################################################################ # # # get CCDC# xxxxxx (from) deposit@ccdc.cam.ac.uk # # for pre-publication to J. Am. Chem. Soc. # # Compound: 11_PCPIrICCPh (iriccph) # # # ################################################################ data_global _publ_contact_author_name 'Alan S. Goldman' _publ_contact_author_address ; Department of Chemistry and Chemical Biology Rutgers, The State University of New Jersey 610 Taylor Road Piscataway, New Jersey 08854-8087 U.S.A. ; _publ_contact_author_email 'alan.goldman@rutgers.edu' _publ_requested_journal 'J. Am. Chem. Soc.' _publ_section_title ; Combined Experimental and Computational Studies on Carbon-Carbon Reductive Elimination from Bis(hydrocarbyl) Complexes of (PCP)Ir ; loop_ _publ_author_name _publ_author_address 'Rajshekhar Ghosh' ; Department of Chemistry and Chemical Biology Rutgers, The State University of New Jersey Piscataway, New Jersey 08854-8087 U.S.A. ; 'Thomas J. Emge' ; Department of Chemistry and Chemical Biology Rutgers, The State University of New Jersey Piscataway, New Jersey 08854-8087 U.S.A. ; 'Karsten Krogh-Jespersen' ; Department of Chemistry and Chemical Biology Rutgers, The State University of New Jersey Piscataway, New Jersey 08854-8087 U.S.A. ; 'Alan S. Goldman' ; Department of Chemistry and Chemical Biology Rutgers, The State University of New Jersey Piscataway, New Jersey 08854-8087 U.S.A. ; data_iriccph _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H48 I Ir P2' _chemical_formula_weight 813.74 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 13.2440(6) _cell_length_b 15.2021(7) _cell_length_c 16.7996(8) _cell_angle_alpha 90.00 _cell_angle_beta 110.383(1) _cell_angle_gamma 90.00 _cell_volume 3170.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8874 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 30.52 _exptl_crystal_description lathe _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 5.305 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8237 _exptl_absorpt_correction_T_max 0.9999 _exptl_absorpt_process_details 'Bruker SAINT (SADABS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 38358 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 30.55 _reflns_number_total 9666 _reflns_number_gt 9055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0160P)^2^+3.1000P] 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 9666 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0390 _refine_ls_wR_factor_gt 0.0384 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.004 _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 0.308001(5) 0.329547(4) 0.123987(4) 0.00970(2) Uani 1 1 d . . . I1 I 0.389294(9) 0.165564(7) 0.178043(7) 0.01441(3) Uani 1 1 d . . . P1 P 0.34502(3) 0.32230(3) -0.00225(3) 0.01151(8) Uani 1 1 d . . . P2 P 0.22011(4) 0.35913(3) 0.22180(3) 0.01262(8) Uani 1 1 d . . . C1 C 0.24428(13) 0.44850(11) 0.07539(10) 0.0121(3) Uani 1 1 d . . . C2 C 0.27134(13) 0.48732(11) 0.00902(11) 0.0134(3) Uani 1 1 d . . . C3 C 0.22747(15) 0.56804(12) -0.02544(11) 0.0163(3) Uani 1 1 d . . . H3 H 0.2451 0.5925 -0.0710 0.020 Uiso 1 1 calc R . . C4 C 0.15827(15) 0.61304(12) 0.00617(12) 0.0168(3) Uani 1 1 d . . . H4 H 0.1300 0.6687 -0.0167 0.020 Uiso 1 1 calc R . . C5 C 0.13066(14) 0.57615(11) 0.07153(11) 0.0153(3) Uani 1 1 d . . . H5 H 0.0828 0.6065 0.0930 0.018 Uiso 1 1 calc R . . C6 C 0.17281(13) 0.49486(11) 0.10580(10) 0.0131(3) Uani 1 1 d . . . C7 C 0.34783(14) 0.44013(11) -0.02475(11) 0.0150(3) Uani 1 1 d . . . H7A H 0.4217 0.4634 0.0026 0.018 Uiso 1 1 calc R . . H7B H 0.3262 0.4497 -0.0868 0.018 Uiso 1 1 calc R . . C8 C 0.13536(15) 0.45415(12) 0.17233(12) 0.0173(3) Uani 1 1 d . . . H8A H 0.0595 0.4349 0.1460 0.021 Uiso 1 1 calc R . . H8B H 0.1388 0.4984 0.2164 0.021 Uiso 1 1 calc R . . C9 C 0.22417(14) 0.27535(12) -0.08854(11) 0.0157(3) Uani 1 1 d . . . C10 C 0.23468(16) 0.27874(14) -0.17669(12) 0.0220(4) Uani 1 1 d . . . H10A H 0.2931 0.2397 -0.1777 0.033 Uiso 1 1 calc R . . H10B H 0.2507 0.3391 -0.1890 0.033 Uiso 1 1 calc R . . H10C H 0.1669 0.2595 -0.2197 0.033 Uiso 1 1 calc R . . C11 C 0.12489(15) 0.33072(13) -0.09307(12) 0.0206(4) Uani 1 1 d . . . H11A H 0.0605 0.3055 -0.1356 0.031 Uiso 1 1 calc R . . H11B H 0.1348 0.3913 -0.1090 0.031 Uiso 1 1 calc R . . H11C H 0.1162 0.3306 -0.0375 0.031 Uiso 1 1 calc R . . C12 C 0.20297(16) 0.18033(13) -0.06711(12) 0.0199(4) Uani 1 1 d . . . H12A H 0.1383 0.1578 -0.1114 0.030 Uiso 1 1 calc R . . H12B H 0.1923 0.1793 -0.0123 0.030 Uiso 1 1 calc R . . H12C H 0.2648 0.1434 -0.0641 0.030 Uiso 1 1 calc R . . C13 C 0.47300(14) 0.27878(12) -0.01287(11) 0.0139(3) Uani 1 1 d . . . C14 C 0.46815(15) 0.17929(12) -0.02983(12) 0.0178(3) Uani 1 1 d . . . H14A H 0.5395 0.1582 -0.0263 0.027 Uiso 1 1 calc R . . H14B H 0.4162 0.1673 -0.0867 0.027 Uiso 1 1 calc R . . H14C H 0.4456 0.1489 0.0126 0.027 Uiso 1 1 calc R . . C15 C 0.49963(16) 0.32704(13) -0.08383(12) 0.0201(4) Uani 1 1 d . . . H15A H 0.5661 0.3029 -0.0882 0.030 Uiso 1 1 calc R . . H15B H 0.5093 0.3899 -0.0704 0.030 Uiso 1 1 calc R . . H15C H 0.4404 0.3190 -0.1380 0.030 Uiso 1 1 calc R . . C16 C 0.56522(14) 0.29630(13) 0.07104(12) 0.0176(3) Uani 1 1 d . . . H16A H 0.5516 0.2646 0.1171 0.026 Uiso 1 1 calc R . . H16B H 0.5698 0.3595 0.0832 0.026 Uiso 1 1 calc R . . H16C H 0.6332 0.2760 0.0665 0.026 Uiso 1 1 calc R . . C17 C 0.11695(14) 0.27163(12) 0.21630(11) 0.0154(3) Uani 1 1 d . . . C18 C 0.08025(15) 0.23819(14) 0.12387(12) 0.0211(4) Uani 1 1 d . . . H18A H 0.1406 0.2088 0.1138 0.032 Uiso 1 1 calc R . . H18B H 0.0561 0.2881 0.0849 0.032 Uiso 1 1 calc R . . H18C H 0.0208 0.1965 0.1142 0.032 Uiso 1 1 calc R . . C19 C 0.01739(15) 0.30495(13) 0.23448(13) 0.0200(4) Uani 1 1 d . . . H19A H -0.0315 0.2556 0.2314 0.030 Uiso 1 1 calc R . . H19B H -0.0198 0.3495 0.1923 0.030 Uiso 1 1 calc R . . H19C H 0.0401 0.3310 0.2914 0.030 Uiso 1 1 calc R . . C20 C 0.16739(15) 0.19481(12) 0.27616(12) 0.0180(3) Uani 1 1 d . . . H20A H 0.1878 0.2146 0.3352 0.027 Uiso 1 1 calc R . . H20B H 0.2316 0.1740 0.2655 0.027 Uiso 1 1 calc R . . H20C H 0.1151 0.1468 0.2660 0.027 Uiso 1 1 calc R . . C21 C 0.29785(15) 0.39199(12) 0.33397(11) 0.0160(3) Uani 1 1 d . . . C22 C 0.34648(17) 0.48331(13) 0.33029(13) 0.0219(4) Uani 1 1 d . . . H22A H 0.2889 0.5274 0.3136 0.033 Uiso 1 1 calc R . . H22B H 0.3829 0.4824 0.2886 0.033 Uiso 1 1 calc R . . H22C H 0.3985 0.4982 0.3863 0.033 Uiso 1 1 calc R . . C23 C 0.22870(17) 0.39917(14) 0.39067(12) 0.0223(4) Uani 1 1 d . . . H23A H 0.2033 0.3406 0.3991 0.034 Uiso 1 1 calc R . . H23B H 0.1667 0.4374 0.3633 0.034 Uiso 1 1 calc R . . H23C H 0.2720 0.4242 0.4458 0.034 Uiso 1 1 calc R . . C24 C 0.39007(16) 0.32628(13) 0.37153(12) 0.0201(4) Uani 1 1 d . . . H24A H 0.4348 0.3454 0.4286 0.030 Uiso 1 1 calc R . . H24B H 0.4341 0.3235 0.3353 0.030 Uiso 1 1 calc R . . H24C H 0.3602 0.2679 0.3747 0.030 Uiso 1 1 calc R . . C25 C 0.43816(14) 0.39433(12) 0.18028(11) 0.0138(3) Uani 1 1 d . . . C26 C 0.52046(15) 0.43472(12) 0.21448(11) 0.0161(3) Uani 1 1 d . . . C27 C 0.62190(14) 0.47741(12) 0.25779(11) 0.0151(3) Uani 1 1 d . . . C28 C 0.71651(14) 0.44923(13) 0.24630(11) 0.0174(3) Uani 1 1 d . . . H28 H 0.7135 0.4018 0.2087 0.021 Uiso 1 1 calc R . . C29 C 0.81466(15) 0.48938(14) 0.28896(12) 0.0225(4) Uani 1 1 d . . . H29 H 0.8779 0.4696 0.2800 0.027 Uiso 1 1 calc R . . C30 C 0.82061(17) 0.55832(15) 0.34459(13) 0.0267(4) Uani 1 1 d . . . H30 H 0.8878 0.5856 0.3741 0.032 Uiso 1 1 calc R . . C31 C 0.72801(18) 0.58695(15) 0.35670(14) 0.0280(4) Uani 1 1 d . . . H31 H 0.7318 0.6341 0.3947 0.034 Uiso 1 1 calc R . . C32 C 0.62929(16) 0.54734(13) 0.31368(13) 0.0222(4) Uani 1 1 d . . . H32 H 0.5662 0.5680 0.3224 0.027 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 0.00954(3) 0.01047(3) 0.00984(3) 0.00068(2) 0.00434(2) 0.00029(2) I1 0.01494(5) 0.01291(5) 0.01699(5) 0.00350(4) 0.00760(4) 0.00253(4) P1 0.01158(19) 0.01344(19) 0.01018(18) -0.00044(14) 0.00464(15) 0.00045(15) P2 0.01341(19) 0.0142(2) 0.01234(19) 0.00223(15) 0.00719(15) 0.00227(16) C1 0.0109(7) 0.0134(7) 0.0110(7) -0.0005(6) 0.0026(6) -0.0012(6) C2 0.0133(7) 0.0140(8) 0.0132(7) 0.0012(6) 0.0048(6) 0.0006(6) C3 0.0176(8) 0.0160(8) 0.0163(8) 0.0036(6) 0.0071(7) -0.0001(6) C4 0.0174(8) 0.0129(8) 0.0191(8) 0.0046(6) 0.0049(7) 0.0020(6) C5 0.0138(8) 0.0142(8) 0.0179(8) 0.0003(6) 0.0057(6) 0.0022(6) C6 0.0132(7) 0.0135(7) 0.0130(7) 0.0001(6) 0.0052(6) 0.0003(6) C7 0.0179(8) 0.0152(8) 0.0150(8) 0.0023(6) 0.0097(6) 0.0007(6) C8 0.0186(8) 0.0178(8) 0.0194(8) 0.0059(7) 0.0117(7) 0.0068(7) C9 0.0146(8) 0.0187(8) 0.0127(8) -0.0031(6) 0.0035(6) 0.0000(6) C10 0.0231(9) 0.0283(10) 0.0133(8) -0.0027(7) 0.0047(7) 0.0018(8) C11 0.0136(8) 0.0265(10) 0.0189(9) -0.0050(7) 0.0021(7) 0.0017(7) C12 0.0185(8) 0.0219(9) 0.0187(9) -0.0054(7) 0.0057(7) -0.0046(7) C13 0.0130(7) 0.0170(8) 0.0140(8) -0.0011(6) 0.0076(6) 0.0003(6) C14 0.0178(8) 0.0179(8) 0.0190(8) -0.0022(7) 0.0083(7) 0.0026(7) C15 0.0220(9) 0.0243(9) 0.0185(9) 0.0007(7) 0.0128(7) 0.0005(7) C16 0.0140(8) 0.0223(9) 0.0175(8) -0.0015(7) 0.0067(6) -0.0005(7) C17 0.0131(8) 0.0186(8) 0.0166(8) 0.0020(6) 0.0078(6) 0.0003(6) C18 0.0169(8) 0.0271(10) 0.0192(9) -0.0024(7) 0.0060(7) -0.0012(7) C19 0.0162(8) 0.0249(9) 0.0227(9) 0.0031(7) 0.0116(7) 0.0018(7) C20 0.0193(8) 0.0170(8) 0.0204(9) 0.0028(7) 0.0101(7) -0.0004(7) C21 0.0178(8) 0.0165(8) 0.0154(8) -0.0006(6) 0.0079(6) -0.0005(6) C22 0.0260(10) 0.0176(9) 0.0263(10) -0.0042(7) 0.0144(8) -0.0023(7) C23 0.0276(10) 0.0259(10) 0.0176(9) -0.0032(7) 0.0131(8) -0.0015(8) C24 0.0199(9) 0.0218(9) 0.0164(8) 0.0000(7) 0.0035(7) 0.0010(7) C25 0.0158(8) 0.0156(8) 0.0115(7) 0.0009(6) 0.0068(6) 0.0021(6) C26 0.0161(8) 0.0177(8) 0.0152(8) 0.0004(6) 0.0065(6) -0.0001(6) C27 0.0144(8) 0.0165(8) 0.0134(7) 0.0017(6) 0.0034(6) -0.0029(6) C28 0.0151(8) 0.0199(9) 0.0158(8) 0.0018(6) 0.0037(6) -0.0012(7) C29 0.0147(8) 0.0290(10) 0.0225(9) 0.0047(8) 0.0047(7) -0.0024(7) C30 0.0206(9) 0.0336(11) 0.0201(9) 0.0010(8) -0.0004(7) -0.0127(8) C31 0.0313(11) 0.0275(11) 0.0222(10) -0.0079(8) 0.0053(8) -0.0114(9) C32 0.0206(9) 0.0235(10) 0.0225(9) -0.0048(7) 0.0073(7) -0.0042(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 C25 1.9236(18) . ? Ir1 C1 2.0417(17) . ? Ir1 P1 2.3397(4) . ? Ir1 P2 2.3643(4) . ? Ir1 I1 2.74175(16) . ? P1 C7 1.8338(18) . ? P1 C13 1.8850(17) . ? P1 C9 1.8858(18) . ? P2 C8 1.8404(18) . ? P2 C21 1.8733(18) . ? P2 C17 1.8859(18) . ? C1 C6 1.411(2) . ? C1 C2 1.414(2) . ? C2 C3 1.394(2) . ? C2 C7 1.504(2) . ? C3 C4 1.389(3) . ? C4 C5 1.391(2) . ? C5 C6 1.395(2) . ? C6 C8 1.505(2) . ? C9 C10 1.536(3) . ? C9 C12 1.538(3) . ? C9 C11 1.541(3) . ? C13 C16 1.533(2) . ? C13 C14 1.536(2) . ? C13 C15 1.542(2) . ? C17 C20 1.534(3) . ? C17 C19 1.539(2) . ? C17 C18 1.543(3) . ? C21 C24 1.533(3) . ? C21 C23 1.538(3) . ? C21 C22 1.541(3) . ? C25 C26 1.208(2) . ? C26 C27 1.440(2) . ? C27 C32 1.399(3) . ? C27 C28 1.400(3) . ? C28 C29 1.388(3) . ? C29 C30 1.388(3) . ? C30 C31 1.382(3) . ? C31 C32 1.391(3) . ? 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 C1 85.29(7) . . ? C25 Ir1 P1 92.00(5) . . ? C1 Ir1 P1 82.37(5) . . ? C25 Ir1 P2 97.75(5) . . ? C1 Ir1 P2 82.79(5) . . ? P1 Ir1 P2 161.484(16) . . ? C25 Ir1 I1 96.97(5) . . ? C1 Ir1 I1 176.07(5) . . ? P1 Ir1 I1 94.320(11) . . ? P2 Ir1 I1 100.042(11) . . ? C7 P1 C13 103.87(8) . . ? C7 P1 C9 106.50(8) . . ? C13 P1 C9 110.17(8) . . ? C7 P1 Ir1 99.59(6) . . ? C13 P1 Ir1 125.56(6) . . ? C9 P1 Ir1 108.96(6) . . ? C8 P2 C21 106.26(9) . . ? C8 P2 C17 102.36(8) . . ? C21 P2 C17 111.86(8) . . ? C8 P2 Ir1 101.88(6) . . ? C21 P2 Ir1 121.24(6) . . ? C17 P2 Ir1 110.82(6) . . ? C6 C1 C2 117.60(15) . . ? C6 C1 Ir1 122.25(12) . . ? C2 C1 Ir1 120.14(12) . . ? C3 C2 C1 120.76(16) . . ? C3 C2 C7 120.07(15) . . ? C1 C2 C7 119.17(15) . . ? C4 C3 C2 120.65(16) . . ? C3 C4 C5 119.55(16) . . ? C4 C5 C6 120.37(16) . . ? C5 C6 C1 121.04(16) . . ? C5 C6 C8 118.87(15) . . ? C1 C6 C8 119.98(15) . . ? C2 C7 P1 108.87(12) . . ? C6 C8 P2 110.57(12) . . ? C10 C9 C12 110.03(15) . . ? C10 C9 C11 107.25(15) . . ? C12 C9 C11 107.60(16) . . ? C10 C9 P1 113.01(13) . . ? C12 C9 P1 110.53(12) . . ? C11 C9 P1 108.20(12) . . ? C16 C13 C14 108.06(15) . . ? C16 C13 C15 107.74(15) . . ? C14 C13 C15 109.34(15) . . ? C16 C13 P1 107.85(12) . . ? C14 C13 P1 112.47(12) . . ? C15 C13 P1 111.20(12) . . ? C20 C17 C19 109.15(15) . . ? C20 C17 C18 108.76(15) . . ? C19 C17 C18 108.47(15) . . ? C20 C17 P2 111.23(12) . . ? C19 C17 P2 114.46(13) . . ? C18 C17 P2 104.51(12) . . ? C24 C21 C23 110.61(16) . . ? C24 C21 C22 108.62(15) . . ? C23 C21 C22 107.96(15) . . ? C24 C21 P2 108.68(12) . . ? C23 C21 P2 113.87(13) . . ? C22 C21 P2 106.91(13) . . ? C26 C25 Ir1 178.89(16) . . ? C25 C26 C27 176.16(19) . . ? C32 C27 C28 117.93(17) . . ? C32 C27 C26 121.09(17) . . ? C28 C27 C26 120.97(17) . . ? C29 C28 C27 121.10(18) . . ? C28 C29 C30 120.19(19) . . ? C31 C30 C29 119.47(18) . . ? C30 C31 C32 120.6(2) . . ? C31 C32 C27 120.72(19) . . ? 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 C25 Ir1 P1 C7 -60.61(8) . . . . ? C1 Ir1 P1 C7 24.37(7) . . . . ? P2 Ir1 P1 C7 61.33(8) . . . . ? I1 Ir1 P1 C7 -157.76(6) . . . . ? C25 Ir1 P1 C13 54.21(9) . . . . ? C1 Ir1 P1 C13 139.19(8) . . . . ? P2 Ir1 P1 C13 176.15(8) . . . . ? I1 Ir1 P1 C13 -42.94(7) . . . . ? C25 Ir1 P1 C9 -171.86(8) . . . . ? C1 Ir1 P1 C9 -86.89(8) . . . . ? P2 Ir1 P1 C9 -49.93(8) . . . . ? I1 Ir1 P1 C9 90.99(6) . . . . ? C25 Ir1 P2 C8 95.54(8) . . . . ? C1 Ir1 P2 C8 11.32(8) . . . . ? P1 Ir1 P2 C8 -25.60(9) . . . . ? I1 Ir1 P2 C8 -165.92(7) . . . . ? C25 Ir1 P2 C21 -22.01(9) . . . . ? C1 Ir1 P2 C21 -106.22(8) . . . . ? P1 Ir1 P2 C21 -143.14(8) . . . . ? I1 Ir1 P2 C21 76.54(7) . . . . ? C25 Ir1 P2 C17 -156.16(8) . . . . ? C1 Ir1 P2 C17 119.62(8) . . . . ? P1 Ir1 P2 C17 82.70(8) . . . . ? I1 Ir1 P2 C17 -57.62(6) . . . . ? C25 Ir1 C1 C6 -104.39(14) . . . . ? P1 Ir1 C1 C6 162.95(14) . . . . ? P2 Ir1 C1 C6 -5.95(13) . . . . ? I1 Ir1 C1 C6 130.3(6) . . . . ? C25 Ir1 C1 C2 75.57(14) . . . . ? P1 Ir1 C1 C2 -17.09(12) . . . . ? P2 Ir1 C1 C2 174.01(13) . . . . ? I1 Ir1 C1 C2 -49.8(7) . . . . ? C6 C1 C2 C3 -0.8(2) . . . . ? Ir1 C1 C2 C3 179.25(13) . . . . ? C6 C1 C2 C7 179.65(15) . . . . ? Ir1 C1 C2 C7 -0.3(2) . . . . ? C1 C2 C3 C4 1.6(3) . . . . ? C7 C2 C3 C4 -178.85(17) . . . . ? C2 C3 C4 C5 -1.5(3) . . . . ? C3 C4 C5 C6 0.6(3) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? C4 C5 C6 C8 -175.91(17) . . . . ? C2 C1 C6 C5 -0.1(2) . . . . ? Ir1 C1 C6 C5 179.85(13) . . . . ? C2 C1 C6 C8 175.98(15) . . . . ? Ir1 C1 C6 C8 -4.1(2) . . . . ? C3 C2 C7 P1 -155.94(14) . . . . ? C1 C2 C7 P1 23.6(2) . . . . ? C13 P1 C7 C2 -161.53(12) . . . . ? C9 P1 C7 C2 82.14(13) . . . . ? Ir1 P1 C7 C2 -31.04(12) . . . . ? C5 C6 C8 P2 -169.20(13) . . . . ? C1 C6 C8 P2 14.6(2) . . . . ? C21 P2 C8 C6 111.62(13) . . . . ? C17 P2 C8 C6 -130.92(13) . . . . ? Ir1 P2 C8 C6 -16.22(14) . . . . ? C7 P1 C9 C10 66.09(15) . . . . ? C13 P1 C9 C10 -45.95(15) . . . . ? Ir1 P1 C9 C10 172.67(12) . . . . ? C7 P1 C9 C12 -170.11(12) . . . . ? C13 P1 C9 C12 77.86(14) . . . . ? Ir1 P1 C9 C12 -63.52(13) . . . . ? C7 P1 C9 C11 -52.52(14) . . . . ? C13 P1 C9 C11 -164.55(12) . . . . ? Ir1 P1 C9 C11 54.07(13) . . . . ? C7 P1 C13 C16 82.51(13) . . . . ? C9 P1 C13 C16 -163.77(12) . . . . ? Ir1 P1 C13 C16 -30.29(15) . . . . ? C7 P1 C13 C14 -158.44(13) . . . . ? C9 P1 C13 C14 -44.72(15) . . . . ? Ir1 P1 C13 C14 88.76(13) . . . . ? C7 P1 C13 C15 -35.42(14) . . . . ? C9 P1 C13 C15 78.30(14) . . . . ? Ir1 P1 C13 C15 -148.22(10) . . . . ? C8 P2 C17 C20 -163.68(13) . . . . ? C21 P2 C17 C20 -50.30(15) . . . . ? Ir1 P2 C17 C20 88.33(12) . . . . ? C8 P2 C17 C19 -39.38(15) . . . . ? C21 P2 C17 C19 74.00(15) . . . . ? Ir1 P2 C17 C19 -147.37(12) . . . . ? C8 P2 C17 C18 79.13(13) . . . . ? C21 P2 C17 C18 -167.49(12) . . . . ? Ir1 P2 C17 C18 -28.86(13) . . . . ? C8 P2 C21 C24 -165.54(13) . . . . ? C17 P2 C21 C24 83.53(14) . . . . ? Ir1 P2 C21 C24 -50.20(14) . . . . ? C8 P2 C21 C23 70.68(15) . . . . ? C17 P2 C21 C23 -40.25(16) . . . . ? Ir1 P2 C21 C23 -173.98(11) . . . . ? C8 P2 C21 C22 -48.46(14) . . . . ? C17 P2 C21 C22 -159.39(12) . . . . ? Ir1 P2 C21 C22 66.87(13) . . . . ? C1 Ir1 C25 C26 -93(9) . . . . ? P1 Ir1 C25 C26 -11(9) . . . . ? P2 Ir1 C25 C26 -175(100) . . . . ? I1 Ir1 C25 C26 84(9) . . . . ? Ir1 C25 C26 C27 -88(9) . . . . ? C25 C26 C27 C32 -123(3) . . . . ? C25 C26 C27 C28 56(3) . . . . ? C32 C27 C28 C29 0.0(3) . . . . ? C26 C27 C28 C29 -179.00(17) . . . . ? C27 C28 C29 C30 0.4(3) . . . . ? C28 C29 C30 C31 -0.4(3) . . . . ? C29 C30 C31 C32 0.0(3) . . . . ? C30 C31 C32 C27 0.4(3) . . . . ? C28 C27 C32 C31 -0.4(3) . . . . ? C26 C27 C32 C31 178.56(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.253 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.086 #==END