Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Cameron Jones' 'Marcus Brym' 'M. Waugh' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UK ; _publ_contact_author_email JONESCA6@CARDIFF.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; The Reactivity of an Iridaphosphirene Complex, [Ir{=C(But)P(Cy)}(CO)(PPh3)2],Cy = Cyclohexyl, Toward Electrophiles ; data_compound_8 _database_code_CSD 208255 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H66 Ir O P3 S' _chemical_formula_weight 1144.32 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.675(3) _cell_length_b 37.548(8) _cell_length_c 12.036(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.17(3) _cell_angle_gamma 90.00 _cell_volume 5341.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 2.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.674 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70879 _diffrn_reflns_av_R_equivalents 0.1108 _diffrn_reflns_av_sigmaI/netI 0.0576 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.34 _reflns_number_total 9740 _reflns_number_gt 7854 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0112P)^2^+41.7359P] 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 9740 _refine_ls_number_parameters 583 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1051 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.09725(2) 0.104687(6) 0.55246(2) 0.01779(8) Uani 1 1 d . . . S1 S 0.15794(17) 0.15054(5) 0.29509(16) 0.0338(4) Uani 1 1 d . . . P1 P 0.05253(15) 0.12426(4) 0.35480(15) 0.0234(4) Uani 1 1 d . . . P2 P -0.05481(14) 0.11470(4) 0.61630(15) 0.0196(3) Uani 1 1 d . . . P3 P 0.22251(14) 0.14795(4) 0.67360(14) 0.0194(3) Uani 1 1 d . . . O1 O 0.2131(4) 0.04460(13) 0.7221(5) 0.0403(13) Uani 1 1 d . . . C1 C 0.0866(5) 0.08067(16) 0.4056(6) 0.0234(14) Uani 1 1 d . . . C2 C 0.1090(6) 0.04600(16) 0.3558(6) 0.0278(15) Uani 1 1 d . . . C3 C 0.1517(8) 0.0534(2) 0.2555(7) 0.050(2) Uani 1 1 d U . . H3A H 0.0964 0.0670 0.1946 0.075 Uiso 1 1 calc R . . H3B H 0.1645 0.0312 0.2225 0.075 Uiso 1 1 calc R . . H3C H 0.2213 0.0665 0.2859 0.075 Uiso 1 1 calc R . . C4 C -0.0026(8) 0.0257(3) 0.3036(9) 0.068(3) Uani 1 1 d U . . H4A H -0.0278 0.0188 0.3667 0.102 Uiso 1 1 calc R . . H4B H 0.0085 0.0048 0.2630 0.102 Uiso 1 1 calc R . . H4C H -0.0584 0.0407 0.2483 0.102 Uiso 1 1 calc R . . C5 C 0.1922(9) 0.0227(2) 0.4493(8) 0.062(3) Uani 1 1 d U . . H5A H 0.2631 0.0349 0.4833 0.093 Uiso 1 1 calc R . . H5B H 0.2033 0.0009 0.4132 0.093 Uiso 1 1 calc R . . H5C H 0.1629 0.0174 0.5107 0.093 Uiso 1 1 calc R . . C6 C -0.0953(6) 0.13063(17) 0.2540(6) 0.0281(15) Uani 1 1 d . . . H6 H -0.1436 0.1164 0.2846 0.034 Uiso 1 1 calc R . . C7 C -0.1162(7) 0.1183(2) 0.1261(7) 0.050(2) Uani 1 1 d . . . H7A H -0.0682 0.1317 0.0944 0.060 Uiso 1 1 calc R . . H7B H -0.0960 0.0933 0.1270 0.060 Uiso 1 1 calc R . . C8 C -0.2396(8) 0.1232(3) 0.0456(8) 0.065(3) Uani 1 1 d . . . H8A H -0.2497 0.1157 -0.0347 0.078 Uiso 1 1 calc R . . H8B H -0.2874 0.1085 0.0741 0.078 Uiso 1 1 calc R . . C9 C -0.2744(8) 0.1618(3) 0.0438(7) 0.057(2) Uani 1 1 d . . . H9A H -0.3540 0.1642 -0.0048 0.068 Uiso 1 1 calc R . . H9B H -0.2315 0.1762 0.0081 0.068 Uiso 1 1 calc R . . C10 C -0.2545(7) 0.1754(2) 0.1684(7) 0.051(2) Uani 1 1 d . . . H10A H -0.3047 0.1631 0.2002 0.062 Uiso 1 1 calc R . . H10B H -0.2720 0.2006 0.1649 0.062 Uiso 1 1 calc R . . C11 C -0.1318(7) 0.1695(2) 0.2510(7) 0.045(2) Uani 1 1 d . . . H11A H -0.0826 0.1842 0.2244 0.055 Uiso 1 1 calc R . . H11B H -0.1231 0.1770 0.3310 0.055 Uiso 1 1 calc R . . C12 C 0.1670(6) 0.06746(17) 0.6609(6) 0.0248(14) Uani 1 1 d . . . C13 C -0.1857(5) 0.10355(17) 0.4926(5) 0.0227(13) Uani 1 1 d . . . C14 C -0.1945(6) 0.06944(17) 0.4455(6) 0.0280(15) Uani 1 1 d . . . H14 H -0.1339 0.0538 0.4756 0.034 Uiso 1 1 calc R . . C15 C -0.2906(7) 0.05839(19) 0.3556(6) 0.0389(18) Uani 1 1 d . . . H15 H -0.2959 0.0352 0.3266 0.047 Uiso 1 1 calc R . . C16 C -0.3796(6) 0.08189(19) 0.3081(6) 0.0376(18) Uani 1 1 d . . . H16 H -0.4446 0.0745 0.2463 0.045 Uiso 1 1 calc R . . C17 C -0.3732(6) 0.11584(19) 0.3510(7) 0.0371(18) Uani 1 1 d . . . H17 H -0.4331 0.1315 0.3177 0.044 Uiso 1 1 calc R . . C18 C -0.2763(6) 0.12704(18) 0.4452(6) 0.0297(16) Uani 1 1 d . . . H18 H -0.2723 0.1500 0.4758 0.036 Uiso 1 1 calc R . . C19 C -0.0643(5) 0.08465(16) 0.7324(5) 0.0217(14) Uani 1 1 d . . . C20 C -0.1699(6) 0.07175(17) 0.7307(6) 0.0275(15) Uani 1 1 d . . . H20 H -0.2355 0.0771 0.6664 0.033 Uiso 1 1 calc R . . C21 C -0.1765(6) 0.05132(17) 0.8235(7) 0.0326(17) Uani 1 1 d . . . H21 H -0.2463 0.0429 0.8209 0.039 Uiso 1 1 calc R . . C22 C -0.0793(7) 0.04322(18) 0.9211(6) 0.0332(17) Uani 1 1 d . . . H22 H -0.0841 0.0297 0.9839 0.040 Uiso 1 1 calc R . . C23 C 0.0246(7) 0.05544(18) 0.9234(6) 0.0331(17) Uani 1 1 d . . . H23 H 0.0901 0.0499 0.9876 0.040 Uiso 1 1 calc R . . C24 C 0.0308(6) 0.07608(16) 0.8292(5) 0.0245(14) Uani 1 1 d . . . H24 H 0.1010 0.0842 0.8319 0.029 Uiso 1 1 calc R . . C25 C -0.0866(5) 0.15801(16) 0.6687(6) 0.0224(14) Uani 1 1 d . . . C26 C -0.1119(6) 0.16196(18) 0.7709(6) 0.0304(16) Uani 1 1 d . . . H26 H -0.1154 0.1420 0.8152 0.036 Uiso 1 1 calc R . . C27 C -0.1321(6) 0.19536(19) 0.8073(7) 0.0388(19) Uani 1 1 d . . . H27 H -0.1486 0.1977 0.8763 0.047 Uiso 1 1 calc R . . C28 C -0.1281(6) 0.22539(19) 0.7424(7) 0.0396(19) Uani 1 1 d . . . H28 H -0.1419 0.2478 0.7673 0.048 Uiso 1 1 calc R . . C29 C -0.1032(6) 0.22178(18) 0.6401(7) 0.0382(19) Uani 1 1 d . . . H29 H -0.1005 0.2419 0.5960 0.046 Uiso 1 1 calc R . . C30 C -0.0823(5) 0.18831(17) 0.6025(6) 0.0256(14) Uani 1 1 d . . . H30 H -0.0656 0.1861 0.5337 0.031 Uiso 1 1 calc R . . C31 C 0.3611(5) 0.14588(16) 0.6578(5) 0.0213(13) Uani 1 1 d . . . C32 C 0.3858(6) 0.11981(18) 0.5895(7) 0.0330(17) Uani 1 1 d . . . H32 H 0.3294 0.1043 0.5446 0.040 Uiso 1 1 calc R . . C33 C 0.4944(7) 0.1167(2) 0.5878(8) 0.043(2) Uani 1 1 d . . . H33 H 0.5105 0.0991 0.5418 0.052 Uiso 1 1 calc R . . C34 C 0.5789(6) 0.1397(2) 0.6546(7) 0.0397(19) Uani 1 1 d . . . H34 H 0.6521 0.1373 0.6550 0.048 Uiso 1 1 calc R . . C35 C 0.5544(6) 0.1662(2) 0.7204(6) 0.0375(18) Uani 1 1 d . . . H35 H 0.6107 0.1820 0.7640 0.045 Uiso 1 1 calc R . . C36 C 0.4466(6) 0.16952(19) 0.7220(6) 0.0339(17) Uani 1 1 d . . . H36 H 0.4307 0.1876 0.7662 0.041 Uiso 1 1 calc R . . C37 C 0.1892(5) 0.19561(15) 0.6533(6) 0.0213(14) Uani 1 1 d . . . C38 C 0.1434(6) 0.20839(17) 0.5367(6) 0.0276(15) Uani 1 1 d . . . H38 H 0.1312 0.1928 0.4731 0.033 Uiso 1 1 calc R . . C39 C 0.1160(6) 0.24407(18) 0.5148(7) 0.0337(17) Uani 1 1 d . . . H39 H 0.0872 0.2524 0.4369 0.040 Uiso 1 1 calc R . . C40 C 0.1313(6) 0.26740(17) 0.6086(6) 0.0337(17) Uani 1 1 d . . . H40 H 0.1097 0.2911 0.5939 0.040 Uiso 1 1 calc R . . C41 C 0.1792(7) 0.25495(18) 0.7250(7) 0.0358(18) Uani 1 1 d . . . H41 H 0.1919 0.2706 0.7883 0.043 Uiso 1 1 calc R . . C42 C 0.2081(6) 0.21959(17) 0.7471(6) 0.0273(15) Uani 1 1 d . . . H42 H 0.2405 0.2116 0.8253 0.033 Uiso 1 1 calc R . . C43 C 0.2597(6) 0.14048(16) 0.8336(6) 0.0235(14) Uani 1 1 d . . . C44 C 0.3565(7) 0.1208(2) 0.8973(7) 0.044(2) Uani 1 1 d . . . H44 H 0.4069 0.1141 0.8610 0.053 Uiso 1 1 calc R . . C45 C 0.3770(9) 0.1114(2) 1.0152(8) 0.062(3) Uani 1 1 d . . . H45 H 0.4409 0.0980 1.0569 0.075 Uiso 1 1 calc R . . C46 C 0.3040(8) 0.1216(2) 1.0708(7) 0.048(2) Uani 1 1 d . . . H46 H 0.3191 0.1154 1.1499 0.058 Uiso 1 1 calc R . . C47 C 0.2095(7) 0.14081(18) 1.0096(6) 0.0352(18) Uani 1 1 d . . . H47 H 0.1598 0.1476 1.0467 0.042 Uiso 1 1 calc R . . C48 C 0.1875(6) 0.15015(17) 0.8917(6) 0.0268(15) Uani 1 1 d . . . H48 H 0.1227 0.1632 0.8507 0.032 Uiso 1 1 calc R . . C49 C -0.5242(6) 0.2185(2) 0.2100(7) 0.0394(18) Uani 1 1 d . . . C50 C -0.4240(7) 0.2363(2) 0.2664(7) 0.0426(19) Uani 1 1 d . . . H50 H -0.3915 0.2494 0.2215 0.051 Uiso 1 1 calc R . . C51 C -0.3712(8) 0.2350(2) 0.3884(8) 0.054(2) Uani 1 1 d . . . H51 H -0.3037 0.2472 0.4248 0.064 Uiso 1 1 calc R . . C52 C -0.4170(8) 0.2159(2) 0.4567(8) 0.053(2) Uani 1 1 d . . . H52 H -0.3804 0.2145 0.5389 0.063 Uiso 1 1 calc R . . C53 C -0.5199(7) 0.1986(2) 0.4004(8) 0.048(2) Uani 1 1 d . . . H53 H -0.5539 0.1863 0.4456 0.057 Uiso 1 1 calc R . . C54 C -0.5711(6) 0.1997(2) 0.2788(7) 0.0391(18) Uani 1 1 d . . . H54 H -0.6387 0.1875 0.2423 0.047 Uiso 1 1 calc R . . C55 C -0.5821(8) 0.2198(3) 0.0753(8) 0.065(3) Uani 1 1 d . . . H55A H -0.5275 0.2153 0.0387 0.098 Uiso 1 1 calc R . . H55B H -0.6152 0.2428 0.0518 0.098 Uiso 1 1 calc R . . H55C H -0.6403 0.2019 0.0502 0.098 Uiso 1 1 calc R . . C56 C -0.4387(11) 0.0033(4) 0.7698(12) 0.124(5) Uiso 1 1 d D . . C57 C -0.3707(7) -0.0188(2) 0.8533(8) 0.055(2) Uiso 1 1 d D . . H57 H -0.3461 -0.0397 0.8291 0.065 Uiso 1 1 calc R . . C58 C -0.3368(12) -0.0114(4) 0.9721(12) 0.135(6) Uiso 1 1 d D . . H58 H -0.2932 -0.0284 1.0251 0.162 Uiso 1 1 calc R . . C59 C -0.3620(13) 0.0188(4) 1.0180(13) 0.130(5) Uiso 1 1 d D . . H59 H -0.3372 0.0249 1.0982 0.156 Uiso 1 1 calc R . . C60 C -0.4364(12) 0.0403(4) 0.9176(12) 0.112(5) Uiso 1 1 d D . . H60 H -0.4581 0.0617 0.9420 0.135 Uiso 1 1 calc R . . C61 C -0.4779(11) 0.0361(3) 0.8033(12) 0.102(4) Uiso 1 1 d D . . H61 H -0.5265 0.0521 0.7500 0.123 Uiso 1 1 calc R . . C62 C -0.4804(14) 0.0011(4) 0.6489(14) 0.145(6) Uiso 1 1 d D . . H62A H -0.4188 0.0004 0.6203 0.218 Uiso 1 1 calc R . . H62B H -0.5268 0.0215 0.6162 0.218 Uiso 1 1 calc R . . H62C H -0.5248 -0.0202 0.6247 0.218 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 0.02053(13) 0.01675(12) 0.01829(13) -0.00012(10) 0.00965(10) -0.00008(11) S1 0.0505(12) 0.0290(9) 0.0313(10) 0.0004(7) 0.0258(9) -0.0054(8) P1 0.0338(10) 0.0207(8) 0.0191(9) -0.0002(7) 0.0136(8) -0.0004(7) P2 0.0202(9) 0.0206(8) 0.0206(9) -0.0001(6) 0.0105(7) 0.0001(6) P3 0.0203(9) 0.0205(8) 0.0190(9) -0.0012(6) 0.0089(7) -0.0012(7) O1 0.047(3) 0.037(3) 0.039(3) 0.016(2) 0.018(3) 0.017(2) C1 0.020(3) 0.023(3) 0.030(4) -0.002(3) 0.012(3) -0.005(3) C2 0.038(4) 0.019(3) 0.028(4) -0.005(3) 0.014(3) -0.001(3) C3 0.065(4) 0.045(4) 0.049(4) -0.004(3) 0.031(3) 0.008(3) C4 0.069(5) 0.061(4) 0.078(5) -0.023(4) 0.033(4) -0.006(4) C5 0.077(5) 0.049(4) 0.054(4) -0.007(3) 0.018(4) 0.020(4) C6 0.038(4) 0.029(4) 0.021(4) 0.001(3) 0.014(3) 0.002(3) C7 0.052(5) 0.061(5) 0.028(4) -0.014(4) 0.005(4) 0.013(4) C8 0.064(7) 0.080(7) 0.033(5) -0.014(5) -0.006(5) 0.015(5) C9 0.048(6) 0.090(7) 0.027(5) 0.021(4) 0.005(4) 0.009(5) C10 0.053(6) 0.048(5) 0.045(5) 0.010(4) 0.007(4) 0.021(4) C11 0.062(6) 0.038(4) 0.029(4) -0.003(3) 0.007(4) 0.013(4) C12 0.026(4) 0.026(3) 0.028(4) -0.001(3) 0.017(3) 0.001(3) C13 0.022(3) 0.028(3) 0.021(3) -0.001(3) 0.010(3) -0.005(3) C14 0.026(4) 0.028(4) 0.029(4) -0.001(3) 0.009(3) -0.001(3) C15 0.051(5) 0.030(4) 0.028(4) -0.003(3) 0.005(4) -0.008(4) C16 0.030(4) 0.042(4) 0.028(4) 0.003(3) -0.005(3) -0.009(3) C17 0.024(4) 0.040(4) 0.040(5) 0.008(3) 0.003(3) 0.001(3) C18 0.024(4) 0.032(4) 0.031(4) -0.001(3) 0.007(3) -0.002(3) C19 0.024(4) 0.024(3) 0.018(3) -0.006(3) 0.009(3) 0.001(3) C20 0.029(4) 0.032(4) 0.024(4) -0.004(3) 0.013(3) -0.005(3) C21 0.037(4) 0.030(4) 0.044(5) -0.004(3) 0.031(4) -0.011(3) C22 0.052(5) 0.028(4) 0.025(4) 0.004(3) 0.020(4) -0.002(3) C23 0.043(5) 0.031(4) 0.025(4) 0.003(3) 0.012(3) -0.003(3) C24 0.029(4) 0.027(3) 0.021(4) -0.001(3) 0.013(3) -0.004(3) C25 0.016(3) 0.026(3) 0.025(4) -0.003(3) 0.006(3) -0.001(3) C26 0.025(4) 0.029(4) 0.041(4) -0.005(3) 0.017(3) -0.001(3) C27 0.031(4) 0.038(4) 0.055(5) -0.016(4) 0.025(4) -0.008(3) C28 0.033(4) 0.029(4) 0.057(5) -0.015(4) 0.017(4) -0.003(3) C29 0.022(4) 0.025(4) 0.062(6) -0.003(3) 0.008(4) -0.002(3) C30 0.023(4) 0.029(3) 0.023(4) -0.004(3) 0.006(3) 0.001(3) C31 0.022(3) 0.026(3) 0.016(3) 0.003(3) 0.007(3) 0.001(3) C32 0.033(4) 0.031(4) 0.041(4) -0.006(3) 0.020(4) -0.005(3) C33 0.040(5) 0.040(4) 0.060(6) -0.011(4) 0.032(4) 0.001(4) C34 0.023(4) 0.049(5) 0.051(5) 0.009(4) 0.019(4) 0.005(3) C35 0.024(4) 0.057(5) 0.031(4) -0.001(4) 0.010(3) -0.011(3) C36 0.035(4) 0.038(4) 0.029(4) -0.008(3) 0.012(3) -0.005(3) C37 0.024(4) 0.020(3) 0.025(4) -0.003(3) 0.015(3) -0.001(3) C38 0.037(4) 0.027(4) 0.025(4) 0.000(3) 0.018(3) -0.005(3) C39 0.045(5) 0.030(4) 0.031(4) 0.006(3) 0.019(4) -0.002(3) C40 0.047(5) 0.017(3) 0.040(4) 0.006(3) 0.019(4) 0.003(3) C41 0.048(5) 0.025(4) 0.041(5) -0.009(3) 0.024(4) -0.010(3) C42 0.034(4) 0.028(4) 0.021(4) -0.006(3) 0.011(3) -0.008(3) C43 0.030(4) 0.018(3) 0.023(4) 0.000(3) 0.010(3) -0.002(3) C44 0.055(5) 0.047(5) 0.034(5) 0.010(4) 0.020(4) 0.023(4) C45 0.082(7) 0.066(6) 0.036(5) 0.020(4) 0.018(5) 0.043(5) C46 0.084(7) 0.041(4) 0.022(4) 0.008(3) 0.023(4) 0.014(4) C47 0.053(5) 0.034(4) 0.028(4) -0.007(3) 0.026(4) -0.011(4) C48 0.024(4) 0.033(4) 0.022(4) -0.007(3) 0.008(3) -0.007(3) C49 0.033(4) 0.040(4) 0.041(5) 0.009(3) 0.007(4) 0.006(3) C50 0.036(5) 0.045(5) 0.043(5) 0.002(4) 0.009(4) -0.002(4) C51 0.041(5) 0.059(6) 0.054(6) -0.004(4) 0.010(5) -0.006(4) C52 0.060(6) 0.051(5) 0.041(5) -0.001(4) 0.012(5) 0.009(5) C53 0.053(6) 0.041(5) 0.055(6) 0.007(4) 0.028(5) 0.009(4) C54 0.030(4) 0.042(4) 0.045(5) 0.005(4) 0.013(4) 0.001(3) C55 0.060(6) 0.076(7) 0.053(6) 0.015(5) 0.011(5) -0.018(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 Ir1 C12 1.899(7) . ? Ir1 C1 1.945(6) . ? Ir1 P2 2.3486(16) . ? Ir1 P1 2.3552(17) . ? Ir1 P3 2.3692(17) . ? S1 P1 1.992(2) . ? P1 C1 1.746(6) . ? P1 C6 1.843(7) . ? P2 C19 1.833(6) . ? P2 C13 1.833(6) . ? P2 C25 1.841(6) . ? P3 C43 1.831(6) . ? P3 C37 1.835(6) . ? P3 C31 1.835(6) . ? O1 C12 1.145(8) . ? C1 C2 1.503(8) . ? C2 C5 1.513(11) . ? C2 C3 1.516(10) . ? C2 C4 1.528(11) . ? C6 C11 1.528(9) . ? C6 C7 1.536(9) . ? C7 C8 1.525(12) . ? C8 C9 1.512(12) . ? C9 C10 1.516(11) . ? C10 C11 1.530(11) . ? C13 C14 1.389(9) . ? C13 C18 1.395(9) . ? C14 C15 1.369(10) . ? C15 C16 1.383(10) . ? C16 C17 1.367(10) . ? C17 C18 1.401(10) . ? C19 C24 1.378(9) . ? C19 C20 1.417(9) . ? C20 C21 1.383(9) . ? C21 C22 1.394(10) . ? C22 C23 1.385(10) . ? C23 C24 1.399(9) . ? C25 C26 1.387(9) . ? C25 C30 1.401(9) . ? C26 C27 1.383(9) . ? C27 C28 1.383(11) . ? C28 C29 1.384(11) . ? C29 C30 1.393(9) . ? C31 C32 1.385(9) . ? C31 C36 1.399(9) . ? C32 C33 1.390(10) . ? C33 C34 1.386(11) . ? C34 C35 1.375(10) . ? C35 C36 1.378(10) . ? C37 C42 1.395(8) . ? C37 C38 1.396(9) . ? C38 C39 1.385(9) . ? C39 C40 1.386(10) . ? C40 C41 1.391(10) . ? C41 C42 1.377(9) . ? C43 C48 1.386(9) . ? C43 C44 1.400(10) . ? C44 C45 1.393(11) . ? C45 C46 1.379(12) . ? C46 C47 1.363(11) . ? C47 C48 1.389(9) . ? C49 C54 1.376(10) . ? C49 C50 1.379(11) . ? C49 C55 1.520(12) . ? C50 C51 1.377(11) . ? C51 C52 1.368(12) . ? C52 C53 1.394(12) . ? C53 C54 1.370(11) . ? C56 C57 1.348(13) . ? C56 C62 1.361(14) . ? C56 C61 1.438(13) . ? C57 C58 1.364(13) . ? C58 C59 1.351(14) . ? C59 C60 1.477(14) . ? C60 C61 1.293(13) . ? 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 C12 Ir1 C1 98.4(3) . . ? C12 Ir1 P2 97.26(19) . . ? C1 Ir1 P2 125.14(19) . . ? C12 Ir1 P1 143.75(19) . . ? C1 Ir1 P1 46.71(19) . . ? P2 Ir1 P1 110.73(6) . . ? C12 Ir1 P3 92.3(2) . . ? C1 Ir1 P3 133.50(18) . . ? P2 Ir1 P3 97.79(6) . . ? P1 Ir1 P3 105.73(6) . . ? C1 P1 C6 114.6(3) . . ? C1 P1 S1 118.5(2) . . ? C6 P1 S1 110.7(2) . . ? C1 P1 Ir1 54.2(2) . . ? C6 P1 Ir1 121.5(2) . . ? S1 P1 Ir1 124.81(10) . . ? C19 P2 C13 100.9(3) . . ? C19 P2 C25 101.5(3) . . ? C13 P2 C25 103.5(3) . . ? C19 P2 Ir1 116.0(2) . . ? C13 P2 Ir1 107.9(2) . . ? C25 P2 Ir1 124.1(2) . . ? C43 P3 C37 104.4(3) . . ? C43 P3 C31 102.1(3) . . ? C37 P3 C31 102.1(3) . . ? C43 P3 Ir1 113.8(2) . . ? C37 P3 Ir1 121.1(2) . . ? C31 P3 Ir1 111.1(2) . . ? C2 C1 P1 137.0(5) . . ? C2 C1 Ir1 143.4(5) . . ? P1 C1 Ir1 79.1(3) . . ? C1 C2 C5 112.7(6) . . ? C1 C2 C3 109.4(6) . . ? C5 C2 C3 110.1(7) . . ? C1 C2 C4 108.5(6) . . ? C5 C2 C4 108.0(7) . . ? C3 C2 C4 107.9(7) . . ? C11 C6 C7 108.9(6) . . ? C11 C6 P1 111.5(5) . . ? C7 C6 P1 112.8(5) . . ? C8 C7 C6 111.5(7) . . ? C9 C8 C7 110.7(8) . . ? C8 C9 C10 111.4(7) . . ? C9 C10 C11 111.2(7) . . ? C6 C11 C10 112.4(7) . . ? O1 C12 Ir1 175.8(6) . . ? C14 C13 C18 118.9(6) . . ? C14 C13 P2 117.2(5) . . ? C18 C13 P2 123.9(5) . . ? C15 C14 C13 121.3(7) . . ? C14 C15 C16 119.6(7) . . ? C17 C16 C15 120.6(7) . . ? C16 C17 C18 120.1(7) . . ? C13 C18 C17 119.5(6) . . ? C24 C19 C20 117.8(6) . . ? C24 C19 P2 120.7(5) . . ? C20 C19 P2 121.4(5) . . ? C21 C20 C19 120.7(7) . . ? C20 C21 C22 120.6(6) . . ? C23 C22 C21 119.3(6) . . ? C22 C23 C24 119.9(7) . . ? C19 C24 C23 121.8(6) . . ? C26 C25 C30 119.1(6) . . ? C26 C25 P2 123.2(5) . . ? C30 C25 P2 117.7(5) . . ? C27 C26 C25 120.5(7) . . ? C26 C27 C28 120.7(7) . . ? C27 C28 C29 119.3(7) . . ? C28 C29 C30 120.5(7) . . ? C29 C30 C25 119.8(6) . . ? C32 C31 C36 118.7(6) . . ? C32 C31 P3 121.5(5) . . ? C36 C31 P3 119.8(5) . . ? C31 C32 C33 120.5(7) . . ? C34 C33 C32 120.0(7) . . ? C35 C34 C33 119.9(7) . . ? C34 C35 C36 120.3(7) . . ? C35 C36 C31 120.7(7) . . ? C42 C37 C38 118.6(6) . . ? C42 C37 P3 123.9(5) . . ? C38 C37 P3 117.5(5) . . ? C39 C38 C37 120.5(6) . . ? C38 C39 C40 120.3(7) . . ? C39 C40 C41 119.3(6) . . ? C42 C41 C40 120.5(6) . . ? C41 C42 C37 120.7(6) . . ? C48 C43 C44 118.0(6) . . ? C48 C43 P3 121.7(5) . . ? C44 C43 P3 119.9(5) . . ? C45 C44 C43 119.8(7) . . ? C46 C45 C44 120.9(8) . . ? C47 C46 C45 119.8(7) . . ? C46 C47 C48 119.9(7) . . ? C43 C48 C47 121.6(7) . . ? C54 C49 C50 118.3(7) . . ? C54 C49 C55 120.8(7) . . ? C50 C49 C55 121.0(7) . . ? C51 C50 C49 121.0(8) . . ? C52 C51 C50 120.7(8) . . ? C51 C52 C53 118.5(8) . . ? C54 C53 C52 120.3(8) . . ? C53 C54 C49 121.1(8) . . ? C57 C56 C62 131.0(14) . . ? C57 C56 C61 120.8(12) . . ? C62 C56 C61 108.2(13) . . ? C56 C57 C58 122.1(11) . . ? C59 C58 C57 124.6(14) . . ? C58 C59 C60 107.6(13) . . ? C61 C60 C59 134.2(13) . . ? C60 C61 C56 110.7(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.990 #(near Ir1) _refine_diff_density_min -1.188 _refine_diff_density_rms 0.145 data_compound_5b _database_code_CSD 208256 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H60 F6 Ir O5 P3' _chemical_formula_weight 1248.18 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.767(2) _cell_length_b 14.326(3) _cell_length_c 18.809(4) _cell_angle_alpha 76.13(3) _cell_angle_beta 84.30(3) _cell_angle_gamma 84.07(3) _cell_volume 2793.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 2.543 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.787 _exptl_absorpt_process_details 'Sortav (Blessing 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43499 _diffrn_reflns_av_R_equivalents 0.0957 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 26.04 _reflns_number_total 10961 _reflns_number_gt 9534 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0686P)^2^+11.7855P] 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 10961 _refine_ls_number_parameters 605 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1404 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.94840(2) 0.096293(16) 0.179612(12) 0.02117(10) Uani 1 1 d . . . P1 P 0.97249(15) 0.25935(12) 0.13801(9) 0.0260(3) Uani 1 1 d . . . F1 F 1.4311(6) 0.5222(4) -0.1334(3) 0.0679(15) Uiso 1 1 d . . . O1 O 1.0262(5) -0.1046(3) 0.1571(3) 0.0421(13) Uani 1 1 d . . . C1 C 1.0543(6) 0.1679(5) 0.1008(4) 0.0261(13) Uani 1 1 d . . . H1 H 0.891(7) 0.314(5) 0.090(4) 0.04(2) Uiso 1 1 d . . . P2 P 0.73004(15) 0.09812(11) 0.17448(9) 0.0221(3) Uani 1 1 d . . . F2 F 1.3642(7) 0.3830(5) -0.0953(4) 0.0864(19) Uiso 1 1 d . . . O2 O 1.1971(6) 0.4226(4) -0.1893(3) 0.0508(14) Uani 1 1 d . . . C2 C 1.1469(7) 0.1651(5) 0.0354(4) 0.0333(15) Uani 1 1 d . . . P3 P 0.96155(15) 0.04847(11) 0.30832(9) 0.0231(3) Uani 1 1 d . . . F3 F 1.2693(6) 0.5027(5) -0.0606(4) 0.0809(17) Uiso 1 1 d . . . O3 O 1.2312(6) 0.5788(4) -0.2179(3) 0.0492(14) Uani 1 1 d . . . C3 C 1.0966(8) 0.2383(6) -0.0320(4) 0.0429(18) Uani 1 1 d . . . H3A H 1.0173 0.2207 -0.0415 0.064 Uiso 1 1 calc R . . H3B H 1.1550 0.2382 -0.0741 0.064 Uiso 1 1 calc R . . H3C H 1.0864 0.3017 -0.0224 0.064 Uiso 1 1 calc R . . F4 F 1.1262(15) 0.3991(13) -0.4472(9) 0.243(7) Uiso 1 1 d D . . O4 O 1.1380(9) 0.2917(6) -0.2955(4) 0.084(2) Uani 1 1 d U . . C4 C 1.1634(8) 0.0649(6) 0.0204(4) 0.0426(18) Uani 1 1 d . . . H4A H 1.2012 0.0204 0.0607 0.064 Uiso 1 1 calc R . . H4B H 1.2163 0.0659 -0.0239 0.064 Uiso 1 1 calc R . . H4C H 1.0832 0.0449 0.0151 0.064 Uiso 1 1 calc R . . F5 F 0.9941(10) 0.3096(8) -0.4073(6) 0.142(3) Uiso 1 1 d D . . O5 O 1.0780(7) 0.4433(4) -0.2961(4) 0.0610(18) Uani 1 1 d . . . H5 H 1.1104 0.4320 -0.2569 0.073 Uiso 1 1 calc R . . C5 C 1.2736(7) 0.1933(6) 0.0509(4) 0.0427(18) Uani 1 1 d . . . H5A H 1.2659 0.2599 0.0533 0.064 Uiso 1 1 calc R . . H5B H 1.3353 0.1840 0.0121 0.064 Uiso 1 1 calc R . . H5C H 1.2987 0.1537 0.0968 0.064 Uiso 1 1 calc R . . F6 F 0.9523(9) 0.4531(7) -0.4107(5) 0.125(3) Uiso 1 1 d D . . C6 C 1.0519(6) 0.3480(5) 0.1686(4) 0.0295(14) Uani 1 1 d . . . H6 H 0.9927 0.3735 0.2038 0.035 Uiso 1 1 calc R . . C7 C 1.0778(7) 0.4336(5) 0.1026(4) 0.0359(16) Uani 1 1 d . . . H7A H 1.1341 0.4110 0.0656 0.043 Uiso 1 1 calc R . . H7B H 0.9999 0.4599 0.0808 0.043 Uiso 1 1 calc R . . C8 C 1.1356(8) 0.5120(5) 0.1267(5) 0.0435(18) Uani 1 1 d . . . H8A H 1.1581 0.5620 0.0839 0.052 Uiso 1 1 calc R . . H8B H 1.0744 0.5410 0.1582 0.052 Uiso 1 1 calc R . . C9 C 1.2512(8) 0.4728(6) 0.1677(5) 0.047(2) Uani 1 1 d . . . H9A H 1.2813 0.5239 0.1856 0.057 Uiso 1 1 calc R . . H9B H 1.3166 0.4521 0.1342 0.057 Uiso 1 1 calc R . . C10 C 1.2250(8) 0.3884(6) 0.2322(4) 0.0438(19) Uani 1 1 d . . . H10A H 1.3023 0.3632 0.2550 0.053 Uiso 1 1 calc R . . H10B H 1.1668 0.4107 0.2685 0.053 Uiso 1 1 calc R . . C11 C 1.1705(7) 0.3088(6) 0.2078(4) 0.0374(16) Uani 1 1 d . . . H11A H 1.1509 0.2574 0.2503 0.045 Uiso 1 1 calc R . . H11B H 1.2317 0.2822 0.1750 0.045 Uiso 1 1 calc R . . C12 C 0.6636(6) -0.0081(4) 0.1598(3) 0.0250(13) Uani 1 1 d . . . C13 C 0.7108(6) -0.1012(5) 0.1895(3) 0.0269(13) Uani 1 1 d . . . H13 H 0.7807 -0.1115 0.2166 0.032 Uiso 1 1 calc R . . C14 C 0.6547(7) -0.1797(5) 0.1793(4) 0.0343(16) Uani 1 1 d . . . H14 H 0.6866 -0.2421 0.2001 0.041 Uiso 1 1 calc R . . C15 C 0.5524(7) -0.1658(5) 0.1387(4) 0.0342(16) Uani 1 1 d . . . H15 H 0.5152 -0.2186 0.1320 0.041 Uiso 1 1 calc R . . C16 C 0.5050(7) -0.0736(5) 0.1081(4) 0.0346(16) Uani 1 1 d . . . H16 H 0.4361 -0.0645 0.0803 0.042 Uiso 1 1 calc R . . C17 C 0.5587(6) 0.0060(5) 0.1181(4) 0.0297(14) Uani 1 1 d . . . H17 H 0.5256 0.0681 0.0975 0.036 Uiso 1 1 calc R . . C18 C 0.6919(6) 0.1855(4) 0.0885(3) 0.0255(13) Uani 1 1 d . . . C19 C 0.5989(7) 0.2608(5) 0.0852(4) 0.0340(15) Uani 1 1 d . . . H19 H 0.5543 0.2709 0.1281 0.041 Uiso 1 1 calc R . . C20 C 0.5728(7) 0.3210(6) 0.0180(4) 0.0409(18) Uani 1 1 d . . . H20 H 0.5103 0.3712 0.0159 0.049 Uiso 1 1 calc R . . C21 C 0.6393(7) 0.3069(5) -0.0468(4) 0.0383(17) Uani 1 1 d . . . H21 H 0.6222 0.3478 -0.0918 0.046 Uiso 1 1 calc R . . C22 C 0.7312(7) 0.2313(6) -0.0427(4) 0.0386(17) Uani 1 1 d . . . H22 H 0.7744 0.2199 -0.0855 0.046 Uiso 1 1 calc R . . C23 C 0.7593(7) 0.1727(5) 0.0239(4) 0.0323(15) Uani 1 1 d . . . H23 H 0.8239 0.1240 0.0259 0.039 Uiso 1 1 calc R . . C24 C 0.6201(6) 0.1362(4) 0.2440(3) 0.0241(13) Uani 1 1 d . . . C25 C 0.6273(6) 0.2283(5) 0.2572(4) 0.0291(14) Uani 1 1 d . . . H25 H 0.6886 0.2673 0.2315 0.035 Uiso 1 1 calc R . . C26 C 0.5428(7) 0.2608(6) 0.3087(4) 0.0408(18) Uani 1 1 d . . . H26 H 0.5475 0.3215 0.3174 0.049 Uiso 1 1 calc R . . C27 C 0.4523(7) 0.2032(6) 0.3466(4) 0.0439(19) Uani 1 1 d . . . H27 H 0.3953 0.2256 0.3805 0.053 Uiso 1 1 calc R . . C28 C 0.4452(7) 0.1124(6) 0.3349(4) 0.0404(17) Uani 1 1 d . . . H28 H 0.3839 0.0738 0.3611 0.049 Uiso 1 1 calc R . . C29 C 0.5293(6) 0.0790(5) 0.2843(4) 0.0328(15) Uani 1 1 d . . . H29 H 0.5248 0.0175 0.2771 0.039 Uiso 1 1 calc R . . C30 C 1.0981(6) -0.0379(5) 0.3313(4) 0.0274(14) Uani 1 1 d . . . C31 C 1.2020(6) -0.0383(5) 0.2821(4) 0.0307(14) Uani 1 1 d . . . H31 H 1.2017 0.0045 0.2363 0.037 Uiso 1 1 calc R . . C32 C 1.3064(7) -0.1013(6) 0.2998(4) 0.0414(18) Uani 1 1 d . . . H32 H 1.3755 -0.1007 0.2659 0.050 Uiso 1 1 calc R . . C33 C 1.3088(8) -0.1656(6) 0.3683(5) 0.0451(19) Uani 1 1 d . . . H33 H 1.3784 -0.2088 0.3801 0.054 Uiso 1 1 calc R . . C34 C 1.2060(8) -0.1644(6) 0.4187(4) 0.0463(19) Uani 1 1 d . . . H34 H 1.2077 -0.2059 0.4649 0.056 Uiso 1 1 calc R . . C35 C 1.1010(7) -0.1022(5) 0.4010(4) 0.0372(16) Uani 1 1 d . . . H35 H 1.0321 -0.1027 0.4351 0.045 Uiso 1 1 calc R . . C36 C 0.9881(6) 0.1466(5) 0.3505(3) 0.0247(13) Uani 1 1 d . . . C37 C 0.9126(7) 0.2334(5) 0.3335(4) 0.0315(15) Uani 1 1 d . . . H37 H 0.8514 0.2406 0.3006 0.038 Uiso 1 1 calc R . . C38 C 0.9286(7) 0.3083(5) 0.3652(4) 0.0366(16) Uani 1 1 d . . . H38 H 0.8778 0.3655 0.3537 0.044 Uiso 1 1 calc R . . C39 C 1.0195(8) 0.2989(5) 0.4140(4) 0.0416(18) Uani 1 1 d . . . H39 H 1.0304 0.3496 0.4352 0.050 Uiso 1 1 calc R . . C40 C 1.0931(7) 0.2143(5) 0.4308(4) 0.0378(17) Uani 1 1 d . . . H40 H 1.1546 0.2079 0.4635 0.045 Uiso 1 1 calc R . . C41 C 1.0779(6) 0.1375(5) 0.4000(4) 0.0291(14) Uani 1 1 d . . . H41 H 1.1281 0.0801 0.4126 0.035 Uiso 1 1 calc R . . C42 C 0.8338(6) -0.0104(5) 0.3683(3) 0.0266(13) Uani 1 1 d . . . C43 C 0.7609(6) 0.0320(5) 0.4193(4) 0.0316(15) Uani 1 1 d . . . H43 H 0.7784 0.0917 0.4253 0.038 Uiso 1 1 calc R . . C44 C 0.6626(7) -0.0145(5) 0.4611(4) 0.0368(16) Uani 1 1 d . . . H44 H 0.6151 0.0135 0.4958 0.044 Uiso 1 1 calc R . . C45 C 0.6344(7) -0.1033(5) 0.4513(4) 0.0372(16) Uani 1 1 d . . . H45 H 0.5670 -0.1335 0.4788 0.045 Uiso 1 1 calc R . . C46 C 0.7052(7) -0.1460(5) 0.4017(4) 0.0354(16) Uani 1 1 d . . . H46 H 0.6860 -0.2052 0.3954 0.042 Uiso 1 1 calc R . . C47 C 0.8069(6) -0.1005(5) 0.3602(4) 0.0290(14) Uani 1 1 d . . . H47 H 0.8564 -0.1302 0.3272 0.035 Uiso 1 1 calc R . . C48 C 0.9961(6) -0.0292(5) 0.1661(3) 0.0291(14) Uani 1 1 d . . . C49 C 1.2454(7) 0.4963(5) -0.1823(4) 0.0332(15) Uani 1 1 d . . . C50 C 1.3290(7) 0.4754(5) -0.1193(5) 0.0417(18) Uani 1 1 d . . . C51 C 1.0880(10) 0.3677(6) -0.3202(5) 0.054(2) Uani 1 1 d D . . C52 C 1.0366(12) 0.3831(9) -0.3926(7) 0.088(4) Uiso 1 1 d D . . C53 C 1.4913(12) 0.5569(10) -0.4204(7) 0.090(4) Uiso 1 1 d D . . C54 C 1.6142(13) 0.5402(10) -0.4001(7) 0.099(4) Uiso 1 1 d D . . H54 H 1.6754 0.5809 -0.4232 0.119 Uiso 1 1 calc R . . C55 C 1.640(2) 0.4619(12) -0.3450(9) 0.154(7) Uiso 1 1 d D . . H55 H 1.7222 0.4494 -0.3313 0.185 Uiso 1 1 calc R . . C56 C 1.5549(15) 0.4011(13) -0.3089(10) 0.125(6) Uiso 1 1 d D . . H56 H 1.5760 0.3487 -0.2709 0.150 Uiso 1 1 calc R . . C57 C 1.4393(18) 0.4198(13) -0.3304(10) 0.141(7) Uiso 1 1 d D . . H57 H 1.3789 0.3779 -0.3079 0.169 Uiso 1 1 calc R . . C58 C 1.4060(14) 0.4977(10) -0.3838(7) 0.091(4) Uiso 1 1 d D . . H58 H 1.3230 0.5103 -0.3953 0.109 Uiso 1 1 calc R . . C59 C 1.4559(18) 0.6368(13) -0.4794(10) 0.136(6) Uiso 1 1 d D . . H59A H 1.4223 0.6132 -0.5165 0.204 Uiso 1 1 calc R . . H59B H 1.5281 0.6708 -0.5002 0.204 Uiso 1 1 calc R . . H59C H 1.3936 0.6797 -0.4607 0.204 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 0.02076(14) 0.02113(14) 0.02151(14) -0.00586(9) 0.00064(9) -0.00125(9) P1 0.0237(8) 0.0235(8) 0.0296(9) -0.0048(7) 0.0012(7) -0.0023(7) O1 0.049(3) 0.026(3) 0.054(3) -0.021(2) 0.006(3) 0.001(2) C1 0.021(3) 0.031(3) 0.028(3) -0.011(3) -0.003(3) 0.002(3) P2 0.0224(8) 0.0212(8) 0.0227(8) -0.0052(6) -0.0006(6) -0.0022(6) O2 0.067(4) 0.034(3) 0.053(3) -0.008(3) -0.017(3) -0.007(3) C2 0.029(4) 0.040(4) 0.029(4) -0.005(3) 0.004(3) -0.009(3) P3 0.0227(8) 0.0232(8) 0.0232(8) -0.0063(6) 0.0004(6) -0.0006(6) O3 0.053(3) 0.028(3) 0.066(4) -0.006(3) -0.015(3) -0.003(2) C3 0.042(4) 0.055(5) 0.029(4) -0.008(3) 0.004(3) -0.005(4) O4 0.109(4) 0.069(4) 0.082(4) -0.031(3) -0.033(3) 0.010(3) C4 0.045(4) 0.047(4) 0.037(4) -0.020(3) 0.019(3) -0.006(4) O5 0.090(5) 0.035(3) 0.065(4) -0.022(3) -0.038(4) 0.014(3) C5 0.025(4) 0.062(5) 0.042(4) -0.015(4) 0.006(3) -0.007(4) C6 0.027(3) 0.029(3) 0.033(4) -0.009(3) 0.002(3) -0.003(3) C7 0.036(4) 0.025(3) 0.043(4) 0.000(3) -0.003(3) -0.004(3) C8 0.052(5) 0.030(4) 0.049(5) -0.009(3) 0.004(4) -0.013(3) C9 0.046(5) 0.043(4) 0.055(5) -0.006(4) -0.010(4) -0.019(4) C10 0.044(4) 0.046(4) 0.044(4) -0.007(4) -0.012(4) -0.014(4) C11 0.033(4) 0.044(4) 0.034(4) -0.004(3) -0.003(3) -0.007(3) C12 0.022(3) 0.025(3) 0.028(3) -0.008(3) 0.003(3) -0.004(3) C13 0.027(3) 0.027(3) 0.026(3) -0.006(3) 0.000(3) -0.004(3) C14 0.042(4) 0.025(3) 0.036(4) -0.007(3) 0.005(3) -0.008(3) C15 0.034(4) 0.035(4) 0.039(4) -0.016(3) 0.004(3) -0.012(3) C16 0.029(4) 0.039(4) 0.039(4) -0.013(3) -0.002(3) -0.008(3) C17 0.023(3) 0.031(3) 0.036(4) -0.011(3) -0.001(3) -0.001(3) C18 0.029(3) 0.021(3) 0.028(3) -0.005(3) -0.005(3) -0.008(3) C19 0.035(4) 0.036(4) 0.032(4) -0.011(3) -0.005(3) 0.001(3) C20 0.038(4) 0.036(4) 0.049(5) -0.010(3) -0.015(4) 0.003(3) C21 0.043(4) 0.036(4) 0.034(4) 0.005(3) -0.015(3) -0.013(3) C22 0.036(4) 0.047(4) 0.031(4) -0.003(3) -0.002(3) -0.010(3) C23 0.033(4) 0.034(4) 0.031(4) -0.008(3) -0.003(3) -0.005(3) C24 0.021(3) 0.026(3) 0.025(3) -0.006(3) 0.000(2) 0.002(3) C25 0.032(4) 0.027(3) 0.028(3) -0.006(3) -0.001(3) -0.005(3) C26 0.042(4) 0.040(4) 0.043(4) -0.018(3) -0.005(3) 0.007(3) C27 0.040(4) 0.053(5) 0.037(4) -0.017(4) 0.008(3) 0.013(4) C28 0.033(4) 0.046(4) 0.039(4) -0.008(3) 0.013(3) -0.006(3) C29 0.032(4) 0.033(4) 0.034(4) -0.010(3) 0.004(3) -0.003(3) C30 0.025(3) 0.027(3) 0.031(3) -0.010(3) -0.003(3) 0.002(3) C31 0.026(3) 0.034(4) 0.032(4) -0.008(3) -0.001(3) 0.000(3) C32 0.029(4) 0.049(5) 0.048(5) -0.019(4) -0.004(3) 0.007(3) C33 0.040(4) 0.037(4) 0.059(5) -0.014(4) -0.009(4) 0.007(3) C34 0.048(5) 0.044(4) 0.037(4) 0.002(3) -0.005(4) 0.013(4) C35 0.035(4) 0.037(4) 0.034(4) -0.002(3) 0.000(3) 0.002(3) C36 0.025(3) 0.027(3) 0.022(3) -0.009(3) 0.004(2) -0.004(3) C37 0.039(4) 0.031(4) 0.025(3) -0.007(3) -0.002(3) -0.005(3) C38 0.047(4) 0.027(3) 0.034(4) -0.010(3) -0.001(3) 0.006(3) C39 0.065(5) 0.033(4) 0.032(4) -0.015(3) 0.003(4) -0.014(4) C40 0.044(4) 0.044(4) 0.030(4) -0.012(3) -0.009(3) -0.008(3) C41 0.031(3) 0.030(3) 0.026(3) -0.007(3) -0.001(3) -0.002(3) C42 0.026(3) 0.030(3) 0.022(3) -0.003(3) -0.004(3) 0.000(3) C43 0.030(3) 0.033(4) 0.030(4) -0.008(3) 0.003(3) 0.000(3) C44 0.032(4) 0.044(4) 0.032(4) -0.009(3) 0.008(3) 0.003(3) C45 0.030(4) 0.039(4) 0.038(4) 0.001(3) 0.003(3) -0.008(3) C46 0.038(4) 0.034(4) 0.034(4) -0.004(3) -0.003(3) -0.010(3) C47 0.032(4) 0.031(3) 0.023(3) -0.008(3) 0.003(3) -0.003(3) C48 0.027(3) 0.040(4) 0.019(3) -0.005(3) 0.006(3) -0.005(3) C49 0.033(4) 0.025(3) 0.042(4) -0.008(3) -0.002(3) -0.002(3) C50 0.041(4) 0.025(4) 0.059(5) -0.012(3) -0.005(4) -0.002(3) C51 0.083(7) 0.025(4) 0.057(5) -0.015(4) -0.028(5) 0.012(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C48 1.887(7) . ? Ir1 C1 1.931(7) . ? Ir1 P1 2.3119(17) . ? Ir1 P2 2.3597(17) . ? Ir1 P3 2.3671(17) . ? P1 C1 1.750(6) . ? P1 C6 1.830(7) . ? F1 C50 1.318(9) . ? O1 C48 1.143(8) . ? C1 C2 1.510(9) . ? P2 C24 1.819(6) . ? P2 C12 1.836(6) . ? P2 C18 1.845(6) . ? F2 C50 1.320(10) . ? O2 C49 1.262(9) . ? C2 C4 1.518(10) . ? C2 C5 1.535(10) . ? C2 C3 1.544(10) . ? P3 C42 1.830(7) . ? P3 C36 1.831(6) . ? P3 C30 1.836(7) . ? F3 C50 1.341(10) . ? O3 C49 1.214(8) . ? F4 C52 1.332(14) . ? O4 C51 1.175(10) . ? F5 C52 1.288(12) . ? O5 C51 1.261(9) . ? F6 C52 1.286(12) . ? C6 C11 1.527(10) . ? C6 C7 1.548(9) . ? C7 C8 1.517(10) . ? C8 C9 1.515(12) . ? C9 C10 1.520(11) . ? C10 C11 1.517(10) . ? C12 C13 1.382(9) . ? C12 C17 1.408(9) . ? C13 C14 1.390(9) . ? C14 C15 1.373(10) . ? C15 C16 1.375(10) . ? C16 C17 1.391(9) . ? C18 C19 1.388(10) . ? C18 C23 1.394(10) . ? C19 C20 1.386(10) . ? C20 C21 1.397(12) . ? C21 C22 1.383(11) . ? C22 C23 1.371(10) . ? C24 C29 1.386(9) . ? C24 C25 1.411(9) . ? C25 C26 1.391(10) . ? C26 C27 1.372(11) . ? C27 C28 1.381(11) . ? C28 C29 1.384(10) . ? C30 C31 1.380(9) . ? C30 C35 1.411(10) . ? C31 C32 1.383(10) . ? C32 C33 1.393(12) . ? C33 C34 1.384(12) . ? C34 C35 1.381(11) . ? C36 C41 1.382(9) . ? C36 C37 1.400(10) . ? C37 C38 1.380(9) . ? C38 C39 1.382(11) . ? C39 C40 1.365(11) . ? C40 C41 1.392(10) . ? C42 C43 1.392(9) . ? C42 C47 1.397(9) . ? C43 C44 1.382(10) . ? C44 C45 1.396(11) . ? C45 C46 1.364(11) . ? C46 C47 1.403(10) . ? C49 C50 1.514(11) . ? C51 C52 1.480(12) . ? C53 C58 1.337(17) . ? C53 C54 1.394(13) . ? C53 C59 1.44(2) . ? C54 C55 1.360(14) . ? C55 C56 1.351(14) . ? C56 C57 1.329(14) . ? C57 C58 1.355(13) . ? 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 C48 Ir1 C1 99.0(3) . . ? C48 Ir1 P1 146.62(19) . . ? C1 Ir1 P1 47.68(19) . . ? C48 Ir1 P2 99.0(2) . . ? C1 Ir1 P2 122.59(19) . . ? P1 Ir1 P2 99.70(6) . . ? C48 Ir1 P3 93.3(2) . . ? C1 Ir1 P3 132.81(19) . . ? P1 Ir1 P3 110.39(6) . . ? P2 Ir1 P3 99.83(6) . . ? C1 P1 C6 122.5(3) . . ? C1 P1 Ir1 54.7(2) . . ? C6 P1 Ir1 135.4(2) . . ? C2 C1 P1 135.0(5) . . ? C2 C1 Ir1 147.1(5) . . ? P1 C1 Ir1 77.7(3) . . ? C24 P2 C12 103.4(3) . . ? C24 P2 C18 103.8(3) . . ? C12 P2 C18 99.5(3) . . ? C24 P2 Ir1 121.4(2) . . ? C12 P2 Ir1 119.6(2) . . ? C18 P2 Ir1 105.9(2) . . ? C1 C2 C4 110.6(6) . . ? C1 C2 C5 109.2(6) . . ? C4 C2 C5 109.4(6) . . ? C1 C2 C3 108.3(6) . . ? C4 C2 C3 109.6(6) . . ? C5 C2 C3 109.6(6) . . ? C42 P3 C36 103.2(3) . . ? C42 P3 C30 103.1(3) . . ? C36 P3 C30 103.0(3) . . ? C42 P3 Ir1 120.7(2) . . ? C36 P3 Ir1 114.0(2) . . ? C30 P3 Ir1 110.9(2) . . ? C11 C6 C7 111.2(6) . . ? C11 C6 P1 115.5(5) . . ? C7 C6 P1 109.2(5) . . ? C8 C7 C6 110.8(6) . . ? C9 C8 C7 111.8(6) . . ? C8 C9 C10 112.1(7) . . ? C11 C10 C9 111.3(6) . . ? C10 C11 C6 110.3(6) . . ? C13 C12 C17 118.9(6) . . ? C13 C12 P2 122.5(5) . . ? C17 C12 P2 118.6(5) . . ? C12 C13 C14 120.6(6) . . ? C15 C14 C13 120.4(7) . . ? C14 C15 C16 119.8(6) . . ? C15 C16 C17 120.9(7) . . ? C16 C17 C12 119.4(6) . . ? C19 C18 C23 119.2(6) . . ? C19 C18 P2 123.5(5) . . ? C23 C18 P2 117.3(5) . . ? C20 C19 C18 119.8(7) . . ? C19 C20 C21 120.7(7) . . ? C22 C21 C20 118.8(7) . . ? C23 C22 C21 120.8(7) . . ? C22 C23 C18 120.6(7) . . ? C29 C24 C25 118.6(6) . . ? C29 C24 P2 123.0(5) . . ? C25 C24 P2 118.5(5) . . ? C26 C25 C24 120.0(6) . . ? C27 C26 C25 120.0(7) . . ? C26 C27 C28 120.6(7) . . ? C27 C28 C29 120.0(7) . . ? C28 C29 C24 120.8(7) . . ? C31 C30 C35 118.7(6) . . ? C31 C30 P3 120.7(5) . . ? C35 C30 P3 120.6(5) . . ? C30 C31 C32 121.0(7) . . ? C31 C32 C33 120.3(7) . . ? C34 C33 C32 119.1(7) . . ? C35 C34 C33 120.8(7) . . ? C34 C35 C30 120.1(7) . . ? C41 C36 C37 118.7(6) . . ? C41 C36 P3 122.5(5) . . ? C37 C36 P3 118.8(5) . . ? C38 C37 C36 120.3(6) . . ? C37 C38 C39 120.6(7) . . ? C40 C39 C38 119.2(6) . . ? C39 C40 C41 121.3(7) . . ? C36 C41 C40 119.9(6) . . ? C43 C42 C47 119.3(6) . . ? C43 C42 P3 122.9(5) . . ? C47 C42 P3 117.8(5) . . ? C44 C43 C42 120.2(7) . . ? C43 C44 C45 120.1(7) . . ? C46 C45 C44 120.4(6) . . ? C45 C46 C47 119.9(7) . . ? C42 C47 C46 120.1(6) . . ? O1 C48 Ir1 178.9(6) . . ? O3 C49 O2 128.7(7) . . ? O3 C49 C50 118.0(6) . . ? O2 C49 C50 113.2(6) . . ? F1 C50 F2 107.4(7) . . ? F1 C50 F3 104.6(6) . . ? F2 C50 F3 104.9(7) . . ? F1 C50 C49 114.2(7) . . ? F2 C50 C49 114.0(6) . . ? F3 C50 C49 110.9(7) . . ? O4 C51 O5 129.0(8) . . ? O4 C51 C52 118.0(8) . . ? O5 C51 C52 112.9(8) . . ? F6 C52 F5 105.3(11) . . ? F6 C52 F4 104.3(12) . . ? F5 C52 F4 98.4(12) . . ? F6 C52 C51 118.4(11) . . ? F5 C52 C51 116.6(11) . . ? F4 C52 C51 111.4(13) . . ? C58 C53 C54 119.0(14) . . ? C58 C53 C59 120.2(14) . . ? C54 C53 C59 120.8(14) . . ? C55 C54 C53 117.0(16) . . ? C56 C55 C54 124(2) . . ? C57 C56 C55 116.7(19) . . ? C56 C57 C58 122.4(19) . . ? C53 C58 C57 120.8(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.972 #(near Ir1) _refine_diff_density_min -1.992 #(near Ir1) _refine_diff_density_rms 0.164 data_compound_6 _database_code_CSD 208257 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H61 B F4 Ir O2 P3' _chemical_formula_weight 1089.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.183(4) _cell_length_b 16.407(3) _cell_length_c 15.806(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4974.7(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 2.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.758 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85374 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5892 _reflns_number_gt 4957 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0392P)^2^+34.6186P] 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 5892 _refine_ls_number_parameters 320 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1258 _refine_ls_wR_factor_gt 0.1199 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.095 _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 Ir1 Ir 0.804230(16) 0.2500 0.06576(2) 0.02816(11) Uani 1 2 d S . . P1 P 0.88344(13) 0.2500 -0.04585(18) 0.0437(6) Uani 1 2 d S . . P2 P 0.79703(7) 0.10784(9) 0.06572(9) 0.0295(3) Uani 1 1 d . . . F1 F 0.5462(4) 0.2500 -0.2389(4) 0.0658(18) Uani 1 2 d S . . F2 F 0.4941(2) 0.1807(2) -0.1321(3) 0.0627(12) Uani 1 1 d . . . F3 F 0.5937(3) 0.2500 -0.1079(4) 0.0604(16) Uani 1 2 d S . . O1 O 0.7022(4) 0.2500 0.2106(5) 0.063(2) Uani 1 2 d S . . O2 O 0.8841(6) 0.2500 0.3819(7) 0.092(3) Uiso 1 2 d SD . . C1 C 0.9664(7) 0.2500 -0.0604(9) 0.078(4) Uani 1 2 d SU . . H1 H 0.9798 0.2500 -0.1170 0.094 Uiso 1 2 calc SR . . C2 C 1.0223(8) 0.2500 -0.0028(10) 0.084(4) Uani 1 2 d SU . . C3 C 0.9985(12) 0.2500 0.0886(13) 0.137(8) Uani 1 2 d SU . . H3A H 0.9488 0.2566 0.0908 0.206 Uiso 0.50 1 calc PR . . H3B H 1.0205 0.2941 0.1183 0.206 Uiso 0.50 1 calc PR . . H3C H 1.0112 0.1993 0.1147 0.206 Uiso 0.50 1 calc PR . . C4 C 1.0717(8) 0.1796(9) -0.0163(10) 0.136(5) Uani 1 1 d U . . H4A H 1.0516 0.1308 0.0068 0.204 Uiso 1 1 calc R . . H4B H 1.1151 0.1908 0.0116 0.204 Uiso 1 1 calc R . . H4C H 1.0797 0.1724 -0.0757 0.204 Uiso 1 1 calc R . . C5 C 0.8427(7) 0.2500 -0.1622(11) 0.096(5) Uani 1 2 d SD . . C6 C 0.7626(6) 0.2347(10) -0.1503(7) 0.037(5) Uani 0.50 1 d PD . . C7 C 0.7314(11) 0.2147(12) -0.2386(11) 0.099(7) Uani 0.50 1 d PDU . . C8 C 0.7596(10) 0.2244(13) -0.3058(12) 0.098(7) Uani 0.50 1 d PDU . . C9 C 0.8393(10) 0.2252(14) -0.3122(13) 0.107(8) Uani 0.50 1 d PDU . . C10 C 0.8605(11) 0.1917(12) -0.2296(11) 0.085(6) Uani 0.50 1 d PDU . . C11 C 0.7413(5) 0.2500 0.1552(6) 0.038(2) Uani 1 2 d S . . C12 C 0.8420(3) 0.0577(4) 0.1535(4) 0.0350(13) Uani 1 1 d . . . C13 C 0.8580(4) 0.1001(4) 0.2256(4) 0.0449(16) Uani 1 1 d . . . H13 H 0.8486 0.1556 0.2288 0.054 Uiso 1 1 calc R . . C14 C 0.8886(4) 0.0600(5) 0.2945(5) 0.061(2) Uani 1 1 d . . . H14 H 0.8999 0.0892 0.3430 0.073 Uiso 1 1 calc R . . C15 C 0.9019(4) -0.0217(5) 0.2907(5) 0.060(2) Uani 1 1 d . . . H15 H 0.9210 -0.0483 0.3372 0.071 Uiso 1 1 calc R . . C16 C 0.8871(4) -0.0648(5) 0.2180(5) 0.062(2) Uani 1 1 d . . . H16 H 0.8973 -0.1202 0.2150 0.075 Uiso 1 1 calc R . . C17 C 0.8570(4) -0.0255(4) 0.1496(5) 0.0490(17) Uani 1 1 d . . . H17 H 0.8467 -0.0548 0.1008 0.059 Uiso 1 1 calc R . . C18 C 0.7065(3) 0.0748(4) 0.0729(4) 0.0325(12) Uani 1 1 d . . . C19 C 0.6858(4) 0.0061(4) 0.1161(4) 0.0503(18) Uani 1 1 d . . . H19 H 0.7185 -0.0244 0.1459 0.060 Uiso 1 1 calc R . . C20 C 0.6171(4) -0.0178(6) 0.1157(5) 0.067(3) Uani 1 1 d . . . H20 H 0.6039 -0.0645 0.1451 0.081 Uiso 1 1 calc R . . C21 C 0.5673(4) 0.0265(5) 0.0722(4) 0.056(2) Uani 1 1 d . . . H21 H 0.5209 0.0101 0.0727 0.067 Uiso 1 1 calc R . . C22 C 0.5869(3) 0.0943(5) 0.0287(5) 0.0499(17) Uani 1 1 d . . . H22 H 0.5538 0.1240 -0.0013 0.060 Uiso 1 1 calc R . . C23 C 0.6568(3) 0.1197(4) 0.0288(4) 0.0395(14) Uani 1 1 d . . . H23 H 0.6698 0.1664 -0.0005 0.047 Uiso 1 1 calc R . . C24 C 0.8290(3) 0.0516(3) -0.0265(4) 0.0321(12) Uani 1 1 d . . . C25 C 0.9007(3) 0.0460(4) -0.0411(4) 0.0401(14) Uani 1 1 d . . . H25 H 0.9314 0.0699 -0.0029 0.048 Uiso 1 1 calc R . . C26 C 0.9271(4) 0.0060(4) -0.1107(5) 0.0489(17) Uani 1 1 d . . . H26 H 0.9749 0.0034 -0.1196 0.059 Uiso 1 1 calc R . . C27 C 0.8818(5) -0.0302(5) -0.1670(5) 0.063(2) Uani 1 1 d . . . H27 H 0.8991 -0.0580 -0.2138 0.075 Uiso 1 1 calc R . . C28 C 0.8114(5) -0.0253(5) -0.1541(5) 0.063(2) Uani 1 1 d . . . H28 H 0.7812 -0.0503 -0.1921 0.076 Uiso 1 1 calc R . . C29 C 0.7843(4) 0.0163(4) -0.0853(4) 0.0456(16) Uani 1 1 d . . . H29 H 0.7363 0.0206 -0.0784 0.055 Uiso 1 1 calc R . . C30 C 1.0006(8) 0.2500 0.3327(10) 0.099(5) Uiso 1 2 d SD . . H30A H 1.0469 0.2614 0.3526 0.148 Uiso 0.50 1 calc PR . . H30B H 0.9868 0.2911 0.2928 0.148 Uiso 0.50 1 calc PR . . H30C H 0.9998 0.1976 0.3058 0.148 Uiso 0.50 1 calc PR . . C31 C 0.9510(7) 0.2500 0.4062(9) 0.083(4) Uiso 1 2 d SD . . H31A H 0.9597 0.2022 0.4408 0.099 Uiso 0.50 1 calc PR . . H31B H 0.9597 0.2978 0.4408 0.099 Uiso 0.50 1 calc PR . . C32 C 0.8397(12) 0.2500 0.4546(13) 0.158(9) Uiso 1 2 d SD . . H32A H 0.8496 0.2978 0.4887 0.190 Uiso 0.50 1 calc PR . . H32B H 0.8496 0.2022 0.4887 0.190 Uiso 0.50 1 calc PR . . C33 C 0.7664(16) 0.2500 0.431(3) 0.31(2) Uiso 1 2 d SD . . H33A H 0.7451 0.2001 0.4493 0.467 Uiso 0.50 1 calc PR . . H33B H 0.7623 0.2547 0.3707 0.467 Uiso 0.50 1 calc PR . . H33C H 0.7433 0.2953 0.4575 0.467 Uiso 0.50 1 calc PR . . B1 B 0.5320(6) 0.2500 -0.1518(8) 0.046(3) Uani 1 2 d S . . 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 0.03126(17) 0.02230(15) 0.03091(17) 0.000 -0.00421(14) 0.000 P1 0.0418(13) 0.0238(10) 0.0655(17) 0.000 0.0175(12) 0.000 P2 0.0330(7) 0.0241(7) 0.0315(7) 0.0032(6) -0.0057(6) -0.0010(6) F1 0.086(5) 0.053(4) 0.059(4) 0.000 -0.005(4) 0.000 F2 0.055(3) 0.044(2) 0.090(3) 0.012(2) -0.010(2) -0.014(2) F3 0.042(3) 0.064(4) 0.075(4) 0.000 -0.011(3) 0.000 O1 0.073(5) 0.061(5) 0.056(5) 0.000 0.020(4) 0.000 C1 0.077(5) 0.074(5) 0.083(5) 0.000 0.001(4) 0.000 C2 0.087(6) 0.076(5) 0.088(6) 0.000 -0.012(4) 0.000 C3 0.133(9) 0.147(9) 0.131(9) 0.000 0.002(5) 0.000 C4 0.132(7) 0.133(7) 0.143(7) -0.003(5) 0.003(5) 0.011(5) C5 0.079(10) 0.098(12) 0.113(13) 0.000 0.045(9) 0.000 C6 0.040(6) 0.034(16) 0.036(5) -0.005(5) 0.001(4) -0.005(5) C7 0.099(8) 0.102(8) 0.097(8) 0.004(5) 0.001(5) -0.004(5) C8 0.097(8) 0.101(9) 0.097(8) -0.003(5) 0.004(5) 0.001(5) C9 0.106(9) 0.109(10) 0.106(9) -0.001(5) -0.002(5) 0.004(5) C10 0.088(7) 0.086(7) 0.082(7) 0.009(5) 0.014(5) 0.020(5) C11 0.044(5) 0.032(4) 0.038(5) 0.000 0.003(4) 0.000 C12 0.037(3) 0.031(3) 0.037(3) 0.007(3) -0.008(3) -0.002(3) C13 0.051(4) 0.038(3) 0.046(4) 0.004(3) -0.018(3) -0.005(3) C14 0.079(6) 0.055(5) 0.050(4) 0.005(4) -0.029(4) -0.009(4) C15 0.056(4) 0.061(5) 0.062(5) 0.023(4) -0.028(4) -0.007(4) C16 0.078(6) 0.039(4) 0.070(5) 0.020(4) -0.013(4) 0.011(4) C17 0.065(5) 0.037(4) 0.045(4) 0.009(3) -0.012(3) 0.009(3) C18 0.037(3) 0.030(3) 0.030(3) 0.003(2) -0.002(2) -0.004(2) C19 0.059(4) 0.049(4) 0.042(4) 0.016(3) -0.014(3) -0.023(3) C20 0.074(5) 0.079(6) 0.050(4) 0.022(4) -0.011(4) -0.044(5) C21 0.045(4) 0.086(6) 0.036(3) -0.006(4) -0.005(3) -0.032(4) C22 0.034(3) 0.065(5) 0.051(4) 0.001(4) -0.003(3) -0.006(3) C23 0.029(3) 0.040(3) 0.050(4) 0.005(3) -0.005(3) -0.004(3) C24 0.040(3) 0.021(3) 0.035(3) 0.004(2) -0.001(3) 0.000(2) C25 0.048(4) 0.027(3) 0.046(4) 0.002(3) 0.004(3) 0.002(3) C26 0.049(4) 0.044(4) 0.053(4) 0.006(3) 0.010(3) 0.012(3) C27 0.076(6) 0.060(5) 0.052(4) -0.014(4) 0.007(4) 0.014(4) C28 0.074(6) 0.067(5) 0.050(4) -0.022(4) -0.006(4) 0.003(4) C29 0.051(4) 0.045(4) 0.040(4) -0.009(3) -0.002(3) -0.004(3) B1 0.040(6) 0.045(6) 0.051(7) 0.000 -0.004(5) 0.000 _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 C11 1.859(9) . ? Ir1 P1 2.328(3) . ? Ir1 P2 2.3365(15) 8_565 ? Ir1 P2 2.3365(15) . ? P1 C1 1.607(14) . ? P1 C5 1.998(18) . ? P2 C18 1.822(6) . ? P2 C12 1.828(6) . ? P2 C24 1.832(6) . ? F1 B1 1.404(14) . ? F2 B1 1.385(8) . ? F3 B1 1.371(13) . ? O1 C11 1.153(11) . ? O2 C31 1.339(13) . ? O2 C32 1.430(16) . ? C1 C2 1.408(19) . ? C2 C4 1.508(16) 8_565 ? C2 C4 1.508(16) . ? C2 C3 1.52(2) . ? C5 C10 1.472(15) . ? C5 C10 1.472(15) 8_565 ? C5 C6 1.567(14) . ? C5 C6 1.567(14) 8_565 ? C6 C7 1.556(16) . ? C6 C7 1.732(19) 8_565 ? C7 C8 1.556(13) 8_565 ? C8 C9 1.533(17) . ? C8 C7 1.556(13) 8_565 ? C9 C10 1.472(17) . ? C9 C8 1.74(2) 8_565 ? C10 C9 1.93(3) 8_565 ? C12 C13 1.370(9) . ? C12 C17 1.397(9) . ? C13 C14 1.400(9) . ? C14 C15 1.365(11) . ? C15 C16 1.379(11) . ? C16 C17 1.385(9) . ? C18 C19 1.377(8) . ? C18 C23 1.393(8) . ? C19 C20 1.374(10) . ? C20 C21 1.384(12) . ? C21 C22 1.361(11) . ? C22 C23 1.404(9) . ? C24 C29 1.390(9) . ? C24 C25 1.397(9) . ? C25 C26 1.378(9) . ? C26 C27 1.377(11) . ? C27 C28 1.370(11) . ? C28 C29 1.384(10) . ? C30 C31 1.501(14) . ? C32 C33 1.456(19) . ? B1 F2 1.385(8) 8_565 ? 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 C11 Ir1 P1 179.7(3) . . ? C11 Ir1 P2 87.81(4) . 8_565 ? P1 Ir1 P2 92.20(4) . 8_565 ? C11 Ir1 P2 87.81(4) . . ? P1 Ir1 P2 92.20(4) . . ? P2 Ir1 P2 173.22(7) 8_565 . ? C1 P1 C5 104.8(7) . . ? C1 P1 Ir1 139.0(6) . . ? C5 P1 Ir1 116.2(4) . . ? C18 P2 C12 105.5(3) . . ? C18 P2 C24 102.7(3) . . ? C12 P2 C24 102.6(3) . . ? C18 P2 Ir1 110.7(2) . . ? C12 P2 Ir1 114.9(2) . . ? C24 P2 Ir1 118.93(19) . . ? C31 O2 C32 109.9(14) . . ? C2 C1 P1 131.4(13) . . ? C1 C2 C4 112.8(10) . 8_565 ? C1 C2 C4 112.8(10) . . ? C4 C2 C4 100.0(15) 8_565 . ? C1 C2 C3 112.8(15) . . ? C4 C2 C3 108.9(11) 8_565 . ? C4 C2 C3 108.9(11) . . ? C10 C5 C10 81.0(17) . 8_565 ? C10 C5 C6 102.2(13) . . ? C10 C5 C6 114.7(14) 8_565 . ? C10 C5 C6 114.7(14) . 8_565 ? C10 C5 C6 102.2(13) 8_565 8_565 ? C6 C5 C6 18.4(12) . 8_565 ? C10 C5 P1 125.1(10) . . ? C10 C5 P1 125.1(10) 8_565 . ? C6 C5 P1 105.8(9) . . ? C6 C5 P1 105.8(9) 8_565 . ? C7 C6 C5 107.7(12) . . ? C7 C6 C7 40.9(14) . 8_565 ? C5 C6 C7 99.5(12) . 8_565 ? C6 C7 C8 110.0(14) . 8_565 ? C9 C8 C7 112.7(17) . 8_565 ? C10 C9 C8 102.3(17) . . ? C10 C9 C8 111.6(16) . 8_565 ? C8 C9 C8 28.9(14) . 8_565 ? C9 C10 C5 109.6(17) . . ? C9 C10 C9 23.0(13) . 8_565 ? C5 C10 C9 89.0(14) . 8_565 ? O1 C11 Ir1 179.9(9) . . ? C13 C12 C17 119.0(6) . . ? C13 C12 P2 120.6(5) . . ? C17 C12 P2 120.3(5) . . ? C12 C13 C14 120.2(7) . . ? C15 C14 C13 120.3(7) . . ? C14 C15 C16 120.1(7) . . ? C15 C16 C17 119.8(7) . . ? C16 C17 C12 120.5(7) . . ? C19 C18 C23 118.9(6) . . ? C19 C18 P2 123.4(5) . . ? C23 C18 P2 117.7(4) . . ? C20 C19 C18 120.6(7) . . ? C19 C20 C21 120.9(7) . . ? C22 C21 C20 119.4(6) . . ? C21 C22 C23 120.4(7) . . ? C18 C23 C22 119.9(6) . . ? C29 C24 C25 118.0(6) . . ? C29 C24 P2 122.4(5) . . ? C25 C24 P2 119.6(5) . . ? C26 C25 C24 121.6(7) . . ? C27 C26 C25 119.4(7) . . ? C28 C27 C26 120.0(7) . . ? C27 C28 C29 121.1(8) . . ? C28 C29 C24 119.9(7) . . ? O2 C31 C30 112.7(13) . . ? O2 C32 C33 112(2) . . ? F3 B1 F2 109.8(6) . 8_565 ? F3 B1 F2 109.8(6) . . ? F2 B1 F2 110.4(9) 8_565 . ? F3 B1 F1 109.1(9) . . ? F2 B1 F1 108.8(6) 8_565 . ? F2 B1 F1 108.8(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.992 #(near Ir1) _refine_diff_density_min -2.100 #(near Ir1) _refine_diff_density_rms 0.139 data_compound_7 _database_code_CSD 208258 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H53 I Ir O P3' _chemical_formula_weight 1069.92 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.369(3) _cell_length_b 15.828(3) _cell_length_c 19.492(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4433.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 3.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.494 _exptl_absorpt_correction_T_max 0.564 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47718 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0440 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10064 _reflns_number_gt 9446 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0153P)^2^+7.5012P] 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 -0.008(4) _refine_ls_number_reflns 10064 _refine_ls_number_parameters 497 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.144717(10) 0.431069(10) 0.949904(8) 0.01407(4) Uani 1 1 d . . . I1 I -0.28261(2) 0.42682(2) 0.793370(16) 0.02922(8) Uani 1 1 d . . . P1 P -0.01309(7) 0.39832(7) 0.95487(6) 0.0176(2) Uani 1 1 d . . . P2 P 0.19660(7) 0.43729(8) 0.83350(5) 0.0156(2) Uani 1 1 d . . . P3 P 0.16600(7) 0.57567(8) 0.97566(5) 0.0150(2) Uani 1 1 d . . . O1 O 0.3365(2) 0.3708(2) 0.99118(18) 0.0365(9) Uani 1 1 d . . . C1 C 0.0729(3) 0.3557(3) 1.0072(2) 0.0212(9) Uani 1 1 d . . . C2 C 0.0802(3) 0.2894(3) 1.0634(2) 0.0259(11) Uani 1 1 d . . . C4 C 0.0754(4) 0.2024(3) 1.0297(3) 0.0403(14) Uani 1 1 d . . . H4A H 0.0175 0.1968 1.0055 0.060 Uiso 1 1 calc R . . H4B H 0.0796 0.1594 1.0643 0.060 Uiso 1 1 calc R . . H4C H 0.1261 0.1962 0.9980 0.060 Uiso 1 1 calc R . . C5 C -0.0018(5) 0.2991(4) 1.1135(3) 0.0512(17) Uani 1 1 d . . . H5A H -0.0593 0.2921 1.0891 0.077 Uiso 1 1 calc R . . H5B H -0.0001 0.3542 1.1340 0.077 Uiso 1 1 calc R . . H5C H 0.0027 0.2569 1.1487 0.077 Uiso 1 1 calc R . . C6 C -0.0700(3) 0.3231(3) 0.8979(2) 0.0255(10) Uani 1 1 d . . . H6A H -0.0241 0.2961 0.8696 0.038 Uiso 1 1 calc R . . H6B H -0.1139 0.3523 0.8694 0.038 Uiso 1 1 calc R . . H6C H -0.1018 0.2812 0.9248 0.038 Uiso 1 1 calc R . . C7 C -0.1047(3) 0.4653(3) 0.9927(2) 0.0230(10) Uani 1 1 d . . . H7 H -0.0805 0.4885 1.0358 0.028 Uiso 1 1 calc R . . C8 C -0.1273(3) 0.5392(3) 0.9457(3) 0.0268(10) Uani 1 1 d . . . H8A H -0.1496 0.5178 0.9020 0.032 Uiso 1 1 calc R . . H8B H -0.0710 0.5714 0.9371 0.032 Uiso 1 1 calc R . . C9 C -0.2009(4) 0.5973(3) 0.9769(3) 0.0403(14) Uani 1 1 d . . . H9A H -0.1759 0.6239 1.0177 0.048 Uiso 1 1 calc R . . H9B H -0.2164 0.6415 0.9443 0.048 Uiso 1 1 calc R . . C10 C -0.2886(3) 0.5480(3) 0.9953(3) 0.0399(14) Uani 1 1 d . . . H10A H -0.3329 0.5856 1.0172 0.048 Uiso 1 1 calc R . . H10B H -0.3170 0.5261 0.9539 0.048 Uiso 1 1 calc R . . C11 C -0.2659(3) 0.4754(4) 1.0434(3) 0.0406(13) Uani 1 1 d . . . H11A H -0.3223 0.4442 1.0539 0.049 Uiso 1 1 calc R . . H11B H -0.2409 0.4974 1.0861 0.049 Uiso 1 1 calc R . . C12 C -0.1943(3) 0.4160(4) 1.0097(3) 0.0328(12) Uani 1 1 d . . . H12A H -0.1799 0.3698 1.0406 0.039 Uiso 1 1 calc R . . H12B H -0.2202 0.3923 0.9680 0.039 Uiso 1 1 calc R . . C13 C 0.2652(3) 0.3961(3) 0.9763(2) 0.0233(10) Uani 1 1 d . . . C14 C 0.1203(3) 0.4758(3) 0.7646(2) 0.0165(9) Uani 1 1 d . . . C15 C 0.1580(3) 0.5060(3) 0.7031(2) 0.0222(10) Uani 1 1 d . . . H15 H 0.2221 0.5066 0.6971 0.027 Uiso 1 1 calc R . . C16 C 0.1002(4) 0.5349(3) 0.6512(2) 0.0303(12) Uani 1 1 d . . . H16 H 0.1254 0.5569 0.6110 0.036 Uiso 1 1 calc R . . C17 C 0.0048(4) 0.5309(3) 0.6596(3) 0.0339(12) Uani 1 1 d . . . H17 H -0.0340 0.5495 0.6246 0.041 Uiso 1 1 calc R . . C18 C -0.0339(3) 0.4997(3) 0.7191(2) 0.0263(11) Uani 1 1 d . . . H18 H -0.0982 0.4970 0.7241 0.032 Uiso 1 1 calc R . . C19 C 0.0243(3) 0.4725(3) 0.7714(2) 0.0212(10) Uani 1 1 d . . . H19 H -0.0015 0.4518 0.8118 0.025 Uiso 1 1 calc R . . C20 C 0.3062(3) 0.4939(3) 0.8207(2) 0.0220(10) Uani 1 1 d . . . C21 C 0.3072(3) 0.5789(3) 0.8009(2) 0.0252(10) Uani 1 1 d . . . H21 H 0.2521 0.6069 0.7903 0.030 Uiso 1 1 calc R . . C22 C 0.3929(4) 0.6208(4) 0.7976(3) 0.0406(15) Uani 1 1 d . . . H22 H 0.3940 0.6774 0.7847 0.049 Uiso 1 1 calc R . . C23 C 0.4732(4) 0.5824(5) 0.8124(3) 0.0481(18) Uani 1 1 d . . . H23 H 0.5290 0.6118 0.8092 0.058 Uiso 1 1 calc R . . C24 C 0.4729(4) 0.4971(5) 0.8327(3) 0.0440(16) Uani 1 1 d . . . H24 H 0.5284 0.4702 0.8438 0.053 Uiso 1 1 calc R . . C25 C 0.3897(3) 0.4538(4) 0.8362(2) 0.0312(13) Uani 1 1 d . . . H25 H 0.3895 0.3972 0.8490 0.037 Uiso 1 1 calc R . . C26 C 0.2259(3) 0.3307(3) 0.8033(2) 0.0191(9) Uani 1 1 d . . . C27 C 0.2827(4) 0.3196(3) 0.7457(2) 0.0295(11) Uani 1 1 d . . . H27 H 0.3052 0.3668 0.7227 0.035 Uiso 1 1 calc R . . C28 C 0.3063(4) 0.2399(3) 0.7223(3) 0.0340(13) Uani 1 1 d . . . H28 H 0.3479 0.2339 0.6861 0.041 Uiso 1 1 calc R . . C29 C 0.2676(4) 0.1692(4) 0.7529(3) 0.0401(14) Uani 1 1 d . . . H29 H 0.2795 0.1155 0.7357 0.048 Uiso 1 1 calc R . . C30 C 0.2108(4) 0.1800(3) 0.8099(3) 0.0416(14) Uani 1 1 d . . . H30 H 0.1859 0.1328 0.8316 0.050 Uiso 1 1 calc R . . C31 C 0.1908(3) 0.2591(3) 0.8347(3) 0.0295(11) Uani 1 1 d . . . H31 H 0.1532 0.2646 0.8733 0.035 Uiso 1 1 calc R . . C32 C 0.2781(3) 0.6041(3) 1.0138(2) 0.0193(9) Uani 1 1 d . . . C33 C 0.3600(3) 0.5781(3) 0.9817(2) 0.0236(9) Uani 1 1 d . . . H33 H 0.3569 0.5449 0.9424 0.028 Uiso 1 1 calc R . . C34 C 0.4466(3) 0.6014(3) 1.0080(2) 0.0272(11) Uani 1 1 d . . . H34 H 0.5010 0.5833 0.9867 0.033 Uiso 1 1 calc R . . C35 C 0.4514(3) 0.6520(3) 1.0667(3) 0.0300(12) Uani 1 1 d . . . H35 H 0.5088 0.6673 1.0848 0.036 Uiso 1 1 calc R . . C36 C 0.3701(4) 0.6789(3) 1.0974(2) 0.0295(11) Uani 1 1 d . . . H36 H 0.3729 0.7134 1.1360 0.035 Uiso 1 1 calc R . . C37 C 0.2845(3) 0.6549(3) 1.0712(2) 0.0225(10) Uani 1 1 d . . . H37 H 0.2304 0.6733 1.0927 0.027 Uiso 1 1 calc R . . C38 C 0.0844(3) 0.6046(3) 1.0434(2) 0.0168(9) Uani 1 1 d . . . C39 C 0.0346(3) 0.6796(3) 1.0420(3) 0.0247(10) Uani 1 1 d . . . H39 H 0.0412 0.7159 1.0049 0.030 Uiso 1 1 calc R . . C40 C -0.0250(3) 0.7013(3) 1.0953(2) 0.0307(12) Uani 1 1 d . . . H40 H -0.0586 0.7514 1.0933 0.037 Uiso 1 1 calc R . . C41 C -0.0344(3) 0.6485(4) 1.1511(3) 0.0326(12) Uani 1 1 d . . . H41 H -0.0744 0.6630 1.1868 0.039 Uiso 1 1 calc R . . C42 C 0.0156(3) 0.5742(4) 1.1541(2) 0.0299(11) Uani 1 1 d . . . H42 H 0.0094 0.5389 1.1919 0.036 Uiso 1 1 calc R . . C43 C 0.0749(3) 0.5518(3) 1.1011(2) 0.0222(10) Uani 1 1 d . . . H43 H 0.1086 0.5017 1.1036 0.027 Uiso 1 1 calc R . . C44 C 0.1495(3) 0.6565(3) 0.9102(2) 0.0177(8) Uani 1 1 d . . . C45 C 0.0807(3) 0.6446(3) 0.8606(2) 0.0196(9) Uani 1 1 d . . . H45 H 0.0432 0.5968 0.8627 0.024 Uiso 1 1 calc R . . C46 C 0.0671(3) 0.7034(3) 0.8078(2) 0.0246(10) Uani 1 1 d . . . H46 H 0.0195 0.6963 0.7760 0.030 Uiso 1 1 calc R . . C47 C 0.1263(3) 0.7724(3) 0.8039(2) 0.0272(11) Uani 1 1 d . . . H47 H 0.1208 0.8103 0.7677 0.033 Uiso 1 1 calc R . . C48 C 0.1936(3) 0.7852(3) 0.8536(2) 0.0278(11) Uani 1 1 d . . . H48 H 0.2316 0.8327 0.8515 0.033 Uiso 1 1 calc R . . C49 C 0.2045(3) 0.7277(2) 0.90616(18) 0.0215(10) Uani 1 1 d . . . H49 H 0.2497 0.7371 0.9394 0.026 Uiso 1 1 calc R . . C3 C 0.1722(3) 0.2996(2) 1.10312(18) 0.0485(17) Uani 1 1 d R . . H3A H 0.1735 0.2605 1.1408 0.073 Uiso 1 1 calc R . . H3B H 0.1768 0.3563 1.1204 0.073 Uiso 1 1 calc R . . H3C H 0.2236 0.2884 1.0730 0.073 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 0.01284(7) 0.01490(8) 0.01446(7) -0.00029(7) 0.00069(6) 0.00008(7) I1 0.02483(15) 0.02975(17) 0.03307(16) -0.00369(17) 0.00045(12) 0.00351(15) P1 0.0160(5) 0.0180(5) 0.0188(5) 0.0001(5) 0.0017(5) -0.0015(4) P2 0.0141(5) 0.0179(6) 0.0147(5) -0.0016(5) 0.0009(4) -0.0002(5) P3 0.0151(5) 0.0166(5) 0.0132(4) 0.0002(5) 0.0003(4) -0.0013(4) O1 0.0214(19) 0.054(2) 0.034(2) 0.0033(18) -0.0052(15) 0.0110(16) C1 0.028(2) 0.016(2) 0.020(2) -0.0006(18) 0.0018(19) -0.0044(18) C2 0.026(2) 0.021(2) 0.030(3) 0.005(2) -0.002(2) -0.0008(19) C4 0.048(3) 0.024(3) 0.049(3) 0.009(3) -0.002(3) 0.002(2) C5 0.065(4) 0.049(4) 0.039(3) 0.027(3) 0.022(3) 0.013(3) C6 0.020(2) 0.031(3) 0.026(2) -0.005(2) 0.000(2) -0.003(2) C7 0.017(2) 0.031(3) 0.021(2) -0.006(2) 0.0046(18) -0.0023(18) C8 0.020(2) 0.026(2) 0.035(3) 0.003(2) 0.006(2) 0.0040(17) C9 0.031(3) 0.034(3) 0.056(4) -0.010(3) 0.002(3) 0.012(2) C10 0.018(2) 0.041(4) 0.061(4) -0.018(3) 0.001(2) 0.010(2) C11 0.023(3) 0.049(3) 0.050(4) -0.007(3) 0.013(3) -0.005(2) C12 0.019(2) 0.040(3) 0.039(3) -0.003(2) 0.010(2) -0.003(2) C13 0.022(2) 0.031(3) 0.018(2) -0.0055(19) -0.0024(18) 0.0019(19) C14 0.020(2) 0.015(2) 0.014(2) -0.0031(17) -0.0004(16) -0.0020(16) C15 0.021(2) 0.025(2) 0.021(2) -0.0066(19) 0.0022(19) 0.0008(19) C16 0.037(3) 0.040(3) 0.014(2) 0.004(2) 0.000(2) 0.001(2) C17 0.032(3) 0.048(3) 0.022(2) 0.002(2) -0.010(2) 0.007(2) C18 0.018(2) 0.034(3) 0.027(3) 0.001(2) -0.0086(19) -0.002(2) C19 0.020(2) 0.020(2) 0.024(2) 0.0006(19) 0.0028(18) -0.0092(18) C20 0.017(2) 0.035(3) 0.014(2) -0.0096(19) 0.0019(17) -0.0051(19) C21 0.029(2) 0.029(3) 0.017(2) -0.007(2) 0.0038(18) -0.010(2) C22 0.053(4) 0.047(4) 0.022(3) -0.016(2) 0.017(2) -0.029(3) C23 0.021(3) 0.084(5) 0.040(3) -0.027(3) 0.015(2) -0.030(3) C24 0.019(3) 0.082(5) 0.031(3) -0.019(3) 0.010(2) -0.007(3) C25 0.022(2) 0.053(4) 0.019(2) -0.011(2) 0.0039(18) -0.002(2) C26 0.019(2) 0.020(2) 0.019(2) -0.0044(18) -0.0018(18) 0.0017(18) C27 0.037(3) 0.028(3) 0.023(3) -0.001(2) 0.005(2) 0.006(2) C28 0.047(3) 0.026(3) 0.029(3) -0.001(2) 0.012(2) 0.009(2) C29 0.053(4) 0.027(3) 0.040(3) -0.009(3) 0.008(3) 0.010(3) C30 0.056(4) 0.021(3) 0.047(4) -0.004(3) 0.015(3) -0.004(2) C31 0.031(3) 0.026(3) 0.031(3) -0.004(2) 0.011(2) -0.001(2) C32 0.016(2) 0.020(2) 0.021(2) 0.0006(18) -0.0063(18) -0.0045(17) C33 0.022(2) 0.031(3) 0.0179(19) -0.003(2) 0.0009(18) -0.005(2) C34 0.016(2) 0.040(3) 0.025(2) 0.001(2) 0.0005(19) -0.0042(19) C35 0.025(3) 0.036(3) 0.029(3) 0.005(2) -0.010(2) -0.012(2) C36 0.035(3) 0.031(3) 0.022(2) -0.006(2) -0.011(2) -0.007(2) C37 0.021(2) 0.023(2) 0.024(2) -0.0025(19) -0.0017(19) -0.0027(19) C38 0.016(2) 0.022(2) 0.013(2) -0.0028(18) 0.0007(17) -0.0053(16) C39 0.025(2) 0.026(3) 0.022(2) 0.000(2) 0.003(2) 0.0001(18) C40 0.030(3) 0.036(3) 0.026(3) 0.000(2) 0.008(2) 0.011(2) C41 0.028(3) 0.044(3) 0.026(3) -0.008(2) 0.010(2) -0.003(2) C42 0.040(3) 0.034(3) 0.016(2) -0.004(2) 0.0079(19) -0.009(3) C43 0.031(2) 0.014(2) 0.022(2) -0.0034(18) -0.0012(19) 0.0005(18) C44 0.021(2) 0.015(2) 0.017(2) 0.0017(16) 0.0049(19) -0.0003(19) C45 0.018(2) 0.019(2) 0.021(2) -0.0019(19) 0.0044(18) -0.0025(17) C46 0.029(3) 0.026(3) 0.019(2) 0.001(2) -0.005(2) 0.002(2) C47 0.040(3) 0.022(3) 0.019(2) 0.0054(19) 0.001(2) 0.004(2) C48 0.034(3) 0.022(3) 0.028(3) 0.001(2) 0.011(2) -0.005(2) C49 0.026(2) 0.018(2) 0.021(2) -0.0011(18) -0.0005(19) -0.0029(18) C3 0.053(4) 0.044(4) 0.048(4) 0.028(3) -0.020(3) -0.009(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 C13 1.888(5) . ? Ir1 C1 1.932(4) . ? Ir1 P1 2.3280(11) . ? Ir1 P3 2.3630(13) . ? Ir1 P2 2.3903(11) . ? P1 C1 1.738(5) . ? P1 C6 1.821(5) . ? P1 C7 1.845(5) . ? P2 C20 1.828(5) . ? P2 C26 1.836(4) . ? P2 C14 1.837(4) . ? P3 C44 1.822(4) . ? P3 C38 1.825(4) . ? P3 C32 1.830(4) . ? O1 C13 1.138(5) . ? C1 C2 1.521(6) . ? C2 C4 1.528(7) . ? C2 C5 1.538(7) . ? C2 C3 1.540(6) . ? C7 C8 1.522(7) . ? C7 C12 1.541(6) . ? C8 C9 1.527(6) . ? C9 C10 1.525(8) . ? C10 C11 1.519(8) . ? C11 C12 1.542(7) . ? C14 C19 1.387(6) . ? C14 C15 1.399(6) . ? C15 C16 1.387(7) . ? C16 C17 1.383(7) . ? C17 C18 1.376(7) . ? C18 C19 1.387(6) . ? C20 C25 1.391(7) . ? C20 C21 1.399(7) . ? C21 C22 1.402(6) . ? C22 C23 1.335(9) . ? C23 C24 1.406(10) . ? C24 C25 1.380(7) . ? C26 C31 1.384(7) . ? C26 C27 1.399(6) . ? C27 C28 1.384(7) . ? C28 C29 1.385(8) . ? C29 C30 1.389(8) . ? C30 C31 1.373(7) . ? C32 C37 1.382(6) . ? C32 C33 1.395(6) . ? C33 C34 1.396(6) . ? C34 C35 1.397(7) . ? C35 C36 1.380(7) . ? C36 C37 1.385(7) . ? C38 C39 1.386(6) . ? C38 C43 1.407(6) . ? C39 C40 1.390(6) . ? C40 C41 1.378(7) . ? C41 C42 1.379(8) . ? C42 C43 1.386(6) . ? C44 C49 1.379(5) . ? C44 C45 1.395(6) . ? C45 C46 1.402(6) . ? C46 C47 1.386(7) . ? C47 C48 1.383(7) . ? C48 C49 1.380(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C13 Ir1 C1 98.7(2) . . ? C13 Ir1 P1 144.71(15) . . ? C1 Ir1 P1 47.03(14) . . ? C13 Ir1 P3 96.16(15) . . ? C1 Ir1 P3 122.96(13) . . ? P1 Ir1 P3 109.44(4) . . ? C13 Ir1 P2 89.11(14) . . ? C1 Ir1 P2 137.78(13) . . ? P1 Ir1 P2 110.64(4) . . ? P3 Ir1 P2 96.97(4) . . ? C1 P1 C6 115.0(2) . . ? C1 P1 C7 119.7(2) . . ? C6 P1 C7 107.4(2) . . ? C1 P1 Ir1 54.43(15) . . ? C6 P1 Ir1 123.87(16) . . ? C7 P1 Ir1 125.74(15) . . ? C20 P2 C26 102.0(2) . . ? C20 P2 C14 104.6(2) . . ? C26 P2 C14 102.0(2) . . ? C20 P2 Ir1 114.75(14) . . ? C26 P2 Ir1 109.75(15) . . ? C14 P2 Ir1 121.43(14) . . ? C44 P3 C38 104.3(2) . . ? C44 P3 C32 103.1(2) . . ? C38 P3 C32 102.1(2) . . ? C44 P3 Ir1 120.94(14) . . ? C38 P3 Ir1 108.29(14) . . ? C32 P3 Ir1 115.99(15) . . ? C2 C1 P1 137.7(4) . . ? C2 C1 Ir1 143.7(4) . . ? P1 C1 Ir1 78.54(18) . . ? C1 C2 C4 108.0(4) . . ? C1 C2 C5 109.7(4) . . ? C4 C2 C5 109.1(5) . . ? C1 C2 C3 110.4(4) . . ? C4 C2 C3 110.4(4) . . ? C5 C2 C3 109.1(4) . . ? C8 C7 C12 109.9(4) . . ? C8 C7 P1 110.7(3) . . ? C12 C7 P1 113.0(3) . . ? C7 C8 C9 111.7(4) . . ? C10 C9 C8 111.0(4) . . ? C11 C10 C9 110.8(4) . . ? C10 C11 C12 110.0(5) . . ? C7 C12 C11 109.9(4) . . ? O1 C13 Ir1 176.4(4) . . ? C19 C14 C15 118.6(4) . . ? C19 C14 P2 120.7(3) . . ? C15 C14 P2 120.6(3) . . ? C16 C15 C14 120.5(4) . . ? C17 C16 C15 119.4(5) . . ? C18 C17 C16 121.2(5) . . ? C17 C18 C19 119.1(4) . . ? C14 C19 C18 121.2(4) . . ? C25 C20 C21 119.3(4) . . ? C25 C20 P2 119.3(4) . . ? C21 C20 P2 121.1(4) . . ? C20 C21 C22 118.5(5) . . ? C23 C22 C21 122.2(6) . . ? C22 C23 C24 119.7(5) . . ? C25 C24 C23 119.5(6) . . ? C24 C25 C20 120.7(6) . . ? C31 C26 C27 117.7(4) . . ? C31 C26 P2 121.8(3) . . ? C27 C26 P2 120.4(4) . . ? C28 C27 C26 121.5(5) . . ? C27 C28 C29 119.7(5) . . ? C28 C29 C30 118.8(5) . . ? C31 C30 C29 121.1(5) . . ? C30 C31 C26 121.0(5) . . ? C37 C32 C33 118.6(4) . . ? C37 C32 P3 122.0(4) . . ? C33 C32 P3 119.2(3) . . ? C32 C33 C34 120.6(4) . . ? C33 C34 C35 119.7(4) . . ? C36 C35 C34 119.4(4) . . ? C35 C36 C37 120.4(4) . . ? C32 C37 C36 121.1(5) . . ? C39 C38 C43 118.3(4) . . ? C39 C38 P3 122.2(3) . . ? C43 C38 P3 119.4(3) . . ? C38 C39 C40 121.0(5) . . ? C41 C40 C39 120.1(5) . . ? C40 C41 C42 119.9(4) . . ? C41 C42 C43 120.6(5) . . ? C42 C43 C38 120.1(4) . . ? C49 C44 C45 118.5(4) . . ? C49 C44 P3 122.7(3) . . ? C45 C44 P3 118.8(3) . . ? C44 C45 C46 121.2(4) . . ? C47 C46 C45 118.5(4) . . ? C48 C47 C46 120.4(4) . . ? C49 C48 C47 120.2(4) . . ? C44 C49 C48 121.1(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.856 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.106 data_compound_5a _database_code_CSD 208259 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H51 F3 Ir O4 P3 S' _chemical_formula_weight 1078.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.616(3) _cell_length_b 15.143(3) _cell_length_c 18.633(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.30(3) _cell_angle_gamma 90.00 _cell_volume 4650.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 3.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6885 _exptl_absorpt_correction_T_max 0.8415 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 1502) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59497 _diffrn_reflns_av_R_equivalents 0.1318 _diffrn_reflns_av_sigmaI/netI 0.0720 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 24.95 _reflns_number_total 8076 _reflns_number_gt 6447 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0000P)^2^+34.4522P] 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 SHELXL _refine_ls_extinction_coef 0.00099(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8076 _refine_ls_number_parameters 574 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1096 _refine_ls_wR_factor_gt 0.1018 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.735765(18) 0.583658(19) 0.227309(16) 0.02235(12) Uani 1 1 d . . . S1 S 0.82234(13) 0.24031(15) 0.39666(12) 0.0364(5) Uani 1 1 d . . . P1 P 0.79012(12) 0.44433(12) 0.21470(11) 0.0236(4) Uani 1 1 d . . . P2 P 0.60814(12) 0.58500(13) 0.27303(10) 0.0233(4) Uani 1 1 d . . . P3 P 0.81780(13) 0.63256(13) 0.33161(11) 0.0257(5) Uani 1 1 d . . . F1 F 0.9766(5) 0.2593(6) 0.3877(5) 0.098(2) Uani 1 1 d U . . F2 F 0.9365(5) 0.3203(6) 0.4811(5) 0.103(3) Uani 1 1 d U . . F3 F 0.9503(5) 0.1777(6) 0.4754(5) 0.111(3) Uani 1 1 d U . . O1 O 0.6901(4) 0.7598(4) 0.1550(4) 0.0538(19) Uani 1 1 d . . . O2 O 0.7778(5) 0.2307(5) 0.4562(4) 0.064(2) Uani 1 1 d . . . O3 O 0.8236(5) 0.1635(4) 0.3521(4) 0.059(2) Uani 1 1 d . . . O4 O 0.8093(5) 0.3214(4) 0.3575(4) 0.0573(19) Uani 1 1 d . . . C1 C 0.7848(5) 0.5276(5) 0.1503(4) 0.0240(17) Uani 1 1 d . A . C2 C 0.8130(5) 0.5437(5) 0.0774(4) 0.0280(18) Uani 1 1 d . . . C3 C 0.9006(8) 0.5055(8) 0.0823(7) 0.033(3) Uani 0.648(13) 1 d P A 1 H3A H 0.9215 0.5140 0.0360 0.050 Uiso 0.648(13) 1 calc PR A 1 H3B H 0.8995 0.4423 0.0935 0.050 Uiso 0.648(13) 1 calc PR A 1 H3C H 0.9358 0.5361 0.1206 0.050 Uiso 0.648(13) 1 calc PR A 1 C3A C 0.8821(19) 0.6068(19) 0.0875(17) 0.055(9) Uiso 0.352(13) 1 d P A 2 H3A1 H 0.9070 0.6106 0.0427 0.082 Uiso 0.352(13) 1 calc PR A 2 H3A2 H 0.9225 0.5861 0.1268 0.082 Uiso 0.352(13) 1 calc PR A 2 H3A3 H 0.8623 0.6652 0.0997 0.082 Uiso 0.352(13) 1 calc PR A 2 C4 C 0.7596(9) 0.4935(9) 0.0202(7) 0.039(4) Uani 0.648(13) 1 d P A 1 H4A H 0.7773 0.5048 -0.0272 0.058 Uiso 0.648(13) 1 calc PR A 1 H4B H 0.7033 0.5128 0.0196 0.058 Uiso 0.648(13) 1 calc PR A 1 H4C H 0.7635 0.4301 0.0308 0.058 Uiso 0.648(13) 1 calc PR A 1 C4A C 0.8337(17) 0.4586(18) 0.0396(15) 0.046(8) Uiso 0.352(13) 1 d P A 2 H4A1 H 0.8441 0.4721 -0.0099 0.070 Uiso 0.352(13) 1 calc PR A 2 H4A2 H 0.7882 0.4173 0.0380 0.070 Uiso 0.352(13) 1 calc PR A 2 H4A3 H 0.8823 0.4318 0.0663 0.070 Uiso 0.352(13) 1 calc PR A 2 C5 C 0.8177(9) 0.6404(9) 0.0602(8) 0.041(4) Uani 0.648(13) 1 d P A 1 H5A H 0.8524 0.6704 0.0993 0.061 Uiso 0.648(13) 1 calc PR A 1 H5B H 0.7632 0.6661 0.0555 0.061 Uiso 0.648(13) 1 calc PR A 1 H5C H 0.8407 0.6479 0.0147 0.061 Uiso 0.648(13) 1 calc PR A 1 C5A C 0.7411(16) 0.589(2) 0.0257(15) 0.049(7) Uiso 0.352(13) 1 d P A 2 H5A1 H 0.7288 0.6467 0.0453 0.073 Uiso 0.352(13) 1 calc PR A 2 H5A2 H 0.6928 0.5513 0.0225 0.073 Uiso 0.352(13) 1 calc PR A 2 H5A3 H 0.7574 0.5965 -0.0227 0.073 Uiso 0.352(13) 1 calc PR A 2 C6 C 0.7411(5) 0.3383(5) 0.1914(4) 0.0272(18) Uani 1 1 d . . . H6 H 0.7298 0.3112 0.2380 0.033 Uiso 1 1 calc R . . C7 C 0.6604(5) 0.3460(5) 0.1447(4) 0.0302(18) Uani 1 1 d . . . H7A H 0.6682 0.3734 0.0979 0.036 Uiso 1 1 calc R . . H7B H 0.6239 0.3845 0.1689 0.036 Uiso 1 1 calc R . . C8 C 0.6216(5) 0.2551(6) 0.1314(5) 0.037(2) Uani 1 1 d . . . H8A H 0.6075 0.2310 0.1776 0.044 Uiso 1 1 calc R . . H8B H 0.5708 0.2609 0.0977 0.044 Uiso 1 1 calc R . . C9 C 0.6774(5) 0.1920(5) 0.1000(5) 0.035(2) Uani 1 1 d . . . H9A H 0.6852 0.2120 0.0508 0.042 Uiso 1 1 calc R . . H9B H 0.6518 0.1329 0.0957 0.042 Uiso 1 1 calc R . . C10 C 0.7597(5) 0.1845(5) 0.1454(5) 0.038(2) Uani 1 1 d . . . H10A H 0.7956 0.1465 0.1201 0.045 Uiso 1 1 calc R . . H10B H 0.7532 0.1562 0.1922 0.045 Uiso 1 1 calc R . . C11 C 0.7992(5) 0.2752(5) 0.1594(5) 0.033(2) Uani 1 1 d . . . H11A H 0.8134 0.2998 0.1134 0.039 Uiso 1 1 calc R . . H11B H 0.8498 0.2691 0.1933 0.039 Uiso 1 1 calc R . . C12 C 0.7091(5) 0.6935(6) 0.1846(5) 0.036(2) Uani 1 1 d . . . C13 C 0.5888(5) 0.6867(5) 0.3197(4) 0.0268(18) Uani 1 1 d . . . C14 C 0.6107(5) 0.6960(5) 0.3942(5) 0.0317(19) Uani 1 1 d . . . H14 H 0.6293 0.6460 0.4224 0.038 Uiso 1 1 calc R . . C15 C 0.6057(5) 0.7778(6) 0.4277(5) 0.037(2) Uani 1 1 d . . . H15 H 0.6204 0.7829 0.4785 0.045 Uiso 1 1 calc R . . C16 C 0.5798(5) 0.8508(5) 0.3881(5) 0.039(2) Uani 1 1 d . . . H16 H 0.5773 0.9067 0.4108 0.047 Uiso 1 1 calc R . . C17 C 0.5570(5) 0.8420(6) 0.3137(5) 0.040(2) Uani 1 1 d . . . H17 H 0.5395 0.8926 0.2858 0.048 Uiso 1 1 calc R . . C18 C 0.5596(5) 0.7630(5) 0.2808(5) 0.0304(19) Uani 1 1 d . . . H18 H 0.5414 0.7584 0.2306 0.036 Uiso 1 1 calc R . . C19 C 0.5248(5) 0.5859(5) 0.1971(4) 0.0274(17) Uani 1 1 d . . . C20 C 0.4443(5) 0.5954(5) 0.2120(4) 0.0267(18) Uani 1 1 d . . . H20 H 0.4333 0.5954 0.2608 0.032 Uiso 1 1 calc R . . C21 C 0.3813(5) 0.6047(5) 0.1569(5) 0.039(2) Uani 1 1 d . . . H21 H 0.3270 0.6100 0.1674 0.046 Uiso 1 1 calc R . . C22 C 0.3982(6) 0.6064(5) 0.0845(5) 0.039(2) Uani 1 1 d . . . H22 H 0.3556 0.6157 0.0462 0.047 Uiso 1 1 calc R . . C23 C 0.4756(6) 0.5946(6) 0.0697(5) 0.038(2) Uani 1 1 d . . . H23 H 0.4863 0.5933 0.0208 0.046 Uiso 1 1 calc R . . C24 C 0.5397(5) 0.5844(6) 0.1258(4) 0.0330(18) Uani 1 1 d . . . H24 H 0.5935 0.5764 0.1148 0.040 Uiso 1 1 calc R . . C25 C 0.5776(5) 0.4975(5) 0.3316(4) 0.0254(18) Uani 1 1 d . . . C26 C 0.6154(5) 0.4152(5) 0.3319(4) 0.0293(17) Uani 1 1 d . . . H26 H 0.6584 0.4060 0.3037 0.035 Uiso 1 1 calc R . . C27 C 0.5904(6) 0.3473(6) 0.3731(5) 0.039(2) Uani 1 1 d . . . H27 H 0.6162 0.2914 0.3724 0.047 Uiso 1 1 calc R . . C28 C 0.5291(6) 0.3588(6) 0.4150(5) 0.040(2) Uani 1 1 d . . . H28 H 0.5134 0.3117 0.4439 0.048 Uiso 1 1 calc R . . C29 C 0.4901(6) 0.4403(6) 0.4147(5) 0.043(2) Uani 1 1 d . . . H29 H 0.4461 0.4483 0.4420 0.052 Uiso 1 1 calc R . . C30 C 0.5153(5) 0.5092(6) 0.3750(4) 0.034(2) Uani 1 1 d . . . H30 H 0.4902 0.5654 0.3769 0.040 Uiso 1 1 calc R . . C31 C 0.8344(5) 0.7518(5) 0.3402(5) 0.033(2) Uani 1 1 d . . . C32 C 0.9111(6) 0.7838(6) 0.3680(5) 0.044(2) Uani 1 1 d . . . H32 H 0.9550 0.7445 0.3813 0.053 Uiso 1 1 calc R . . C33 C 0.9218(8) 0.8762(7) 0.3759(6) 0.059(3) Uani 1 1 d . . . H33 H 0.9732 0.8991 0.3955 0.071 Uiso 1 1 calc R . . C34 C 0.8587(7) 0.9331(6) 0.3556(5) 0.053(3) Uani 1 1 d . . . H34 H 0.8669 0.9950 0.3600 0.064 Uiso 1 1 calc R . . C35 C 0.7839(7) 0.9009(5) 0.3290(5) 0.050(3) Uani 1 1 d . . . H35 H 0.7399 0.9401 0.3153 0.060 Uiso 1 1 calc R . . C36 C 0.7730(6) 0.8102(6) 0.3222(5) 0.044(2) Uani 1 1 d . . . H36 H 0.7208 0.7882 0.3043 0.053 Uiso 1 1 calc R . . C37 C 0.7961(5) 0.5971(5) 0.4209(4) 0.0266(17) Uani 1 1 d . . . C38 C 0.8046(5) 0.6530(6) 0.4811(5) 0.039(2) Uani 1 1 d . . . H38 H 0.8239 0.7116 0.4768 0.047 Uiso 1 1 calc R . . C39 C 0.7851(6) 0.6232(7) 0.5463(5) 0.043(2) Uani 1 1 d . . . H39 H 0.7914 0.6611 0.5872 0.052 Uiso 1 1 calc R . . C40 C 0.7564(6) 0.5379(6) 0.5527(5) 0.040(2) Uani 1 1 d . . . H40 H 0.7415 0.5180 0.5975 0.048 Uiso 1 1 calc R . . C41 C 0.7496(5) 0.4819(6) 0.4934(5) 0.040(2) Uani 1 1 d . . . H41 H 0.7314 0.4230 0.4980 0.048 Uiso 1 1 calc R . . C42 C 0.7692(5) 0.5114(5) 0.4277(5) 0.033(2) Uani 1 1 d . . . H42 H 0.7642 0.4729 0.3871 0.040 Uiso 1 1 calc R . . C43 C 0.9189(5) 0.5883(6) 0.3252(4) 0.0323(19) Uani 1 1 d . . . C44 C 0.9531(6) 0.5215(6) 0.3722(5) 0.042(2) Uani 1 1 d . . . H44 H 0.9251 0.4999 0.4101 0.051 Uiso 1 1 calc R . . C45 C 1.0275(6) 0.4884(7) 0.3620(6) 0.053(3) Uani 1 1 d . . . H45 H 1.0503 0.4425 0.3929 0.064 Uiso 1 1 calc R . . C46 C 1.0706(6) 0.5191(7) 0.3088(6) 0.049(3) Uani 1 1 d . . . H46 H 1.1220 0.4944 0.3032 0.059 Uiso 1 1 calc R . . C47 C 1.0388(5) 0.5858(7) 0.2636(5) 0.046(2) Uani 1 1 d . . . H47 H 1.0685 0.6084 0.2273 0.055 Uiso 1 1 calc R . . C48 C 0.9623(5) 0.6198(6) 0.2716(5) 0.038(2) Uani 1 1 d . . . H48 H 0.9397 0.6651 0.2400 0.046 Uiso 1 1 calc R . . C49 C 0.9273(8) 0.2512(8) 0.4386(7) 0.073(4) Uani 1 1 d . . . H1 H 0.864(4) 0.424(5) 0.243(4) 0.021(18) 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 0.02739(18) 0.01628(16) 0.02427(17) 0.00142(14) 0.00672(11) 0.00167(14) S1 0.0387(12) 0.0351(12) 0.0352(12) -0.0013(10) 0.0034(10) 0.0050(10) P1 0.0281(11) 0.0178(10) 0.0245(11) -0.0014(8) 0.0018(9) 0.0039(8) P2 0.0294(10) 0.0163(9) 0.0250(10) 0.0018(9) 0.0071(8) 0.0018(9) P3 0.0319(11) 0.0199(10) 0.0268(11) -0.0035(8) 0.0091(9) -0.0038(9) F1 0.075(4) 0.100(4) 0.122(4) 0.011(4) 0.023(4) -0.011(3) F2 0.101(4) 0.099(4) 0.098(4) -0.009(4) -0.022(4) -0.017(4) F3 0.097(4) 0.104(4) 0.123(5) 0.034(4) -0.022(4) 0.008(4) O1 0.075(5) 0.030(3) 0.065(5) 0.027(3) 0.039(4) 0.025(3) O2 0.074(5) 0.067(5) 0.054(5) -0.005(4) 0.026(4) -0.006(4) O3 0.071(5) 0.037(4) 0.073(5) -0.017(3) 0.023(4) -0.005(3) O4 0.079(5) 0.043(4) 0.046(4) 0.011(3) -0.008(4) 0.014(4) C1 0.025(4) 0.017(4) 0.029(4) 0.002(3) 0.004(3) -0.002(3) C2 0.035(5) 0.023(4) 0.028(4) -0.006(3) 0.010(4) 0.001(4) C3 0.032(7) 0.030(7) 0.041(8) 0.009(6) 0.013(6) 0.006(6) C4 0.048(9) 0.041(8) 0.029(8) 0.004(6) 0.011(7) -0.002(7) C5 0.051(10) 0.035(8) 0.040(8) 0.004(6) 0.024(7) 0.000(7) C6 0.040(5) 0.021(4) 0.022(4) 0.003(3) 0.009(4) 0.006(4) C7 0.037(5) 0.021(4) 0.033(5) -0.003(3) 0.006(4) 0.003(4) C8 0.034(5) 0.035(5) 0.043(5) -0.012(4) 0.011(4) -0.009(4) C9 0.046(5) 0.022(4) 0.039(5) -0.010(4) 0.010(4) -0.008(4) C10 0.052(6) 0.020(4) 0.044(5) -0.008(4) 0.014(4) 0.005(4) C11 0.032(5) 0.025(4) 0.040(5) -0.005(4) 0.004(4) 0.008(4) C12 0.038(5) 0.043(6) 0.029(5) -0.006(4) 0.013(4) 0.004(4) C13 0.023(4) 0.023(4) 0.035(5) 0.001(3) 0.007(4) 0.003(3) C14 0.032(5) 0.027(4) 0.038(5) -0.006(4) 0.013(4) 0.006(4) C15 0.035(5) 0.040(5) 0.039(5) -0.012(4) 0.009(4) -0.002(4) C16 0.040(5) 0.020(4) 0.059(6) -0.020(4) 0.008(5) 0.000(4) C17 0.040(5) 0.024(5) 0.058(6) 0.005(4) 0.013(5) 0.008(4) C18 0.030(4) 0.017(4) 0.044(5) 0.006(4) 0.003(4) -0.002(3) C19 0.036(4) 0.013(3) 0.033(4) 0.004(3) 0.000(3) 0.002(4) C20 0.029(4) 0.014(4) 0.039(5) 0.001(3) 0.011(4) 0.002(3) C21 0.031(5) 0.022(5) 0.062(6) 0.006(4) 0.002(4) 0.005(3) C22 0.043(5) 0.028(5) 0.042(5) -0.002(4) -0.014(4) 0.004(4) C23 0.052(6) 0.028(5) 0.033(5) -0.002(4) 0.001(4) 0.002(4) C24 0.039(5) 0.025(4) 0.036(5) -0.001(4) 0.013(4) -0.001(4) C25 0.029(4) 0.025(4) 0.023(4) -0.004(3) 0.005(4) -0.001(3) C26 0.040(5) 0.021(4) 0.027(4) -0.003(4) 0.005(3) -0.001(4) C27 0.054(6) 0.020(4) 0.044(6) 0.008(4) 0.005(5) -0.002(4) C28 0.049(6) 0.032(5) 0.040(5) 0.013(4) 0.013(5) -0.005(4) C29 0.046(6) 0.041(6) 0.045(6) 0.004(4) 0.019(5) -0.007(4) C30 0.038(5) 0.029(4) 0.034(5) 0.000(4) 0.007(4) -0.004(4) C31 0.045(5) 0.022(4) 0.037(5) -0.005(4) 0.023(4) -0.009(4) C32 0.051(6) 0.041(5) 0.039(5) -0.008(4) 0.005(5) -0.013(5) C33 0.087(9) 0.038(6) 0.051(7) -0.017(5) 0.008(6) -0.042(6) C34 0.089(8) 0.030(6) 0.047(6) -0.013(4) 0.033(6) -0.032(6) C35 0.081(8) 0.016(5) 0.062(6) -0.005(4) 0.037(6) -0.004(5) C36 0.050(6) 0.028(5) 0.061(6) -0.006(4) 0.028(5) -0.004(4) C37 0.026(4) 0.028(5) 0.027(4) -0.002(3) 0.005(3) 0.003(3) C38 0.041(5) 0.039(5) 0.039(5) -0.004(4) 0.010(4) 0.004(4) C39 0.048(6) 0.054(6) 0.030(5) -0.001(4) 0.013(4) 0.014(5) C40 0.048(6) 0.046(6) 0.029(5) 0.009(4) 0.012(4) 0.002(5) C41 0.041(5) 0.039(5) 0.041(6) 0.010(4) 0.007(4) 0.000(4) C42 0.036(5) 0.030(5) 0.033(5) -0.003(4) 0.003(4) -0.004(4) C43 0.030(4) 0.037(5) 0.029(4) -0.017(4) 0.001(4) -0.005(4) C44 0.040(5) 0.052(6) 0.037(5) -0.003(4) 0.012(4) 0.002(5) C45 0.041(6) 0.052(6) 0.065(7) 0.001(5) 0.002(5) 0.010(5) C46 0.036(5) 0.060(7) 0.054(6) -0.008(5) 0.010(5) 0.013(5) C47 0.037(5) 0.064(6) 0.039(5) -0.013(5) 0.015(4) -0.004(5) C48 0.039(5) 0.041(5) 0.034(5) -0.007(4) 0.005(4) -0.004(4) C49 0.090(9) 0.044(7) 0.077(9) 0.019(6) -0.019(7) 0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C12 1.873(9) . ? Ir1 C1 1.934(8) . ? Ir1 P1 2.3186(19) . ? Ir1 P3 2.347(2) . ? Ir1 P2 2.384(2) . ? S1 O2 1.417(7) . ? S1 O4 1.430(7) . ? S1 O3 1.431(7) . ? S1 C49 1.826(13) . ? P1 C1 1.735(8) . ? P1 C6 1.828(8) . ? P2 C13 1.818(8) . ? P2 C25 1.829(8) . ? P2 C19 1.851(8) . ? P3 C43 1.826(8) . ? P3 C37 1.828(8) . ? P3 C31 1.830(8) . ? F1 C49 1.335(15) . ? F2 C49 1.310(14) . ? F3 C49 1.338(13) . ? O1 C12 1.169(10) . ? C1 C2 1.512(11) . ? C2 C3A 1.49(3) . ? C2 C5 1.504(15) . ? C2 C4 1.505(16) . ? C2 C4A 1.53(3) . ? C2 C3 1.558(14) . ? C2 C5A 1.59(3) . ? C6 C7 1.507(11) . ? C6 C11 1.531(10) . ? C7 C8 1.527(11) . ? C8 C9 1.500(11) . ? C9 C10 1.518(12) . ? C10 C11 1.530(11) . ? C13 C14 1.397(11) . ? C13 C18 1.416(11) . ? C14 C15 1.394(11) . ? C15 C16 1.369(13) . ? C16 C17 1.395(13) . ? C17 C18 1.347(12) . ? C19 C24 1.381(11) . ? C19 C20 1.407(11) . ? C20 C21 1.378(12) . ? C21 C22 1.412(13) . ? C22 C23 1.360(13) . ? C23 C24 1.404(12) . ? C25 C26 1.395(11) . ? C25 C30 1.404(11) . ? C26 C27 1.379(11) . ? C27 C28 1.372(13) . ? C28 C29 1.395(12) . ? C29 C30 1.374(12) . ? C31 C36 1.359(13) . ? C31 C32 1.400(12) . ? C32 C33 1.416(13) . ? C33 C34 1.373(16) . ? C34 C35 1.368(15) . ? C35 C36 1.389(12) . ? C37 C42 1.383(11) . ? C37 C38 1.397(11) . ? C38 C39 1.372(12) . ? C39 C40 1.387(13) . ? C40 C41 1.385(13) . ? C41 C42 1.381(12) . ? C43 C48 1.389(12) . ? C43 C44 1.410(13) . ? C44 C45 1.371(13) . ? C45 C46 1.374(14) . ? C46 C47 1.377(14) . ? C47 C48 1.397(12) . ? 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 C12 Ir1 C1 100.0(3) . . ? C12 Ir1 P1 147.1(2) . . ? C1 Ir1 P1 47.1(2) . . ? C12 Ir1 P3 98.8(3) . . ? C1 Ir1 P3 119.8(2) . . ? P1 Ir1 P3 100.27(7) . . ? C12 Ir1 P2 88.4(3) . . ? C1 Ir1 P2 138.3(2) . . ? P1 Ir1 P2 114.81(7) . . ? P3 Ir1 P2 98.67(7) . . ? O2 S1 O4 115.3(5) . . ? O2 S1 O3 114.8(4) . . ? O4 S1 O3 114.5(4) . . ? O2 S1 C49 103.9(6) . . ? O4 S1 C49 102.4(5) . . ? O3 S1 C49 103.7(5) . . ? C1 P1 C6 119.5(4) . . ? C1 P1 Ir1 54.7(3) . . ? C6 P1 Ir1 131.0(3) . . ? C13 P2 C25 104.4(4) . . ? C13 P2 C19 101.5(4) . . ? C25 P2 C19 103.0(4) . . ? C13 P2 Ir1 113.4(3) . . ? C25 P2 Ir1 122.3(3) . . ? C19 P2 Ir1 109.9(3) . . ? C43 P3 C37 104.0(4) . . ? C43 P3 C31 103.8(4) . . ? C37 P3 C31 104.8(4) . . ? C43 P3 Ir1 105.8(2) . . ? C37 P3 Ir1 120.0(3) . . ? C31 P3 Ir1 116.7(3) . . ? C2 C1 P1 138.1(6) . . ? C2 C1 Ir1 143.5(5) . . ? P1 C1 Ir1 78.2(3) . . ? C3A C2 C5 48.8(13) . . ? C3A C2 C4 142.3(14) . . ? C5 C2 C4 112.5(10) . . ? C3A C2 C1 108.2(13) . . ? C5 C2 C1 112.3(7) . . ? C4 C2 C1 109.5(8) . . ? C3A C2 C4A 112.6(17) . . ? C5 C2 C4A 134.6(13) . . ? C4 C2 C4A 52.7(12) . . ? C1 C2 C4A 113.1(12) . . ? C3A C2 C3 62.1(13) . . ? C5 C2 C3 107.5(9) . . ? C4 C2 C3 108.4(9) . . ? C1 C2 C3 106.4(8) . . ? C4A C2 C3 56.7(12) . . ? C3A C2 C5A 108.0(17) . . ? C5 C2 C5A 60.5(12) . . ? C4 C2 C5A 57.2(12) . . ? C1 C2 C5A 108.6(11) . . ? C4A C2 C5A 106.2(16) . . ? C3 C2 C5A 145.0(12) . . ? C7 C6 C11 112.4(7) . . ? C7 C6 P1 113.9(5) . . ? C11 C6 P1 110.9(6) . . ? C6 C7 C8 110.5(7) . . ? C9 C8 C7 111.6(7) . . ? C8 C9 C10 112.9(7) . . ? C9 C10 C11 111.3(7) . . ? C10 C11 C6 110.4(7) . . ? O1 C12 Ir1 176.5(8) . . ? C14 C13 C18 117.1(7) . . ? C14 C13 P2 121.4(6) . . ? C18 C13 P2 121.1(6) . . ? C15 C14 C13 120.8(8) . . ? C16 C15 C14 120.5(8) . . ? C15 C16 C17 119.1(8) . . ? C18 C17 C16 121.0(8) . . ? C17 C18 C13 121.4(8) . . ? C24 C19 C20 118.9(7) . . ? C24 C19 P2 121.8(6) . . ? C20 C19 P2 119.2(6) . . ? C21 C20 C19 121.0(8) . . ? C20 C21 C22 119.2(8) . . ? C23 C22 C21 120.0(8) . . ? C22 C23 C24 120.7(8) . . ? C19 C24 C23 120.1(8) . . ? C26 C25 C30 118.4(7) . . ? C26 C25 P2 119.4(6) . . ? C30 C25 P2 122.2(6) . . ? C27 C26 C25 120.1(8) . . ? C28 C27 C26 121.4(8) . . ? C27 C28 C29 119.3(8) . . ? C30 C29 C28 120.1(8) . . ? C29 C30 C25 120.8(8) . . ? C36 C31 C32 119.0(8) . . ? C36 C31 P3 121.4(7) . . ? C32 C31 P3 119.6(7) . . ? C31 C32 C33 118.5(10) . . ? C34 C33 C32 120.6(10) . . ? C35 C34 C33 120.3(9) . . ? C34 C35 C36 119.1(10) . . ? C31 C36 C35 122.5(10) . . ? C42 C37 C38 119.7(8) . . ? C42 C37 P3 117.5(6) . . ? C38 C37 P3 122.7(6) . . ? C39 C38 C37 120.0(9) . . ? C38 C39 C40 120.3(9) . . ? C41 C40 C39 119.7(8) . . ? C42 C41 C40 120.3(8) . . ? C41 C42 C37 120.0(8) . . ? C48 C43 C44 119.2(8) . . ? C48 C43 P3 119.1(7) . . ? C44 C43 P3 121.6(6) . . ? C45 C44 C43 118.4(9) . . ? C44 C45 C46 122.6(10) . . ? C45 C46 C47 119.6(9) . . ? C46 C47 C48 119.3(9) . . ? C43 C48 C47 120.8(9) . . ? F2 C49 F1 108.8(11) . . ? F2 C49 F3 110.5(11) . . ? F1 C49 F3 106.3(11) . . ? F2 C49 S1 111.2(10) . . ? F1 C49 S1 110.1(9) . . ? F3 C49 S1 109.8(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.820 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.141