 110.3(7) . . ? C1 N1 C4 116.3(7) . . ? C2 N1 C4 133.3(8) . . ? C1 N2 C3 110.6(7) . . ? C1 N2 C7 114.1(7) . . ? C3 N2 C7 135.3(8) . . ? C3 C2 N1 105.4(8) . . ? C2 C3 N2 107.0(8) . . ? N1 C4 C5 107.7(7) . . ? C6 C5 C4 121.1(8) . . ? C6 C5 Ir1 72.0(5) . . ? C4 C5 Ir1 110.6(6) . . ? C5 C6 Ir1 71.2(5) . . ? N2 C7 C8 109.2(7) . . ? C9 C8 C7 122.2(9) . . ? C9 C8 Ir1 70.7(6) . . ? C7 C8 Ir1 109.1(6) . . ? C8 C9 Ir1 74.4(5) . . ? C11 C10 C17 124.8(9) . . ? C11 C10 Ir1 71.8(5) . . ? C17 C10 Ir1 111.7(6) . . ? C10 C11 C12 126.0(9) . . ? C10 C11 Ir1 73.3(5) . . ? C12 C11 Ir1 110.8(6) . . ? C11 C12 C13 113.0(7) . . ? C14 C13 C12 114.6(7) . . ? C15 C14 C13 124.2(8) . . ? C15 C14 Ir1 70.6(5) . . ? C13 C14 Ir1 112.9(6) . . ? C14 C15 C16 125.8(9) . . ? C14 C15 Ir1 73.5(5) . . ? C16 C15 Ir1 111.7(6) . . ? C15 C16 C17 112.8(8) . . ? C10 C17 C16 114.9(8) . . ? C31 Ir31 C36 83.7(4) . . ? C31 Ir31 C35 76.3(4) . . ? C36 Ir31 C35 37.1(4) . . ? C31 Ir31 C44 93.2(4) . . ? C36 Ir31 C44 127.0(4) . . ? C35 Ir31 C44 90.7(4) . . ? C31 Ir31 C45 98.2(4) . . ? C36 Ir31 C45 162.6(4) . . ? C35 Ir31 C45 126.5(4) . . ? C44 Ir31 C45 35.9(3) . . ? C31 Ir31 C39 82.8(4) . . ? C36 Ir31 C39 86.6(5) . . ? C35 Ir31 C39 120.9(4) . . ? C44 Ir31 C39 145.7(4) . . ? C45 Ir31 C39 110.8(4) . . ? C31 Ir31 C40 164.8(4) . . ? C36 Ir31 C40 103.7(4) . . ? C35 Ir31 C40 117.6(4) . . ? C44 Ir31 C40 92.7(4) . . ? C45 Ir31 C40 78.7(3) . . ? C39 Ir31 C40 84.5(4) . . ? C31 Ir31 C41 159.9(4) . . ? C36 Ir31 C41 87.9(4) . . ? C35 Ir31 C41 86.1(4) . . ? C44 Ir31 C41 77.3(3) . . ? C45 Ir31 C41 84.5(3) . . ? C39 Ir31 C41 115.0(4) . . ? C40 Ir31 C41 35.2(3) . . ? C31 Ir31 C38 73.0(4) . . ? C36 Ir31 C38 117.2(5) . . ? C35 Ir31 C38 142.3(4) . . ? C44 Ir31 C38 112.1(4) . . ? C45 Ir31 C38 79.6(4) . . ? C39 Ir31 C38 34.3(4) . . ? C40 Ir31 C38 91.9(4) . . ? C41 Ir31 C38 126.9(4) . . ? C31 N31 C32 109.1(8) . . ? C31 N31 C34 115.8(8) . . ? C32 N31 C34 135.0(8) . . ? N32 C31 N31 106.9(8) . . ? N32 C31 Ir31 127.9(7) . . ? N31 C31 Ir31 124.5(7) . . ? F34 B31 F33 111.5(10) . . ? F34 B31 F32 113.8(11) . . ? F33 B31 F32 110.4(10) . . ? F34 B31 F31 107.1(10) . . ? F33 B31 F31 108.9(10) . . ? F32 B31 F31 104.7(10) . . ? C31 N32 C33 110.4(8) . . ? C31 N32 C37 116.4(7) . . ? C33 N32 C37 133.2(8) . . ? C33 C32 N31 107.1(8) . . ? C32 C33 N32 106.6(8) . . ? N31 C34 C35 107.4(8) . . ? C36 C35 C34 119.1(10) . . ? C36 C35 Ir31 71.2(6) . . ? C34 C35 Ir31 110.6(6) . . ? C35 C36 Ir31 71.7(6) . . ? N32 C37 C38 106.0(8) . . ? C39 C38 C37 123.0(10) . . ? C39 C38 Ir31 71.6(6) . . ? C37 C38 Ir31 110.9(6) . . ? C38 C39 Ir31 74.1(6) . . ? C41 C40 C47 123.2(9) . . ? C41 C40 Ir31 72.8(5) . . ? C47 C40 Ir31 107.9(6) . . ? C40 C41 C42 126.3(9) . . ? C40 C41 Ir31 72.0(5) . . ? C42 C41 Ir31 112.4(6) . . ? C41 C42 C43 114.8(8) . . ? C44 C43 C42 112.7(8) . . ? C45 C44 C43 126.6(9) . . ? C45 C44 Ir31 73.4(5) . . ? C43 C44 Ir31 111.3(6) . . ? C44 C45 C46 123.8(9) . . ? C44 C45 Ir31 70.7(5) . . ? C46 C45 Ir31 112.1(6) . . ? C47 C46 C45 114.8(7) . . ? C46 C47 C40 115.6(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Ir1 C1 N2 162.7(9) . . . . ? C6 Ir1 C1 N2 126.3(9) . . . . ? C15 Ir1 C1 N2 -109.3(9) . . . . ? C9 Ir1 C1 N2 40.6(9) . . . . ? C14 Ir1 C1 N2 -73.7(9) . . . . ? C11 Ir1 C1 N2 -5(2) . . . . ? C10 Ir1 C1 N2 -166.9(8) . . . . ? C8 Ir1 C1 N2 6.3(8) . . . . ? C5 Ir1 C1 N1 -8.0(7) . . . . ? C6 Ir1 C1 N1 -44.4(8) . . . . ? C15 Ir1 C1 N1 80.0(8) . . . . ? C9 Ir1 C1 N1 -130.1(8) . . . . ? C14 Ir1 C1 N1 115.6(8) . . . . ? C11 Ir1 C1 N1 -176.0(10) . . . . ? C10 Ir1 C1 N1 22.4(16) . . . . ? C8 Ir1 C1 N1 -164.4(9) . . . . ? N2 C1 N1 C2 1.3(11) . . . . ? Ir1 C1 N1 C2 173.8(6) . . . . ? N2 C1 N1 C4 -176.4(7) . . . . ? Ir1 C1 N1 C4 -3.9(12) . . . . ? N1 C1 N2 C3 -1.7(10) . . . . ? Ir1 C1 N2 C3 -173.6(7) . . . . ? N1 C1 N2 C7 178.0(8) . . . . ? Ir1 C1 N2 C7 6.0(12) . . . . ? C1 N1 C2 C3 -0.5(10) . . . . ? C4 N1 C2 C3 176.7(9) . . . . ? N1 C2 C3 N2 -0.5(10) . . . . ? C1 N2 C3 C2 1.4(10) . . . . ? C7 N2 C3 C2 -178.1(10) . . . . ? C1 N1 C4 C5 18.5(11) . . . . ? C2 N1 C4 C5 -158.6(9) . . . . ? N1 C4 C5 C6 57.7(11) . . . . ? N1 C4 C5 Ir1 -23.1(9) . . . . ? C1 Ir1 C5 C6 -100.1(6) . . . . ? C15 Ir1 C5 C6 168.3(6) . . . . ? C9 Ir1 C5 C6 -25.2(7) . . . . ? C14 Ir1 C5 C6 171.1(5) . . . . ? C11 Ir1 C5 C6 76.3(6) . . . . ? C10 Ir1 C5 C6 89.9(6) . . . . ? C8 Ir1 C5 C6 -60.9(8) . . . . ? C1 Ir1 C5 C4 17.2(6) . . . . ? C6 Ir1 C5 C4 117.3(9) . . . . ? C15 Ir1 C5 C4 -74.5(7) . . . . ? C9 Ir1 C5 C4 92.0(7) . . . . ? C14 Ir1 C5 C4 -71.7(7) . . . . ? C11 Ir1 C5 C4 -166.4(6) . . . . ? C10 Ir1 C5 C4 -152.8(7) . . . . ? C8 Ir1 C5 C4 56.4(9) . . . . ? C4 C5 C6 Ir1 -103.6(8) . . . . ? C1 Ir1 C6 C5 74.1(6) . . . . ? C15 Ir1 C6 C5 -14.2(7) . . . . ? C9 Ir1 C6 C5 158.1(6) . . . . ? C14 Ir1 C6 C5 -22.0(13) . . . . ? C11 Ir1 C6 C5 -117.7(6) . . . . ? C10 Ir1 C6 C5 -87.6(6) . . . . ? C8 Ir1 C6 C5 143.3(6) . . . . ? C1 N2 C7 C8 -20.2(11) . . . . ? C3 N2 C7 C8 159.3(9) . . . . ? N2 C7 C8 C9 -55.5(11) . . . . ? N2 C7 C8 Ir1 23.2(9) . . . . ? C1 Ir1 C8 C9 102.3(7) . . . . ? C5 Ir1 C8 C9 62.5(9) . . . . ? C6 Ir1 C8 C9 26.4(7) . . . . ? C15 Ir1 C8 C9 -174.0(6) . . . . ? C14 Ir1 C8 C9 -158.6(7) . . . . ? C11 Ir1 C8 C9 -80.7(6) . . . . ? C10 Ir1 C8 C9 -80.6(7) . . . . ? C1 Ir1 C8 C7 -16.1(7) . . . . ? C5 Ir1 C8 C7 -56.0(10) . . . . ? C6 Ir1 C8 C7 -92.1(7) . . . . ? C15 Ir1 C8 C7 67.5(8) . . . . ? C9 Ir1 C8 C7 -118.5(10) . . . . ? C14 Ir1 C8 C7 82.9(7) . . . . ? C11 Ir1 C8 C7 160.8(7) . . . . ? C10 Ir1 C8 C7 161.0(6) . . . . ? C7 C8 C9 Ir1 100.8(8) . . . . ? C1 Ir1 C9 C8 -70.8(6) . . . . ? C5 Ir1 C9 C8 -141.8(6) . . . . ? C6 Ir1 C9 C8 -156.6(7) . . . . ? C15 Ir1 C9 C8 10.8(11) . . . . ? C14 Ir1 C9 C8 23.4(7) . . . . ? C11 Ir1 C9 C8 98.2(6) . . . . ? C10 Ir1 C9 C8 119.1(6) . . . . ? C1 Ir1 C10 C11 171.6(9) . . . . ? C5 Ir1 C10 C11 -158.8(6) . . . . ? C6 Ir1 C10 C11 -121.8(6) . . . . ? C15 Ir1 C10 C11 112.1(6) . . . . ? C9 Ir1 C10 C11 -38.5(7) . . . . ? C14 Ir1 C10 C11 76.4(6) . . . . ? C8 Ir1 C10 C11 -0.3(7) . . . . ? C1 Ir1 C10 C17 50.6(13) . . . . ? C5 Ir1 C10 C17 80.2(7) . . . . ? C6 Ir1 C10 C17 117.1(7) . . . . ? C15 Ir1 C10 C17 -9.0(6) . . . . ? C9 Ir1 C10 C17 -159.5(6) . . . . ? C14 Ir1 C10 C17 -44.6(7) . . . . ? C11 Ir1 C10 C17 -121.1(9) . . . . ? C8 Ir1 C10 C17 -121.3(7) . . . . ? C17 C10 C11 C12 0.3(15) . . . . ? Ir1 C10 C11 C12 -103.9(9) . . . . ? C17 C10 C11 Ir1 104.2(8) . . . . ? C1 Ir1 C11 C10 -169.1(12) . . . . ? C5 Ir1 C11 C10 24.2(7) . . . . ? C6 Ir1 C11 C10 61.3(6) . . . . ? C15 Ir1 C11 C10 -65.2(6) . . . . ? C9 Ir1 C11 C10 145.2(6) . . . . ? C14 Ir1 C11 C10 -98.4(6) . . . . ? C8 Ir1 C11 C10 179.8(6) . . . . ? C1 Ir1 C11 C12 -46.3(17) . . . . ? C5 Ir1 C11 C12 147.0(7) . . . . ? C6 Ir1 C11 C12 -175.9(7) . . . . ? C15 Ir1 C11 C12 57.6(7) . . . . ? C9 Ir1 C11 C12 -92.0(7) . . . . ? C14 Ir1 C11 C12 24.4(7) . . . . ? C10 Ir1 C11 C12 122.8(10) . . . . ? C8 Ir1 C11 C12 -57.4(7) . . . . ? C10 C11 C12 C13 47.7(13) . . . . ? Ir1 C11 C12 C13 -36.3(10) . . . . ? C11 C12 C13 C14 30.0(12) . . . . ? C12 C13 C14 C15 -89.7(11) . . . . ? C12 C13 C14 Ir1 -8.2(10) . . . . ? C1 Ir1 C14 C15 -83.1(6) . . . . ? C5 Ir1 C14 C15 -4.7(7) . . . . ? C6 Ir1 C14 C15 11.0(13) . . . . ? C9 Ir1 C14 C15 -169.1(6) . . . . ? C11 Ir1 C14 C15 111.5(6) . . . . ? C10 Ir1 C14 C15 76.8(6) . . . . ? C8 Ir1 C14 C15 -155.8(6) . . . . ? C1 Ir1 C14 C13 157.0(6) . . . . ? C5 Ir1 C14 C13 -124.6(6) . . . . ? C6 Ir1 C14 C13 -108.9(11) . . . . ? C15 Ir1 C14 C13 -119.9(9) . . . . ? C9 Ir1 C14 C13 71.0(7) . . . . ? C11 Ir1 C14 C13 -8.4(6) . . . . ? C10 Ir1 C14 C13 -43.1(6) . . . . ? C8 Ir1 C14 C13 84.3(6) . . . . ? C13 C14 C15 C16 0.0(14) . . . . ? Ir1 C14 C15 C16 -105.1(9) . . . . ? C13 C14 C15 Ir1 105.1(8) . . . . ? C1 Ir1 C15 C14 99.3(6) . . . . ? C5 Ir1 C15 C14 176.1(6) . . . . ? C6 Ir1 C15 C14 -175.4(5) . . . . ? C9 Ir1 C15 C14 19.8(10) . . . . ? C11 Ir1 C15 C14 -65.8(6) . . . . ? C10 Ir1 C15 C14 -97.8(6) . . . . ? C8 Ir1 C15 C14 26.6(6) . . . . ? C1 Ir1 C15 C16 -138.0(7) . . . . ? C5 Ir1 C15 C16 -61.3(7) . . . . ? C6 Ir1 C15 C16 -52.8(8) . . . . ? C9 Ir1 C15 C16 142.4(7) . . . . ? C14 Ir1 C15 C16 122.6(9) . . . . ? C11 Ir1 C15 C16 56.9(7) . . . . ? C10 Ir1 C15 C16 24.8(7) . . . . ? C8 Ir1 C15 C16 149.2(6) . . . . ? C14 C15 C16 C17 48.0(13) . . . . ? Ir1 C15 C16 C17 -36.8(10) . . . . ? C11 C10 C17 C16 -90.2(11) . . . . ? Ir1 C10 C17 C16 -7.9(10) . . . . ? C15 C16 C17 C10 29.5(12) . . . . ? C32 N31 C31 N32 -0.1(10) . . . . ? C34 N31 C31 N32 -177.9(8) . . . . ? C32 N31 C31 Ir31 170.7(7) . . . . ? C34 N31 C31 Ir31 -7.1(12) . . . . ? C36 Ir31 C31 N32 125.4(9) . . . . ? C35 Ir31 C31 N32 162.4(9) . . . . ? C44 Ir31 C31 N32 -107.7(9) . . . . ? C45 Ir31 C31 N32 -72.0(9) . . . . ? C39 Ir31 C31 N32 38.1(9) . . . . ? C40 Ir31 C31 N32 5(2) . . . . ? C41 Ir31 C31 N32 -168.5(8) . . . . ? C38 Ir31 C31 N32 4.4(8) . . . . ? C36 Ir31 C31 N31 -43.4(8) . . . . ? C35 Ir31 C31 N31 -6.4(8) . . . . ? C44 Ir31 C31 N31 83.5(8) . . . . ? C45 Ir31 C31 N31 119.2(8) . . . . ? C39 Ir31 C31 N31 -130.7(9) . . . . ? C40 Ir31 C31 N31 -163.7(11) . . . . ? C41 Ir31 C31 N31 22.7(16) . . . . ? C38 Ir31 C31 N31 -164.4(9) . . . . ? N31 C31 N32 C33 0.1(10) . . . . ? Ir31 C31 N32 C33 -170.2(7) . . . . ? N31 C31 N32 C37 -179.5(8) . . . . ? Ir31 C31 N32 C37 10.2(13) . . . . ? C31 N31 C32 C33 0.0(11) . . . . ? C34 N31 C32 C33 177.2(10) . . . . ? N31 C32 C33 N32 0.1(11) . . . . ? C31 N32 C33 C32 -0.1(11) . . . . ? C37 N32 C33 C32 179.4(10) . . . . ? C31 N31 C34 C35 21.1(12) . . . . ? C32 N31 C34 C35 -156.0(10) . . . . ? N31 C34 C35 C36 54.7(12) . . . . ? N31 C34 C35 Ir31 -24.6(10) . . . . ? C31 Ir31 C35 C36 -97.9(7) . . . . ? C44 Ir31 C35 C36 169.0(7) . . . . ? C45 Ir31 C35 C36 172.0(6) . . . . ? C39 Ir31 C35 C36 -25.1(8) . . . . ? C40 Ir31 C35 C36 75.6(7) . . . . ? C41 Ir31 C35 C36 91.8(7) . . . . ? C38 Ir31 C35 C36 -61.9(10) . . . . ? C31 Ir31 C35 C34 17.1(7) . . . . ? C36 Ir31 C35 C34 114.9(10) . . . . ? C44 Ir31 C35 C34 -76.1(8) . . . . ? C45 Ir31 C35 C34 -73.1(8) . . . . ? C39 Ir31 C35 C34 89.8(8) . . . . ? C40 Ir31 C35 C34 -169.5(7) . . . . ? C41 Ir31 C35 C34 -153.3(8) . . . . ? C38 Ir31 C35 C34 53.0(11) . . . . ? C34 C35 C36 Ir31 -103.6(8) . . . . ? C31 Ir31 C36 C35 75.5(7) . . . . ? C44 Ir31 C36 C35 -13.8(8) . . . . ? C45 Ir31 C36 C35 -22.1(16) . . . . ? C39 Ir31 C36 C35 158.6(7) . . . . ? C40 Ir31 C36 C35 -117.9(7) . . . . ? C41 Ir31 C36 C35 -86.2(7) . . . . ? C38 Ir31 C36 C35 142.7(6) . . . . ? C31 N32 C37 C38 -23.4(12) . . . . ? C33 N32 C37 C38 157.1(10) . . . . ? N32 C37 C38 C39 -56.1(13) . . . . ? N32 C37 C38 Ir31 25.1(11) . . . . ? C31 Ir31 C38 C39 102.5(7) . . . . ? C36 Ir31 C38 C39 29.1(8) . . . . ? C35 Ir31 C38 C39 65.8(9) . . . . ? C44 Ir31 C38 C39 -171.0(6) . . . . ? C45 Ir31 C38 C39 -155.5(7) . . . . ? C40 Ir31 C38 C39 -77.4(7) . . . . ? C41 Ir31 C38 C39 -80.6(7) . . . . ? C31 Ir31 C38 C37 -16.8(8) . . . . ? C36 Ir31 C38 C37 -90.2(9) . . . . ? C35 Ir31 C38 C37 -53.4(12) . . . . ? C44 Ir31 C38 C37 69.7(9) . . . . ? C45 Ir31 C38 C37 85.3(8) . . . . ? C39 Ir31 C38 C37 -119.2(11) . . . . ? C40 Ir31 C38 C37 163.4(8) . . . . ? C41 Ir31 C38 C37 160.2(7) . . . . ? C37 C38 C39 Ir31 103.4(9) . . . . ? C31 Ir31 C39 C38 -70.2(7) . . . . ? C36 Ir31 C39 C38 -154.4(7) . . . . ? C35 Ir31 C39 C38 -139.5(7) . . . . ? C44 Ir31 C39 C38 14.8(10) . . . . ? C45 Ir31 C39 C38 25.9(7) . . . . ? C40 Ir31 C39 C38 101.5(7) . . . . ? C41 Ir31 C39 C38 119.5(6) . . . . ? C31 Ir31 C40 C41 -176.2(12) . . . . ? C36 Ir31 C40 C41 65.9(7) . . . . ? C35 Ir31 C40 C41 28.9(7) . . . . ? C44 Ir31 C40 C41 -63.3(6) . . . . ? C45 Ir31 C40 C41 -96.5(6) . . . . ? C39 Ir31 C40 C41 151.0(6) . . . . ? C38 Ir31 C40 C41 -175.5(6) . . . . ? C31 Ir31 C40 C47 -56.1(17) . . . . ? C36 Ir31 C40 C47 -174.0(7) . . . . ? C35 Ir31 C40 C47 149.0(7) . . . . ? C44 Ir31 C40 C47 56.8(7) . . . . ? C45 Ir31 C40 C47 23.6(7) . . . . ? C39 Ir31 C40 C47 -88.9(8) . . . . ? C41 Ir31 C40 C47 120.1(10) . . . . ? C38 Ir31 C40 C47 -55.4(8) . . . . ? C47 C40 C41 C42 4.4(15) . . . . ? Ir31 C40 C41 C42 104.9(9) . . . . ? C47 C40 C41 Ir31 -100.5(9) . . . . ? C31 Ir31 C41 C40 177.1(9) . . . . ? C36 Ir31 C41 C40 -117.5(6) . . . . ? C35 Ir31 C41 C40 -154.6(6) . . . . ? C44 Ir31 C41 C40 113.8(6) . . . . ? C45 Ir31 C41 C40 78.2(6) . . . . ? C39 Ir31 C41 C40 -32.2(7) . . . . ? C38 Ir31 C41 C40 5.6(8) . . . . ? C31 Ir31 C41 C42 54.4(14) . . . . ? C36 Ir31 C41 C42 119.9(8) . . . . ? C35 Ir31 C41 C42 82.7(8) . . . . ? C44 Ir31 C41 C42 -8.8(7) . . . . ? C45 Ir31 C41 C42 -44.5(8) . . . . ? C39 Ir31 C41 C42 -154.9(8) . . . . ? C40 Ir31 C41 C42 -122.7(10) . . . . ? C38 Ir31 C41 C42 -117.1(8) . . . . ? C40 C41 C42 C43 -92.4(13) . . . . ? Ir31 C41 C42 C43 -8.9(12) . . . . ? C41 C42 C43 C44 31.1(14) . . . . ? C42 C43 C44 C45 46.6(13) . . . . ? C42 C43 C44 Ir31 -38.2(11) . . . . ? C31 Ir31 C44 C45 99.6(6) . . . . ? C36 Ir31 C44 C45 -175.8(6) . . . . ? C35 Ir31 C44 C45 175.9(6) . . . . ? C39 Ir31 C44 C45 17.7(10) . . . . ? C40 Ir31 C44 C45 -66.4(6) . . . . ? C41 Ir31 C44 C45 -98.3(6) . . . . ? C38 Ir31 C44 C45 26.7(7) . . . . ? C31 Ir31 C44 C43 -137.0(7) . . . . ? C36 Ir31 C44 C43 -52.4(9) . . . . ? C35 Ir31 C44 C43 -60.7(7) . . . . ? C45 Ir31 C44 C43 123.4(10) . . . . ? C39 Ir31 C44 C43 141.2(7) . . . . ? C40 Ir31 C44 C43 57.0(7) . . . . ? C41 Ir31 C44 C43 25.1(7) . . . . ? C38 Ir31 C44 C43 150.1(7) . . . . ? C43 C44 C45 C46 -0.4(14) . . . . ? Ir31 C44 C45 C46 104.2(8) . . . . ? C43 C44 C45 Ir31 -104.6(9) . . . . ? C31 Ir31 C45 C44 -84.1(6) . . . . ? C36 Ir31 C45 C44 11.3(15) . . . . ? C35 Ir31 C45 C44 -5.1(8) . . . . ? C39 Ir31 C45 C44 -169.4(6) . . . . ? C40 Ir31 C45 C44 111.0(6) . . . . ? C41 Ir31 C45 C44 75.9(6) . . . . ? C38 Ir31 C45 C44 -155.0(6) . . . . ? C31 Ir31 C45 C46 156.4(7) . . . . ? C36 Ir31 C45 C46 -108.3(13) . . . . ? C35 Ir31 C45 C46 -124.7(7) . . . . ? C44 Ir31 C45 C46 -119.6(10) . . . . ? C39 Ir31 C45 C46 71.0(8) . . . . ? C40 Ir31 C45 C46 -8.6(7) . . . . ? C41 Ir31 C45 C46 -43.7(7) . . . . ? C38 Ir31 C45 C46 85.5(7) . . . . ? C44 C45 C46 C47 -89.6(11) . . . . ? Ir31 C45 C46 C47 -8.6(11) . . . . ? C45 C46 C47 C40 31.4(13) . . . . ? C41 C40 C47 C46 43.9(14) . . . . ? Ir31 C40 C47 C46 -36.9(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.281 _refine_diff_density_min -1.175 _refine_diff_density_rms 0.197 data_str862mm _database_code_depnum_ccdc_archive 'CCDC 656991' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety C17H22Cl2IrN2,PF6 _chemical_formula_sum 'C17 H22 Cl2 F6 Ir N2 P' _chemical_formula_weight 662.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_H-M P21/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 15.2900(11) _cell_length_b 10.7009(8) _cell_length_c 12.7347(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.789(2) _cell_angle_gamma 90.00 _cell_volume 2069.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8374 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 50.00 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 8374 _exptl_crystal_density_diffrn 2.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 6.848 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8374 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3109 _reflns_number_gt 2380 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms could not be found in the difference maps and had been added in 'idealized' positions. No reliance should be placed on the reported ethylenic H-atom coordinates ; _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^)+(0.0750P)^2^+41.7435P] 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 3109 _refine_ls_number_parameters 262 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1743 _refine_ls_wR_factor_gt 0.1315 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir -0.29366(3) 0.57605(4) -0.17716(4) 0.0204(2) Uani 1 1 d . . . P1 P 0.2455(3) -0.0691(4) 0.1346(4) 0.0409(11) Uani 1 1 d . . . Cl1 Cl -0.0397(3) 0.3094(4) 0.0894(4) 0.0473(10) Uani 1 1 d . . . N1 N -0.1741(8) 0.4278(10) -0.0331(11) 0.030(3) Uani 1 1 d . . . C1 C -0.1959(8) 0.4649(11) -0.1315(10) 0.017(2) Uani 1 1 d U . . F1 F 0.211(2) -0.139(2) 0.0330(15) 0.185(13) Uani 1 1 d . . . Cl2 Cl 0.0323(3) 0.3300(4) -0.1633(4) 0.0513(11) Uani 1 1 d . . . N2 N -0.1288(8) 0.4403(10) -0.1866(11) 0.032(3) Uani 1 1 d . . . C2 C -0.0904(10) 0.3716(14) -0.0232(13) 0.035(3) Uani 1 1 d . . . F2 F 0.3276(13) -0.1520(18) 0.132(3) 0.178(13) Uani 1 1 d . . . C3 C -0.0619(8) 0.3804(13) -0.1194(11) 0.025(3) Uani 1 1 d . . . F3 F 0.2022(15) -0.1698(16) 0.1954(16) 0.146(9) Uani 1 1 d . . . C4 C -0.2356(9) 0.4537(14) 0.0430(12) 0.030(3) Uani 1 1 d U . . H4A H -0.2041 0.4746 0.1113 0.037 Uiso 1 1 calc R . . H4B H -0.2726 0.3815 0.0512 0.037 Uiso 1 1 calc R . . F4 F 0.2884(14) 0.001(2) 0.2367(12) 0.131(8) Uani 1 1 d . . . C5 C -0.2928(9) 0.5671(12) -0.0028(11) 0.024(3) Uani 1 1 d U . . H5 H -0.3538 0.5615 -0.0149 0.029 Uiso 1 1 calc R . . F5 F 0.1708(14) 0.013(2) 0.149(4) 0.26(2) Uani 1 1 d . . . C6 C -0.2496(14) 0.6753(15) -0.0245(14) 0.048(5) Uani 1 1 d . . . H6A H -0.1885 0.6793 -0.0119 0.058 Uiso 1 1 calc R . . H6B H -0.2815 0.7444 -0.0517 0.058 Uiso 1 1 calc R . . F6 F 0.2939(16) 0.0311(14) 0.0740(13) 0.133(8) Uani 1 1 d . . . C7 C -0.1383(11) 0.4831(16) -0.2945(11) 0.037(3) Uani 1 1 d . . . H7A H -0.1590 0.4154 -0.3417 0.044 Uiso 1 1 calc R . . H7B H -0.0820 0.5116 -0.3132 0.044 Uiso 1 1 calc R . . C8 C -0.2046(10) 0.5901(15) -0.3049(12) 0.035(4) Uani 1 1 d . . . H8 H -0.2531 0.5859 -0.3562 0.041 Uiso 1 1 calc R . . C9 C -0.1936(10) 0.6951(13) -0.2383(13) 0.034(3) Uani 1 1 d . . . H9A H -0.1452 0.7000 -0.1868 0.040 Uiso 1 1 calc R . . H9B H -0.2346 0.7595 -0.2458 0.040 Uiso 1 1 calc R . . C10 C -0.3917(11) 0.6897(16) -0.285(2) 0.060(6) Uani 1 1 d . . . H10 H -0.3439 0.7369 -0.3014 0.071 Uiso 1 1 calc R . . C11 C -0.4150(9) 0.6971(13) -0.1896(12) 0.031(3) Uani 1 1 d U . . H11 H -0.3809 0.7491 -0.1426 0.037 Uiso 1 1 calc R . . C12 C -0.4895(13) 0.6321(19) -0.1473(18) 0.061(6) Uani 1 1 d . . . H12A H -0.5445 0.6642 -0.1832 0.073 Uiso 1 1 calc R . . H12B H -0.4880 0.6518 -0.0728 0.073 Uiso 1 1 calc R . . C13 C -0.4883(13) 0.4930(17) -0.160(2) 0.066(7) Uani 1 1 d . . . H13A H -0.5325 0.4709 -0.2180 0.079 Uiso 1 1 calc R . . H13B H -0.5063 0.4561 -0.0964 0.079 Uiso 1 1 calc R . . C14 C -0.4024(10) 0.4330(13) -0.1801(16) 0.038(4) Uani 1 1 d . . . H14 H -0.3711 0.3950 -0.1217 0.045 Uiso 1 1 calc R . . C15 C -0.3661(9) 0.4267(12) -0.2666(12) 0.025(3) Uani 1 1 d U . . H15 H -0.3101 0.3926 -0.2658 0.030 Uiso 1 1 calc R . . C16 C -0.4167(17) 0.477(2) -0.3736(17) 0.079(8) Uani 1 1 d . . . H16A H -0.3802 0.4632 -0.4299 0.095 Uiso 1 1 calc R . . H16B H -0.4702 0.4284 -0.3902 0.095 Uiso 1 1 calc R . . C17 C -0.4396(12) 0.6071(17) -0.3715(15) 0.047(4) Uani 1 1 d U . . H17A H -0.5022 0.6125 -0.3657 0.056 Uiso 1 1 calc R . . H17B H -0.4304 0.6427 -0.4394 0.056 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 0.0217(4) 0.0175(3) 0.0229(3) 0.00129(19) 0.0063(2) 0.00042(18) P1 0.056(3) 0.028(2) 0.039(2) 0.0016(17) 0.009(2) 0.0020(17) Cl1 0.041(2) 0.044(2) 0.053(3) 0.0153(19) -0.0096(18) 0.0000(17) N1 0.030(7) 0.035(7) 0.025(7) 0.011(5) 0.002(6) 0.002(5) C1 0.015(3) 0.018(3) 0.016(3) -0.0002(19) -0.0027(19) 0.0015(19) F1 0.34(3) 0.151(19) 0.061(11) -0.030(12) 0.012(15) -0.14(2) Cl2 0.031(2) 0.064(3) 0.059(3) -0.017(2) 0.0068(19) 0.0171(18) N2 0.029(7) 0.029(6) 0.039(8) -0.006(5) 0.011(6) 0.002(5) C2 0.036(8) 0.029(7) 0.041(9) -0.002(7) 0.011(7) 0.001(6) F2 0.111(14) 0.086(13) 0.34(4) 0.038(18) 0.05(2) 0.053(11) C3 0.017(6) 0.027(7) 0.030(8) -0.008(6) -0.007(5) 0.005(5) F3 0.23(2) 0.108(13) 0.123(15) -0.037(11) 0.104(16) -0.102(14) C4 0.026(5) 0.038(5) 0.027(5) 0.001(4) 0.001(4) -0.001(4) F4 0.177(18) 0.164(18) 0.057(9) -0.018(11) 0.032(10) -0.091(15) C5 0.015(4) 0.034(5) 0.022(5) -0.003(4) -0.006(4) 0.002(4) F5 0.099(15) 0.102(15) 0.58(7) -0.08(3) 0.01(3) 0.041(13) C6 0.082(13) 0.027(8) 0.040(10) -0.008(7) 0.025(9) 0.010(8) F6 0.27(2) 0.061(8) 0.077(11) 0.002(8) 0.065(14) -0.062(12) C7 0.046(9) 0.047(9) 0.018(7) -0.002(7) 0.005(6) 0.008(7) C8 0.037(9) 0.052(10) 0.017(7) 0.016(6) 0.010(6) 0.002(7) C9 0.026(8) 0.029(7) 0.047(9) 0.010(7) 0.010(7) -0.010(6) C10 0.031(9) 0.036(9) 0.117(19) 0.041(10) 0.028(10) 0.009(7) C11 0.024(5) 0.033(5) 0.030(5) -0.002(4) -0.019(4) 0.008(4) C12 0.051(11) 0.070(13) 0.070(14) 0.008(11) 0.034(10) 0.029(10) C13 0.053(12) 0.052(12) 0.103(18) -0.027(12) 0.048(12) -0.019(9) C14 0.023(8) 0.029(8) 0.061(12) -0.004(7) -0.001(8) -0.013(6) C15 0.023(3) 0.026(3) 0.024(3) 0.000(2) -0.001(2) -0.0009(19) C16 0.103(18) 0.087(16) 0.044(12) 0.008(12) 0.001(11) -0.063(15) C17 0.046(4) 0.049(4) 0.045(4) 0.000(2) 0.003(2) 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 Ir1 C1 1.944(12) . ? Ir1 C15 2.186(14) . ? Ir1 C9 2.203(12) . ? Ir1 C5 2.221(14) . ? Ir1 C8 2.247(12) . ? Ir1 C6 2.248(18) . ? Ir1 C11 2.253(13) . ? Ir1 C14 2.257(13) . ? Ir1 C10 2.266(19) . ? P1 F5 1.472(19) . ? P1 F3 1.522(14) . ? P1 F1 1.537(18) . ? P1 F2 1.540(16) . ? P1 F6 1.559(13) . ? P1 F4 1.576(17) . ? Cl1 C2 1.685(17) . ? N1 C1 1.320(18) . ? N1 C2 1.407(19) . ? N1 C4 1.454(18) . ? C1 N2 1.336(16) . ? Cl2 C3 1.694(13) . ? N2 C3 1.408(19) . ? N2 C7 1.44(2) . ? C2 C3 1.35(2) . ? C4 C5 1.567(19) . ? C5 C6 1.38(2) . ? C7 C8 1.52(2) . ? C8 C9 1.41(2) . ? C10 C11 1.31(3) . ? C10 C17 1.53(3) . ? C11 C12 1.49(2) . ? C12 C13 1.50(3) . ? C13 C14 1.51(2) . ? C14 C15 1.29(2) . ? C15 C16 1.58(3) . ? C16 C17 1.44(3) . ? 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 C15 91.9(5) . . ? C1 Ir1 C9 85.3(5) . . ? C15 Ir1 C9 124.7(6) . . ? C1 Ir1 C5 76.2(5) . . ? C15 Ir1 C5 115.6(5) . . ? C9 Ir1 C5 117.1(6) . . ? C1 Ir1 C8 75.4(5) . . ? C15 Ir1 C8 89.2(6) . . ? C9 Ir1 C8 36.8(6) . . ? C5 Ir1 C8 142.6(5) . . ? C1 Ir1 C6 83.7(6) . . ? C15 Ir1 C6 151.4(6) . . ? C9 Ir1 C6 83.3(6) . . ? C5 Ir1 C6 35.9(5) . . ? C8 Ir1 C6 116.7(6) . . ? C1 Ir1 C11 166.0(5) . . ? C15 Ir1 C11 91.2(5) . . ? C9 Ir1 C11 104.1(6) . . ? C5 Ir1 C11 90.2(5) . . ? C8 Ir1 C11 118.4(5) . . ? C6 Ir1 C11 87.1(6) . . ? C1 Ir1 C14 97.4(6) . . ? C15 Ir1 C14 33.8(6) . . ? C9 Ir1 C14 158.0(7) . . ? C5 Ir1 C14 84.6(6) . . ? C8 Ir1 C14 122.8(6) . . ? C6 Ir1 C14 118.7(7) . . ? C11 Ir1 C14 77.9(6) . . ? C1 Ir1 C10 160.0(7) . . ? C15 Ir1 C10 79.5(7) . . ? C9 Ir1 C10 84.9(6) . . ? C5 Ir1 C10 123.8(6) . . ? C8 Ir1 C10 86.4(6) . . ? C6 Ir1 C10 112.4(8) . . ? C11 Ir1 C10 33.8(6) . . ? C14 Ir1 C10 85.5(6) . . ? F5 P1 F3 88.4(17) . . ? F5 P1 F1 102(2) . . ? F3 P1 F1 87.4(10) . . ? F5 P1 F2 174(2) . . ? F3 P1 F2 90.5(13) . . ? F1 P1 F2 84.3(17) . . ? F5 P1 F6 94.0(16) . . ? F3 P1 F6 177.4(14) . . ? F1 P1 F6 93.3(10) . . ? F2 P1 F6 87.1(13) . . ? F5 P1 F4 82.3(17) . . ? F3 P1 F4 94.7(10) . . ? F1 P1 F4 175.7(14) . . ? F2 P1 F4 91.8(16) . . ? F6 P1 F4 84.5(9) . . ? C1 N1 C2 109.8(12) . . ? C1 N1 C4 117.7(12) . . ? C2 N1 C4 132.5(14) . . ? N1 C1 N2 108.4(12) . . ? N1 C1 Ir1 124.5(9) . . ? N2 C1 Ir1 125.1(10) . . ? C1 N2 C3 108.6(12) . . ? C1 N2 C7 116.1(12) . . ? C3 N2 C7 135.2(12) . . ? C3 C2 N1 106.1(13) . . ? C3 C2 Cl1 129.3(11) . . ? N1 C2 Cl1 124.6(11) . . ? C2 C3 N2 107.1(11) . . ? C2 C3 Cl2 130.9(11) . . ? N2 C3 Cl2 122.0(11) . . ? N1 C4 C5 106.0(11) . . ? C6 C5 C4 117.8(13) . . ? C6 C5 Ir1 73.1(9) . . ? C4 C5 Ir1 110.0(9) . . ? C5 C6 Ir1 71.0(9) . . ? N2 C7 C8 108.3(11) . . ? C9 C8 C7 121.1(15) . . ? C9 C8 Ir1 69.9(7) . . ? C7 C8 Ir1 109.9(9) . . ? C8 C9 Ir1 73.3(7) . . ? C11 C10 C17 122.8(15) . . ? C11 C10 Ir1 72.6(11) . . ? C17 C10 Ir1 110.6(11) . . ? C10 C11 C12 127.7(16) . . ? C10 C11 Ir1 73.7(9) . . ? C12 C11 Ir1 111.4(10) . . ? C11 C12 C13 113.9(13) . . ? C12 C13 C14 117.6(14) . . ? C15 C14 C13 129.6(18) . . ? C15 C14 Ir1 70.1(8) . . ? C13 C14 Ir1 111.2(10) . . ? C14 C15 C16 120.1(16) . . ? C14 C15 Ir1 76.1(9) . . ? C16 C15 Ir1 111.6(10) . . ? C17 C16 C15 114.1(17) . . ? C16 C17 C10 118.5(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 -2.5(16) . . . . ? C4 N1 C1 N2 175.8(12) . . . . ? C2 N1 C1 Ir1 -167.1(10) . . . . ? C4 N1 C1 Ir1 11.1(18) . . . . ? C15 Ir1 C1 N1 -112.3(12) . . . . ? C9 Ir1 C1 N1 123.1(12) . . . . ? C5 Ir1 C1 N1 3.7(11) . . . . ? C8 Ir1 C1 N1 159.1(13) . . . . ? C6 Ir1 C1 N1 39.3(12) . . . . ? C11 Ir1 C1 N1 -10(3) . . . . ? C14 Ir1 C1 N1 -78.8(13) . . . . ? C10 Ir1 C1 N1 -176.0(15) . . . . ? C15 Ir1 C1 N2 85.6(12) . . . . ? C9 Ir1 C1 N2 -39.0(12) . . . . ? C5 Ir1 C1 N2 -158.5(12) . . . . ? C8 Ir1 C1 N2 -3.0(12) . . . . ? C6 Ir1 C1 N2 -122.8(12) . . . . ? C11 Ir1 C1 N2 -171.7(17) . . . . ? C14 Ir1 C1 N2 119.0(12) . . . . ? C10 Ir1 C1 N2 22(2) . . . . ? N1 C1 N2 C3 2.0(15) . . . . ? Ir1 C1 N2 C3 166.6(9) . . . . ? N1 C1 N2 C7 -175.5(13) . . . . ? Ir1 C1 N2 C7 -11.0(18) . . . . ? C1 N1 C2 C3 2.0(17) . . . . ? C4 N1 C2 C3 -176.0(14) . . . . ? C1 N1 C2 Cl1 -178.7(11) . . . . ? C4 N1 C2 Cl1 3(2) . . . . ? N1 C2 C3 N2 -0.7(16) . . . . ? Cl1 C2 C3 N2 -179.9(12) . . . . ? N1 C2 C3 Cl2 -178.9(11) . . . . ? Cl1 C2 C3 Cl2 2(2) . . . . ? C1 N2 C3 C2 -0.8(16) . . . . ? C7 N2 C3 C2 176.1(16) . . . . ? C1 N2 C3 Cl2 177.6(10) . . . . ? C7 N2 C3 Cl2 -5(2) . . . . ? C1 N1 C4 C5 -23.3(17) . . . . ? C2 N1 C4 C5 154.5(14) . . . . ? N1 C4 C5 C6 -56.8(17) . . . . ? N1 C4 C5 Ir1 24.1(13) . . . . ? C1 Ir1 C5 C6 98.4(10) . . . . ? C15 Ir1 C5 C6 -176.2(10) . . . . ? C9 Ir1 C5 C6 21.1(11) . . . . ? C8 Ir1 C5 C6 56.9(13) . . . . ? C11 Ir1 C5 C6 -84.8(10) . . . . ? C14 Ir1 C5 C6 -162.6(10) . . . . ? C10 Ir1 C5 C6 -81.8(12) . . . . ? C1 Ir1 C5 C4 -15.7(9) . . . . ? C15 Ir1 C5 C4 69.7(10) . . . . ? C9 Ir1 C5 C4 -93.0(10) . . . . ? C8 Ir1 C5 C4 -57.2(13) . . . . ? C6 Ir1 C5 C4 -114.1(14) . . . . ? C11 Ir1 C5 C4 161.1(9) . . . . ? C14 Ir1 C5 C4 83.3(9) . . . . ? C10 Ir1 C5 C4 164.1(9) . . . . ? C4 C5 C6 Ir1 104.1(12) . . . . ? C1 Ir1 C6 C5 -75.2(9) . . . . ? C15 Ir1 C6 C5 7.1(18) . . . . ? C9 Ir1 C6 C5 -161.1(10) . . . . ? C8 Ir1 C6 C5 -145.2(9) . . . . ? C11 Ir1 C6 C5 94.3(10) . . . . ? C14 Ir1 C6 C5 19.8(12) . . . . ? C10 Ir1 C6 C5 117.2(9) . . . . ? C1 N2 C7 C8 23.0(19) . . . . ? C3 N2 C7 C8 -153.7(15) . . . . ? N2 C7 C8 C9 54.2(18) . . . . ? N2 C7 C8 Ir1 -23.7(16) . . . . ? C1 Ir1 C8 C9 -102.0(10) . . . . ? C15 Ir1 C8 C9 165.8(10) . . . . ? C5 Ir1 C8 C9 -60.4(13) . . . . ? C6 Ir1 C8 C9 -27.0(11) . . . . ? C11 Ir1 C8 C9 74.9(11) . . . . ? C14 Ir1 C8 C9 168.6(9) . . . . ? C10 Ir1 C8 C9 86.3(11) . . . . ? C1 Ir1 C8 C7 14.9(11) . . . . ? C15 Ir1 C8 C7 -77.2(12) . . . . ? C9 Ir1 C8 C7 116.9(16) . . . . ? C5 Ir1 C8 C7 56.6(15) . . . . ? C6 Ir1 C8 C7 89.9(12) . . . . ? C11 Ir1 C8 C7 -168.1(10) . . . . ? C14 Ir1 C8 C7 -74.5(13) . . . . ? C10 Ir1 C8 C7 -156.8(12) . . . . ? C7 C8 C9 Ir1 -101.6(12) . . . . ? C1 Ir1 C9 C8 71.7(9) . . . . ? C15 Ir1 C9 C8 -17.3(12) . . . . ? C5 Ir1 C9 C8 143.6(9) . . . . ? C6 Ir1 C9 C8 155.9(10) . . . . ? C11 Ir1 C9 C8 -118.8(9) . . . . ? C14 Ir1 C9 C8 -26(2) . . . . ? C10 Ir1 C9 C8 -90.8(11) . . . . ? C1 Ir1 C10 C11 174.1(13) . . . . ? C15 Ir1 C10 C11 108.4(11) . . . . ? C9 Ir1 C10 C11 -124.9(11) . . . . ? C5 Ir1 C10 C11 -5.5(13) . . . . ? C8 Ir1 C10 C11 -161.8(11) . . . . ? C6 Ir1 C10 C11 -44.3(12) . . . . ? C14 Ir1 C10 C11 74.9(11) . . . . ? C1 Ir1 C10 C17 55(2) . . . . ? C15 Ir1 C10 C17 -10.8(11) . . . . ? C9 Ir1 C10 C17 115.9(12) . . . . ? C5 Ir1 C10 C17 -124.7(12) . . . . ? C8 Ir1 C10 C17 79.0(12) . . . . ? C6 Ir1 C10 C17 -163.6(11) . . . . ? C11 Ir1 C10 C17 -119.2(15) . . . . ? C14 Ir1 C10 C17 -44.4(12) . . . . ? C17 C10 C11 C12 -1(3) . . . . ? Ir1 C10 C11 C12 -104.8(16) . . . . ? C17 C10 C11 Ir1 103.7(15) . . . . ? C1 Ir1 C11 C10 -171.7(19) . . . . ? C15 Ir1 C11 C10 -68.9(11) . . . . ? C9 Ir1 C11 C10 57.4(12) . . . . ? C5 Ir1 C11 C10 175.5(11) . . . . ? C8 Ir1 C11 C10 20.8(13) . . . . ? C6 Ir1 C11 C10 139.7(11) . . . . ? C14 Ir1 C11 C10 -100.1(12) . . . . ? C1 Ir1 C11 C12 -47(3) . . . . ? C15 Ir1 C11 C12 55.8(13) . . . . ? C9 Ir1 C11 C12 -177.9(13) . . . . ? C5 Ir1 C11 C12 -59.8(13) . . . . ? C8 Ir1 C11 C12 145.5(12) . . . . ? C6 Ir1 C11 C12 -95.6(13) . . . . ? C14 Ir1 C11 C12 24.6(13) . . . . ? C10 Ir1 C11 C12 124.7(17) . . . . ? C10 C11 C12 C13 55(3) . . . . ? Ir1 C11 C12 C13 -31(2) . . . . ? C11 C12 C13 C14 18(3) . . . . ? C12 C13 C14 C15 -78(3) . . . . ? C12 C13 C14 Ir1 3(3) . . . . ? C1 Ir1 C14 C15 -82.2(10) . . . . ? C9 Ir1 C14 C15 14(2) . . . . ? C5 Ir1 C14 C15 -157.5(10) . . . . ? C8 Ir1 C14 C15 -4.9(12) . . . . ? C6 Ir1 C14 C15 -169.0(10) . . . . ? C11 Ir1 C14 C15 111.1(10) . . . . ? C10 Ir1 C14 C15 77.8(11) . . . . ? C1 Ir1 C14 C13 151.9(15) . . . . ? C15 Ir1 C14 C13 -126(2) . . . . ? C9 Ir1 C14 C13 -112.3(18) . . . . ? C5 Ir1 C14 C13 76.6(15) . . . . ? C8 Ir1 C14 C13 -130.8(14) . . . . ? C6 Ir1 C14 C13 65.1(16) . . . . ? C11 Ir1 C14 C13 -14.7(14) . . . . ? C10 Ir1 C14 C13 -48.0(15) . . . . ? C13 C14 C15 C16 -6(2) . . . . ? Ir1 C14 C15 C16 -107.2(13) . . . . ? C13 C14 C15 Ir1 101.6(16) . . . . ? C1 Ir1 C15 C14 100.5(10) . . . . ? C9 Ir1 C15 C14 -173.9(10) . . . . ? C5 Ir1 C15 C14 25.0(11) . . . . ? C8 Ir1 C15 C14 175.9(10) . . . . ? C6 Ir1 C15 C14 20.4(18) . . . . ? C11 Ir1 C15 C14 -65.8(10) . . . . ? C10 Ir1 C15 C14 -97.6(11) . . . . ? C1 Ir1 C15 C16 -142.2(13) . . . . ? C9 Ir1 C15 C16 -56.6(14) . . . . ? C5 Ir1 C15 C16 142.2(12) . . . . ? C8 Ir1 C15 C16 -66.9(13) . . . . ? C6 Ir1 C15 C16 137.6(15) . . . . ? C11 Ir1 C15 C16 51.5(13) . . . . ? C14 Ir1 C15 C16 117.3(16) . . . . ? C10 Ir1 C15 C16 19.7(13) . . . . ? C14 C15 C16 C17 59(2) . . . . ? Ir1 C15 C16 C17 -27(2) . . . . ? C15 C16 C17 C10 18(2) . . . . ? C11 C10 C17 C16 -83(2) . . . . ? Ir1 C10 C17 C16 -1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.854 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.854 _refine_diff_density_max 2.075 _refine_diff_density_min -2.127 _refine_diff_density_rms 0.265