Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_R-3 _database_code_CSD 161686 _publ_contact_author 'Tani, Kazuhide' _publ_contact_author_address ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka, Osaka, 560-8531 Japan ; _publ_contact_author_email tani@chem.es.osaka-u.ac.jp _publ_contact_author_phone ' +81 6 850 6245' _publ_contact_author_fax ' +81 6 850 6296' loop_ _publ_author_name 'Tani, Kazuhide' 'Nakajima, Kouji' 'Iseki, Aika' 'Yamagata, Tsuneaki' _journal_name_full ? _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ; ? ; _ccdc_temp_data_collection ? _ccdc_ls_R_squared ? _ccdc_disorder ? _ccdc_comments ; ? ; _audit_creation_date 2001-06-05T21:52:16-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _chemical_name_systematic ; ? ; _chemical_formula_sum 'C62 H47 Cl Ir P3' _chemical_formula_weight 1112.56 _chemical_melting_point 503-513 #(in capillary under vacuum) _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M P31 _symmetry_space_group_name_Hall 'P 31' _symmetry_Int_Tables_number 144 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' _cell_length_a 18.579(5) _cell_length_b 18.579 _cell_length_c 13.368(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3996(2) _cell_formula_units_Z 3 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 17 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.1 _exptl_crystal_description 'triganal prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1674 _exptl_special_details ; \w scan width (1.15 + 0.30tan\q) deg, \w scan rate 16.0 deg/min. The ratio of peak counting time to background counting time was 2:1. The diameter of the incident beam collimeter was 1.0 mm, the crystal to detector distance was 235 mm, and the detector aperture was 9.0 x 13.0 mm (horizontal x vertical). ; _exptl_absorpt_coefficient_mu 2.684 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '( North, Phillips, & Mathews (1968), Acta Cryst. A24, 351-359. )' _exptl_absorpt_correction_T_min 0.2958 _exptl_absorpt_correction_T_max 0.4998 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type AFC7R _diffrn_measurement_method \w-2\t _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 24.94 _diffrn_reflns_number 13348 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_unetI/netI 0.0534 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 12250 _reflns_number_gt 9697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC/AFC7R Diffractometer Control' _computing_cell_refinement 'MSC/AFC7R Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution 'SIR97(Cascarano al.,Acta Cryst.,1996,A52,C-79)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'WINGX' # Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. WINGX Main Reference # ORTEP-III(version 1.0.2) - Burnett, M. N. & Johnson, C.K.(1996) # Report ORNL-6895. # A FORTRAN Thermal-Ellipsoid Plot Program, # Oak Ridge National Laboratory, Oak Ridge, Tennessee, U.S # Ortep-3 for Windows, Version 1.05. _computing_publication_material 'SHELXL-97, WinGX, and, and modified' _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^)+(0.0973P)^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_number_reflns 12250 _refine_ls_number_parameters 581 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1429 _refine_ls_wR_factor_gt 0.1288 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(7) _refine_diff_density_max 1.513 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.135 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 0 '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' 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' 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 0.249656(16) 0.938340(16) 0.3333 0.03970(9) Uani 1 1 d . . . Cl Cl 0.15186(15) 0.84658(19) 0.4545(2) 0.0751(8) Uani 1 1 d . . . P1 P 0.34133(11) 1.05529(12) 0.26166(14) 0.0355(4) Uani 1 1 d . . . P2 P 0.35078(13) 0.93211(13) 0.42266(16) 0.0422(4) Uani 1 1 d . . . P3 P 0.14260(13) 0.89611(14) 0.21988(16) 0.0485(5) Uani 1 1 d . . . C1 C 0.4152(5) 1.1241(4) 0.3585(6) 0.0367(15) Uani 1 1 d . . . C2 C 0.3964(6) 1.1789(5) 0.4124(7) 0.0519(19) Uani 1 1 d . . . H2 H 0.351 1.1833 0.3916 0.062 Uiso 1 1 calc R . . C3 C 0.4405(6) 1.2248(6) 0.4921(7) 0.059(2) Uani 1 1 d . . . H3 H 0.4257 1.2597 0.5248 0.071 Uiso 1 1 calc R . . C4 C 0.5086(7) 1.2184(6) 0.5239(7) 0.060(3) Uani 1 1 d . . . C5 C 0.5542(7) 1.2630(7) 0.6118(9) 0.076(3) Uani 1 1 d . . . H5 H 0.538 1.2955 0.6475 0.091 Uiso 1 1 calc R . . C6 C 0.6224(8) 1.2569(9) 0.6430(9) 0.094(5) Uani 1 1 d . . . H6 H 0.6515 1.2854 0.6999 0.113 Uiso 1 1 calc R . . C7 C 0.6479(6) 1.2085(9) 0.5895(9) 0.080(3) Uani 1 1 d . . . H7 H 0.6949 1.2071 0.6106 0.096 Uiso 1 1 calc R . . C8 C 0.6049(6) 1.1623(8) 0.5057(8) 0.068(3) Uani 1 1 d . . . H8 H 0.6214 1.1289 0.4727 0.082 Uiso 1 1 calc R . . C9 C 0.5350(5) 1.1677(5) 0.4718(7) 0.052(2) Uani 1 1 d . . . C10 C 0.4848(4) 1.1195(5) 0.3871(6) 0.0407(16) Uani 1 1 d . . . C11 C 0.5041(5) 1.0580(5) 0.3413(6) 0.0433(16) Uani 1 1 d . . . C12 C 0.5793(5) 1.0857(6) 0.2837(6) 0.0482(18) Uani 1 1 d . . . C13 C 0.6353(5) 1.1719(6) 0.2652(7) 0.057(2) Uani 1 1 d . . . H13 H 0.6237 1.2114 0.2913 0.069 Uiso 1 1 calc R . . C14 C 0.7057(7) 1.1970(8) 0.2095(9) 0.075(3) Uani 1 1 d . . . H14 H 0.7427 1.2533 0.2 0.091 Uiso 1 1 calc R . . C15 C 0.7218(7) 1.1386(8) 0.1675(8) 0.075(3) Uani 1 1 d . . . H15 H 0.7686 1.156 0.1277 0.09 Uiso 1 1 calc R . . C16 C 0.6699(6) 1.0560(7) 0.1836(8) 0.067(3) Uani 1 1 d . . . H16 H 0.6826 1.0179 0.1558 0.08 Uiso 1 1 calc R . . C17 C 0.5974(6) 1.0272(6) 0.2414(7) 0.054(2) Uani 1 1 d . . . C18 C 0.5394(7) 0.9394(8) 0.2565(8) 0.065(3) Uani 1 1 d . . . H18 H 0.549 0.8995 0.2273 0.078 Uiso 1 1 calc R . . C19 C 0.4726(6) 0.9168(6) 0.3124(7) 0.056(2) Uani 1 1 d . . . H19 H 0.4373 0.8601 0.3223 0.067 Uiso 1 1 calc R . . C20 C 0.4508(5) 0.9707(5) 0.3577(7) 0.0469(17) Uani 1 1 d . . . C21 C 0.2958(5) 1.1172(5) 0.2165(6) 0.0469(17) Uani 1 1 d . . . C22 C 0.3239(7) 1.1701(6) 0.1340(8) 0.065(3) Uani 1 1 d . . . H22 H 0.3678 1.1755 0.0951 0.078 Uiso 1 1 calc R . . C23 C 0.2834(10) 1.2154(9) 0.1115(11) 0.091(4) Uani 1 1 d . . . H23 H 0.3033 1.2512 0.0569 0.11 Uiso 1 1 calc R . . C24 C 0.2186(8) 1.2118(8) 0.1615(11) 0.079(3) Uani 1 1 d . . . H24 H 0.1945 1.2432 0.1428 0.095 Uiso 1 1 calc R . . C25 C 0.1892(8) 1.1559(8) 0.2459(8) 0.072(3) Uani 1 1 d . . . H25 H 0.1447 1.1506 0.2835 0.086 Uiso 1 1 calc R . . C26 C 0.2272(6) 1.1096(7) 0.2716(7) 0.055(2) Uani 1 1 d . . . H26 H 0.2071 1.0733 0.3257 0.066 Uiso 1 1 calc R . . C27 C 0.4117(5) 1.0652(5) 0.1596(6) 0.0402(15) Uani 1 1 d . . . C28 C 0.4743(5) 1.1411(6) 0.1280(7) 0.053(2) Uani 1 1 d . . . H28 H 0.4831 1.1882 0.1628 0.063 Uiso 1 1 calc R . . C29 C 0.5240(7) 1.1510(8) 0.0484(8) 0.070(3) Uani 1 1 d . . . H29 H 0.5653 1.2033 0.0275 0.084 Uiso 1 1 calc R . . C30 C 0.5094(7) 1.0761(8) -0.0019(7) 0.074(3) Uani 1 1 d . . . H30 H 0.5403 1.0804 -0.0586 0.088 Uiso 1 1 calc R . . C31 C 0.4506(8) 0.9980(8) 0.0319(9) 0.079(3) Uani 1 1 d . . . H31 H 0.4441 0.95 0.0017 0.095 Uiso 1 1 calc R . . C32 C 0.4001(5) 0.9940(6) 0.1150(6) 0.0485(19) Uani 1 1 d . . . H32 H 0.3592 0.9427 0.1389 0.058 Uiso 1 1 calc R . . C33 C 0.3791(5) 0.9817(5) 0.5466(6) 0.0479(18) Uani 1 1 d . . . C34 C 0.3257(6) 1.0058(6) 0.5891(7) 0.057(2) Uani 1 1 d . . . H34 H 0.2782 0.996 0.5545 0.068 Uiso 1 1 calc R . . C35 C 0.3420(8) 1.0435(9) 0.6802(8) 0.076(3) Uani 1 1 d . . . H35 H 0.3055 1.0579 0.7094 0.091 Uiso 1 1 calc R . . C36 C 0.4190(10) 1.0607(9) 0.7307(9) 0.105(5) Uani 1 1 d . . . H36 H 0.4329 1.0888 0.7915 0.126 Uiso 1 1 calc R . . C37 C 0.4700(8) 1.0364(9) 0.6904(9) 0.080(3) Uani 1 1 d . . . H37 H 0.5172 1.0451 0.7249 0.096 Uiso 1 1 calc R . . C38 C 0.4517(6) 0.9983(7) 0.5969(7) 0.064(2) Uani 1 1 d . . . H38 H 0.4881 0.9837 0.5677 0.077 Uiso 1 1 calc R . . C39 C 0.3197(7) 0.8239(6) 0.4460(8) 0.065(3) Uani 1 1 d . . . C40 C 0.2691(9) 0.7644(7) 0.3798(11) 0.086(4) Uani 1 1 d . . . H40 H 0.2517 0.7804 0.3231 0.103 Uiso 1 1 calc R . . C41 C 0.2419(10) 0.6788(8) 0.3935(17) 0.112(6) Uani 1 1 d . . . H41 H 0.2075 0.6417 0.3448 0.134 Uiso 1 1 calc R . . C42 C 0.2610(15) 0.6500(11) 0.466(2) 0.139(10) Uani 1 1 d . . . H42 H 0.242 0.5935 0.473 0.167 Uiso 1 1 calc R . . C43 C 0.3100(14) 0.7052(14) 0.5325(18) 0.145(10) Uani 1 1 d . . . H43 H 0.3257 0.6854 0.5874 0.174 Uiso 1 1 calc R . . C44 C 0.3427(10) 0.7966(9) 0.5273(12) 0.097(4) Uani 1 1 d . . . H44 H 0.3767 0.8326 0.5769 0.116 Uiso 1 1 calc R . . C45 C 0.1617(5) 0.9476(6) 0.0952(6) 0.053(2) Uani 1 1 d . . . C46 C 0.1268(6) 0.9935(7) 0.0691(7) 0.063(2) Uani 1 1 d . . . H46 H 0.0894 0.9971 0.1123 0.076 Uiso 1 1 calc R . . C47 C 0.1463(8) 1.0355(8) -0.0216(8) 0.080(3) Uani 1 1 d . . . H47 H 0.1225 1.0676 -0.0387 0.096 Uiso 1 1 calc R . . C48 C 0.2001(8) 1.0299(10) -0.0853(9) 0.091(4) Uani 1 1 d . . . H48 H 0.2142 1.0585 -0.1458 0.11 Uiso 1 1 calc R . . C49 C 0.2329(8) 0.9820(11) -0.0593(9) 0.097(5) Uani 1 1 d . . . H49 H 0.2676 0.9752 -0.1036 0.117 Uiso 1 1 calc R . . C50 C 0.2155(7) 0.9435(9) 0.0315(8) 0.083(4) Uani 1 1 d . . . H50 H 0.2414 0.9138 0.0498 0.1 Uiso 1 1 calc R . . C51 C 0.0418(6) 0.8881(6) 0.2558(7) 0.058(2) Uani 1 1 d . . . C52 C 0.0367(7) 0.9206(7) 0.3436(8) 0.065(3) Uani 1 1 d . . . H52 H 0.0827 0.946 0.3856 0.078 Uiso 1 1 calc R . . C53 C -0.0393(7) 0.9158(9) 0.3716(11) 0.090(4) Uani 1 1 d . . . H53 H -0.0444 0.9399 0.4303 0.108 Uiso 1 1 calc R . . C54 C -0.1060(7) 0.8729(9) 0.3060(13) 0.091(4) Uani 1 1 d . . . H54 H -0.1573 0.8672 0.3221 0.109 Uiso 1 1 calc R . . C55 C -0.0983(7) 0.8402(9) 0.2217(11) 0.086(4) Uani 1 1 d . . . H55 H -0.1437 0.8119 0.1795 0.103 Uiso 1 1 calc R . . C56 C -0.0280(7) 0.8476(8) 0.1982(8) 0.074(3) Uani 1 1 d . . . H56 H -0.0244 0.8239 0.1385 0.088 Uiso 1 1 calc R . . C57 C 0.1093(7) 0.7876(7) 0.1904(8) 0.072(3) Uani 1 1 d D . . C58 C 0.1582(19) 0.766(2) 0.127(2) 0.237(10) Uiso 1 1 d D . . H58 H 0.2014 0.8055 0.0878 0.285 Uiso 1 1 calc R . . C59 C 0.136(2) 0.677(2) 0.126(3) 0.237(10) Uiso 1 1 d D . . H59 H 0.1702 0.661 0.0932 0.285 Uiso 1 1 calc R . . C60 C 0.065(2) 0.618(3) 0.174(3) 0.237(10) Uiso 1 1 d D . . H60 H 0.0421 0.5621 0.1581 0.285 Uiso 1 1 calc R . . C61 C 0.0275(17) 0.6446(17) 0.249(2) 0.163(9) Uiso 1 1 d D . . H61 H -0.0103 0.6066 0.2949 0.196 Uiso 1 1 calc R . . C62 C 0.0480(13) 0.7262(10) 0.2528(17) 0.147(9) Uani 1 1 d D . . H62 H 0.0205 0.7419 0.2981 0.176 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 0.03738(16) 0.03813(16) 0.03348(12) 0.00263(12) 0.00161(13) 0.01130(13) Cl 0.0494(12) 0.0884(19) 0.0656(15) 0.0309(14) 0.0087(11) 0.0181(12) P1 0.0346(9) 0.0326(8) 0.0327(9) 0.0008(7) 0.0044(7) 0.0119(7) P2 0.0451(11) 0.0415(10) 0.0400(10) 0.0060(8) 0.0053(8) 0.0218(9) P3 0.0415(10) 0.0500(12) 0.0363(10) 0.0011(9) -0.0024(8) 0.0095(9) C1 0.040(4) 0.027(3) 0.038(4) 0.003(3) 0.003(3) 0.012(3) C2 0.064(5) 0.046(4) 0.048(5) -0.007(4) 0.002(4) 0.029(4) C3 0.064(5) 0.048(5) 0.051(5) -0.015(4) -0.001(4) 0.018(4) C4 0.067(6) 0.043(5) 0.041(4) -0.007(4) 0.010(4) 0.006(4) C5 0.071(7) 0.061(6) 0.061(6) -0.015(5) -0.009(5) 0.008(5) C6 0.063(7) 0.104(10) 0.056(6) -0.015(6) -0.007(5) -0.003(7) C7 0.043(5) 0.110(10) 0.066(6) -0.007(6) -0.011(5) 0.022(6) C8 0.047(5) 0.090(8) 0.057(6) 0.000(5) -0.010(4) 0.026(5) C9 0.039(4) 0.044(4) 0.053(5) -0.004(4) 0.001(3) 0.005(3) C10 0.026(3) 0.036(4) 0.046(4) -0.001(3) 0.002(3) 0.005(3) C11 0.043(4) 0.039(4) 0.045(4) 0.000(3) -0.001(3) 0.018(3) C12 0.039(4) 0.057(5) 0.047(4) 0.001(4) 0.003(3) 0.023(4) C13 0.045(4) 0.065(5) 0.048(5) 0.008(4) 0.010(4) 0.017(4) C14 0.062(6) 0.076(7) 0.072(7) -0.003(6) 0.008(5) 0.023(5) C15 0.048(5) 0.099(8) 0.065(6) -0.001(6) 0.012(5) 0.028(6) C16 0.050(5) 0.084(7) 0.074(6) -0.006(5) 0.009(5) 0.039(5) C17 0.050(5) 0.071(6) 0.052(5) 0.005(4) 0.002(4) 0.039(4) C18 0.070(6) 0.086(7) 0.053(5) 0.000(5) 0.012(5) 0.050(6) C19 0.060(5) 0.048(5) 0.065(5) 0.003(4) 0.004(4) 0.031(4) C20 0.040(4) 0.052(4) 0.047(4) -0.005(4) 0.003(3) 0.021(4) C21 0.048(4) 0.048(4) 0.043(4) -0.004(3) 0.002(3) 0.024(4) C22 0.075(6) 0.061(6) 0.060(6) 0.019(4) 0.014(5) 0.034(5) C23 0.116(11) 0.094(9) 0.087(9) 0.033(7) 0.011(8) 0.070(9) C24 0.094(9) 0.077(7) 0.085(8) -0.004(6) -0.009(7) 0.057(7) C25 0.079(7) 0.096(8) 0.066(6) -0.005(6) 0.010(5) 0.063(7) C26 0.058(5) 0.075(6) 0.045(5) 0.000(4) 0.003(4) 0.042(5) C27 0.037(4) 0.045(4) 0.039(4) 0.000(3) 0.004(3) 0.020(3) C28 0.049(5) 0.060(5) 0.045(4) 0.006(4) 0.008(4) 0.025(4) C29 0.056(5) 0.092(8) 0.055(6) 0.018(5) 0.017(4) 0.032(5) C30 0.073(7) 0.110(9) 0.046(5) 0.015(5) 0.028(5) 0.052(7) C31 0.092(8) 0.090(8) 0.068(7) -0.022(6) 0.010(6) 0.056(7) C32 0.050(4) 0.056(5) 0.038(4) -0.005(3) 0.006(3) 0.025(4) C33 0.053(4) 0.051(5) 0.041(4) 0.011(3) 0.005(3) 0.027(4) C34 0.051(5) 0.077(6) 0.041(4) -0.001(4) -0.002(4) 0.031(5) C35 0.078(7) 0.111(9) 0.051(6) -0.009(6) 0.005(5) 0.056(7) C36 0.126(12) 0.096(10) 0.042(6) -0.009(6) -0.021(7) 0.017(9) C37 0.070(7) 0.107(9) 0.059(6) 0.007(6) -0.008(5) 0.042(7) C38 0.064(6) 0.081(7) 0.051(5) 0.013(5) -0.009(4) 0.039(5) C39 0.071(6) 0.053(5) 0.074(7) 0.013(5) 0.019(5) 0.035(5) C40 0.094(9) 0.047(6) 0.103(10) -0.005(6) 0.026(7) 0.025(6) C41 0.109(12) 0.042(6) 0.174(17) 0.004(8) 0.054(12) 0.030(7) C42 0.149(19) 0.071(10) 0.21(3) 0.050(14) 0.098(18) 0.065(12) C43 0.17(2) 0.145(17) 0.17(2) 0.119(17) 0.082(17) 0.117(17) C44 0.108(11) 0.080(8) 0.112(11) 0.031(8) 0.018(9) 0.054(8) C45 0.042(4) 0.073(6) 0.032(4) 0.002(4) -0.008(3) 0.019(4) C46 0.057(5) 0.075(6) 0.049(5) 0.006(5) -0.001(4) 0.027(5) C47 0.072(7) 0.093(8) 0.060(6) 0.026(6) 0.009(5) 0.031(6) C48 0.074(7) 0.131(12) 0.051(6) 0.033(7) -0.001(5) 0.038(8) C49 0.073(8) 0.170(15) 0.052(6) 0.013(8) 0.017(5) 0.064(9) C50 0.067(6) 0.133(11) 0.054(6) 0.031(6) 0.012(5) 0.054(7) C51 0.040(4) 0.062(5) 0.052(5) 0.005(4) 0.003(4) 0.010(4) C52 0.059(6) 0.064(6) 0.058(6) 0.005(5) 0.012(5) 0.021(5) C53 0.059(7) 0.100(9) 0.097(9) 0.030(7) 0.039(7) 0.029(7) C54 0.045(6) 0.091(9) 0.127(12) 0.044(8) 0.013(7) 0.026(6) C55 0.042(5) 0.104(10) 0.080(8) 0.033(7) 0.005(5) 0.014(6) C56 0.051(5) 0.097(8) 0.053(5) 0.009(6) 0.005(5) 0.023(5) C57 0.074(7) 0.058(6) 0.056(6) -0.018(4) -0.011(5) 0.012(5) C62 0.163(19) 0.058(8) 0.19(2) 0.032(11) 0.063(16) 0.033(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) - 15.9816 (0.0634) x + 6.1457 (0.0968) y + 6.6421 (0.0785) z = 2.9185 (0.0765) * -0.0020 (0.0089) C39 * 0.0004 (0.0094) C40 * 0.0003 (0.0115) C41 * 0.0009 (0.0142) C42 * -0.0026 (0.0140) C43 * 0.0030 (0.0106) C44 Rms deviation of fitted atoms = 0.0018 1.2142 (0.0929) x + 13.7025 (0.0642) y - 6.0489 (0.0574) z = 10.6094 (0.0734) Angle to previous plane (with approximate esd) = 67.48 ( 0.47 ) * -0.0039 (0.0066) C33 * 0.0052 (0.0079) C34 * -0.0098 (0.0094) C35 * 0.0138 (0.0100) C36 * -0.0129 (0.0094) C37 * 0.0076 (0.0077) C38 Rms deviation of fitted atoms = 0.0096 4.4040 (0.0467) x + 10.1812 (0.0478) y - 7.9250 (0.0254) z = 10.4755 (0.0482) Angle to previous plane (with approximate esd) = 14.48 ( 0.62 ) * -0.0434 (0.0063) C1 * 0.0041 (0.0074) C2 * 0.0345 (0.0079) C3 * 0.0179 (0.0084) C4 * -0.0252 (0.0092) C5 * -0.0328 (0.0102) C6 * 0.0099 (0.0099) C7 * 0.0151 (0.0088) C8 * 0.0300 (0.0080) C9 * -0.0102 (0.0067) C10 Rms deviation of fitted atoms = 0.0254 10.5465 (0.0399) x - 4.7135 (0.0532) y + 10.9953 (0.0197) z = 4.0986 (0.0448) Angle to previous plane (with approximate esd) = 70.96 ( 0.21 ) * -0.0172 (0.0069) C11 * 0.0125 (0.0078) C12 * -0.0065 (0.0079) C13 * 0.0059 (0.0095) C14 * -0.0117 (0.0094) C15 * 0.0073 (0.0092) C16 * 0.0147 (0.0086) C17 * -0.0173 (0.0087) C18 * -0.0003 (0.0082) C19 * 0.0126 (0.0074) C20 Rms deviation of fitted atoms = 0.0118 - 14.5648 (0.0495) x + 7.9793 (0.0763) y - 8.2787 (0.0452) z = 1.1571 (0.0776) Angle to previous plane (with approximate esd) = 17.65 ( 0.43 ) * 0.0249 (0.0060) C27 * -0.0193 (0.0068) C28 * -0.0063 (0.0074) C29 * 0.0260 (0.0085) C30 * -0.0200 (0.0084) C31 * -0.0054 (0.0070) C32 Rms deviation of fitted atoms = 0.0189 5.6177 (0.0831) x + 9.1513 (0.0763) y + 7.9760 (0.0563) z = 13.6029 (0.0673) Angle to previous plane (with approximate esd) = 54.94 ( 0.41 ) * 0.0091 (0.0069) C21 * -0.0067 (0.0084) C22 * 0.0007 (0.0103) C23 * 0.0028 (0.0095) C24 * -0.0004 (0.0085) C25 * -0.0056 (0.0076) C26 Rms deviation of fitted atoms = 0.0053 7.7738 (0.0971) x + 9.0140 (0.0914) y + 5.7030 (0.0631) z = 10.3436 (0.0755) Angle to previous plane (with approximate esd) = 12.29 ( 0.90 ) * -0.0022 (0.0078) C45 * -0.0082 (0.0081) C46 * 0.0048 (0.0095) C47 * 0.0089 (0.0103) C48 * -0.0195 (0.0107) C49 * 0.0162 (0.0098) C50 Rms deviation of fitted atoms = 0.0117 ; 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 P1 2.1998(19) . ? Ir P2 2.277(2) . ? Ir P3 2.305(2) . ? Ir Cl 2.394(2) . ? P1 C27 1.834(8) . ? P1 C21 1.837(9) . ? P1 C1 1.855(8) . ? P2 C39 1.820(10) . ? P2 C33 1.840(9) . ? P2 C20 1.841(8) . ? P3 C57 1.831(11) . ? P3 C45 1.865(9) . ? P3 C51 1.866(10) . ? C1 C10 1.391(11) . ? C1 C2 1.425(11) . ? C2 C3 1.354(12) . ? C2 H2 0.93 . ? C3 C4 1.394(16) . ? C3 H3 0.93 . ? C4 C9 1.440(14) . ? C4 C5 1.444(13) . ? C5 C6 1.39(2) . ? C5 H5 0.93 . ? C6 C7 1.40(2) . ? C6 H6 0.93 . ? C7 C8 1.394(15) . ? C7 H7 0.93 . ? C8 C9 1.425(15) . ? C8 H8 0.93 . ? C9 C10 1.456(11) . ? C10 C11 1.488(11) . ? C11 C20 1.433(11) . ? C11 C12 1.446(11) . ? C12 C17 1.408(13) . ? C12 C13 1.428(13) . ? C13 C14 1.369(14) . ? C13 H13 0.93 . ? C14 C15 1.380(17) . ? C14 H14 0.93 . ? C15 C16 1.360(17) . ? C15 H15 0.93 . ? C16 C17 1.405(13) . ? C16 H16 0.93 . ? C17 C18 1.451(15) . ? C18 C19 1.325(14) . ? C18 H18 0.93 . ? C19 C20 1.393(12) . ? C19 H19 0.93 . ? C21 C22 1.394(12) . ? C21 C26 1.416(12) . ? C22 C23 1.413(16) . ? C22 H22 0.93 . ? C23 C24 1.348(19) . ? C23 H23 0.93 . ? C24 C25 1.443(18) . ? C24 H24 0.93 . ? C25 C26 1.402(14) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C27 C32 1.365(12) . ? C27 C28 1.371(12) . ? C28 C29 1.360(12) . ? C28 H28 0.93 . ? C29 C30 1.444(17) . ? C29 H29 0.93 . ? C30 C31 1.384(18) . ? C30 H30 0.93 . ? C31 C32 1.432(13) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? C33 C38 1.396(13) . ? C33 C34 1.397(13) . ? C34 C35 1.361(14) . ? C34 H34 0.93 . ? C35 C36 1.46(2) . ? C35 H35 0.93 . ? C36 C37 1.35(2) . ? C36 H36 0.93 . ? C37 C38 1.393(16) . ? C37 H37 0.93 . ? C38 H38 0.93 . ? C39 C44 1.356(18) . ? C39 C40 1.360(17) . ? C40 C41 1.419(18) . ? C40 H40 0.93 . ? C41 C42 1.24(3) . ? C41 H41 0.93 . ? C42 C43 1.32(3) . ? C42 H42 0.93 . ? C43 C44 1.49(3) . ? C43 H43 0.93 . ? C44 H44 0.93 . ? C45 C50 1.342(15) . ? C45 C46 1.353(15) . ? C46 C47 1.388(14) . ? C46 H46 0.93 . ? C47 C48 1.358(19) . ? C47 H47 0.93 . ? C48 C49 1.35(2) . ? C48 H48 0.93 . ? C49 C50 1.363(16) . ? C49 H49 0.93 . ? C50 H50 0.93 . ? C51 C52 1.345(14) . ? C51 C56 1.365(14) . ? C52 C53 1.421(16) . ? C52 H52 0.93 . ? C53 C54 1.40(2) . ? C53 H53 0.93 . ? C54 C55 1.32(2) . ? C54 H54 0.93 . ? C55 C56 1.281(17) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C57 C62 1.41(2) . ? C57 C58 1.44(2) . ? C58 C59 1.49(3) . ? C58 H58 0.93 . ? C59 C60 1.38(5) . ? C59 H59 0.93 . ? C60 C61 1.45(4) . ? C60 H60 0.93 . ? C61 C62 1.37(3) . ? C61 H61 0.93 . ? C62 H62 0.93 . ? 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 P1 Ir P2 91.58(7) . . ? P1 Ir P3 99.20(8) . . ? P2 Ir P3 157.11(8) . . ? P1 Ir Cl 159.23(10) . . ? P2 Ir Cl 87.76(9) . . ? P3 Ir Cl 89.09(9) . . ? C27 P1 C21 102.8(4) . . ? C27 P1 C1 101.9(3) . . ? C21 P1 C1 102.2(4) . . ? C27 P1 Ir 125.7(3) . . ? C21 P1 Ir 112.9(3) . . ? C1 P1 Ir 108.5(2) . . ? C39 P2 C33 104.6(5) . . ? C39 P2 C20 102.2(4) . . ? C33 P2 C20 104.5(4) . . ? C39 P2 Ir 109.4(4) . . ? C33 P2 Ir 118.9(3) . . ? C20 P2 Ir 115.5(3) . . ? C57 P3 C45 104.2(5) . . ? C57 P3 C51 101.2(5) . . ? C45 P3 C51 101.4(4) . . ? C57 P3 Ir 106.0(4) . . ? C45 P3 Ir 120.2(3) . . ? C51 P3 Ir 121.3(3) . . ? C10 C1 C2 118.2(7) . . ? C10 C1 P1 122.6(6) . . ? C2 C1 P1 118.9(6) . . ? C3 C2 C1 124.0(9) . . ? C3 C2 H2 118 . . ? C1 C2 H2 118 . . ? C2 C3 C4 118.4(9) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C9 121.8(8) . . ? C3 C4 C5 119.9(10) . . ? C9 C4 C5 118.3(11) . . ? C6 C5 C4 119.7(12) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 120.8(10) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C8 C7 C6 122.1(11) . . ? C8 C7 H7 119 . . ? C6 C7 H7 119 . . ? C7 C8 C9 118.3(11) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C8 C9 C4 120.8(9) . . ? C8 C9 C10 121.9(9) . . ? C4 C9 C10 117.2(8) . . ? C1 C10 C9 120.2(8) . . ? C1 C10 C11 121.5(7) . . ? C9 C10 C11 117.9(7) . . ? C20 C11 C12 118.8(7) . . ? C20 C11 C10 120.7(7) . . ? C12 C11 C10 120.4(7) . . ? C17 C12 C13 118.4(8) . . ? C17 C12 C11 120.1(8) . . ? C13 C12 C11 121.5(8) . . ? C14 C13 C12 120.8(10) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.9(11) . . ? C13 C14 H14 120 . . ? C15 C14 H14 120 . . ? C16 C15 C14 120.8(10) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 121.4(10) . . ? C15 C16 H16 119.3 . . ? C17 C16 H16 119.3 . . ? C16 C17 C12 118.6(9) . . ? C16 C17 C18 122.5(9) . . ? C12 C17 C18 118.9(8) . . ? C19 C18 C17 119.1(10) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C18 C19 C20 125.5(10) . . ? C18 C19 H19 117.2 . . ? C20 C19 H19 117.2 . . ? C19 C20 C11 117.5(8) . . ? C19 C20 P2 121.7(7) . . ? C11 C20 P2 120.3(6) . . ? C22 C21 C26 118.8(9) . . ? C22 C21 P1 125.1(7) . . ? C26 C21 P1 116.1(7) . . ? C21 C22 C23 117.8(10) . . ? C21 C22 H22 121.1 . . ? C23 C22 H22 121.1 . . ? C24 C23 C22 126.3(12) . . ? C24 C23 H23 116.9 . . ? C22 C23 H23 116.9 . . ? C23 C24 C25 115.6(11) . . ? C23 C24 H24 122.2 . . ? C25 C24 H24 122.2 . . ? C26 C25 C24 120.5(10) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 121.0(9) . . ? C25 C26 H26 119.5 . . ? C21 C26 H26 119.5 . . ? C32 C27 C28 120.2(8) . . ? C32 C27 P1 117.9(6) . . ? C28 C27 P1 121.9(6) . . ? C29 C28 C27 123.4(10) . . ? C29 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? C28 C29 C30 116.5(10) . . ? C28 C29 H29 121.8 . . ? C30 C29 H29 121.8 . . ? C31 C30 C29 121.9(9) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 117.4(10) . . ? C30 C31 H31 121.3 . . ? C32 C31 H31 121.3 . . ? C27 C32 C31 120.5(9) . . ? C27 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C38 C33 C34 119.7(9) . . ? C38 C33 P2 123.1(7) . . ? C34 C33 P2 117.1(7) . . ? C35 C34 C33 121.2(9) . . ? C35 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C34 C35 C36 117.7(11) . . ? C34 C35 H35 121.1 . . ? C36 C35 H35 121.1 . . ? C37 C36 C35 121.1(11) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C36 C37 C38 119.6(11) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C33 120.5(10) . . ? C37 C38 H38 119.7 . . ? C33 C38 H38 119.7 . . ? C44 C39 C40 115.8(12) . . ? C44 C39 P2 124.5(10) . . ? C40 C39 P2 119.7(9) . . ? C39 C40 C41 122.8(16) . . ? C39 C40 H40 118.6 . . ? C41 C40 H40 118.6 . . ? C42 C41 C40 124(2) . . ? C42 C41 H41 117.8 . . ? C40 C41 H41 117.8 . . ? C41 C42 C43 115.3(17) . . ? C41 C42 H42 122.3 . . ? C43 C42 H42 122.3 . . ? C42 C43 C44 125.7(19) . . ? C42 C43 H43 117.2 . . ? C44 C43 H43 117.2 . . ? C39 C44 C43 116.0(17) . . ? C39 C44 H44 122 . . ? C43 C44 H44 122 . . ? C50 C45 C46 118.5(9) . . ? C50 C45 P3 119.7(8) . . ? C46 C45 P3 121.7(7) . . ? C45 C46 C47 120.5(11) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C48 C47 C46 120.0(12) . . ? C48 C47 H47 120 . . ? C46 C47 H47 120 . . ? C49 C48 C47 118.7(11) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 120.6(12) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C45 C50 C49 121.6(12) . . ? C45 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C52 C51 C56 118.6(10) . . ? C52 C51 P3 118.8(8) . . ? C56 C51 P3 122.6(9) . . ? C51 C52 C53 119.5(12) . . ? C51 C52 H52 120.2 . . ? C53 C52 H52 120.2 . . ? C54 C53 C52 116.1(13) . . ? C54 C53 H53 121.9 . . ? C52 C53 H53 121.9 . . ? C55 C54 C53 121.8(12) . . ? C55 C54 H54 119.1 . . ? C53 C54 H54 119.1 . . ? C56 C55 C54 119.9(13) . . ? C56 C55 H55 120 . . ? C54 C55 H55 120 . . ? C55 C56 C51 123.9(13) . . ? C55 C56 H56 118.1 . . ? C51 C56 H56 118.1 . . ? C62 C57 C58 119(2) . . ? C62 C57 P3 117.1(11) . . ? C58 C57 P3 121.4(18) . . ? C57 C58 C59 117(3) . . ? C57 C58 H58 121.6 . . ? C59 C58 H58 121.6 . . ? C60 C59 C58 120(4) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C61 119(4) . . ? C59 C60 H60 120.3 . . ? C61 C60 H60 120.3 . . ? C62 C61 C60 119(3) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? C61 C62 C57 123(2) . . ? C61 C62 H62 118.6 . . ? C57 C62 H62 118.6 . . ? 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 P2 Ir P1 C27 76.8(3) . . . . ? P3 Ir P1 C27 -83.0(3) . . . . ? Cl Ir P1 C27 164.6(4) . . . . ? P2 Ir P1 C21 -156.3(3) . . . . ? P3 Ir P1 C21 43.9(3) . . . . ? Cl Ir P1 C21 -68.5(4) . . . . ? P2 Ir P1 C1 -43.7(3) . . . . ? P3 Ir P1 C1 156.5(3) . . . . ? Cl Ir P1 C1 44.1(4) . . . . ? P1 Ir P2 C39 -150.2(4) . . . . ? P3 Ir P2 C39 -31.7(4) . . . . ? Cl Ir P2 C39 50.6(4) . . . . ? P1 Ir P2 C33 89.9(3) . . . . ? P3 Ir P2 C33 -151.7(3) . . . . ? Cl Ir P2 C33 -69.4(3) . . . . ? P1 Ir P2 C20 -35.5(3) . . . . ? P3 Ir P2 C20 82.9(4) . . . . ? Cl Ir P2 C20 165.2(3) . . . . ? P1 Ir P3 C57 130.6(4) . . . . ? P2 Ir P3 C57 13.6(5) . . . . ? Cl Ir P3 C57 -68.5(4) . . . . ? P1 Ir P3 C45 13.2(4) . . . . ? P2 Ir P3 C45 -103.9(4) . . . . ? Cl Ir P3 C45 174.0(4) . . . . ? P1 Ir P3 C51 -115.1(4) . . . . ? P2 Ir P3 C51 127.8(4) . . . . ? Cl Ir P3 C51 45.7(4) . . . . ? C27 P1 C1 C10 -49.2(7) . . . . ? C21 P1 C1 C10 -155.3(6) . . . . ? Ir P1 C1 C10 85.2(6) . . . . ? C27 P1 C1 C2 136.6(6) . . . . ? C21 P1 C1 C2 30.5(7) . . . . ? Ir P1 C1 C2 -89.0(6) . . . . ? C10 C1 C2 C3 -2.3(13) . . . . ? P1 C1 C2 C3 172.2(7) . . . . ? C1 C2 C3 C4 0.0(14) . . . . ? C2 C3 C4 C9 2.8(14) . . . . ? C2 C3 C4 C5 -176.6(9) . . . . ? C3 C4 C5 C6 -179.6(10) . . . . ? C9 C4 C5 C6 1.0(15) . . . . ? C4 C5 C6 C7 0.4(18) . . . . ? C5 C6 C7 C8 -2(2) . . . . ? C6 C7 C8 C9 2.5(18) . . . . ? C7 C8 C9 C4 -1.0(15) . . . . ? C7 C8 C9 C10 -177.8(9) . . . . ? C3 C4 C9 C8 179.9(9) . . . . ? C5 C4 C9 C8 -0.7(13) . . . . ? C3 C4 C9 C10 -3.1(13) . . . . ? C5 C4 C9 C10 176.3(8) . . . . ? C2 C1 C10 C9 1.9(11) . . . . ? P1 C1 C10 C9 -172.4(6) . . . . ? C2 C1 C10 C11 174.0(7) . . . . ? P1 C1 C10 C11 -0.3(10) . . . . ? C8 C9 C10 C1 177.6(8) . . . . ? C4 C9 C10 C1 0.7(12) . . . . ? C8 C9 C10 C11 5.2(12) . . . . ? C4 C9 C10 C11 -171.7(7) . . . . ? C1 C10 C11 C20 -66.5(11) . . . . ? C9 C10 C11 C20 105.8(9) . . . . ? C1 C10 C11 C12 116.7(9) . . . . ? C9 C10 C11 C12 -71.0(10) . . . . ? C20 C11 C12 C17 2.6(12) . . . . ? C10 C11 C12 C17 179.4(8) . . . . ? C20 C11 C12 C13 -179.6(8) . . . . ? C10 C11 C12 C13 -2.8(12) . . . . ? C17 C12 C13 C14 -1.4(14) . . . . ? C11 C12 C13 C14 -179.2(9) . . . . ? C12 C13 C14 C15 2.3(17) . . . . ? C13 C14 C15 C16 -2.4(18) . . . . ? C14 C15 C16 C17 1.5(18) . . . . ? C15 C16 C17 C12 -0.5(16) . . . . ? C15 C16 C17 C18 177.6(11) . . . . ? C13 C12 C17 C16 0.4(13) . . . . ? C11 C12 C17 C16 178.3(8) . . . . ? C13 C12 C17 C18 -177.7(9) . . . . ? C11 C12 C17 C18 0.2(13) . . . . ? C16 C17 C18 C19 179.6(10) . . . . ? C12 C17 C18 C19 -2.3(15) . . . . ? C17 C18 C19 C20 1.7(17) . . . . ? C18 C19 C20 C11 1.1(16) . . . . ? C18 C19 C20 P2 173.4(9) . . . . ? C12 C11 C20 C19 -3.2(13) . . . . ? C10 C11 C20 C19 180.0(8) . . . . ? C12 C11 C20 P2 -175.6(6) . . . . ? C10 C11 C20 P2 7.6(11) . . . . ? C39 P2 C20 C19 19.1(9) . . . . ? C33 P2 C20 C19 127.9(8) . . . . ? Ir P2 C20 C19 -99.5(8) . . . . ? C39 P2 C20 C11 -168.8(8) . . . . ? C33 P2 C20 C11 -60.0(8) . . . . ? Ir P2 C20 C11 72.5(8) . . . . ? C27 P1 C21 C22 -11.2(9) . . . . ? C1 P1 C21 C22 94.1(8) . . . . ? Ir P1 C21 C22 -149.5(8) . . . . ? C27 P1 C21 C26 169.2(7) . . . . ? C1 P1 C21 C26 -85.5(7) . . . . ? Ir P1 C21 C26 30.9(8) . . . . ? C26 C21 C22 C23 1.7(15) . . . . ? P1 C21 C22 C23 -177.9(9) . . . . ? C21 C22 C23 C24 -1(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C23 C24 C25 C26 0.0(19) . . . . ? C24 C25 C26 C21 0.8(17) . . . . ? C22 C21 C26 C25 -1.7(15) . . . . ? P1 C21 C26 C25 178.0(8) . . . . ? C21 P1 C27 C32 -122.3(7) . . . . ? C1 P1 C27 C32 132.1(7) . . . . ? Ir P1 C27 C32 8.7(8) . . . . ? C21 P1 C27 C28 57.7(8) . . . . ? C1 P1 C27 C28 -47.9(8) . . . . ? Ir P1 C27 C28 -171.3(6) . . . . ? C32 C27 C28 C29 4.4(14) . . . . ? P1 C27 C28 C29 -175.6(8) . . . . ? C27 C28 C29 C30 -1.4(15) . . . . ? C28 C29 C30 C31 -3.1(17) . . . . ? C29 C30 C31 C32 4.3(18) . . . . ? C28 C27 C32 C31 -3.0(14) . . . . ? P1 C27 C32 C31 177.0(8) . . . . ? C30 C31 C32 C27 -1.3(16) . . . . ? C39 P2 C33 C38 72.9(9) . . . . ? C20 P2 C33 C38 -34.2(8) . . . . ? Ir P2 C33 C38 -164.7(7) . . . . ? C39 P2 C33 C34 -109.4(8) . . . . ? C20 P2 C33 C34 143.5(7) . . . . ? Ir P2 C33 C34 13.0(8) . . . . ? C38 C33 C34 C35 -1.7(15) . . . . ? P2 C33 C34 C35 -179.5(9) . . . . ? C33 C34 C35 C36 2.2(18) . . . . ? C34 C35 C36 C37 -3(2) . . . . ? C35 C36 C37 C38 3(2) . . . . ? C36 C37 C38 C33 -2.8(19) . . . . ? C34 C33 C38 C37 2.0(15) . . . . ? P2 C33 C38 C37 179.6(9) . . . . ? C33 P2 C39 C44 -21.6(12) . . . . ? C20 P2 C39 C44 87.1(11) . . . . ? Ir P2 C39 C44 -150.0(10) . . . . ? C33 P2 C39 C40 157.5(9) . . . . ? C20 P2 C39 C40 -93.8(10) . . . . ? Ir P2 C39 C40 29.1(10) . . . . ? C44 C39 C40 C41 -0.3(19) . . . . ? P2 C39 C40 C41 -179.5(11) . . . . ? C39 C40 C41 C42 0(3) . . . . ? C40 C41 C42 C43 0(3) . . . . ? C41 C42 C43 C44 0(3) . . . . ? C40 C39 C44 C43 0.5(19) . . . . ? P2 C39 C44 C43 179.7(11) . . . . ? C42 C43 C44 C39 -1(3) . . . . ? C57 P3 C45 C50 -56.3(11) . . . . ? C51 P3 C45 C50 -161.1(10) . . . . ? Ir P3 C45 C50 62.1(10) . . . . ? C57 P3 C45 C46 127.9(9) . . . . ? C51 P3 C45 C46 23.1(9) . . . . ? Ir P3 C45 C46 -113.7(8) . . . . ? C50 C45 C46 C47 0.0(17) . . . . ? P3 C45 C46 C47 175.8(9) . . . . ? C45 C46 C47 C48 0.7(19) . . . . ? C46 C47 C48 C49 1(2) . . . . ? C47 C48 C49 C50 -3(2) . . . . ? C46 C45 C50 C49 -2.4(19) . . . . ? P3 C45 C50 C49 -178.3(11) . . . . ? C48 C49 C50 C45 4(2) . . . . ? C57 P3 C51 C52 127.8(9) . . . . ? C45 P3 C51 C52 -125.1(9) . . . . ? Ir P3 C51 C52 11.2(10) . . . . ? C57 P3 C51 C56 -49.4(11) . . . . ? C45 P3 C51 C56 57.7(11) . . . . ? Ir P3 C51 C56 -166.1(8) . . . . ? C56 C51 C52 C53 -3.3(17) . . . . ? P3 C51 C52 C53 179.4(9) . . . . ? C51 C52 C53 C54 3.1(18) . . . . ? C52 C53 C54 C55 -1.4(19) . . . . ? C53 C54 C55 C56 0(2) . . . . ? C54 C55 C56 C51 0(2) . . . . ? C52 C51 C56 C55 1.8(19) . . . . ? P3 C51 C56 C55 179.0(11) . . . . ? C45 P3 C57 C62 -144.2(13) . . . . ? C51 P3 C57 C62 -39.3(13) . . . . ? Ir P3 C57 C62 88.1(13) . . . . ? C45 P3 C57 C58 53.0(13) . . . . ? C51 P3 C57 C58 157.9(12) . . . . ? Ir P3 C57 C58 -74.7(12) . . . . ? C62 C57 C58 C59 4.1(15) . . . . ? P3 C57 C58 C59 166.5(12) . . . . ? C57 C58 C59 C60 8(2) . . . . ? C58 C59 C60 C61 -19(3) . . . . ? C59 C60 C61 C62 17(4) . . . . ? C60 C61 C62 C57 -5(4) . . . . ? C58 C57 C62 C61 -6(3) . . . . ? P3 C57 C62 C61 -169.1(19) . . . . ? #===end #===end #===end #===end #===end #===end data_4a _database_code_CSD 161687 _publ_contact_author 'Tani, Kazuhide' _publ_contact_author_address ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka, Osaka, 560-8531 Japan ; _publ_contact_author_email tani@chem.es.osaka-u.ac.jp _publ_contact_author_phone ' +81 6 850 6245' _publ_contact_author_fax ' +81 6 850 6296' _publ_contact_author_email tani@chem.es.osaka-u.ac.jp loop_ _publ_author_name 'Tani, Kazuhide' 'Nakajima, Kouji' 'Iseki, Aika' 'Yamagata, Tsuneaki' _journal_name_full ? _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _ccdc_journal_depnumber ? #4 Chemical and physical data _ccdc_compound_id ? _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ; ? ; #5 Other data relating to the structure determination and refinement _ccdc_temp_data_collection ? _ccdc_ls_R_squared ? _ccdc_disorder ? _ccdc_comments ; ? ; #6 Include your "standard" CIF file here #------------------------------------------------------------------------- _audit_creation_date 2001-01-22T18:58:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# # CIF produced by WinGX routine CIF_UPDATE # Created on 2000-11-07 at 20:29:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Created on 2001-01-22 at 18:58:05 # Using CIFtbx version 2.6.2 16 Jun 1998 _audit_creation_date 2001-01-29 17:00:00-00:00 _audit_update_record 'Jan 29 20:29:06 2001' _computing_data_collection 'Rigaku/AFC5R Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC5R Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC. 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97, WinGX, and, and modified' _computing_molecular_graphics 'WINGX' # Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. WINGX Main Reference # ORTEP-III(version 1.0.2) - Burnett, M. N. & Johnson, C.K.(1996) # Report ORNL-6895. # A FORTRAN Thermal-Ellipsoid Plot Program, # Oak Ridge National Laboratory, Oak Ridge, Tennessee, U.S # Ortep-3 for Windows, Version 1.05. _computing_structure_refinement 'SHELXH-97 (Sheldrick, 1997)' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 503-518 #(decomp.,in capillary under vacuum) _chemical_formula_moiety ? _chemical_formula_sum 'C62 H49 Cl Ir P3' _chemical_formula_weight 1114.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21' _symmetry_space_group_name_Hall 'P 2Y1' _symmetry_int_table_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.070(3) _cell_length_b 21.979(4) _cell_length_c 11.788(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.50(2) _cell_angle_gamma 90.00 _cell_volume 2849.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 13.915 _cell_measurement_theta_max 14.975 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 2.509 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.4023 _exptl_absorpt_correction_T_max 0.8168 _exptl_absorpt_process_details '( North, Phillips, & Mathews, (1968). Acta Cryst. A24, 351-359.)' _exptl_special_details ; \w scan width (0.84 + 0.30tan\q) deg, \w scan rate 16.0 deg/min. The ratio of peak counting time to background counting time was 2:1. The diameter of the incident beam collimeter was 1.0 mm, the crystal to detector distance was 285 mm, and the detector aperture was 6.0 x 6.0 mm (horizontal x vertical). ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w-2\t _diffrn_measurement_device_type 'AFC7R' _diffrn_detector_area_resol_mean ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 21894 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.2596 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 32.48 _reflns_number_total 20525 _reflns_number_gt 8479 _reflns_threshold_expression >2sigma(I) _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^)+(0.0867P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.050(9) _refine_ls_number_reflns 20525 _refine_ls_number_parameters 603 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2305 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1953 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.24229(3) 0.2500 0.35300(3) 0.03389(9) Uani 1 1 d . . . H0A H 0.1049 0.2238 0.3060 0.041 Uiso 1 1 d . . . H0B H 0.2288 0.2476 0.4920 0.041 Uiso 1 1 d . . . Cl Cl 0.4462(3) 0.28569(13) 0.4420(2) 0.0497(6) Uani 1 1 d . . . P1 P 0.3109(3) 0.15147(12) 0.3737(2) 0.0356(6) Uani 1 1 d . . . P2 P 0.26318(19) 0.2512(3) 0.15576(17) 0.0321(4) Uani 1 1 d . . . P3 P 0.1691(3) 0.34800(13) 0.3751(2) 0.0392(6) Uani 1 1 d . . . C1 C 0.4499(10) 0.1415(5) 0.3028(8) 0.036(2) Uani 1 1 d . . . C2 C 0.4471(9) 0.1382(4) 0.1861(9) 0.036(2) Uani 1 1 d . . . C3 C 0.5618(9) 0.1430(4) 0.1378(8) 0.034(2) Uani 1 1 d . . . C4 C 0.5657(10) 0.1435(5) 0.0183(9) 0.044(2) Uani 1 1 d . . . H4 H 0.4936 0.1422 -0.0304 0.053 Uiso 1 1 calc R . . C5 C 0.6771(12) 0.1460(5) -0.0276(11) 0.055(3) Uani 1 1 d . . . H5 H 0.6788 0.1454 -0.1063 0.066 Uiso 1 1 calc R . . C6 C 0.7849(11) 0.1496(6) 0.0453(13) 0.064(4) Uani 1 1 d . . . H6 H 0.8583 0.1512 0.0140 0.076 Uiso 1 1 calc R . . C7 C 0.7863(11) 0.1507(6) 0.1612(12) 0.061(3) Uani 1 1 d . . . H7 H 0.8591 0.1533 0.2088 0.073 Uiso 1 1 calc R . . C8 C 0.6713(10) 0.1477(5) 0.2077(10) 0.043(2) Uani 1 1 d . . . C9 C 0.6688(11) 0.1494(5) 0.3277(10) 0.050(3) Uani 1 1 d . . . H9 H 0.7415 0.1511 0.3755 0.060 Uiso 1 1 calc R . . C10 C 0.5621(10) 0.1487(5) 0.3736(9) 0.042(2) Uani 1 1 d . . . H10 H 0.5621 0.1529 0.4521 0.051 Uiso 1 1 calc R . . C11 C 0.3324(9) 0.1303(4) 0.1069(8) 0.033(2) Uani 1 1 d . . . C12 C 0.2436(9) 0.1751(5) 0.0856(8) 0.037(2) Uani 1 1 d . . . C13 C 0.1428(16) 0.1638(8) 0.0036(14) 0.052(4) Uani 1 1 d . . . H13 H 0.0828 0.1933 -0.0103 0.062 Uiso 1 1 calc R . . C14 C 0.1322(12) 0.1112(7) -0.0543(12) 0.056(4) Uani 1 1 d . . . H14 H 0.0656 0.1064 -0.1092 0.068 Uiso 1 1 calc R . . C15 C 0.2139(11) 0.0640(5) -0.0376(10) 0.051(3) Uani 1 1 d . . . C16 C 0.2054(13) 0.0083(7) -0.0994(12) 0.068(4) Uani 1 1 d . . . H16 H 0.1417 0.0032 -0.1573 0.081 Uiso 1 1 calc R . . C17 C 0.2861(14) -0.0375(6) -0.0774(13) 0.069(4) Uani 1 1 d . . . H17 H 0.2766 -0.0736 -0.1185 0.082 Uiso 1 1 calc R . . C18 C 0.3809(15) -0.0305(6) 0.0049(13) 0.069(4) Uani 1 1 d . . . H18 H 0.4355 -0.0625 0.0196 0.083 Uiso 1 1 calc R . . C19 C 0.4002(12) 0.0244(5) 0.0702(11) 0.052(3) Uani 1 1 d . . . H19 H 0.4662 0.0279 0.1262 0.063 Uiso 1 1 calc R . . C20 C 0.3169(9) 0.0735(5) 0.0481(9) 0.039(2) Uani 1 1 d . . . C21 C 0.3607(10) 0.1262(5) 0.5197(9) 0.041(2) Uani 1 1 d . . . C22 C 0.3543(12) 0.1636(6) 0.6137(10) 0.058(3) Uani 1 1 d . . . H22 H 0.3310 0.2040 0.6029 0.069 Uiso 1 1 calc R . . C23 C 0.3829(17) 0.1411(7) 0.7254(11) 0.078(5) Uani 1 1 d . . . H23 H 0.3755 0.1662 0.7877 0.093 Uiso 1 1 calc R . . C24 C 0.4204(14) 0.0839(7) 0.7422(11) 0.068(4) Uani 1 1 d . . . H24 H 0.4409 0.0695 0.8161 0.081 Uiso 1 1 calc R . . C25 C 0.4289(17) 0.0460(7) 0.6505(12) 0.078(5) Uani 1 1 d . . . H25 H 0.4560 0.0063 0.6628 0.094 Uiso 1 1 calc R . . C26 C 0.3971(17) 0.0668(6) 0.5387(11) 0.076(5) Uani 1 1 d . . . H26 H 0.4006 0.0405 0.4774 0.092 Uiso 1 1 calc R . . C27 C 0.2048(13) 0.0894(5) 0.3294(9) 0.047(3) Uani 1 1 d . . . C28 C 0.0839(12) 0.0961(7) 0.3430(13) 0.069(4) Uani 1 1 d . . . H28 H 0.0536 0.1335 0.3635 0.082 Uiso 1 1 calc R . . C29 C 0.0063(14) 0.0450(9) 0.3252(14) 0.084(5) Uani 1 1 d . . . H29 H -0.0750 0.0487 0.3372 0.101 Uiso 1 1 calc R . . C30 C 0.048(2) -0.0099(8) 0.2906(13) 0.091(6) Uani 1 1 d . . . H30 H -0.0049 -0.0427 0.2788 0.110 Uiso 1 1 calc R . . C31 C 0.1640(19) -0.0169(6) 0.2740(13) 0.080(5) Uani 1 1 d . . . H31 H 0.1918 -0.0541 0.2496 0.096 Uiso 1 1 calc R . . C32 C 0.2436(14) 0.0324(6) 0.2936(10) 0.062(4) Uani 1 1 d . . . H32 H 0.3249 0.0273 0.2826 0.074 Uiso 1 1 calc R . . C33 C 0.3957(9) 0.2747(4) 0.0877(9) 0.036(2) Uani 1 1 d . . . C34 C 0.3915(10) 0.2719(4) -0.0318(9) 0.042(2) Uani 1 1 d . . . H34 H 0.3215 0.2580 -0.0750 0.051 Uiso 1 1 calc R . . C35 C 0.4925(11) 0.2900(5) -0.0869(11) 0.051(3) Uani 1 1 d . . . H35 H 0.4882 0.2901 -0.1661 0.061 Uiso 1 1 calc R . . C36 C 0.5974(11) 0.3075(6) -0.0209(11) 0.056(3) Uani 1 1 d . . . H36 H 0.6645 0.3189 -0.0568 0.067 Uiso 1 1 calc R . . C37 C 0.6065(11) 0.3087(5) 0.0997(11) 0.054(3) Uani 1 1 d . . . H37 H 0.6785 0.3200 0.1428 0.065 Uiso 1 1 calc R . . C38 C 0.5046(10) 0.2924(5) 0.1522(10) 0.044(2) Uani 1 1 d . . . H38 H 0.5087 0.2933 0.2314 0.053 Uiso 1 1 calc R . . C39 C 0.1403(10) 0.2966(5) 0.0805(9) 0.042(2) Uani 1 1 d . . . C40 C 0.1589(15) 0.3436(8) 0.0069(13) 0.051(4) Uani 1 1 d . . . H40 H 0.2380 0.3532 -0.0060 0.061 Uiso 1 1 calc R . . C41 C 0.0649(15) 0.3765(7) -0.0478(12) 0.069(4) Uani 1 1 d . . . H41 H 0.0805 0.4097 -0.0929 0.082 Uiso 1 1 calc R . . C42 C -0.0561(16) 0.3599(9) -0.0352(14) 0.092(6) Uani 1 1 d . . . H42 H -0.1211 0.3784 -0.0787 0.111 Uiso 1 1 calc R . . C43 C -0.0763(12) 0.3131(8) 0.0474(14) 0.084(5) Uani 1 1 d . . . H43 H -0.1548 0.3039 0.0630 0.100 Uiso 1 1 calc R . . C44 C 0.0214(10) 0.2824(6) 0.1024(11) 0.057(3) Uani 1 1 d . . . H44 H 0.0087 0.2520 0.1546 0.068 Uiso 1 1 calc R . . C45 C 0.0071(10) 0.3574(5) 0.3839(9) 0.041(2) Uani 1 1 d . . . C46 C -0.0382(12) 0.4150(6) 0.4145(13) 0.064(4) Uani 1 1 d . . . H46 H 0.0144 0.4477 0.4290 0.077 Uiso 1 1 calc R . . C47 C -0.1639(14) 0.4219(8) 0.4226(15) 0.088(5) Uani 1 1 d . . . H47 H -0.1929 0.4599 0.4412 0.106 Uiso 1 1 calc R . . C48 C -0.2440(15) 0.3751(8) 0.4043(14) 0.082(5) Uani 1 1 d . . . H48 H -0.3260 0.3803 0.4123 0.098 Uiso 1 1 calc R . . C49 C -0.1988(14) 0.3181(8) 0.3728(15) 0.080(4) Uani 1 1 d . . . H49 H -0.2524 0.2861 0.3544 0.096 Uiso 1 1 calc R . . C50 C -0.0748(12) 0.3095(6) 0.3690(11) 0.059(3) Uani 1 1 d . . . H50 H -0.0461 0.2706 0.3561 0.071 Uiso 1 1 calc R . . C51 C 0.2318(11) 0.3835(5) 0.5101(9) 0.045(3) Uani 1 1 d . . . C52 C 0.2253(15) 0.3544(7) 0.6096(11) 0.067(4) Uani 1 1 d . . . H52 H 0.1933 0.3152 0.6082 0.080 Uiso 1 1 calc R . . C53 C 0.2656(19) 0.3814(9) 0.7164(12) 0.092(6) Uani 1 1 d . . . H53 H 0.2588 0.3603 0.7838 0.110 Uiso 1 1 calc R . . C54 C 0.3130(17) 0.4367(8) 0.7194(14) 0.086(5) Uani 1 1 d . . . H54 H 0.3414 0.4539 0.7894 0.103 Uiso 1 1 calc R . . C55 C 0.3208(18) 0.4687(8) 0.6223(13) 0.087(5) Uani 1 1 d . . . H55 H 0.3532 0.5077 0.6256 0.104 Uiso 1 1 calc R . . C56 C 0.2799(17) 0.4426(7) 0.5175(13) 0.083(5) Uani 1 1 d . . . H56 H 0.2845 0.4648 0.4510 0.100 Uiso 1 1 calc R . . C57 C 0.2049(11) 0.4048(5) 0.2732(10) 0.043(3) Uani 1 1 d . . . C58 C 0.1222(15) 0.4429(6) 0.2130(12) 0.070(4) Uani 1 1 d . . . H58 H 0.0406 0.4413 0.2250 0.084 Uiso 1 1 calc R . . C59 C 0.1603(17) 0.4840(7) 0.1340(14) 0.082(5) Uani 1 1 d . . . H59 H 0.1046 0.5109 0.0966 0.098 Uiso 1 1 calc R . . C60 C 0.2784(18) 0.4850(6) 0.1110(14) 0.084(5) Uani 1 1 d . . . H60 H 0.3020 0.5102 0.0541 0.101 Uiso 1 1 calc R . . C61 C 0.3635(14) 0.4476(6) 0.1742(13) 0.069(4) Uani 1 1 d . . . H61 H 0.4452 0.4501 0.1632 0.083 Uiso 1 1 calc R . . C62 C 0.3277(12) 0.4081(5) 0.2506(10) 0.051(3) Uani 1 1 d . . . H62 H 0.3848 0.3824 0.2896 0.061 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 0.03773(16) 0.03141(14) 0.03302(15) 0.0023(4) 0.00606(11) 0.0014(4) Cl 0.0487(16) 0.0526(15) 0.0461(15) -0.0031(12) -0.0023(12) 0.0002(13) P1 0.0432(15) 0.0328(13) 0.0308(13) 0.0014(10) 0.0041(11) 0.0014(11) P2 0.0302(9) 0.0333(9) 0.0330(9) 0.000(2) 0.0036(7) -0.001(2) P3 0.0434(15) 0.0360(14) 0.0391(14) 0.0021(11) 0.0087(12) 0.0067(12) C1 0.045(6) 0.032(5) 0.032(5) 0.003(4) 0.005(4) -0.001(4) C2 0.032(5) 0.031(5) 0.046(6) 0.001(4) 0.008(4) 0.004(4) C3 0.042(6) 0.032(5) 0.029(5) -0.007(4) 0.012(4) 0.002(4) C4 0.043(6) 0.048(6) 0.042(6) 0.003(5) 0.011(5) 0.010(5) C5 0.074(9) 0.044(6) 0.052(7) 0.000(5) 0.029(6) -0.001(6) C6 0.038(7) 0.076(9) 0.079(10) 0.009(7) 0.017(7) -0.003(6) C7 0.050(8) 0.060(8) 0.074(9) -0.001(7) 0.014(7) 0.008(6) C8 0.040(6) 0.039(5) 0.050(6) 0.004(5) 0.001(5) 0.002(5) C9 0.043(7) 0.052(7) 0.051(7) -0.007(5) -0.012(5) 0.011(5) C10 0.040(6) 0.053(6) 0.031(5) -0.010(5) -0.006(4) 0.010(5) C11 0.033(5) 0.032(5) 0.035(5) -0.006(4) 0.006(4) -0.003(4) C12 0.038(6) 0.045(6) 0.027(5) 0.002(4) 0.001(4) -0.001(5) C13 0.048(9) 0.060(10) 0.045(9) 0.008(7) -0.004(7) 0.001(7) C14 0.035(7) 0.071(9) 0.058(8) -0.006(7) -0.016(6) -0.012(7) C15 0.047(7) 0.052(7) 0.053(7) -0.008(5) 0.000(5) -0.009(6) C16 0.060(8) 0.076(10) 0.064(8) -0.013(7) -0.010(7) -0.013(8) C17 0.070(9) 0.052(8) 0.084(10) -0.040(7) 0.010(8) -0.018(7) C18 0.087(11) 0.037(6) 0.092(11) -0.007(6) 0.045(9) 0.004(7) C19 0.054(7) 0.043(6) 0.062(7) 0.002(5) 0.016(6) -0.006(5) C20 0.035(5) 0.042(6) 0.041(6) -0.003(5) 0.010(4) 0.000(4) C21 0.043(6) 0.044(6) 0.035(5) -0.002(4) 0.005(4) 0.001(5) C22 0.078(9) 0.047(7) 0.046(7) -0.015(5) -0.003(6) 0.010(6) C23 0.134(15) 0.061(8) 0.032(6) 0.004(6) -0.014(8) 0.024(9) C24 0.082(10) 0.075(9) 0.042(7) 0.025(7) -0.010(7) -0.005(8) C25 0.121(14) 0.052(8) 0.052(8) 0.015(6) -0.027(8) 0.015(8) C26 0.138(15) 0.050(7) 0.040(7) -0.002(6) 0.003(8) 0.018(9) C27 0.074(9) 0.040(6) 0.025(6) 0.010(5) 0.002(6) -0.010(6) C28 0.051(8) 0.069(9) 0.083(10) 0.018(7) -0.005(7) -0.019(7) C29 0.056(9) 0.109(14) 0.084(11) 0.004(10) -0.005(8) -0.035(9) C30 0.134(17) 0.075(11) 0.063(10) -0.005(8) 0.005(10) -0.047(11) C31 0.135(16) 0.046(8) 0.064(9) -0.010(6) 0.029(10) -0.032(9) C32 0.093(11) 0.050(7) 0.045(7) -0.003(6) 0.018(7) -0.017(7) C33 0.034(5) 0.031(4) 0.044(5) 0.002(4) 0.013(4) 0.000(4) C34 0.038(6) 0.041(5) 0.049(6) -0.002(4) 0.008(5) -0.001(4) C35 0.059(7) 0.045(6) 0.054(7) 0.005(5) 0.029(6) -0.004(6) C36 0.044(7) 0.059(8) 0.066(8) 0.010(6) 0.014(6) -0.007(6) C37 0.045(7) 0.056(7) 0.064(8) -0.002(6) 0.015(6) -0.011(6) C38 0.044(6) 0.040(6) 0.048(6) 0.003(5) 0.006(5) -0.002(5) C39 0.046(6) 0.042(6) 0.037(5) -0.002(4) 0.007(5) 0.020(5) C40 0.047(9) 0.057(9) 0.048(9) 0.021(7) 0.002(7) 0.017(7) C41 0.073(11) 0.075(10) 0.058(8) 0.026(7) 0.010(8) 0.047(9) C42 0.082(12) 0.115(14) 0.079(11) 0.019(10) 0.005(9) 0.058(11) C43 0.032(6) 0.135(14) 0.088(11) 0.039(10) 0.021(7) 0.032(8) C44 0.032(6) 0.081(8) 0.057(7) 0.010(6) 0.005(5) 0.021(6) C45 0.045(6) 0.045(6) 0.037(5) 0.000(4) 0.014(5) 0.006(5) C46 0.047(7) 0.055(7) 0.093(10) -0.011(7) 0.021(7) 0.007(6) C47 0.058(9) 0.084(11) 0.124(15) -0.032(10) 0.013(9) 0.022(8) C48 0.057(9) 0.107(13) 0.084(11) -0.001(10) 0.015(8) 0.007(9) C49 0.047(8) 0.087(11) 0.107(13) 0.011(9) 0.016(8) 0.000(8) C50 0.063(8) 0.060(8) 0.057(8) 0.002(6) 0.014(6) 0.003(7) C51 0.052(7) 0.037(6) 0.046(6) -0.003(5) 0.008(5) 0.009(5) C52 0.096(11) 0.059(8) 0.045(7) 0.001(6) 0.008(7) 0.003(8) C53 0.140(17) 0.100(13) 0.035(7) 0.001(8) 0.005(9) 0.019(12) C54 0.104(14) 0.087(12) 0.065(10) -0.031(9) 0.008(9) -0.008(11) C55 0.118(15) 0.081(11) 0.060(9) -0.025(8) 0.003(9) -0.032(11) C56 0.117(14) 0.084(11) 0.053(8) -0.023(8) 0.027(9) -0.029(10) C57 0.049(7) 0.041(6) 0.040(6) 0.001(5) -0.003(6) 0.002(5) C58 0.086(10) 0.059(8) 0.066(9) 0.020(7) 0.018(8) 0.006(8) C59 0.109(14) 0.064(9) 0.078(10) 0.024(8) 0.030(9) 0.032(9) C60 0.134(16) 0.046(8) 0.080(10) 0.017(7) 0.042(10) -0.012(9) C61 0.078(10) 0.057(8) 0.076(9) 0.004(7) 0.024(8) -0.021(7) C62 0.065(8) 0.041(6) 0.048(6) -0.008(5) 0.010(6) -0.012(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir P1 2.299(3) . ? Ir P3 2.326(3) . ? Ir P2 2.363(2) . ? Ir Cl 2.505(3) . ? Ir H0A 1.6619(5) . ? Ir H0B 1.6632(6) . ? P1 C21 1.833(11) . ? P1 C27 1.838(13) . ? P1 C1 1.845(11) . ? P2 C33 1.825(10) . ? P2 C39 1.833(10) . ? P2 C12 1.868(12) . ? P3 C57 1.807(12) . ? P3 C45 1.820(11) . ? P3 C51 1.836(11) . ? C1 C2 1.374(14) . ? C1 C10 1.424(14) . ? C2 C3 1.453(13) . ? C2 C11 1.498(14) . ? C3 C8 1.390(14) . ? C3 C4 1.414(13) . ? C4 C5 1.402(16) . ? C4 H4 0.9300 . ? C5 C6 1.392(18) . ? C5 H5 0.9300 . ? C6 C7 1.365(18) . ? C6 H6 0.9300 . ? C7 C8 1.444(16) . ? C7 H7 0.9300 . ? C8 C9 1.418(16) . ? C9 C10 1.354(16) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.393(14) . ? C11 C20 1.429(14) . ? C12 C13 1.413(19) . ? C13 C14 1.34(2) . ? C13 H13 0.9300 . ? C14 C15 1.376(18) . ? C14 H14 0.9300 . ? C15 C16 1.422(18) . ? C15 C20 1.450(16) . ? C16 C17 1.35(2) . ? C16 H16 0.9300 . ? C17 C18 1.35(2) . ? C17 H17 0.9300 . ? C18 C19 1.434(17) . ? C18 H18 0.9300 . ? C19 C20 1.425(16) . ? C19 H19 0.9300 . ? C21 C26 1.376(17) . ? C21 C22 1.389(15) . ? C22 C23 1.408(17) . ? C22 H22 0.9300 . ? C23 C24 1.33(2) . ? C23 H23 0.9300 . ? C24 C25 1.38(2) . ? C24 H24 0.9300 . ? C25 C26 1.402(17) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.374(19) . ? C27 C32 1.404(18) . ? C28 C29 1.42(2) . ? C28 H28 0.9300 . ? C29 C30 1.37(3) . ? C29 H29 0.9300 . ? C30 C31 1.33(2) . ? C30 H30 0.9300 . ? C31 C32 1.400(19) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.405(14) . ? C33 C38 1.405(15) . ? C34 C35 1.411(15) . ? C34 H34 0.9300 . ? C35 C36 1.378(17) . ? C35 H35 0.9300 . ? C36 C37 1.413(18) . ? C36 H36 0.9300 . ? C37 C38 1.394(16) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? C39 C40 1.379(18) . ? C39 C44 1.406(16) . ? C40 C41 1.367(18) . ? C40 H40 0.9300 . ? C41 C42 1.41(2) . ? C41 H41 0.9300 . ? C42 C43 1.45(2) . ? C42 H42 0.9300 . ? C43 C44 1.373(17) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? C45 C50 1.387(17) . ? C45 C46 1.423(16) . ? C46 C47 1.414(19) . ? C46 H46 0.9300 . ? C47 C48 1.36(2) . ? C47 H47 0.9300 . ? C48 C49 1.41(2) . ? C48 H48 0.9300 . ? C49 C50 1.392(19) . ? C49 H49 0.9300 . ? C50 H50 0.9300 . ? C51 C52 1.346(17) . ? C51 C56 1.401(19) . ? C52 C53 1.42(2) . ? C52 H52 0.9300 . ? C53 C54 1.32(2) . ? C53 H53 0.9300 . ? C54 C55 1.35(2) . ? C54 H54 0.9300 . ? C55 C56 1.390(19) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.377(18) . ? C57 C62 1.417(17) . ? C58 C59 1.396(19) . ? C58 H58 0.9300 . ? C59 C60 1.36(2) . ? C59 H59 0.9300 . ? C60 C61 1.40(2) . ? C60 H60 0.9300 . ? C61 C62 1.342(17) . ? C61 H61 0.9300 . ? C62 H62 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 P1 Ir P3 167.30(9) . . ? P1 Ir P2 92.70(16) . . ? P3 Ir P2 100.00(16) . . ? P1 Ir Cl 88.81(10) . . ? P3 Ir Cl 88.38(10) . . ? P2 Ir Cl 102.98(10) . . ? P1 Ir H0A 89.28(7) . . ? P3 Ir H0A 92.38(7) . . ? P2 Ir H0A 82.19(8) . . ? Cl Ir H0A 174.57(7) . . ? P1 Ir H0B 86.05(6) . . ? P3 Ir H0B 81.25(7) . . ? P2 Ir H0B 178.75(14) . . ? Cl Ir H0B 76.97(7) . . ? H0A Ir H0B 97.83(3) . . ? C21 P1 C27 99.0(5) . . ? C21 P1 C1 102.2(5) . . ? C27 P1 C1 108.8(5) . . ? C21 P1 Ir 116.5(3) . . ? C27 P1 Ir 118.5(4) . . ? C1 P1 Ir 110.3(3) . . ? C33 P2 C39 102.9(5) . . ? C33 P2 C12 96.7(5) . . ? C39 P2 C12 103.3(5) . . ? C33 P2 Ir 127.6(4) . . ? C39 P2 Ir 109.4(4) . . ? C12 P2 Ir 114.0(4) . . ? C57 P3 C45 104.5(5) . . ? C57 P3 C51 101.1(5) . . ? C45 P3 C51 100.4(5) . . ? C57 P3 Ir 117.4(4) . . ? C45 P3 Ir 118.0(4) . . ? C51 P3 Ir 112.9(4) . . ? C2 C1 C10 120.8(10) . . ? C2 C1 P1 122.2(8) . . ? C10 C1 P1 116.0(7) . . ? C1 C2 C3 117.8(9) . . ? C1 C2 C11 123.5(9) . . ? C3 C2 C11 118.7(9) . . ? C8 C3 C4 117.8(9) . . ? C8 C3 C2 121.0(9) . . ? C4 C3 C2 121.2(9) . . ? C5 C4 C3 120.8(11) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C6 C5 C4 119.6(11) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C7 C6 C5 122.0(12) . . ? C7 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C6 C7 C8 117.9(12) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 121.0 . . ? C3 C8 C9 118.6(10) . . ? C3 C8 C7 121.8(10) . . ? C9 C8 C7 119.7(11) . . ? C10 C9 C8 121.0(10) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C1 120.6(10) . . ? C9 C10 H10 119.7 . . ? C1 C10 H10 119.7 . . ? C12 C11 C20 119.1(9) . . ? C12 C11 C2 124.1(9) . . ? C20 C11 C2 116.8(9) . . ? C11 C12 C13 119.0(11) . . ? C11 C12 P2 120.6(7) . . ? C13 C12 P2 120.2(10) . . ? C14 C13 C12 121.1(15) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 124.0(13) . . ? C13 C14 H14 118.0 . . ? C15 C14 H14 118.0 . . ? C14 C15 C16 124.8(12) . . ? C14 C15 C20 116.3(11) . . ? C16 C15 C20 118.9(11) . . ? C17 C16 C15 122.6(12) . . ? C17 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C16 C17 C18 119.7(12) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C17 C18 C19 122.4(13) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 119.0(12) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C11 122.2(10) . . ? C19 C20 C15 117.4(10) . . ? C11 C20 C15 120.4(10) . . ? C26 C21 C22 118.1(11) . . ? C26 C21 P1 119.5(9) . . ? C22 C21 P1 122.2(9) . . ? C21 C22 C23 120.8(12) . . ? C21 C22 H22 119.6 . . ? C23 C22 H22 119.6 . . ? C24 C23 C22 120.3(13) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.1(11) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C26 120.6(13) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C21 C26 C25 120.0(12) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C32 117.8(13) . . ? C28 C27 P1 119.2(10) . . ? C32 C27 P1 122.7(11) . . ? C27 C28 C29 118.6(16) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C30 C29 C28 121.5(17) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C31 C30 C29 120.8(15) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C32 119.1(15) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C31 C32 C27 122.1(15) . . ? C31 C32 H32 118.9 . . ? C27 C32 H32 118.9 . . ? C34 C33 C38 118.9(9) . . ? C34 C33 P2 119.5(8) . . ? C38 C33 P2 121.5(8) . . ? C33 C34 C35 120.7(10) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C36 C35 C34 118.7(11) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C35 C36 C37 122.1(11) . . ? C35 C36 H36 118.9 . . ? C37 C36 H36 118.9 . . ? C38 C37 C36 118.3(11) . . ? C38 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? C37 C38 C33 121.2(11) . . ? C37 C38 H38 119.4 . . ? C33 C38 H38 119.4 . . ? C40 C39 C44 119.4(11) . . ? C40 C39 P2 123.9(10) . . ? C44 C39 P2 116.7(8) . . ? C41 C40 C39 122.2(15) . . ? C41 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? C40 C41 C42 119.5(15) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C41 C42 C43 118.3(13) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C44 C43 C42 119.5(13) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C39 120.5(12) . . ? C43 C44 H44 119.7 . . ? C39 C44 H44 119.7 . . ? C50 C45 C46 117.5(11) . . ? C50 C45 P3 122.8(9) . . ? C46 C45 P3 119.6(9) . . ? C47 C46 C45 119.4(13) . . ? C47 C46 H46 120.3 . . ? C45 C46 H46 120.3 . . ? C48 C47 C46 122.5(15) . . ? C48 C47 H47 118.8 . . ? C46 C47 H47 118.8 . . ? C47 C48 C49 117.9(15) . . ? C47 C48 H48 121.1 . . ? C49 C48 H48 121.1 . . ? C50 C49 C48 120.7(16) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C45 C50 C49 121.7(13) . . ? C45 C50 H50 119.2 . . ? C49 C50 H50 119.2 . . ? C52 C51 C56 116.3(12) . . ? C52 C51 P3 120.0(10) . . ? C56 C51 P3 123.5(10) . . ? C51 C52 C53 122.2(15) . . ? C51 C52 H52 118.9 . . ? C53 C52 H52 118.9 . . ? C54 C53 C52 119.5(15) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 121.1(15) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? C54 C55 C56 119.4(16) . . ? C54 C55 H55 120.3 . . ? C56 C55 H55 120.3 . . ? C55 C56 C51 121.4(15) . . ? C55 C56 H56 119.3 . . ? C51 C56 H56 119.3 . . ? C58 C57 C62 117.9(12) . . ? C58 C57 P3 125.5(11) . . ? C62 C57 P3 116.6(9) . . ? C57 C58 C59 120.2(15) . . ? C57 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C60 C59 C58 120.8(15) . . ? C60 C59 H59 119.6 . . ? C58 C59 H59 119.6 . . ? C59 C60 C61 119.1(13) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C62 C61 C60 120.3(14) . . ? C62 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? C61 C62 C57 121.4(13) . . ? C61 C62 H62 119.3 . . ? C57 C62 H62 119.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P3 Ir P1 C21 -17.4(7) . . . . ? P2 Ir P1 C21 162.8(4) . . . . ? Cl Ir P1 C21 59.8(4) . . . . ? P3 Ir P1 C27 100.5(6) . . . . ? P2 Ir P1 C27 -79.3(4) . . . . ? Cl Ir P1 C27 177.7(4) . . . . ? P3 Ir P1 C1 -133.3(5) . . . . ? P2 Ir P1 C1 46.9(4) . . . . ? Cl Ir P1 C1 -56.0(4) . . . . ? P1 Ir P2 C33 -90.8(5) . . . . ? P3 Ir P2 C33 89.2(5) . . . . ? Cl Ir P2 C33 -1.4(5) . . . . ? P1 Ir P2 C39 144.5(4) . . . . ? P3 Ir P2 C39 -35.5(5) . . . . ? Cl Ir P2 C39 -126.1(4) . . . . ? P1 Ir P2 C12 29.4(4) . . . . ? P3 Ir P2 C12 -150.6(4) . . . . ? Cl Ir P2 C12 118.8(4) . . . . ? P1 Ir P3 C57 155.6(6) . . . . ? P2 Ir P3 C57 -24.6(5) . . . . ? Cl Ir P3 C57 78.3(5) . . . . ? P1 Ir P3 C45 -77.8(6) . . . . ? P2 Ir P3 C45 102.0(4) . . . . ? Cl Ir P3 C45 -155.2(4) . . . . ? P1 Ir P3 C51 38.7(7) . . . . ? P2 Ir P3 C51 -141.5(4) . . . . ? Cl Ir P3 C51 -38.7(4) . . . . ? C21 P1 C1 C2 160.9(9) . . . . ? C27 P1 C1 C2 56.9(10) . . . . ? Ir P1 C1 C2 -74.6(9) . . . . ? C21 P1 C1 C10 -30.3(9) . . . . ? C27 P1 C1 C10 -134.3(8) . . . . ? Ir P1 C1 C10 94.2(8) . . . . ? C10 C1 C2 C3 -0.7(14) . . . . ? P1 C1 C2 C3 167.5(7) . . . . ? C10 C1 C2 C11 179.7(9) . . . . ? P1 C1 C2 C11 -12.1(14) . . . . ? C1 C2 C3 C8 3.1(14) . . . . ? C11 C2 C3 C8 -177.2(9) . . . . ? C1 C2 C3 C4 -176.3(9) . . . . ? C11 C2 C3 C4 3.4(14) . . . . ? C8 C3 C4 C5 2.8(15) . . . . ? C2 C3 C4 C5 -177.8(10) . . . . ? C3 C4 C5 C6 -1.6(18) . . . . ? C4 C5 C6 C7 0(2) . . . . ? C5 C6 C7 C8 0(2) . . . . ? C4 C3 C8 C9 177.8(10) . . . . ? C2 C3 C8 C9 -1.6(15) . . . . ? C4 C3 C8 C7 -2.4(16) . . . . ? C2 C3 C8 C7 178.2(10) . . . . ? C6 C7 C8 C3 0.9(18) . . . . ? C6 C7 C8 C9 -179.3(12) . . . . ? C3 C8 C9 C10 -2.4(17) . . . . ? C7 C8 C9 C10 177.8(11) . . . . ? C8 C9 C10 C1 4.8(17) . . . . ? C2 C1 C10 C9 -3.2(16) . . . . ? P1 C1 C10 C9 -172.2(9) . . . . ? C1 C2 C11 C12 70.4(14) . . . . ? C3 C2 C11 C12 -109.2(11) . . . . ? C1 C2 C11 C20 -111.4(11) . . . . ? C3 C2 C11 C20 69.0(12) . . . . ? C20 C11 C12 C13 -2.1(16) . . . . ? C2 C11 C12 C13 176.1(11) . . . . ? C20 C11 C12 P2 -177.4(7) . . . . ? C2 C11 C12 P2 0.8(14) . . . . ? C33 P2 C12 C11 64.6(9) . . . . ? C39 P2 C12 C11 169.6(8) . . . . ? Ir P2 C12 C11 -71.7(9) . . . . ? C33 P2 C12 C13 -110.6(11) . . . . ? C39 P2 C12 C13 -5.6(11) . . . . ? Ir P2 C12 C13 113.0(10) . . . . ? C11 C12 C13 C14 -1(2) . . . . ? P2 C12 C13 C14 174.6(12) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C13 C14 C15 C16 -178.9(15) . . . . ? C13 C14 C15 C20 0(2) . . . . ? C14 C15 C16 C17 -177.9(15) . . . . ? C20 C15 C16 C17 4(2) . . . . ? C15 C16 C17 C18 -1(2) . . . . ? C16 C17 C18 C19 0(2) . . . . ? C17 C18 C19 C20 0.0(19) . . . . ? C18 C19 C20 C11 -177.8(10) . . . . ? C18 C19 C20 C15 2.1(16) . . . . ? C12 C11 C20 C19 -176.3(10) . . . . ? C2 C11 C20 C19 5.4(15) . . . . ? C12 C11 C20 C15 3.7(15) . . . . ? C2 C11 C20 C15 -174.6(10) . . . . ? C14 C15 C20 C19 177.6(11) . . . . ? C16 C15 C20 C19 -3.8(17) . . . . ? C14 C15 C20 C11 -2.5(17) . . . . ? C16 C15 C20 C11 176.1(11) . . . . ? C27 P1 C21 C26 48.6(13) . . . . ? C1 P1 C21 C26 -63.0(12) . . . . ? Ir P1 C21 C26 176.8(11) . . . . ? C27 P1 C21 C22 -126.3(11) . . . . ? C1 P1 C21 C22 122.1(11) . . . . ? Ir P1 C21 C22 1.8(12) . . . . ? C26 C21 C22 C23 -1(2) . . . . ? P1 C21 C22 C23 174.2(12) . . . . ? C21 C22 C23 C24 2(3) . . . . ? C22 C23 C24 C25 -1(3) . . . . ? C23 C24 C25 C26 -1(3) . . . . ? C22 C21 C26 C25 -1(2) . . . . ? P1 C21 C26 C25 -176.5(13) . . . . ? C24 C25 C26 C21 2(3) . . . . ? C21 P1 C27 C28 92.7(10) . . . . ? C1 P1 C27 C28 -161.0(10) . . . . ? Ir P1 C27 C28 -34.1(11) . . . . ? C21 P1 C27 C32 -80.2(10) . . . . ? C1 P1 C27 C32 26.1(11) . . . . ? Ir P1 C27 C32 153.0(8) . . . . ? C32 C27 C28 C29 2.7(19) . . . . ? P1 C27 C28 C29 -170.5(11) . . . . ? C27 C28 C29 C30 -3(2) . . . . ? C28 C29 C30 C31 1(3) . . . . ? C29 C30 C31 C32 1(3) . . . . ? C30 C31 C32 C27 -1(2) . . . . ? C28 C27 C32 C31 -1.2(19) . . . . ? P1 C27 C32 C31 171.7(11) . . . . ? C39 P2 C33 C34 -53.1(9) . . . . ? C12 P2 C33 C34 52.3(9) . . . . ? Ir P2 C33 C34 179.6(6) . . . . ? C39 P2 C33 C38 130.4(8) . . . . ? C12 P2 C33 C38 -124.2(8) . . . . ? Ir P2 C33 C38 3.1(11) . . . . ? C38 C33 C34 C35 -3.7(15) . . . . ? P2 C33 C34 C35 179.7(8) . . . . ? C33 C34 C35 C36 3.3(16) . . . . ? C34 C35 C36 C37 -0.9(19) . . . . ? C35 C36 C37 C38 -1.1(19) . . . . ? C36 C37 C38 C33 0.6(17) . . . . ? C34 C33 C38 C37 1.7(15) . . . . ? P2 C33 C38 C37 178.2(9) . . . . ? C33 P2 C39 C40 -10.2(13) . . . . ? C12 P2 C39 C40 -110.4(12) . . . . ? Ir P2 C39 C40 127.8(11) . . . . ? C33 P2 C39 C44 171.1(9) . . . . ? C12 P2 C39 C44 70.8(10) . . . . ? Ir P2 C39 C44 -50.9(10) . . . . ? C44 C39 C40 C41 -1(2) . . . . ? P2 C39 C40 C41 -179.9(12) . . . . ? C39 C40 C41 C42 -4(3) . . . . ? C40 C41 C42 C43 8(3) . . . . ? C41 C42 C43 C44 -6(3) . . . . ? C42 C43 C44 C39 1(2) . . . . ? C40 C39 C44 C43 3(2) . . . . ? P2 C39 C44 C43 -178.3(12) . . . . ? C57 P3 C45 C50 127.3(10) . . . . ? C51 P3 C45 C50 -128.3(10) . . . . ? Ir P3 C45 C50 -5.2(11) . . . . ? C57 P3 C45 C46 -56.9(11) . . . . ? C51 P3 C45 C46 47.5(11) . . . . ? Ir P3 C45 C46 170.6(9) . . . . ? C50 C45 C46 C47 -3(2) . . . . ? P3 C45 C46 C47 -179.2(12) . . . . ? C45 C46 C47 C48 1(3) . . . . ? C46 C47 C48 C49 -2(3) . . . . ? C47 C48 C49 C50 5(3) . . . . ? C46 C45 C50 C49 6.0(19) . . . . ? P3 C45 C50 C49 -178.1(11) . . . . ? C48 C49 C50 C45 -7(2) . . . . ? C57 P3 C51 C52 -178.9(11) . . . . ? C45 P3 C51 C52 73.9(12) . . . . ? Ir P3 C51 C52 -52.6(12) . . . . ? C57 P3 C51 C56 5.8(14) . . . . ? C45 P3 C51 C56 -101.4(13) . . . . ? Ir P3 C51 C56 132.1(12) . . . . ? C56 C51 C52 C53 0(2) . . . . ? P3 C51 C52 C53 -176.1(14) . . . . ? C51 C52 C53 C54 -1(3) . . . . ? C52 C53 C54 C55 2(3) . . . . ? C53 C54 C55 C56 -1(3) . . . . ? C54 C55 C56 C51 -1(3) . . . . ? C52 C51 C56 C55 1(2) . . . . ? P3 C51 C56 C55 176.8(14) . . . . ? C45 P3 C57 C58 -3.6(13) . . . . ? C51 P3 C57 C58 -107.5(12) . . . . ? Ir P3 C57 C58 129.3(11) . . . . ? C45 P3 C57 C62 179.3(9) . . . . ? C51 P3 C57 C62 75.4(10) . . . . ? Ir P3 C57 C62 -47.8(10) . . . . ? C62 C57 C58 C59 -1(2) . . . . ? P3 C57 C58 C59 -178.2(12) . . . . ? C57 C58 C59 C60 3(2) . . . . ? C58 C59 C60 C61 -5(3) . . . . ? C59 C60 C61 C62 5(2) . . . . ? C60 C61 C62 C57 -3(2) . . . . ? C58 C57 C62 C61 0.9(19) . . . . ? P3 C57 C62 C61 178.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.780 _refine_diff_density_min -2.635 _refine_diff_density_rms 0.209 #===end #===end #===end #===end #===end #===end #===end #===end #===end