# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Adams, Jeramie' 'Arulsamy, Navamoney' 'Roddick, Dean' _publ_contact_author_name 'Dr Dean Roddick' _publ_contact_author_email dmr@uwyo.edu _publ_section_title ; Acceptor CF3PCPH Pincer Reactivity with (PPh3)3Ir(CO)H ; _publ_contact_author_address ; Chemistry, Dept. 3838 University of Wyoming 1000 E University Ave. Laramie, WY 82071 ; _publ_requested_journal ; Dalton Trans. ; # Attachment '- CIF files.txt' data_jja37 _database_code_depnum_ccdc_archive 'CCDC 826940' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(?-CF3PCPH)Ir(H)(CO)(PPh3)]2' _chemical_melting_point ? _chemical_formula_moiety 'C62 H48 F24 Ir2 O2 P6' _chemical_formula_sum 'C62 H48 F24 Ir2 O2 P6' _chemical_formula_weight 1851.22 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.9880(6) _cell_length_b 20.5558(7) _cell_length_c 20.3552(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.474(2) _cell_angle_gamma 90.00 _cell_volume 6669.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9910 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 33.79 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 4.241 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2746 _exptl_absorpt_correction_T_max 0.5502 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108305 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 33.14 _reflns_number_total 25166 _reflns_number_gt 18171 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _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^)+(0.0526P)^2^+37.9072P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25166 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0553 _refine_ls_wR_factor_ref 0.1390 _refine_ls_wR_factor_gt 0.1263 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.245776(11) 0.527182(10) 0.207463(9) 0.01809(5) Uani 1 1 d . . . P1 P 0.29135(8) 0.60932(7) 0.14762(7) 0.0197(2) Uani 1 1 d . . . P2 P 0.13605(8) 0.46709(7) 0.16840(7) 0.0219(3) Uani 1 1 d . . . P3 P 0.26485(8) 0.53053(7) 0.32142(6) 0.0194(2) Uani 1 1 d . . . C25 C 0.3350(3) 0.4672(3) 0.1932(3) 0.0270(11) Uani 1 1 d . . . O1 O 0.3872(3) 0.4307(2) 0.1859(3) 0.0386(11) Uani 1 1 d . . . Ir2 Ir -0.239959(11) 0.645751(10) 0.216035(10) 0.01931(5) Uani 1 1 d . . . P4 P -0.29931(8) 0.56946(7) 0.14899(7) 0.0218(3) Uani 1 1 d . . . P5 P -0.13531(8) 0.70540(7) 0.18169(7) 0.0232(3) Uani 1 1 d . . . P6 P -0.23543(8) 0.63624(7) 0.33003(7) 0.0202(2) Uani 1 1 d . . . C26 C -0.3285(4) 0.7090(3) 0.2054(3) 0.0298(12) Uani 1 1 d . . . O2 O -0.3801(3) 0.7469(3) 0.1998(3) 0.0471(13) Uani 1 1 d . . . C1 C 0.0949(3) 0.6869(3) 0.1658(3) 0.0243(10) Uani 1 1 d . . . H1A H 0.0770 0.6438 0.1551 0.029 Uiso 1 1 calc R . . C2 C 0.1693(3) 0.7099(3) 0.1431(3) 0.0248(11) Uani 1 1 d . . . C3 C 0.1944(4) 0.7739(3) 0.1584(4) 0.0345(14) Uani 1 1 d . . . H3A H 0.2445 0.7907 0.1426 0.041 Uiso 1 1 calc R . . C4 C 0.1463(4) 0.8127(3) 0.1962(4) 0.0376(15) Uani 1 1 d . . . H4A H 0.1633 0.8561 0.2060 0.045 Uiso 1 1 calc R . . C5 C 0.0735(4) 0.7887(3) 0.2201(3) 0.0328(13) Uani 1 1 d . . . H5A H 0.0420 0.8150 0.2476 0.039 Uiso 1 1 calc R . . C6 C 0.0467(3) 0.7256(3) 0.2035(3) 0.0256(11) Uani 1 1 d . . . C7 C -0.0328(3) 0.6990(3) 0.2291(3) 0.0257(11) Uani 1 1 d . . . H7A H -0.0389 0.7202 0.2722 0.031 Uiso 1 1 calc R . . H7B H -0.0230 0.6522 0.2382 0.031 Uiso 1 1 calc R . . C8 C -0.1538(4) 0.7958(4) 0.1743(4) 0.0404(16) Uani 1 1 d . . . F8A F -0.1716(5) 0.8203(2) 0.2307(3) 0.0782(18) Uani 1 1 d . . . F8B F -0.2208(3) 0.8058(2) 0.1316(3) 0.0653(15) Uani 1 1 d . . . F8C F -0.0928(3) 0.8305(2) 0.1508(3) 0.0667(16) Uani 1 1 d . . . C9 C -0.1062(4) 0.6919(3) 0.0940(3) 0.0321(13) Uani 1 1 d . . . F9A F -0.0718(3) 0.6327(2) 0.08974(19) 0.0412(9) Uani 1 1 d . . . F9B F -0.1746(2) 0.6935(2) 0.05163(19) 0.0450(10) Uani 1 1 d . . . F9C F -0.0517(2) 0.7343(2) 0.0713(2) 0.0448(10) Uani 1 1 d . . . C10 C 0.2208(3) 0.6679(3) 0.1015(3) 0.0246(11) Uani 1 1 d . . . H10A H 0.2553 0.6965 0.0752 0.030 Uiso 1 1 calc R . . H10B H 0.1823 0.6432 0.0702 0.030 Uiso 1 1 calc R . . C11 C 0.3718(3) 0.6680(3) 0.1871(3) 0.0278(11) Uani 1 1 d . . . F11A F 0.4427(2) 0.63764(19) 0.2074(2) 0.0368(9) Uani 1 1 d . . . F11B F 0.3424(2) 0.6950(2) 0.2406(2) 0.0404(9) Uani 1 1 d . . . F11C F 0.3927(3) 0.7176(2) 0.1485(2) 0.0440(10) Uani 1 1 d . . . C12 C 0.3545(4) 0.5854(3) 0.0767(3) 0.0320(13) Uani 1 1 d . . . F12A F 0.4172(2) 0.5456(2) 0.0957(2) 0.0407(9) Uani 1 1 d . . . F12B F 0.3876(3) 0.6341(2) 0.0449(2) 0.0494(11) Uani 1 1 d . . . F12C F 0.3033(3) 0.5532(3) 0.0331(2) 0.0628(15) Uani 1 1 d . . . C13 C -0.0991(3) 0.4882(3) 0.1585(3) 0.0223(10) Uani 1 1 d . . . H13A H -0.0830 0.5322 0.1531 0.027 Uiso 1 1 calc R . . C14 C -0.1793(3) 0.4677(3) 0.1345(3) 0.0265(11) Uani 1 1 d . . . C15 C -0.2024(4) 0.4032(3) 0.1430(4) 0.0397(16) Uani 1 1 d . . . H15A H -0.2568 0.3888 0.1276 0.048 Uiso 1 1 calc R . . C16 C -0.1463(4) 0.3604(4) 0.1737(5) 0.0468(19) Uani 1 1 d . . . H16A H -0.1623 0.3163 0.1787 0.056 Uiso 1 1 calc R . . C17 C -0.0663(4) 0.3803(3) 0.1977(4) 0.0370(14) Uani 1 1 d . . . H17A H -0.0284 0.3500 0.2190 0.044 Uiso 1 1 calc R . . C18 C -0.0426(3) 0.4447(3) 0.1900(3) 0.0259(11) Uani 1 1 d . . . C19 C 0.0429(3) 0.4690(3) 0.2160(3) 0.0270(11) Uani 1 1 d . . . H19A H 0.0579 0.4447 0.2572 0.032 Uiso 1 1 calc R . . H19B H 0.0353 0.5149 0.2290 0.032 Uiso 1 1 calc R . . C20 C 0.0910(4) 0.4841(3) 0.0811(3) 0.0309(13) Uani 1 1 d . . . F20A F 0.0272(2) 0.4467(2) 0.05839(19) 0.0413(9) Uani 1 1 d . . . F20B F 0.0629(3) 0.5454(2) 0.0785(2) 0.0493(11) Uani 1 1 d . . . F20C F 0.1502(3) 0.4789(3) 0.0389(2) 0.0572(14) Uani 1 1 d . . . C21 C 0.1549(4) 0.3776(3) 0.1567(4) 0.0381(15) Uani 1 1 d . . . F21A F 0.0922(3) 0.3439(2) 0.1260(3) 0.0542(13) Uani 1 1 d . . . F21B F 0.1713(4) 0.3492(2) 0.2148(3) 0.082(2) Uani 1 1 d . . . F21C F 0.2219(3) 0.3682(2) 0.1238(4) 0.083(2) Uani 1 1 d . . . C22 C -0.2385(3) 0.5153(3) 0.0982(3) 0.0293(12) Uani 1 1 d . . . H22A H -0.2786 0.4901 0.0687 0.035 Uiso 1 1 calc R . . H22B H -0.2053 0.5428 0.0700 0.035 Uiso 1 1 calc R . . C23 C -0.3745(3) 0.6009(4) 0.0794(3) 0.0329(13) Uani 1 1 d . . . F23A F -0.4324(2) 0.6397(2) 0.1012(2) 0.0444(10) Uani 1 1 d . . . F23B F -0.4151(2) 0.5547(2) 0.0436(2) 0.0482(11) Uani 1 1 d . . . F23C F -0.3310(3) 0.6353(3) 0.0378(2) 0.0572(14) Uani 1 1 d . . . C24 C -0.3736(3) 0.5082(3) 0.1827(3) 0.0291(12) Uani 1 1 d . . . F24A F -0.3351(2) 0.4772(2) 0.2336(2) 0.0416(9) Uani 1 1 d . . . F24B F -0.4408(2) 0.5379(2) 0.2041(2) 0.0405(9) Uani 1 1 d . . . F24C F -0.4020(3) 0.4618(2) 0.1396(2) 0.0484(11) Uani 1 1 d . . . C27 C 0.1813(3) 0.4882(3) 0.3620(3) 0.0234(10) Uani 1 1 d . . . C28 C 0.1181(4) 0.5207(3) 0.3915(4) 0.0366(14) Uani 1 1 d . . . H28A H 0.1194 0.5669 0.3944 0.044 Uiso 1 1 calc R . . C29 C 0.0531(4) 0.4866(4) 0.4169(4) 0.0423(17) Uani 1 1 d . . . H29A H 0.0101 0.5096 0.4367 0.051 Uiso 1 1 calc R . . C30 C 0.0500(4) 0.4204(4) 0.4138(4) 0.0422(16) Uani 1 1 d . . . H30A H 0.0056 0.3974 0.4318 0.051 Uiso 1 1 calc R . . C31 C 0.1115(4) 0.3871(3) 0.3844(4) 0.0429(17) Uani 1 1 d . . . H31A H 0.1101 0.3410 0.3822 0.051 Uiso 1 1 calc R . . C32 C 0.1759(4) 0.4213(3) 0.3579(4) 0.0366(14) Uani 1 1 d . . . H32A H 0.2173 0.3981 0.3363 0.044 Uiso 1 1 calc R . . C33 C 0.3620(3) 0.4944(3) 0.3601(3) 0.0232(10) Uani 1 1 d . . . C34 C 0.3643(4) 0.4567(3) 0.4169(3) 0.0303(12) Uani 1 1 d . . . H34A H 0.3136 0.4461 0.4360 0.036 Uiso 1 1 calc R . . C35 C 0.4407(4) 0.4343(4) 0.4457(3) 0.0389(15) Uani 1 1 d . . . H35A H 0.4421 0.4085 0.4845 0.047 Uiso 1 1 calc R . . C36 C 0.5141(4) 0.4495(4) 0.4185(3) 0.0378(15) Uani 1 1 d . . . H36A H 0.5661 0.4338 0.4382 0.045 Uiso 1 1 calc R . . C37 C 0.5126(4) 0.4878(4) 0.3619(3) 0.0373(15) Uani 1 1 d . . . H37A H 0.5634 0.4989 0.3434 0.045 Uiso 1 1 calc R . . C38 C 0.4362(4) 0.5096(3) 0.3327(3) 0.0312(13) Uani 1 1 d . . . H38A H 0.4349 0.5351 0.2937 0.037 Uiso 1 1 calc R . . C39 C 0.2634(3) 0.6106(3) 0.3610(2) 0.0217(10) Uani 1 1 d . . . C40 C 0.3115(4) 0.6234(3) 0.4198(3) 0.0280(11) Uani 1 1 d . . . H40A H 0.3509 0.5921 0.4370 0.034 Uiso 1 1 calc R . . C41 C 0.3024(4) 0.6811(3) 0.4530(3) 0.0348(14) Uani 1 1 d . . . H41A H 0.3358 0.6893 0.4929 0.042 Uiso 1 1 calc R . . C42 C 0.2450(4) 0.7272(3) 0.4288(3) 0.0335(13) Uani 1 1 d . . . H42A H 0.2370 0.7659 0.4529 0.040 Uiso 1 1 calc R . . C43 C 0.1996(4) 0.7166(3) 0.3695(3) 0.0331(13) Uani 1 1 d . . . H43A H 0.1620 0.7491 0.3519 0.040 Uiso 1 1 calc R . . C44 C 0.2081(4) 0.6589(3) 0.3351(3) 0.0283(12) Uani 1 1 d . . . H44A H 0.1766 0.6521 0.2942 0.034 Uiso 1 1 calc R . . C45 C -0.1477(3) 0.6810(3) 0.3732(3) 0.0237(10) Uani 1 1 d . . . C46 C -0.0800(4) 0.6496(3) 0.4059(3) 0.0330(13) Uani 1 1 d . . . H46A H -0.0796 0.6035 0.4096 0.040 Uiso 1 1 calc R . . C47 C -0.0123(4) 0.6862(4) 0.4335(4) 0.0456(17) Uani 1 1 d . . . H47A H 0.0348 0.6648 0.4549 0.055 Uiso 1 1 calc R . . C48 C -0.0135(4) 0.7531(4) 0.4297(4) 0.0446(17) Uani 1 1 d . . . H48A H 0.0322 0.7776 0.4496 0.053 Uiso 1 1 calc R . . C49 C -0.0813(4) 0.7849(4) 0.3970(4) 0.0396(15) Uani 1 1 d . . . H49A H -0.0822 0.8310 0.3943 0.048 Uiso 1 1 calc R . . C50 C -0.1475(4) 0.7487(3) 0.3683(3) 0.0319(13) Uani 1 1 d . . . H50A H -0.1933 0.7702 0.3449 0.038 Uiso 1 1 calc R . . C51 C -0.2218(3) 0.5545(3) 0.3646(3) 0.0248(11) Uani 1 1 d . . . C52 C -0.2489(5) 0.5394(4) 0.4259(3) 0.0418(16) Uani 1 1 d . . . H52A H -0.2780 0.5712 0.4492 0.050 Uiso 1 1 calc R . . C53 C -0.2339(6) 0.4777(4) 0.4538(3) 0.0483(19) Uani 1 1 d . . . H53A H -0.2517 0.4682 0.4962 0.058 Uiso 1 1 calc R . . C54 C -0.1932(4) 0.4307(3) 0.4197(3) 0.0367(14) Uani 1 1 d . . . H54A H -0.1829 0.3890 0.4387 0.044 Uiso 1 1 calc R . . C55 C -0.1677(4) 0.4443(3) 0.3587(3) 0.0376(14) Uani 1 1 d . . . H55A H -0.1401 0.4119 0.3350 0.045 Uiso 1 1 calc R . . C56 C -0.1826(4) 0.5062(3) 0.3310(3) 0.0360(14) Uani 1 1 d . . . H56A H -0.1652 0.5151 0.2883 0.043 Uiso 1 1 calc R . . C57 C -0.3258(3) 0.6672(3) 0.3700(3) 0.0230(10) Uani 1 1 d . . . C58 C -0.3189(4) 0.6993(3) 0.4313(3) 0.0331(13) Uani 1 1 d . . . H58A H -0.2651 0.7050 0.4539 0.040 Uiso 1 1 calc R . . C59 C -0.3895(4) 0.7228(4) 0.4594(3) 0.0377(15) Uani 1 1 d . . . H59A H -0.3835 0.7444 0.5008 0.045 Uiso 1 1 calc R . . C60 C -0.4676(4) 0.7148(4) 0.4275(3) 0.0380(15) Uani 1 1 d . . . H60A H -0.5155 0.7318 0.4465 0.046 Uiso 1 1 calc R . . C61 C -0.4772(4) 0.6822(4) 0.3676(3) 0.0392(15) Uani 1 1 d . . . H61A H -0.5315 0.6756 0.3463 0.047 Uiso 1 1 calc R . . C62 C -0.4065(3) 0.6592(3) 0.3391(3) 0.0297(12) Uani 1 1 d . . . H62A H -0.4132 0.6376 0.2978 0.036 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 0.01579(8) 0.01846(9) 0.02003(9) -0.00224(7) 0.00136(6) 0.00111(6) P1 0.0165(5) 0.0218(7) 0.0209(6) -0.0004(5) 0.0020(5) 0.0004(4) P2 0.0171(5) 0.0213(7) 0.0271(6) -0.0054(5) 0.0013(5) 0.0010(5) P3 0.0190(5) 0.0197(6) 0.0196(6) -0.0008(5) 0.0014(5) 0.0014(5) C25 0.024(2) 0.027(3) 0.030(3) -0.001(2) 0.001(2) 0.002(2) O1 0.028(2) 0.036(3) 0.052(3) 0.003(2) 0.009(2) 0.0149(18) Ir2 0.01521(8) 0.02180(10) 0.02130(9) 0.00154(7) 0.00373(6) 0.00124(6) P4 0.0137(5) 0.0301(8) 0.0217(6) -0.0024(5) 0.0022(5) 0.0013(5) P5 0.0166(5) 0.0235(7) 0.0298(7) 0.0074(6) 0.0044(5) 0.0018(5) P6 0.0179(5) 0.0229(7) 0.0203(6) -0.0005(5) 0.0041(5) 0.0007(5) C26 0.028(3) 0.024(3) 0.038(3) 0.002(2) 0.004(2) 0.002(2) O2 0.031(2) 0.046(3) 0.064(3) -0.004(3) 0.001(2) 0.019(2) C1 0.019(2) 0.023(3) 0.031(3) 0.004(2) 0.000(2) -0.0009(18) C2 0.019(2) 0.026(3) 0.030(3) 0.002(2) 0.003(2) 0.0014(19) C3 0.020(2) 0.028(3) 0.056(4) 0.003(3) 0.012(3) -0.002(2) C4 0.026(3) 0.022(3) 0.066(5) -0.004(3) 0.016(3) -0.007(2) C5 0.025(3) 0.026(3) 0.048(4) -0.003(3) 0.009(3) -0.001(2) C6 0.015(2) 0.029(3) 0.033(3) 0.005(2) 0.003(2) -0.0014(18) C7 0.015(2) 0.027(3) 0.035(3) 0.011(2) 0.005(2) 0.0004(18) C8 0.031(3) 0.032(4) 0.059(4) 0.018(3) 0.010(3) 0.005(3) F8A 0.141(6) 0.029(3) 0.069(3) -0.001(2) 0.036(4) 0.013(3) F8B 0.041(2) 0.046(3) 0.105(4) 0.027(3) -0.018(3) 0.009(2) F8C 0.043(2) 0.030(2) 0.130(5) 0.029(3) 0.030(3) -0.0012(19) C9 0.021(2) 0.043(4) 0.032(3) 0.016(3) 0.003(2) 0.000(2) F9A 0.043(2) 0.047(3) 0.0349(19) 0.0067(17) 0.0117(17) 0.0100(18) F9B 0.0286(18) 0.073(3) 0.0323(19) 0.018(2) -0.0027(15) -0.0018(19) F9C 0.0316(18) 0.064(3) 0.040(2) 0.024(2) 0.0099(16) -0.0074(18) C10 0.018(2) 0.030(3) 0.026(2) 0.007(2) 0.0014(19) 0.0014(19) C11 0.021(2) 0.030(3) 0.031(3) -0.002(2) -0.003(2) -0.002(2) F11A 0.0225(15) 0.036(2) 0.051(2) -0.0049(17) -0.0068(15) 0.0012(14) F11B 0.0349(19) 0.040(2) 0.047(2) -0.0209(18) 0.0080(17) -0.0074(16) F11C 0.039(2) 0.042(2) 0.050(2) 0.0117(19) -0.0033(18) -0.0192(17) C12 0.025(2) 0.043(4) 0.029(3) -0.005(3) 0.008(2) -0.002(2) F12A 0.0303(18) 0.048(2) 0.046(2) -0.0001(18) 0.0159(17) 0.0109(16) F12B 0.046(2) 0.057(3) 0.048(2) 0.017(2) 0.025(2) 0.009(2) F12C 0.037(2) 0.113(4) 0.039(2) -0.042(3) 0.0089(18) -0.012(3) C13 0.016(2) 0.023(3) 0.029(2) -0.005(2) 0.0056(19) -0.0007(17) C14 0.020(2) 0.032(3) 0.028(3) -0.012(2) 0.005(2) 0.001(2) C15 0.020(2) 0.033(4) 0.065(5) -0.010(3) 0.000(3) -0.007(2) C16 0.023(3) 0.032(4) 0.085(6) 0.003(4) 0.002(3) -0.009(2) C17 0.027(3) 0.028(3) 0.057(4) 0.006(3) 0.003(3) -0.001(2) C18 0.018(2) 0.028(3) 0.032(3) -0.002(2) 0.005(2) -0.0015(19) C19 0.018(2) 0.036(3) 0.028(3) -0.003(2) 0.003(2) -0.001(2) C20 0.024(2) 0.044(4) 0.024(3) -0.007(2) 0.000(2) -0.003(2) F20A 0.0295(18) 0.059(3) 0.0341(19) -0.0136(18) -0.0059(15) -0.0103(17) F20B 0.061(3) 0.046(3) 0.037(2) 0.0001(18) -0.016(2) 0.007(2) F20C 0.032(2) 0.110(4) 0.030(2) -0.014(2) 0.0095(17) -0.010(2) C21 0.027(3) 0.031(3) 0.055(4) -0.013(3) -0.004(3) -0.002(2) F21A 0.045(2) 0.027(2) 0.089(4) -0.026(2) -0.007(2) -0.0082(17) F21B 0.121(5) 0.024(2) 0.091(4) 0.001(2) -0.044(4) 0.007(3) F21C 0.051(3) 0.031(3) 0.175(6) -0.042(3) 0.049(4) 0.000(2) C22 0.022(2) 0.040(4) 0.025(3) -0.011(2) 0.001(2) 0.007(2) C23 0.017(2) 0.050(4) 0.032(3) 0.001(3) 0.000(2) 0.003(2) F23A 0.0266(17) 0.053(3) 0.052(2) -0.005(2) -0.0051(17) 0.0144(17) F23B 0.0313(19) 0.068(3) 0.043(2) -0.014(2) -0.0108(17) 0.0060(19) F23C 0.031(2) 0.097(4) 0.042(2) 0.032(2) -0.0074(18) -0.008(2) C24 0.021(2) 0.032(3) 0.035(3) -0.006(2) 0.003(2) -0.006(2) F24A 0.0342(19) 0.041(2) 0.050(2) 0.0120(19) 0.0028(17) -0.0063(17) F24B 0.0212(16) 0.047(2) 0.055(2) 0.0020(19) 0.0153(16) -0.0010(15) F24C 0.044(2) 0.045(3) 0.056(3) -0.018(2) 0.005(2) -0.0191(19) C27 0.022(2) 0.025(3) 0.023(2) 0.003(2) 0.0031(19) 0.0012(19) C28 0.036(3) 0.030(3) 0.046(4) 0.001(3) 0.017(3) 0.003(3) C29 0.031(3) 0.047(4) 0.052(4) 0.007(3) 0.020(3) 0.008(3) C30 0.030(3) 0.043(4) 0.055(4) 0.017(3) 0.015(3) 0.000(3) C31 0.039(3) 0.023(3) 0.068(5) 0.009(3) 0.013(3) -0.004(3) C32 0.027(3) 0.034(4) 0.051(4) 0.003(3) 0.018(3) 0.005(2) C33 0.025(2) 0.024(3) 0.021(2) -0.001(2) 0.0006(19) 0.0058(19) C34 0.031(3) 0.032(3) 0.028(3) 0.004(2) 0.003(2) 0.000(2) C35 0.036(3) 0.044(4) 0.036(3) 0.010(3) -0.004(3) 0.009(3) C36 0.033(3) 0.040(4) 0.039(3) -0.003(3) -0.009(3) 0.014(3) C37 0.024(3) 0.050(4) 0.038(3) 0.001(3) 0.001(2) 0.005(3) C38 0.023(2) 0.043(4) 0.027(3) 0.001(2) 0.000(2) 0.003(2) C39 0.024(2) 0.023(3) 0.018(2) -0.0011(19) 0.0024(18) -0.0015(19) C40 0.031(3) 0.024(3) 0.029(3) -0.002(2) 0.000(2) -0.003(2) C41 0.044(3) 0.031(3) 0.028(3) -0.008(2) -0.003(3) -0.007(3) C42 0.045(3) 0.024(3) 0.032(3) -0.005(2) 0.005(3) 0.001(2) C43 0.042(3) 0.024(3) 0.034(3) -0.002(2) 0.003(3) 0.001(2) C44 0.031(3) 0.027(3) 0.026(3) -0.002(2) 0.002(2) 0.008(2) C45 0.019(2) 0.026(3) 0.026(2) -0.002(2) 0.0040(19) 0.0013(19) C46 0.026(3) 0.031(3) 0.041(3) 0.004(3) -0.002(2) -0.001(2) C47 0.031(3) 0.052(5) 0.052(4) 0.003(3) -0.011(3) -0.005(3) C48 0.034(3) 0.044(4) 0.055(4) -0.009(3) -0.006(3) -0.009(3) C49 0.035(3) 0.030(4) 0.054(4) -0.012(3) 0.002(3) -0.007(3) C50 0.029(3) 0.023(3) 0.043(3) -0.004(2) 0.001(2) 0.000(2) C51 0.024(2) 0.030(3) 0.020(2) 0.003(2) 0.0018(19) 0.001(2) C52 0.058(4) 0.038(4) 0.031(3) 0.003(3) 0.012(3) 0.000(3) C53 0.078(6) 0.039(4) 0.030(3) 0.011(3) 0.016(3) -0.004(4) C54 0.043(3) 0.023(3) 0.042(3) 0.006(3) -0.008(3) -0.006(3) C55 0.043(3) 0.030(3) 0.040(3) 0.001(3) 0.004(3) 0.005(3) C56 0.043(3) 0.034(4) 0.032(3) 0.006(3) 0.008(3) 0.001(3) C57 0.015(2) 0.030(3) 0.024(2) 0.000(2) 0.0059(18) -0.0041(18) C58 0.028(3) 0.039(4) 0.034(3) -0.010(3) 0.007(2) -0.003(2) C59 0.034(3) 0.049(4) 0.032(3) -0.011(3) 0.011(3) 0.004(3) C60 0.027(3) 0.051(4) 0.038(3) -0.006(3) 0.013(3) 0.006(3) C61 0.023(3) 0.056(5) 0.039(3) -0.006(3) 0.007(2) 0.001(3) C62 0.022(2) 0.044(4) 0.023(2) -0.006(2) 0.004(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C25 1.925(6) . ? Ir1 P1 2.2369(14) . ? Ir1 P2 2.2401(13) . ? Ir1 P3 2.3170(13) . ? P1 C10 1.854(5) . ? P1 C12 1.890(6) . ? P1 C11 1.895(6) . ? P2 C19 1.839(6) . ? P2 C21 1.882(7) . ? P2 C20 1.896(6) . ? P3 C39 1.834(6) . ? P3 C33 1.842(5) . ? P3 C27 1.843(6) . ? C25 O1 1.140(7) . ? Ir2 C26 1.922(6) . ? Ir2 P5 2.2302(14) . ? Ir2 P4 2.2405(14) . ? Ir2 P6 2.3242(13) . ? P4 C22 1.847(6) . ? P4 C24 1.897(6) . ? P4 C23 1.899(6) . ? P5 C7 1.841(5) . ? P5 C8 1.886(7) . ? P5 C9 1.900(7) . ? P6 C57 1.827(5) . ? P6 C51 1.827(6) . ? P6 C45 1.843(6) . ? C26 O2 1.134(7) . ? C1 C6 1.383(8) . ? C1 C2 1.391(7) . ? C1 H1A 0.9500 . ? C2 C3 1.403(9) . ? C2 C10 1.501(8) . ? C3 C4 1.382(9) . ? C3 H3A 0.9500 . ? C4 C5 1.386(8) . ? C4 H4A 0.9500 . ? C5 C6 1.399(9) . ? C5 H5A 0.9500 . ? C6 C7 1.513(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 F8A 1.306(9) . ? C8 F8C 1.328(8) . ? C8 F8B 1.341(8) . ? C9 F9B 1.338(7) . ? C9 F9C 1.341(7) . ? C9 F9A 1.341(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 F11A 1.330(7) . ? C11 F11B 1.341(7) . ? C11 F11C 1.345(7) . ? C12 F12B 1.325(8) . ? C12 F12A 1.328(7) . ? C12 F12C 1.335(7) . ? C13 C18 1.390(8) . ? C13 C14 1.402(7) . ? C13 H13A 0.9500 . ? C14 C15 1.391(9) . ? C14 C22 1.512(8) . ? C15 C16 1.371(10) . ? C15 H15A 0.9500 . ? C16 C17 1.393(9) . ? C16 H16A 0.9500 . ? C17 C18 1.390(9) . ? C17 H17A 0.9500 . ? C18 C19 1.512(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 F20C 1.331(7) . ? C20 F20A 1.332(7) . ? C20 F20B 1.337(8) . ? C21 F21C 1.320(8) . ? C21 F21B 1.327(9) . ? C21 F21A 1.334(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 F23A 1.324(7) . ? C23 F23B 1.334(8) . ? C23 F23C 1.339(8) . ? C24 F24A 1.325(7) . ? C24 F24B 1.338(7) . ? C24 F24C 1.351(7) . ? C27 C32 1.379(9) . ? C27 C28 1.387(8) . ? C28 C29 1.388(9) . ? C28 H28A 0.9500 . ? C29 C30 1.362(11) . ? C29 H29A 0.9500 . ? C30 C31 1.373(10) . ? C30 H30A 0.9500 . ? C31 C32 1.390(9) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.386(8) . ? C33 C34 1.391(8) . ? C34 C35 1.392(9) . ? C34 H34A 0.9500 . ? C35 C36 1.372(10) . ? C35 H35A 0.9500 . ? C36 C37 1.393(10) . ? C36 H36A 0.9500 . ? C37 C38 1.389(8) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.395(7) . ? C39 C44 1.404(8) . ? C40 C41 1.378(9) . ? C40 H40A 0.9500 . ? C41 C42 1.383(10) . ? C41 H41A 0.9500 . ? C42 C43 1.376(9) . ? C42 H42A 0.9500 . ? C43 C44 1.388(9) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C46 1.385(8) . ? C45 C50 1.396(9) . ? C46 C47 1.400(9) . ? C46 H46A 0.9500 . ? C47 C48 1.376(11) . ? C47 H47A 0.9500 . ? C48 C49 1.391(10) . ? C48 H48A 0.9500 . ? C49 C50 1.385(9) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C56 1.384(9) . ? C51 C52 1.388(9) . ? C52 C53 1.403(10) . ? C52 H52A 0.9500 . ? C53 C54 1.380(11) . ? C53 H53A 0.9500 . ? C54 C55 1.366(10) . ? C54 H54A 0.9500 . ? C55 C56 1.404(10) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C62 1.399(7) . ? C57 C58 1.408(8) . ? C58 C59 1.391(9) . ? C58 H58A 0.9500 . ? C59 C60 1.372(9) . ? C59 H59A 0.9500 . ? C60 C61 1.389(10) . ? C60 H60A 0.9500 . ? C61 C62 1.393(9) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? 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 C25 Ir1 P1 97.14(19) . . ? C25 Ir1 P2 99.36(18) . . ? P1 Ir1 P2 120.15(5) . . ? C25 Ir1 P3 97.41(18) . . ? P1 Ir1 P3 119.98(5) . . ? P2 Ir1 P3 114.21(5) . . ? C10 P1 C12 97.0(3) . . ? C10 P1 C11 99.7(3) . . ? C12 P1 C11 96.0(3) . . ? C10 P1 Ir1 123.70(18) . . ? C12 P1 Ir1 115.8(2) . . ? C11 P1 Ir1 119.2(2) . . ? C19 P2 C21 103.4(3) . . ? C19 P2 C20 103.0(3) . . ? C21 P2 C20 96.6(3) . . ? C19 P2 Ir1 116.42(19) . . ? C21 P2 Ir1 117.1(2) . . ? C20 P2 Ir1 117.4(2) . . ? C39 P3 C33 102.3(2) . . ? C39 P3 C27 101.1(3) . . ? C33 P3 C27 103.5(3) . . ? C39 P3 Ir1 117.49(17) . . ? C33 P3 Ir1 117.19(18) . . ? C27 P3 Ir1 113.05(18) . . ? O1 C25 Ir1 178.3(6) . . ? C26 Ir2 P5 99.03(19) . . ? C26 Ir2 P4 97.57(19) . . ? P5 Ir2 P4 119.10(5) . . ? C26 Ir2 P6 97.72(19) . . ? P5 Ir2 P6 113.18(5) . . ? P4 Ir2 P6 121.87(5) . . ? C22 P4 C24 100.0(3) . . ? C22 P4 C23 96.8(3) . . ? C24 P4 C23 96.8(3) . . ? C22 P4 Ir2 123.13(19) . . ? C24 P4 Ir2 119.45(19) . . ? C23 P4 Ir2 115.4(2) . . ? C7 P5 C8 103.9(3) . . ? C7 P5 C9 102.1(3) . . ? C8 P5 C9 96.7(3) . . ? C7 P5 Ir2 117.08(18) . . ? C8 P5 Ir2 116.7(2) . . ? C9 P5 Ir2 117.3(2) . . ? C57 P6 C51 102.9(3) . . ? C57 P6 C45 102.3(2) . . ? C51 P6 C45 102.2(3) . . ? C57 P6 Ir2 116.79(18) . . ? C51 P6 Ir2 117.07(18) . . ? C45 P6 Ir2 113.43(18) . . ? O2 C26 Ir2 179.0(6) . . ? C6 C1 C2 121.1(5) . . ? C6 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C1 C2 C3 118.9(5) . . ? C1 C2 C10 120.8(5) . . ? C3 C2 C10 120.3(5) . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.6(6) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5A 120.2 . . ? C6 C5 H5A 120.2 . . ? C1 C6 C5 119.6(5) . . ? C1 C6 C7 120.2(5) . . ? C5 C6 C7 120.1(5) . . ? C6 C7 P5 122.0(4) . . ? C6 C7 H7A 106.8 . . ? P5 C7 H7A 106.8 . . ? C6 C7 H7B 106.8 . . ? P5 C7 H7B 106.8 . . ? H7A C7 H7B 106.7 . . ? F8A C8 F8C 109.0(7) . . ? F8A C8 F8B 107.0(6) . . ? F8C C8 F8B 104.8(6) . . ? F8A C8 P5 110.7(5) . . ? F8C C8 P5 116.3(5) . . ? F8B C8 P5 108.4(5) . . ? F9B C9 F9C 106.4(5) . . ? F9B C9 F9A 107.5(6) . . ? F9C C9 F9A 106.7(5) . . ? F9B C9 P5 110.8(4) . . ? F9C C9 P5 116.2(5) . . ? F9A C9 P5 108.9(4) . . ? C2 C10 P1 115.3(4) . . ? C2 C10 H10A 108.5 . . ? P1 C10 H10A 108.5 . . ? C2 C10 H10B 108.5 . . ? P1 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? F11A C11 F11B 106.6(5) . . ? F11A C11 F11C 107.1(5) . . ? F11B C11 F11C 106.2(5) . . ? F11A C11 P1 111.6(4) . . ? F11B C11 P1 109.7(4) . . ? F11C C11 P1 115.2(4) . . ? F12B C12 F12A 106.7(5) . . ? F12B C12 F12C 107.3(5) . . ? F12A C12 F12C 107.4(6) . . ? F12B C12 P1 115.7(5) . . ? F12A C12 P1 112.0(4) . . ? F12C C12 P1 107.5(4) . . ? C18 C13 C14 120.8(5) . . ? C18 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C15 C14 C13 119.1(6) . . ? C15 C14 C22 121.1(5) . . ? C13 C14 C22 119.8(5) . . ? C16 C15 C14 119.9(6) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 121.4(6) . . ? C15 C16 H16A 119.3 . . ? C17 C16 H16A 119.3 . . ? C18 C17 C16 119.4(6) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C13 119.4(5) . . ? C17 C18 C19 121.5(5) . . ? C13 C18 C19 119.1(5) . . ? C18 C19 P2 123.8(4) . . ? C18 C19 H19A 106.4 . . ? P2 C19 H19A 106.4 . . ? C18 C19 H19B 106.4 . . ? P2 C19 H19B 106.4 . . ? H19A C19 H19B 106.5 . . ? F20C C20 F20A 107.0(5) . . ? F20C C20 F20B 107.6(6) . . ? F20A C20 F20B 106.5(5) . . ? F20C C20 P2 110.7(4) . . ? F20A C20 P2 116.3(5) . . ? F20B C20 P2 108.3(4) . . ? F21C C21 F21B 106.0(7) . . ? F21C C21 F21A 107.2(6) . . ? F21B C21 F21A 106.1(6) . . ? F21C C21 P2 110.7(5) . . ? F21B C21 P2 109.9(5) . . ? F21A C21 P2 116.4(5) . . ? C14 C22 P4 116.9(4) . . ? C14 C22 H22A 108.1 . . ? P4 C22 H22A 108.1 . . ? C14 C22 H22B 108.1 . . ? P4 C22 H22B 108.1 . . ? H22A C22 H22B 107.3 . . ? F23A C23 F23B 106.9(5) . . ? F23A C23 F23C 107.8(6) . . ? F23B C23 F23C 106.5(5) . . ? F23A C23 P4 111.9(4) . . ? F23B C23 P4 114.7(5) . . ? F23C C23 P4 108.7(4) . . ? F24A C24 F24B 107.5(5) . . ? F24A C24 F24C 106.3(5) . . ? F24B C24 F24C 107.2(5) . . ? F24A C24 P4 109.7(4) . . ? F24B C24 P4 110.9(4) . . ? F24C C24 P4 114.9(4) . . ? C32 C27 C28 117.6(5) . . ? C32 C27 P3 119.2(4) . . ? C28 C27 P3 122.9(5) . . ? C27 C28 C29 120.6(6) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C30 C29 C28 120.8(6) . . ? C30 C29 H29A 119.6 . . ? C28 C29 H29A 119.6 . . ? C29 C30 C31 119.6(6) . . ? C29 C30 H30A 120.2 . . ? C31 C30 H30A 120.2 . . ? C30 C31 C32 119.6(7) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? C27 C32 C31 121.7(6) . . ? C27 C32 H32A 119.2 . . ? C31 C32 H32A 119.2 . . ? C38 C33 C34 119.5(5) . . ? C38 C33 P3 117.2(4) . . ? C34 C33 P3 123.2(4) . . ? C33 C34 C35 120.0(6) . . ? C33 C34 H34A 120.0 . . ? C35 C34 H34A 120.0 . . ? C36 C35 C34 120.3(6) . . ? C36 C35 H35A 119.8 . . ? C34 C35 H35A 119.8 . . ? C35 C36 C37 120.1(6) . . ? C35 C36 H36A 119.9 . . ? C37 C36 H36A 119.9 . . ? C38 C37 C36 119.6(6) . . ? C38 C37 H37A 120.2 . . ? C36 C37 H37A 120.2 . . ? C33 C38 C37 120.5(6) . . ? C33 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C40 C39 C44 118.5(5) . . ? C40 C39 P3 121.4(4) . . ? C44 C39 P3 119.9(4) . . ? C41 C40 C39 120.8(6) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C40 C41 C42 120.4(6) . . ? C40 C41 H41A 119.8 . . ? C42 C41 H41A 119.8 . . ? C43 C42 C41 119.7(6) . . ? C43 C42 H42A 120.2 . . ? C41 C42 H42A 120.2 . . ? C42 C43 C44 120.7(6) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C43 C44 C39 119.9(5) . . ? C43 C44 H44A 120.1 . . ? C39 C44 H44A 120.1 . . ? C46 C45 C50 119.6(5) . . ? C46 C45 P6 122.2(5) . . ? C50 C45 P6 118.0(4) . . ? C45 C46 C47 119.4(6) . . ? C45 C46 H46A 120.3 . . ? C47 C46 H46A 120.3 . . ? C48 C47 C46 120.6(7) . . ? C48 C47 H47A 119.7 . . ? C46 C47 H47A 119.7 . . ? C47 C48 C49 120.1(6) . . ? C47 C48 H48A 119.9 . . ? C49 C48 H48A 119.9 . . ? C50 C49 C48 119.5(7) . . ? C50 C49 H49A 120.3 . . ? C48 C49 H49A 120.3 . . ? C49 C50 C45 120.7(6) . . ? C49 C50 H50A 119.6 . . ? C45 C50 H50A 119.6 . . ? C56 C51 C52 117.9(6) . . ? C56 C51 P6 121.0(4) . . ? C52 C51 P6 121.1(5) . . ? C51 C52 C53 120.7(7) . . ? C51 C52 H52A 119.6 . . ? C53 C52 H52A 119.6 . . ? C54 C53 C52 120.1(6) . . ? C54 C53 H53A 120.0 . . ? C52 C53 H53A 120.0 . . ? C55 C54 C53 120.0(6) . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C56 119.7(7) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C51 C56 C55 121.5(6) . . ? C51 C56 H56A 119.3 . . ? C55 C56 H56A 119.3 . . ? C62 C57 C58 117.3(5) . . ? C62 C57 P6 119.5(4) . . ? C58 C57 P6 123.2(4) . . ? C59 C58 C57 121.2(6) . . ? C59 C58 H58A 119.4 . . ? C57 C58 H58A 119.4 . . ? C60 C59 C58 120.1(6) . . ? C60 C59 H59A 119.9 . . ? C58 C59 H59A 119.9 . . ? C59 C60 C61 120.4(6) . . ? C59 C60 H60A 119.8 . . ? C61 C60 H60A 119.8 . . ? C60 C61 C62 119.4(6) . . ? C60 C61 H61A 120.3 . . ? C62 C61 H61A 120.3 . . ? C61 C62 C57 121.6(6) . . ? C61 C62 H62A 119.2 . . ? C57 C62 H62A 119.2 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.901 _refine_diff_density_min -4.014 _refine_diff_density_rms 0.232 #####end #===================================================================== data_jja94a _database_code_depnum_ccdc_archive 'CCDC 826941' #TrackingRef '- CIF files.txt' #===================================================================== _vrf_PLAT601_jja94a ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 500.00 A^3^ RESPONSE: The observed void is expected. The network is stabilized by strong bonding between the metal centers and the bridging pcp ligands. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[(?-CF3PCPH)Ir(H)(CO)(PPh3)]4' _chemical_melting_point ? _chemical_formula_moiety 'C124 H96 F48 Ir4 O4 P12' _chemical_formula_sum 'C124 H96 F48 Ir4 O4 P12' _chemical_formula_weight 3702.45 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 Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.067(2) _cell_length_b 12.4089(8) _cell_length_c 37.446(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.509(1) _cell_angle_gamma 90.00 _cell_volume 14451.9(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7023 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 25.13 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.702 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7168 _exptl_absorpt_coefficient_mu 3.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.782 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2001)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42695 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.37 _reflns_number_total 14702 _reflns_number_gt 11014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 V. 2.2 (Bruker AXS Inc, 2007)' _computing_cell_refinement 'Bruker APEX2 V. 2.2 (Bruker AXS Inc, 2007)' _computing_data_reduction 'Bruker SAINT V. 7.34a (Bruker AXS Inc, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.14 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.14 (Bruker, 2001)' _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^)+(0.0801P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14702 _refine_ls_number_parameters 865 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1396 _refine_ls_wR_factor_gt 0.1261 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.398562(8) 0.38643(2) 0.081036(8) 0.02205(9) Uani 1 1 d . . . P1 P 0.46061(6) 0.45299(15) 0.08689(6) 0.0250(4) Uani 1 1 d . . . P2 P 0.40073(6) 0.26775(15) 0.12637(6) 0.0250(4) Uani 1 1 d . . . P3 P 0.33598(6) 0.48601(15) 0.04463(6) 0.0242(4) Uani 1 1 d . . . C25 C 0.3865(2) 0.2856(6) 0.0382(2) 0.0296(17) Uani 1 1 d . . . O1 O 0.3784(2) 0.2259(5) 0.01268(18) 0.0463(15) Uani 1 1 d . . . Ir2 Ir 0.643479(9) 0.80434(2) 0.229723(8) 0.02230(9) Uani 1 1 d . . . P4 P 0.33024(6) 0.73342(16) 0.20822(5) 0.0246(4) Uani 1 1 d . . . P5 P 0.65618(6) 0.71127(15) 0.18233(6) 0.0252(4) Uani 1 1 d . . . P6 P 0.58920(6) 0.92112(15) 0.20933(6) 0.0246(4) Uani 1 1 d . . . C26 C 0.6891(3) 0.9066(6) 0.2399(2) 0.0317(17) Uani 1 1 d . . . O2 O 0.71527(19) 0.9668(5) 0.24472(19) 0.0486(16) Uani 1 1 d . . . C1 C 0.5180(2) 0.6997(6) 0.1493(2) 0.0261(16) Uani 1 1 d . . . H1A H 0.5333 0.7009 0.1340 0.031 Uiso 1 1 calc R . . C2 C 0.5146(2) 0.7948(6) 0.1683(2) 0.0294(17) Uani 1 1 d . . . C3 C 0.4905(2) 0.7916(7) 0.1883(2) 0.0367(19) Uani 1 1 d . . . H3A H 0.4866 0.8556 0.2002 0.044 Uiso 1 1 calc R . . C4 C 0.4718(2) 0.6962(7) 0.1916(2) 0.0368(19) Uani 1 1 d . . . H4A H 0.4557 0.6953 0.2063 0.044 Uiso 1 1 calc R . . C5 C 0.4760(2) 0.6042(6) 0.1742(2) 0.0301(17) Uani 1 1 d . . . H5A H 0.4629 0.5395 0.1768 0.036 Uiso 1 1 calc R . . C6 C 0.4992(2) 0.6044(6) 0.1527(2) 0.0262(16) Uani 1 1 d . . . C7 C 0.5059(2) 0.5025(6) 0.1340(2) 0.0275(16) Uani 1 1 d . . . H7A H 0.5141 0.4443 0.1543 0.033 Uiso 1 1 calc R . . H7B H 0.5308 0.5144 0.1287 0.033 Uiso 1 1 calc R . . C8 C 0.4588(3) 0.5641(7) 0.0519(2) 0.038(2) Uani 1 1 d . . . F8A F 0.44367(17) 0.5260(5) 0.01376(14) 0.0546(14) Uani 1 1 d . . . F8B F 0.43257(18) 0.6408(4) 0.05105(17) 0.0567(14) Uani 1 1 d . . . F8C F 0.49665(16) 0.6108(4) 0.06070(15) 0.0532(14) Uani 1 1 d . . . C9 C 0.4941(3) 0.3554(7) 0.0738(3) 0.038(2) Uani 1 1 d . . . F9A F 0.51146(17) 0.2822(4) 0.10316(16) 0.0529(14) Uani 1 1 d . . . F9B F 0.47124(17) 0.3044(5) 0.03970(16) 0.0566(15) Uani 1 1 d . . . F9C F 0.52689(16) 0.4020(5) 0.07039(17) 0.0569(15) Uani 1 1 d . . . C10 C 0.5360(2) 0.8963(6) 0.1655(2) 0.0299(17) Uani 1 1 d . . . H10A H 0.5168 0.9579 0.1627 0.036 Uiso 1 1 calc R . . H10B H 0.5397 0.8934 0.1408 0.036 Uiso 1 1 calc R . . C11 C 0.5725(2) 0.9697(6) 0.2485(3) 0.0350(18) Uani 1 1 d . . . F11A F 0.56835(17) 0.8853(4) 0.26900(15) 0.0474(13) Uani 1 1 d . . . F11B F 0.53532(15) 1.0231(4) 0.23391(14) 0.0453(12) Uani 1 1 d . . . F11C F 0.60203(16) 1.0343(4) 0.27497(15) 0.0530(14) Uani 1 1 d . . . C12 C 0.5977(3) 1.0611(6) 0.1948(3) 0.0361(19) Uani 1 1 d . . . F12A F 0.56740(17) 1.1328(4) 0.19055(18) 0.0572(15) Uani 1 1 d . . . F12B F 0.63454(18) 1.1033(4) 0.2220(2) 0.073(2) Uani 1 1 d . . . F12C F 0.5981(2) 1.0597(4) 0.15981(19) 0.0654(17) Uani 1 1 d . . . C13 C 0.3695(2) 0.4830(6) 0.1745(2) 0.0280(16) Uani 1 1 d . . . H13A H 0.3459 0.4906 0.1485 0.034 Uiso 1 1 calc R . . C14 C 0.3894(2) 0.3813(6) 0.1865(2) 0.0262(16) Uani 1 1 d . . . C15 C 0.4230(3) 0.3696(7) 0.2243(2) 0.0345(18) Uani 1 1 d . . . H15A H 0.4362 0.3013 0.2331 0.041 Uiso 1 1 calc R . . C16 C 0.4378(3) 0.4590(7) 0.2500(2) 0.0367(19) Uani 1 1 d . . . H16A H 0.4614 0.4512 0.2761 0.044 Uiso 1 1 calc R . . C17 C 0.4183(2) 0.5574(7) 0.2379(2) 0.0320(18) Uani 1 1 d . . . H17A H 0.4284 0.6175 0.2555 0.038 Uiso 1 1 calc R . . C18 C 0.3832(2) 0.5696(6) 0.1989(2) 0.0256(15) Uani 1 1 d . . . C19 C 0.3624(2) 0.6775(6) 0.1849(2) 0.0293(17) Uani 1 1 d . . . H19A H 0.3434 0.6728 0.1555 0.035 Uiso 1 1 calc R . . H19B H 0.3853 0.7301 0.1891 0.035 Uiso 1 1 calc R . . C20 C 0.2876(3) 0.6267(7) 0.1922(2) 0.0361(19) Uani 1 1 d . . . F20A F 0.27835(15) 0.5768(4) 0.15678(14) 0.0462(12) Uani 1 1 d . . . F20B F 0.24999(15) 0.6669(5) 0.18735(16) 0.0516(13) Uani 1 1 d . . . F20C F 0.29878(16) 0.5489(4) 0.21984(14) 0.0465(12) Uani 1 1 d . . . C21 C 0.2987(3) 0.8308(7) 0.1665(2) 0.039(2) Uani 1 1 d . . . F21A F 0.27004(17) 0.8866(4) 0.17310(16) 0.0582(15) Uani 1 1 d . . . F21B F 0.32539(17) 0.9014(4) 0.16250(15) 0.0521(13) Uani 1 1 d . . . F21C F 0.27601(17) 0.7848(4) 0.12988(14) 0.0527(14) Uani 1 1 d . . . C22 C 0.3732(2) 0.2853(6) 0.1577(2) 0.0276(16) Uani 1 1 d . . . H22A H 0.3421 0.2945 0.1397 0.033 Uiso 1 1 calc R . . H22B H 0.3770 0.2188 0.1736 0.033 Uiso 1 1 calc R . . C23 C 0.3792(3) 0.1293(6) 0.1067(3) 0.0353(19) Uani 1 1 d . . . F23A F 0.39892(17) 0.0855(4) 0.08653(16) 0.0517(14) Uani 1 1 d . . . F23B F 0.38286(19) 0.0565(4) 0.13466(16) 0.0547(14) Uani 1 1 d . . . F23C F 0.33743(15) 0.1366(4) 0.08042(17) 0.0534(14) Uani 1 1 d . . . C24 C 0.4556(3) 0.2191(7) 0.1657(3) 0.039(2) Uani 1 1 d . . . F24A F 0.45512(15) 0.1553(4) 0.19448(14) 0.0461(12) Uani 1 1 d . . . F24B F 0.47467(15) 0.1609(4) 0.14773(15) 0.0478(13) Uani 1 1 d . . . F24C F 0.48114(14) 0.3017(4) 0.18392(14) 0.0413(12) Uani 1 1 d . . . C27 C 0.3401(3) 0.6332(6) 0.0510(2) 0.0333(18) Uani 1 1 d . . . C28 C 0.3118(3) 0.6994(6) 0.0191(3) 0.050(3) Uani 1 1 d . . . H28A H 0.2921 0.6686 -0.0059 0.060 Uiso 1 1 calc R . . C29 C 0.3131(4) 0.8094(7) 0.0247(4) 0.072(4) Uani 1 1 d . . . H29A H 0.2949 0.8547 0.0031 0.087 Uiso 1 1 calc R . . C30 C 0.3408(3) 0.8546(7) 0.0616(3) 0.061(3) Uani 1 1 d . . . H30A H 0.3404 0.9303 0.0654 0.073 Uiso 1 1 calc R . . C31 C 0.3692(3) 0.7894(6) 0.0933(3) 0.046(2) Uani 1 1 d . . . H31A H 0.3888 0.8205 0.1182 0.055 Uiso 1 1 calc R . . C32 C 0.3683(3) 0.6793(6) 0.0876(3) 0.0370(19) Uani 1 1 d . . . H32A H 0.3872 0.6344 0.1091 0.044 Uiso 1 1 calc R . . C33 C 0.3110(2) 0.4718(6) -0.0101(2) 0.0270(16) Uani 1 1 d . . . C34 C 0.3368(3) 0.4608(8) -0.0288(2) 0.043(2) Uani 1 1 d . . . H34A H 0.3672 0.4585 -0.0130 0.051 Uiso 1 1 calc R . . C35 C 0.3189(3) 0.4531(8) -0.0700(2) 0.050(2) Uani 1 1 d . . . H35A H 0.3372 0.4463 -0.0823 0.060 Uiso 1 1 calc R . . C36 C 0.2749(3) 0.4552(7) -0.0939(2) 0.042(2) Uani 1 1 d . . . H36A H 0.2628 0.4478 -0.1223 0.051 Uiso 1 1 calc R . . C37 C 0.2493(3) 0.4679(6) -0.0761(2) 0.0365(19) Uani 1 1 d . . . H37A H 0.2190 0.4725 -0.0921 0.044 Uiso 1 1 calc R . . C38 C 0.2672(2) 0.4745(6) -0.0339(2) 0.0303(17) Uani 1 1 d . . . H38A H 0.2488 0.4809 -0.0217 0.036 Uiso 1 1 calc R . . C39 C 0.2904(2) 0.4551(6) 0.0542(2) 0.0274(16) Uani 1 1 d . . . C40 C 0.2739(3) 0.3496(7) 0.0463(2) 0.0386(19) Uani 1 1 d . . . H40A H 0.2887 0.2950 0.0398 0.046 Uiso 1 1 calc R . . C41 C 0.2362(3) 0.3250(7) 0.0480(3) 0.039(2) Uani 1 1 d . . . H41A H 0.2246 0.2544 0.0414 0.047 Uiso 1 1 calc R . . C42 C 0.2156(3) 0.4011(8) 0.0592(3) 0.048(2) Uani 1 1 d . . . H42A H 0.1901 0.3831 0.0607 0.057 Uiso 1 1 calc R . . C43 C 0.2324(3) 0.5068(8) 0.0685(3) 0.045(2) Uani 1 1 d . . . H43A H 0.2187 0.5603 0.0767 0.053 Uiso 1 1 calc R . . C44 C 0.2691(2) 0.5300(7) 0.0656(2) 0.0351(18) Uani 1 1 d . . . H44A H 0.2804 0.6011 0.0717 0.042 Uiso 1 1 calc R . . C45 C 0.7093(2) 0.7368(6) 0.1861(2) 0.0284(16) Uani 1 1 d . . . C46 C 0.7448(3) 0.7261(8) 0.2239(3) 0.046(2) Uani 1 1 d . . . H46A H 0.7410 0.7036 0.2463 0.055 Uiso 1 1 calc R . . C47 C 0.7859(3) 0.7483(9) 0.2290(3) 0.053(3) Uani 1 1 d . . . H47A H 0.8102 0.7409 0.2547 0.063 Uiso 1 1 calc R . . C48 C 0.7911(3) 0.7815(8) 0.1961(3) 0.050(2) Uani 1 1 d . . . H48A H 0.8192 0.7964 0.1995 0.060 Uiso 1 1 calc R . . C49 C 0.7575(3) 0.7928(9) 0.1602(3) 0.063(3) Uani 1 1 d . . . H49A H 0.7619 0.8152 0.1381 0.075 Uiso 1 1 calc R . . C50 C 0.7154(3) 0.7720(9) 0.1541(3) 0.055(3) Uani 1 1 d . . . H50A H 0.6916 0.7821 0.1283 0.066 Uiso 1 1 calc R . . C51 C 0.6202(3) 0.7440(6) 0.1296(2) 0.0303(17) Uani 1 1 d . . . C52 C 0.6003(3) 0.6680(7) 0.0997(2) 0.0372(19) Uani 1 1 d . . . H52A H 0.6033 0.5936 0.1064 0.045 Uiso 1 1 calc R . . C53 C 0.5757(3) 0.6996(8) 0.0600(3) 0.047(2) Uani 1 1 d . . . H53A H 0.5623 0.6469 0.0395 0.057 Uiso 1 1 calc R . . C54 C 0.5710(4) 0.8046(9) 0.0505(3) 0.062(3) Uani 1 1 d . . . H54A H 0.5542 0.8258 0.0232 0.074 Uiso 1 1 calc R . . C55 C 0.5899(4) 0.8815(8) 0.0793(3) 0.065(3) Uani 1 1 d . . . H55A H 0.5863 0.9556 0.0721 0.078 Uiso 1 1 calc R . . C56 C 0.6141(3) 0.8515(7) 0.1186(3) 0.048(2) Uani 1 1 d . . . H56A H 0.6269 0.9055 0.1386 0.058 Uiso 1 1 calc R . . C57 C 0.6531(2) 0.5641(6) 0.1816(2) 0.0291(17) Uani 1 1 d . . . C58 C 0.6782(3) 0.5007(7) 0.1703(3) 0.047(2) Uani 1 1 d . . . H58A H 0.6996 0.5336 0.1652 0.056 Uiso 1 1 calc R . . C59 C 0.6725(3) 0.3917(6) 0.1663(3) 0.051(3) Uani 1 1 d . . . H59A H 0.6909 0.3493 0.1597 0.061 Uiso 1 1 calc R . . C60 C 0.6402(3) 0.3426(7) 0.1719(3) 0.051(2) Uani 1 1 d . . . H60A H 0.6352 0.2675 0.1672 0.062 Uiso 1 1 calc R . . C61 C 0.6159(3) 0.4014(6) 0.1841(3) 0.040(2) Uani 1 1 d . . . H61A H 0.5947 0.3674 0.1893 0.048 Uiso 1 1 calc R . . C62 C 0.6223(2) 0.5135(6) 0.1889(2) 0.0325(18) Uani 1 1 d . . . H62A H 0.6051 0.5551 0.1972 0.039 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 0.01857(15) 0.02263(15) 0.02194(15) -0.00244(11) 0.00680(11) -0.00139(11) P1 0.0220(9) 0.0297(10) 0.0216(9) -0.0030(8) 0.0085(8) -0.0035(8) P2 0.0218(9) 0.0227(9) 0.0289(10) -0.0004(8) 0.0105(8) -0.0005(8) P3 0.0225(9) 0.0234(9) 0.0239(10) -0.0020(8) 0.0084(8) 0.0022(8) C25 0.020(4) 0.034(4) 0.030(4) -0.009(3) 0.008(3) -0.004(3) O1 0.050(4) 0.045(4) 0.041(4) -0.021(3) 0.018(3) -0.007(3) Ir2 0.02263(15) 0.02136(15) 0.02379(16) 0.00013(11) 0.01147(12) -0.00184(11) P4 0.0218(9) 0.0298(10) 0.0210(9) 0.0002(8) 0.0088(8) 0.0025(8) P5 0.0277(10) 0.0249(10) 0.0263(10) 0.0008(8) 0.0153(8) -0.0008(8) P6 0.0216(9) 0.0207(9) 0.0297(10) -0.0012(8) 0.0103(8) -0.0018(8) C26 0.035(4) 0.028(4) 0.035(4) -0.002(3) 0.019(4) 0.000(4) O2 0.038(3) 0.044(4) 0.066(4) -0.003(3) 0.026(3) -0.018(3) C1 0.012(3) 0.040(4) 0.025(4) 0.000(3) 0.008(3) -0.002(3) C2 0.020(4) 0.031(4) 0.029(4) -0.001(3) 0.005(3) -0.001(3) C3 0.023(4) 0.043(5) 0.040(5) -0.016(4) 0.012(4) -0.004(4) C4 0.024(4) 0.056(5) 0.033(4) -0.014(4) 0.015(4) -0.008(4) C5 0.023(4) 0.039(4) 0.022(4) -0.009(3) 0.006(3) -0.013(3) C6 0.024(4) 0.032(4) 0.019(4) -0.003(3) 0.007(3) -0.004(3) C7 0.023(4) 0.029(4) 0.028(4) -0.001(3) 0.010(3) -0.001(3) C8 0.033(4) 0.044(5) 0.034(5) 0.008(4) 0.013(4) -0.009(4) F8A 0.056(3) 0.074(4) 0.029(3) 0.004(2) 0.015(2) -0.014(3) F8B 0.063(4) 0.046(3) 0.073(4) 0.022(3) 0.041(3) 0.005(3) F8C 0.044(3) 0.066(4) 0.047(3) 0.008(3) 0.019(3) -0.023(3) C9 0.028(4) 0.051(5) 0.038(5) -0.013(4) 0.018(4) -0.004(4) F9A 0.049(3) 0.052(3) 0.058(3) 0.002(3) 0.025(3) 0.018(3) F9B 0.048(3) 0.074(4) 0.046(3) -0.030(3) 0.021(3) -0.005(3) F9C 0.041(3) 0.075(4) 0.069(4) -0.019(3) 0.038(3) -0.008(3) C10 0.028(4) 0.028(4) 0.030(4) 0.004(3) 0.011(3) -0.001(3) C11 0.029(4) 0.033(4) 0.042(5) -0.005(4) 0.015(4) 0.003(4) F11A 0.055(3) 0.053(3) 0.050(3) 0.008(2) 0.037(3) 0.012(2) F11B 0.039(3) 0.047(3) 0.053(3) -0.004(2) 0.024(2) 0.013(2) F11C 0.040(3) 0.064(3) 0.051(3) -0.029(3) 0.017(2) -0.004(3) C12 0.033(4) 0.021(4) 0.047(5) 0.005(4) 0.013(4) 0.000(3) F12A 0.050(3) 0.029(3) 0.092(4) 0.015(3) 0.032(3) 0.012(2) F12B 0.046(3) 0.036(3) 0.107(5) 0.016(3) 0.010(3) -0.013(3) F12C 0.106(5) 0.033(3) 0.081(4) 0.010(3) 0.064(4) -0.005(3) C13 0.025(4) 0.035(4) 0.021(4) 0.005(3) 0.008(3) 0.004(3) C14 0.025(4) 0.030(4) 0.026(4) 0.003(3) 0.014(3) 0.000(3) C15 0.044(5) 0.036(4) 0.029(4) 0.004(3) 0.021(4) 0.010(4) C16 0.038(5) 0.045(5) 0.024(4) 0.002(4) 0.012(4) 0.015(4) C17 0.025(4) 0.046(5) 0.024(4) -0.011(3) 0.010(3) 0.003(4) C18 0.021(4) 0.034(4) 0.026(4) 0.001(3) 0.015(3) 0.003(3) C19 0.030(4) 0.035(4) 0.024(4) 0.002(3) 0.014(3) 0.006(3) C20 0.033(4) 0.046(5) 0.030(4) -0.017(4) 0.015(4) -0.009(4) F20A 0.041(3) 0.060(3) 0.037(3) -0.018(2) 0.017(2) -0.009(2) F20B 0.031(3) 0.071(4) 0.056(3) -0.021(3) 0.023(3) -0.007(3) F20C 0.058(3) 0.041(3) 0.036(3) -0.004(2) 0.018(2) -0.017(2) C21 0.040(5) 0.045(5) 0.027(4) 0.007(4) 0.013(4) 0.016(4) F21A 0.053(3) 0.073(4) 0.045(3) 0.016(3) 0.019(3) 0.039(3) F21B 0.059(3) 0.048(3) 0.045(3) 0.017(2) 0.021(3) 0.005(3) F21C 0.058(3) 0.060(3) 0.025(3) 0.002(2) 0.006(2) 0.009(3) C22 0.029(4) 0.024(4) 0.036(4) 0.006(3) 0.020(3) 0.002(3) C23 0.033(4) 0.032(4) 0.040(5) -0.005(4) 0.016(4) -0.003(4) F23A 0.060(3) 0.034(3) 0.077(4) -0.023(3) 0.044(3) -0.011(2) F23B 0.090(4) 0.025(3) 0.057(3) -0.001(2) 0.040(3) -0.012(3) F23C 0.034(3) 0.036(3) 0.074(4) -0.009(3) 0.011(3) -0.011(2) C24 0.043(5) 0.032(4) 0.042(5) -0.001(4) 0.020(4) -0.003(4) F24A 0.045(3) 0.048(3) 0.045(3) 0.026(2) 0.021(2) 0.015(2) F24B 0.035(3) 0.059(3) 0.053(3) 0.010(3) 0.023(2) 0.020(2) F24C 0.028(2) 0.043(3) 0.035(3) 0.005(2) -0.001(2) -0.005(2) C27 0.033(4) 0.019(4) 0.037(5) -0.001(3) 0.007(4) 0.004(3) C28 0.057(6) 0.022(4) 0.041(5) -0.003(4) -0.004(4) 0.003(4) C29 0.075(8) 0.024(5) 0.072(8) 0.005(5) -0.005(6) 0.010(5) C30 0.059(7) 0.024(5) 0.076(8) -0.010(5) 0.011(6) 0.001(5) C31 0.049(5) 0.028(4) 0.050(6) -0.014(4) 0.013(5) -0.008(4) C32 0.043(5) 0.029(4) 0.035(5) -0.003(3) 0.015(4) -0.001(4) C33 0.029(4) 0.021(4) 0.025(4) 0.002(3) 0.007(3) 0.006(3) C34 0.032(4) 0.066(6) 0.031(5) 0.014(4) 0.016(4) 0.012(4) C35 0.040(5) 0.089(7) 0.024(4) 0.005(4) 0.017(4) 0.013(5) C36 0.045(5) 0.057(6) 0.020(4) 0.004(4) 0.010(4) 0.007(4) C37 0.037(4) 0.034(4) 0.027(4) 0.003(3) 0.005(4) 0.001(4) C38 0.025(4) 0.036(4) 0.026(4) 0.004(3) 0.008(3) -0.001(3) C39 0.019(4) 0.030(4) 0.028(4) 0.000(3) 0.007(3) 0.005(3) C40 0.039(5) 0.040(5) 0.038(5) 0.005(4) 0.019(4) 0.000(4) C41 0.037(5) 0.035(5) 0.047(5) 0.002(4) 0.020(4) -0.009(4) C42 0.029(4) 0.079(7) 0.037(5) 0.016(5) 0.017(4) -0.001(5) C43 0.029(4) 0.064(6) 0.041(5) -0.009(4) 0.016(4) 0.007(4) C44 0.027(4) 0.041(5) 0.030(4) -0.010(4) 0.007(3) 0.001(4) C45 0.037(4) 0.023(4) 0.032(4) -0.004(3) 0.022(4) -0.004(3) C46 0.028(4) 0.077(7) 0.039(5) 0.026(5) 0.021(4) 0.019(4) C47 0.035(5) 0.077(7) 0.047(6) 0.012(5) 0.020(4) 0.018(5) C48 0.035(5) 0.060(6) 0.063(7) -0.009(5) 0.030(5) -0.013(5) C49 0.045(6) 0.103(9) 0.046(6) 0.015(6) 0.026(5) -0.023(6) C50 0.050(6) 0.084(7) 0.025(5) 0.001(5) 0.012(4) -0.023(5) C51 0.036(4) 0.032(4) 0.031(4) 0.003(3) 0.023(4) 0.003(3) C52 0.038(5) 0.041(5) 0.036(5) -0.003(4) 0.020(4) -0.004(4) C53 0.039(5) 0.067(7) 0.034(5) -0.001(4) 0.015(4) -0.008(5) C54 0.078(8) 0.075(8) 0.032(5) 0.012(5) 0.026(5) 0.020(6) C55 0.107(9) 0.052(6) 0.035(6) 0.012(5) 0.033(6) 0.024(6) C56 0.074(7) 0.041(5) 0.026(5) 0.010(4) 0.020(5) 0.007(5) C57 0.029(4) 0.031(4) 0.022(4) 0.004(3) 0.008(3) 0.003(3) C58 0.055(6) 0.032(5) 0.070(6) -0.001(4) 0.043(5) 0.000(4) C59 0.071(7) 0.018(4) 0.088(7) -0.003(4) 0.058(6) 0.005(4) C60 0.065(6) 0.030(5) 0.069(7) 0.000(5) 0.040(6) -0.001(5) C61 0.028(4) 0.033(4) 0.062(6) 0.001(4) 0.022(4) -0.006(4) C62 0.026(4) 0.036(4) 0.039(5) -0.001(4) 0.018(4) -0.005(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 C25 1.920(8) . ? Ir1 P2 2.222(2) . ? Ir1 P1 2.241(2) . ? Ir1 P3 2.331(2) . ? P1 C7 1.851(7) . ? P1 C8 1.882(8) . ? P1 C9 1.902(8) . ? P2 C22 1.842(7) . ? P2 C23 1.884(8) . ? P2 C24 1.901(9) . ? P3 C33 1.829(7) . ? P3 C39 1.833(8) . ? P3 C27 1.839(7) . ? C25 O1 1.137(9) . ? Ir2 C26 1.935(8) . ? Ir2 P6 2.228(2) . ? Ir2 P4 2.246(2) 2_655 ? Ir2 P5 2.326(2) . ? P4 C19 1.850(7) . ? P4 C20 1.876(8) . ? P4 C21 1.878(8) . ? P4 Ir2 2.246(2) 2_655 ? P5 C45 1.828(8) . ? P5 C57 1.829(8) . ? P5 C51 1.830(8) . ? P6 C10 1.856(8) . ? P6 C12 1.885(8) . ? P6 C11 1.909(8) . ? C26 O2 1.133(9) . ? C1 C6 1.386(10) . ? C1 C2 1.409(10) . ? C1 H1A 0.9500 . ? C2 C3 1.366(11) . ? C2 C10 1.494(10) . ? C3 C4 1.388(11) . ? C3 H3A 0.9500 . ? C4 C5 1.356(11) . ? C4 H4A 0.9500 . ? C5 C6 1.387(10) . ? C5 H5A 0.9500 . ? C6 C7 1.515(10) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 F8B 1.314(10) . ? C8 F8C 1.342(9) . ? C8 F8A 1.359(9) . ? C9 F9B 1.313(9) . ? C9 F9A 1.338(10) . ? C9 F9C 1.345(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 F11C 1.323(9) . ? C11 F11B 1.334(9) . ? C11 F11A 1.346(9) . ? C12 F12C 1.317(10) . ? C12 F12B 1.328(9) . ? C12 F12A 1.337(9) . ? C13 C18 1.347(10) . ? C13 C14 1.410(10) . ? C13 H13A 0.9500 . ? C14 C15 1.369(10) . ? C14 C22 1.530(10) . ? C15 C16 1.402(11) . ? C15 H15A 0.9500 . ? C16 C17 1.370(11) . ? C16 H16A 0.9500 . ? C17 C18 1.417(10) . ? C17 H17A 0.9500 . ? C18 C19 1.499(10) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 F20C 1.334(10) . ? C20 F20B 1.342(9) . ? C20 F20A 1.361(9) . ? C21 F21A 1.333(9) . ? C21 F21B 1.341(10) . ? C21 F21C 1.353(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 F23C 1.339(9) . ? C23 F23B 1.345(9) . ? C23 F23A 1.349(9) . ? C24 F24C 1.324(9) . ? C24 F24A 1.344(9) . ? C24 F24B 1.356(10) . ? C27 C32 1.390(11) . ? C27 C28 1.411(11) . ? C28 C29 1.379(12) . ? C28 H28A 0.9500 . ? C29 C30 1.387(14) . ? C29 H29A 0.9500 . ? C30 C31 1.402(13) . ? C30 H30A 0.9500 . ? C31 C32 1.381(11) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C38 1.375(10) . ? C33 C34 1.382(11) . ? C34 C35 1.374(11) . ? C34 H34A 0.9500 . ? C35 C36 1.383(12) . ? C35 H35A 0.9500 . ? C36 C37 1.354(11) . ? C36 H36A 0.9500 . ? C37 C38 1.407(10) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C44 1.378(10) . ? C39 C40 1.406(11) . ? C40 C41 1.388(11) . ? C40 H40A 0.9500 . ? C41 C42 1.367(12) . ? C41 H41A 0.9500 . ? C42 C43 1.413(13) . ? C42 H42A 0.9500 . ? C43 C44 1.371(11) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 C50 1.385(11) . ? C45 C46 1.394(11) . ? C46 C47 1.392(12) . ? C46 H46A 0.9500 . ? C47 C48 1.388(13) . ? C47 H47A 0.9500 . ? C48 C49 1.325(13) . ? C48 H48A 0.9500 . ? C49 C50 1.408(13) . ? C49 H49A 0.9500 . ? C50 H50A 0.9500 . ? C51 C52 1.382(11) . ? C51 C56 1.384(11) . ? C52 C53 1.389(12) . ? C52 H52A 0.9500 . ? C53 C54 1.341(14) . ? C53 H53A 0.9500 . ? C54 C55 1.361(15) . ? C54 H54A 0.9500 . ? C55 C56 1.367(12) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C62 1.378(10) . ? C57 C58 1.386(11) . ? C58 C59 1.365(11) . ? C58 H58A 0.9500 . ? C59 C60 1.385(13) . ? C59 H59A 0.9500 . ? C60 C61 1.351(13) . ? C60 H60A 0.9500 . ? C61 C62 1.408(11) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? 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 C25 Ir1 P2 97.0(2) . . ? C25 Ir1 P1 98.7(2) . . ? P2 Ir1 P1 118.71(7) . . ? C25 Ir1 P3 94.1(2) . . ? P2 Ir1 P3 119.26(7) . . ? P1 Ir1 P3 118.09(7) . . ? C25 Ir1 Ir2 130.3(2) . . ? P2 Ir1 Ir2 102.40(5) . . ? P1 Ir1 Ir2 32.27(5) . . ? P3 Ir1 Ir2 114.31(5) . . ? C25 Ir1 Ir2 159.2(2) . 2_655 ? P2 Ir1 Ir2 75.67(5) . 2_655 ? P1 Ir1 Ir2 101.86(5) . 2_655 ? P3 Ir1 Ir2 73.52(5) . 2_655 ? Ir2 Ir1 Ir2 70.553(5) . 2_655 ? C25 Ir1 Ir1 135.8(2) . 2_655 ? P2 Ir1 Ir1 50.39(5) . 2_655 ? P1 Ir1 Ir1 79.03(5) . 2_655 ? P3 Ir1 Ir1 126.20(5) . 2_655 ? Ir2 Ir1 Ir1 53.349(3) . 2_655 ? Ir2 Ir1 Ir1 52.722(5) 2_655 2_655 ? C7 P1 C8 99.1(4) . . ? C7 P1 C9 95.6(3) . . ? C8 P1 C9 96.5(4) . . ? C7 P1 Ir1 125.6(2) . . ? C8 P1 Ir1 118.9(3) . . ? C9 P1 Ir1 115.3(3) . . ? C22 P2 C23 97.2(3) . . ? C22 P2 C24 100.6(4) . . ? C23 P2 C24 95.3(4) . . ? C22 P2 Ir1 124.4(2) . . ? C23 P2 Ir1 116.0(3) . . ? C24 P2 Ir1 117.9(3) . . ? C33 P3 C39 100.9(3) . . ? C33 P3 C27 102.1(3) . . ? C39 P3 C27 101.9(4) . . ? C33 P3 Ir1 116.0(2) . . ? C39 P3 Ir1 116.5(2) . . ? C27 P3 Ir1 117.0(3) . . ? O1 C25 Ir1 178.5(7) . . ? C26 Ir2 P6 97.9(2) . . ? C26 Ir2 P4 98.4(2) . 2_655 ? P6 Ir2 P4 119.14(7) . 2_655 ? C26 Ir2 P5 92.5(2) . . ? P6 Ir2 P5 119.71(7) . . ? P4 Ir2 P5 117.59(7) 2_655 . ? C26 Ir2 Ir1 158.2(2) . . ? P6 Ir2 Ir1 75.66(5) . . ? P4 Ir2 Ir1 102.93(5) 2_655 . ? P5 Ir2 Ir1 73.58(5) . . ? C26 Ir2 Ir1 127.9(2) . 2_655 ? P6 Ir2 Ir1 102.12(5) . 2_655 ? P4 Ir2 Ir1 30.58(5) 2_655 2_655 ? P5 Ir2 Ir1 116.85(5) . 2_655 ? Ir1 Ir2 Ir1 73.929(6) . 2_655 ? C26 Ir2 Ir2 135.0(2) . 2_655 ? P6 Ir2 Ir2 49.24(5) . 2_655 ? P4 Ir2 Ir2 79.58(5) 2_655 2_655 ? P5 Ir2 Ir2 128.58(5) . 2_655 ? Ir1 Ir2 Ir2 55.057(5) . 2_655 ? Ir1 Ir2 Ir2 54.390(3) 2_655 2_655 ? C19 P4 C20 98.8(4) . . ? C19 P4 C21 95.8(4) . . ? C20 P4 C21 96.5(4) . . ? C19 P4 Ir2 126.0(3) . 2_655 ? C20 P4 Ir2 119.5(3) . 2_655 ? C21 P4 Ir2 114.3(3) . 2_655 ? C45 P5 C57 103.0(3) . . ? C45 P5 C51 102.4(3) . . ? C57 P5 C51 101.5(3) . . ? C45 P5 Ir2 113.7(2) . . ? C57 P5 Ir2 118.4(2) . . ? C51 P5 Ir2 115.7(2) . . ? C10 P6 C12 97.2(3) . . ? C10 P6 C11 101.1(4) . . ? C12 P6 C11 94.3(4) . . ? C10 P6 Ir2 123.1(3) . . ? C12 P6 Ir2 118.3(3) . . ? C11 P6 Ir2 117.3(3) . . ? O2 C26 Ir2 178.0(7) . . ? C6 C1 C2 121.0(7) . . ? C6 C1 H1A 119.5 . . ? C2 C1 H1A 119.5 . . ? C3 C2 C1 118.0(7) . . ? C3 C2 C10 121.4(7) . . ? C1 C2 C10 120.6(7) . . ? C2 C3 C4 120.8(7) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 121.0(7) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 120.1(7) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C1 C6 C5 119.0(7) . . ? C1 C6 C7 119.3(6) . . ? C5 C6 C7 121.7(7) . . ? C6 C7 P1 118.0(5) . . ? C6 C7 H7A 107.8 . . ? P1 C7 H7A 107.8 . . ? C6 C7 H7B 107.8 . . ? P1 C7 H7B 107.8 . . ? H7A C7 H7B 107.1 . . ? F8B C8 F8C 107.2(7) . . ? F8B C8 F8A 107.3(7) . . ? F8C C8 F8A 105.7(7) . . ? F8B C8 P1 110.2(6) . . ? F8C C8 P1 115.8(6) . . ? F8A C8 P1 110.4(6) . . ? F9B C9 F9A 108.2(7) . . ? F9B C9 F9C 106.3(7) . . ? F9A C9 F9C 106.5(7) . . ? F9B C9 P1 112.7(6) . . ? F9A C9 P1 108.7(5) . . ? F9C C9 P1 114.0(6) . . ? C2 C10 P6 114.2(5) . . ? C2 C10 H10A 108.7 . . ? P6 C10 H10A 108.7 . . ? C2 C10 H10B 108.7 . . ? P6 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? F11C C11 F11B 106.5(6) . . ? F11C C11 F11A 107.2(7) . . ? F11B C11 F11A 106.0(6) . . ? F11C C11 P6 110.9(5) . . ? F11B C11 P6 115.6(6) . . ? F11A C11 P6 110.2(5) . . ? F12C C12 F12B 108.4(7) . . ? F12C C12 F12A 105.3(7) . . ? F12B C12 F12A 105.5(7) . . ? F12C C12 P6 110.5(5) . . ? F12B C12 P6 111.6(6) . . ? F12A C12 P6 115.1(6) . . ? C18 C13 C14 122.1(7) . . ? C18 C13 H13A 119.0 . . ? C14 C13 H13A 119.0 . . ? C15 C14 C13 119.1(7) . . ? C15 C14 C22 120.6(7) . . ? C13 C14 C22 120.4(6) . . ? C14 C15 C16 119.7(7) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 120.5(7) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 120.0(7) . . ? C16 C17 H17A 120.0 . . ? C18 C17 H17A 120.0 . . ? C13 C18 C17 118.6(7) . . ? C13 C18 C19 120.8(7) . . ? C17 C18 C19 120.5(7) . . ? C18 C19 P4 118.2(5) . . ? C18 C19 H19A 107.8 . . ? P4 C19 H19A 107.8 . . ? C18 C19 H19B 107.8 . . ? P4 C19 H19B 107.8 . . ? H19A C19 H19B 107.1 . . ? F20C C20 F20B 107.0(7) . . ? F20C C20 F20A 106.2(6) . . ? F20B C20 F20A 105.0(6) . . ? F20C C20 P4 111.0(5) . . ? F20B C20 P4 111.7(6) . . ? F20A C20 P4 115.4(6) . . ? F21A C21 F21B 107.8(7) . . ? F21A C21 F21C 105.5(6) . . ? F21B C21 F21C 106.0(7) . . ? F21A C21 P4 112.6(6) . . ? F21B C21 P4 109.8(6) . . ? F21C C21 P4 114.6(6) . . ? C14 C22 P2 114.2(5) . . ? C14 C22 H22A 108.7 . . ? P2 C22 H22A 108.7 . . ? C14 C22 H22B 108.7 . . ? P2 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? F23C C23 F23B 107.1(7) . . ? F23C C23 F23A 106.7(7) . . ? F23B C23 F23A 106.0(6) . . ? F23C C23 P2 109.3(5) . . ? F23B C23 P2 115.5(6) . . ? F23A C23 P2 111.8(5) . . ? F24C C24 F24A 107.4(7) . . ? F24C C24 F24B 107.2(7) . . ? F24A C24 F24B 106.0(6) . . ? F24C C24 P2 110.8(5) . . ? F24A C24 P2 115.2(6) . . ? F24B C24 P2 109.9(6) . . ? C32 C27 C28 119.8(7) . . ? C32 C27 P3 120.9(6) . . ? C28 C27 P3 119.1(6) . . ? C29 C28 C27 119.1(8) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? C28 C29 C30 120.7(9) . . ? C28 C29 H29A 119.6 . . ? C30 C29 H29A 119.6 . . ? C29 C30 C31 120.4(8) . . ? C29 C30 H30A 119.8 . . ? C31 C30 H30A 119.8 . . ? C32 C31 C30 119.0(8) . . ? C32 C31 H31A 120.5 . . ? C30 C31 H31A 120.5 . . ? C31 C32 C27 120.9(8) . . ? C31 C32 H32A 119.5 . . ? C27 C32 H32A 119.5 . . ? C38 C33 C34 118.2(7) . . ? C38 C33 P3 122.4(6) . . ? C34 C33 P3 119.3(6) . . ? C35 C34 C33 120.5(8) . . ? C35 C34 H34A 119.7 . . ? C33 C34 H34A 119.7 . . ? C34 C35 C36 121.3(8) . . ? C34 C35 H35A 119.3 . . ? C36 C35 H35A 119.3 . . ? C37 C36 C35 118.7(7) . . ? C37 C36 H36A 120.7 . . ? C35 C36 H36A 120.7 . . ? C36 C37 C38 120.5(8) . . ? C36 C37 H37A 119.8 . . ? C38 C37 H37A 119.8 . . ? C33 C38 C37 120.7(7) . . ? C33 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C44 C39 C40 117.7(7) . . ? C44 C39 P3 124.4(6) . . ? C40 C39 P3 117.7(6) . . ? C41 C40 C39 120.2(8) . . ? C41 C40 H40A 119.9 . . ? C39 C40 H40A 119.9 . . ? C42 C41 C40 120.8(8) . . ? C42 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? C41 C42 C43 119.8(8) . . ? C41 C42 H42A 120.1 . . ? C43 C42 H42A 120.1 . . ? C44 C43 C42 118.3(8) . . ? C44 C43 H43A 120.8 . . ? C42 C43 H43A 120.8 . . ? C43 C44 C39 123.0(8) . . ? C43 C44 H44A 118.5 . . ? C39 C44 H44A 118.5 . . ? C50 C45 C46 119.0(8) . . ? C50 C45 P5 123.3(7) . . ? C46 C45 P5 117.6(6) . . ? C47 C46 C45 120.3(8) . . ? C47 C46 H46A 119.8 . . ? C45 C46 H46A 119.8 . . ? C48 C47 C46 119.3(9) . . ? C48 C47 H47A 120.4 . . ? C46 C47 H47A 120.4 . . ? C49 C48 C47 120.9(9) . . ? C49 C48 H48A 119.6 . . ? C47 C48 H48A 119.6 . . ? C48 C49 C50 121.3(9) . . ? C48 C49 H49A 119.4 . . ? C50 C49 H49A 119.4 . . ? C45 C50 C49 119.3(9) . . ? C45 C50 H50A 120.4 . . ? C49 C50 H50A 120.4 . . ? C52 C51 C56 117.7(8) . . ? C52 C51 P5 124.1(6) . . ? C56 C51 P5 118.1(6) . . ? C51 C52 C53 120.5(8) . . ? C51 C52 H52A 119.8 . . ? C53 C52 H52A 119.8 . . ? C54 C53 C52 119.8(9) . . ? C54 C53 H53A 120.1 . . ? C52 C53 H53A 120.1 . . ? C53 C54 C55 121.1(9) . . ? C53 C54 H54A 119.5 . . ? C55 C54 H54A 119.5 . . ? C54 C55 C56 119.7(10) . . ? C54 C55 H55A 120.1 . . ? C56 C55 H55A 120.1 . . ? C55 C56 C51 121.2(9) . . ? C55 C56 H56A 119.4 . . ? C51 C56 H56A 119.4 . . ? C62 C57 C58 117.9(7) . . ? C62 C57 P5 119.9(6) . . ? C58 C57 P5 121.9(6) . . ? C59 C58 C57 121.0(8) . . ? C59 C58 H58A 119.5 . . ? C57 C58 H58A 119.5 . . ? C58 C59 C60 120.5(8) . . ? C58 C59 H59A 119.8 . . ? C60 C59 H59A 119.8 . . ? C61 C60 C59 120.1(8) . . ? C61 C60 H60A 120.0 . . ? C59 C60 H60A 120.0 . . ? C60 C61 C62 119.2(8) . . ? C60 C61 H61A 120.4 . . ? C62 C61 H61A 120.4 . . ? C57 C62 C61 121.2(8) . . ? C57 C62 H62A 119.4 . . ? C61 C62 H62A 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C6 C7 P1 -105.1(7) . . . . ? C1 C10 C11 P6 93.2(5) . . . . ? C13 C14 C22 P2 91.7(7) . . . . ? C13 C18 C19 P4 111.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 4.942 _refine_diff_density_min -0.685 _refine_diff_density_rms 0.188 #####end data_jja30 _database_code_depnum_ccdc_archive 'CCDC 826942' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (CF3PCP)Ir(PPh3)(CO) _chemical_melting_point ? _chemical_formula_moiety 'C31 H22 F12 Ir O P3' _chemical_formula_sum 'C31 H22 F12 Ir O P3' _chemical_formula_weight 923.60 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7409(3) _cell_length_b 17.7775(4) _cell_length_c 16.8167(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.8670(10) _cell_angle_gamma 90.00 _cell_volume 3180.87(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9800 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 34.47 _exptl_crystal_description rectangular_prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 4.445 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3423 _exptl_absorpt_correction_T_max 0.4345 _exptl_absorpt_process_details 'SADABS (Bruker, 2001)' _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79940 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 33.14 _reflns_number_total 12064 _reflns_number_gt 10501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 2001)' _computing_cell_refinement 'Bruker SMART (Bruker, 2001)' _computing_data_reduction 'Bruker SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL V. 6.10 (Bruker, 2001)' _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^)+(0.0258P)^2^+2.4206P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12064 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.910963(6) 0.096871(3) 0.295216(3) 0.01494(2) Uani 1 1 d . . . P1 P 0.97893(5) -0.01064(3) 0.24821(3) 0.02106(8) Uani 1 1 d . . . P2 P 0.97279(4) 0.21346(3) 0.27211(3) 0.02052(8) Uani 1 1 d . . . P3 P 0.69727(4) 0.09542(2) 0.31698(2) 0.01514(7) Uani 1 1 d . . . C1 C 0.85743(17) 0.10644(11) 0.16880(10) 0.0209(3) Uani 1 1 d . . . C13 C 0.98289(18) 0.08858(11) 0.40478(11) 0.0228(3) Uani 1 1 d . . . O1 O 1.03003(17) 0.08425(11) 0.46950(10) 0.0383(4) Uani 1 1 d . . . C2 C 0.84519(18) 0.17699(12) 0.13070(11) 0.0248(4) Uani 1 1 d . . . C3 C 0.8023(2) 0.18304(15) 0.04880(12) 0.0333(5) Uani 1 1 d . . . H3A H 0.7901 0.2312 0.0246 0.040 Uiso 1 1 calc R . . C4 C 0.7774(2) 0.11889(17) 0.00277(12) 0.0382(5) Uani 1 1 d . . . H4A H 0.7449 0.1230 -0.0525 0.046 Uiso 1 1 calc R . . C5 C 0.7998(2) 0.04867(15) 0.03738(12) 0.0354(5) Uani 1 1 d . . . H5A H 0.7878 0.0048 0.0050 0.042 Uiso 1 1 calc R . . C6 C 0.84016(18) 0.04198(13) 0.11967(11) 0.0267(4) Uani 1 1 d . . . C7 C 0.8725(2) -0.03379(13) 0.15763(13) 0.0331(4) Uani 1 1 d . . . H7A H 0.9144 -0.0663 0.1215 0.040 Uiso 1 1 calc R . . H7B H 0.7964 -0.0596 0.1709 0.040 Uiso 1 1 calc R . . C8 C 0.9981(3) -0.10175(12) 0.30567(14) 0.0345(5) Uani 1 1 d . . . F8A F 0.8895(2) -0.12316(10) 0.32741(14) 0.0658(6) Uani 1 1 d . . . F8B F 1.0781(3) -0.09352(10) 0.37315(11) 0.0670(6) Uani 1 1 d . . . F8C F 1.04005(19) -0.15918(8) 0.26667(10) 0.0533(4) Uani 1 1 d . . . C9 C 1.1377(2) -0.01212(14) 0.21129(14) 0.0332(4) Uani 1 1 d . . . F9A F 1.1682(2) -0.07711(11) 0.17972(16) 0.0753(7) Uani 1 1 d . . . F9B F 1.22781(15) 0.00464(16) 0.26979(11) 0.0740(7) Uani 1 1 d . . . F9C F 1.14093(15) 0.03913(10) 0.15415(10) 0.0464(4) Uani 1 1 d . . . C10 C 0.8815(2) 0.24693(12) 0.17981(12) 0.0302(4) Uani 1 1 d . . . H10A H 0.8057 0.2742 0.1915 0.036 Uiso 1 1 calc R . . H10B H 0.9323 0.2811 0.1507 0.036 Uiso 1 1 calc R . . C11 C 1.1398(2) 0.23511(14) 0.25570(17) 0.0381(5) Uani 1 1 d . . . F11A F 1.17941(17) 0.18418(10) 0.20690(13) 0.0601(5) Uani 1 1 d . . . F11B F 1.21630(16) 0.23333(13) 0.32500(13) 0.0693(6) Uani 1 1 d . . . F11C F 1.15617(17) 0.30179(10) 0.22205(13) 0.0611(5) Uani 1 1 d . . . C12 C 0.9585(3) 0.29278(12) 0.34475(14) 0.0355(5) Uani 1 1 d . . . F12A F 1.0063(2) 0.27283(9) 0.41907(9) 0.0538(4) Uani 1 1 d . . . F12B F 1.01598(19) 0.35662(8) 0.32873(11) 0.0565(5) Uani 1 1 d . . . F12C F 0.83722(17) 0.30932(9) 0.34595(11) 0.0511(4) Uani 1 1 d . . . C14 C 0.65110(16) 0.17197(10) 0.38068(10) 0.0183(3) Uani 1 1 d . . . C15 C 0.72830(19) 0.18578(13) 0.45289(12) 0.0292(4) Uani 1 1 d . . . H15A H 0.8029 0.1571 0.4663 0.035 Uiso 1 1 calc R . . C16 C 0.6975(2) 0.24097(14) 0.50554(13) 0.0334(5) Uani 1 1 d . . . H16A H 0.7503 0.2491 0.5549 0.040 Uiso 1 1 calc R . . C17 C 0.5901(2) 0.28417(12) 0.48617(13) 0.0309(4) Uani 1 1 d . . . H17A H 0.5705 0.3232 0.5211 0.037 Uiso 1 1 calc R . . C18 C 0.5118(2) 0.26978(12) 0.41546(13) 0.0303(4) Uani 1 1 d . . . H18A H 0.4374 0.2986 0.4022 0.036 Uiso 1 1 calc R . . C19 C 0.54081(18) 0.21338(11) 0.36347(11) 0.0238(3) Uani 1 1 d . . . H19A H 0.4849 0.2031 0.3159 0.029 Uiso 1 1 calc R . . C20 C 0.59019(16) 0.10072(10) 0.22347(10) 0.0180(3) Uani 1 1 d . . . C21 C 0.54145(19) 0.03498(12) 0.18576(11) 0.0258(4) Uani 1 1 d . . . H21A H 0.5566 -0.0122 0.2119 0.031 Uiso 1 1 calc R . . C22 C 0.4707(2) 0.03833(14) 0.11007(13) 0.0335(4) Uani 1 1 d . . . H22A H 0.4373 -0.0065 0.0849 0.040 Uiso 1 1 calc R . . C23 C 0.4490(2) 0.10665(14) 0.07142(13) 0.0339(5) Uani 1 1 d . . . H23A H 0.4002 0.1087 0.0199 0.041 Uiso 1 1 calc R . . C24 C 0.4981(2) 0.17171(13) 0.10736(12) 0.0297(4) Uani 1 1 d . . . H24A H 0.4832 0.2186 0.0806 0.036 Uiso 1 1 calc R . . C25 C 0.56940(17) 0.16880(11) 0.18295(11) 0.0214(3) Uani 1 1 d . . . H25A H 0.6043 0.2138 0.2071 0.026 Uiso 1 1 calc R . . C26 C 0.63732(16) 0.01602(10) 0.36980(10) 0.0184(3) Uani 1 1 d . . . C27 C 0.50759(18) 0.00483(12) 0.36671(12) 0.0251(3) Uani 1 1 d . . . H27A H 0.4505 0.0370 0.3347 0.030 Uiso 1 1 calc R . . C28 C 0.46208(19) -0.05290(12) 0.41020(12) 0.0275(4) Uani 1 1 d . . . H28A H 0.3741 -0.0611 0.4065 0.033 Uiso 1 1 calc R . . C29 C 0.5447(2) -0.09868(11) 0.45903(13) 0.0278(4) Uani 1 1 d . . . H29A H 0.5132 -0.1379 0.4891 0.033 Uiso 1 1 calc R . . C30 C 0.6728(2) -0.08714(12) 0.46387(13) 0.0294(4) Uani 1 1 d . . . H30A H 0.7294 -0.1179 0.4980 0.035 Uiso 1 1 calc R . . C31 C 0.71898(18) -0.03029(11) 0.41871(11) 0.0241(3) Uani 1 1 d . . . H31A H 0.8071 -0.0232 0.4215 0.029 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 0.01511(3) 0.01486(3) 0.01471(3) -0.00022(2) 0.00150(2) -0.00049(2) P1 0.0221(2) 0.0178(2) 0.0236(2) -0.00423(15) 0.00438(16) 0.00067(16) P2 0.0221(2) 0.0168(2) 0.02274(19) 0.00087(15) 0.00352(16) -0.00325(16) P3 0.01519(17) 0.01499(18) 0.01493(16) 0.00103(13) 0.00099(14) 0.00002(14) C1 0.0170(7) 0.0305(9) 0.0151(6) 0.0001(6) 0.0023(6) -0.0025(6) C13 0.0206(8) 0.0237(9) 0.0236(8) 0.0011(6) 0.0010(6) 0.0024(6) O1 0.0364(9) 0.0525(11) 0.0231(7) 0.0023(6) -0.0066(6) 0.0057(7) C2 0.0214(8) 0.0342(10) 0.0192(7) 0.0058(7) 0.0042(6) -0.0019(7) C3 0.0286(9) 0.0505(13) 0.0207(8) 0.0121(8) 0.0034(7) -0.0022(9) C4 0.0283(10) 0.0693(17) 0.0164(8) 0.0026(9) 0.0015(7) -0.0069(10) C5 0.0297(10) 0.0535(14) 0.0225(9) -0.0097(9) 0.0021(8) -0.0065(10) C6 0.0228(8) 0.0353(10) 0.0217(8) -0.0062(7) 0.0020(7) -0.0041(7) C7 0.0350(11) 0.0314(11) 0.0313(10) -0.0124(8) -0.0009(8) -0.0029(8) C8 0.0512(14) 0.0194(9) 0.0349(10) -0.0025(7) 0.0136(10) 0.0049(9) F8A 0.0707(12) 0.0324(8) 0.1056(16) 0.0179(9) 0.0522(12) 0.0015(8) F8B 0.1110(18) 0.0410(10) 0.0419(9) 0.0127(7) -0.0152(10) 0.0011(9) F8C 0.0868(13) 0.0220(7) 0.0577(10) -0.0025(6) 0.0331(9) 0.0147(7) C9 0.0310(10) 0.0333(11) 0.0372(10) -0.0054(8) 0.0116(8) 0.0053(9) F9A 0.0815(14) 0.0384(9) 0.1224(19) -0.0164(11) 0.0726(14) 0.0075(9) F9B 0.0225(7) 0.147(2) 0.0512(10) -0.0031(12) 0.0010(7) 0.0025(10) F9C 0.0437(8) 0.0495(9) 0.0510(9) 0.0091(7) 0.0242(7) 0.0004(7) C10 0.0331(10) 0.0272(10) 0.0293(9) 0.0101(7) 0.0009(8) -0.0030(8) C11 0.0280(10) 0.0332(12) 0.0542(14) 0.0010(10) 0.0094(10) -0.0101(9) F11A 0.0479(9) 0.0484(10) 0.0934(14) -0.0099(9) 0.0433(10) -0.0074(8) F11B 0.0318(8) 0.0938(16) 0.0769(13) 0.0070(11) -0.0116(8) -0.0163(9) F11C 0.0509(10) 0.0389(9) 0.0990(15) 0.0120(9) 0.0297(10) -0.0177(7) C12 0.0509(13) 0.0185(9) 0.0382(11) -0.0024(8) 0.0097(10) -0.0027(9) F12A 0.0880(13) 0.0392(9) 0.0318(7) -0.0116(6) -0.0002(8) -0.0019(8) F12B 0.0849(13) 0.0198(7) 0.0683(11) -0.0069(7) 0.0229(10) -0.0151(7) F12C 0.0595(10) 0.0347(8) 0.0641(10) -0.0055(7) 0.0257(8) 0.0117(7) C14 0.0184(7) 0.0176(7) 0.0199(7) -0.0017(5) 0.0055(6) -0.0010(6) C15 0.0212(8) 0.0384(11) 0.0276(9) -0.0107(8) 0.0018(7) 0.0014(8) C16 0.0261(9) 0.0442(13) 0.0309(9) -0.0174(9) 0.0081(8) -0.0076(9) C17 0.0383(11) 0.0251(10) 0.0330(9) -0.0078(7) 0.0184(8) -0.0050(8) C18 0.0379(11) 0.0258(9) 0.0299(9) 0.0037(7) 0.0145(8) 0.0097(8) C19 0.0266(8) 0.0247(9) 0.0211(7) 0.0018(6) 0.0068(6) 0.0059(7) C20 0.0164(7) 0.0203(8) 0.0169(6) 0.0017(5) 0.0004(5) 0.0010(6) C21 0.0278(9) 0.0257(9) 0.0220(8) -0.0011(6) -0.0033(7) -0.0029(7) C22 0.0334(10) 0.0380(12) 0.0260(9) -0.0028(8) -0.0070(8) -0.0059(9) C23 0.0284(10) 0.0494(14) 0.0216(8) 0.0037(8) -0.0056(8) -0.0015(9) C24 0.0288(9) 0.0367(11) 0.0228(8) 0.0107(7) 0.0013(7) 0.0046(8) C25 0.0225(8) 0.0209(8) 0.0207(7) 0.0036(6) 0.0024(6) 0.0010(6) C26 0.0189(7) 0.0190(7) 0.0176(6) 0.0012(5) 0.0033(6) -0.0016(6) C27 0.0198(8) 0.0270(9) 0.0288(8) 0.0044(7) 0.0041(7) -0.0023(7) C28 0.0257(9) 0.0276(10) 0.0305(9) 0.0005(7) 0.0091(7) -0.0075(7) C29 0.0359(10) 0.0221(9) 0.0272(9) 0.0027(7) 0.0106(8) -0.0066(7) C30 0.0334(10) 0.0262(10) 0.0284(9) 0.0094(7) 0.0041(8) -0.0009(8) C31 0.0240(8) 0.0222(9) 0.0258(8) 0.0067(6) 0.0018(7) -0.0003(7) _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 1.9036(19) . ? Ir1 C1 2.1318(17) . ? Ir1 P2 2.2268(5) . ? Ir1 P1 2.2290(5) . ? Ir1 P3 2.3734(4) . ? P1 C7 1.822(2) . ? P1 C8 1.883(2) . ? P1 C9 1.893(2) . ? P2 C10 1.819(2) . ? P2 C12 1.885(2) . ? P2 C11 1.891(2) . ? P3 C20 1.8191(18) . ? P3 C26 1.8310(17) . ? P3 C14 1.8414(17) . ? C1 C2 1.406(3) . ? C1 C6 1.410(3) . ? C13 O1 1.138(2) . ? C2 C3 1.396(3) . ? C2 C10 1.514(3) . ? C3 C4 1.384(4) . ? C3 H3A 0.9500 . ? C4 C5 1.384(4) . ? C4 H4A 0.9500 . ? C5 C6 1.397(3) . ? C5 H5A 0.9500 . ? C6 C7 1.511(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 F8A 1.325(3) . ? C8 F8C 1.325(2) . ? C8 F8B 1.335(3) . ? C9 F9B 1.316(3) . ? C9 F9C 1.328(3) . ? C9 F9A 1.331(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 F11A 1.330(3) . ? C11 F11B 1.331(3) . ? C11 F11C 1.336(3) . ? C12 F12A 1.332(3) . ? C12 F12B 1.337(3) . ? C12 F12C 1.339(3) . ? C14 C19 1.391(3) . ? C14 C15 1.395(3) . ? C15 C16 1.391(3) . ? C15 H15A 0.9500 . ? C16 C17 1.387(3) . ? C16 H16A 0.9500 . ? C17 C18 1.383(3) . ? C17 H17A 0.9500 . ? C18 C19 1.393(3) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? C20 C25 1.392(2) . ? C20 C21 1.397(3) . ? C21 C22 1.391(3) . ? C21 H21A 0.9500 . ? C22 C23 1.382(3) . ? C22 H22A 0.9500 . ? C23 C24 1.376(3) . ? C23 H23A 0.9500 . ? C24 C25 1.392(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C31 1.388(2) . ? C26 C27 1.401(3) . ? C27 C28 1.387(3) . ? C27 H27A 0.9500 . ? C28 C29 1.387(3) . ? C28 H28A 0.9500 . ? C29 C30 1.383(3) . ? C29 H29A 0.9500 . ? C30 C31 1.396(3) . ? C30 H30A 0.9500 . ? C31 H31A 0.9500 . ? 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 171.79(7) . . ? C13 Ir1 P2 98.61(6) . . ? C1 Ir1 P2 78.34(5) . . ? C13 Ir1 P1 99.65(6) . . ? C1 Ir1 P1 76.79(5) . . ? P2 Ir1 P1 128.042(18) . . ? C13 Ir1 P3 97.06(6) . . ? C1 Ir1 P3 91.15(5) . . ? P2 Ir1 P3 110.783(16) . . ? P1 Ir1 P3 114.577(16) . . ? C7 P1 C8 104.28(11) . . ? C7 P1 C9 102.29(11) . . ? C8 P1 C9 96.68(11) . . ? C7 P1 Ir1 106.97(8) . . ? C8 P1 Ir1 125.01(7) . . ? C9 P1 Ir1 118.79(8) . . ? C10 P2 C12 103.07(11) . . ? C10 P2 C11 102.73(11) . . ? C12 P2 C11 96.04(11) . . ? C10 P2 Ir1 108.33(7) . . ? C12 P2 Ir1 122.03(7) . . ? C11 P2 Ir1 121.75(8) . . ? C20 P3 C26 103.69(8) . . ? C20 P3 C14 106.01(8) . . ? C26 P3 C14 98.45(8) . . ? C20 P3 Ir1 112.12(6) . . ? C26 P3 Ir1 119.67(6) . . ? C14 P3 Ir1 115.14(6) . . ? C2 C1 C6 117.47(17) . . ? C2 C1 Ir1 121.41(14) . . ? C6 C1 Ir1 121.02(14) . . ? O1 C13 Ir1 177.52(19) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 C10 120.05(19) . . ? C1 C2 C10 118.88(16) . . ? C4 C3 C2 120.1(2) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 119.92(19) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C4 C5 C6 120.4(2) . . ? C4 C5 H5A 119.8 . . ? C6 C5 H5A 119.8 . . ? C5 C6 C1 120.6(2) . . ? C5 C6 C7 121.10(19) . . ? C1 C6 C7 118.22(17) . . ? C6 C7 P1 103.51(14) . . ? C6 C7 H7A 111.1 . . ? P1 C7 H7A 111.1 . . ? C6 C7 H7B 111.1 . . ? P1 C7 H7B 111.1 . . ? H7A C7 H7B 109.0 . . ? F8A C8 F8C 106.7(2) . . ? F8A C8 F8B 106.6(2) . . ? F8C C8 F8B 106.4(2) . . ? F8A C8 P1 110.50(17) . . ? F8C C8 P1 115.42(16) . . ? F8B C8 P1 110.76(16) . . ? F9B C9 F9C 107.2(2) . . ? F9B C9 F9A 107.4(2) . . ? F9C C9 F9A 105.9(2) . . ? F9B C9 P1 110.79(15) . . ? F9C C9 P1 109.96(15) . . ? F9A C9 P1 115.12(18) . . ? C2 C10 P2 105.39(14) . . ? C2 C10 H10A 110.7 . . ? P2 C10 H10A 110.7 . . ? C2 C10 H10B 110.7 . . ? P2 C10 H10B 110.7 . . ? H10A C10 H10B 108.8 . . ? F11A C11 F11B 108.2(2) . . ? F11A C11 F11C 105.7(2) . . ? F11B C11 F11C 106.9(2) . . ? F11A C11 P2 109.96(16) . . ? F11B C11 P2 110.58(18) . . ? F11C C11 P2 115.15(18) . . ? F12A C12 F12B 106.6(2) . . ? F12A C12 F12C 107.2(2) . . ? F12B C12 F12C 107.1(2) . . ? F12A C12 P2 110.71(16) . . ? F12B C12 P2 115.07(17) . . ? F12C C12 P2 109.85(17) . . ? C19 C14 C15 118.39(16) . . ? C19 C14 P3 124.03(13) . . ? C15 C14 P3 117.46(14) . . ? C16 C15 C14 120.89(19) . . ? C16 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C18 C17 C16 119.21(18) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.7(2) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C14 C19 C18 120.51(18) . . ? C14 C19 H19A 119.7 . . ? C18 C19 H19A 119.7 . . ? C25 C20 C21 118.69(17) . . ? C25 C20 P3 120.55(14) . . ? C21 C20 P3 120.17(13) . . ? C22 C21 C20 120.22(19) . . ? C22 C21 H21A 119.9 . . ? C20 C21 H21A 119.9 . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 120.15(19) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C23 C24 C25 119.97(19) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C20 C25 C24 120.70(18) . . ? C20 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C31 C26 C27 118.84(16) . . ? C31 C26 P3 120.60(13) . . ? C27 C26 P3 120.35(14) . . ? C28 C27 C26 120.38(18) . . ? C28 C27 H27A 119.8 . . ? C26 C27 H27A 119.8 . . ? C29 C28 C27 120.22(19) . . ? C29 C28 H28A 119.9 . . ? C27 C28 H28A 119.9 . . ? C30 C29 C28 119.89(18) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C31 120.05(19) . . ? C29 C30 H30A 120.0 . . ? C31 C30 H30A 120.0 . . ? C26 C31 C30 120.60(18) . . ? C26 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.330 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.102 #####end