data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Maria Garralda' _publ_contact_author_email MARIAANGELES.GARRALDA@EHU.ES _publ_section_title ; Reactivity of hydridoirida-b-diketones with bases: The selective formation of new di-m-acyl-m-hydridodiiridium(III) or dihydridoirida-b-diketone complexes and of heterometallic Ir(III)/Rh(I) derivatives. ; loop_ _publ_author_name 'Maria Garralda' 'Francisco Acha' 'Roberto Ciganda' 'Ricardo Hernandez' 'Lourdes Ibarlucea' 'Elena Pinilla' ; M.R.Torres ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. #============================================================================ data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 679480' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H58 Ir2 O4 P4' _chemical_formula_weight 1543.50 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.462(3) _cell_length_b 13.688(3) _cell_length_c 23.598(5) _cell_angle_alpha 79.179(4) _cell_angle_beta 88.238(4) _cell_angle_gamma 67.565(4) _cell_volume 3357.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.103 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; After repeated attempts, Only polysinthetically twined crystals of poor quality could be obtained. The hydrogen atoms bonded to the Ir atoms could not be located in a difference Fourier synthesis and were not included in the model, however their location is undoubtedly by the NMR data. Also, the high values of residual non-modelled electronic density are due to the bad quality of the crystal. ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 22 _diffrn_reflns_number 27987 _diffrn_reflns_av_R_equivalents 0.2025 _diffrn_reflns_av_sigmaI/netI 0.4137 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.88 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12755 _reflns_number_gt 4375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1534P)^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 12755 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2779 _refine_ls_R_factor_gt 0.1034 _refine_ls_wR_factor_ref 0.3540 _refine_ls_wR_factor_gt 0.2471 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.025 _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 0.56435(10) 0.74027(10) 0.33185(4) 0.0306(4) Uani 1 1 d . . . Ir2 Ir 0.38380(10) 0.87661(10) 0.19276(5) 0.0339(4) Uani 1 1 d . . . P1 P 0.5566(7) 0.8301(6) 0.4071(3) 0.0316(18) Uani 1 1 d . . . P2 P 0.7720(7) 0.6184(6) 0.3314(3) 0.0331(19) Uani 1 1 d . . . P3 P 0.2660(8) 0.7989(7) 0.1535(3) 0.043(2) Uani 1 1 d . . . P4 P 0.2637(7) 1.0606(7) 0.1723(3) 0.036(2) Uani 1 1 d . . . O1 O 0.3092(16) 0.8633(15) 0.2831(7) 0.033(5) Uani 1 1 d . . . O2 O 0.4322(19) 0.6145(18) 0.3992(11) 0.068(7) Uani 1 1 d . . . O3 O 0.560(2) 0.905(2) 0.1055(10) 0.078(8) Uani 1 1 d . . . O4 O 0.5816(16) 0.8804(16) 0.2690(8) 0.040(5) Uani 1 1 d . . . C1 C 0.379(3) 0.830(3) 0.3251(11) 0.042(8) Uani 1 1 d . . . C20 C 0.537(3) 0.619(3) 0.3802(13) 0.057(10) Uani 1 1 d . . . C39 C 0.464(3) 0.875(3) 0.1160(13) 0.056(9) Uani 1 1 d . . . C58 C 0.502(3) 0.927(2) 0.2275(11) 0.035(7) Uani 1 1 d . . . C2 C 0.3147(15) 0.8724(15) 0.3784(6) 0.030(6) Uiso 1 1 d G . . C3 C 0.3892(11) 0.8786(15) 0.4220(7) 0.031(6) Uiso 1 1 d G . . C4 C 0.3332(15) 0.9223(16) 0.4693(6) 0.042(8) Uiso 1 1 d G . . H4 H 0.3830 0.9265 0.4984 0.051 Uiso 1 1 calc R . . C5 C 0.2027(15) 0.9599(15) 0.4731(6) 0.048(8) Uiso 1 1 d G . . H5 H 0.1652 0.9891 0.5048 0.057 Uiso 1 1 calc R . . C6 C 0.1282(11) 0.9537(15) 0.4296(8) 0.042(8) Uiso 1 1 d G . . H6 H 0.0409 0.9788 0.4321 0.051 Uiso 1 1 calc R . . C7 C 0.1842(14) 0.9099(15) 0.3823(6) 0.045(8) Uiso 1 1 d G . . H7 H 0.1344 0.9058 0.3531 0.054 Uiso 1 1 calc R . . C8 C 0.6338(15) 0.7596(14) 0.4794(6) 0.032(7) Uiso 1 1 d G . . C9 C 0.6189(16) 0.6652(15) 0.5050(7) 0.042(8) Uiso 1 1 d G . . H9 H 0.5662 0.6414 0.4872 0.050 Uiso 1 1 calc R . . C10 C 0.6826(18) 0.6065(12) 0.5572(8) 0.046(8) Uiso 1 1 d G . . H10 H 0.6726 0.5434 0.5743 0.055 Uiso 1 1 calc R . . C11 C 0.7612(17) 0.6422(16) 0.5838(6) 0.057(9) Uiso 1 1 d G . . H11 H 0.8038 0.6029 0.6188 0.068 Uiso 1 1 calc R . . C12 C 0.7761(17) 0.7366(17) 0.5583(8) 0.066(10) Uiso 1 1 d G . . H12 H 0.8287 0.7604 0.5761 0.079 Uiso 1 1 calc R . . C13 C 0.7124(17) 0.7953(13) 0.5061(8) 0.042(8) Uiso 1 1 d G . . H13 H 0.7224 0.8585 0.4890 0.050 Uiso 1 1 calc R . . C14 C 0.5939(17) 0.9501(14) 0.3880(8) 0.037(7) Uiso 1 1 d G . . C15 C 0.5038(13) 1.0533(16) 0.3865(9) 0.062(10) Uiso 1 1 d G . . H15 H 0.4203 1.0632 0.3942 0.074 Uiso 1 1 calc R . . C16 C 0.5384(17) 1.1416(12) 0.3736(9) 0.057(9) Uiso 1 1 d G . . H16 H 0.4781 1.2106 0.3726 0.069 Uiso 1 1 calc R . . C17 C 0.6630(19) 1.1268(13) 0.3622(9) 0.062(10) Uiso 1 1 d G . . H17 H 0.6862 1.1859 0.3536 0.074 Uiso 1 1 calc R . . C18 C 0.7532(14) 1.0237(16) 0.3637(8) 0.053(9) Uiso 1 1 d G . . H18 H 0.8366 1.0137 0.3561 0.064 Uiso 1 1 calc R . . C19 C 0.7186(15) 0.9353(12) 0.3766(8) 0.038(7) Uiso 1 1 d G . . H19 H 0.7789 0.8663 0.3776 0.046 Uiso 1 1 calc R . . C21 C 0.6437(14) 0.5097(13) 0.3967(8) 0.043(8) Uiso 1 1 d G . . C22 C 0.7633(17) 0.4991(13) 0.3778(7) 0.034(7) Uiso 1 1 d G . . C23 C 0.8657(13) 0.4025(16) 0.3949(8) 0.047(8) Uiso 1 1 d G . . H23 H 0.9457 0.3954 0.3822 0.056 Uiso 1 1 calc R . . C24 C 0.8486(16) 0.3167(13) 0.4309(9) 0.060(10) Uiso 1 1 d G . . H24 H 0.9171 0.2521 0.4423 0.072 Uiso 1 1 calc R . . C25 C 0.729(2) 0.3274(14) 0.4498(8) 0.075(11) Uiso 1 1 d G . . H25 H 0.7176 0.2699 0.4739 0.090 Uiso 1 1 calc R . . C26 C 0.6266(14) 0.4239(17) 0.4327(8) 0.050(8) Uiso 1 1 d G . . H26 H 0.5466 0.4310 0.4454 0.060 Uiso 1 1 calc R . . C27 C 0.8211(19) 0.5843(18) 0.2620(7) 0.036(7) Uiso 1 1 d G . . C28 C 0.906(2) 0.4836(16) 0.2548(9) 0.085(13) Uiso 1 1 d G . . H28 H 0.9381 0.4284 0.2867 0.102 Uiso 1 1 calc R . . C29 C 0.944(2) 0.4655(16) 0.1999(11) 0.116(17) Uiso 1 1 d G . . H29 H 1.0014 0.3982 0.1951 0.139 Uiso 1 1 calc R . . C30 C 0.897(2) 0.548(2) 0.1522(8) 0.082(12) Uiso 1 1 d G . . H30 H 0.9223 0.5360 0.1154 0.099 Uiso 1 1 calc R . . C31 C 0.812(2) 0.6488(18) 0.1593(7) 0.073(11) Uiso 1 1 d G . . H31 H 0.7800 0.7040 0.1274 0.087 Uiso 1 1 calc R . . C32 C 0.7738(17) 0.6669(14) 0.2142(9) 0.052(9) Uiso 1 1 d G . . H32 H 0.7167 0.7342 0.2190 0.063 Uiso 1 1 calc R . . C33 C 0.9047(15) 0.6365(16) 0.3599(7) 0.037(7) Uiso 1 1 d G . . C34 C 0.9236(16) 0.6172(15) 0.4195(7) 0.036(7) Uiso 1 1 d G . . H34 H 0.8707 0.5927 0.4434 0.043 Uiso 1 1 calc R . . C35 C 1.0217(19) 0.6348(17) 0.4433(6) 0.060(10) Uiso 1 1 d G . . H35 H 1.0344 0.6219 0.4832 0.072 Uiso 1 1 calc R . . C36 C 1.1009(16) 0.6715(18) 0.4075(9) 0.072(11) Uiso 1 1 d G . . H36 H 1.1665 0.6832 0.4234 0.087 Uiso 1 1 calc R . . C37 C 1.0820(18) 0.6907(18) 0.3479(8) 0.068(10) Uiso 1 1 d G . . H37 H 1.1349 0.7153 0.3239 0.081 Uiso 1 1 calc R . . C38 C 0.9839(19) 0.6732(17) 0.3241(6) 0.055(9) Uiso 1 1 d G . . H38 H 0.9712 0.6861 0.2842 0.066 Uiso 1 1 calc R . . C40 C 0.4226(19) 0.8343(17) 0.0720(8) 0.047(8) Uiso 1 1 d G . . C41 C 0.3274(18) 0.7945(17) 0.0823(7) 0.040(7) Uiso 1 1 d G . . C42 C 0.2848(18) 0.7589(18) 0.0388(10) 0.077(12) Uiso 1 1 d G . . H42 H 0.2211 0.7323 0.0457 0.093 Uiso 1 1 calc R . . C43 C 0.337(2) 0.763(2) -0.0150(9) 0.096(14) Uiso 1 1 d G . . H43 H 0.3089 0.7391 -0.0441 0.115 Uiso 1 1 calc R . . C44 C 0.433(2) 0.803(2) -0.0253(7) 0.084(12) Uiso 1 1 d G . . H44 H 0.4678 0.8054 -0.0613 0.100 Uiso 1 1 calc R . . C45 C 0.4752(18) 0.8383(18) 0.0182(9) 0.073(11) Uiso 1 1 d G . . H45 H 0.5389 0.8649 0.0113 0.087 Uiso 1 1 calc R . . C46 C 0.0951(14) 0.8668(16) 0.1403(9) 0.042(8) Uiso 1 1 d G . . C47 C 0.014(2) 0.8427(16) 0.1804(8) 0.061(10) Uiso 1 1 d G . . H47 H 0.0464 0.7902 0.2134 0.073 Uiso 1 1 calc R . . C48 C -0.1160(19) 0.8970(19) 0.1711(9) 0.084(12) Uiso 1 1 d G . . H48 H -0.1704 0.8809 0.1979 0.101 Uiso 1 1 calc R . . C49 C -0.1647(15) 0.9754(18) 0.1218(10) 0.069(11) Uiso 1 1 d G . . H49 H -0.2517 1.0118 0.1156 0.083 Uiso 1 1 calc R . . C50 C -0.084(2) 0.9995(16) 0.0817(8) 0.089(13) Uiso 1 1 d G . . H50 H -0.1161 1.0520 0.0487 0.107 Uiso 1 1 calc R . . C51 C 0.0464(19) 0.9452(17) 0.0910(8) 0.055(9) Uiso 1 1 d G . . H51 H 0.1008 0.9613 0.0642 0.067 Uiso 1 1 calc R . . C52 C 0.284(2) 0.6625(16) 0.1882(10) 0.055(9) Uiso 1 1 d G . . C53 C 0.355(2) 0.6165(19) 0.2400(10) 0.065(10) Uiso 1 1 d G . . H53 H 0.3979 0.6526 0.2545 0.078 Uiso 1 1 calc R . . C54 C 0.362(2) 0.517(2) 0.2699(8) 0.089(13) Uiso 1 1 d G . . H54 H 0.4094 0.4860 0.3045 0.106 Uiso 1 1 calc R . . C55 C 0.298(3) 0.4628(16) 0.2481(11) 0.090(13) Uiso 1 1 d G . . H55 H 0.3021 0.3960 0.2682 0.108 Uiso 1 1 calc R . . C56 C 0.226(2) 0.509(2) 0.1964(12) 0.099(14) Uiso 1 1 d G . . H56 H 0.1834 0.4726 0.1818 0.118 Uiso 1 1 calc R . . C57 C 0.220(2) 0.609(2) 0.1664(9) 0.130(19) Uiso 1 1 d G . . H57 H 0.1720 0.6393 0.1318 0.156 Uiso 1 1 calc R . . C59 C 0.4951(17) 1.0409(12) 0.2081(8) 0.046(8) Uiso 1 1 d G . . C60 C 0.3833(15) 1.1147(16) 0.1794(8) 0.031(6) Uiso 1 1 d G . . C61 C 0.3681(15) 1.2215(14) 0.1608(8) 0.055(9) Uiso 1 1 d G . . H61 H 0.2932 1.2709 0.1416 0.067 Uiso 1 1 calc R . . C62 C 0.4648(19) 1.2546(12) 0.1710(9) 0.062(10) Uiso 1 1 d G . . H62 H 0.4546 1.3261 0.1586 0.074 Uiso 1 1 calc R . . C63 C 0.5767(16) 1.1808(16) 0.1998(9) 0.060(10) Uiso 1 1 d G . . H63 H 0.6414 1.2030 0.2066 0.072 Uiso 1 1 calc R . . C64 C 0.5918(14) 1.0739(15) 0.2183(8) 0.039(7) Uiso 1 1 d G . . H64 H 0.6667 1.0246 0.2375 0.047 Uiso 1 1 calc R . . C65 C 0.1811(18) 1.1392(16) 0.1019(6) 0.034(7) Uiso 1 1 d G . . C66 C 0.2486(15) 1.1132(16) 0.0533(9) 0.069(11) Uiso 1 1 d G . . H66 H 0.3317 1.0634 0.0574 0.083 Uiso 1 1 calc R . . C67 C 0.192(2) 1.1615(18) -0.0015(7) 0.063(10) Uiso 1 1 d G . . H67 H 0.2374 1.1441 -0.0341 0.075 Uiso 1 1 calc R . . C68 C 0.068(2) 1.2359(18) -0.0077(7) 0.069(10) Uiso 1 1 d G . . H68 H 0.0303 1.2682 -0.0443 0.082 Uiso 1 1 calc R . . C69 C 0.0005(15) 1.2619(16) 0.0409(9) 0.075(11) Uiso 1 1 d G . . H69 H -0.0825 1.3117 0.0368 0.090 Uiso 1 1 calc R . . C70 C 0.0570(17) 1.2136(17) 0.0957(7) 0.060(9) Uiso 1 1 d G . . H70 H 0.0118 1.2310 0.1283 0.072 Uiso 1 1 calc R . . C71 C 0.1498(17) 1.1092(17) 0.2255(8) 0.054(9) Uiso 1 1 d G . . C72 C 0.1692(16) 1.1633(18) 0.2662(9) 0.062(10) Uiso 1 1 d G . . H72 H 0.2434 1.1759 0.2669 0.075 Uiso 1 1 calc R . . C73 C 0.078(2) 1.1988(17) 0.3059(8) 0.071(11) Uiso 1 1 d G . . H73 H 0.0909 1.2351 0.3332 0.086 Uiso 1 1 calc R . . C74 C -0.0329(18) 1.1801(18) 0.3049(8) 0.070(11) Uiso 1 1 d G . . H74 H -0.0941 1.2039 0.3314 0.084 Uiso 1 1 calc R . . C75 C -0.0524(15) 1.1259(18) 0.2641(9) 0.063(10) Uiso 1 1 d G . . H75 H -0.1265 1.1134 0.2634 0.075 Uiso 1 1 calc R . . C76 C 0.0390(19) 1.0905(16) 0.2244(8) 0.053(9) Uiso 1 1 d G . . H76 H 0.0259 1.0542 0.1971 0.064 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 0.0331(7) 0.0405(9) 0.0255(6) -0.0085(6) 0.0103(5) -0.0215(6) Ir2 0.0346(7) 0.0404(9) 0.0305(7) -0.0062(6) 0.0101(5) -0.0193(6) P1 0.034(4) 0.042(5) 0.028(4) -0.008(4) 0.006(3) -0.024(4) P2 0.036(4) 0.039(5) 0.028(4) -0.010(4) 0.013(3) -0.018(4) P3 0.051(5) 0.048(6) 0.037(5) -0.013(4) 0.012(4) -0.024(5) P4 0.035(4) 0.042(6) 0.033(4) -0.005(4) 0.011(3) -0.019(4) O1 0.042(11) 0.053(14) 0.015(9) -0.014(9) 0.009(8) -0.027(11) O2 0.046(13) 0.058(17) 0.11(2) -0.003(14) 0.027(13) -0.040(13) O3 0.089(18) 0.13(2) 0.066(16) -0.049(16) 0.052(14) -0.081(18) O4 0.027(10) 0.061(16) 0.033(11) -0.006(11) 0.010(9) -0.020(10) C1 0.06(2) 0.08(3) 0.014(14) -0.004(15) 0.010(14) -0.055(19) C20 0.07(2) 0.06(3) 0.05(2) -0.023(18) -0.018(18) -0.03(2) C39 0.06(2) 0.06(3) 0.04(2) -0.011(18) -0.001(17) -0.03(2) C58 0.037(17) 0.04(2) 0.017(14) 0.013(13) -0.002(12) -0.010(15) _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 C20 1.96(3) . ? Ir1 C1 2.00(3) . ? Ir1 O4 2.263(18) . ? Ir1 P1 2.324(7) . ? Ir1 P2 2.329(7) . ? Ir2 C39 2.01(3) . ? Ir2 C58 2.00(3) . ? Ir2 O1 2.273(15) . ? Ir2 P3 2.314(8) . ? Ir2 P4 2.326(8) . ? P1 C3 1.822(13) . ? P1 C14 1.825(15) . ? P1 C8 1.857(15) . ? P2 C27 1.803(17) . ? P2 C33 1.800(15) . ? P2 C22 1.823(16) . ? P3 C41 1.804(17) . ? P3 C46 1.826(17) . ? P3 C52 1.83(2) . ? P4 C71 1.809(16) . ? P4 C60 1.813(15) . ? P4 C65 1.861(16) . ? O1 C1 1.20(3) . ? O2 C20 1.29(4) . ? O3 C39 1.31(4) . ? O4 C58 1.25(3) . ? C1 C2 1.54(3) . ? C20 C21 1.51(4) . ? C39 C40 1.43(3) . ? C58 C59 1.51(3) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 C6 1.3900 . ? C5 H5 0.9300 . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 C11 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 C17 1.3900 . ? C16 H16 0.9300 . ? C17 C18 1.3900 . ? C17 H17 0.9300 . ? C18 C19 1.3900 . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C23 H23 0.9300 . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28 0.9300 . ? C29 C30 1.3900 . ? C29 H29 0.9300 . ? C30 C31 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34 0.9300 . ? C35 C36 1.3900 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3900 . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C40 C41 1.3900 . ? C40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C42 H42 0.9300 . ? C43 C44 1.3900 . ? C43 H43 0.9300 . ? C44 C45 1.3900 . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.3900 . ? C46 C51 1.3900 . ? C47 C48 1.3900 . ? C47 H47 0.9300 . ? C48 C49 1.3900 . ? C48 H48 0.9300 . ? C49 C50 1.3900 . ? C49 H49 0.9300 . ? C50 C51 1.3900 . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.3900 . ? C52 C57 1.3900 . ? C53 C54 1.3900 . ? C53 H53 0.9300 . ? C54 C55 1.3900 . ? C54 H54 0.9300 . ? C55 C56 1.3900 . ? C55 H55 0.9300 . ? C56 C57 1.3900 . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C59 C60 1.3900 . ? C59 C64 1.3900 . ? C60 C61 1.3900 . ? C61 C62 1.3900 . ? C61 H61 0.9300 . ? C62 C63 1.3900 . ? C62 H62 0.9300 . ? C63 C64 1.3900 . ? C63 H63 0.9300 . ? C64 H64 0.9300 . ? C65 C66 1.3900 . ? C65 C70 1.3900 . ? C66 C67 1.3900 . ? C66 H66 0.9300 . ? C67 C68 1.3900 . ? C67 H67 0.9300 . ? C68 C69 1.3900 . ? C68 H68 0.9300 . ? C69 C70 1.3900 . ? C69 H69 0.9300 . ? C70 H70 0.9300 . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C72 H72 0.9300 . ? C73 C74 1.3900 . ? C73 H73 0.9300 . ? C74 C75 1.3900 . ? C74 H74 0.9300 . ? C75 C76 1.3900 . ? C75 H75 0.9300 . ? C76 H76 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Ir1 C1 91.7(13) . . ? C20 Ir1 O4 173.9(10) . . ? C1 Ir1 O4 84.9(9) . . ? C20 Ir1 P1 95.0(9) . . ? C1 Ir1 P1 82.2(8) . . ? O4 Ir1 P1 89.5(5) . . ? C20 Ir1 P2 84.5(10) . . ? C1 Ir1 P2 170.7(8) . . ? O4 Ir1 P2 98.1(5) . . ? P1 Ir1 P2 106.5(3) . . ? C39 Ir2 C58 94.5(12) . . ? C39 Ir2 O1 174.3(11) . . ? C58 Ir2 O1 84.2(8) . . ? C39 Ir2 P3 83.6(10) . . ? C58 Ir2 P3 173.2(9) . . ? O1 Ir2 P3 97.0(5) . . ? C39 Ir2 P4 94.3(10) . . ? C58 Ir2 P4 81.6(8) . . ? O1 Ir2 P4 91.0(5) . . ? P3 Ir2 P4 105.0(3) . . ? C3 P1 C14 105.7(9) . . ? C3 P1 C8 102.8(8) . . ? C14 P1 C8 106.4(9) . . ? C3 P1 Ir1 102.0(6) . . ? C14 P1 Ir1 115.1(7) . . ? C8 P1 Ir1 122.7(7) . . ? C27 P2 C33 103.9(9) . . ? C27 P2 C22 107.6(10) . . ? C33 P2 C22 105.7(9) . . ? C27 P2 Ir1 114.6(8) . . ? C33 P2 Ir1 123.2(7) . . ? C22 P2 Ir1 100.8(6) . . ? C41 P3 C46 104.3(10) . . ? C41 P3 C52 108.3(11) . . ? C46 P3 C52 102.5(11) . . ? C41 P3 Ir2 101.2(7) . . ? C46 P3 Ir2 121.9(8) . . ? C52 P3 Ir2 117.5(9) . . ? C71 P4 C60 105.4(10) . . ? C71 P4 C65 104.3(10) . . ? C60 P4 C65 102.9(9) . . ? C71 P4 Ir2 114.7(8) . . ? C60 P4 Ir2 101.1(7) . . ? C65 P4 Ir2 126.0(7) . . ? C1 O1 Ir2 121.4(16) . . ? C58 O4 Ir1 119.2(17) . . ? O1 C1 C2 113(3) . . ? O1 C1 Ir1 129(2) . . ? C2 C1 Ir1 118.2(17) . . ? O2 C20 C21 110(3) . . ? O2 C20 Ir1 128(3) . . ? C21 C20 Ir1 121(2) . . ? O3 C39 C40 118(3) . . ? O3 C39 Ir2 121(2) . . ? C40 C39 Ir2 120(2) . . ? O4 C58 C59 109(2) . . ? O4 C58 Ir2 130(2) . . ? C59 C58 Ir2 120.4(17) . . ? C3 C2 C7 120.0 . . ? C3 C2 C1 118.6(15) . . ? C7 C2 C1 121.3(15) . . ? C4 C3 C2 120.0 . . ? C4 C3 P1 127.0(10) . . ? C2 C3 P1 112.9(10) . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C7 C6 C5 120.0 . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.0 . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 P1 118.6(10) . . ? C13 C8 P1 121.3(10) . . ? C8 C9 C10 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C8 120.0 . . ? C12 C13 H13 120.0 . . ? C8 C13 H13 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 P1 122.4(11) . . ? C19 C14 P1 117.5(11) . . ? C16 C15 C14 120.0 . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C18 120.0 . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 120.0 . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C14 120.0 . . ? C18 C19 H19 120.0 . . ? C14 C19 H19 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 C20 117.9(18) . . ? C26 C21 C20 122.0(18) . . ? C21 C22 C23 120.0 . . ? C21 C22 P2 115.3(11) . . ? C23 C22 P2 124.7(11) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C25 C24 C23 120.0 . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C28 C27 C32 120.0 . . ? C28 C27 P2 123.6(14) . . ? C32 C27 P2 116.3(14) . . ? C27 C28 C29 120.0 . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.0 . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.0 . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C34 C33 C38 120.0 . . ? C34 C33 P2 118.1(11) . . ? C38 C33 P2 121.8(11) . . ? C33 C34 C35 120.0 . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36 120.0 . . ? C37 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C41 C40 C45 120.0 . . ? C41 C40 C39 120.4(19) . . ? C45 C40 C39 119.6(19) . . ? C40 C41 C42 120.0 . . ? C40 C41 P3 114.4(13) . . ? C42 C41 P3 125.6(13) . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C40 120.0 . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C47 C46 C51 120.0 . . ? C47 C46 P3 120.2(12) . . ? C51 C46 P3 119.8(12) . . ? C46 C47 C48 120.0 . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C50 C49 C48 120.0 . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C46 120.0 . . ? C50 C51 H51 120.0 . . ? C46 C51 H51 120.0 . . ? C53 C52 C57 120.0 . . ? C53 C52 P3 118.5(16) . . ? C57 C52 P3 121.3(16) . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.0 . . ? C55 C56 H56 120.0 . . ? C57 C56 H56 120.0 . . ? C56 C57 C52 120.0 . . ? C56 C57 H57 120.0 . . ? C52 C57 H57 120.0 . . ? C60 C59 C64 120.0 . . ? C60 C59 C58 116.4(16) . . ? C64 C59 C58 123.6(16) . . ? C59 C60 C61 120.0 . . ? C59 C60 P4 114.7(11) . . ? C61 C60 P4 125.2(12) . . ? C62 C61 C60 120.0 . . ? C62 C61 H61 120.0 . . ? C60 C61 H61 120.0 . . ? C61 C62 C63 120.0 . . ? C61 C62 H62 120.0 . . ? C63 C62 H62 120.0 . . ? C62 C63 C64 120.0 . . ? C62 C63 H63 120.0 . . ? C64 C63 H63 120.0 . . ? C63 C64 C59 120.0 . . ? C63 C64 H64 120.0 . . ? C59 C64 H64 120.0 . . ? C66 C65 C70 120.0 . . ? C66 C65 P4 115.4(12) . . ? C70 C65 P4 124.4(12) . . ? C65 C66 C67 120.0 . . ? C65 C66 H66 120.0 . . ? C67 C66 H66 120.0 . . ? C68 C67 C66 120.0 . . ? C68 C67 H67 120.0 . . ? C66 C67 H67 120.0 . . ? C67 C68 C69 120.0 . . ? C67 C68 H68 120.0 . . ? C69 C68 H68 120.0 . . ? C70 C69 C68 120.0 . . ? C70 C69 H69 120.0 . . ? C68 C69 H69 120.0 . . ? C69 C70 C65 120.0 . . ? C69 C70 H70 120.0 . . ? C65 C70 H70 120.0 . . ? C72 C71 C76 120.0 . . ? C72 C71 P4 122.7(12) . . ? C76 C71 P4 117.3(12) . . ? C71 C72 C73 120.0 . . ? C71 C72 H72 120.0 . . ? C73 C72 H72 120.0 . . ? C74 C73 C72 120.0 . . ? C74 C73 H73 120.0 . . ? C72 C73 H73 120.0 . . ? C75 C74 C73 120.0 . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.0 . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? C75 C76 C71 120.0 . . ? C75 C76 H76 120.0 . . ? C71 C76 H76 120.0 . . ? 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 C20 Ir1 P1 C3 -72.3(12) . . . . ? C1 Ir1 P1 C3 18.7(10) . . . . ? O4 Ir1 P1 C3 103.7(8) . . . . ? P2 Ir1 P1 C3 -157.9(7) . . . . ? C20 Ir1 P1 C14 173.9(12) . . . . ? C1 Ir1 P1 C14 -95.1(10) . . . . ? O4 Ir1 P1 C14 -10.1(9) . . . . ? P2 Ir1 P1 C14 88.2(8) . . . . ? C20 Ir1 P1 C8 41.7(12) . . . . ? C1 Ir1 P1 C8 132.7(10) . . . . ? O4 Ir1 P1 C8 -142.3(8) . . . . ? P2 Ir1 P1 C8 -44.0(7) . . . . ? C20 Ir1 P2 C27 113.3(12) . . . . ? C1 Ir1 P2 C27 48(5) . . . . ? O4 Ir1 P2 C27 -61.2(9) . . . . ? P1 Ir1 P2 C27 -153.1(8) . . . . ? C20 Ir1 P2 C33 -118.8(11) . . . . ? C1 Ir1 P2 C33 175(5) . . . . ? O4 Ir1 P2 C33 66.7(9) . . . . ? P1 Ir1 P2 C33 -25.2(8) . . . . ? C20 Ir1 P2 C22 -1.9(11) . . . . ? C1 Ir1 P2 C22 -68(5) . . . . ? O4 Ir1 P2 C22 -176.3(8) . . . . ? P1 Ir1 P2 C22 91.7(7) . . . . ? C39 Ir2 P3 C41 -1.1(12) . . . . ? C58 Ir2 P3 C41 -75(6) . . . . ? O1 Ir2 P3 C41 -175.4(9) . . . . ? P4 Ir2 P3 C41 91.7(8) . . . . ? C39 Ir2 P3 C46 -115.8(13) . . . . ? C58 Ir2 P3 C46 170(6) . . . . ? O1 Ir2 P3 C46 69.9(10) . . . . ? P4 Ir2 P3 C46 -23.0(9) . . . . ? C39 Ir2 P3 C52 116.6(13) . . . . ? C58 Ir2 P3 C52 42(6) . . . . ? O1 Ir2 P3 C52 -57.7(10) . . . . ? P4 Ir2 P3 C52 -150.6(9) . . . . ? C39 Ir2 P4 C71 172.1(12) . . . . ? C58 Ir2 P4 C71 -94.0(11) . . . . ? O1 Ir2 P4 C71 -9.9(9) . . . . ? P3 Ir2 P4 C71 87.6(8) . . . . ? C39 Ir2 P4 C60 -75.1(12) . . . . ? C58 Ir2 P4 C60 18.8(10) . . . . ? O1 Ir2 P4 C60 102.9(8) . . . . ? P3 Ir2 P4 C60 -159.6(7) . . . . ? C39 Ir2 P4 C65 40.0(12) . . . . ? C58 Ir2 P4 C65 133.9(11) . . . . ? O1 Ir2 P4 C65 -142.0(9) . . . . ? P3 Ir2 P4 C65 -44.5(8) . . . . ? C39 Ir2 O1 C1 38(11) . . . . ? C58 Ir2 O1 C1 -40(2) . . . . ? P3 Ir2 O1 C1 133(2) . . . . ? P4 Ir2 O1 C1 -122(2) . . . . ? C20 Ir1 O4 C58 15(11) . . . . ? C1 Ir1 O4 C58 -41(2) . . . . ? P1 Ir1 O4 C58 -123(2) . . . . ? P2 Ir1 O4 C58 130.0(19) . . . . ? Ir2 O1 C1 C2 154.1(14) . . . . ? Ir2 O1 C1 Ir1 -20(4) . . . . ? C20 Ir1 C1 O1 -115(3) . . . . ? O4 Ir1 C1 O1 60(3) . . . . ? P1 Ir1 C1 O1 151(3) . . . . ? P2 Ir1 C1 O1 -49(6) . . . . ? C20 Ir1 C1 C2 72(2) . . . . ? O4 Ir1 C1 C2 -113.2(19) . . . . ? P1 Ir1 C1 C2 -23.0(17) . . . . ? P2 Ir1 C1 C2 137(4) . . . . ? C1 Ir1 C20 O2 -3(3) . . . . ? O4 Ir1 C20 O2 -59(12) . . . . ? P1 Ir1 C20 O2 79(3) . . . . ? P2 Ir1 C20 O2 -175(3) . . . . ? C1 Ir1 C20 C21 172(2) . . . . ? O4 Ir1 C20 C21 116(10) . . . . ? P1 Ir1 C20 C21 -106(2) . . . . ? P2 Ir1 C20 C21 0.5(19) . . . . ? C58 Ir2 C39 O3 -2(3) . . . . ? O1 Ir2 C39 O3 -79(12) . . . . ? P3 Ir2 C39 O3 -175(3) . . . . ? P4 Ir2 C39 O3 80(3) . . . . ? C58 Ir2 C39 C40 175(2) . . . . ? O1 Ir2 C39 C40 97(10) . . . . ? P3 Ir2 C39 C40 1(2) . . . . ? P4 Ir2 C39 C40 -103(2) . . . . ? Ir1 O4 C58 C59 155.3(14) . . . . ? Ir1 O4 C58 Ir2 -18(3) . . . . ? C39 Ir2 C58 O4 -116(3) . . . . ? O1 Ir2 C58 O4 59(2) . . . . ? P3 Ir2 C58 O4 -42(8) . . . . ? P4 Ir2 C58 O4 150(3) . . . . ? C39 Ir2 C58 C59 71(2) . . . . ? O1 Ir2 C58 C59 -114.5(19) . . . . ? P3 Ir2 C58 C59 145(5) . . . . ? P4 Ir2 C58 C59 -22.6(17) . . . . ? O1 C1 C2 C3 -153.9(18) . . . . ? Ir1 C1 C2 C3 21(2) . . . . ? O1 C1 C2 C7 23(3) . . . . ? Ir1 C1 C2 C7 -162.9(11) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 176(2) . . . . ? C7 C2 C3 P1 -177.7(13) . . . . ? C1 C2 C3 P1 -1.2(18) . . . . ? C14 P1 C3 C4 -71.1(13) . . . . ? C8 P1 C3 C4 40.3(13) . . . . ? Ir1 P1 C3 C4 168.3(10) . . . . ? C14 P1 C3 C2 106.4(11) . . . . ? C8 P1 C3 C2 -142.2(10) . . . . ? Ir1 P1 C3 C2 -14.2(10) . . . . ? C2 C3 C4 C5 0.0 . . . . ? P1 C3 C4 C5 177.3(15) . . . . ? C3 C4 C5 C6 0.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? C5 C6 C7 C2 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 -176(2) . . . . ? C3 P1 C8 C9 68.2(11) . . . . ? C14 P1 C8 C9 179.0(10) . . . . ? Ir1 P1 C8 C9 -45.4(11) . . . . ? C3 P1 C8 C13 -116.4(11) . . . . ? C14 P1 C8 C13 -5.6(13) . . . . ? Ir1 P1 C8 C13 130.0(9) . . . . ? C13 C8 C9 C10 0.0 . . . . ? P1 C8 C9 C10 175.4(13) . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C8 0.0 . . . . ? C9 C8 C13 C12 0.0 . . . . ? P1 C8 C13 C12 -175.3(13) . . . . ? C3 P1 C14 C15 -0.2(13) . . . . ? C8 P1 C14 C15 -109.1(11) . . . . ? Ir1 P1 C14 C15 111.5(10) . . . . ? C3 P1 C14 C19 177.7(10) . . . . ? C8 P1 C14 C19 68.8(12) . . . . ? Ir1 P1 C14 C19 -70.6(11) . . . . ? C19 C14 C15 C16 0.0 . . . . ? P1 C14 C15 C16 177.8(15) . . . . ? C14 C15 C16 C17 0.0 . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C14 0.0 . . . . ? C15 C14 C19 C18 0.0 . . . . ? P1 C14 C19 C18 -177.9(14) . . . . ? O2 C20 C21 C22 177.8(19) . . . . ? Ir1 C20 C21 C22 2(3) . . . . ? O2 C20 C21 C26 -6(3) . . . . ? Ir1 C20 C21 C26 177.6(13) . . . . ? C26 C21 C22 C23 0.0 . . . . ? C20 C21 C22 C23 176(2) . . . . ? C26 C21 C22 P2 -179.5(14) . . . . ? C20 C21 C22 P2 -3.5(18) . . . . ? C27 P2 C22 C21 -117.0(11) . . . . ? C33 P2 C22 C21 132.6(11) . . . . ? Ir1 P2 C22 C21 3.4(10) . . . . ? C27 P2 C22 C23 63.6(14) . . . . ? C33 P2 C22 C23 -46.9(14) . . . . ? Ir1 P2 C22 C23 -176.1(10) . . . . ? C21 C22 C23 C24 0.0 . . . . ? P2 C22 C23 C24 179.4(15) . . . . ? C22 C23 C24 C25 0.0 . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C21 0.0 . . . . ? C22 C21 C26 C25 0.0 . . . . ? C20 C21 C26 C25 -176(2) . . . . ? C33 P2 C27 C28 76.1(14) . . . . ? C22 P2 C27 C28 -35.6(15) . . . . ? Ir1 P2 C27 C28 -146.8(11) . . . . ? C33 P2 C27 C32 -100.7(13) . . . . ? C22 P2 C27 C32 147.6(12) . . . . ? Ir1 P2 C27 C32 36.4(13) . . . . ? C32 C27 C28 C29 0.0 . . . . ? P2 C27 C28 C29 -176.7(16) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? P2 C27 C32 C31 176.9(15) . . . . ? C27 P2 C33 C34 -152.4(12) . . . . ? C22 P2 C33 C34 -39.3(13) . . . . ? Ir1 P2 C33 C34 75.2(12) . . . . ? C27 P2 C33 C38 30.4(14) . . . . ? C22 P2 C33 C38 143.5(12) . . . . ? Ir1 P2 C33 C38 -101.9(11) . . . . ? C38 C33 C34 C35 0.0 . . . . ? P2 C33 C34 C35 -177.2(15) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C33 0.0 . . . . ? C34 C33 C38 C37 0.0 . . . . ? P2 C33 C38 C37 177.1(15) . . . . ? O3 C39 C40 C41 176(2) . . . . ? Ir2 C39 C40 C41 -1(3) . . . . ? O3 C39 C40 C45 -7(4) . . . . ? Ir2 C39 C40 C45 176.9(14) . . . . ? C45 C40 C41 C42 0.0 . . . . ? C39 C40 C41 C42 178(2) . . . . ? C45 C40 C41 P3 -178.1(15) . . . . ? C39 C40 C41 P3 0(2) . . . . ? C46 P3 C41 C40 128.3(12) . . . . ? C52 P3 C41 C40 -123.1(13) . . . . ? Ir2 P3 C41 C40 1.0(12) . . . . ? C46 P3 C41 C42 -49.7(15) . . . . ? C52 P3 C41 C42 58.9(16) . . . . ? Ir2 P3 C41 C42 -177.0(11) . . . . ? C40 C41 C42 C43 0.0 . . . . ? P3 C41 C42 C43 177.8(17) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C40 0.0 . . . . ? C41 C40 C45 C44 0.0 . . . . ? C39 C40 C45 C44 -178(2) . . . . ? C41 P3 C46 C47 149.9(13) . . . . ? C52 P3 C46 C47 37.1(15) . . . . ? Ir2 P3 C46 C47 -96.9(12) . . . . ? C41 P3 C46 C51 -32.2(15) . . . . ? C52 P3 C46 C51 -145.1(13) . . . . ? Ir2 P3 C46 C51 81.0(13) . . . . ? C51 C46 C47 C48 0.0 . . . . ? P3 C46 C47 C48 177.9(15) . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C46 0.0 . . . . ? C47 C46 C51 C50 0.0 . . . . ? P3 C46 C51 C50 -177.9(15) . . . . ? C41 P3 C52 C53 121.1(14) . . . . ? C46 P3 C52 C53 -129.0(14) . . . . ? Ir2 P3 C52 C53 7.4(16) . . . . ? C41 P3 C52 C57 -64.3(15) . . . . ? C46 P3 C52 C57 45.6(14) . . . . ? Ir2 P3 C52 C57 -178.0(10) . . . . ? C57 C52 C53 C54 0.0 . . . . ? P3 C52 C53 C54 174.7(17) . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C52 0.0 . . . . ? C53 C52 C57 C56 0.0 . . . . ? P3 C52 C57 C56 -174.5(17) . . . . ? O4 C58 C59 C60 -156.0(16) . . . . ? Ir2 C58 C59 C60 18(2) . . . . ? O4 C58 C59 C64 23(3) . . . . ? Ir2 C58 C59 C64 -162.6(12) . . . . ? C64 C59 C60 C61 0.0 . . . . ? C58 C59 C60 C61 179.0(19) . . . . ? C64 C59 C60 P4 -177.3(13) . . . . ? C58 C59 C60 P4 1.7(17) . . . . ? C71 P4 C60 C59 103.6(11) . . . . ? C65 P4 C60 C59 -147.3(10) . . . . ? Ir2 P4 C60 C59 -16.1(10) . . . . ? C71 P4 C60 C61 -73.5(14) . . . . ? C65 P4 C60 C61 35.5(14) . . . . ? Ir2 P4 C60 C61 166.8(10) . . . . ? C59 C60 C61 C62 0.0 . . . . ? P4 C60 C61 C62 177.0(15) . . . . ? C60 C61 C62 C63 0.0 . . . . ? C61 C62 C63 C64 0.0 . . . . ? C62 C63 C64 C59 0.0 . . . . ? C60 C59 C64 C63 0.0 . . . . ? C58 C59 C64 C63 -179(2) . . . . ? C71 P4 C65 C66 -177.6(11) . . . . ? C60 P4 C65 C66 72.5(12) . . . . ? Ir2 P4 C65 C66 -41.7(13) . . . . ? C71 P4 C65 C70 -2.5(15) . . . . ? C60 P4 C65 C70 -112.4(13) . . . . ? Ir2 P4 C65 C70 133.4(11) . . . . ? C70 C65 C66 C67 0.0 . . . . ? P4 C65 C66 C67 175.3(14) . . . . ? C65 C66 C67 C68 0.0 . . . . ? C66 C67 C68 C69 0.0 . . . . ? C67 C68 C69 C70 0.0 . . . . ? C68 C69 C70 C65 0.0 . . . . ? C66 C65 C70 C69 0.0 . . . . ? P4 C65 C70 C69 -174.9(15) . . . . ? C60 P4 C71 C72 -7.8(15) . . . . ? C65 P4 C71 C72 -115.8(13) . . . . ? Ir2 P4 C71 C72 102.5(11) . . . . ? C60 P4 C71 C76 172.1(11) . . . . ? C65 P4 C71 C76 64.1(13) . . . . ? Ir2 P4 C71 C76 -77.6(12) . . . . ? C76 C71 C72 C73 0.0 . . . . ? P4 C71 C72 C73 179.9(16) . . . . ? C71 C72 C73 C74 0.0 . . . . ? C72 C73 C74 C75 0.0 . . . . ? C73 C74 C75 C76 0.0 . . . . ? C74 C75 C76 C71 0.0 . . . . ? C72 C71 C76 C75 0.0 . . . . ? P4 C71 C76 C75 -179.9(15) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 5.218 _refine_diff_density_min -3.532 _refine_diff_density_rms 0.339 #============================================================================ data_[8]ClO4 _database_code_depnum_ccdc_archive 'CCDC 679481' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H57 Ir2 O4 P4, Cl O4, C H Cl3' _chemical_formula_sum 'C77 H58 Cl4 Ir2 O8 P4' _chemical_formula_weight 1761.31 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' O O 0.0106 0.0060 '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 12.3375(8) _cell_length_b 15.6694(10) _cell_length_c 18.6401(12) _cell_angle_alpha 92.2000(10) _cell_angle_beta 103.9520(10) _cell_angle_gamma 96.6120(10) _cell_volume 3465.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1732 _exptl_absorpt_coefficient_mu 4.140 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26717 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11888 _reflns_number_gt 8363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0541P)^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 11888 _refine_ls_number_parameters 836 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.041 _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 0.87483(2) 0.701131(18) 0.695045(16) 0.02763(10) Uani 1 1 d . . . Ir2 Ir 0.90799(2) 0.889279(18) 0.732821(16) 0.02722(10) Uani 1 1 d . . . H1 H 0.9651 0.7946 0.7373 0.050 Uiso 1 1 d . . . C1 C 0.8013(6) 0.7668(5) 0.6091(4) 0.0324(18) Uani 1 1 d . . . O1 O 0.8176(4) 0.8483(3) 0.6134(3) 0.0323(12) Uani 1 1 d . . . P1 P 0.73409(17) 0.59588(13) 0.63402(12) 0.0336(5) Uani 1 1 d . . . C2 C 0.7294(6) 0.7231(5) 0.5399(5) 0.0358(19) Uani 1 1 d . . . O2 O 0.9747(5) 0.6698(4) 0.5713(3) 0.0454(15) Uani 1 1 d . . . P2 P 0.98351(17) 0.63245(13) 0.79247(12) 0.0333(5) Uani 1 1 d . . . C3 C 0.6955(6) 0.6339(5) 0.5434(5) 0.040(2) Uani 1 1 d . . . O3 O 0.9496(5) 0.8649(4) 0.8884(3) 0.0566(17) Uani 1 1 d . . . P3 P 1.07952(16) 0.96776(13) 0.71936(11) 0.0308(5) Uani 1 1 d . . . C4 C 0.6315(7) 0.5881(6) 0.4781(5) 0.047(2) Uani 1 1 d . . . H4A H 0.6089 0.5295 0.4789 0.056 Uiso 1 1 calc R . . O4 O 0.7606(4) 0.7437(3) 0.7579(3) 0.0387(14) Uani 1 1 d . . . P4 P 0.80961(17) 1.00293(13) 0.74498(12) 0.0318(5) Uani 1 1 d . . . C5 C 0.6018(8) 0.6265(7) 0.4140(5) 0.058(3) Uani 1 1 d . . . H5A H 0.5605 0.5941 0.3713 0.069 Uiso 1 1 calc R . . C6 C 0.6322(8) 0.7137(7) 0.4115(5) 0.058(3) Uani 1 1 d . . . H6A H 0.6105 0.7399 0.3673 0.070 Uiso 1 1 calc R . . C7 C 0.6943(7) 0.7616(6) 0.4739(5) 0.047(2) Uani 1 1 d . . . H7A H 0.7132 0.8206 0.4721 0.057 Uiso 1 1 calc R . . C8 C 0.7515(6) 0.4844(5) 0.6190(5) 0.041(2) Uani 1 1 d . . . C9 C 0.8168(7) 0.4616(5) 0.5710(5) 0.044(2) Uani 1 1 d . . . H9A H 0.8486 0.5045 0.5464 0.053 Uiso 1 1 calc R . . C10 C 0.8355(8) 0.3777(6) 0.5589(5) 0.052(2) Uani 1 1 d . . . H10A H 0.8826 0.3650 0.5289 0.062 Uiso 1 1 calc R . . C11 C 0.7840(9) 0.3127(6) 0.5917(6) 0.061(3) Uani 1 1 d . . . H11A H 0.7919 0.2555 0.5814 0.073 Uiso 1 1 calc R . . C12 C 0.7209(9) 0.3336(6) 0.6396(6) 0.062(3) Uani 1 1 d . . . H12A H 0.6883 0.2897 0.6628 0.074 Uiso 1 1 calc R . . C13 C 0.7040(7) 0.4178(5) 0.6549(5) 0.046(2) Uani 1 1 d . . . H13A H 0.6618 0.4300 0.6883 0.055 Uiso 1 1 calc R . . C14 C 0.6082(7) 0.5938(5) 0.6701(5) 0.040(2) Uani 1 1 d . . . C15 C 0.5062(7) 0.6131(5) 0.6260(6) 0.054(3) Uani 1 1 d . . . H15A H 0.5006 0.6260 0.5771 0.065 Uiso 1 1 calc R . . C16 C 0.4135(9) 0.6127(7) 0.6560(8) 0.079(4) Uani 1 1 d . . . H16A H 0.3455 0.6254 0.6269 0.095 Uiso 1 1 calc R . . C17 C 0.4215(9) 0.5937(7) 0.7283(9) 0.084(4) Uani 1 1 d . . . H17A H 0.3586 0.5930 0.7475 0.100 Uiso 1 1 calc R . . C18 C 0.5227(9) 0.5756(7) 0.7730(7) 0.070(3) Uani 1 1 d . . . H18A H 0.5285 0.5634 0.8221 0.084 Uiso 1 1 calc R . . C19 C 0.6148(8) 0.5761(6) 0.7424(6) 0.054(3) Uani 1 1 d . . . H19A H 0.6830 0.5640 0.7718 0.065 Uiso 1 1 calc R . . C20 C 0.9723(6) 0.6530(5) 0.6356(5) 0.0357(19) Uani 1 1 d . . . C21 C 1.0425(6) 0.5823(5) 0.6685(4) 0.0335(19) Uani 1 1 d . . . C22 C 1.0508(7) 0.5619(5) 0.7408(5) 0.040(2) Uani 1 1 d . . . C23 C 1.1136(7) 0.4982(6) 0.7714(6) 0.052(2) Uani 1 1 d . . . H23A H 1.1220 0.4872 0.8210 0.063 Uiso 1 1 calc R . . C24 C 1.1634(8) 0.4513(6) 0.7265(6) 0.056(3) Uani 1 1 d . . . H24A H 1.2028 0.4067 0.7454 0.067 Uiso 1 1 calc R . . C25 C 1.1548(8) 0.4703(6) 0.6542(7) 0.060(3) Uani 1 1 d . . . H25A H 1.1899 0.4393 0.6249 0.072 Uiso 1 1 calc R . . C26 C 1.0946(7) 0.5350(6) 0.6247(5) 0.047(2) Uani 1 1 d . . . H26A H 1.0889 0.5472 0.5756 0.057 Uiso 1 1 calc R . . C27 C 1.1038(7) 0.6932(5) 0.8584(5) 0.0363(19) Uani 1 1 d . . . C28 C 1.1327(8) 0.6816(6) 0.9320(5) 0.058(3) Uani 1 1 d . . . H28A H 1.0888 0.6410 0.9515 0.069 Uiso 1 1 calc R . . C29 C 1.2280(10) 0.7301(8) 0.9794(6) 0.080(4) Uani 1 1 d . . . H29A H 1.2475 0.7211 1.0297 0.096 Uiso 1 1 calc R . . C30 C 1.2913(8) 0.7904(8) 0.9506(7) 0.072(3) Uani 1 1 d . . . H30A H 1.3535 0.8233 0.9819 0.087 Uiso 1 1 calc R . . C31 C 1.2654(8) 0.8034(7) 0.8771(6) 0.066(3) Uani 1 1 d . . . H31A H 1.3094 0.8443 0.8579 0.079 Uiso 1 1 calc R . . C32 C 1.1714(7) 0.7541(6) 0.8312(5) 0.056(3) Uani 1 1 d . . . H32A H 1.1534 0.7623 0.7807 0.067 Uiso 1 1 calc R . . C33 C 0.9061(7) 0.5689(5) 0.8480(5) 0.038(2) Uani 1 1 d . . . C34 C 0.8741(8) 0.4815(6) 0.8334(5) 0.050(2) Uani 1 1 d . . . H34A H 0.9015 0.4517 0.7989 0.060 Uiso 1 1 calc R . . C35 C 0.8010(10) 0.4376(7) 0.8698(7) 0.071(3) Uani 1 1 d . . . H35A H 0.7779 0.3789 0.8589 0.086 Uiso 1 1 calc R . . C36 C 0.7635(10) 0.4815(8) 0.9218(7) 0.084(4) Uani 1 1 d . . . H36A H 0.7158 0.4522 0.9469 0.101 Uiso 1 1 calc R . . C37 C 0.7955(10) 0.5687(8) 0.9374(7) 0.076(3) Uani 1 1 d . . . H37A H 0.7707 0.5982 0.9735 0.091 Uiso 1 1 calc R . . C39 C 0.9864(6) 0.9040(5) 0.8421(4) 0.0318(18) Uani 1 1 d . . . C38 C 0.8643(8) 0.6113(6) 0.8992(5) 0.055(3) Uani 1 1 d . . . H39A H 0.8832 0.6706 0.9080 0.066 Uiso 1 1 calc R . . C40 C 1.0943(7) 0.9642(5) 0.8661(4) 0.038(2) Uani 1 1 d . . . C41 C 1.1469(7) 1.0020(5) 0.8158(4) 0.0359(19) Uani 1 1 d . . . C42 C 1.2445(7) 1.0609(6) 0.8405(5) 0.052(2) Uani 1 1 d . . . H42A H 1.2797 1.0868 0.8066 0.063 Uiso 1 1 calc R . . C43 C 1.2880(9) 1.0802(7) 0.9154(6) 0.070(3) Uani 1 1 d . . . H43A H 1.3534 1.1187 0.9323 0.084 Uiso 1 1 calc R . . C44 C 1.2339(10) 1.0418(7) 0.9658(6) 0.076(4) Uani 1 1 d . . . H44A H 1.2625 1.0561 1.0162 0.092 Uiso 1 1 calc R . . C45 C 1.1408(9) 0.9844(7) 0.9423(5) 0.062(3) Uani 1 1 d . . . H45A H 1.1071 0.9578 0.9767 0.074 Uiso 1 1 calc R . . C46 C 1.0782(6) 1.0652(5) 0.6675(5) 0.036(2) Uani 1 1 d . . . C47 C 1.0697(9) 1.0569(6) 0.5928(6) 0.059(3) Uani 1 1 d . . . H47A H 1.0691 1.0027 0.5703 0.071 Uiso 1 1 calc R . . C48 C 1.0622(10) 1.1269(8) 0.5505(6) 0.072(3) Uani 1 1 d . . . H48A H 1.0590 1.1202 0.5002 0.087 Uiso 1 1 calc R . . C49 C 1.0593(10) 1.2070(7) 0.5824(8) 0.075(3) Uani 1 1 d . . . H49A H 1.0487 1.2540 0.5537 0.090 Uiso 1 1 calc R . . C50 C 1.0720(10) 1.2155(7) 0.6553(8) 0.081(4) Uani 1 1 d . . . H50A H 1.0747 1.2700 0.6778 0.097 Uiso 1 1 calc R . . C51 C 1.0815(8) 1.1451(6) 0.6989(6) 0.060(3) Uani 1 1 d . . . H51A H 1.0901 1.1531 0.7498 0.072 Uiso 1 1 calc R . . C52 C 1.1817(6) 0.9114(5) 0.6856(4) 0.0360(19) Uani 1 1 d . . . C53 C 1.1435(7) 0.8375(6) 0.6401(5) 0.048(2) Uani 1 1 d . . . H53A H 1.0669 0.8176 0.6265 0.057 Uiso 1 1 calc R . . C54 C 1.2182(9) 0.7926(6) 0.6143(6) 0.065(3) Uani 1 1 d . . . H54A H 1.1921 0.7426 0.5835 0.078 Uiso 1 1 calc R . . C55 C 1.3317(9) 0.8223(7) 0.6347(6) 0.063(3) Uani 1 1 d . . . H55A H 1.3823 0.7918 0.6181 0.076 Uiso 1 1 calc R . . C56 C 1.3695(8) 0.8946(8) 0.6781(6) 0.064(3) Uani 1 1 d . . . H56A H 1.4461 0.9145 0.6906 0.077 Uiso 1 1 calc R . . C57 C 1.2965(7) 0.9404(7) 0.7048(6) 0.064(3) Uani 1 1 d . . . H57A H 1.3239 0.9903 0.7355 0.077 Uiso 1 1 calc R . . C58 C 0.7783(6) 0.8237(5) 0.7650(5) 0.037(2) Uani 1 1 d . . . C59 C 0.7002(6) 0.8703(5) 0.7985(4) 0.0355(19) Uani 1 1 d . . . C60 C 0.7093(6) 0.9588(5) 0.7953(4) 0.0349(19) Uani 1 1 d . . . C61 C 0.6414(7) 1.0052(6) 0.8284(5) 0.046(2) Uani 1 1 d . . . H61A H 0.6482 1.0649 0.8280 0.055 Uiso 1 1 calc R . . C62 C 0.5650(7) 0.9625(7) 0.8616(5) 0.055(3) Uani 1 1 d . . . H62A H 0.5187 0.9933 0.8823 0.066 Uiso 1 1 calc R . . C63 C 0.5564(7) 0.8741(7) 0.8644(5) 0.052(2) Uani 1 1 d . . . H63A H 0.5054 0.8458 0.8877 0.063 Uiso 1 1 calc R . . C64 C 0.6232(7) 0.8276(6) 0.8326(5) 0.049(2) Uani 1 1 d . . . H64A H 0.6168 0.7680 0.8341 0.059 Uiso 1 1 calc R . . C65 C 0.8731(6) 1.1033(5) 0.7986(5) 0.039(2) Uani 1 1 d . . . C66 C 0.9179(8) 1.1021(6) 0.8754(5) 0.050(2) Uani 1 1 d . . . H66A H 0.9154 1.0503 0.8980 0.060 Uiso 1 1 calc R . . C67 C 0.9654(9) 1.1776(7) 0.9171(6) 0.065(3) Uani 1 1 d . . . H67A H 0.9934 1.1770 0.9681 0.077 Uiso 1 1 calc R . . C68 C 0.9712(9) 1.2526(7) 0.8838(7) 0.068(3) Uani 1 1 d . . . H68A H 1.0054 1.3031 0.9119 0.081 Uiso 1 1 calc R . . C69 C 0.9274(9) 1.2550(6) 0.8093(7) 0.064(3) Uani 1 1 d . . . H69A H 0.9303 1.3075 0.7878 0.077 Uiso 1 1 calc R . . C70 C 0.8796(8) 1.1815(5) 0.7661(5) 0.049(2) Uani 1 1 d . . . H70A H 0.8515 1.1838 0.7153 0.059 Uiso 1 1 calc R . . C71 C 0.7280(7) 1.0356(5) 0.6573(5) 0.038(2) Uani 1 1 d . . . C72 C 0.7685(8) 1.0326(6) 0.5949(5) 0.049(2) Uani 1 1 d . . . H72A H 0.8370 1.0122 0.5968 0.058 Uiso 1 1 calc R . . C73 C 0.7084(10) 1.0593(7) 0.5299(6) 0.068(3) Uani 1 1 d . . . H73A H 0.7361 1.0572 0.4878 0.081 Uiso 1 1 calc R . . C74 C 0.6049(9) 1.0900(7) 0.5265(6) 0.067(3) Uani 1 1 d . . . H74A H 0.5632 1.1067 0.4820 0.081 Uiso 1 1 calc R . . C75 C 0.5661(9) 1.0951(7) 0.5886(6) 0.069(3) Uani 1 1 d . . . H75A H 0.4989 1.1173 0.5871 0.082 Uiso 1 1 calc R . . C76 C 0.6259(8) 1.0675(7) 0.6535(6) 0.058(3) Uani 1 1 d . . . H76A H 0.5981 1.0701 0.6956 0.070 Uiso 1 1 calc R . . Cl1 Cl 0.5213(2) 0.22754(19) 0.79636(16) 0.0695(7) Uani 1 1 d . . . C77 C 0.6186(10) 0.6464(8) 0.0834(7) 0.087(4) Uani 1 1 d . . . H77A H 0.5752 0.6642 0.1177 0.104 Uiso 1 1 calc R . . Cl2 Cl 0.6184(3) 0.5350(3) 0.0824(2) 0.1115(13) Uani 1 1 d . . . Cl4 Cl 0.7534(3) 0.6974(2) 0.1114(2) 0.1188(13) Uani 1 1 d . . . Cl3 Cl 0.5540(4) 0.6736(3) -0.0079(3) 0.1395(17) Uani 1 1 d . . . O5 O 0.5180(9) 0.2048(7) 0.8673(6) 0.125(3) Uiso 1 1 d . . . O6 O 0.4843(9) 0.3071(8) 0.7820(6) 0.131(4) Uiso 1 1 d . . . O7 O 0.6327(10) 0.2289(8) 0.7880(6) 0.144(4) Uiso 1 1 d . . . O8 O 0.4556(8) 0.1597(7) 0.7452(5) 0.113(3) Uiso 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 Ir1 0.02849(16) 0.02081(17) 0.03337(19) 0.00405(13) 0.00748(13) 0.00191(12) Ir2 0.02930(17) 0.02085(17) 0.03170(19) 0.00415(13) 0.00780(13) 0.00269(12) C1 0.027(4) 0.026(4) 0.043(5) -0.006(4) 0.008(4) 0.002(3) O1 0.045(3) 0.029(3) 0.022(3) 0.007(2) 0.004(2) 0.009(2) P1 0.0338(11) 0.0249(11) 0.0410(13) 0.0015(10) 0.0092(9) -0.0001(8) C2 0.038(4) 0.029(5) 0.039(5) 0.005(4) 0.002(4) 0.012(4) O2 0.059(4) 0.039(4) 0.040(4) 0.003(3) 0.018(3) 0.004(3) P2 0.0368(11) 0.0280(11) 0.0361(12) 0.0074(9) 0.0095(9) 0.0058(9) C3 0.033(4) 0.036(5) 0.049(5) 0.001(4) 0.006(4) 0.007(4) O3 0.058(4) 0.071(5) 0.040(4) 0.020(3) 0.014(3) -0.004(3) P3 0.0320(10) 0.0250(11) 0.0341(12) 0.0031(9) 0.0075(9) 0.0002(8) C4 0.043(5) 0.046(6) 0.044(6) -0.006(5) 0.002(4) 0.001(4) O4 0.041(3) 0.022(3) 0.057(4) 0.009(3) 0.020(3) 0.005(2) P4 0.0382(11) 0.0241(11) 0.0341(12) 0.0035(9) 0.0099(9) 0.0051(9) C5 0.057(6) 0.057(7) 0.049(6) -0.008(5) -0.008(5) 0.014(5) C6 0.059(6) 0.067(7) 0.039(6) 0.013(5) -0.012(5) 0.021(5) C7 0.051(5) 0.040(5) 0.048(6) 0.009(5) 0.003(4) 0.011(4) C8 0.032(4) 0.032(5) 0.057(6) 0.003(4) 0.009(4) 0.000(4) C9 0.047(5) 0.032(5) 0.053(6) -0.001(4) 0.014(4) 0.003(4) C10 0.070(6) 0.035(5) 0.061(6) 0.003(5) 0.031(5) 0.017(5) C11 0.089(8) 0.032(6) 0.061(7) -0.008(5) 0.012(6) 0.016(5) C12 0.081(7) 0.030(5) 0.080(8) 0.018(5) 0.029(6) 0.000(5) C13 0.047(5) 0.033(5) 0.059(6) 0.006(5) 0.017(5) 0.000(4) C14 0.033(4) 0.026(4) 0.061(6) -0.004(4) 0.018(4) -0.002(3) C15 0.045(5) 0.035(5) 0.082(7) 0.004(5) 0.018(5) 0.001(4) C16 0.044(6) 0.067(8) 0.132(12) 0.007(8) 0.034(7) 0.008(5) C17 0.052(7) 0.052(7) 0.157(14) -0.011(8) 0.052(8) -0.004(5) C18 0.059(7) 0.072(8) 0.083(8) -0.006(6) 0.033(6) -0.008(6) C19 0.039(5) 0.054(6) 0.073(7) 0.005(5) 0.027(5) -0.005(4) C20 0.036(4) 0.028(5) 0.041(5) 0.005(4) 0.006(4) -0.001(3) C21 0.033(4) 0.032(5) 0.035(5) 0.006(4) 0.005(4) 0.008(3) C22 0.037(4) 0.028(5) 0.057(6) 0.009(4) 0.010(4) 0.012(4) C23 0.053(6) 0.042(6) 0.068(7) 0.020(5) 0.016(5) 0.020(4) C24 0.053(6) 0.048(6) 0.076(8) 0.009(6) 0.023(5) 0.020(5) C25 0.053(6) 0.044(6) 0.089(9) -0.002(6) 0.028(6) 0.015(5) C26 0.053(5) 0.043(6) 0.051(6) 0.007(5) 0.019(5) 0.013(4) C27 0.038(4) 0.033(5) 0.040(5) 0.013(4) 0.009(4) 0.009(4) C28 0.055(6) 0.059(7) 0.055(7) 0.013(5) 0.009(5) -0.007(5) C29 0.074(8) 0.108(10) 0.042(6) 0.004(6) -0.006(6) -0.009(7) C30 0.044(6) 0.083(9) 0.073(8) -0.001(7) -0.015(6) 0.002(6) C31 0.043(5) 0.055(7) 0.088(9) 0.023(6) -0.004(6) -0.005(5) C32 0.035(5) 0.074(7) 0.055(6) 0.021(5) 0.001(4) 0.005(5) C33 0.044(5) 0.039(5) 0.038(5) 0.016(4) 0.018(4) 0.013(4) C34 0.060(6) 0.034(5) 0.064(6) 0.021(5) 0.029(5) 0.008(4) C35 0.091(8) 0.043(6) 0.098(9) 0.030(6) 0.050(7) 0.015(6) C36 0.094(9) 0.085(10) 0.093(9) 0.029(8) 0.062(8) 0.005(7) C37 0.097(9) 0.070(8) 0.080(8) 0.009(7) 0.056(7) 0.016(7) C39 0.042(4) 0.042(5) 0.009(4) 0.011(3) 0.000(3) 0.007(4) C38 0.062(6) 0.047(6) 0.063(7) 0.004(5) 0.026(5) 0.011(5) C40 0.047(5) 0.032(5) 0.034(5) 0.006(4) 0.006(4) 0.001(4) C41 0.043(5) 0.035(5) 0.031(5) 0.005(4) 0.010(4) 0.008(4) C42 0.043(5) 0.053(6) 0.056(6) -0.010(5) 0.011(5) -0.003(4) C43 0.058(6) 0.070(8) 0.064(7) 0.001(6) -0.005(6) -0.019(5) C44 0.081(8) 0.080(8) 0.042(6) -0.006(6) -0.022(6) -0.015(6) C45 0.074(7) 0.063(7) 0.041(6) 0.003(5) 0.004(5) -0.006(5) C46 0.035(4) 0.031(5) 0.047(5) 0.010(4) 0.016(4) 0.002(3) C47 0.078(7) 0.030(5) 0.064(7) 0.011(5) 0.009(6) -0.005(5) C48 0.090(8) 0.072(8) 0.059(7) 0.032(7) 0.026(6) 0.005(7) C49 0.092(9) 0.049(8) 0.094(10) 0.036(7) 0.037(8) 0.017(6) C50 0.105(9) 0.035(6) 0.122(12) 0.031(7) 0.055(9) 0.018(6) C51 0.074(7) 0.041(6) 0.068(7) 0.002(5) 0.027(6) 0.002(5) C52 0.039(4) 0.038(5) 0.034(5) 0.008(4) 0.014(4) 0.006(4) C53 0.047(5) 0.039(5) 0.064(6) 0.009(5) 0.026(5) 0.005(4) C54 0.081(8) 0.033(5) 0.098(9) 0.003(6) 0.054(7) 0.007(5) C55 0.071(7) 0.061(7) 0.077(8) 0.024(6) 0.042(6) 0.032(6) C56 0.039(5) 0.088(9) 0.067(7) -0.003(6) 0.011(5) 0.014(5) C57 0.039(5) 0.081(8) 0.069(7) -0.015(6) 0.011(5) 0.002(5) C58 0.034(4) 0.028(5) 0.048(5) 0.005(4) 0.011(4) 0.001(3) C59 0.031(4) 0.036(5) 0.037(5) -0.002(4) 0.006(4) 0.006(4) C60 0.035(4) 0.034(5) 0.037(5) 0.005(4) 0.010(4) 0.008(4) C61 0.051(5) 0.045(6) 0.044(5) 0.003(4) 0.011(4) 0.017(4) C62 0.042(5) 0.075(8) 0.057(6) 0.007(6) 0.019(5) 0.024(5) C63 0.040(5) 0.061(7) 0.061(6) 0.008(5) 0.021(5) 0.009(5) C64 0.049(5) 0.044(6) 0.056(6) 0.004(5) 0.019(5) 0.000(4) C65 0.036(4) 0.035(5) 0.052(6) 0.000(4) 0.019(4) 0.015(4) C66 0.067(6) 0.040(5) 0.042(6) -0.003(4) 0.016(5) 0.002(4) C67 0.072(7) 0.057(7) 0.057(7) -0.013(6) 0.010(5) -0.003(5) C68 0.071(7) 0.052(7) 0.073(8) -0.018(6) 0.014(6) -0.007(5) C69 0.065(7) 0.033(6) 0.096(9) 0.004(6) 0.024(6) 0.004(5) C70 0.066(6) 0.029(5) 0.055(6) 0.009(5) 0.018(5) 0.007(4) C71 0.049(5) 0.025(4) 0.039(5) 0.012(4) 0.004(4) 0.009(4) C72 0.056(6) 0.039(5) 0.057(6) 0.011(5) 0.019(5) 0.014(4) C73 0.104(9) 0.052(7) 0.052(7) 0.019(5) 0.024(6) 0.017(6) C74 0.075(7) 0.067(8) 0.052(7) 0.018(6) -0.007(6) 0.022(6) C75 0.070(7) 0.070(8) 0.069(8) 0.012(6) 0.009(6) 0.035(6) C76 0.058(6) 0.068(7) 0.051(6) 0.005(5) 0.012(5) 0.019(5) Cl1 0.0796(18) 0.0706(19) 0.0693(19) 0.0103(15) 0.0314(15) 0.0259(15) C77 0.079(8) 0.092(10) 0.088(9) -0.010(8) 0.017(7) 0.021(7) Cl2 0.118(3) 0.108(3) 0.104(3) 0.010(2) 0.031(2) -0.015(2) Cl4 0.104(3) 0.092(3) 0.146(4) -0.010(3) 0.014(3) -0.006(2) Cl3 0.155(4) 0.137(4) 0.122(3) 0.001(3) 0.002(3) 0.074(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 2.022(8) . ? Ir1 C20 2.007(8) . ? Ir1 O4 2.181(5) . ? Ir1 P1 2.296(2) . ? Ir1 P2 2.358(2) . ? Ir1 Ir2 2.9629(4) . ? Ir1 H1 1.7660 . ? Ir2 C39 2.025(7) . ? Ir2 C58 2.027(8) . ? Ir2 O1 2.268(5) . ? Ir2 P4 2.301(2) . ? Ir2 P3 2.3947(19) . ? Ir2 H1 1.7101 . ? C1 O1 1.266(9) . ? C1 C2 1.471(11) . ? P1 C3 1.787(9) . ? P1 C8 1.803(9) . ? P1 C14 1.833(8) . ? C2 C3 1.420(11) . ? C2 C7 1.387(11) . ? O2 C20 1.243(9) . ? P2 C27 1.823(8) . ? P2 C22 1.831(8) . ? P2 C33 1.820(8) . ? C3 C4 1.400(11) . ? O3 C39 1.222(9) . ? P3 C41 1.821(8) . ? P3 C46 1.838(8) . ? P3 C52 1.834(8) . ? C4 C5 1.349(13) . ? C4 H4A 0.9300 . ? O4 C58 1.244(9) . ? P4 C71 1.827(8) . ? P4 C65 1.818(8) . ? P4 C60 1.818(8) . ? C5 C6 1.380(13) . ? C5 H5A 0.9300 . ? C6 C7 1.370(12) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.407(11) . ? C8 C9 1.403(11) . ? C9 C10 1.381(11) . ? C9 H9A 0.9300 . ? C10 C11 1.378(13) . ? C10 H10A 0.9300 . ? C11 C12 1.372(13) . ? C11 H11A 0.9300 . ? C12 C13 1.388(12) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C19 1.372(12) . ? C14 C15 1.398(12) . ? C15 C16 1.388(13) . ? C15 H15A 0.9300 . ? C16 C17 1.374(17) . ? C16 H16A 0.9300 . ? C17 C18 1.390(16) . ? C17 H17A 0.9300 . ? C18 C19 1.388(12) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.540(11) . ? C21 C26 1.394(11) . ? C21 C22 1.380(11) . ? C22 C23 1.390(11) . ? C23 C24 1.387(13) . ? C23 H23A 0.9300 . ? C24 C25 1.373(13) . ? C24 H24A 0.9300 . ? C25 C26 1.378(13) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.357(12) . ? C27 C32 1.387(12) . ? C28 C29 1.407(13) . ? C28 H28A 0.9300 . ? C29 C30 1.366(15) . ? C29 H29A 0.9300 . ? C30 C31 1.358(14) . ? C30 H30A 0.9300 . ? C31 C32 1.392(13) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.378(12) . ? C33 C38 1.374(12) . ? C34 C35 1.392(12) . ? C34 H34A 0.9300 . ? C35 C36 1.365(15) . ? C35 H35A 0.9300 . ? C36 C37 1.377(16) . ? C36 H36A 0.9300 . ? C37 C38 1.369(13) . ? C37 H37A 0.9300 . ? C39 C40 1.501(11) . ? C38 H39A 0.9300 . ? C40 C41 1.378(11) . ? C40 C45 1.406(12) . ? C41 C42 1.399(11) . ? C42 C43 1.378(13) . ? C42 H42A 0.9300 . ? C43 C44 1.394(14) . ? C43 H43A 0.9300 . ? C44 C45 1.345(13) . ? C44 H44A 0.9300 . ? C45 H45A 0.9300 . ? C46 C51 1.353(12) . ? C46 C47 1.371(12) . ? C47 C48 1.375(13) . ? C47 H47A 0.9300 . ? C48 C49 1.376(15) . ? C48 H48A 0.9300 . ? C49 C50 1.329(16) . ? C49 H49A 0.9300 . ? C50 C51 1.395(14) . ? C50 H50A 0.9300 . ? C51 H51A 0.9300 . ? C52 C53 1.374(11) . ? C52 C57 1.391(11) . ? C53 C54 1.383(12) . ? C53 H53A 0.9300 . ? C54 C55 1.379(14) . ? C54 H54A 0.9300 . ? C55 C56 1.335(14) . ? C55 H55A 0.9300 . ? C56 C57 1.383(13) . ? C56 H56A 0.9300 . ? C57 H57A 0.9300 . ? C58 C59 1.507(11) . ? C59 C60 1.382(11) . ? C59 C64 1.390(11) . ? C60 C61 1.402(11) . ? C61 C62 1.373(12) . ? C61 H61A 0.9300 . ? C62 C63 1.381(13) . ? C62 H62A 0.9300 . ? C63 C64 1.378(12) . ? C63 H63A 0.9300 . ? C64 H64A 0.9300 . ? C65 C66 1.406(12) . ? C65 C70 1.391(12) . ? C66 C67 1.378(12) . ? C66 H66A 0.9300 . ? C67 C68 1.353(14) . ? C67 H67A 0.9300 . ? C68 C69 1.365(15) . ? C68 H68A 0.9300 . ? C69 C70 1.366(13) . ? C69 H69A 0.9300 . ? C70 H70A 0.9300 . ? C71 C76 1.395(12) . ? C71 C72 1.374(11) . ? C72 C73 1.368(13) . ? C72 H72A 0.9300 . ? C73 C74 1.403(15) . ? C73 H73A 0.9300 . ? C74 C75 1.358(14) . ? C74 H74A 0.9300 . ? C75 C76 1.371(13) . ? C75 H75A 0.9300 . ? C76 H76A 0.9300 . ? Cl1 O7 1.418(12) . ? Cl1 O5 1.391(11) . ? Cl1 O6 1.390(12) . ? Cl1 O8 1.430(10) . ? C77 Cl4 1.709(12) . ? C77 Cl2 1.744(13) . ? C77 Cl3 1.786(13) . ? C77 H77A 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C20 91.3(3) . . ? C1 Ir1 O4 89.6(3) . . ? C20 Ir1 O4 175.5(2) . . ? C1 Ir1 P1 80.6(2) . . ? C20 Ir1 P1 86.8(2) . . ? O4 Ir1 P1 89.00(15) . . ? C1 Ir1 P2 172.4(2) . . ? C20 Ir1 P2 83.7(3) . . ? O4 Ir1 P2 95.80(15) . . ? P1 Ir1 P2 104.80(8) . . ? C1 Ir1 Ir2 67.8(2) . . ? C20 Ir1 Ir2 118.4(2) . . ? O4 Ir1 Ir2 65.92(13) . . ? P1 Ir1 Ir2 138.89(6) . . ? P2 Ir1 Ir2 109.51(5) . . ? C1 Ir1 H1 91.3 . . ? C20 Ir1 H1 99.6 . . ? O4 Ir1 H1 84.8 . . ? P1 Ir1 H1 169.8 . . ? P2 Ir1 H1 83.8 . . ? Ir2 Ir1 H1 31.0 . . ? C39 Ir2 C58 85.6(3) . . ? C39 Ir2 O1 170.2(3) . . ? C58 Ir2 O1 88.9(3) . . ? C39 Ir2 P4 90.8(2) . . ? C58 Ir2 P4 81.8(2) . . ? O1 Ir2 P4 96.48(14) . . ? C39 Ir2 P3 83.5(2) . . ? C58 Ir2 P3 169.0(2) . . ? O1 Ir2 P3 101.79(14) . . ? P4 Ir2 P3 99.19(7) . . ? C39 Ir2 Ir1 105.1(2) . . ? C58 Ir2 Ir1 65.4(2) . . ? O1 Ir2 Ir1 65.09(13) . . ? P4 Ir2 Ir1 141.71(5) . . ? P3 Ir2 Ir1 116.80(5) . . ? C39 Ir2 H1 83.3 . . ? C58 Ir2 H1 86.3 . . ? O1 Ir2 H1 88.3 . . ? P4 Ir2 H1 167.1 . . ? P3 Ir2 H1 91.6 . . ? Ir1 Ir2 H1 32.1 . . ? O1 C1 C2 117.7(7) . . ? O1 C1 Ir1 120.1(5) . . ? C2 C1 Ir1 122.2(6) . . ? C1 O1 Ir2 106.2(5) . . ? C3 P1 C8 105.0(4) . . ? C3 P1 C14 105.7(4) . . ? C8 P1 C14 105.3(4) . . ? C3 P1 Ir1 102.3(3) . . ? C8 P1 Ir1 124.8(3) . . ? C14 P1 Ir1 112.1(3) . . ? C3 C2 C7 119.4(8) . . ? C3 C2 C1 115.1(7) . . ? C7 C2 C1 125.5(8) . . ? C27 P2 C22 102.4(4) . . ? C27 P2 C33 105.7(4) . . ? C22 P2 C33 109.9(4) . . ? C27 P2 Ir1 120.3(3) . . ? C22 P2 Ir1 100.8(3) . . ? C33 P2 Ir1 116.3(3) . . ? C2 C3 C4 117.6(8) . . ? C2 C3 P1 114.3(6) . . ? C4 C3 P1 128.0(7) . . ? C41 P3 C46 106.7(4) . . ? C41 P3 C52 105.6(4) . . ? C46 P3 C52 101.8(4) . . ? C41 P3 Ir2 100.2(3) . . ? C46 P3 Ir2 121.0(3) . . ? C52 P3 Ir2 120.0(3) . . ? C5 C4 C3 121.8(9) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C58 O4 Ir1 107.1(5) . . ? C71 P4 C65 104.8(4) . . ? C71 P4 C60 107.0(4) . . ? C65 P4 C60 103.0(4) . . ? C71 P4 Ir2 114.3(3) . . ? C65 P4 Ir2 123.4(3) . . ? C60 P4 Ir2 102.8(3) . . ? C6 C5 C4 120.3(9) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C7 120.2(9) . . ? C5 C6 H6A 119.9 . . ? C7 C6 H6A 119.9 . . ? C6 C7 C2 120.6(9) . . ? C6 C7 H7A 119.7 . . ? C2 C7 H7A 119.7 . . ? C13 C8 C9 117.4(8) . . ? C13 C8 P1 122.9(7) . . ? C9 C8 P1 119.7(6) . . ? C10 C9 C8 122.3(8) . . ? C10 C9 H9A 118.9 . . ? C8 C9 H9A 118.9 . . ? C11 C10 C9 119.6(9) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C10 C11 C12 119.1(9) . . ? C10 C11 H11A 120.5 . . ? C12 C11 H11A 120.5 . . ? C13 C12 C11 122.5(9) . . ? C13 C12 H12A 118.7 . . ? C11 C12 H12A 118.7 . . ? C8 C13 C12 119.1(8) . . ? C8 C13 H13A 120.5 . . ? C12 C13 H13A 120.5 . . ? C19 C14 C15 119.2(8) . . ? C19 C14 P1 119.5(7) . . ? C15 C14 P1 121.3(8) . . ? C14 C15 C16 119.4(10) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C17 C16 C15 120.5(11) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 120.7(11) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C19 118.3(11) . . ? C17 C18 H18A 120.9 . . ? C19 C18 H18A 120.9 . . ? C14 C19 C18 121.9(10) . . ? C14 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? O2 C20 C21 115.7(7) . . ? O2 C20 Ir1 125.9(6) . . ? C21 C20 Ir1 118.0(6) . . ? C26 C21 C22 118.7(8) . . ? C26 C21 C20 120.6(8) . . ? C22 C21 C20 120.6(7) . . ? C23 C22 C21 121.5(8) . . ? C23 C22 P2 124.6(7) . . ? C21 C22 P2 113.7(6) . . ? C22 C23 C24 118.7(9) . . ? C22 C23 H23A 120.7 . . ? C24 C23 H23A 120.7 . . ? C25 C24 C23 120.4(9) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 120.6(9) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.1(9) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C28 C27 C32 117.9(8) . . ? C28 C27 P2 124.4(7) . . ? C32 C27 P2 117.7(7) . . ? C27 C28 C29 121.2(9) . . ? C27 C28 H28A 119.4 . . ? C29 C28 H28A 119.4 . . ? C30 C29 C28 119.1(10) . . ? C30 C29 H29A 120.5 . . ? C28 C29 H29A 120.5 . . ? C29 C30 C31 121.4(10) . . ? C29 C30 H30A 119.3 . . ? C31 C30 H30A 119.3 . . ? C30 C31 C32 118.5(10) . . ? C30 C31 H31A 120.7 . . ? C32 C31 H31A 120.7 . . ? C27 C32 C31 121.9(9) . . ? C27 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C34 C33 C38 118.5(8) . . ? C34 C33 P2 122.4(7) . . ? C38 C33 P2 118.4(7) . . ? C33 C34 C35 120.5(9) . . ? C33 C34 H34A 119.7 . . ? C35 C34 H34A 119.7 . . ? C36 C35 C34 119.3(11) . . ? C36 C35 H35A 120.4 . . ? C34 C35 H35A 120.4 . . ? C37 C36 C35 120.9(10) . . ? C37 C36 H36A 119.5 . . ? C35 C36 H36A 119.5 . . ? C36 C37 C38 118.9(10) . . ? C36 C37 H37A 120.5 . . ? C38 C37 H37A 120.5 . . ? O3 C39 C40 119.4(7) . . ? O3 C39 Ir2 122.3(6) . . ? C40 C39 Ir2 118.3(5) . . ? C33 C38 C37 121.8(10) . . ? C33 C38 H39A 119.1 . . ? C37 C38 H39A 119.1 . . ? C41 C40 C45 119.3(8) . . ? C41 C40 C39 122.0(7) . . ? C45 C40 C39 118.7(7) . . ? C40 C41 C42 120.2(8) . . ? C40 C41 P3 114.5(6) . . ? C42 C41 P3 125.3(7) . . ? C41 C42 C43 119.5(9) . . ? C41 C42 H42A 120.3 . . ? C43 C42 H42A 120.3 . . ? C42 C43 C44 119.8(9) . . ? C42 C43 H43A 120.1 . . ? C44 C43 H43A 120.1 . . ? C45 C44 C43 120.8(9) . . ? C45 C44 H44A 119.6 . . ? C43 C44 H44A 119.6 . . ? C44 C45 C40 120.3(10) . . ? C44 C45 H45A 119.8 . . ? C40 C45 H45A 119.8 . . ? C51 C46 C47 118.0(9) . . ? C51 C46 P3 123.3(7) . . ? C47 C46 P3 118.8(7) . . ? C48 C47 C46 121.3(10) . . ? C48 C47 H47A 119.3 . . ? C46 C47 H47A 119.3 . . ? C47 C48 C49 120.1(11) . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C50 C49 C48 118.4(11) . . ? C50 C49 H49A 120.8 . . ? C48 C49 H49A 120.8 . . ? C49 C50 C51 121.9(12) . . ? C49 C50 H50A 119.1 . . ? C51 C50 H50A 119.1 . . ? C46 C51 C50 120.2(11) . . ? C46 C51 H51A 119.9 . . ? C50 C51 H51A 119.9 . . ? C53 C52 C57 118.9(8) . . ? C53 C52 P3 118.8(6) . . ? C57 C52 P3 122.3(7) . . ? C52 C53 C54 120.4(9) . . ? C52 C53 H53A 119.8 . . ? C54 C53 H53A 119.8 . . ? C55 C54 C53 119.6(10) . . ? C55 C54 H54A 120.2 . . ? C53 C54 H54A 120.2 . . ? C56 C55 C54 120.5(9) . . ? C56 C55 H55A 119.8 . . ? C54 C55 H55A 119.8 . . ? C55 C56 C57 121.0(10) . . ? C55 C56 H56A 119.5 . . ? C57 C56 H56A 119.5 . . ? C56 C57 C52 119.6(9) . . ? C56 C57 H57A 120.2 . . ? C52 C57 H57A 120.2 . . ? O4 C58 C59 117.8(7) . . ? O4 C58 Ir2 121.1(6) . . ? C59 C58 Ir2 121.1(6) . . ? C60 C59 C64 120.7(8) . . ? C60 C59 C58 117.1(7) . . ? C64 C59 C58 122.3(8) . . ? C59 C60 C61 119.0(8) . . ? C59 C60 P4 114.5(6) . . ? C61 C60 P4 126.4(7) . . ? C62 C61 C60 120.0(9) . . ? C62 C61 H61A 120.0 . . ? C60 C61 H61A 120.0 . . ? C63 C62 C61 120.5(9) . . ? C63 C62 H62A 119.8 . . ? C61 C62 H62A 119.8 . . ? C62 C63 C64 120.3(9) . . ? C62 C63 H63A 119.9 . . ? C64 C63 H63A 119.9 . . ? C63 C64 C59 119.6(9) . . ? C63 C64 H64A 120.2 . . ? C59 C64 H64A 120.2 . . ? C66 C65 C70 118.7(8) . . ? C66 C65 P4 119.2(7) . . ? C70 C65 P4 122.2(7) . . ? C65 C66 C67 120.0(9) . . ? C65 C66 H66A 120.0 . . ? C67 C66 H66A 120.0 . . ? C68 C67 C66 119.8(10) . . ? C68 C67 H67A 120.1 . . ? C66 C67 H67A 120.1 . . ? C67 C68 C69 120.9(10) . . ? C67 C68 H68A 119.6 . . ? C69 C68 H68A 119.6 . . ? C70 C69 C68 121.0(10) . . ? C70 C69 H69A 119.5 . . ? C68 C69 H69A 119.5 . . ? C69 C70 C65 119.6(10) . . ? C69 C70 H70A 120.2 . . ? C65 C70 H70A 120.2 . . ? C76 C71 C72 119.0(8) . . ? C76 C71 P4 120.4(7) . . ? C72 C71 P4 120.5(7) . . ? C73 C72 C71 120.2(9) . . ? C73 C72 H72A 119.9 . . ? C71 C72 H72A 119.9 . . ? C72 C73 C74 120.2(10) . . ? C72 C73 H73A 119.9 . . ? C74 C73 H73A 119.9 . . ? C75 C74 C73 119.7(10) . . ? C75 C74 H74A 120.1 . . ? C73 C74 H74A 120.1 . . ? C74 C75 C76 120.0(10) . . ? C74 C75 H75A 120.0 . . ? C76 C75 H75A 120.0 . . ? C71 C76 C75 120.8(9) . . ? C71 C76 H76A 119.6 . . ? C75 C76 H76A 119.6 . . ? O7 Cl1 O5 109.4(7) . . ? O7 Cl1 O6 110.1(7) . . ? O5 Cl1 O6 111.7(7) . . ? O7 Cl1 O8 105.4(6) . . ? O5 Cl1 O8 107.4(6) . . ? O6 Cl1 O8 112.6(7) . . ? Cl4 C77 Cl2 110.2(7) . . ? Cl4 C77 Cl3 110.2(7) . . ? Cl2 C77 Cl3 108.5(7) . . ? Cl4 C77 H77A 109.3 . . ? Cl2 C77 H77A 109.3 . . ? Cl3 C77 H77A 109.3 . . ? 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 C1 Ir1 Ir2 C39 174.7(3) . . . . ? C20 Ir1 Ir2 C39 -106.4(4) . . . . ? O4 Ir1 Ir2 C39 74.7(3) . . . . ? P1 Ir1 Ir2 C39 132.0(2) . . . . ? P2 Ir1 Ir2 C39 -12.9(2) . . . . ? C1 Ir1 Ir2 C58 96.9(3) . . . . ? C20 Ir1 Ir2 C58 175.8(4) . . . . ? O4 Ir1 Ir2 C58 -3.1(3) . . . . ? P1 Ir1 Ir2 C58 54.2(3) . . . . ? P2 Ir1 Ir2 C58 -90.7(3) . . . . ? C1 Ir1 Ir2 O1 -4.0(3) . . . . ? C20 Ir1 Ir2 O1 74.9(3) . . . . ? O4 Ir1 Ir2 O1 -104.0(2) . . . . ? P1 Ir1 Ir2 O1 -46.72(17) . . . . ? P2 Ir1 Ir2 O1 168.38(15) . . . . ? C1 Ir1 Ir2 P4 63.2(2) . . . . ? C20 Ir1 Ir2 P4 142.1(3) . . . . ? O4 Ir1 Ir2 P4 -36.77(18) . . . . ? P1 Ir1 Ir2 P4 20.47(13) . . . . ? P2 Ir1 Ir2 P4 -124.42(10) . . . . ? C1 Ir1 Ir2 P3 -95.0(2) . . . . ? C20 Ir1 Ir2 P3 -16.1(3) . . . . ? O4 Ir1 Ir2 P3 165.02(17) . . . . ? P1 Ir1 Ir2 P3 -137.74(10) . . . . ? P2 Ir1 Ir2 P3 77.37(8) . . . . ? C20 Ir1 C1 O1 -112.8(6) . . . . ? O4 Ir1 C1 O1 71.6(6) . . . . ? P1 Ir1 C1 O1 160.7(6) . . . . ? P2 Ir1 C1 O1 -63.3(19) . . . . ? Ir2 Ir1 C1 O1 7.5(5) . . . . ? C20 Ir1 C1 C2 66.3(6) . . . . ? O4 Ir1 C1 C2 -109.3(6) . . . . ? P1 Ir1 C1 C2 -20.3(6) . . . . ? P2 Ir1 C1 C2 115.8(15) . . . . ? Ir2 Ir1 C1 C2 -173.4(7) . . . . ? C2 C1 O1 Ir2 171.4(5) . . . . ? Ir1 C1 O1 Ir2 -9.5(6) . . . . ? C39 Ir2 O1 C1 -1.1(17) . . . . ? C58 Ir2 O1 C1 -57.1(5) . . . . ? P4 Ir2 O1 C1 -138.7(4) . . . . ? P3 Ir2 O1 C1 120.4(4) . . . . ? Ir1 Ir2 O1 C1 6.2(4) . . . . ? C1 Ir1 P1 C3 18.9(3) . . . . ? C20 Ir1 P1 C3 -73.0(4) . . . . ? O4 Ir1 P1 C3 108.6(3) . . . . ? P2 Ir1 P1 C3 -155.7(3) . . . . ? Ir2 Ir1 P1 C3 58.4(3) . . . . ? C1 Ir1 P1 C8 137.2(4) . . . . ? C20 Ir1 P1 C8 45.3(4) . . . . ? O4 Ir1 P1 C8 -133.1(4) . . . . ? P2 Ir1 P1 C8 -37.3(4) . . . . ? Ir2 Ir1 P1 C8 176.8(3) . . . . ? C1 Ir1 P1 C14 -93.8(4) . . . . ? C20 Ir1 P1 C14 174.3(4) . . . . ? O4 Ir1 P1 C14 -4.1(4) . . . . ? P2 Ir1 P1 C14 91.6(3) . . . . ? Ir2 Ir1 P1 C14 -54.3(3) . . . . ? O1 C1 C2 C3 -167.8(7) . . . . ? Ir1 C1 C2 C3 13.1(10) . . . . ? O1 C1 C2 C7 12.5(12) . . . . ? Ir1 C1 C2 C7 -166.6(7) . . . . ? C1 Ir1 P2 C27 47.2(17) . . . . ? C20 Ir1 P2 C27 97.0(4) . . . . ? O4 Ir1 P2 C27 -87.5(3) . . . . ? P1 Ir1 P2 C27 -178.0(3) . . . . ? Ir2 Ir1 P2 C27 -21.0(3) . . . . ? C1 Ir1 P2 C22 -64.3(16) . . . . ? C20 Ir1 P2 C22 -14.5(3) . . . . ? O4 Ir1 P2 C22 161.0(3) . . . . ? P1 Ir1 P2 C22 70.5(3) . . . . ? Ir2 Ir1 P2 C22 -132.5(3) . . . . ? C1 Ir1 P2 C33 176.8(16) . . . . ? C20 Ir1 P2 C33 -133.3(4) . . . . ? O4 Ir1 P2 C33 42.2(3) . . . . ? P1 Ir1 P2 C33 -48.3(3) . . . . ? Ir2 Ir1 P2 C33 108.7(3) . . . . ? C7 C2 C3 C4 2.8(12) . . . . ? C1 C2 C3 C4 -176.9(7) . . . . ? C7 C2 C3 P1 -173.6(6) . . . . ? C1 C2 C3 P1 6.7(9) . . . . ? C8 P1 C3 C2 -150.8(6) . . . . ? C14 P1 C3 C2 98.2(6) . . . . ? Ir1 P1 C3 C2 -19.2(6) . . . . ? C8 P1 C3 C4 33.3(9) . . . . ? C14 P1 C3 C4 -77.7(8) . . . . ? Ir1 P1 C3 C4 164.9(7) . . . . ? C39 Ir2 P3 C41 -10.1(4) . . . . ? C58 Ir2 P3 C41 -14.7(13) . . . . ? O1 Ir2 P3 C41 178.3(3) . . . . ? P4 Ir2 P3 C41 79.7(3) . . . . ? Ir1 Ir2 P3 C41 -113.8(3) . . . . ? C39 Ir2 P3 C46 -126.8(4) . . . . ? C58 Ir2 P3 C46 -131.4(13) . . . . ? O1 Ir2 P3 C46 61.6(4) . . . . ? P4 Ir2 P3 C46 -37.0(3) . . . . ? Ir1 Ir2 P3 C46 129.5(3) . . . . ? C39 Ir2 P3 C52 104.7(4) . . . . ? C58 Ir2 P3 C52 100.1(13) . . . . ? O1 Ir2 P3 C52 -66.9(3) . . . . ? P4 Ir2 P3 C52 -165.5(3) . . . . ? Ir1 Ir2 P3 C52 1.0(3) . . . . ? C2 C3 C4 C5 -0.5(13) . . . . ? P1 C3 C4 C5 175.2(7) . . . . ? C1 Ir1 O4 C58 -61.0(6) . . . . ? C20 Ir1 O4 C58 -163(3) . . . . ? P1 Ir1 O4 C58 -141.7(5) . . . . ? P2 Ir1 O4 C58 113.6(5) . . . . ? Ir2 Ir1 O4 C58 4.8(5) . . . . ? C39 Ir2 P4 C71 172.5(4) . . . . ? C58 Ir2 P4 C71 -102.0(4) . . . . ? O1 Ir2 P4 C71 -14.1(3) . . . . ? P3 Ir2 P4 C71 89.0(3) . . . . ? Ir1 Ir2 P4 C71 -71.4(3) . . . . ? C39 Ir2 P4 C65 43.2(4) . . . . ? C58 Ir2 P4 C65 128.7(4) . . . . ? O1 Ir2 P4 C65 -143.4(4) . . . . ? P3 Ir2 P4 C65 -40.3(4) . . . . ? Ir1 Ir2 P4 C65 159.3(3) . . . . ? C39 Ir2 P4 C60 -72.0(3) . . . . ? C58 Ir2 P4 C60 13.5(4) . . . . ? O1 Ir2 P4 C60 101.4(3) . . . . ? P3 Ir2 P4 C60 -155.5(3) . . . . ? Ir1 Ir2 P4 C60 44.1(3) . . . . ? C3 C4 C5 C6 -1.3(15) . . . . ? C4 C5 C6 C7 1.0(15) . . . . ? C5 C6 C7 C2 1.3(15) . . . . ? C3 C2 C7 C6 -3.2(13) . . . . ? C1 C2 C7 C6 176.5(8) . . . . ? C3 P1 C8 C13 -132.6(7) . . . . ? C14 P1 C8 C13 -21.3(8) . . . . ? Ir1 P1 C8 C13 110.3(7) . . . . ? C3 P1 C8 C9 48.7(8) . . . . ? C14 P1 C8 C9 160.0(7) . . . . ? Ir1 P1 C8 C9 -68.3(8) . . . . ? C13 C8 C9 C10 -0.5(13) . . . . ? P1 C8 C9 C10 178.3(7) . . . . ? C8 C9 C10 C11 3.6(15) . . . . ? C9 C10 C11 C12 -4.3(16) . . . . ? C10 C11 C12 C13 2.0(16) . . . . ? C9 C8 C13 C12 -1.8(13) . . . . ? P1 C8 C13 C12 179.5(7) . . . . ? C11 C12 C13 C8 1.1(15) . . . . ? C3 P1 C14 C19 -173.0(7) . . . . ? C8 P1 C14 C19 76.2(7) . . . . ? Ir1 P1 C14 C19 -62.4(7) . . . . ? C3 P1 C14 C15 4.7(8) . . . . ? C8 P1 C14 C15 -106.1(7) . . . . ? Ir1 P1 C14 C15 115.4(6) . . . . ? C19 C14 C15 C16 -0.8(13) . . . . ? P1 C14 C15 C16 -178.6(7) . . . . ? C14 C15 C16 C17 0.1(15) . . . . ? C15 C16 C17 C18 0.8(17) . . . . ? C16 C17 C18 C19 -0.8(16) . . . . ? C15 C14 C19 C18 0.8(13) . . . . ? P1 C14 C19 C18 178.5(7) . . . . ? C17 C18 C19 C14 0.0(15) . . . . ? C1 Ir1 C20 O2 2.4(7) . . . . ? O4 Ir1 C20 O2 104(4) . . . . ? P1 Ir1 C20 O2 82.9(7) . . . . ? P2 Ir1 C20 O2 -171.9(7) . . . . ? Ir2 Ir1 C20 O2 -63.0(7) . . . . ? C1 Ir1 C20 C21 -171.2(6) . . . . ? O4 Ir1 C20 C21 -70(4) . . . . ? P1 Ir1 C20 C21 -90.7(5) . . . . ? P2 Ir1 C20 C21 14.6(5) . . . . ? Ir2 Ir1 C20 C21 123.4(5) . . . . ? O2 C20 C21 C26 -6.4(11) . . . . ? Ir1 C20 C21 C26 167.7(6) . . . . ? O2 C20 C21 C22 176.4(7) . . . . ? Ir1 C20 C21 C22 -9.4(9) . . . . ? C26 C21 C22 C23 2.6(12) . . . . ? C20 C21 C22 C23 179.9(7) . . . . ? C26 C21 C22 P2 177.4(6) . . . . ? C20 C21 C22 P2 -5.3(10) . . . . ? C27 P2 C22 C23 64.2(8) . . . . ? C33 P2 C22 C23 -47.8(8) . . . . ? Ir1 P2 C22 C23 -171.1(7) . . . . ? C27 P2 C22 C21 -110.4(6) . . . . ? C33 P2 C22 C21 137.6(6) . . . . ? Ir1 P2 C22 C21 14.2(6) . . . . ? C21 C22 C23 C24 -3.5(13) . . . . ? P2 C22 C23 C24 -177.8(7) . . . . ? C22 C23 C24 C25 2.9(14) . . . . ? C23 C24 C25 C26 -1.4(15) . . . . ? C24 C25 C26 C21 0.5(14) . . . . ? C22 C21 C26 C25 -1.1(13) . . . . ? C20 C21 C26 C25 -178.3(8) . . . . ? C22 P2 C27 C28 -107.4(8) . . . . ? C33 P2 C27 C28 7.7(9) . . . . ? Ir1 P2 C27 C28 141.9(7) . . . . ? C22 P2 C27 C32 71.2(8) . . . . ? C33 P2 C27 C32 -173.6(7) . . . . ? Ir1 P2 C27 C32 -39.4(8) . . . . ? C32 C27 C28 C29 0.3(15) . . . . ? P2 C27 C28 C29 179.0(9) . . . . ? C27 C28 C29 C30 0.8(18) . . . . ? C28 C29 C30 C31 -1(2) . . . . ? C29 C30 C31 C32 0.5(18) . . . . ? C28 C27 C32 C31 -1.0(15) . . . . ? P2 C27 C32 C31 -179.7(8) . . . . ? C30 C31 C32 C27 0.6(16) . . . . ? C27 P2 C33 C34 -129.4(8) . . . . ? C22 P2 C33 C34 -19.5(9) . . . . ? Ir1 P2 C33 C34 94.3(8) . . . . ? C27 P2 C33 C38 60.3(8) . . . . ? C22 P2 C33 C38 170.2(7) . . . . ? Ir1 P2 C33 C38 -76.0(8) . . . . ? C38 C33 C34 C35 -0.1(14) . . . . ? P2 C33 C34 C35 -170.4(8) . . . . ? C33 C34 C35 C36 -1.7(17) . . . . ? C34 C35 C36 C37 1.2(19) . . . . ? C35 C36 C37 C38 1(2) . . . . ? C58 Ir2 C39 O3 10.5(7) . . . . ? O1 Ir2 C39 O3 -46(2) . . . . ? P4 Ir2 C39 O3 92.2(7) . . . . ? P3 Ir2 C39 O3 -168.7(8) . . . . ? Ir1 Ir2 C39 O3 -52.6(8) . . . . ? C58 Ir2 C39 C40 -170.4(7) . . . . ? O1 Ir2 C39 C40 133.4(13) . . . . ? P4 Ir2 C39 C40 -88.7(6) . . . . ? P3 Ir2 C39 C40 10.5(6) . . . . ? Ir1 Ir2 C39 C40 126.5(6) . . . . ? C34 C33 C38 C37 2.4(15) . . . . ? P2 C33 C38 C37 173.1(9) . . . . ? C36 C37 C38 C33 -2.9(18) . . . . ? O3 C39 C40 C41 172.0(8) . . . . ? Ir2 C39 C40 C41 -7.1(11) . . . . ? O3 C39 C40 C45 -9.8(13) . . . . ? Ir2 C39 C40 C45 171.0(7) . . . . ? C45 C40 C41 C42 -1.1(13) . . . . ? C39 C40 C41 C42 177.0(8) . . . . ? C45 C40 C41 P3 178.4(7) . . . . ? C39 C40 C41 P3 -3.5(11) . . . . ? C46 P3 C41 C40 136.8(6) . . . . ? C52 P3 C41 C40 -115.4(7) . . . . ? Ir2 P3 C41 C40 9.9(7) . . . . ? C46 P3 C41 C42 -43.7(8) . . . . ? C52 P3 C41 C42 64.1(8) . . . . ? Ir2 P3 C41 C42 -170.6(7) . . . . ? C40 C41 C42 C43 0.6(14) . . . . ? P3 C41 C42 C43 -178.9(8) . . . . ? C41 C42 C43 C44 -0.8(17) . . . . ? C42 C43 C44 C45 1.6(19) . . . . ? C43 C44 C45 C40 -2.2(18) . . . . ? C41 C40 C45 C44 2.0(15) . . . . ? C39 C40 C45 C44 -176.3(10) . . . . ? C41 P3 C46 C51 -24.8(8) . . . . ? C52 P3 C46 C51 -135.3(8) . . . . ? Ir2 P3 C46 C51 88.5(8) . . . . ? C41 P3 C46 C47 157.4(7) . . . . ? C52 P3 C46 C47 46.9(8) . . . . ? Ir2 P3 C46 C47 -89.3(7) . . . . ? C51 C46 C47 C48 -1.5(14) . . . . ? P3 C46 C47 C48 176.4(8) . . . . ? C46 C47 C48 C49 -2.1(17) . . . . ? C47 C48 C49 C50 4.7(18) . . . . ? C48 C49 C50 C51 -3.8(19) . . . . ? C47 C46 C51 C50 2.5(14) . . . . ? P3 C46 C51 C50 -175.4(8) . . . . ? C49 C50 C51 C46 0.2(18) . . . . ? C41 P3 C52 C53 139.4(7) . . . . ? C46 P3 C52 C53 -109.3(7) . . . . ? Ir2 P3 C52 C53 27.4(8) . . . . ? C41 P3 C52 C57 -40.2(9) . . . . ? C46 P3 C52 C57 71.2(8) . . . . ? Ir2 P3 C52 C57 -152.1(7) . . . . ? C57 C52 C53 C54 0.4(14) . . . . ? P3 C52 C53 C54 -179.1(8) . . . . ? C52 C53 C54 C55 0.1(15) . . . . ? C53 C54 C55 C56 -1.0(17) . . . . ? C54 C55 C56 C57 1.3(17) . . . . ? C55 C56 C57 C52 -0.8(17) . . . . ? C53 C52 C57 C56 -0.1(15) . . . . ? P3 C52 C57 C56 179.4(8) . . . . ? Ir1 O4 C58 C59 172.7(6) . . . . ? Ir1 O4 C58 Ir2 -7.4(8) . . . . ? C39 Ir2 C58 O4 -103.1(7) . . . . ? O1 Ir2 C58 O4 68.7(7) . . . . ? P4 Ir2 C58 O4 165.4(7) . . . . ? P3 Ir2 C58 O4 -98.5(13) . . . . ? Ir1 Ir2 C58 O4 5.7(6) . . . . ? C39 Ir2 C58 C59 76.7(7) . . . . ? O1 Ir2 C58 C59 -111.4(6) . . . . ? P4 Ir2 C58 C59 -14.7(6) . . . . ? P3 Ir2 C58 C59 81.3(15) . . . . ? Ir1 Ir2 C58 C59 -174.4(7) . . . . ? O4 C58 C59 C60 -169.9(8) . . . . ? Ir2 C58 C59 C60 10.2(10) . . . . ? O4 C58 C59 C64 11.2(12) . . . . ? Ir2 C58 C59 C64 -168.6(7) . . . . ? C64 C59 C60 C61 1.4(12) . . . . ? C58 C59 C60 C61 -177.5(7) . . . . ? C64 C59 C60 P4 -177.3(7) . . . . ? C58 C59 C60 P4 3.8(10) . . . . ? C71 P4 C60 C59 107.5(6) . . . . ? C65 P4 C60 C59 -142.3(6) . . . . ? Ir2 P4 C60 C59 -13.1(7) . . . . ? C71 P4 C60 C61 -71.1(8) . . . . ? C65 P4 C60 C61 39.1(8) . . . . ? Ir2 P4 C60 C61 168.3(7) . . . . ? C59 C60 C61 C62 -1.9(13) . . . . ? P4 C60 C61 C62 176.7(7) . . . . ? C60 C61 C62 C63 1.7(14) . . . . ? C61 C62 C63 C64 -1.2(15) . . . . ? C62 C63 C64 C59 0.7(14) . . . . ? C60 C59 C64 C63 -0.8(13) . . . . ? C58 C59 C64 C63 178.0(8) . . . . ? C71 P4 C65 C66 163.9(7) . . . . ? C60 P4 C65 C66 52.1(7) . . . . ? Ir2 P4 C65 C66 -62.9(7) . . . . ? C71 P4 C65 C70 -16.4(8) . . . . ? C60 P4 C65 C70 -128.2(7) . . . . ? Ir2 P4 C65 C70 116.7(7) . . . . ? C70 C65 C66 C67 1.0(13) . . . . ? P4 C65 C66 C67 -179.3(7) . . . . ? C65 C66 C67 C68 -1.5(15) . . . . ? C66 C67 C68 C69 2.0(17) . . . . ? C67 C68 C69 C70 -1.9(17) . . . . ? C68 C69 C70 C65 1.4(15) . . . . ? C66 C65 C70 C69 -0.9(13) . . . . ? P4 C65 C70 C69 179.4(7) . . . . ? C65 P4 C71 C76 -75.1(8) . . . . ? C60 P4 C71 C76 33.8(8) . . . . ? Ir2 P4 C71 C76 146.8(7) . . . . ? C65 P4 C71 C72 102.1(7) . . . . ? C60 P4 C71 C72 -148.9(7) . . . . ? Ir2 P4 C71 C72 -35.9(8) . . . . ? C76 C71 C72 C73 -0.9(13) . . . . ? P4 C71 C72 C73 -178.2(7) . . . . ? C71 C72 C73 C74 -0.1(15) . . . . ? C72 C73 C74 C75 1.7(17) . . . . ? C73 C74 C75 C76 -2.3(17) . . . . ? C72 C71 C76 C75 0.3(15) . . . . ? P4 C71 C76 C75 177.6(8) . . . . ? C74 C75 C76 C71 1.3(17) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.978 _refine_diff_density_min -1.949 _refine_diff_density_rms 0.171 #============================================================================ data_4 _database_code_depnum_ccdc_archive 'CCDC 679482' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H44 Ir O2 P3, C H2 Cl2' _chemical_formula_sum 'C57 H46 Cl2 Ir O2 P3' _chemical_formula_weight 1118.95 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' O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 '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 11.1432(11) _cell_length_b 12.9638(13) _cell_length_c 17.8304(17) _cell_angle_alpha 84.247(2) _cell_angle_beta 74.945(2) _cell_angle_gamma 76.930(2) _cell_volume 2420.5(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 3.010 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18421 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8228 _reflns_number_gt 7082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0688P)^2^+4.0967P] 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 8228 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1169 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.008 _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 0.51374(2) 0.245153(16) 0.688345(13) 0.02791(10) Uani 1 1 d . . . H1 H 0.4499 0.3472 0.6159 0.050 Uiso 1 1 d . . . P1 P 0.59639(15) 0.08717(12) 0.75117(9) 0.0308(3) Uani 1 1 d . . . P2 P 0.69558(14) 0.27905(11) 0.59515(9) 0.0279(3) Uani 1 1 d . . . P3 P 0.47717(17) 0.37844(12) 0.77941(10) 0.0365(4) Uani 1 1 d . . . O1 O 0.2358(4) 0.2652(4) 0.7538(3) 0.0495(12) Uani 1 1 d . . . O2 O 0.4043(4) 0.1189(4) 0.6056(3) 0.0426(11) Uani 1 1 d . . . C1 C 0.3406(6) 0.2079(5) 0.7459(4) 0.0344(14) Uani 1 1 d . . . C2 C 0.3424(6) 0.0946(5) 0.7797(4) 0.0347(14) Uani 1 1 d . . . C3 C 0.4557(6) 0.0294(5) 0.7875(4) 0.0383(15) Uani 1 1 d . . . C4 C 0.4603(7) -0.0760(6) 0.8151(4) 0.0468(17) Uani 1 1 d . . . H4 H 0.5371 -0.1200 0.8190 0.056 Uiso 1 1 calc R . . C5 C 0.3494(8) -0.1138(6) 0.8365(5) 0.056(2) Uani 1 1 d . . . H5 H 0.3512 -0.1838 0.8548 0.068 Uiso 1 1 calc R . . C6 C 0.2370(8) -0.0486(7) 0.8307(5) 0.058(2) Uani 1 1 d . . . H6 H 0.1629 -0.0750 0.8459 0.069 Uiso 1 1 calc R . . C7 C 0.2303(7) 0.0554(6) 0.8030(4) 0.0477(17) Uani 1 1 d . . . H7 H 0.1527 0.0987 0.7999 0.057 Uiso 1 1 calc R . . C8 C 0.6693(6) 0.0883(5) 0.8321(4) 0.0379(15) Uani 1 1 d . . . C9 C 0.6288(8) 0.0422(8) 0.9057(5) 0.065(2) Uani 1 1 d . . . H9 H 0.5579 0.0115 0.9174 0.077 Uiso 1 1 calc R . . C10 C 0.6954(10) 0.0426(9) 0.9617(5) 0.085(3) Uani 1 1 d . . . H10 H 0.6698 0.0107 1.0106 0.101 Uiso 1 1 calc R . . C11 C 0.7974(9) 0.0891(8) 0.9455(5) 0.076(3) Uani 1 1 d . . . H11 H 0.8400 0.0907 0.9837 0.091 Uiso 1 1 calc R . . C12 C 0.8376(8) 0.1339(7) 0.8727(5) 0.067(2) Uani 1 1 d . . . H12 H 0.9085 0.1644 0.8614 0.080 Uiso 1 1 calc R . . C13 C 0.7738(7) 0.1337(6) 0.8169(5) 0.0524(19) Uani 1 1 d . . . H13 H 0.8015 0.1646 0.7679 0.063 Uiso 1 1 calc R . . C14 C 0.7059(6) -0.0242(4) 0.6959(4) 0.0342(14) Uani 1 1 d . . . C15 C 0.6737(7) -0.0575(5) 0.6342(4) 0.0408(16) Uani 1 1 d . . . H15 H 0.5965 -0.0254 0.6230 0.049 Uiso 1 1 calc R . . C16 C 0.7535(8) -0.1376(6) 0.5888(5) 0.056(2) Uani 1 1 d . . . H16 H 0.7312 -0.1576 0.5464 0.067 Uiso 1 1 calc R . . C17 C 0.8662(8) -0.1881(6) 0.6064(5) 0.061(2) Uani 1 1 d . . . H17 H 0.9193 -0.2433 0.5766 0.074 Uiso 1 1 calc R . . C18 C 0.8996(7) -0.1572(6) 0.6669(5) 0.061(2) Uani 1 1 d . . . H18 H 0.9766 -0.1903 0.6780 0.073 Uiso 1 1 calc R . . C19 C 0.8190(6) -0.0757(5) 0.7129(4) 0.0467(17) Uani 1 1 d . . . H19 H 0.8418 -0.0561 0.7552 0.056 Uiso 1 1 calc R . . C20 C 0.4906(6) 0.1638(4) 0.6010(4) 0.0325(14) Uani 1 1 d . . . C21 C 0.5828(6) 0.1680(4) 0.5208(4) 0.0314(14) Uani 1 1 d . . . C22 C 0.6816(6) 0.2211(4) 0.5093(3) 0.0309(13) Uani 1 1 d . . . C23 C 0.7583(6) 0.2309(5) 0.4347(4) 0.0419(16) Uani 1 1 d . . . H23 H 0.8243 0.2669 0.4264 0.050 Uiso 1 1 calc R . . C24 C 0.7365(7) 0.1871(6) 0.3724(4) 0.0508(18) Uani 1 1 d . . . H24 H 0.7865 0.1953 0.3224 0.061 Uiso 1 1 calc R . . C25 C 0.6405(7) 0.1315(5) 0.3852(4) 0.0462(17) Uani 1 1 d . . . H25 H 0.6277 0.1002 0.3439 0.055 Uiso 1 1 calc R . . C26 C 0.5634(7) 0.1219(5) 0.4586(4) 0.0397(15) Uani 1 1 d . . . H26 H 0.4985 0.0848 0.4668 0.048 Uiso 1 1 calc R . . C27 C 0.8580(6) 0.2184(5) 0.6023(4) 0.0343(14) Uani 1 1 d . . . C28 C 0.9120(6) 0.1157(5) 0.5807(4) 0.0367(14) Uani 1 1 d . . . H28 H 0.8685 0.0788 0.5584 0.044 Uiso 1 1 calc R . . C29 C 1.0318(7) 0.0667(6) 0.5921(5) 0.0510(19) Uani 1 1 d . . . H29 H 1.0667 -0.0031 0.5783 0.061 Uiso 1 1 calc R . . C30 C 1.0976(7) 0.1205(6) 0.6233(5) 0.054(2) Uani 1 1 d . . . H30 H 1.1773 0.0876 0.6306 0.065 Uiso 1 1 calc R . . C31 C 1.0456(7) 0.2251(7) 0.6443(5) 0.058(2) Uani 1 1 d . . . H31 H 1.0904 0.2632 0.6646 0.070 Uiso 1 1 calc R . . C32 C 0.9266(7) 0.2705(6) 0.6341(5) 0.0494(18) Uani 1 1 d . . . H32 H 0.8908 0.3395 0.6495 0.059 Uiso 1 1 calc R . . C33 C 0.7090(6) 0.4145(4) 0.5560(4) 0.0315(13) Uani 1 1 d . . . C34 C 0.6017(7) 0.4930(5) 0.5662(4) 0.0410(16) Uani 1 1 d . . . H34 H 0.5251 0.4788 0.5965 0.049 Uiso 1 1 calc R . . C35 C 0.6054(8) 0.5941(5) 0.5316(5) 0.055(2) Uani 1 1 d . . . H35 H 0.5316 0.6465 0.5388 0.067 Uiso 1 1 calc R . . C36 C 0.7177(8) 0.6163(6) 0.4870(5) 0.056(2) Uani 1 1 d . . . H36 H 0.7199 0.6834 0.4634 0.067 Uiso 1 1 calc R . . C37 C 0.8275(8) 0.5386(5) 0.4773(5) 0.0521(19) Uani 1 1 d . . . H37 H 0.9041 0.5536 0.4477 0.063 Uiso 1 1 calc R . . C38 C 0.8234(7) 0.4382(5) 0.5116(4) 0.0461(17) Uani 1 1 d . . . H38 H 0.8975 0.3861 0.5049 0.055 Uiso 1 1 calc R . . C39 C 0.5883(8) 0.4693(5) 0.7621(4) 0.0464(17) Uani 1 1 d . . . C40 C 0.5537(10) 0.5751(6) 0.7417(5) 0.065(2) Uani 1 1 d . . . H40 H 0.4713 0.6038 0.7373 0.078 Uiso 1 1 calc R . . C41 C 0.6448(14) 0.6398(8) 0.7275(6) 0.091(4) Uani 1 1 d . . . H41 H 0.6231 0.7109 0.7124 0.109 Uiso 1 1 calc R . . C42 C 0.7660(13) 0.5971(10) 0.7362(7) 0.096(4) Uani 1 1 d . . . H42 H 0.8252 0.6400 0.7279 0.115 Uiso 1 1 calc R . . C43 C 0.7984(11) 0.4961(9) 0.7561(6) 0.085(3) Uani 1 1 d . . . H43 H 0.8803 0.4683 0.7616 0.102 Uiso 1 1 calc R . . C44 C 0.7113(8) 0.4301(7) 0.7690(5) 0.063(2) Uani 1 1 d . . . H44 H 0.7363 0.3588 0.7824 0.076 Uiso 1 1 calc R . . C45 C 0.4622(7) 0.3396(5) 0.8836(4) 0.0457(17) Uani 1 1 d . . . C46 C 0.3759(9) 0.2780(7) 0.9186(5) 0.066(2) Uani 1 1 d . . . H46 H 0.3332 0.2524 0.8885 0.079 Uiso 1 1 calc R . . C47 C 0.3510(11) 0.2533(8) 0.9978(5) 0.085(3) Uani 1 1 d . . . H47 H 0.2925 0.2112 1.0201 0.102 Uiso 1 1 calc R . . C48 C 0.4118(11) 0.2902(7) 1.0428(5) 0.076(3) Uani 1 1 d . . . H48 H 0.3928 0.2755 1.0962 0.091 Uiso 1 1 calc R . . C49 C 0.4989(13) 0.3477(10) 1.0105(6) 0.099(4) Uani 1 1 d . . . H49 H 0.5421 0.3715 1.0412 0.119 Uiso 1 1 calc R . . C50 C 0.5257(10) 0.3725(8) 0.9300(5) 0.075(3) Uani 1 1 d . . . H50 H 0.5874 0.4118 0.9079 0.090 Uiso 1 1 calc R . . C51 C 0.3249(7) 0.4747(5) 0.7860(4) 0.0430(16) Uani 1 1 d . . . C52 C 0.2592(8) 0.4907(6) 0.7288(5) 0.056(2) Uani 1 1 d . . . H52 H 0.2898 0.4492 0.6855 0.067 Uiso 1 1 calc R . . C53 C 0.1489(8) 0.5671(6) 0.7341(5) 0.067(2) Uani 1 1 d . . . H53 H 0.1068 0.5764 0.6945 0.080 Uiso 1 1 calc R . . C54 C 0.1012(10) 0.6290(7) 0.7970(6) 0.087(3) Uani 1 1 d . . . H54 H 0.0268 0.6802 0.8005 0.104 Uiso 1 1 calc R . . C55 C 0.1644(11) 0.6144(8) 0.8549(6) 0.091(4) Uani 1 1 d . . . H55 H 0.1324 0.6564 0.8979 0.109 Uiso 1 1 calc R . . C56 C 0.2748(9) 0.5387(6) 0.8505(5) 0.072(3) Uani 1 1 d . . . H56 H 0.3162 0.5299 0.8905 0.087 Uiso 1 1 calc R . . C57 C -0.0354(17) 0.6471(14) 0.0808(11) 0.164(7) Uiso 1 1 d . . . H57A H -0.0944 0.6111 0.0679 0.197 Uiso 1 1 calc R . . H57B H -0.0648 0.6599 0.1359 0.197 Uiso 1 1 calc R . . Cl2 Cl 0.1102(6) 0.5608(5) 0.0663(4) 0.194(2) Uiso 1 1 d . . . Cl1 Cl -0.0459(5) 0.7637(4) 0.0330(3) 0.1476(15) Uiso 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 0.02665(14) 0.02819(13) 0.03045(15) -0.00353(9) -0.00802(10) -0.00671(9) P1 0.0304(8) 0.0327(7) 0.0314(9) 0.0016(6) -0.0095(7) -0.0099(6) P2 0.0264(8) 0.0270(7) 0.0326(8) -0.0020(6) -0.0099(7) -0.0069(6) P3 0.0437(10) 0.0338(8) 0.0329(9) -0.0055(6) -0.0084(8) -0.0093(7) O1 0.030(3) 0.052(3) 0.064(3) -0.009(2) -0.007(2) -0.007(2) O2 0.040(3) 0.051(3) 0.046(3) -0.008(2) -0.010(2) -0.027(2) C1 0.031(3) 0.038(3) 0.035(4) -0.006(3) -0.008(3) -0.007(3) C2 0.031(3) 0.048(3) 0.028(3) -0.005(3) -0.004(3) -0.017(3) C3 0.037(4) 0.052(4) 0.029(3) -0.001(3) -0.005(3) -0.018(3) C4 0.052(4) 0.050(4) 0.042(4) 0.008(3) -0.013(3) -0.020(3) C5 0.066(5) 0.054(4) 0.053(5) 0.014(4) -0.010(4) -0.031(4) C6 0.057(5) 0.076(5) 0.047(5) 0.008(4) -0.005(4) -0.041(4) C7 0.038(4) 0.063(4) 0.046(4) -0.004(3) -0.004(3) -0.026(3) C8 0.036(4) 0.045(3) 0.039(4) 0.000(3) -0.018(3) -0.010(3) C9 0.060(5) 0.106(7) 0.041(5) 0.010(4) -0.019(4) -0.042(5) C10 0.089(7) 0.139(9) 0.039(5) 0.020(5) -0.024(5) -0.052(7) C11 0.081(7) 0.117(8) 0.050(5) 0.006(5) -0.036(5) -0.044(6) C12 0.053(5) 0.100(7) 0.067(6) -0.004(5) -0.028(4) -0.041(5) C13 0.055(5) 0.064(4) 0.051(5) 0.008(4) -0.022(4) -0.032(4) C14 0.033(3) 0.031(3) 0.037(4) 0.003(3) -0.005(3) -0.009(3) C15 0.045(4) 0.034(3) 0.046(4) -0.003(3) -0.017(3) -0.005(3) C16 0.059(5) 0.050(4) 0.057(5) -0.013(3) -0.006(4) -0.012(4) C17 0.050(5) 0.048(4) 0.070(6) -0.013(4) 0.008(4) 0.001(4) C18 0.040(4) 0.054(4) 0.079(6) 0.002(4) -0.010(4) -0.001(3) C19 0.039(4) 0.049(4) 0.052(5) -0.001(3) -0.014(3) -0.005(3) C20 0.031(3) 0.032(3) 0.035(3) -0.001(2) -0.010(3) -0.006(3) C21 0.031(3) 0.025(3) 0.034(3) -0.002(2) -0.007(3) 0.003(2) C22 0.034(3) 0.027(3) 0.029(3) -0.001(2) -0.005(3) -0.003(2) C23 0.036(4) 0.051(4) 0.037(4) -0.005(3) -0.002(3) -0.011(3) C24 0.055(5) 0.060(4) 0.036(4) -0.006(3) -0.005(3) -0.013(4) C25 0.053(4) 0.051(4) 0.037(4) -0.010(3) -0.012(3) -0.011(3) C26 0.049(4) 0.033(3) 0.040(4) -0.004(3) -0.014(3) -0.009(3) C27 0.028(3) 0.039(3) 0.036(4) 0.006(3) -0.007(3) -0.010(3) C28 0.031(3) 0.041(3) 0.039(4) -0.001(3) -0.010(3) -0.009(3) C29 0.038(4) 0.049(4) 0.059(5) 0.004(3) -0.011(4) 0.001(3) C30 0.033(4) 0.071(5) 0.053(5) 0.009(4) -0.014(3) -0.004(4) C31 0.050(5) 0.082(6) 0.054(5) 0.017(4) -0.021(4) -0.035(4) C32 0.047(4) 0.044(4) 0.063(5) 0.009(3) -0.028(4) -0.010(3) C33 0.038(3) 0.029(3) 0.032(3) -0.001(2) -0.013(3) -0.009(2) C34 0.047(4) 0.035(3) 0.040(4) 0.004(3) -0.014(3) -0.007(3) C35 0.062(5) 0.037(4) 0.067(5) 0.004(3) -0.027(4) -0.002(3) C36 0.077(6) 0.038(4) 0.060(5) 0.015(3) -0.026(4) -0.021(4) C37 0.057(5) 0.048(4) 0.063(5) 0.008(3) -0.021(4) -0.032(4) C38 0.043(4) 0.041(3) 0.056(5) 0.006(3) -0.013(3) -0.016(3) C39 0.067(5) 0.045(4) 0.035(4) -0.010(3) -0.010(3) -0.027(3) C40 0.086(6) 0.050(4) 0.062(5) -0.002(4) -0.013(5) -0.025(4) C41 0.145(11) 0.054(5) 0.076(7) -0.003(5) -0.003(7) -0.051(7) C42 0.121(10) 0.090(8) 0.095(9) -0.008(6) -0.012(8) -0.076(8) C43 0.084(7) 0.111(8) 0.079(7) -0.005(6) -0.020(6) -0.062(6) C44 0.057(5) 0.067(5) 0.077(6) -0.010(4) -0.019(5) -0.028(4) C45 0.062(5) 0.038(3) 0.038(4) -0.003(3) -0.013(4) -0.010(3) C46 0.080(6) 0.090(6) 0.038(4) -0.008(4) -0.006(4) -0.044(5) C47 0.116(9) 0.098(7) 0.042(5) 0.007(5) -0.006(5) -0.045(7) C48 0.118(9) 0.076(6) 0.038(5) 0.002(4) -0.026(5) -0.024(6) C49 0.146(11) 0.119(9) 0.059(7) 0.003(6) -0.050(7) -0.057(8) C50 0.111(8) 0.090(6) 0.049(5) 0.004(5) -0.036(5) -0.053(6) C51 0.049(4) 0.041(3) 0.035(4) -0.004(3) -0.009(3) -0.002(3) C52 0.056(5) 0.043(4) 0.059(5) -0.004(3) -0.006(4) -0.001(3) C53 0.064(5) 0.059(5) 0.064(6) -0.001(4) -0.011(4) 0.008(4) C54 0.082(7) 0.065(5) 0.077(7) 0.009(5) 0.009(6) 0.021(5) C55 0.102(8) 0.076(6) 0.064(6) -0.022(5) -0.003(6) 0.030(6) C56 0.086(7) 0.061(5) 0.054(5) -0.020(4) -0.006(5) 0.015(5) _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 C20 2.065(6) . ? Ir C1 2.074(6) . ? Ir P1 2.3495(15) . ? Ir P2 2.3595(16) . ? Ir P3 2.3850(16) . ? Ir H1 1.9059 . ? P1 C8 1.833(7) . ? P1 C3 1.829(7) . ? P1 C14 1.846(6) . ? P2 C22 1.827(6) . ? P2 C27 1.835(6) . ? P2 C33 1.847(6) . ? P3 C39 1.845(7) . ? P3 C51 1.849(7) . ? P3 C45 1.850(7) . ? O1 C1 1.216(7) . ? O2 C20 1.214(7) . ? C1 C2 1.529(8) . ? C2 C3 1.384(9) . ? C2 C7 1.402(9) . ? C3 C4 1.398(9) . ? C4 C5 1.380(11) . ? C4 H4 0.9300 . ? C5 C6 1.365(12) . ? C5 H5 0.9300 . ? C6 C7 1.381(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.375(10) . ? C8 C9 1.394(10) . ? C9 C10 1.391(12) . ? C9 H9 0.9300 . ? C10 C11 1.358(13) . ? C10 H10 0.9300 . ? C11 C12 1.373(12) . ? C11 H11 0.9300 . ? C12 C13 1.366(11) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.376(9) . ? C14 C19 1.380(9) . ? C15 C16 1.379(9) . ? C15 H15 0.9300 . ? C16 C17 1.377(12) . ? C16 H16 0.9300 . ? C17 C18 1.351(12) . ? C17 H17 0.9300 . ? C18 C19 1.400(11) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C21 1.532(8) . ? C21 C22 1.387(9) . ? C21 C26 1.396(9) . ? C22 C23 1.393(9) . ? C23 C24 1.394(10) . ? C23 H23 0.9300 . ? C24 C25 1.381(11) . ? C24 H24 0.9300 . ? C25 C26 1.378(10) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.378(10) . ? C27 C28 1.380(9) . ? C28 C29 1.400(9) . ? C28 H28 0.9300 . ? C29 C30 1.362(11) . ? C29 H29 0.9300 . ? C30 C31 1.396(11) . ? C30 H30 0.9300 . ? C31 C32 1.374(10) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.369(9) . ? C33 C38 1.396(9) . ? C34 C35 1.396(9) . ? C34 H34 0.9300 . ? C35 C36 1.371(12) . ? C35 H35 0.9300 . ? C36 C37 1.382(11) . ? C36 H36 0.9300 . ? C37 C38 1.387(9) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.377(10) . ? C39 C44 1.382(11) . ? C40 C41 1.417(14) . ? C40 H40 0.9300 . ? C41 C42 1.381(16) . ? C41 H41 0.9300 . ? C42 C43 1.315(15) . ? C42 H42 0.9300 . ? C43 C44 1.395(12) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C46 1.373(11) . ? C45 C50 1.370(11) . ? C46 C47 1.385(12) . ? C46 H46 0.9300 . ? C47 C48 1.356(14) . ? C47 H47 0.9300 . ? C48 C49 1.335(15) . ? C48 H48 0.9300 . ? C49 C50 1.407(13) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.378(11) . ? C51 C56 1.404(10) . ? C52 C53 1.381(10) . ? C52 H52 0.9300 . ? C53 C54 1.364(13) . ? C53 H53 0.9300 . ? C54 C55 1.370(15) . ? C54 H54 0.9300 . ? C55 C56 1.379(12) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 Cl1 1.655(17) . ? C57 Cl2 1.723(17) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C20 Ir C1 82.3(2) . . ? C20 Ir P1 92.00(16) . . ? C1 Ir P1 83.23(17) . . ? C20 Ir P2 84.20(18) . . ? C1 Ir P2 165.65(18) . . ? P1 Ir P2 102.08(5) . . ? C20 Ir P3 160.20(17) . . ? C1 Ir P3 89.01(17) . . ? P1 Ir P3 104.64(6) . . ? P2 Ir P3 102.30(6) . . ? C20 Ir H1 72.3 . . ? C1 Ir H1 96.3 . . ? P1 Ir H1 164.2 . . ? P2 Ir H1 74.9 . . ? P3 Ir H1 91.1 . . ? C8 P1 C3 108.2(3) . . ? C8 P1 C14 101.5(3) . . ? C3 P1 C14 99.9(3) . . ? C8 P1 Ir 121.5(2) . . ? C3 P1 Ir 101.7(2) . . ? C14 P1 Ir 121.5(2) . . ? C22 P2 C27 103.5(3) . . ? C22 P2 C33 100.4(3) . . ? C27 P2 C33 102.8(3) . . ? C22 P2 Ir 101.5(2) . . ? C27 P2 Ir 122.9(2) . . ? C33 P2 Ir 121.8(2) . . ? C39 P3 C51 100.5(3) . . ? C39 P3 C45 102.0(3) . . ? C51 P3 C45 99.7(3) . . ? C39 P3 Ir 118.5(2) . . ? C51 P3 Ir 113.5(2) . . ? C45 P3 Ir 119.4(2) . . ? O1 C1 C2 115.4(6) . . ? O1 C1 Ir 127.3(5) . . ? C2 C1 Ir 117.3(4) . . ? C3 C2 C7 119.2(6) . . ? C3 C2 C1 119.9(6) . . ? C7 C2 C1 120.9(6) . . ? C4 C3 C2 120.8(6) . . ? C4 C3 P1 123.7(5) . . ? C2 C3 P1 115.3(5) . . ? C3 C4 C5 119.2(7) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.0(7) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C7 121.9(7) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C6 C7 C2 118.9(7) . . ? C6 C7 H7 120.6 . . ? C2 C7 H7 120.6 . . ? C13 C8 C9 118.9(7) . . ? C13 C8 P1 116.9(5) . . ? C9 C8 P1 124.1(6) . . ? C8 C9 C10 119.3(8) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 120.5(8) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.0(8) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C8 C13 C12 120.9(7) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C19 118.1(6) . . ? C15 C14 P1 118.5(5) . . ? C19 C14 P1 123.4(5) . . ? C14 C15 C16 121.4(7) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 119.8(8) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 119.9(7) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 120.4(7) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C14 C19 C18 120.3(8) . . ? C14 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? O2 C20 C21 116.2(6) . . ? O2 C20 Ir 125.7(5) . . ? C21 C20 Ir 117.9(4) . . ? C22 C21 C26 120.2(6) . . ? C22 C21 C20 120.3(6) . . ? C26 C21 C20 119.5(6) . . ? C21 C22 C23 119.3(6) . . ? C21 C22 P2 115.9(4) . . ? C23 C22 P2 124.8(5) . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 119.7(7) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.4(7) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 120.0(7) . . ? C25 C26 H26 120.0 . . ? C21 C26 H26 120.0 . . ? C32 C27 C28 117.8(6) . . ? C32 C27 P2 121.5(5) . . ? C28 C27 P2 120.5(5) . . ? C27 C28 C29 120.4(7) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C30 C29 C28 120.4(7) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 120.1(7) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 118.3(8) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C31 C32 C27 123.0(7) . . ? C31 C32 H32 118.5 . . ? C27 C32 H32 118.5 . . ? C34 C33 C38 118.6(6) . . ? C34 C33 P2 119.0(5) . . ? C38 C33 P2 122.3(5) . . ? C33 C34 C35 120.9(7) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C36 120.2(7) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C37 C36 C35 119.7(6) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C38 C37 C36 120.0(7) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C33 120.6(7) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C40 C39 C44 118.4(7) . . ? C40 C39 P3 122.4(7) . . ? C44 C39 P3 119.2(6) . . ? C39 C40 C41 119.4(10) . . ? C39 C40 H40 120.3 . . ? C41 C40 H40 120.3 . . ? C40 C41 C42 119.9(9) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 120.1 . . ? C43 C42 C41 120.4(10) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 120.8(11) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C39 C44 C43 121.0(9) . . ? C39 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C46 C45 C50 117.0(7) . . ? C46 C45 P3 117.9(6) . . ? C50 C45 P3 124.9(6) . . ? C45 C46 C47 121.5(9) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C46 C47 C48 120.2(10) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C49 C48 C47 119.9(9) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.2(10) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C45 121.0(9) . . ? C49 C50 H50 119.5 . . ? C45 C50 H50 119.5 . . ? C52 C51 C56 117.3(7) . . ? C52 C51 P3 123.3(5) . . ? C56 C51 P3 119.3(6) . . ? C53 C52 C51 121.5(8) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C54 120.7(9) . . ? C52 C53 H53 119.7 . . ? C54 C53 H53 119.7 . . ? C53 C54 C55 119.0(8) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C56 C55 C54 121.2(9) . . ? C56 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C55 C56 C51 120.3(9) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? Cl1 C57 Cl2 118.7(11) . . ? Cl1 C57 H57A 107.6 . . ? Cl2 C57 H57A 107.6 . . ? Cl1 C57 H57B 107.6 . . ? Cl2 C57 H57B 107.6 . . ? H57A C57 H57B 107.1 . . ? 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 C20 Ir P1 C8 170.0(3) . . . . ? C1 Ir P1 C8 -108.0(3) . . . . ? P2 Ir P1 C8 85.5(3) . . . . ? P3 Ir P1 C8 -20.8(3) . . . . ? C20 Ir P1 C3 -69.9(3) . . . . ? C1 Ir P1 C3 12.0(3) . . . . ? P2 Ir P1 C3 -154.4(2) . . . . ? P3 Ir P1 C3 99.2(2) . . . . ? C20 Ir P1 C14 39.5(3) . . . . ? C1 Ir P1 C14 121.4(3) . . . . ? P2 Ir P1 C14 -45.0(3) . . . . ? P3 Ir P1 C14 -151.4(3) . . . . ? C20 Ir P2 C22 4.9(2) . . . . ? C1 Ir P2 C22 -14.8(7) . . . . ? P1 Ir P2 C22 95.67(18) . . . . ? P3 Ir P2 C22 -156.20(18) . . . . ? C20 Ir P2 C27 -109.6(3) . . . . ? C1 Ir P2 C27 -129.3(7) . . . . ? P1 Ir P2 C27 -18.8(3) . . . . ? P3 Ir P2 C27 89.3(3) . . . . ? C20 Ir P2 C33 114.9(3) . . . . ? C1 Ir P2 C33 95.3(7) . . . . ? P1 Ir P2 C33 -154.3(2) . . . . ? P3 Ir P2 C33 -46.1(2) . . . . ? C20 Ir P3 C39 -108.9(6) . . . . ? C1 Ir P3 C39 -172.5(3) . . . . ? P1 Ir P3 C39 104.8(3) . . . . ? P2 Ir P3 C39 -1.4(3) . . . . ? C20 Ir P3 C51 8.6(6) . . . . ? C1 Ir P3 C51 -55.0(3) . . . . ? P1 Ir P3 C51 -137.7(2) . . . . ? P2 Ir P3 C51 116.1(2) . . . . ? C20 Ir P3 C45 125.8(6) . . . . ? C1 Ir P3 C45 62.2(3) . . . . ? P1 Ir P3 C45 -20.6(3) . . . . ? P2 Ir P3 C45 -126.7(3) . . . . ? C20 Ir C1 O1 -99.9(6) . . . . ? P1 Ir C1 O1 167.2(6) . . . . ? P2 Ir C1 O1 -80.1(9) . . . . ? P3 Ir C1 O1 62.3(6) . . . . ? C20 Ir C1 C2 77.4(5) . . . . ? P1 Ir C1 C2 -15.6(4) . . . . ? P2 Ir C1 C2 97.1(8) . . . . ? P3 Ir C1 C2 -120.5(5) . . . . ? O1 C1 C2 C3 -167.4(6) . . . . ? Ir C1 C2 C3 15.0(8) . . . . ? O1 C1 C2 C7 12.7(9) . . . . ? Ir C1 C2 C7 -164.9(5) . . . . ? C7 C2 C3 C4 2.8(10) . . . . ? C1 C2 C3 C4 -177.2(6) . . . . ? C7 C2 C3 P1 177.4(5) . . . . ? C1 C2 C3 P1 -2.6(8) . . . . ? C8 P1 C3 C4 -65.1(7) . . . . ? C14 P1 C3 C4 40.6(7) . . . . ? Ir P1 C3 C4 165.9(6) . . . . ? C8 P1 C3 C2 120.5(5) . . . . ? C14 P1 C3 C2 -133.8(5) . . . . ? Ir P1 C3 C2 -8.5(5) . . . . ? C2 C3 C4 C5 -1.6(11) . . . . ? P1 C3 C4 C5 -175.7(6) . . . . ? C3 C4 C5 C6 -0.1(12) . . . . ? C4 C5 C6 C7 0.7(13) . . . . ? C5 C6 C7 C2 0.5(12) . . . . ? C3 C2 C7 C6 -2.2(10) . . . . ? C1 C2 C7 C6 177.8(7) . . . . ? C3 P1 C8 C13 -177.1(5) . . . . ? C14 P1 C8 C13 78.4(6) . . . . ? Ir P1 C8 C13 -60.3(6) . . . . ? C3 P1 C8 C9 5.9(7) . . . . ? C14 P1 C8 C9 -98.6(7) . . . . ? Ir P1 C8 C9 122.8(6) . . . . ? C13 C8 C9 C10 -0.4(13) . . . . ? P1 C8 C9 C10 176.5(8) . . . . ? C8 C9 C10 C11 1.3(16) . . . . ? C9 C10 C11 C12 -1.7(17) . . . . ? C10 C11 C12 C13 1.3(16) . . . . ? C9 C8 C13 C12 0.0(12) . . . . ? P1 C8 C13 C12 -177.1(7) . . . . ? C11 C12 C13 C8 -0.5(14) . . . . ? C8 P1 C14 C15 172.7(5) . . . . ? C3 P1 C14 C15 61.6(5) . . . . ? Ir P1 C14 C15 -48.7(6) . . . . ? C8 P1 C14 C19 -7.5(6) . . . . ? C3 P1 C14 C19 -118.6(6) . . . . ? Ir P1 C14 C19 131.0(5) . . . . ? C19 C14 C15 C16 -2.2(10) . . . . ? P1 C14 C15 C16 177.6(5) . . . . ? C14 C15 C16 C17 2.0(11) . . . . ? C15 C16 C17 C18 -1.6(12) . . . . ? C16 C17 C18 C19 1.3(12) . . . . ? C15 C14 C19 C18 1.9(10) . . . . ? P1 C14 C19 C18 -177.8(6) . . . . ? C17 C18 C19 C14 -1.6(12) . . . . ? C1 Ir C20 O2 -3.8(5) . . . . ? P1 Ir C20 O2 79.1(5) . . . . ? P2 Ir C20 O2 -179.0(5) . . . . ? P3 Ir C20 O2 -68.5(8) . . . . ? C1 Ir C20 C21 170.4(4) . . . . ? P1 Ir C20 C21 -106.7(4) . . . . ? P2 Ir C20 C21 -4.8(4) . . . . ? P3 Ir C20 C21 105.7(6) . . . . ? O2 C20 C21 C22 177.6(5) . . . . ? Ir C20 C21 C22 2.8(7) . . . . ? O2 C20 C21 C26 0.4(8) . . . . ? Ir C20 C21 C26 -174.4(4) . . . . ? C26 C21 C22 C23 2.2(8) . . . . ? C20 C21 C22 C23 -175.1(5) . . . . ? C26 C21 C22 P2 179.4(4) . . . . ? C20 C21 C22 P2 2.1(7) . . . . ? C27 P2 C22 C21 123.2(4) . . . . ? C33 P2 C22 C21 -130.8(4) . . . . ? Ir P2 C22 C21 -5.1(4) . . . . ? C27 P2 C22 C23 -59.8(6) . . . . ? C33 P2 C22 C23 46.2(6) . . . . ? Ir P2 C22 C23 171.9(5) . . . . ? C21 C22 C23 C24 -0.5(9) . . . . ? P2 C22 C23 C24 -177.4(5) . . . . ? C22 C23 C24 C25 -1.6(10) . . . . ? C23 C24 C25 C26 2.1(11) . . . . ? C24 C25 C26 C21 -0.5(10) . . . . ? C22 C21 C26 C25 -1.7(9) . . . . ? C20 C21 C26 C25 175.6(6) . . . . ? C22 P2 C27 C32 150.5(6) . . . . ? C33 P2 C27 C32 46.3(6) . . . . ? Ir P2 C27 C32 -96.0(6) . . . . ? C22 P2 C27 C28 -34.1(6) . . . . ? C33 P2 C27 C28 -138.3(5) . . . . ? Ir P2 C27 C28 79.4(6) . . . . ? C32 C27 C28 C29 0.8(10) . . . . ? P2 C27 C28 C29 -174.8(5) . . . . ? C27 C28 C29 C30 -1.3(11) . . . . ? C28 C29 C30 C31 0.2(11) . . . . ? C29 C30 C31 C32 1.3(11) . . . . ? C30 C31 C32 C27 -1.8(12) . . . . ? C28 C27 C32 C31 0.7(11) . . . . ? P2 C27 C32 C31 176.3(6) . . . . ? C22 P2 C33 C34 94.5(6) . . . . ? C27 P2 C33 C34 -158.9(5) . . . . ? Ir P2 C33 C34 -16.1(6) . . . . ? C22 P2 C33 C38 -80.7(6) . . . . ? C27 P2 C33 C38 25.8(6) . . . . ? Ir P2 C33 C38 168.6(5) . . . . ? C38 C33 C34 C35 1.3(11) . . . . ? P2 C33 C34 C35 -174.2(6) . . . . ? C33 C34 C35 C36 -0.3(12) . . . . ? C34 C35 C36 C37 -0.9(13) . . . . ? C35 C36 C37 C38 1.0(12) . . . . ? C36 C37 C38 C33 0.0(12) . . . . ? C34 C33 C38 C37 -1.2(11) . . . . ? P2 C33 C38 C37 174.1(6) . . . . ? C51 P3 C39 C40 -13.5(7) . . . . ? C45 P3 C39 C40 -116.0(7) . . . . ? Ir P3 C39 C40 110.6(6) . . . . ? C51 P3 C39 C44 167.1(6) . . . . ? C45 P3 C39 C44 64.7(7) . . . . ? Ir P3 C39 C44 -68.7(7) . . . . ? C44 C39 C40 C41 0.8(12) . . . . ? P3 C39 C40 C41 -178.5(7) . . . . ? C39 C40 C41 C42 -1.7(15) . . . . ? C40 C41 C42 C43 1.4(18) . . . . ? C41 C42 C43 C44 -0.1(18) . . . . ? C40 C39 C44 C43 0.4(13) . . . . ? P3 C39 C44 C43 179.8(7) . . . . ? C42 C43 C44 C39 -0.8(16) . . . . ? C39 P3 C45 C46 174.3(6) . . . . ? C51 P3 C45 C46 71.2(7) . . . . ? Ir P3 C45 C46 -52.9(7) . . . . ? C39 P3 C45 C50 -1.7(8) . . . . ? C51 P3 C45 C50 -104.8(8) . . . . ? Ir P3 C45 C50 131.1(7) . . . . ? C50 C45 C46 C47 2.1(14) . . . . ? P3 C45 C46 C47 -174.3(8) . . . . ? C45 C46 C47 C48 0.3(16) . . . . ? C46 C47 C48 C49 -2.2(17) . . . . ? C47 C48 C49 C50 1.7(18) . . . . ? C48 C49 C50 C45 0.8(18) . . . . ? C46 C45 C50 C49 -2.6(14) . . . . ? P3 C45 C50 C49 173.5(8) . . . . ? C39 P3 C51 C52 107.4(7) . . . . ? C45 P3 C51 C52 -148.3(7) . . . . ? Ir P3 C51 C52 -20.1(7) . . . . ? C39 P3 C51 C56 -69.7(7) . . . . ? C45 P3 C51 C56 34.6(7) . . . . ? Ir P3 C51 C56 162.8(6) . . . . ? C56 C51 C52 C53 0.4(12) . . . . ? P3 C51 C52 C53 -176.7(7) . . . . ? C51 C52 C53 C54 -0.3(14) . . . . ? C52 C53 C54 C55 0.1(15) . . . . ? C53 C54 C55 C56 0.0(17) . . . . ? C54 C55 C56 C51 0.1(17) . . . . ? C52 C51 C56 C55 -0.3(14) . . . . ? P3 C51 C56 C55 176.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 2.262 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.137 # Attachment 'compound7.cif' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 679483' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H31 Ir O2 P2' _chemical_formula_weight 773.77 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' O O 0.0106 0.0060 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4493(7) _cell_length_b 11.4628(7) _cell_length_c 13.7750(8) _cell_angle_alpha 72.0760(10) _cell_angle_beta 67.5550(10) _cell_angle_gamma 79.9430(10) _cell_volume 1586.44(17) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 4.342 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12249 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5563 _reflns_number_gt 4591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0133P)^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 5563 _refine_ls_number_parameters 393 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.006 _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 0.51667(2) 0.201243(19) 0.716569(18) 0.03391(9) Uani 1 1 d D . . H1 H 0.5259 0.3174 0.6046 0.047(15) Uiso 1 1 d RD . . H2 H 0.4922 0.0936 0.8358 0.043(14) Uiso 1 1 d RD . . C1 C 0.6784(6) 0.1343(6) 0.6232(5) 0.0483(16) Uani 1 1 d . . . O1 O 0.6890(4) 0.0524(4) 0.5739(4) 0.0685(14) Uani 1 1 d . . . H3 H 0.570(8) 0.027(7) 0.599(6) 0.100 Uiso 1 1 d . . . P1 P 0.64845(14) 0.31785(13) 0.73603(12) 0.0363(4) Uani 1 1 d . . . C2 C 0.8034(6) 0.1837(5) 0.5963(5) 0.0474(16) Uani 1 1 d . . . O2 O 0.4675(5) 0.0173(4) 0.6297(4) 0.0631(13) Uani 1 1 d . . . P2 P 0.31775(13) 0.26665(13) 0.81959(12) 0.0346(3) Uani 1 1 d . . . C3 C 0.8040(5) 0.2753(5) 0.6437(5) 0.0438(15) Uani 1 1 d . . . C4 C 0.9169(6) 0.3282(7) 0.6149(7) 0.074(2) Uani 1 1 d . . . H4A H 0.9175 0.3924 0.6428 0.088 Uiso 1 1 calc R . . C5 C 1.0270(7) 0.2871(9) 0.5463(7) 0.091(3) Uani 1 1 d . . . H5A H 1.1021 0.3220 0.5297 0.109 Uiso 1 1 calc R . . C6 C 1.0287(7) 0.1959(8) 0.5017(7) 0.087(3) Uani 1 1 d . . . H6A H 1.1045 0.1683 0.4555 0.104 Uiso 1 1 calc R . . C7 C 0.9161(7) 0.1440(6) 0.5256(5) 0.064(2) Uani 1 1 d . . . H7A H 0.9166 0.0827 0.4942 0.076 Uiso 1 1 calc R . . C8 C 0.6748(5) 0.2949(5) 0.8630(5) 0.0400(14) Uani 1 1 d . . . C9 C 0.7536(6) 0.3676(6) 0.8736(5) 0.0512(16) Uani 1 1 d . . . H9A H 0.7918 0.4321 0.8150 0.061 Uiso 1 1 calc R . . C10 C 0.7753(6) 0.3445(7) 0.9706(6) 0.064(2) Uani 1 1 d . . . H10A H 0.8276 0.3933 0.9769 0.076 Uiso 1 1 calc R . . C11 C 0.7189(7) 0.2487(7) 1.0578(6) 0.063(2) Uani 1 1 d . . . H11A H 0.7348 0.2318 1.1222 0.075 Uiso 1 1 calc R . . C12 C 0.6400(7) 0.1789(6) 1.0495(6) 0.0629(19) Uani 1 1 d . . . H12A H 0.6006 0.1160 1.1092 0.076 Uiso 1 1 calc R . . C13 C 0.6179(6) 0.2007(5) 0.9528(5) 0.0466(15) Uani 1 1 d . . . H13A H 0.5644 0.1518 0.9482 0.056 Uiso 1 1 calc R . . C14 C 0.6325(5) 0.4853(5) 0.6832(5) 0.0386(14) Uani 1 1 d . . . C15 C 0.5712(6) 0.5618(5) 0.7501(5) 0.0503(16) Uani 1 1 d . . . H15A H 0.5437 0.5304 0.8254 0.060 Uiso 1 1 calc R . . C16 C 0.5507(7) 0.6867(6) 0.7039(6) 0.066(2) Uani 1 1 d . . . H16A H 0.5105 0.7387 0.7489 0.079 Uiso 1 1 calc R . . C17 C 0.5889(7) 0.7336(6) 0.5937(6) 0.063(2) Uani 1 1 d . . . H17A H 0.5740 0.8169 0.5639 0.076 Uiso 1 1 calc R . . C18 C 0.6492(6) 0.6577(6) 0.5268(6) 0.0573(18) Uani 1 1 d . . . H18A H 0.6761 0.6891 0.4515 0.069 Uiso 1 1 calc R . . C19 C 0.6700(5) 0.5327(5) 0.5732(5) 0.0451(15) Uani 1 1 d . . . H19A H 0.7101 0.4809 0.5280 0.054 Uiso 1 1 calc R . . C20 C 0.4207(6) 0.0940(5) 0.6868(5) 0.0412(14) Uani 1 1 d . . . C21 C 0.2789(6) 0.0942(5) 0.7376(5) 0.0422(14) Uani 1 1 d . . . C22 C 0.2141(5) 0.1702(5) 0.8083(5) 0.0384(14) Uani 1 1 d . . . C23 C 0.0831(6) 0.1694(6) 0.8585(6) 0.0617(19) Uani 1 1 d . . . H23A H 0.0403 0.2205 0.9038 0.074 Uiso 1 1 calc R . . C24 C 0.0164(7) 0.0925(7) 0.8413(6) 0.072(2) Uani 1 1 d . . . H24A H -0.0706 0.0898 0.8775 0.086 Uiso 1 1 calc R . . C25 C 0.0776(7) 0.0206(7) 0.7714(7) 0.077(2) Uani 1 1 d . . . H25A H 0.0313 -0.0283 0.7583 0.092 Uiso 1 1 calc R . . C26 C 0.2084(7) 0.0197(6) 0.7196(6) 0.0604(19) Uani 1 1 d . . . H26A H 0.2492 -0.0303 0.6729 0.073 Uiso 1 1 calc R . . C27 C 0.2489(5) 0.4250(5) 0.7827(4) 0.0371(13) Uani 1 1 d . . . C28 C 0.1330(6) 0.4634(6) 0.8491(5) 0.0575(18) Uani 1 1 d . . . H28A H 0.0888 0.4097 0.9144 0.069 Uiso 1 1 calc R . . C29 C 0.0825(7) 0.5825(7) 0.8181(6) 0.071(2) Uani 1 1 d . . . H29A H 0.0037 0.6076 0.8622 0.086 Uiso 1 1 calc R . . C30 C 0.1476(7) 0.6628(6) 0.7234(6) 0.065(2) Uani 1 1 d . . . H30A H 0.1132 0.7422 0.7029 0.078 Uiso 1 1 calc R . . C31 C 0.2637(7) 0.6260(6) 0.6589(5) 0.0609(19) Uani 1 1 d . . . H31A H 0.3094 0.6806 0.5949 0.073 Uiso 1 1 calc R . . C32 C 0.3125(6) 0.5073(5) 0.6892(5) 0.0455(15) Uani 1 1 d . . . H32A H 0.3913 0.4827 0.6446 0.055 Uiso 1 1 calc R . . C33 C 0.2818(5) 0.2354(5) 0.9652(4) 0.0379(14) Uani 1 1 d . . . C34 C 0.2573(6) 0.1177(6) 1.0319(5) 0.0508(16) Uani 1 1 d . . . H34A H 0.2486 0.0568 1.0040 0.061 Uiso 1 1 calc R . . C35 C 0.2456(6) 0.0903(7) 1.1409(5) 0.0594(18) Uani 1 1 d . . . H35A H 0.2295 0.0110 1.1852 0.071 Uiso 1 1 calc R . . C36 C 0.2576(7) 0.1794(7) 1.1834(6) 0.066(2) Uani 1 1 d . . . H36A H 0.2488 0.1606 1.2564 0.079 Uiso 1 1 calc R . . C37 C 0.2821(7) 0.2947(7) 1.1190(6) 0.066(2) Uani 1 1 d . . . H37A H 0.2914 0.3546 1.1477 0.079 Uiso 1 1 calc R . . C38 C 0.2934(6) 0.3242(6) 1.0100(5) 0.0518(16) Uani 1 1 d . . . H38A H 0.3090 0.4041 0.9668 0.062 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 0.03401(13) 0.02812(13) 0.03666(14) -0.00809(10) -0.01033(10) -0.00031(9) C1 0.049(4) 0.035(3) 0.054(4) -0.005(3) -0.018(3) 0.002(3) O1 0.060(3) 0.065(3) 0.080(4) -0.042(3) -0.010(3) 0.006(3) P1 0.0309(8) 0.0328(8) 0.0409(9) -0.0074(7) -0.0096(7) -0.0028(6) C2 0.041(4) 0.042(4) 0.043(4) -0.003(3) -0.009(3) 0.009(3) O2 0.067(3) 0.052(3) 0.078(3) -0.038(3) -0.018(3) -0.007(2) P2 0.0315(8) 0.0315(8) 0.0395(9) -0.0076(7) -0.0122(7) -0.0027(6) C3 0.036(3) 0.040(4) 0.045(4) -0.004(3) -0.010(3) 0.002(3) C4 0.038(4) 0.063(5) 0.124(7) -0.042(5) -0.023(4) 0.005(3) C5 0.038(5) 0.118(8) 0.104(7) -0.027(6) -0.007(5) -0.013(5) C6 0.044(5) 0.096(7) 0.090(7) -0.028(5) 0.008(4) 0.008(5) C7 0.056(5) 0.055(4) 0.062(5) -0.018(4) -0.009(4) 0.016(4) C8 0.031(3) 0.034(3) 0.055(4) -0.013(3) -0.016(3) 0.003(3) C9 0.047(4) 0.048(4) 0.057(4) -0.011(3) -0.018(3) -0.006(3) C10 0.062(5) 0.064(5) 0.080(6) -0.023(4) -0.040(4) -0.002(4) C11 0.075(5) 0.067(5) 0.056(5) -0.022(4) -0.036(4) 0.010(4) C12 0.077(5) 0.052(4) 0.054(5) -0.006(4) -0.022(4) -0.007(4) C13 0.057(4) 0.037(4) 0.050(4) -0.010(3) -0.024(3) -0.004(3) C14 0.027(3) 0.033(3) 0.054(4) -0.007(3) -0.016(3) -0.004(2) C15 0.054(4) 0.047(4) 0.048(4) -0.013(3) -0.018(3) 0.003(3) C16 0.068(5) 0.052(5) 0.087(6) -0.033(5) -0.032(5) 0.015(4) C17 0.078(5) 0.032(4) 0.081(6) 0.001(4) -0.041(5) -0.005(3) C18 0.060(4) 0.046(4) 0.065(5) 0.005(4) -0.032(4) -0.014(3) C19 0.043(4) 0.045(4) 0.051(4) -0.014(3) -0.020(3) 0.000(3) C20 0.049(4) 0.034(3) 0.045(4) -0.016(3) -0.017(3) -0.003(3) C21 0.050(4) 0.035(3) 0.040(4) -0.002(3) -0.017(3) -0.011(3) C22 0.042(4) 0.035(3) 0.041(4) -0.004(3) -0.020(3) -0.009(3) C23 0.050(4) 0.072(5) 0.070(5) -0.024(4) -0.020(4) -0.012(4) C24 0.040(4) 0.086(6) 0.095(6) -0.023(5) -0.024(4) -0.019(4) C25 0.068(5) 0.080(6) 0.107(7) -0.036(5) -0.043(5) -0.018(4) C26 0.067(5) 0.055(4) 0.073(5) -0.025(4) -0.031(4) -0.009(4) C27 0.033(3) 0.038(3) 0.038(3) -0.010(3) -0.013(3) 0.003(3) C28 0.053(4) 0.052(4) 0.055(4) -0.009(3) -0.013(4) 0.006(3) C29 0.058(5) 0.073(5) 0.073(5) -0.030(5) -0.017(4) 0.027(4) C30 0.078(5) 0.046(4) 0.067(5) -0.010(4) -0.034(4) 0.020(4) C31 0.072(5) 0.043(4) 0.058(5) -0.008(3) -0.021(4) 0.005(4) C32 0.047(4) 0.040(4) 0.052(4) -0.014(3) -0.019(3) 0.000(3) C33 0.029(3) 0.047(4) 0.035(3) -0.017(3) -0.006(3) 0.001(3) C34 0.052(4) 0.046(4) 0.056(4) -0.006(3) -0.024(3) -0.011(3) C35 0.062(5) 0.065(5) 0.044(4) 0.002(4) -0.022(4) -0.009(4) C36 0.073(5) 0.085(6) 0.043(4) -0.017(4) -0.030(4) 0.009(4) C37 0.083(6) 0.063(5) 0.064(5) -0.029(4) -0.034(4) 0.001(4) C38 0.059(4) 0.042(4) 0.054(4) -0.013(3) -0.021(4) -0.001(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 Ir C1 1.991(6) . ? Ir C20 2.003(6) . ? Ir P2 2.3138(14) . ? Ir P1 2.3171(15) . ? Ir H1 1.6797 . ? Ir H2 1.6789 . ? C1 O1 1.284(7) . ? C1 C2 1.502(9) . ? O1 H3 1.34(8) . ? O1 H3 1.34(8) . ? P1 C14 1.835(5) . ? P1 C3 1.838(6) . ? P1 C8 1.820(6) . ? C2 C3 1.399(8) . ? C2 C7 1.389(8) . ? O2 C20 1.272(6) . ? O2 H3 1.09(8) . ? P2 C33 1.817(5) . ? P2 C22 1.833(6) . ? P2 C27 1.847(5) . ? C3 C4 1.389(9) . ? C4 C5 1.365(10) . ? C4 H4A 0.9300 . ? C5 C6 1.359(10) . ? C5 H5A 0.9300 . ? C6 C7 1.396(11) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C13 1.389(8) . ? C8 C9 1.404(8) . ? C9 C10 1.389(8) . ? C9 H9A 0.9300 . ? C10 C11 1.382(9) . ? C10 H10A 0.9300 . ? C11 C12 1.362(9) . ? C11 H11A 0.9300 . ? C12 C13 1.390(8) . ? C12 H12A 0.9300 . ? C13 H13A 0.9300 . ? C14 C19 1.362(7) . ? C14 C15 1.378(7) . ? C15 C16 1.394(8) . ? C15 H15A 0.9300 . ? C16 C17 1.363(9) . ? C16 H16A 0.9300 . ? C17 C18 1.371(9) . ? C17 H17A 0.9300 . ? C18 C19 1.397(8) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C20 C21 1.503(8) . ? C21 C26 1.403(8) . ? C21 C22 1.415(7) . ? C22 C23 1.391(8) . ? C23 C24 1.385(9) . ? C23 H23A 0.9300 . ? C24 C25 1.368(9) . ? C24 H24A 0.9300 . ? C25 C26 1.391(10) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C28 1.381(8) . ? C27 C32 1.362(8) . ? C28 C29 1.391(8) . ? C28 H28A 0.9300 . ? C29 C30 1.365(9) . ? C29 H29A 0.9300 . ? C30 C31 1.366(9) . ? C30 H30A 0.9300 . ? C31 C32 1.379(8) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.384(8) . ? C33 C38 1.390(7) . ? C34 C35 1.393(8) . ? C34 H34A 0.9300 . ? C35 C36 1.372(9) . ? C35 H35A 0.9300 . ? C36 C37 1.352(10) . ? C36 H36A 0.9300 . ? C37 C38 1.392(8) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir C20 89.7(3) . . ? C1 Ir P2 173.9(2) . . ? C20 Ir P2 84.15(17) . . ? C1 Ir P1 83.6(2) . . ? C20 Ir P1 173.31(17) . . ? P2 Ir P1 102.47(5) . . ? C1 Ir H1 85.4 . . ? C20 Ir H1 96.0 . . ? P2 Ir H1 94.8 . . ? P1 Ir H1 82.6 . . ? C1 Ir H2 101.1 . . ? C20 Ir H2 84.3 . . ? P2 Ir H2 78.8 . . ? P1 Ir H2 97.8 . . ? H1 Ir H2 173.5 . . ? O1 C1 C2 112.2(5) . . ? O1 C1 Ir 125.7(5) . . ? C2 C1 Ir 122.0(5) . . ? H3 O1 C1 104(3) . . ? H3 O1 H3 0(7) . . ? C1 O1 H3 104(3) . . ? C14 P1 C3 103.2(3) . . ? C14 P1 C8 104.5(3) . . ? C3 P1 C8 103.5(3) . . ? C14 P1 Ir 117.72(17) . . ? C3 P1 Ir 101.8(2) . . ? C8 P1 Ir 123.2(2) . . ? C3 C2 C7 119.5(6) . . ? C3 C2 C1 117.6(5) . . ? C7 C2 C1 122.9(6) . . ? C20 O2 H3 104(4) . . ? C33 P2 C22 104.3(3) . . ? C33 P2 C27 103.3(2) . . ? C22 P2 C27 104.6(2) . . ? C33 P2 Ir 117.54(17) . . ? C22 P2 Ir 102.40(19) . . ? C27 P2 Ir 122.57(19) . . ? C2 C3 C4 118.9(6) . . ? C2 C3 P1 114.6(4) . . ? C4 C3 P1 126.4(5) . . ? C3 C4 C5 120.7(7) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? C6 C5 C4 121.0(8) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 119.5 . . ? C5 C6 C7 119.7(7) . . ? C5 C6 H6A 120.2 . . ? C7 C6 H6A 120.2 . . ? C6 C7 C2 120.0(7) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C13 C8 C9 118.0(5) . . ? C13 C8 P1 119.7(4) . . ? C9 C8 P1 122.4(5) . . ? C10 C9 C8 120.8(6) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C11 C10 C9 119.7(7) . . ? C11 C10 H10A 120.1 . . ? C9 C10 H10A 120.1 . . ? C12 C11 C10 120.2(6) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? C11 C12 C13 120.7(7) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C8 C13 C12 120.6(6) . . ? C8 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C19 C14 C15 119.3(5) . . ? C19 C14 P1 117.8(4) . . ? C15 C14 P1 122.4(5) . . ? C14 C15 C16 119.4(6) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C17 C16 C15 120.9(6) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C18 C17 C16 119.9(6) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C19 119.2(6) . . ? C17 C18 H18A 120.4 . . ? C19 C18 H18A 120.4 . . ? C14 C19 C18 121.3(6) . . ? C14 C19 H19A 119.4 . . ? C18 C19 H19A 119.4 . . ? O2 C20 C21 112.5(5) . . ? O2 C20 Ir 126.7(5) . . ? C21 C20 Ir 120.7(4) . . ? C26 C21 C22 118.6(6) . . ? C26 C21 C20 122.4(5) . . ? C22 C21 C20 118.9(5) . . ? C23 C22 C21 119.9(5) . . ? C23 C22 P2 126.4(5) . . ? C21 C22 P2 113.7(4) . . ? C22 C23 C24 120.2(6) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C25 C24 C23 120.5(7) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 120.7(7) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C25 C26 C21 120.1(6) . . ? C25 C26 H26A 119.9 . . ? C21 C26 H26A 119.9 . . ? C28 C27 C32 118.4(5) . . ? C28 C27 P2 121.3(5) . . ? C32 C27 P2 120.4(4) . . ? C27 C28 C29 119.9(6) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 120.6(6) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 C31 119.6(6) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C32 C31 C30 119.6(7) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C31 C32 C27 121.9(6) . . ? C31 C32 H32A 119.0 . . ? C27 C32 H32A 119.0 . . ? C34 C33 C38 118.3(5) . . ? C34 C33 P2 120.2(5) . . ? C38 C33 P2 121.1(5) . . ? C33 C34 C35 120.2(6) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C36 C35 C34 120.5(7) . . ? C36 C35 H35A 119.7 . . ? C34 C35 H35A 119.7 . . ? C37 C36 C35 120.0(6) . . ? C37 C36 H36A 120.0 . . ? C35 C36 H36A 120.0 . . ? C36 C37 C38 120.4(7) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C33 C38 C37 120.6(6) . . ? C33 C38 H38A 119.7 . . ? C37 C38 H38A 119.7 . . ? 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 C20 Ir C1 O1 -0.9(5) . . . . ? P2 Ir C1 O1 -5(2) . . . . ? P1 Ir C1 O1 179.9(5) . . . . ? C20 Ir C1 C2 174.3(5) . . . . ? P2 Ir C1 C2 169.9(12) . . . . ? P1 Ir C1 C2 -4.8(4) . . . . ? C2 C1 O1 H3 -175(3) . . . . ? Ir C1 O1 H3 1(3) . . . . ? C1 Ir P1 C14 116.4(3) . . . . ? C20 Ir P1 C14 108.9(14) . . . . ? P2 Ir P1 C14 -63.0(2) . . . . ? C1 Ir P1 C3 4.5(2) . . . . ? C20 Ir P1 C3 -3.0(14) . . . . ? P2 Ir P1 C3 -174.92(18) . . . . ? C1 Ir P1 C8 -110.5(3) . . . . ? C20 Ir P1 C8 -118.0(14) . . . . ? P2 Ir P1 C8 70.1(2) . . . . ? O1 C1 C2 C3 179.0(5) . . . . ? Ir C1 C2 C3 3.2(7) . . . . ? O1 C1 C2 C7 0.2(8) . . . . ? Ir C1 C2 C7 -175.6(4) . . . . ? C1 Ir P2 C33 121.0(16) . . . . ? C20 Ir P2 C33 116.6(3) . . . . ? P1 Ir P2 C33 -64.4(2) . . . . ? C1 Ir P2 C22 7.4(16) . . . . ? C20 Ir P2 C22 3.0(2) . . . . ? P1 Ir P2 C22 -177.98(17) . . . . ? C1 Ir P2 C27 -109.1(16) . . . . ? C20 Ir P2 C27 -113.5(3) . . . . ? P1 Ir P2 C27 65.5(2) . . . . ? C7 C2 C3 C4 2.9(9) . . . . ? C1 C2 C3 C4 -176.0(6) . . . . ? C7 C2 C3 P1 -179.6(4) . . . . ? C1 C2 C3 P1 1.6(7) . . . . ? C14 P1 C3 C2 -127.0(4) . . . . ? C8 P1 C3 C2 124.3(4) . . . . ? Ir P1 C3 C2 -4.5(4) . . . . ? C14 P1 C3 C4 50.4(6) . . . . ? C8 P1 C3 C4 -58.4(6) . . . . ? Ir P1 C3 C4 172.9(6) . . . . ? C2 C3 C4 C5 -3.6(11) . . . . ? P1 C3 C4 C5 179.2(6) . . . . ? C3 C4 C5 C6 1.9(13) . . . . ? C4 C5 C6 C7 0.6(13) . . . . ? C5 C6 C7 C2 -1.3(12) . . . . ? C3 C2 C7 C6 -0.5(9) . . . . ? C1 C2 C7 C6 178.3(6) . . . . ? C14 P1 C8 C13 140.5(4) . . . . ? C3 P1 C8 C13 -111.7(5) . . . . ? Ir P1 C8 C13 2.4(5) . . . . ? C14 P1 C8 C9 -41.0(5) . . . . ? C3 P1 C8 C9 66.8(5) . . . . ? Ir P1 C8 C9 -179.1(4) . . . . ? C13 C8 C9 C10 1.0(9) . . . . ? P1 C8 C9 C10 -177.6(4) . . . . ? C8 C9 C10 C11 0.1(10) . . . . ? C9 C10 C11 C12 -1.5(10) . . . . ? C10 C11 C12 C13 1.7(10) . . . . ? C9 C8 C13 C12 -0.8(9) . . . . ? P1 C8 C13 C12 177.9(5) . . . . ? C11 C12 C13 C8 -0.6(10) . . . . ? C3 P1 C14 C19 42.0(5) . . . . ? C8 P1 C14 C19 150.0(4) . . . . ? Ir P1 C14 C19 -69.1(5) . . . . ? C3 P1 C14 C15 -145.8(5) . . . . ? C8 P1 C14 C15 -37.8(5) . . . . ? Ir P1 C14 C15 103.1(5) . . . . ? C19 C14 C15 C16 -1.2(9) . . . . ? P1 C14 C15 C16 -173.3(5) . . . . ? C14 C15 C16 C17 1.0(10) . . . . ? C15 C16 C17 C18 -0.6(11) . . . . ? C16 C17 C18 C19 0.4(10) . . . . ? C15 C14 C19 C18 1.0(9) . . . . ? P1 C14 C19 C18 173.5(5) . . . . ? C17 C18 C19 C14 -0.6(9) . . . . ? C1 Ir C20 O2 1.7(5) . . . . ? P2 Ir C20 O2 -178.7(5) . . . . ? P1 Ir C20 O2 9.2(18) . . . . ? C1 Ir C20 C21 178.8(4) . . . . ? P2 Ir C20 C21 -1.7(4) . . . . ? P1 Ir C20 C21 -173.8(10) . . . . ? O2 C20 C21 C26 -2.0(8) . . . . ? Ir C20 C21 C26 -179.4(4) . . . . ? O2 C20 C21 C22 176.6(5) . . . . ? Ir C20 C21 C22 -0.8(7) . . . . ? C26 C21 C22 C23 0.4(8) . . . . ? C20 C21 C22 C23 -178.3(5) . . . . ? C26 C21 C22 P2 -177.7(4) . . . . ? C20 C21 C22 P2 3.7(6) . . . . ? C33 P2 C22 C23 54.8(6) . . . . ? C27 P2 C22 C23 -53.4(6) . . . . ? Ir P2 C22 C23 177.8(5) . . . . ? C33 P2 C22 C21 -127.3(4) . . . . ? C27 P2 C22 C21 124.5(4) . . . . ? Ir P2 C22 C21 -4.3(4) . . . . ? C21 C22 C23 C24 1.3(9) . . . . ? P2 C22 C23 C24 179.0(5) . . . . ? C22 C23 C24 C25 -2.7(11) . . . . ? C23 C24 C25 C26 2.5(12) . . . . ? C24 C25 C26 C21 -0.8(11) . . . . ? C22 C21 C26 C25 -0.6(9) . . . . ? C20 C21 C26 C25 178.0(6) . . . . ? C33 P2 C27 C28 -40.6(6) . . . . ? C22 P2 C27 C28 68.3(5) . . . . ? Ir P2 C27 C28 -176.2(4) . . . . ? C33 P2 C27 C32 138.7(5) . . . . ? C22 P2 C27 C32 -112.3(5) . . . . ? Ir P2 C27 C32 3.1(6) . . . . ? C32 C27 C28 C29 1.9(10) . . . . ? P2 C27 C28 C29 -178.8(5) . . . . ? C27 C28 C29 C30 -1.2(11) . . . . ? C28 C29 C30 C31 -0.3(11) . . . . ? C29 C30 C31 C32 1.2(11) . . . . ? C30 C31 C32 C27 -0.5(10) . . . . ? C28 C27 C32 C31 -1.0(9) . . . . ? P2 C27 C32 C31 179.6(5) . . . . ? C22 P2 C33 C34 37.7(5) . . . . ? C27 P2 C33 C34 146.8(5) . . . . ? Ir P2 C33 C34 -74.9(5) . . . . ? C22 P2 C33 C38 -150.3(4) . . . . ? C27 P2 C33 C38 -41.2(5) . . . . ? Ir P2 C33 C38 97.1(4) . . . . ? C38 C33 C34 C35 -0.4(8) . . . . ? P2 C33 C34 C35 171.9(5) . . . . ? C33 C34 C35 C36 0.3(9) . . . . ? C34 C35 C36 C37 -0.6(10) . . . . ? C35 C36 C37 C38 1.0(11) . . . . ? C34 C33 C38 C37 0.7(9) . . . . ? P2 C33 C38 C37 -171.4(5) . . . . ? C36 C37 C38 C33 -1.0(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.341 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.119 # Attachment 'compound9.cif' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 679484' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H41 Cl Ir O2 P2 Rh' _chemical_formula_weight 1018.29 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' O O 0.0106 0.0060 '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' Rh Rh -1.1178 0.9187 '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 12.2643(11) _cell_length_b 13.0300(11) _cell_length_c 14.3161(13) _cell_angle_alpha 87.480(2) _cell_angle_beta 78.631(2) _cell_angle_gamma 63.784(2) _cell_volume 2009.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 3.902 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17331 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1058 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 26.37 _reflns_number_total 7929 _reflns_number_gt 5545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0133P)^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 7929 _refine_ls_number_parameters 479 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _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 C1 C 0.7834(5) 0.9079(5) 0.6242(4) 0.0274(15) Uani 1 1 d . . . C2 C 0.7289(5) 0.8385(5) 0.5850(4) 0.0264(15) Uani 1 1 d . . . C3 C 0.7316(5) 0.7422(5) 0.6341(4) 0.0266(15) Uani 1 1 d . . . C4 C 0.6799(5) 0.6768(5) 0.6025(4) 0.0317(16) Uani 1 1 d . . . H4 H 0.6789 0.6145 0.6364 0.038 Uiso 1 1 calc R . . C5 C 0.6305(6) 0.7046(6) 0.5213(4) 0.0388(17) Uani 1 1 d . . . H5 H 0.5994 0.6590 0.4990 0.047 Uiso 1 1 calc R . . C6 C 0.6268(6) 0.7993(6) 0.4728(4) 0.0385(18) Uani 1 1 d . . . H6 H 0.5926 0.8180 0.4184 0.046 Uiso 1 1 calc R . . C7 C 0.6740(6) 0.8668(5) 0.5051(4) 0.0366(16) Uani 1 1 d . . . H7 H 0.6691 0.9319 0.4731 0.044 Uiso 1 1 calc R . . C8 C 0.6671(6) 0.7344(5) 0.8378(4) 0.0290(15) Uani 1 1 d . . . C9 C 0.6289(6) 0.6504(6) 0.8600(4) 0.0422(18) Uani 1 1 d . . . H9 H 0.6735 0.5791 0.8277 0.051 Uiso 1 1 calc R . . C10 C 0.5248(7) 0.6700(7) 0.9297(5) 0.050(2) Uani 1 1 d . . . H10 H 0.5006 0.6118 0.9438 0.061 Uiso 1 1 calc R . . C11 C 0.4582(7) 0.7734(8) 0.9774(5) 0.062(2) Uani 1 1 d . . . H11 H 0.3878 0.7869 1.0236 0.074 Uiso 1 1 calc R . . C12 C 0.4955(7) 0.8574(7) 0.9567(5) 0.068(3) Uani 1 1 d . . . H12 H 0.4502 0.9282 0.9897 0.081 Uiso 1 1 calc R . . C13 C 0.6001(6) 0.8396(6) 0.8873(5) 0.054(2) Uani 1 1 d . . . H13 H 0.6246 0.8977 0.8745 0.064 Uiso 1 1 calc R . . C14 C 0.8998(6) 0.5649(5) 0.7307(4) 0.0321(16) Uani 1 1 d . . . C15 C 0.9256(6) 0.4997(6) 0.8100(4) 0.0390(17) Uani 1 1 d . . . H15 H 0.8882 0.5351 0.8705 0.047 Uiso 1 1 calc R . . C16 C 1.0055(6) 0.3831(6) 0.8017(5) 0.0488(19) Uani 1 1 d . . . H16 H 1.0205 0.3411 0.8558 0.059 Uiso 1 1 calc R . . C17 C 1.0613(6) 0.3315(6) 0.7133(5) 0.051(2) Uani 1 1 d . . . H17 H 1.1143 0.2535 0.7066 0.061 Uiso 1 1 calc R . . C18 C 1.0395(6) 0.3942(6) 0.6345(5) 0.0454(19) Uani 1 1 d . . . H18 H 1.0790 0.3582 0.5745 0.055 Uiso 1 1 calc R . . C19 C 0.9601(6) 0.5099(6) 0.6415(4) 0.0374(17) Uani 1 1 d . . . H19 H 0.9472 0.5510 0.5867 0.045 Uiso 1 1 calc R . . C20 C 1.0017(6) 0.9223(6) 0.6693(4) 0.0302(16) Uani 1 1 d . . . C21 C 1.1307(5) 0.8766(5) 0.6888(4) 0.0286(15) Uani 1 1 d . . . C22 C 1.1618(6) 0.7981(5) 0.7603(4) 0.0325(16) Uani 1 1 d . . . C23 C 1.2793(6) 0.7577(6) 0.7811(5) 0.0477(19) Uani 1 1 d . . . H23 H 1.3011 0.7053 0.8284 0.057 Uiso 1 1 calc R . . C24 C 1.3644(7) 0.7938(7) 0.7331(5) 0.057(2) Uani 1 1 d . . . H24 H 1.4427 0.7661 0.7480 0.068 Uiso 1 1 calc R . . C25 C 1.3326(6) 0.8708(6) 0.6633(5) 0.0473(19) Uani 1 1 d . . . H25 H 1.3898 0.8952 0.6308 0.057 Uiso 1 1 calc R . . C26 C 1.2158(6) 0.9128(6) 0.6402(4) 0.0381(17) Uani 1 1 d . . . H26 H 1.1952 0.9647 0.5925 0.046 Uiso 1 1 calc R . . C27 C 0.9945(6) 0.8163(5) 0.9420(4) 0.0335(16) Uani 1 1 d . . . C28 C 1.0696(7) 0.8399(6) 0.9894(4) 0.051(2) Uani 1 1 d . . . H28 H 1.1494 0.8257 0.9584 0.061 Uiso 1 1 calc R . . C29 C 1.0268(9) 0.8847(7) 1.0827(5) 0.065(3) Uani 1 1 d . . . H29 H 1.0783 0.8990 1.1144 0.078 Uiso 1 1 calc R . . C30 C 0.9092(9) 0.9077(6) 1.1280(5) 0.064(3) Uani 1 1 d . . . H30 H 0.8808 0.9397 1.1899 0.076 Uiso 1 1 calc R . . C31 C 0.8318(7) 0.8849(6) 1.0846(5) 0.061(2) Uani 1 1 d . . . H31 H 0.7522 0.8998 1.1165 0.073 Uiso 1 1 calc R . . C32 C 0.8759(6) 0.8385(6) 0.9906(4) 0.0431(18) Uani 1 1 d . . . H32 H 0.8246 0.8222 0.9600 0.052 Uiso 1 1 calc R . . C33 C 1.1297(5) 0.6067(5) 0.8277(4) 0.0318(16) Uani 1 1 d . . . C34 C 1.1441(7) 0.5532(6) 0.9126(4) 0.053(2) Uani 1 1 d . . . H34 H 1.1020 0.5955 0.9699 0.064 Uiso 1 1 calc R . . C35 C 1.2214(7) 0.4362(7) 0.9135(5) 0.068(3) Uani 1 1 d . . . H35 H 1.2288 0.4014 0.9716 0.082 Uiso 1 1 calc R . . C36 C 1.2859(7) 0.3721(7) 0.8314(5) 0.062(2) Uani 1 1 d . . . H36 H 1.3393 0.2948 0.8330 0.074 Uiso 1 1 calc R . . C37 C 1.2711(7) 0.4237(6) 0.7456(5) 0.0483(19) Uani 1 1 d . . . H37 H 1.3130 0.3804 0.6887 0.058 Uiso 1 1 calc R . . C38 C 1.1938(6) 0.5401(6) 0.7434(4) 0.0410(18) Uani 1 1 d . . . H38 H 1.1849 0.5738 0.6851 0.049 Uiso 1 1 calc R . . C39 C 0.8307(7) 1.2533(6) 0.6903(5) 0.056(2) Uani 1 1 d . . . H39 H 0.9027 1.2198 0.7211 0.067 Uiso 1 1 calc R . . C40 C 0.8597(7) 1.2533(6) 0.5902(5) 0.049(2) Uani 1 1 d . . . H40 H 0.9489 1.2181 0.5634 0.059 Uiso 1 1 calc R . . C41 C 0.7832(7) 1.3450(7) 0.5308(6) 0.067(2) Uani 1 1 d . . . H41A H 0.7750 1.4181 0.5522 0.081 Uiso 1 1 calc R . . H41B H 0.8277 1.3299 0.4650 0.081 Uiso 1 1 calc R . . C42 C 0.6580(8) 1.3548(7) 0.5335(6) 0.073(3) Uani 1 1 d . . . H42A H 0.6449 1.3567 0.4687 0.087 Uiso 1 1 calc R . . H42B H 0.5972 1.4268 0.5664 0.087 Uiso 1 1 calc R . . C43 C 0.6361(6) 1.2594(6) 0.5818(5) 0.0471(19) Uani 1 1 d . . . H43 H 0.5959 1.2275 0.5469 0.057 Uiso 1 1 calc R . . C44 C 0.6074(6) 1.2547(6) 0.6804(5) 0.051(2) Uani 1 1 d . . . H44 H 0.5503 1.2206 0.7016 0.062 Uiso 1 1 calc R . . C45 C 0.5974(8) 1.3423(7) 0.7516(6) 0.089(3) Uani 1 1 d . . . H45A H 0.5361 1.4172 0.7387 0.106 Uiso 1 1 calc R . . H45B H 0.5683 1.3241 0.8152 0.106 Uiso 1 1 calc R . . C46 C 0.7162(10) 1.3478(8) 0.7492(6) 0.091(3) Uani 1 1 d . . . H46A H 0.7286 1.3465 0.8142 0.109 Uiso 1 1 calc R . . H46B H 0.7087 1.4207 0.7246 0.109 Uiso 1 1 calc R . . Cl Cl 0.75318(15) 1.01589(14) 0.82033(10) 0.0391(4) Uani 1 1 d . . . Ir Ir 0.89577(2) 0.83896(2) 0.718558(16) 0.02530(8) Uani 1 1 d D . . H1 H 1.0231 0.7388 0.6499 0.16(4) Uiso 1 1 d RD . . O1 O 0.7451(4) 1.0067(3) 0.5919(3) 0.0317(10) Uani 1 1 d . . . O2 O 0.9714(4) 1.0143(4) 0.6264(3) 0.0399(11) Uani 1 1 d . . . P1 P 0.79854(15) 0.71806(14) 0.74137(10) 0.0269(4) Uani 1 1 d . . . P2 P 1.03999(15) 0.76062(15) 0.81894(10) 0.0291(4) Uani 1 1 d . . . Rh Rh 0.78906(5) 1.13519(4) 0.63221(4) 0.03832(15) 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 C1 0.031(4) 0.021(4) 0.030(3) -0.002(3) 0.003(3) -0.014(3) C2 0.033(4) 0.020(4) 0.027(3) 0.001(3) -0.009(3) -0.011(3) C3 0.025(4) 0.029(4) 0.025(3) -0.003(3) -0.008(3) -0.010(3) C4 0.037(4) 0.030(4) 0.033(3) 0.004(3) -0.009(3) -0.018(3) C5 0.037(4) 0.043(5) 0.046(4) -0.003(4) -0.015(3) -0.023(4) C6 0.042(4) 0.043(5) 0.036(4) 0.001(3) -0.021(3) -0.018(4) C7 0.036(4) 0.032(4) 0.042(4) 0.004(3) -0.010(3) -0.014(3) C8 0.032(4) 0.032(4) 0.026(3) -0.001(3) -0.004(3) -0.018(3) C9 0.041(5) 0.039(5) 0.044(4) 0.006(3) -0.009(3) -0.016(4) C10 0.049(5) 0.060(6) 0.057(5) 0.018(4) -0.010(4) -0.038(5) C11 0.041(5) 0.095(8) 0.048(5) -0.005(5) 0.011(4) -0.037(5) C12 0.051(6) 0.077(7) 0.068(5) -0.031(5) 0.019(4) -0.030(5) C13 0.052(5) 0.051(5) 0.059(5) -0.020(4) 0.014(4) -0.032(4) C14 0.035(4) 0.030(4) 0.034(3) 0.003(3) -0.009(3) -0.016(3) C15 0.042(4) 0.043(5) 0.031(3) 0.003(3) -0.003(3) -0.020(4) C16 0.046(5) 0.036(5) 0.055(5) 0.018(4) -0.010(4) -0.012(4) C17 0.046(5) 0.028(4) 0.068(5) -0.006(4) -0.005(4) -0.008(4) C18 0.048(5) 0.036(5) 0.042(4) -0.009(4) -0.003(3) -0.011(4) C19 0.041(4) 0.035(4) 0.032(3) -0.002(3) -0.003(3) -0.014(4) C20 0.037(4) 0.030(4) 0.027(3) 0.003(3) -0.008(3) -0.018(4) C21 0.022(4) 0.031(4) 0.028(3) 0.000(3) -0.008(3) -0.007(3) C22 0.026(4) 0.041(4) 0.032(3) 0.001(3) -0.007(3) -0.015(3) C23 0.042(5) 0.061(5) 0.047(4) 0.018(4) -0.013(4) -0.028(4) C24 0.034(5) 0.083(7) 0.054(5) 0.019(4) -0.014(4) -0.027(5) C25 0.028(4) 0.066(6) 0.045(4) 0.003(4) 0.003(3) -0.021(4) C26 0.035(4) 0.042(5) 0.037(4) 0.002(3) 0.001(3) -0.020(4) C27 0.047(4) 0.034(4) 0.024(3) 0.002(3) -0.012(3) -0.020(4) C28 0.072(6) 0.064(6) 0.037(4) 0.012(4) -0.018(4) -0.044(5) C29 0.123(8) 0.064(6) 0.036(4) 0.010(4) -0.035(5) -0.059(6) C30 0.113(8) 0.036(5) 0.032(4) 0.000(4) -0.009(5) -0.026(6) C31 0.062(6) 0.060(6) 0.038(4) -0.001(4) 0.001(4) -0.011(5) C32 0.044(5) 0.050(5) 0.033(4) 0.007(3) -0.011(3) -0.018(4) C33 0.026(4) 0.040(4) 0.028(3) 0.004(3) -0.011(3) -0.012(3) C34 0.066(5) 0.048(5) 0.031(4) 0.001(4) -0.007(4) -0.013(4) C35 0.088(6) 0.046(5) 0.038(4) 0.011(4) -0.023(4) 0.003(5) C36 0.057(5) 0.045(5) 0.059(5) 0.000(4) -0.013(4) 0.000(4) C37 0.055(5) 0.041(5) 0.040(4) -0.007(4) -0.006(4) -0.013(4) C38 0.036(4) 0.047(5) 0.030(3) 0.001(3) -0.004(3) -0.010(4) C39 0.068(6) 0.055(6) 0.072(5) 0.003(4) -0.029(5) -0.045(5) C40 0.042(5) 0.047(5) 0.072(5) 0.006(4) -0.014(4) -0.030(4) C41 0.067(6) 0.051(6) 0.076(6) 0.025(5) -0.022(5) -0.019(5) C42 0.088(7) 0.058(6) 0.085(6) 0.030(5) -0.042(5) -0.036(6) C43 0.044(5) 0.043(5) 0.058(5) 0.009(4) -0.023(4) -0.017(4) C44 0.036(4) 0.042(5) 0.073(5) -0.008(4) -0.010(4) -0.013(4) C45 0.077(7) 0.070(7) 0.092(7) -0.023(5) -0.016(6) -0.006(6) C46 0.139(10) 0.085(8) 0.068(6) -0.027(5) -0.002(6) -0.072(8) Cl 0.0419(10) 0.0313(10) 0.0382(9) -0.0097(7) -0.0018(7) -0.0126(9) Ir 0.02564(14) 0.02700(16) 0.02299(12) -0.00082(10) -0.00562(9) -0.01090(12) O1 0.040(3) 0.024(3) 0.036(2) 0.008(2) -0.020(2) -0.015(2) O2 0.032(3) 0.033(3) 0.060(3) 0.017(2) -0.012(2) -0.018(2) P1 0.0302(10) 0.0266(10) 0.0235(8) -0.0009(7) -0.0060(7) -0.0116(8) P2 0.0282(10) 0.0337(11) 0.0241(8) 0.0014(7) -0.0068(7) -0.0117(9) Rh 0.0361(3) 0.0278(3) 0.0573(3) 0.0050(3) -0.0202(3) -0.0155(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 C1 O1 1.262(6) . ? C1 C2 1.517(7) . ? C1 Ir 2.017(6) . ? C2 C3 1.402(7) . ? C2 C7 1.395(7) . ? C3 C4 1.399(7) . ? C3 P1 1.833(5) . ? C4 C5 1.378(8) . ? C4 H4 0.9300 . ? C5 C6 1.377(8) . ? C5 H5 0.9300 . ? C6 C7 1.383(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.372(8) . ? C8 C13 1.385(8) . ? C8 P1 1.842(6) . ? C9 C10 1.387(9) . ? C9 H9 0.9300 . ? C10 C11 1.356(9) . ? C10 H10 0.9300 . ? C11 C12 1.362(9) . ? C11 H11 0.9300 . ? C12 C13 1.393(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.389(7) . ? C14 C15 1.388(8) . ? C14 P1 1.820(6) . ? C15 C16 1.392(8) . ? C15 H15 0.9300 . ? C16 C17 1.359(9) . ? C16 H16 0.9300 . ? C17 C18 1.362(9) . ? C17 H17 0.9300 . ? C18 C19 1.382(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 O2 1.258(7) . ? C20 C21 1.504(8) . ? C20 Ir 2.046(6) . ? C21 C22 1.398(8) . ? C21 C26 1.384(8) . ? C22 C23 1.389(8) . ? C22 P2 1.813(6) . ? C23 C24 1.381(8) . ? C23 H23 0.9300 . ? C24 C25 1.370(9) . ? C24 H24 0.9300 . ? C25 C26 1.392(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C32 1.390(8) . ? C27 C28 1.385(8) . ? C27 P2 1.819(6) . ? C28 C29 1.385(9) . ? C28 H28 0.9300 . ? C29 C30 1.363(10) . ? C29 H29 0.9300 . ? C30 C31 1.368(10) . ? C30 H30 0.9300 . ? C31 C32 1.402(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.377(8) . ? C33 C38 1.394(8) . ? C33 P2 1.825(6) . ? C34 C35 1.397(9) . ? C34 H34 0.9300 . ? C35 C36 1.356(9) . ? C35 H35 0.9300 . ? C36 C37 1.380(9) . ? C36 H36 0.9300 . ? C37 C38 1.391(8) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.407(9) . ? C39 C46 1.515(10) . ? C39 Rh 2.072(6) . ? C39 H39 0.9800 . ? C40 C41 1.505(9) . ? C40 Rh 2.092(7) . ? C40 H40 0.9800 . ? C41 C42 1.476(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.497(9) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.391(9) . ? C43 Rh 2.099(7) . ? C43 H43 0.9800 . ? C44 C45 1.512(9) . ? C44 Rh 2.070(7) . ? C44 H44 0.9800 . ? C45 C46 1.484(10) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? Cl Ir 2.4950(15) . ? Ir P1 2.3389(17) . ? Ir P2 2.3482(16) . ? Ir H1 1.6779 . ? O1 Rh 2.104(4) . ? O2 Rh 2.077(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 O1 C1 C2 111.0(5) . . ? O1 C1 Ir 129.3(4) . . ? C2 C1 Ir 119.6(4) . . ? C3 C2 C7 118.6(5) . . ? C3 C2 C1 117.5(5) . . ? C7 C2 C1 123.8(6) . . ? C2 C3 C4 120.0(5) . . ? C2 C3 P1 114.6(4) . . ? C4 C3 P1 125.4(5) . . ? C5 C4 C3 120.0(6) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.5(6) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.0(6) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C2 C7 C6 120.9(6) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C9 C8 C13 118.5(6) . . ? C9 C8 P1 123.7(5) . . ? C13 C8 P1 117.7(5) . . ? C8 C9 C10 121.2(7) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C11 C10 C9 120.4(7) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 119.2(7) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C13 121.5(7) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 119.3(7) . . ? C8 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C19 C14 C15 117.3(6) . . ? C19 C14 P1 120.4(5) . . ? C15 C14 P1 122.2(5) . . ? C16 C15 C14 122.1(6) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 C17 119.1(7) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 119.9(7) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 121.7(6) . . ? C17 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C14 C19 C18 119.8(6) . . ? C14 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? O2 C20 C21 112.4(5) . . ? O2 C20 Ir 128.1(5) . . ? C21 C20 Ir 119.4(5) . . ? C22 C21 C26 120.4(6) . . ? C22 C21 C20 117.9(6) . . ? C26 C21 C20 121.7(6) . . ? C21 C22 C23 118.6(6) . . ? C21 C22 P2 115.3(5) . . ? C23 C22 P2 126.1(5) . . ? C24 C23 C22 121.3(7) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C25 C24 C23 119.4(7) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C21 119.5(6) . . ? C25 C26 H26 120.3 . . ? C21 C26 H26 120.3 . . ? C32 C27 C28 118.2(6) . . ? C32 C27 P2 117.6(5) . . ? C28 C27 P2 124.2(5) . . ? C27 C28 C29 120.6(7) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C30 C29 C28 120.0(7) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 121.7(7) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C30 C31 C32 118.2(7) . . ? C30 C31 H31 120.9 . . ? C32 C31 H31 120.9 . . ? C27 C32 C31 121.3(6) . . ? C27 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C38 117.8(6) . . ? C34 C33 P2 124.0(5) . . ? C38 C33 P2 118.0(5) . . ? C33 C34 C35 120.7(6) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 121.3(7) . . ? C36 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? C35 C36 C37 118.8(7) . . ? C35 C36 H36 120.6 . . ? C37 C36 H36 120.6 . . ? C36 C37 C38 120.5(6) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C33 C38 C37 120.8(6) . . ? C33 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C46 122.2(7) . . ? C40 C39 Rh 71.0(4) . . ? C46 C39 Rh 111.7(5) . . ? C40 C39 H39 114.8 . . ? C46 C39 H39 114.8 . . ? Rh C39 H39 114.8 . . ? C39 C40 C41 124.6(7) . . ? C39 C40 Rh 69.5(4) . . ? C41 C40 Rh 113.0(5) . . ? C39 C40 H40 113.9 . . ? C41 C40 H40 113.9 . . ? Rh C40 H40 113.9 . . ? C42 C41 C40 115.2(7) . . ? C42 C41 H41A 108.5 . . ? C40 C41 H41A 108.5 . . ? C42 C41 H41B 108.5 . . ? C40 C41 H41B 108.5 . . ? H41A C41 H41B 107.5 . . ? C41 C42 C43 114.0(7) . . ? C41 C42 H42A 108.8 . . ? C43 C42 H42A 108.8 . . ? C41 C42 H42B 108.8 . . ? C43 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C42 123.3(7) . . ? C44 C43 Rh 69.4(4) . . ? C42 C43 Rh 114.4(5) . . ? C44 C43 H43 114.0 . . ? C42 C43 H43 114.0 . . ? Rh C43 H43 114.0 . . ? C43 C44 C45 124.8(7) . . ? C43 C44 Rh 71.6(4) . . ? C45 C44 Rh 112.3(5) . . ? C43 C44 H44 113.6 . . ? C45 C44 H44 113.6 . . ? Rh C44 H44 113.6 . . ? C46 C45 C44 113.5(7) . . ? C46 C45 H45A 108.9 . . ? C44 C45 H45A 108.9 . . ? C46 C45 H45B 108.9 . . ? C44 C45 H45B 108.9 . . ? H45A C45 H45B 107.7 . . ? C45 C46 C39 116.0(6) . . ? C45 C46 H46A 108.3 . . ? C39 C46 H46A 108.3 . . ? C45 C46 H46B 108.3 . . ? C39 C46 H46B 108.3 . . ? H46A C46 H46B 107.4 . . ? C1 Ir C20 93.6(2) . . ? C1 Ir P1 82.57(17) . . ? C20 Ir P1 166.56(16) . . ? C1 Ir P2 175.09(17) . . ? C20 Ir P2 82.08(18) . . ? P1 Ir P2 101.16(6) . . ? C1 Ir Cl 85.39(16) . . ? C20 Ir Cl 86.60(17) . . ? P1 Ir Cl 105.82(5) . . ? P2 Ir Cl 96.56(5) . . ? C1 Ir H1 101.8 . . ? C20 Ir H1 76.0 . . ? P1 Ir H1 92.1 . . ? P2 Ir H1 75.0 . . ? Cl Ir H1 161.5 . . ? C1 O1 Rh 124.3(4) . . ? C20 O2 Rh 123.8(4) . . ? C14 P1 C3 102.7(3) . . ? C14 P1 C8 104.4(3) . . ? C3 P1 C8 103.0(3) . . ? C14 P1 Ir 116.5(2) . . ? C3 P1 Ir 100.9(2) . . ? C8 P1 Ir 125.9(2) . . ? C22 P2 C27 107.2(3) . . ? C22 P2 C33 100.4(3) . . ? C27 P2 C33 103.6(3) . . ? C22 P2 Ir 101.4(2) . . ? C27 P2 Ir 118.6(2) . . ? C33 P2 Ir 122.99(19) . . ? O2 Rh C39 88.6(3) . . ? O2 Rh C44 163.2(2) . . ? C39 Rh C44 83.6(3) . . ? O2 Rh O1 89.95(16) . . ? C39 Rh O1 172.2(2) . . ? C44 Rh O1 95.8(2) . . ? O2 Rh C43 157.3(2) . . ? C39 Rh C43 94.6(3) . . ? C44 Rh C43 39.0(2) . . ? O1 Rh C43 89.7(2) . . ? O2 Rh C40 86.9(2) . . ? C39 Rh C40 39.5(2) . . ? C44 Rh C40 96.4(3) . . ? O1 Rh C40 148.0(2) . . ? C43 Rh C40 81.5(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 O1 C1 C2 C3 -161.4(5) . . . . ? Ir C1 C2 C3 16.7(7) . . . . ? O1 C1 C2 C7 16.9(8) . . . . ? Ir C1 C2 C7 -165.1(5) . . . . ? C7 C2 C3 C4 0.1(8) . . . . ? C1 C2 C3 C4 178.4(5) . . . . ? C7 C2 C3 P1 -176.9(4) . . . . ? C1 C2 C3 P1 1.5(7) . . . . ? C2 C3 C4 C5 2.3(9) . . . . ? P1 C3 C4 C5 179.0(5) . . . . ? C3 C4 C5 C6 -2.7(9) . . . . ? C4 C5 C6 C7 0.6(10) . . . . ? C3 C2 C7 C6 -2.1(9) . . . . ? C1 C2 C7 C6 179.6(6) . . . . ? C5 C6 C7 C2 1.8(9) . . . . ? C13 C8 C9 C10 0.6(10) . . . . ? P1 C8 C9 C10 -176.2(5) . . . . ? C8 C9 C10 C11 0.2(10) . . . . ? C9 C10 C11 C12 -0.8(11) . . . . ? C10 C11 C12 C13 0.4(12) . . . . ? C9 C8 C13 C12 -1.0(10) . . . . ? P1 C8 C13 C12 176.1(6) . . . . ? C11 C12 C13 C8 0.4(12) . . . . ? C19 C14 C15 C16 -1.9(10) . . . . ? P1 C14 C15 C16 -178.4(5) . . . . ? C14 C15 C16 C17 0.8(10) . . . . ? C15 C16 C17 C18 0.6(11) . . . . ? C16 C17 C18 C19 -0.8(11) . . . . ? C15 C14 C19 C18 1.7(9) . . . . ? P1 C14 C19 C18 178.2(5) . . . . ? C17 C18 C19 C14 -0.4(10) . . . . ? O2 C20 C21 C22 160.2(5) . . . . ? Ir C20 C21 C22 -16.6(7) . . . . ? O2 C20 C21 C26 -18.0(8) . . . . ? Ir C20 C21 C26 165.2(4) . . . . ? C26 C21 C22 C23 0.1(9) . . . . ? C20 C21 C22 C23 -178.1(5) . . . . ? C26 C21 C22 P2 179.0(4) . . . . ? C20 C21 C22 P2 0.8(7) . . . . ? C21 C22 C23 C24 0.2(10) . . . . ? P2 C22 C23 C24 -178.7(5) . . . . ? C22 C23 C24 C25 -0.2(11) . . . . ? C23 C24 C25 C26 0.0(11) . . . . ? C24 C25 C26 C21 0.3(10) . . . . ? C22 C21 C26 C25 -0.3(9) . . . . ? C20 C21 C26 C25 177.8(6) . . . . ? C32 C27 C28 C29 -0.1(10) . . . . ? P2 C27 C28 C29 178.5(5) . . . . ? C27 C28 C29 C30 -1.2(12) . . . . ? C28 C29 C30 C31 1.8(13) . . . . ? C29 C30 C31 C32 -1.1(12) . . . . ? C28 C27 C32 C31 0.8(10) . . . . ? P2 C27 C32 C31 -177.9(5) . . . . ? C30 C31 C32 C27 -0.2(11) . . . . ? C38 C33 C34 C35 0.5(11) . . . . ? P2 C33 C34 C35 -175.4(6) . . . . ? C33 C34 C35 C36 1.1(13) . . . . ? C34 C35 C36 C37 -2.2(13) . . . . ? C35 C36 C37 C38 1.8(12) . . . . ? C34 C33 C38 C37 -0.9(10) . . . . ? P2 C33 C38 C37 175.3(5) . . . . ? C36 C37 C38 C33 -0.2(11) . . . . ? C46 C39 C40 C41 0.3(11) . . . . ? Rh C39 C40 C41 104.4(7) . . . . ? C46 C39 C40 Rh -104.2(7) . . . . ? C39 C40 C41 C42 -64.9(10) . . . . ? Rh C40 C41 C42 15.4(9) . . . . ? C40 C41 C42 C43 -9.7(10) . . . . ? C41 C42 C43 C44 80.0(10) . . . . ? C41 C42 C43 Rh -0.5(9) . . . . ? C42 C43 C44 C45 -1.5(11) . . . . ? Rh C43 C44 C45 104.8(7) . . . . ? C42 C43 C44 Rh -106.3(7) . . . . ? C43 C44 C45 C46 -64.4(11) . . . . ? Rh C44 C45 C46 18.2(10) . . . . ? C44 C45 C46 C39 -10.3(12) . . . . ? C40 C39 C46 C45 78.1(10) . . . . ? Rh C39 C46 C45 -2.5(10) . . . . ? O1 C1 Ir C20 -35.8(6) . . . . ? C2 C1 Ir C20 146.6(4) . . . . ? O1 C1 Ir P1 157.1(5) . . . . ? C2 C1 Ir P1 -20.5(4) . . . . ? O1 C1 Ir P2 -63(2) . . . . ? C2 C1 Ir P2 119.2(19) . . . . ? O1 C1 Ir Cl 50.5(5) . . . . ? C2 C1 Ir Cl -127.1(4) . . . . ? O2 C20 Ir C1 24.8(5) . . . . ? C21 C20 Ir C1 -159.0(4) . . . . ? O2 C20 Ir P1 97.5(9) . . . . ? C21 C20 Ir P1 -86.3(9) . . . . ? O2 C20 Ir P2 -157.5(5) . . . . ? C21 C20 Ir P2 18.7(4) . . . . ? O2 C20 Ir Cl -60.4(5) . . . . ? C21 C20 Ir Cl 115.8(4) . . . . ? C2 C1 O1 Rh 176.7(3) . . . . ? Ir C1 O1 Rh -1.0(7) . . . . ? C21 C20 O2 Rh -155.3(3) . . . . ? Ir C20 O2 Rh 21.2(7) . . . . ? C19 C14 P1 C3 33.4(6) . . . . ? C15 C14 P1 C3 -150.3(5) . . . . ? C19 C14 P1 C8 140.7(5) . . . . ? C15 C14 P1 C8 -43.0(6) . . . . ? C19 C14 P1 Ir -75.8(5) . . . . ? C15 C14 P1 Ir 100.6(5) . . . . ? C2 C3 P1 C14 -135.2(4) . . . . ? C4 C3 P1 C14 48.1(6) . . . . ? C2 C3 P1 C8 116.5(5) . . . . ? C4 C3 P1 C8 -60.3(6) . . . . ? C2 C3 P1 Ir -14.6(4) . . . . ? C4 C3 P1 Ir 168.6(5) . . . . ? C9 C8 P1 C14 -27.5(6) . . . . ? C13 C8 P1 C14 155.6(5) . . . . ? C9 C8 P1 C3 79.6(6) . . . . ? C13 C8 P1 C3 -97.3(5) . . . . ? C9 C8 P1 Ir -166.5(4) . . . . ? C13 C8 P1 Ir 16.7(6) . . . . ? C1 Ir P1 C14 127.4(3) . . . . ? C20 Ir P1 C14 53.4(8) . . . . ? P2 Ir P1 C14 -49.4(2) . . . . ? Cl Ir P1 C14 -149.6(2) . . . . ? C1 Ir P1 C3 17.1(2) . . . . ? C20 Ir P1 C3 -56.8(8) . . . . ? P2 Ir P1 C3 -159.63(19) . . . . ? Cl Ir P1 C3 100.18(19) . . . . ? C1 Ir P1 C8 -97.8(3) . . . . ? C20 Ir P1 C8 -171.8(8) . . . . ? P2 Ir P1 C8 85.4(2) . . . . ? Cl Ir P1 C8 -14.8(2) . . . . ? C21 C22 P2 C27 -113.4(5) . . . . ? C23 C22 P2 C27 65.5(6) . . . . ? C21 C22 P2 C33 138.7(4) . . . . ? C23 C22 P2 C33 -42.5(6) . . . . ? C21 C22 P2 Ir 11.7(5) . . . . ? C23 C22 P2 Ir -169.5(5) . . . . ? C32 C27 P2 C22 155.6(5) . . . . ? C28 C27 P2 C22 -23.0(7) . . . . ? C32 C27 P2 C33 -98.7(5) . . . . ? C28 C27 P2 C33 82.6(6) . . . . ? C32 C27 P2 Ir 41.7(6) . . . . ? C28 C27 P2 Ir -136.9(5) . . . . ? C34 C33 P2 C22 115.8(6) . . . . ? C38 C33 P2 C22 -60.0(5) . . . . ? C34 C33 P2 C27 5.1(7) . . . . ? C38 C33 P2 C27 -170.8(5) . . . . ? C34 C33 P2 Ir -133.1(5) . . . . ? C38 C33 P2 Ir 51.0(6) . . . . ? C1 Ir P2 C22 13(2) . . . . ? C20 Ir P2 C22 -14.8(3) . . . . ? P1 Ir P2 C22 152.0(2) . . . . ? Cl Ir P2 C22 -100.4(2) . . . . ? C1 Ir P2 C27 130(2) . . . . ? C20 Ir P2 C27 102.2(3) . . . . ? P1 Ir P2 C27 -91.0(2) . . . . ? Cl Ir P2 C27 16.6(2) . . . . ? C1 Ir P2 C33 -98(2) . . . . ? C20 Ir P2 C33 -125.3(3) . . . . ? P1 Ir P2 C33 41.4(2) . . . . ? Cl Ir P2 C33 149.1(2) . . . . ? C20 O2 Rh C39 119.8(5) . . . . ? C20 O2 Rh C44 57.6(10) . . . . ? C20 O2 Rh O1 -52.6(5) . . . . ? C20 O2 Rh C43 -141.7(6) . . . . ? C20 O2 Rh C40 159.2(5) . . . . ? C40 C39 Rh O2 86.8(4) . . . . ? C46 C39 Rh O2 -155.2(6) . . . . ? C40 C39 Rh C44 -108.1(5) . . . . ? C46 C39 Rh C44 9.9(6) . . . . ? C40 C39 Rh O1 166.0(16) . . . . ? C46 C39 Rh O1 -76(2) . . . . ? C40 C39 Rh C43 -70.6(5) . . . . ? C46 C39 Rh C43 47.4(6) . . . . ? C46 C39 Rh C40 118.0(8) . . . . ? C43 C44 Rh O2 168.3(6) . . . . ? C45 C44 Rh O2 47.3(11) . . . . ? C43 C44 Rh C39 105.4(5) . . . . ? C45 C44 Rh C39 -15.5(6) . . . . ? C43 C44 Rh O1 -82.4(4) . . . . ? C45 C44 Rh O1 156.7(6) . . . . ? C45 C44 Rh C43 -121.0(8) . . . . ? C43 C44 Rh C40 68.0(5) . . . . ? C45 C44 Rh C40 -53.0(6) . . . . ? C1 O1 Rh O2 42.1(5) . . . . ? C1 O1 Rh C39 -37(2) . . . . ? C1 O1 Rh C44 -122.1(5) . . . . ? C1 O1 Rh C43 -160.6(5) . . . . ? C1 O1 Rh C40 126.1(5) . . . . ? C44 C43 Rh O2 -171.3(5) . . . . ? C42 C43 Rh O2 -53.0(9) . . . . ? C44 C43 Rh C39 -73.9(5) . . . . ? C42 C43 Rh C39 44.3(6) . . . . ? C42 C43 Rh C44 118.3(7) . . . . ? C44 C43 Rh O1 99.6(4) . . . . ? C42 C43 Rh O1 -142.2(5) . . . . ? C44 C43 Rh C40 -111.3(5) . . . . ? C42 C43 Rh C40 7.0(5) . . . . ? C39 C40 Rh O2 -91.5(5) . . . . ? C41 C40 Rh O2 148.4(5) . . . . ? C41 C40 Rh C39 -120.0(8) . . . . ? C39 C40 Rh C44 71.9(5) . . . . ? C41 C40 Rh C44 -48.1(6) . . . . ? C39 C40 Rh O1 -176.4(4) . . . . ? C41 C40 Rh O1 63.5(7) . . . . ? C39 C40 Rh C43 108.0(5) . . . . ? C41 C40 Rh C43 -12.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.226 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.140