Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Jones, Cameron' 'Brym, Marcus' 'Richards, Anne F.' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry University of Wales P.O. Box 912 Park Place Cardiff CF10 3TB UNITED KINGDOM ; _publ_contact_author_email 'JONESCA6@CARDIFF.AC.UK' _publ_section_title ; Synthesis, Characterisation and Reactivity of a Novel Iridaphosphirene Complex, [Ir{C(But)P(C6H11)}(CO)(PPh3)2] ; data_compound_4 _database_code_CSD 184725 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H50 Ir O P3' _chemical_formula_weight 927.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.552(2) _cell_length_b 12.359(3) _cell_length_c 32.250(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4205.8(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 block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 3.324 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.393 _exptl_absorpt_correction_T_max 0.519 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 30060 _diffrn_reflns_av_R_equivalents 0.0949 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7325 _reflns_number_gt 6514 _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^)+(0.0527P)^2^+43.0553P] 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 0.009(13) _refine_ls_number_reflns 7325 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.37844(4) 0.40098(4) 0.862839(13) 0.02065(13) Uani 1 1 d . . . P1 P 0.3376(3) 0.4894(3) 0.92921(10) 0.0272(7) Uani 1 1 d . . . O1 O 0.5696(9) 0.3335(8) 0.7972(3) 0.036(2) Uani 1 1 d . . . C1 C 0.4715(12) 0.4995(11) 0.8973(4) 0.028(3) Uani 1 1 d . . . P2 P 0.2180(3) 0.4428(3) 0.81529(10) 0.0220(7) Uani 1 1 d . . . C2 C 0.6007(11) 0.5537(10) 0.9003(4) 0.026(3) Uani 1 1 d . . . P3 P 0.3217(3) 0.2179(3) 0.87722(9) 0.0233(7) Uani 1 1 d . . . C3 C 0.6831(12) 0.5320(12) 0.8616(5) 0.044(3) Uani 1 1 d . . . H3A H 0.6910 0.4554 0.8575 0.066 Uiso 1 1 calc R . . H3B H 0.7656 0.5631 0.8656 0.066 Uiso 1 1 calc R . . H3C H 0.6438 0.5641 0.8378 0.066 Uiso 1 1 calc R . . C4 C 0.6681(15) 0.5031(15) 0.9387(5) 0.056(5) Uani 1 1 d . . . H4A H 0.6213 0.5206 0.9634 0.085 Uiso 1 1 calc R . . H4B H 0.7524 0.5317 0.9409 0.085 Uiso 1 1 calc R . . H4C H 0.6720 0.4259 0.9356 0.085 Uiso 1 1 calc R . . C5 C 0.5852(16) 0.6724(12) 0.9060(5) 0.042(4) Uani 1 1 d . . . H5A H 0.5390 0.7018 0.8830 0.063 Uiso 1 1 calc R . . H5B H 0.6672 0.7060 0.9075 0.063 Uiso 1 1 calc R . . H5C H 0.5396 0.6861 0.9312 0.063 Uiso 1 1 calc R . . C6 C 0.2454(12) 0.6178(11) 0.9260(4) 0.029(3) Uani 1 1 d . . . H6 H 0.2608 0.6529 0.8993 0.035 Uiso 1 1 calc R . . C7 C 0.2846(15) 0.6941(14) 0.9614(5) 0.051(4) Uani 1 1 d . . . H7A H 0.3725 0.7150 0.9577 0.061 Uiso 1 1 calc R . . H7B H 0.2779 0.6559 0.9876 0.061 Uiso 1 1 calc R . . C8 C 0.2004(16) 0.7985(13) 0.9632(6) 0.054(5) Uani 1 1 d . . . H8A H 0.2289 0.8450 0.9856 0.065 Uiso 1 1 calc R . . H8B H 0.2081 0.8383 0.9374 0.065 Uiso 1 1 calc R . . C9 C 0.0641(15) 0.7671(13) 0.9701(5) 0.045(4) Uani 1 1 d . . . H9A H 0.0116 0.8315 0.9709 0.054 Uiso 1 1 calc R . . H9B H 0.0559 0.7300 0.9965 0.054 Uiso 1 1 calc R . . C10 C 0.0200(15) 0.6933(13) 0.9353(5) 0.047(4) Uani 1 1 d . . . H10A H 0.0220 0.7333 0.9094 0.056 Uiso 1 1 calc R . . H10B H -0.0673 0.6725 0.9404 0.056 Uiso 1 1 calc R . . C11 C 0.1011(14) 0.5897(15) 0.9305(5) 0.050(4) Uani 1 1 d . . . H11A H 0.0733 0.5500 0.9061 0.060 Uiso 1 1 calc R . . H11B H 0.0888 0.5436 0.9545 0.060 Uiso 1 1 calc R . . C12 C 0.4936(11) 0.3604(10) 0.8217(4) 0.023(3) Uani 1 1 d . . . C13 C 0.1846(12) 0.5869(12) 0.8169(3) 0.027(3) Uani 1 1 d . . . C14 C 0.2862(15) 0.6608(11) 0.8154(4) 0.033(3) Uani 1 1 d . . . H14 H 0.3690 0.6353 0.8138 0.040 Uiso 1 1 calc R . . C15 C 0.2635(18) 0.7711(12) 0.8163(4) 0.043(4) Uani 1 1 d . . . H15 H 0.3312 0.8192 0.8149 0.051 Uiso 1 1 calc R . . C16 C 0.141(2) 0.8105(12) 0.8190(4) 0.051(4) Uani 1 1 d . . . H16 H 0.1271 0.8847 0.8195 0.061 Uiso 1 1 calc R . . C17 C 0.0441(18) 0.7422(13) 0.8210(4) 0.050(5) Uani 1 1 d . . . H17 H -0.0376 0.7700 0.8230 0.060 Uiso 1 1 calc R . . C18 C 0.0609(16) 0.6286(11) 0.8200(4) 0.035(4) Uani 1 1 d . . . H18 H -0.0085 0.5824 0.8214 0.043 Uiso 1 1 calc R . . C19 C 0.2525(12) 0.4248(10) 0.7593(3) 0.027(3) Uani 1 1 d . . . C20 C 0.2145(12) 0.5015(12) 0.7298(4) 0.031(3) Uani 1 1 d . . . H20 H 0.1743 0.5649 0.7381 0.037 Uiso 1 1 calc R . . C21 C 0.2373(14) 0.4822(13) 0.6888(4) 0.039(3) Uani 1 1 d . . . H21 H 0.2102 0.5321 0.6692 0.047 Uiso 1 1 calc R . . C22 C 0.3006(14) 0.3889(13) 0.6758(4) 0.040(4) Uani 1 1 d . . . H22 H 0.3196 0.3784 0.6479 0.048 Uiso 1 1 calc R . . C23 C 0.3343(13) 0.3128(12) 0.7050(4) 0.035(3) Uani 1 1 d . . . H23 H 0.3732 0.2489 0.6967 0.042 Uiso 1 1 calc R . . C24 C 0.3107(11) 0.3308(11) 0.7462(4) 0.026(3) Uani 1 1 d . . . H24 H 0.3342 0.2788 0.7656 0.031 Uiso 1 1 calc R . . C25 C 0.0625(11) 0.3791(10) 0.8211(3) 0.023(3) Uani 1 1 d . . . C26 C -0.0147(11) 0.3480(9) 0.7879(4) 0.021(2) Uani 1 1 d . . . H26 H 0.0098 0.3644 0.7610 0.025 Uiso 1 1 calc R . . C27 C -0.1249(14) 0.2942(10) 0.7947(4) 0.030(3) Uani 1 1 d . . . H27 H -0.1750 0.2735 0.7723 0.036 Uiso 1 1 calc R . . C28 C -0.1635(13) 0.2696(11) 0.8350(4) 0.035(3) Uani 1 1 d . . . H28 H -0.2391 0.2327 0.8394 0.042 Uiso 1 1 calc R . . C29 C -0.0908(11) 0.2997(10) 0.8679(4) 0.031(3) Uani 1 1 d . . . H29 H -0.1161 0.2828 0.8948 0.038 Uiso 1 1 calc R . . C30 C 0.0215(10) 0.3558(9) 0.8610(4) 0.024(2) Uani 1 1 d . . . H30 H 0.0699 0.3780 0.8836 0.029 Uiso 1 1 calc R . . C31 C 0.4525(13) 0.1452(11) 0.9035(4) 0.029(3) Uani 1 1 d . . . C32 C 0.5662(15) 0.1946(13) 0.9118(4) 0.038(4) Uani 1 1 d . . . H32 H 0.5781 0.2665 0.9043 0.045 Uiso 1 1 calc R . . C33 C 0.6625(14) 0.1396(14) 0.9312(5) 0.049(4) Uani 1 1 d . . . H33 H 0.7384 0.1749 0.9369 0.058 Uiso 1 1 calc R . . C34 C 0.6478(15) 0.0316(13) 0.9423(5) 0.046(4) Uani 1 1 d . . . H34 H 0.7141 -0.0051 0.9551 0.055 Uiso 1 1 calc R . . C35 C 0.5347(17) -0.0213(14) 0.9345(6) 0.060(5) Uani 1 1 d . . . H35 H 0.5227 -0.0934 0.9419 0.073 Uiso 1 1 calc R . . C36 C 0.4379(15) 0.0396(12) 0.9148(5) 0.047(4) Uani 1 1 d . . . H36 H 0.3609 0.0059 0.9094 0.057 Uiso 1 1 calc R . . C37 C 0.1872(11) 0.1775(10) 0.9106(4) 0.022(3) Uani 1 1 d . . . C38 C 0.1166(14) 0.0838(10) 0.9036(3) 0.033(3) Uani 1 1 d . . . H38 H 0.1339 0.0397 0.8810 0.039 Uiso 1 1 calc R . . C39 C 0.0194(14) 0.0573(13) 0.9313(5) 0.042(4) Uani 1 1 d . . . H39 H -0.0314 -0.0027 0.9262 0.051 Uiso 1 1 calc R . . C40 C -0.0014(13) 0.1192(14) 0.9658(4) 0.045(4) Uani 1 1 d . . . H40 H -0.0640 0.0993 0.9846 0.055 Uiso 1 1 calc R . . C41 C 0.0692(14) 0.2100(15) 0.9729(5) 0.048(4) Uani 1 1 d . . . H41 H 0.0532 0.2531 0.9959 0.058 Uiso 1 1 calc R . . C42 C 0.1652(14) 0.2374(14) 0.9453(4) 0.043(4) Uani 1 1 d . . . H42 H 0.2153 0.2977 0.9507 0.052 Uiso 1 1 calc R . . C43 C 0.3017(12) 0.1357(10) 0.8301(4) 0.026(3) Uani 1 1 d . . . C44 C 0.1830(12) 0.1298(10) 0.8102(4) 0.026(3) Uani 1 1 d . . . H44 H 0.1119 0.1606 0.8225 0.031 Uiso 1 1 calc R . . C45 C 0.1727(13) 0.0779(10) 0.7722(4) 0.032(3) Uani 1 1 d . . . H45 H 0.0946 0.0745 0.7589 0.038 Uiso 1 1 calc R . . C46 C 0.2772(15) 0.0317(12) 0.7544(4) 0.038(3) Uani 1 1 d . . . H46 H 0.2693 -0.0044 0.7292 0.046 Uiso 1 1 calc R . . C47 C 0.3946(15) 0.0380(11) 0.7733(4) 0.037(3) Uani 1 1 d . . . H47 H 0.4660 0.0093 0.7605 0.044 Uiso 1 1 calc R . . C48 C 0.4045(12) 0.0866(10) 0.8110(4) 0.029(3) Uani 1 1 d . . . H48 H 0.4826 0.0871 0.8244 0.035 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 0.01982(19) 0.0149(2) 0.0273(2) 0.0008(2) -0.0012(2) 0.0000(2) P1 0.0304(18) 0.0192(18) 0.0319(17) -0.0007(13) 0.0003(13) 0.0015(13) O1 0.021(5) 0.040(6) 0.048(6) -0.002(4) 0.005(4) 0.003(4) C1 0.029(7) 0.031(8) 0.025(6) 0.006(5) 0.000(5) 0.007(6) P2 0.0214(16) 0.0164(16) 0.0281(16) 0.0000(12) -0.0031(13) 0.0008(13) C2 0.016(7) 0.026(7) 0.036(7) -0.001(5) -0.003(5) -0.016(5) P3 0.0239(16) 0.0164(17) 0.0295(16) 0.0036(12) -0.0015(12) 0.0017(13) C3 0.029(7) 0.039(9) 0.065(9) -0.013(8) 0.004(8) 0.001(6) C4 0.033(8) 0.059(12) 0.077(11) 0.021(9) -0.021(8) -0.027(8) C5 0.060(12) 0.023(8) 0.044(8) -0.013(6) 0.019(7) -0.008(7) C6 0.029(7) 0.025(8) 0.034(7) -0.003(5) -0.002(5) 0.003(6) C7 0.029(8) 0.042(10) 0.081(12) -0.027(9) -0.003(7) 0.003(7) C8 0.052(11) 0.023(9) 0.087(13) -0.033(8) 0.005(8) 0.002(8) C9 0.051(10) 0.038(10) 0.046(9) -0.003(7) 0.021(7) 0.016(8) C10 0.032(8) 0.033(10) 0.075(11) -0.005(8) 0.003(7) 0.012(7) C11 0.039(9) 0.052(10) 0.060(9) -0.002(8) 0.008(7) 0.001(9) C12 0.018(6) 0.015(6) 0.038(7) 0.009(5) -0.012(5) -0.005(5) C13 0.042(7) 0.021(8) 0.017(6) 0.002(5) -0.004(5) 0.001(6) C14 0.041(8) 0.016(7) 0.043(8) 0.007(6) -0.004(6) -0.010(6) C15 0.075(12) 0.016(8) 0.037(8) 0.001(6) -0.009(8) -0.022(8) C16 0.087(15) 0.022(8) 0.043(8) 0.005(6) 0.013(9) 0.003(9) C17 0.071(12) 0.040(11) 0.039(8) 0.006(7) 0.005(8) 0.040(9) C18 0.060(10) 0.017(8) 0.030(7) 0.000(5) -0.003(6) -0.007(6) C19 0.038(7) 0.026(9) 0.018(6) -0.003(5) -0.006(5) -0.007(6) C20 0.029(7) 0.029(8) 0.034(7) 0.006(6) 0.001(5) 0.005(6) C21 0.045(9) 0.034(9) 0.038(8) 0.009(6) -0.002(6) -0.008(7) C22 0.059(9) 0.038(9) 0.023(6) -0.004(6) 0.008(6) -0.017(8) C23 0.028(7) 0.034(9) 0.044(8) -0.002(6) -0.002(6) -0.005(6) C24 0.018(6) 0.033(8) 0.028(7) 0.000(5) -0.001(5) -0.006(5) C25 0.023(6) 0.015(7) 0.030(6) -0.002(5) -0.002(5) 0.003(5) C26 0.018(6) 0.012(6) 0.034(6) 0.004(5) -0.003(5) 0.002(5) C27 0.024(6) 0.020(6) 0.048(7) 0.002(5) -0.006(7) 0.004(7) C28 0.023(7) 0.023(8) 0.058(9) -0.001(6) 0.001(6) 0.003(5) C29 0.028(7) 0.021(7) 0.045(8) 0.000(6) 0.008(6) 0.006(5) C30 0.019(5) 0.018(6) 0.035(6) -0.005(6) -0.010(6) 0.008(4) C31 0.027(7) 0.034(8) 0.025(7) 0.003(5) -0.007(5) -0.005(6) C32 0.058(10) 0.020(8) 0.035(8) 0.010(6) -0.001(7) 0.005(7) C33 0.025(8) 0.045(10) 0.076(11) 0.018(8) -0.007(7) 0.006(6) C34 0.037(10) 0.039(10) 0.062(9) 0.021(7) -0.007(7) 0.012(7) C35 0.052(11) 0.020(9) 0.110(15) 0.023(9) -0.013(10) 0.008(8) C36 0.031(8) 0.016(8) 0.094(13) 0.000(7) -0.008(8) -0.002(6) C37 0.013(6) 0.016(7) 0.038(7) 0.005(5) -0.003(5) 0.005(5) C38 0.043(7) 0.020(7) 0.035(6) 0.009(5) 0.001(6) -0.012(7) C39 0.029(8) 0.037(9) 0.061(10) 0.019(7) -0.003(7) -0.002(7) C40 0.033(8) 0.060(12) 0.043(8) 0.028(8) 0.007(6) 0.008(8) C41 0.037(8) 0.067(12) 0.042(8) -0.006(8) 0.006(6) -0.014(8) C42 0.040(9) 0.055(11) 0.035(8) 0.012(7) -0.004(6) -0.018(7) C43 0.026(7) 0.021(7) 0.032(7) 0.003(5) 0.000(5) 0.002(5) C44 0.023(6) 0.019(7) 0.037(7) 0.009(5) -0.001(5) -0.011(5) C45 0.037(7) 0.014(8) 0.045(8) -0.003(5) -0.003(6) 0.001(5) C46 0.053(10) 0.024(8) 0.038(8) -0.004(6) -0.001(7) 0.001(7) C47 0.037(9) 0.029(8) 0.044(8) 0.003(6) 0.012(7) 0.006(7) C48 0.030(7) 0.014(7) 0.043(7) 0.003(5) 0.002(5) 0.003(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 1.867(13) . ? Ir1 C1 1.918(14) . ? Ir1 P2 2.342(3) . ? Ir1 P3 2.386(3) . ? Ir1 P1 2.442(3) . ? P1 C1 1.753(13) . ? P1 C6 1.864(14) . ? O1 C12 1.176(15) . ? C1 C2 1.523(17) . ? P2 C13 1.817(15) . ? P2 C25 1.828(13) . ? P2 C19 1.854(12) . ? C2 C5 1.488(18) . ? C2 C3 1.543(19) . ? C2 C4 1.561(19) . ? P3 C43 1.841(13) . ? P3 C37 1.850(13) . ? P3 C31 1.852(13) . ? C6 C7 1.537(19) . ? C6 C11 1.569(19) . ? C7 C8 1.57(2) . ? C8 C9 1.51(2) . ? C9 C10 1.52(2) . ? C10 C11 1.55(2) . ? C13 C18 1.41(2) . ? C13 C14 1.409(18) . ? C14 C15 1.38(2) . ? C15 C16 1.38(2) . ? C16 C17 1.33(2) . ? C17 C18 1.42(2) . ? C19 C24 1.381(18) . ? C19 C20 1.402(17) . ? C20 C21 1.365(18) . ? C21 C22 1.40(2) . ? C22 C23 1.38(2) . ? C23 C24 1.370(18) . ? C25 C30 1.389(17) . ? C25 C26 1.398(16) . ? C26 C27 1.358(18) . ? C27 C28 1.395(18) . ? C28 C29 1.361(18) . ? C29 C30 1.391(17) . ? C31 C36 1.364(19) . ? C31 C32 1.37(2) . ? C32 C33 1.37(2) . ? C33 C34 1.39(2) . ? C34 C35 1.38(2) . ? C35 C36 1.42(2) . ? C37 C42 1.36(2) . ? C37 C38 1.395(17) . ? C38 C39 1.397(19) . ? C39 C40 1.37(2) . ? C40 C41 1.37(2) . ? C41 C42 1.39(2) . ? C43 C48 1.386(17) . ? C43 C44 1.409(17) . ? C44 C45 1.387(17) . ? C45 C46 1.37(2) . ? C46 C47 1.38(2) . ? C47 C48 1.359(18) . ? 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 104.4(5) . . ? C12 Ir1 P2 93.7(4) . . ? C1 Ir1 P2 127.5(4) . . ? C12 Ir1 P3 92.7(4) . . ? C1 Ir1 P3 128.2(4) . . ? P2 Ir1 P3 98.93(12) . . ? C12 Ir1 P1 149.1(4) . . ? C1 Ir1 P1 45.5(4) . . ? P2 Ir1 P1 110.33(11) . . ? P3 Ir1 P1 102.11(11) . . ? C1 P1 C6 109.2(6) . . ? C1 P1 Ir1 51.3(4) . . ? C6 P1 Ir1 115.2(4) . . ? C2 C1 P1 135.7(9) . . ? C2 C1 Ir1 140.8(9) . . ? P1 C1 Ir1 83.3(6) . . ? C13 P2 C25 104.2(6) . . ? C13 P2 C19 100.6(5) . . ? C25 P2 C19 103.0(6) . . ? C13 P2 Ir1 109.7(4) . . ? C25 P2 Ir1 119.1(4) . . ? C19 P2 Ir1 117.9(4) . . ? C5 C2 C1 110.1(12) . . ? C5 C2 C3 109.4(11) . . ? C1 C2 C3 112.1(10) . . ? C5 C2 C4 110.3(12) . . ? C1 C2 C4 106.4(10) . . ? C3 C2 C4 108.4(12) . . ? C43 P3 C37 104.1(6) . . ? C43 P3 C31 101.3(6) . . ? C37 P3 C31 100.1(6) . . ? C43 P3 Ir1 113.0(4) . . ? C37 P3 Ir1 124.2(4) . . ? C31 P3 Ir1 111.2(5) . . ? C7 C6 C11 109.3(12) . . ? C7 C6 P1 109.9(10) . . ? C11 C6 P1 108.2(10) . . ? C6 C7 C8 112.3(13) . . ? C9 C8 C7 109.5(14) . . ? C8 C9 C10 109.8(12) . . ? C9 C10 C11 113.6(13) . . ? C10 C11 C6 111.2(14) . . ? O1 C12 Ir1 177.1(10) . . ? C18 C13 C14 118.1(13) . . ? C18 C13 P2 122.7(10) . . ? C14 C13 P2 119.1(10) . . ? C15 C14 C13 120.4(15) . . ? C16 C15 C14 120.6(15) . . ? C17 C16 C15 120.0(15) . . ? C16 C17 C18 122.1(16) . . ? C13 C18 C17 118.8(15) . . ? C24 C19 C20 119.2(11) . . ? C24 C19 P2 119.1(9) . . ? C20 C19 P2 121.5(10) . . ? C21 C20 C19 119.2(13) . . ? C20 C21 C22 121.4(13) . . ? C23 C22 C21 118.8(12) . . ? C24 C23 C22 120.4(14) . . ? C23 C24 C19 121.0(12) . . ? C30 C25 C26 118.0(11) . . ? C30 C25 P2 117.7(9) . . ? C26 C25 P2 124.2(9) . . ? C27 C26 C25 120.7(11) . . ? C26 C27 C28 120.4(12) . . ? C29 C28 C27 120.2(13) . . ? C28 C29 C30 119.5(13) . . ? C25 C30 C29 121.2(12) . . ? C36 C31 C32 118.2(14) . . ? C36 C31 P3 120.2(11) . . ? C32 C31 P3 121.6(11) . . ? C31 C32 C33 121.0(15) . . ? C32 C33 C34 120.7(16) . . ? C35 C34 C33 120.2(14) . . ? C34 C35 C36 116.8(15) . . ? C31 C36 C35 123.1(15) . . ? C42 C37 C38 119.5(12) . . ? C42 C37 P3 117.5(10) . . ? C38 C37 P3 122.7(10) . . ? C37 C38 C39 118.9(13) . . ? C40 C39 C38 120.4(15) . . ? C41 C40 C39 120.5(14) . . ? C40 C41 C42 119.4(15) . . ? C37 C42 C41 121.2(15) . . ? C48 C43 C44 118.1(12) . . ? C48 C43 P3 121.2(10) . . ? C44 C43 P3 120.4(10) . . ? C45 C44 C43 119.7(12) . . ? C46 C45 C44 120.1(13) . . ? C45 C46 C47 120.7(13) . . ? C48 C47 C46 119.3(13) . . ? C47 C48 C43 122.0(12) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 3.613 (near Ir1) _refine_diff_density_min -2.095 _refine_diff_density_rms 0.187 data_compound_7 _database_code_CSD 184726 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H35 Ir O2 P2' _chemical_formula_weight 693.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 11.381(2) _cell_length_b 14.501(3) _cell_length_c 16.922(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.83(3) _cell_angle_gamma 90.00 _cell_volume 2782.8(10) _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 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 4.939 _exptl_absorpt_correction_type 'Sortav (Blessing 1995)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.68 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 48226 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 6327 _reflns_number_gt 5165 _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^)+(0.0228P)^2^+29.4194P] 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 6327 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1090 _refine_ls_wR_factor_gt 0.1033 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 0.01176(3) 0.608064(17) 0.063907(15) 0.02469(9) Uani 1 1 d . . . P1 P -0.05655(17) 0.45323(12) 0.06542(10) 0.0264(4) Uani 1 1 d . . . P2 P 0.00784(18) 0.76685(12) 0.03661(10) 0.0274(4) Uani 1 1 d . . . O1 O -0.1399(5) 0.6229(4) 0.2052(3) 0.0420(14) Uani 1 1 d . . . O2 O 0.2325(6) 0.6332(4) 0.1750(3) 0.0477(15) Uani 1 1 d . . . C1 C -0.1138(7) 0.5970(5) 0.1408(4) 0.0349(17) Uani 1 1 d . . . C2 C -0.1623(7) 0.5441(5) 0.0744(4) 0.0309(16) Uani 1 1 d . . . C3 C -0.2901(7) 0.5555(5) 0.0402(5) 0.0355(17) Uani 1 1 d . . . C4 C -0.3394(9) 0.6479(7) 0.0662(6) 0.054(2) Uani 1 1 d . . . H4A H -0.2987 0.6974 0.0426 0.081 Uiso 1 1 calc R . . H4B H -0.3284 0.6529 0.1229 0.081 Uiso 1 1 calc R . . H4C H -0.4220 0.6513 0.0494 0.081 Uiso 1 1 calc R . . C5 C -0.3001(8) 0.5519(7) -0.0489(5) 0.050(2) Uani 1 1 d . . . H5A H -0.2963 0.4889 -0.0660 0.075 Uiso 1 1 calc R . . H5B H -0.2365 0.5861 -0.0685 0.075 Uiso 1 1 calc R . . H5C H -0.3740 0.5783 -0.0691 0.075 Uiso 1 1 calc R . . C6 C -0.3638(10) 0.4791(8) 0.0735(8) 0.078(4) Uani 1 1 d . . . H6A H -0.4452 0.4878 0.0554 0.116 Uiso 1 1 calc R . . H6B H -0.3549 0.4812 0.1304 0.116 Uiso 1 1 calc R . . H6C H -0.3375 0.4203 0.0557 0.116 Uiso 1 1 calc R . . C7 C -0.0344(7) 0.3897(5) 0.1622(4) 0.0309(15) Uani 1 1 d . . . H7 H -0.0121 0.3266 0.1489 0.037 Uiso 1 1 calc R . . C8 C -0.1465(7) 0.3812(6) 0.2052(4) 0.0374(18) Uani 1 1 d . . . H8A H -0.2084 0.3538 0.1698 0.045 Uiso 1 1 calc R . . H8B H -0.1725 0.4421 0.2197 0.045 Uiso 1 1 calc R . . C9 C -0.1257(8) 0.3210(7) 0.2808(5) 0.049(2) Uani 1 1 d . . . H9A H -0.1968 0.3202 0.3086 0.059 Uiso 1 1 calc R . . H9B H -0.1087 0.2582 0.2658 0.059 Uiso 1 1 calc R . . C10 C -0.0252(9) 0.3576(7) 0.3348(5) 0.055(3) Uani 1 1 d . . . H10A H -0.0115 0.3168 0.3801 0.066 Uiso 1 1 calc R . . H10B H -0.0460 0.4178 0.3543 0.066 Uiso 1 1 calc R . . C11 C 0.0857(9) 0.3653(7) 0.2933(5) 0.052(2) Uani 1 1 d . . . H11A H 0.1100 0.3044 0.2775 0.063 Uiso 1 1 calc R . . H11B H 0.1481 0.3907 0.3295 0.063 Uiso 1 1 calc R . . C12 C 0.0677(7) 0.4272(6) 0.2197(4) 0.0383(18) Uani 1 1 d . . . H12A H 0.1398 0.4291 0.1930 0.046 Uiso 1 1 calc R . . H12B H 0.0496 0.4894 0.2357 0.046 Uiso 1 1 calc R . . C13 C 0.1531(7) 0.6228(5) 0.1297(4) 0.0311(16) Uani 1 1 d . . . C14 C -0.1297(6) 0.8163(5) -0.0104(4) 0.0300(15) Uani 1 1 d . . . C15 C -0.1808(8) 0.7777(6) -0.0804(5) 0.043(2) Uani 1 1 d . . . H15 H -0.1443 0.7280 -0.1031 0.052 Uiso 1 1 calc R . . C16 C -0.2858(8) 0.8125(7) -0.1169(5) 0.050(2) Uani 1 1 d . . . H16 H -0.3185 0.7867 -0.1641 0.061 Uiso 1 1 calc R . . C17 C -0.3411(8) 0.8853(7) -0.0828(6) 0.054(2) Uani 1 1 d . . . H17 H -0.4112 0.9088 -0.1070 0.065 Uiso 1 1 calc R . . C18 C -0.2926(8) 0.9230(6) -0.0133(6) 0.053(2) Uani 1 1 d . . . H18 H -0.3306 0.9716 0.0099 0.063 Uiso 1 1 calc R . . C19 C -0.1854(7) 0.8886(6) 0.0234(5) 0.0426(19) Uani 1 1 d . . . H19 H -0.1526 0.9148 0.0704 0.051 Uiso 1 1 calc R . . C20 C 0.1230(7) 0.8033(5) -0.0269(4) 0.0276(15) Uani 1 1 d . . . C21 C 0.1027(9) 0.8582(6) -0.0939(5) 0.045(2) Uani 1 1 d . . . H21 H 0.0266 0.8789 -0.1083 0.054 Uiso 1 1 calc R . . C22 C 0.1928(7) 0.8830(5) -0.1399(4) 0.0368(18) Uani 1 1 d . . . H22 H 0.1764 0.9187 -0.1851 0.044 Uiso 1 1 calc R . . C23 C 0.3036(8) 0.8554(6) -0.1191(5) 0.044(2) Uani 1 1 d . . . H23 H 0.3638 0.8717 -0.1503 0.052 Uiso 1 1 calc R . . C24 C 0.3288(8) 0.8031(7) -0.0517(5) 0.048(2) Uani 1 1 d . . . H24 H 0.4060 0.7855 -0.0367 0.058 Uiso 1 1 calc R . . C25 C 0.2379(8) 0.7769(6) -0.0060(5) 0.0404(19) Uani 1 1 d . . . H25 H 0.2549 0.7411 0.0391 0.049 Uiso 1 1 calc R . . C26 C 0.0387(7) 0.8409(5) 0.1234(4) 0.0291(15) Uani 1 1 d . . . C27 C 0.0966(7) 0.9234(5) 0.1194(4) 0.0346(17) Uani 1 1 d . . . H27 H 0.1248 0.9411 0.0717 0.042 Uiso 1 1 calc R . . C28 C 0.1142(8) 0.9812(6) 0.1845(5) 0.0411(19) Uani 1 1 d . . . H28 H 0.1550 1.0364 0.1807 0.049 Uiso 1 1 calc R . . C29 C 0.0710(8) 0.9565(6) 0.2546(5) 0.044(2) Uani 1 1 d . . . H29 H 0.0809 0.9956 0.2982 0.052 Uiso 1 1 calc R . . C30 C 0.0132(9) 0.8742(6) 0.2605(5) 0.045(2) Uani 1 1 d . . . H30 H -0.0161 0.8579 0.3082 0.054 Uiso 1 1 calc R . . C31 C -0.0021(8) 0.8146(5) 0.1960(4) 0.0396(19) Uani 1 1 d . . . H31 H -0.0390 0.7579 0.2010 0.048 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 0.03511(16) 0.02236(13) 0.01754(13) -0.00003(11) 0.00774(10) -0.00168(12) P1 0.0353(10) 0.0256(9) 0.0195(8) 0.0009(7) 0.0095(7) -0.0012(8) P2 0.0376(11) 0.0244(9) 0.0208(8) 0.0013(7) 0.0068(7) -0.0011(8) O1 0.059(4) 0.044(3) 0.027(3) -0.008(2) 0.025(3) -0.012(3) O2 0.059(4) 0.039(3) 0.043(3) -0.002(3) -0.010(3) -0.004(3) C1 0.049(5) 0.032(4) 0.027(4) 0.002(3) 0.020(3) 0.002(3) C2 0.035(4) 0.033(4) 0.026(3) 0.003(3) 0.013(3) 0.000(3) C3 0.039(4) 0.035(4) 0.035(4) 0.005(3) 0.016(3) 0.002(3) C4 0.050(6) 0.065(6) 0.049(5) 0.000(5) 0.015(4) 0.018(5) C5 0.042(5) 0.061(6) 0.046(5) -0.007(4) 0.003(4) 0.007(4) C6 0.050(6) 0.074(8) 0.107(9) 0.043(7) -0.007(6) -0.020(6) C7 0.038(4) 0.028(3) 0.027(3) 0.005(3) 0.003(3) -0.010(3) C8 0.049(5) 0.038(4) 0.026(4) 0.006(3) 0.008(3) -0.012(4) C9 0.059(6) 0.059(6) 0.031(4) 0.013(4) 0.014(4) -0.012(5) C10 0.077(7) 0.058(6) 0.028(4) 0.011(4) 0.001(4) -0.022(5) C11 0.058(6) 0.061(6) 0.037(5) 0.017(4) -0.005(4) -0.015(5) C12 0.044(5) 0.042(4) 0.030(4) 0.009(3) 0.004(3) -0.007(4) C13 0.030(4) 0.033(4) 0.030(4) -0.001(3) -0.001(3) -0.001(3) C14 0.033(4) 0.030(4) 0.028(4) 0.003(3) 0.006(3) -0.003(3) C15 0.051(5) 0.048(5) 0.032(4) 0.004(4) 0.011(4) -0.006(4) C16 0.046(5) 0.065(6) 0.040(5) 0.010(4) -0.002(4) -0.012(5) C17 0.035(5) 0.056(6) 0.070(6) 0.022(5) 0.001(4) -0.003(4) C18 0.044(5) 0.040(5) 0.074(7) 0.003(5) 0.008(5) 0.008(4) C19 0.039(5) 0.036(4) 0.052(5) 0.009(4) 0.000(4) 0.003(4) C20 0.036(4) 0.027(3) 0.021(3) 0.000(3) 0.009(3) -0.004(3) C21 0.068(6) 0.041(4) 0.027(4) 0.011(3) 0.009(4) 0.016(4) C22 0.046(5) 0.041(4) 0.025(4) 0.011(3) 0.010(3) -0.010(4) C23 0.048(5) 0.054(5) 0.030(4) -0.002(4) 0.012(4) -0.015(4) C24 0.046(5) 0.060(6) 0.041(5) 0.003(4) 0.011(4) -0.011(4) C25 0.049(5) 0.046(5) 0.027(4) 0.007(3) 0.007(3) -0.009(4) C26 0.036(4) 0.029(4) 0.022(3) -0.003(3) 0.003(3) 0.001(3) C27 0.044(5) 0.030(4) 0.031(4) 0.003(3) 0.004(3) -0.004(3) C28 0.046(5) 0.036(4) 0.040(4) -0.006(4) -0.004(4) -0.006(4) C29 0.060(6) 0.035(4) 0.035(4) -0.013(3) -0.004(4) 0.003(4) C30 0.069(6) 0.040(5) 0.026(4) -0.007(3) 0.012(4) -0.002(4) C31 0.060(5) 0.031(4) 0.028(4) -0.001(3) 0.008(4) -0.007(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 C13 1.889(7) . ? Ir1 C1 2.018(7) . ? Ir1 C2 2.209(7) . ? Ir1 P2 2.3481(19) . ? Ir1 P1 2.3769(19) . ? Ir1 P1 2.4550(17) 3_565 ? P1 C2 1.800(8) . ? P1 C7 1.877(7) . ? P1 Ir1 2.4550(17) 3_565 ? P2 C26 1.829(7) . ? P2 C14 1.840(8) . ? P2 C20 1.842(7) . ? O1 C1 1.213(8) . ? O2 C13 1.145(9) . ? C1 C2 1.433(11) . ? C2 C3 1.528(11) . ? C3 C5 1.503(11) . ? C3 C6 1.526(12) . ? C3 C4 1.532(12) . ? C7 C8 1.526(10) . ? C7 C12 1.551(10) . ? C8 C9 1.550(10) . ? C9 C10 1.500(13) . ? C10 C11 1.501(13) . ? C11 C12 1.534(11) . ? C14 C19 1.374(11) . ? C14 C15 1.394(11) . ? C15 C16 1.392(13) . ? C16 C17 1.381(14) . ? C17 C18 1.371(14) . ? C18 C19 1.413(12) . ? C20 C25 1.379(11) . ? C20 C21 1.388(10) . ? C21 C22 1.385(11) . ? C22 C23 1.342(12) . ? C23 C24 1.380(12) . ? C24 C25 1.396(11) . ? C26 C27 1.370(10) . ? C26 C31 1.402(10) . ? C27 C28 1.386(11) . ? C28 C29 1.369(12) . ? C29 C30 1.371(12) . ? C30 C31 1.392(11) . ? 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 104.0(3) . . ? C13 Ir1 C2 136.5(3) . . ? C1 Ir1 C2 39.3(3) . . ? C13 Ir1 P2 90.4(2) . . ? C1 Ir1 P2 101.7(2) . . ? C2 Ir1 P2 115.2(2) . . ? C13 Ir1 P1 111.3(2) . . ? C1 Ir1 P1 70.6(2) . . ? C2 Ir1 P1 46.0(2) . . ? P2 Ir1 P1 158.06(7) . . ? C13 Ir1 P1 109.6(2) . 3_565 ? C1 Ir1 P1 139.2(2) . 3_565 ? C2 Ir1 P1 100.06(19) . 3_565 ? P2 Ir1 P1 100.46(6) . 3_565 ? P1 Ir1 P1 76.13(6) . 3_565 ? C2 P1 C7 109.1(3) . . ? C2 P1 Ir1 62.0(2) . . ? C7 P1 Ir1 116.9(2) . . ? C2 P1 Ir1 122.1(2) . 3_565 ? C7 P1 Ir1 125.2(3) . 3_565 ? Ir1 P1 Ir1 103.87(6) . 3_565 ? C26 P2 C14 102.5(3) . . ? C26 P2 C20 101.7(3) . . ? C14 P2 C20 104.9(3) . . ? C26 P2 Ir1 114.7(2) . . ? C14 P2 Ir1 117.9(2) . . ? C20 P2 Ir1 113.2(2) . . ? O1 C1 C2 139.7(8) . . ? O1 C1 Ir1 142.7(7) . . ? C2 C1 Ir1 77.5(4) . . ? C1 C2 C3 122.1(7) . . ? C1 C2 P1 104.0(5) . . ? C3 C2 P1 132.0(6) . . ? C1 C2 Ir1 63.2(4) . . ? C3 C2 Ir1 139.1(5) . . ? P1 C2 Ir1 71.9(3) . . ? C5 C3 C6 110.4(8) . . ? C5 C3 C2 111.5(6) . . ? C6 C3 C2 108.4(7) . . ? C5 C3 C4 108.7(7) . . ? C6 C3 C4 107.6(8) . . ? C2 C3 C4 110.2(7) . . ? C8 C7 C12 110.0(6) . . ? C8 C7 P1 113.5(5) . . ? C12 C7 P1 114.5(5) . . ? C7 C8 C9 111.3(7) . . ? C10 C9 C8 111.1(7) . . ? C9 C10 C11 111.7(7) . . ? C10 C11 C12 111.3(8) . . ? C11 C12 C7 110.3(7) . . ? O2 C13 Ir1 173.9(7) . . ? C19 C14 C15 119.1(8) . . ? C19 C14 P2 121.5(6) . . ? C15 C14 P2 119.3(6) . . ? C16 C15 C14 120.8(8) . . ? C17 C16 C15 119.8(9) . . ? C18 C17 C16 119.9(9) . . ? C17 C18 C19 120.5(9) . . ? C14 C19 C18 119.9(8) . . ? C25 C20 C21 117.2(7) . . ? C25 C20 P2 118.4(5) . . ? C21 C20 P2 124.3(6) . . ? C22 C21 C20 121.8(8) . . ? C23 C22 C21 119.9(7) . . ? C22 C23 C24 120.4(8) . . ? C23 C24 C25 119.7(9) . . ? C20 C25 C24 120.8(8) . . ? C27 C26 C31 118.5(7) . . ? C27 C26 P2 122.2(5) . . ? C31 C26 P2 119.2(6) . . ? C26 C27 C28 121.8(7) . . ? C29 C28 C27 119.5(8) . . ? C28 C29 C30 120.0(7) . . ? C29 C30 C31 120.9(8) . . ? C30 C31 C26 119.3(7) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.843 (near Ir(1)) _refine_diff_density_min -1.425 _refine_diff_density_rms 0.165