# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jens Langer' _publ_contact_author_email JENS.LANGER@YAHOO.DE _publ_section_title ; A C-H activation / CO2-carboxylation reaction sequence mediated by an 'Iridium(dppm)' species. Formation of the anionic ligand (Ph2P)2C-COOH. ; loop_ _publ_author_name 'Jens Langer' 'Pilar Garcia-Orduna' 'Maria Jose Fabra' 'F Lahoz' 'Luis Oro' # Attachment 'compnd_1d_2.cif' data_compound_1d _database_code_depnum_ccdc_archive 'CCDC 689715' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H44 Cl Ir P4, C7 H8, 0.5 (C7 H8)' _chemical_formula_sum 'C60.50 H56 Cl Ir P4' _chemical_formula_weight 1134.58 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6704(7) _cell_length_b 11.7099(8) _cell_length_c 20.3601(14) _cell_angle_alpha 85.152(1) _cell_angle_beta 76.129(1) _cell_angle_gamma 88.756(1) _cell_volume 2461.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6206 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 23.61 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1146 _exptl_absorpt_coefficient_mu 2.938 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5578 _exptl_absorpt_correction_T_max 0.8670 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 30715 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.91 _reflns_number_total 11798 _reflns_number_gt 10945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. All non-hydrogen atoms, including those of solvent molecules (1.5 toluene molecules), were refined with anisotropic displacement parameters. Most of hydrogens were found in the difference Fourier maps showing reasonable positional parameters. Hydrogens of the metal complex were allowed to refine as free isotropic atoms, although a reduced number of C-H distances showed slightly out-of-usual-range values. Displacement parameters showed a broad range in Ueq, but these values were not restricted. Hydride was included in the refinement in a position obtained from electros- tatic potential calculations (HYDEX program) and allowed to freely refine with a weak restriction in the Ir-H bond distance. Hydrogens for the solvent molecules were included from observed positions, and refined with riding thermal parameters, and geometrical restrictions only for the terminal methyl groups. All the residuals over 1 e/A3 were in close proximity of the metal atom with no chemical sense. ; _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^)+(0.0408P)^2^+1.2366P] 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 11798 _refine_ls_number_parameters 802 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.105 _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 Cl1 Cl 0.33097(8) 0.34928(7) 0.37205(4) 0.01907(15) Uani 1 1 d . . . Ir1 Ir 0.351556(11) 0.426743(10) 0.251993(6) 0.01295(4) Uani 1 1 d D . . H0 H 0.366(4) 0.478(3) 0.1844(17) 0.032(11) Uiso 1 1 d D . . P1 P 0.53116(8) 0.54246(7) 0.24817(4) 0.01438(16) Uani 1 1 d . . . P2 P 0.54447(8) 0.33599(7) 0.20260(4) 0.01510(16) Uani 1 1 d . . . P3 P 0.17901(8) 0.31632(7) 0.24270(4) 0.01590(16) Uani 1 1 d . . . P4 P 0.15895(8) 0.52196(7) 0.29404(4) 0.01565(16) Uani 1 1 d . . . C1 C 0.6440(3) 0.4455(3) 0.21020(17) 0.0184(6) Uani 1 1 d . . . H1 H 0.726(4) 0.449(3) 0.201(2) 0.021(10) Uiso 1 1 d . . . C3 C 0.0603(3) 0.3908(3) 0.30625(17) 0.0189(7) Uani 1 1 d . . . H3A H 0.056(4) 0.357(3) 0.349(2) 0.027(11) Uiso 1 1 d . . . H3B H -0.018(4) 0.399(3) 0.3008(19) 0.020(10) Uiso 1 1 d . . . C4 C 0.5705(3) 0.5852(3) 0.32554(15) 0.0159(6) Uani 1 1 d . . . C5 C 0.5704(3) 0.6975(3) 0.34278(18) 0.0209(7) Uani 1 1 d . . . H5 H 0.549(4) 0.756(4) 0.320(2) 0.045(14) Uiso 1 1 d . . . C6 C 0.6013(4) 0.7225(3) 0.40263(19) 0.0258(8) Uani 1 1 d . . . H6 H 0.602(4) 0.802(4) 0.411(2) 0.028(11) Uiso 1 1 d . . . C7 C 0.6318(4) 0.6352(3) 0.44590(19) 0.0276(8) Uani 1 1 d . . . H7 H 0.643(4) 0.645(4) 0.485(2) 0.030(11) Uiso 1 1 d . . . C8 C 0.6327(4) 0.5235(3) 0.42929(19) 0.0280(8) Uani 1 1 d . . . H8 H 0.657(4) 0.466(4) 0.452(2) 0.034(12) Uiso 1 1 d . . . C9 C 0.6035(4) 0.4981(3) 0.36949(18) 0.0237(7) Uani 1 1 d . . . H9 H 0.605(5) 0.423(4) 0.353(2) 0.050(14) Uiso 1 1 d . . . C10 C 0.5407(3) 0.6798(3) 0.19720(15) 0.0158(6) Uani 1 1 d . . . C11 C 0.4459(3) 0.7636(3) 0.20997(17) 0.0192(7) Uani 1 1 d . . . H11 H 0.373(3) 0.751(3) 0.2371(18) 0.010(8) Uiso 1 1 d . . . C12 C 0.4617(4) 0.8704(3) 0.17422(18) 0.0242(7) Uani 1 1 d . . . H12 H 0.396(4) 0.920(3) 0.186(2) 0.026(11) Uiso 1 1 d . . . C13 C 0.5732(4) 0.8940(3) 0.12398(18) 0.0248(7) Uani 1 1 d . . . H13 H 0.586(3) 0.966(3) 0.1014(18) 0.016(9) Uiso 1 1 d . . . C14 C 0.6665(4) 0.8104(3) 0.10902(18) 0.0236(7) Uani 1 1 d . . . H14 H 0.740(4) 0.827(3) 0.0762(19) 0.016(9) Uiso 1 1 d . . . C15 C 0.6510(3) 0.7042(3) 0.14507(17) 0.0198(7) Uani 1 1 d . . . H15 H 0.708(3) 0.653(3) 0.1382(18) 0.013(9) Uiso 1 1 d . . . C16 C 0.5960(3) 0.1958(3) 0.23355(17) 0.0193(7) Uani 1 1 d . . . C17 C 0.5163(4) 0.1278(3) 0.28500(19) 0.0280(8) Uani 1 1 d . . . H17 H 0.436(4) 0.156(4) 0.306(2) 0.039(12) Uiso 1 1 d . . . C18 C 0.5613(4) 0.0220(3) 0.3070(2) 0.0314(9) Uani 1 1 d . . . H18 H 0.501(4) -0.025(4) 0.346(2) 0.046(13) Uiso 1 1 d . . . C19 C 0.6841(4) -0.0139(3) 0.2788(2) 0.0297(8) Uani 1 1 d . . . H19 H 0.706(5) -0.080(4) 0.302(3) 0.054(15) Uiso 1 1 d . . . C20 C 0.7629(4) 0.0523(3) 0.2269(2) 0.0293(8) Uani 1 1 d . . . H20 H 0.843(4) 0.029(3) 0.209(2) 0.024(10) Uiso 1 1 d . . . C21 C 0.7181(4) 0.1567(3) 0.2041(2) 0.0262(8) Uani 1 1 d . . . H21 H 0.767(4) 0.203(3) 0.171(2) 0.019(10) Uiso 1 1 d . . . C22 C 0.5587(3) 0.3088(3) 0.11368(16) 0.0172(6) Uani 1 1 d . . . C23 C 0.6018(4) 0.3952(3) 0.06283(18) 0.0233(7) Uani 1 1 d . . . H23 H 0.620(4) 0.461(4) 0.078(2) 0.033(11) Uiso 1 1 d . . . C24 C 0.6035(4) 0.3792(3) -0.00422(19) 0.0268(8) Uani 1 1 d . . . H24 H 0.626(4) 0.430(4) -0.036(2) 0.031(11) Uiso 1 1 d . . . C25 C 0.5626(4) 0.2778(3) -0.02104(18) 0.0237(7) Uani 1 1 d . . . H25 H 0.566(4) 0.270(3) -0.064(2) 0.026(10) Uiso 1 1 d . . . C26 C 0.5193(4) 0.1912(3) 0.02913(19) 0.0254(8) Uani 1 1 d . . . H26 H 0.491(4) 0.122(3) 0.0204(19) 0.023(10) Uiso 1 1 d . . . C27 C 0.5178(3) 0.2057(3) 0.09606(18) 0.0220(7) Uani 1 1 d . . . H27 H 0.483(4) 0.148(3) 0.131(2) 0.025(10) Uiso 1 1 d . . . C28 C 0.1598(3) 0.1628(3) 0.26439(18) 0.0200(7) Uani 1 1 d . . . C29 C 0.1782(4) 0.1167(3) 0.3264(2) 0.0341(9) Uani 1 1 d . . . H29 H 0.200(4) 0.161(4) 0.353(2) 0.042(13) Uiso 1 1 d . . . C30 C 0.1702(5) -0.0011(4) 0.3430(2) 0.0394(10) Uani 1 1 d . . . H30 H 0.189(5) -0.028(4) 0.388(3) 0.053(15) Uiso 1 1 d . . . C31 C 0.1419(4) -0.0727(3) 0.2982(2) 0.0347(10) Uani 1 1 d . . . H31 H 0.122(5) -0.134(5) 0.311(3) 0.052(16) Uiso 1 1 d . . . C32 C 0.1209(4) -0.0279(3) 0.2377(2) 0.0368(10) Uani 1 1 d . . . H32 H 0.106(4) -0.069(4) 0.207(2) 0.036(12) Uiso 1 1 d . . . C33 C 0.1310(4) 0.0888(3) 0.2203(2) 0.0297(8) Uani 1 1 d . . . H33 H 0.120(5) 0.116(4) 0.177(2) 0.046(14) Uiso 1 1 d . . . C34 C 0.1289(3) 0.3417(3) 0.16322(16) 0.0175(6) Uani 1 1 d . . . C35 C 0.0003(3) 0.3548(3) 0.16102(18) 0.0234(7) Uani 1 1 d . . . H35 H -0.063(4) 0.351(3) 0.1999(19) 0.018(9) Uiso 1 1 d . . . C36 C -0.0322(4) 0.3731(3) 0.0989(2) 0.0283(8) Uani 1 1 d . . . H36 H -0.108(4) 0.381(4) 0.099(2) 0.036(12) Uiso 1 1 d . . . C37 C 0.0623(4) 0.3758(3) 0.03881(19) 0.0256(8) Uani 1 1 d . . . H37 H 0.040(4) 0.389(4) -0.002(2) 0.035(12) Uiso 1 1 d . . . C38 C 0.1899(4) 0.3621(3) 0.04085(18) 0.0241(7) Uani 1 1 d . . . H38 H 0.253(4) 0.365(3) 0.003(2) 0.027(11) Uiso 1 1 d . . . C39 C 0.2230(3) 0.3462(3) 0.10288(17) 0.0213(7) Uani 1 1 d . . . H39 H 0.309(4) 0.339(3) 0.105(2) 0.028(11) Uiso 1 1 d . . . C40 C 0.1227(3) 0.5883(3) 0.37349(16) 0.0177(6) Uani 1 1 d . . . C41 C -0.0002(4) 0.5849(3) 0.41702(18) 0.0254(7) Uani 1 1 d . . . H41 H -0.068(4) 0.544(3) 0.4082(19) 0.022(10) Uiso 1 1 d . . . C42 C -0.0244(4) 0.6425(4) 0.47576(19) 0.0312(8) Uani 1 1 d . . . H42 H -0.110(4) 0.644(4) 0.505(2) 0.037(12) Uiso 1 1 d . . . C43 C 0.0717(4) 0.7041(3) 0.49074(19) 0.0298(8) Uani 1 1 d . . . H43 H 0.055(4) 0.742(4) 0.530(2) 0.030(11) Uiso 1 1 d . . . C44 C 0.1951(4) 0.7062(3) 0.44872(19) 0.0266(8) Uani 1 1 d . . . H44 H 0.264(3) 0.746(3) 0.4590(17) 0.012(9) Uiso 1 1 d . . . C45 C 0.2205(3) 0.6464(3) 0.39082(17) 0.0211(7) Uani 1 1 d . . . H45 H 0.304(4) 0.651(4) 0.362(2) 0.035(12) Uiso 1 1 d . . . C46 C 0.0893(3) 0.6180(3) 0.23672(16) 0.0181(6) Uani 1 1 d . . . C47 C 0.1603(3) 0.6487(3) 0.17166(18) 0.0214(7) Uani 1 1 d . . . H47 H 0.244(4) 0.627(3) 0.1571(19) 0.023(10) Uiso 1 1 d . . . C48 C 0.1054(4) 0.7175(3) 0.12661(19) 0.0251(7) Uani 1 1 d . . . H48 H 0.155(4) 0.737(3) 0.086(2) 0.023(10) Uiso 1 1 d . . . C49 C -0.0192(4) 0.7551(3) 0.1462(2) 0.0250(7) Uani 1 1 d . . . H49 H -0.046(5) 0.800(5) 0.118(3) 0.061(17) Uiso 1 1 d . . . C50 C -0.0906(3) 0.7260(3) 0.21220(19) 0.0261(8) Uani 1 1 d . . . H50 H -0.180(3) 0.746(3) 0.2218(17) 0.013(8) Uiso 1 1 d . . . C51 C -0.0383(3) 0.6579(3) 0.25707(18) 0.0227(7) Uani 1 1 d . . . H51 H -0.086(4) 0.632(4) 0.301(2) 0.028(11) Uiso 1 1 d . . . C52 C 0.7366(4) 0.1002(4) 0.4311(2) 0.0353(9) Uani 1 1 d . . . C53 C 0.8438(5) 0.0349(4) 0.4065(3) 0.0472(12) Uani 1 1 d . . . H53 H 0.910(5) 0.065(4) 0.355(3) 0.057 Uiso 1 1 d . . . C54 C 0.8675(5) -0.0697(4) 0.4382(3) 0.0490(12) Uani 1 1 d . . . H54 H 0.963(5) -0.118(4) 0.419(3) 0.059 Uiso 1 1 d . . . C55 C 0.7809(5) -0.1106(4) 0.4973(2) 0.0402(10) Uani 1 1 d . . . H55 H 0.800(4) -0.193(4) 0.524(2) 0.048 Uiso 1 1 d . . . C56 C 0.6714(5) -0.0485(4) 0.5222(2) 0.0413(10) Uani 1 1 d . . . H56 H 0.591(5) -0.079(4) 0.558(3) 0.050 Uiso 1 1 d . . . C57 C 0.6504(5) 0.0559(4) 0.4898(2) 0.0434(11) Uani 1 1 d . . . H57 H 0.5752 0.0985 0.5081 0.052 Uiso 1 1 calc R . . C58 C 0.7147(5) 0.2124(4) 0.3952(3) 0.0494(12) Uani 1 1 d . . . H58A H 0.7680 0.2713 0.4067 0.059 Uiso 1 1 calc R . . H58B H 0.6234 0.2337 0.4094 0.059 Uiso 1 1 calc R . . H58C H 0.7383 0.2061 0.3461 0.059 Uiso 1 1 calc R . . C59 C 0.1029(6) -0.0693(4) -0.0243(2) 0.0457(12) Uani 1 1 d . . . H59 H 0.157(5) -0.111(4) -0.038(3) 0.044(15) Uiso 1 1 d . . . C60 C 0.1104(5) 0.0043(4) 0.0248(2) 0.0416(11) Uani 1 1 d . . . C61 C 0.0051(6) 0.0733(4) 0.0482(2) 0.0455(12) Uani 1 1 d . . . H61 H 0.008(5) 0.120(4) 0.077(2) 0.044(14) Uiso 1 1 d . . . C62 C 0.2158(7) 0.0066(6) 0.0483(4) 0.0288(16) Uani 0.50 1 d P . . H62A H 0.2386 0.0863 0.0512 0.043 Uiso 0.50 1 calc PR . . H62B H 0.2870 -0.0303 0.0174 0.043 Uiso 0.50 1 calc PR . . H62C H 0.1997 -0.0345 0.0934 0.043 Uiso 0.50 1 calc PR . . 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 Cl1 0.0252(4) 0.0184(4) 0.0134(3) 0.0002(3) -0.0046(3) -0.0008(3) Ir1 0.01586(7) 0.01140(6) 0.01138(6) -0.00148(4) -0.00259(4) -0.00061(4) P1 0.0170(4) 0.0134(4) 0.0128(4) -0.0010(3) -0.0039(3) -0.0008(3) P2 0.0189(4) 0.0131(4) 0.0129(4) -0.0017(3) -0.0029(3) 0.0006(3) P3 0.0188(4) 0.0140(4) 0.0150(4) -0.0015(3) -0.0041(3) -0.0014(3) P4 0.0171(4) 0.0153(4) 0.0138(4) -0.0023(3) -0.0018(3) -0.0011(3) C1 0.0193(17) 0.0159(16) 0.0195(16) -0.0024(13) -0.0033(13) 0.0001(12) C3 0.0200(17) 0.0192(16) 0.0162(16) -0.0029(13) -0.0010(13) -0.0044(13) C4 0.0159(15) 0.0193(16) 0.0121(14) -0.0014(12) -0.0023(11) -0.0011(12) C5 0.0267(18) 0.0180(17) 0.0189(17) -0.0024(13) -0.0071(14) -0.0007(13) C6 0.0308(19) 0.0244(19) 0.0246(18) -0.0092(15) -0.0087(15) -0.0007(15) C7 0.030(2) 0.037(2) 0.0172(17) -0.0049(15) -0.0083(15) -0.0047(16) C8 0.032(2) 0.030(2) 0.0243(19) 0.0060(16) -0.0125(16) -0.0033(16) C9 0.0298(19) 0.0232(18) 0.0204(17) -0.0002(14) -0.0109(14) -0.0019(14) C10 0.0209(16) 0.0159(15) 0.0125(14) -0.0014(12) -0.0074(12) -0.0036(12) C11 0.0216(17) 0.0204(17) 0.0158(15) -0.0028(13) -0.0044(13) 0.0010(13) C12 0.032(2) 0.0204(17) 0.0221(18) -0.0029(14) -0.0095(15) 0.0033(15) C13 0.038(2) 0.0168(17) 0.0208(17) 0.0039(14) -0.0106(15) -0.0060(15) C14 0.0253(18) 0.0250(18) 0.0200(17) 0.0021(14) -0.0048(14) -0.0059(14) C15 0.0208(17) 0.0209(17) 0.0186(16) -0.0036(13) -0.0062(13) 0.0013(13) C16 0.0274(18) 0.0149(15) 0.0172(16) -0.0023(12) -0.0083(13) 0.0002(13) C17 0.033(2) 0.0211(18) 0.0253(19) -0.0009(15) 0.0016(16) 0.0042(15) C18 0.049(2) 0.0187(18) 0.0229(19) 0.0017(15) -0.0020(17) 0.0012(16) C19 0.045(2) 0.0166(17) 0.030(2) -0.0019(15) -0.0143(18) 0.0049(16) C20 0.0247(19) 0.0226(18) 0.040(2) -0.0033(16) -0.0068(17) 0.0059(15) C21 0.0242(18) 0.0254(19) 0.0273(19) 0.0015(15) -0.0042(15) 0.0012(15) C22 0.0151(15) 0.0194(16) 0.0178(16) -0.0046(12) -0.0045(12) 0.0020(12) C23 0.0291(19) 0.0208(18) 0.0203(17) -0.0021(14) -0.0060(14) -0.0040(14) C24 0.031(2) 0.029(2) 0.0184(17) 0.0029(15) -0.0032(15) -0.0031(16) C25 0.0276(18) 0.0306(19) 0.0139(16) -0.0055(14) -0.0057(14) 0.0025(15) C26 0.033(2) 0.0197(18) 0.0255(19) -0.0077(14) -0.0092(15) 0.0004(15) C27 0.0276(18) 0.0175(16) 0.0210(17) -0.0021(14) -0.0059(14) -0.0001(14) C28 0.0201(16) 0.0149(15) 0.0263(18) -0.0018(13) -0.0078(13) -0.0004(12) C29 0.054(3) 0.0217(19) 0.031(2) 0.0026(16) -0.0204(19) -0.0127(18) C30 0.054(3) 0.026(2) 0.043(3) 0.0099(18) -0.024(2) -0.0106(19) C31 0.041(2) 0.0147(18) 0.050(3) 0.0017(18) -0.014(2) -0.0068(16) C32 0.050(3) 0.022(2) 0.045(3) -0.0093(18) -0.021(2) -0.0014(17) C33 0.043(2) 0.0185(18) 0.033(2) -0.0043(15) -0.0188(18) -0.0011(16) C34 0.0221(16) 0.0144(15) 0.0174(16) -0.0017(12) -0.0076(13) -0.0010(12) C35 0.0237(18) 0.0258(18) 0.0201(17) -0.0035(14) -0.0041(14) 0.0033(14) C36 0.026(2) 0.032(2) 0.031(2) -0.0042(16) -0.0131(16) 0.0047(16) C37 0.034(2) 0.0240(18) 0.0217(18) -0.0027(14) -0.0118(15) 0.0026(15) C38 0.0299(19) 0.0236(18) 0.0172(17) -0.0030(14) -0.0019(14) -0.0050(14) C39 0.0211(17) 0.0230(17) 0.0200(17) -0.0029(13) -0.0050(13) -0.0009(13) C40 0.0237(16) 0.0166(15) 0.0120(14) -0.0030(12) -0.0027(12) 0.0036(12) C41 0.0217(18) 0.031(2) 0.0230(18) -0.0055(15) -0.0034(14) -0.0006(15) C42 0.031(2) 0.037(2) 0.0217(18) -0.0059(16) 0.0015(15) 0.0056(17) C43 0.042(2) 0.031(2) 0.0175(18) -0.0101(15) -0.0064(16) 0.0061(17) C44 0.035(2) 0.0237(19) 0.0236(18) -0.0042(15) -0.0099(15) -0.0028(15) C45 0.0251(18) 0.0206(17) 0.0162(16) 0.0000(13) -0.0028(13) 0.0008(13) C46 0.0201(16) 0.0180(16) 0.0177(16) -0.0031(13) -0.0072(13) 0.0007(12) C47 0.0207(17) 0.0203(17) 0.0232(17) -0.0007(14) -0.0056(14) 0.0012(13) C48 0.0265(19) 0.0255(19) 0.0220(18) 0.0029(15) -0.0046(15) -0.0001(15) C49 0.0272(19) 0.0226(18) 0.0272(19) 0.0017(15) -0.0116(15) 0.0003(14) C50 0.0188(17) 0.030(2) 0.030(2) -0.0082(16) -0.0066(15) 0.0043(14) C51 0.0204(17) 0.0264(18) 0.0206(17) -0.0022(14) -0.0035(14) 0.0021(14) C52 0.048(3) 0.029(2) 0.033(2) -0.0037(17) -0.0188(19) -0.0006(18) C53 0.046(3) 0.044(3) 0.048(3) 0.009(2) -0.007(2) 0.001(2) C54 0.048(3) 0.047(3) 0.046(3) 0.009(2) -0.005(2) 0.004(2) C55 0.045(3) 0.040(2) 0.036(2) 0.0015(19) -0.012(2) -0.004(2) C56 0.049(3) 0.041(3) 0.033(2) -0.0046(19) -0.008(2) -0.004(2) C57 0.047(3) 0.044(3) 0.043(3) -0.015(2) -0.013(2) 0.004(2) C58 0.071(3) 0.030(2) 0.058(3) -0.002(2) -0.036(3) 0.003(2) C59 0.067(4) 0.030(2) 0.032(2) 0.0031(19) 0.002(2) 0.001(2) C60 0.060(3) 0.030(2) 0.027(2) 0.0087(17) 0.0030(19) -0.010(2) C61 0.076(4) 0.027(2) 0.027(2) 0.0001(18) 0.000(2) -0.008(2) C62 0.034(4) 0.022(4) 0.029(4) -0.002(3) -0.006(3) -0.001(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 Cl1 Ir1 2.4945(8) . ? Ir1 P3 2.3258(8) . ? Ir1 P4 2.3277(8) . ? Ir1 P2 2.3390(8) . ? Ir1 P1 2.3534(8) . ? Ir1 H0 1.43(3) . ? P1 C1 1.726(3) . ? P1 C10 1.830(3) . ? P1 C4 1.835(3) . ? P2 C1 1.723(3) . ? P2 C16 1.829(3) . ? P2 C22 1.834(3) . ? P3 C28 1.818(3) . ? P3 C34 1.822(3) . ? P3 C3 1.843(3) . ? P4 C40 1.808(3) . ? P4 C46 1.826(3) . ? P4 C3 1.847(3) . ? C1 H1 0.85(4) . ? C3 H3A 0.92(4) . ? C3 H3B 0.87(4) . ? C4 C5 1.390(5) . ? C4 C9 1.395(5) . ? C5 C6 1.392(5) . ? C5 H5 0.85(5) . ? C6 C7 1.377(5) . ? C6 H6 0.96(4) . ? C7 C8 1.378(6) . ? C7 H7 0.86(4) . ? C8 C9 1.384(5) . ? C8 H8 0.86(4) . ? C9 H9 0.96(5) . ? C10 C11 1.388(5) . ? C10 C15 1.399(5) . ? C11 C12 1.386(5) . ? C11 H11 0.85(3) . ? C12 C13 1.386(5) . ? C12 H12 0.90(4) . ? C13 C14 1.381(5) . ? C13 H13 0.92(4) . ? C14 C15 1.381(5) . ? C14 H14 0.91(4) . ? C15 H15 0.84(4) . ? C16 C21 1.383(5) . ? C16 C17 1.384(5) . ? C17 C18 1.396(5) . ? C17 H17 0.93(4) . ? C18 C19 1.371(6) . ? C18 H18 1.02(5) . ? C19 C20 1.374(6) . ? C19 H19 0.93(5) . ? C20 C21 1.388(5) . ? C20 H20 0.89(4) . ? C21 H21 0.89(4) . ? C22 C23 1.386(5) . ? C22 C27 1.396(5) . ? C23 C24 1.389(5) . ? C23 H23 0.89(4) . ? C24 C25 1.371(5) . ? C24 H24 0.84(4) . ? C25 C26 1.380(5) . ? C25 H25 0.88(4) . ? C26 C27 1.383(5) . ? C26 H26 0.92(4) . ? C27 H27 0.95(4) . ? C28 C29 1.387(5) . ? C28 C33 1.388(5) . ? C29 C30 1.391(5) . ? C29 H29 0.86(5) . ? C30 C31 1.378(6) . ? C30 H30 1.00(5) . ? C31 C32 1.364(6) . ? C31 H31 0.75(5) . ? C32 C33 1.383(5) . ? C32 H32 0.87(4) . ? C33 H33 0.96(5) . ? C34 C39 1.386(5) . ? C34 C35 1.389(5) . ? C35 C36 1.388(5) . ? C35 H35 0.91(4) . ? C36 C37 1.385(5) . ? C36 H36 0.81(4) . ? C37 C38 1.377(5) . ? C37 H37 0.92(4) . ? C38 C39 1.388(5) . ? C38 H38 0.89(4) . ? C39 H39 0.93(4) . ? C40 C45 1.387(5) . ? C40 C41 1.395(5) . ? C41 C42 1.390(5) . ? C41 H41 0.94(4) . ? C42 C43 1.373(6) . ? C42 H42 0.96(4) . ? C43 C44 1.387(5) . ? C43 H43 0.92(4) . ? C44 C45 1.390(5) . ? C44 H44 0.95(4) . ? C45 H45 0.94(4) . ? C46 C47 1.381(5) . ? C46 C51 1.407(5) . ? C47 C48 1.395(5) . ? C47 H47 0.91(4) . ? C48 C49 1.367(5) . ? C48 H48 0.88(4) . ? C49 C50 1.394(5) . ? C49 H49 0.84(5) . ? C50 C51 1.372(5) . ? C50 H50 0.95(3) . ? C51 H51 0.94(4) . ? C52 C53 1.377(6) . ? C52 C57 1.391(6) . ? C52 C58 1.490(6) . ? C53 C54 1.383(7) . ? C53 H53 1.14(5) . ? C54 C55 1.386(6) . ? C54 H54 1.15(5) . ? C55 C56 1.375(7) . ? C55 H55 1.10(5) . ? C56 C57 1.379(7) . ? C56 H56 1.03(5) . ? C57 H57 0.9500 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C61 1.357(8) 2 ? C59 C60 1.391(7) . ? C59 H59 0.77(5) . ? C60 C62 1.324(9) . ? C60 C61 1.382(7) . ? C61 C59 1.357(8) 2 ? C61 H61 0.84(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? 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 P3 Ir1 P4 70.61(3) . . ? P3 Ir1 P2 108.91(3) . . ? P4 Ir1 P2 176.24(3) . . ? P3 Ir1 P1 173.62(3) . . ? P4 Ir1 P1 111.26(3) . . ? P2 Ir1 P1 68.80(3) . . ? P3 Ir1 Cl1 91.62(3) . . ? P4 Ir1 Cl1 85.23(3) . . ? P2 Ir1 Cl1 98.52(3) . . ? P1 Ir1 Cl1 94.60(3) . . ? P3 Ir1 H0 91.7(16) . . ? P4 Ir1 H0 94.0(16) . . ? P2 Ir1 H0 82.3(16) . . ? P1 Ir1 H0 82.1(16) . . ? Cl1 Ir1 H0 176.1(17) . . ? C1 P1 C10 112.04(16) . . ? C1 P1 C4 110.02(15) . . ? C10 P1 C4 101.47(14) . . ? C1 P1 Ir1 95.07(12) . . ? C10 P1 Ir1 116.43(10) . . ? C4 P1 Ir1 121.97(11) . . ? C1 P2 C16 112.75(16) . . ? C1 P2 C22 112.03(16) . . ? C16 P2 C22 99.02(15) . . ? C1 P2 Ir1 95.66(12) . . ? C16 P2 Ir1 124.41(12) . . ? C22 P2 Ir1 113.53(10) . . ? C28 P3 C34 104.68(15) . . ? C28 P3 C3 108.31(16) . . ? C34 P3 C3 106.21(16) . . ? C28 P3 Ir1 126.07(11) . . ? C34 P3 Ir1 115.44(11) . . ? C3 P3 Ir1 93.90(11) . . ? C40 P4 C46 104.95(15) . . ? C40 P4 C3 107.67(15) . . ? C46 P4 C3 103.91(16) . . ? C40 P4 Ir1 123.69(11) . . ? C46 P4 Ir1 119.72(11) . . ? C3 P4 Ir1 93.74(11) . . ? P2 C1 P1 100.47(18) . . ? P2 C1 H1 130(3) . . ? P1 C1 H1 129(3) . . ? P3 C3 P4 93.60(16) . . ? P3 C3 H3A 111(2) . . ? P4 C3 H3A 109(3) . . ? P3 C3 H3B 118(3) . . ? P4 C3 H3B 117(3) . . ? H3A C3 H3B 108(3) . . ? C5 C4 C9 118.3(3) . . ? C5 C4 P1 124.6(2) . . ? C9 C4 P1 117.1(3) . . ? C4 C5 C6 120.9(3) . . ? C4 C5 H5 125(3) . . ? C6 C5 H5 114(3) . . ? C7 C6 C5 120.0(3) . . ? C7 C6 H6 123(2) . . ? C5 C6 H6 117(2) . . ? C6 C7 C8 119.7(3) . . ? C6 C7 H7 123(3) . . ? C8 C7 H7 117(3) . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8 124(3) . . ? C9 C8 H8 115(3) . . ? C8 C9 C4 120.5(3) . . ? C8 C9 H9 126(3) . . ? C4 C9 H9 113(3) . . ? C11 C10 C15 118.2(3) . . ? C11 C10 P1 122.9(3) . . ? C15 C10 P1 118.8(2) . . ? C12 C11 C10 121.2(3) . . ? C12 C11 H11 116(2) . . ? C10 C11 H11 123(2) . . ? C11 C12 C13 119.7(3) . . ? C11 C12 H12 115(3) . . ? C13 C12 H12 125(3) . . ? C14 C13 C12 119.8(3) . . ? C14 C13 H13 120(2) . . ? C12 C13 H13 120(2) . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 120(2) . . ? C15 C14 H14 120(2) . . ? C14 C15 C10 120.6(3) . . ? C14 C15 H15 122(3) . . ? C10 C15 H15 117(2) . . ? C21 C16 C17 119.3(3) . . ? C21 C16 P2 118.7(3) . . ? C17 C16 P2 122.0(3) . . ? C16 C17 C18 119.5(4) . . ? C16 C17 H17 119(3) . . ? C18 C17 H17 121(3) . . ? C19 C18 C17 120.6(4) . . ? C19 C18 H18 122(3) . . ? C17 C18 H18 118(3) . . ? C18 C19 C20 120.2(4) . . ? C18 C19 H19 112(3) . . ? C20 C19 H19 128(3) . . ? C19 C20 C21 119.5(4) . . ? C19 C20 H20 120(3) . . ? C21 C20 H20 121(3) . . ? C16 C21 C20 120.9(4) . . ? C16 C21 H21 117(2) . . ? C20 C21 H21 122(2) . . ? C23 C22 C27 118.7(3) . . ? C23 C22 P2 119.7(3) . . ? C27 C22 P2 121.5(3) . . ? C22 C23 C24 120.4(3) . . ? C22 C23 H23 114(3) . . ? C24 C23 H23 125(3) . . ? C25 C24 C23 120.5(3) . . ? C25 C24 H24 116(3) . . ? C23 C24 H24 124(3) . . ? C24 C25 C26 119.6(3) . . ? C24 C25 H25 118(3) . . ? C26 C25 H25 122(3) . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26 123(2) . . ? C27 C26 H26 117(2) . . ? C26 C27 C22 120.2(3) . . ? C26 C27 H27 121(2) . . ? C22 C27 H27 119(2) . . ? C29 C28 C33 118.3(3) . . ? C29 C28 P3 119.2(3) . . ? C33 C28 P3 122.5(3) . . ? C28 C29 C30 120.4(4) . . ? C28 C29 H29 119(3) . . ? C30 C29 H29 121(3) . . ? C31 C30 C29 120.2(4) . . ? C31 C30 H30 124(3) . . ? C29 C30 H30 116(3) . . ? C32 C31 C30 119.9(4) . . ? C32 C31 H31 119(4) . . ? C30 C31 H31 119(4) . . ? C31 C32 C33 120.3(4) . . ? C31 C32 H32 124(3) . . ? C33 C32 H32 116(3) . . ? C32 C33 C28 120.9(4) . . ? C32 C33 H33 118(3) . . ? C28 C33 H33 121(3) . . ? C39 C34 C35 119.1(3) . . ? C39 C34 P3 118.4(2) . . ? C35 C34 P3 122.4(3) . . ? C36 C35 C34 119.9(3) . . ? C36 C35 H35 119(2) . . ? C34 C35 H35 121(2) . . ? C37 C36 C35 120.6(4) . . ? C37 C36 H36 122(3) . . ? C35 C36 H36 118(3) . . ? C38 C37 C36 119.6(3) . . ? C38 C37 H37 120(3) . . ? C36 C37 H37 120(3) . . ? C37 C38 C39 120.0(3) . . ? C37 C38 H38 122(3) . . ? C39 C38 H38 118(3) . . ? C34 C39 C38 120.8(3) . . ? C34 C39 H39 119(3) . . ? C38 C39 H39 120(3) . . ? C45 C40 C41 119.2(3) . . ? C45 C40 P4 118.4(3) . . ? C41 C40 P4 122.4(3) . . ? C42 C41 C40 119.9(3) . . ? C42 C41 H41 118(2) . . ? C40 C41 H41 122(2) . . ? C43 C42 C41 120.3(4) . . ? C43 C42 H42 119(3) . . ? C41 C42 H42 121(3) . . ? C42 C43 C44 120.3(3) . . ? C42 C43 H43 120(3) . . ? C44 C43 H43 120(3) . . ? C43 C44 C45 119.5(4) . . ? C43 C44 H44 122(2) . . ? C45 C44 H44 119(2) . . ? C40 C45 C44 120.6(3) . . ? C40 C45 H45 121(3) . . ? C44 C45 H45 119(3) . . ? C47 C46 C51 119.2(3) . . ? C47 C46 P4 120.0(3) . . ? C51 C46 P4 120.7(3) . . ? C46 C47 C48 120.3(3) . . ? C46 C47 H47 122(2) . . ? C48 C47 H47 118(2) . . ? C49 C48 C47 120.5(3) . . ? C49 C48 H48 123(3) . . ? C47 C48 H48 117(3) . . ? C48 C49 C50 119.5(3) . . ? C48 C49 H49 116(4) . . ? C50 C49 H49 124(4) . . ? C51 C50 C49 120.8(3) . . ? C51 C50 H50 122(2) . . ? C49 C50 H50 116(2) . . ? C50 C51 C46 119.8(3) . . ? C50 C51 H51 123(2) . . ? C46 C51 H51 117(2) . . ? C53 C52 C57 117.0(4) . . ? C53 C52 C58 120.8(4) . . ? C57 C52 C58 122.2(4) . . ? C52 C53 C54 122.5(5) . . ? C52 C53 H53 118(3) . . ? C54 C53 H53 119(3) . . ? C53 C54 C55 119.1(5) . . ? C53 C54 H54 121(3) . . ? C55 C54 H54 120(3) . . ? C56 C55 C54 119.7(4) . . ? C56 C55 H55 121(3) . . ? C54 C55 H55 120(3) . . ? C55 C56 C57 120.1(5) . . ? C55 C56 H56 126(3) . . ? C57 C56 H56 113(3) . . ? C56 C57 C52 121.6(4) . . ? C56 C57 H57 119.2 . . ? C52 C57 H57 119.2 . . ? C52 C58 H58A 109.5 . . ? C52 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C52 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C61 C59 C60 120.8(5) 2 . ? C61 C59 H59 116(4) 2 . ? C60 C59 H59 123(4) . . ? C62 C60 C61 121.7(5) . . ? C62 C60 C59 120.2(6) . . ? C61 C60 C59 118.0(5) . . ? C59 C61 C60 121.2(5) 2 . ? C59 C61 H61 118(3) 2 . ? C60 C61 H61 120(3) . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.251 _refine_diff_density_min -1.093 _refine_diff_density_rms 0.132 #===END # ---------------------------------------------------------- # Data for compound_2 (local labelling as fjl66as) # CCDC number 689716 data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 689716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H44 Cl Ir O2 P4, 3 (C3 H6 O)' _chemical_formula_sum 'C60 H62 Cl Ir O5 P4' _chemical_formula_weight 1214.63 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3699(12) _cell_length_b 13.1164(13) _cell_length_c 17.4537(17) _cell_angle_alpha 83.760(2) _cell_angle_beta 79.883(2) _cell_angle_gamma 79.480(2) _cell_volume 2732.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6846 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.66 _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.074 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 2.658 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7238 _exptl_absorpt_correction_T_max 0.8786 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within SAINT+ package, v. 6.45. ; _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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 32782 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.10 _reflns_number_total 11929 _reflns_number_gt 10585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 6.45 (Bruker AXS, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS' _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. All non-hydrogen atoms, including those of solvent molecules, were refined with anisotropic displacement parameters. Three acetone solvent molecules were observed included in the crystal structure. Atoms of these molecules were also refined with an anisotropic thermal model. Most of hydrogens were found in the difference Fourier maps showing reasonable positional parameters. Hydrogens of the metal complex were allowed to refine as free isotropic atoms, although a reduced number of C-H distances showed slightly out-of-usual-range values. Displacement parameters Ueq for both C and H atoms showed slightly broad ranges, but these values were not restricted. Hydride was included in the refinement in a position obtained from electros- tatic potential calculations (HYDEX program) and allowed to freely refine with a weak restriction in the Ir-H bond distance. Hydrogens for the solvent molecules (terminal methyl groups) were included from observed positions, and refined with riding positional and free thermal parameters. All the residuals -four peaks- over 1 e/A3 were in close proximity of the metal atom with no chemical sense. ; _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^)+(0.0336P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11929 _refine_ls_number_parameters 840 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0744 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.832360(10) 0.791315(11) 0.733415(8) 0.01279(5) Uani 1 1 d D . . H0 H 0.870(3) 0.887(3) 0.698(2) 0.032(11) Uiso 1 1 d D . . Cl1 Cl 0.75326(7) 0.63645(7) 0.79635(5) 0.02222(19) Uani 1 1 d . . . P1 P 0.78278(7) 0.78322(7) 0.61076(5) 0.01529(19) Uani 1 1 d . . . P2 P 0.66012(7) 0.89666(7) 0.72606(5) 0.01538(19) Uani 1 1 d . . . P3 P 0.88792(7) 0.82097(7) 0.84816(5) 0.01492(19) Uani 1 1 d . . . P4 P 1.00921(7) 0.69278(7) 0.73879(5) 0.01564(19) Uani 1 1 d . . . O1 O 0.5069(2) 0.9977(2) 0.59714(15) 0.0248(6) Uani 1 1 d . . . H1 H 0.461(5) 1.047(5) 0.553(4) 0.11(2) Uiso 1 1 d . . . O2 O 0.5963(2) 0.8877(2) 0.50778(14) 0.0244(6) Uani 1 1 d . . . C1 C 0.6570(3) 0.8714(3) 0.6293(2) 0.0189(8) Uani 1 1 d . . . C2 C 0.5844(3) 0.9205(3) 0.5766(2) 0.0197(8) Uani 1 1 d . . . C3 C 1.0089(3) 0.7155(3) 0.8418(2) 0.0189(8) Uani 1 1 d . . . H3A H 1.075(3) 0.731(3) 0.852(2) 0.018(10) Uiso 1 1 d . . . H3B H 0.987(3) 0.658(3) 0.874(2) 0.021(10) Uiso 1 1 d . . . C4 C 0.7587(3) 0.6605(3) 0.5829(2) 0.0187(8) Uani 1 1 d . . . C5 C 0.8357(4) 0.6007(3) 0.5302(2) 0.0258(9) Uani 1 1 d . . . H5 H 0.891(3) 0.624(3) 0.504(2) 0.029(12) Uiso 1 1 d . . . C6 C 0.8214(4) 0.5029(3) 0.5170(3) 0.0341(10) Uani 1 1 d . . . H6 H 0.871(4) 0.460(4) 0.480(3) 0.050(14) Uiso 1 1 d . . . C7 C 0.7293(4) 0.4627(4) 0.5565(3) 0.0385(12) Uani 1 1 d . . . H7 H 0.714(3) 0.400(3) 0.545(2) 0.018(10) Uiso 1 1 d . . . C8 C 0.6512(4) 0.5209(4) 0.6087(3) 0.0369(11) Uani 1 1 d . . . H8 H 0.585(4) 0.493(3) 0.639(3) 0.042(13) Uiso 1 1 d . . . C9 C 0.6657(3) 0.6186(3) 0.6221(2) 0.0271(9) Uani 1 1 d . . . H9 H 0.616(3) 0.657(3) 0.657(2) 0.019(10) Uiso 1 1 d . . . C10 C 0.8767(3) 0.8275(3) 0.5264(2) 0.0186(7) Uani 1 1 d U . . C11 C 0.9807(4) 0.8437(5) 0.5350(3) 0.0548(17) Uani 1 1 d U . . H11 H 0.998(3) 0.838(3) 0.580(3) 0.036(13) Uiso 1 1 d . . . C12 C 1.0535(4) 0.8786(6) 0.4720(3) 0.080(2) Uani 1 1 d U . . H12 H 1.123(5) 0.897(5) 0.478(3) 0.09(2) Uiso 1 1 d . . . C13 C 1.0220(4) 0.8983(4) 0.3994(3) 0.0440(13) Uani 1 1 d U . . H13 H 1.066(4) 0.915(4) 0.357(3) 0.055(15) Uiso 1 1 d . . . C14 C 0.9196(3) 0.8817(3) 0.3895(2) 0.0243(8) Uani 1 1 d U . . H14 H 0.900(4) 0.893(3) 0.336(3) 0.045(13) Uiso 1 1 d . . . C15 C 0.8474(3) 0.8463(3) 0.4523(2) 0.0239(8) Uani 1 1 d U . . H15 H 0.785(4) 0.834(4) 0.446(3) 0.066(17) Uiso 1 1 d . . . C16 C 0.5362(3) 0.8716(3) 0.7939(2) 0.0185(8) Uani 1 1 d . . . C17 C 0.5454(3) 0.8205(3) 0.8675(2) 0.0218(8) Uani 1 1 d . . . H17 H 0.618(3) 0.794(3) 0.878(2) 0.017(10) Uiso 1 1 d . . . C18 C 0.4503(3) 0.8061(3) 0.9208(2) 0.0275(9) Uani 1 1 d . . . H18 H 0.449(3) 0.772(3) 0.971(2) 0.031(12) Uiso 1 1 d . . . C19 C 0.3457(3) 0.8415(3) 0.9003(2) 0.0290(10) Uani 1 1 d . . . H19 H 0.289(3) 0.832(3) 0.933(2) 0.026(11) Uiso 1 1 d . . . C20 C 0.3360(3) 0.8927(3) 0.8277(2) 0.0255(9) Uani 1 1 d . . . H20 H 0.265(3) 0.921(3) 0.813(2) 0.036(12) Uiso 1 1 d . . . C21 C 0.4308(3) 0.9078(3) 0.7748(2) 0.0222(8) Uani 1 1 d . . . H21 H 0.423(3) 0.944(3) 0.723(2) 0.029(11) Uiso 1 1 d . . . C22 C 0.6544(3) 1.0351(3) 0.7340(2) 0.0194(8) Uani 1 1 d . . . C23 C 0.6933(3) 1.0973(3) 0.6692(2) 0.0250(9) Uani 1 1 d . . . H23 H 0.709(3) 1.070(3) 0.624(2) 0.016(10) Uiso 1 1 d . . . C24 C 0.6987(4) 1.2005(4) 0.6764(3) 0.0374(11) Uani 1 1 d . . . H24 H 0.725(4) 1.236(4) 0.634(3) 0.053(16) Uiso 1 1 d . . . C25 C 0.6668(4) 1.2424(4) 0.7471(3) 0.0398(12) Uani 1 1 d . . . H25 H 0.670(3) 1.311(3) 0.751(2) 0.025(11) Uiso 1 1 d . . . C26 C 0.6275(3) 1.1818(3) 0.8122(3) 0.0357(11) Uani 1 1 d . . . H26 H 0.599(4) 1.210(4) 0.862(3) 0.053(15) Uiso 1 1 d . . . C27 C 0.6204(3) 1.0786(3) 0.8050(3) 0.0258(9) Uani 1 1 d . . . H27 H 0.598(3) 1.034(3) 0.849(2) 0.033(12) Uiso 1 1 d . . . C28 C 0.8022(3) 0.8051(3) 0.94350(19) 0.0182(8) Uani 1 1 d . . . C29 C 0.7860(3) 0.7066(3) 0.9759(2) 0.0233(8) Uani 1 1 d . . . H29 H 0.825(3) 0.649(3) 0.952(2) 0.019(10) Uiso 1 1 d . . . C30 C 0.7150(3) 0.6946(4) 1.0460(2) 0.0311(10) Uani 1 1 d . . . H30 H 0.707(3) 0.633(3) 1.066(2) 0.011(9) Uiso 1 1 d . . . C31 C 0.6580(3) 0.7806(4) 1.0828(2) 0.0332(10) Uani 1 1 d . . . H31 H 0.609(3) 0.769(3) 1.132(2) 0.025(10) Uiso 1 1 d . . . C32 C 0.6718(3) 0.8784(4) 1.0506(2) 0.0308(10) Uani 1 1 d . . . H32 H 0.635(3) 0.936(3) 1.076(2) 0.029(12) Uiso 1 1 d . . . C33 C 0.7439(3) 0.8910(3) 0.9813(2) 0.0223(8) Uani 1 1 d . . . H33 H 0.749(3) 0.958(3) 0.961(2) 0.020(10) Uiso 1 1 d . . . C34 C 0.9437(3) 0.9389(3) 0.8524(2) 0.0156(7) Uani 1 1 d . . . C35 C 0.9079(3) 1.0301(3) 0.8093(2) 0.0195(8) Uani 1 1 d . . . H35 H 0.853(3) 1.030(3) 0.780(2) 0.013(9) Uiso 1 1 d . . . C36 C 0.9505(3) 1.1196(3) 0.8144(2) 0.0221(8) Uani 1 1 d . . . H36 H 0.928(3) 1.176(3) 0.7854(19) 0.008(9) Uiso 1 1 d . . . C37 C 1.0305(3) 1.1172(3) 0.8615(2) 0.0237(8) Uani 1 1 d . . . H37 H 1.061(3) 1.180(3) 0.863(2) 0.033(12) Uiso 1 1 d . . . C38 C 1.0656(3) 1.0274(3) 0.9045(2) 0.0255(9) Uani 1 1 d . . . H38 H 1.117(3) 1.027(3) 0.931(2) 0.015(9) Uiso 1 1 d . . . C39 C 1.0228(3) 0.9376(3) 0.9009(2) 0.0208(8) Uani 1 1 d . . . H39 H 1.041(3) 0.879(3) 0.931(2) 0.012(9) Uiso 1 1 d . . . C40 C 1.0367(3) 0.5529(3) 0.7345(2) 0.0172(7) Uani 1 1 d . . . C41 C 1.1172(3) 0.4930(3) 0.7741(2) 0.0222(8) Uani 1 1 d . . . H41 H 1.153(3) 0.522(3) 0.805(2) 0.022(10) Uiso 1 1 d . . . C42 C 1.1404(3) 0.3868(3) 0.7687(2) 0.0277(9) Uani 1 1 d . . . H42 H 1.192(3) 0.349(3) 0.796(2) 0.022(10) Uiso 1 1 d . . . C43 C 1.0855(3) 0.3404(3) 0.7236(2) 0.0272(9) Uani 1 1 d . . . H43 H 1.102(3) 0.274(3) 0.722(2) 0.016(10) Uiso 1 1 d . . . C44 C 1.0047(3) 0.3993(3) 0.6845(2) 0.0274(9) Uani 1 1 d . . . H44 H 0.969(4) 0.367(3) 0.656(3) 0.042(13) Uiso 1 1 d . . . C45 C 0.9796(3) 0.5053(3) 0.6906(2) 0.0222(8) Uani 1 1 d . . . H45 H 0.929(3) 0.541(3) 0.670(2) 0.017(10) Uiso 1 1 d . . . C46 C 1.1350(3) 0.7346(3) 0.6829(2) 0.0181(7) Uani 1 1 d . . . H47 H 1.207(3) 0.603(3) 0.632(2) 0.021(11) Uiso 1 1 d . . . C47 C 1.2140(3) 0.6677(3) 0.6362(2) 0.0273(9) Uani 1 1 d . . . H48 H 1.366(3) 0.653(3) 0.564(2) 0.023(10) Uiso 1 1 d . . . C48 C 1.3079(3) 0.7014(4) 0.5933(2) 0.0307(10) Uani 1 1 d . . . H49 H 1.383(3) 0.828(3) 0.568(2) 0.022(10) Uiso 1 1 d . . . C49 C 1.3251(3) 0.8019(3) 0.5956(2) 0.0279(9) Uani 1 1 d . . . H50 H 1.258(3) 0.935(3) 0.642(2) 0.036(13) Uiso 1 1 d . . . C50 C 1.2472(3) 0.8686(3) 0.6412(2) 0.0271(9) Uani 1 1 d . . . C51 C 1.1526(3) 0.8359(3) 0.6838(2) 0.0241(8) Uani 1 1 d . . . H51 H 1.106(3) 0.878(3) 0.714(2) 0.020(10) Uiso 1 1 d . . . O3 O 0.7114(2) 0.4326(2) 0.10888(17) 0.0360(7) Uani 1 1 d . . . C52 C 0.5171(4) 0.4979(4) 0.1223(4) 0.0579(16) Uani 1 1 d . . . H52A H 0.4590 0.4551 0.1263 0.071(17) Uiso 1 1 calc R . . H52B H 0.5347 0.5264 0.0682 0.053(16) Uiso 1 1 calc R . . H52C H 0.4907 0.5551 0.1563 0.10(3) Uiso 1 1 calc R . . C53 C 0.6195(3) 0.4326(3) 0.1471(2) 0.0286(9) Uani 1 1 d . . . C54 C 0.6014(4) 0.3710(3) 0.2233(2) 0.0354(10) Uani 1 1 d . . . H54A H 0.5413 0.3314 0.2241 0.031(11) Uiso 1 1 calc R . . H54B H 0.5810 0.4181 0.2654 0.039(13) Uiso 1 1 calc R . . H54C H 0.6701 0.3230 0.2308 0.057(15) Uiso 1 1 calc R . . O4 O 0.4179(3) 0.3734(3) 0.7142(2) 0.0467(9) Uani 1 1 d . . . C55 C 0.4300(5) 0.3468(5) 0.5807(3) 0.0616(16) Uani 1 1 d . . . H55A H 0.4856 0.2931 0.5544 0.12(3) Uiso 1 1 calc R . . H55B H 0.4576 0.4132 0.5718 0.080(19) Uiso 1 1 calc R . . H55C H 0.3604 0.3541 0.5596 0.08(2) Uiso 1 1 calc R . . C56 C 0.4095(3) 0.3164(3) 0.6660(3) 0.0330(10) Uani 1 1 d . . . C57 C 0.3811(4) 0.2102(3) 0.6885(3) 0.0336(10) Uani 1 1 d . . . H57A H 0.3554 0.2026 0.7449 0.049(14) Uiso 1 1 calc R . . H57B H 0.4473 0.1579 0.6746 0.055(15) Uiso 1 1 calc R . . H57C H 0.3220 0.2003 0.6607 0.054(15) Uiso 1 1 calc R . . O5 O 0.8681(3) 0.2557(2) 0.98510(18) 0.0410(8) Uani 1 1 d . . . C58 C 0.7472(4) 0.3816(4) 0.9199(3) 0.0486(13) Uani 1 1 d . . . H58A H 0.7029 0.3258 0.9244 0.09(2) Uiso 1 1 calc R . . H58B H 0.7684 0.4038 0.8646 0.076(19) Uiso 1 1 calc R . . H58C H 0.7031 0.4407 0.9471 0.11(3) Uiso 1 1 calc R . . C59 C 0.8494(3) 0.3429(3) 0.9555(2) 0.0251(9) Uani 1 1 d . . . C60 C 0.9261(4) 0.4182(4) 0.9536(3) 0.0371(11) Uani 1 1 d . . . H60A H 0.9991 0.3806 0.9632 0.039(12) Uiso 1 1 calc R . . H60B H 0.8958 0.4666 0.9940 0.073(18) Uiso 1 1 calc R . . H60C H 0.9339 0.4571 0.9023 0.057(15) 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 0.01161(7) 0.01500(7) 0.01231(7) -0.00018(5) -0.00238(5) -0.00371(5) Cl1 0.0235(4) 0.0206(5) 0.0230(5) 0.0005(4) -0.0006(4) -0.0090(4) P1 0.0135(4) 0.0189(5) 0.0139(4) -0.0013(4) -0.0021(3) -0.0039(4) P2 0.0134(4) 0.0178(5) 0.0155(5) -0.0020(4) -0.0025(3) -0.0034(4) P3 0.0143(4) 0.0166(5) 0.0139(4) -0.0009(4) -0.0028(3) -0.0025(4) P4 0.0153(4) 0.0163(5) 0.0157(5) -0.0007(4) -0.0030(3) -0.0037(4) O1 0.0237(14) 0.0267(15) 0.0237(14) -0.0017(12) -0.0080(11) 0.0008(12) O2 0.0265(14) 0.0299(16) 0.0172(13) -0.0058(12) -0.0062(11) -0.0007(12) C1 0.0176(18) 0.024(2) 0.0161(18) -0.0063(15) -0.0013(14) -0.0035(15) C2 0.0147(17) 0.024(2) 0.0206(19) -0.0018(16) -0.0012(14) -0.0063(15) C3 0.0177(18) 0.023(2) 0.0164(19) -0.0031(16) -0.0028(14) -0.0033(16) C4 0.0215(18) 0.0207(19) 0.0163(18) 0.0005(15) -0.0078(14) -0.0065(15) C5 0.028(2) 0.024(2) 0.025(2) -0.0007(17) -0.0081(17) -0.0003(18) C6 0.052(3) 0.025(2) 0.025(2) -0.0084(19) -0.009(2) 0.000(2) C7 0.071(3) 0.024(2) 0.029(2) 0.0028(19) -0.019(2) -0.023(2) C8 0.055(3) 0.038(3) 0.025(2) 0.000(2) -0.007(2) -0.030(2) C9 0.027(2) 0.038(2) 0.021(2) -0.0047(19) -0.0021(17) -0.0173(19) C10 0.0150(17) 0.022(2) 0.0177(18) -0.0009(15) -0.0018(14) -0.0016(15) C11 0.031(2) 0.122(5) 0.016(2) 0.016(3) -0.0088(19) -0.033(3) C12 0.039(3) 0.183(8) 0.029(3) 0.026(4) -0.009(2) -0.066(4) C13 0.036(3) 0.082(4) 0.018(2) 0.010(2) -0.0008(18) -0.030(3) C14 0.026(2) 0.028(2) 0.0181(19) 0.0009(17) -0.0046(15) -0.0016(17) C15 0.021(2) 0.031(2) 0.021(2) -0.0031(17) -0.0045(15) -0.0055(17) C16 0.0184(18) 0.0199(19) 0.0182(18) -0.0090(15) 0.0000(14) -0.0038(15) C17 0.0168(18) 0.027(2) 0.021(2) -0.0020(16) -0.0032(15) -0.0033(16) C18 0.026(2) 0.037(2) 0.019(2) -0.0043(18) 0.0013(16) -0.0100(18) C19 0.021(2) 0.036(2) 0.030(2) -0.0111(19) 0.0095(17) -0.0114(18) C20 0.0150(19) 0.032(2) 0.030(2) -0.0062(18) -0.0018(16) -0.0049(17) C21 0.0172(18) 0.026(2) 0.024(2) -0.0051(17) -0.0027(15) -0.0021(16) C22 0.0116(16) 0.0203(19) 0.028(2) -0.0006(16) -0.0076(15) -0.0021(14) C23 0.024(2) 0.024(2) 0.028(2) 0.0013(18) -0.0081(17) -0.0060(17) C24 0.035(3) 0.029(2) 0.051(3) 0.012(2) -0.014(2) -0.015(2) C25 0.028(2) 0.016(2) 0.079(4) -0.010(2) -0.015(2) -0.0016(18) C26 0.021(2) 0.029(2) 0.059(3) -0.020(2) -0.005(2) -0.0014(18) C27 0.0175(19) 0.028(2) 0.033(2) -0.0044(19) -0.0066(17) -0.0039(17) C28 0.0163(17) 0.027(2) 0.0122(17) -0.0001(15) -0.0030(13) -0.0063(15) C29 0.026(2) 0.025(2) 0.020(2) 0.0038(17) -0.0075(16) -0.0071(17) C30 0.031(2) 0.038(3) 0.025(2) 0.014(2) -0.0076(18) -0.014(2) C31 0.028(2) 0.059(3) 0.016(2) -0.003(2) 0.0004(17) -0.020(2) C32 0.022(2) 0.046(3) 0.028(2) -0.017(2) 0.0038(17) -0.014(2) C33 0.0190(19) 0.025(2) 0.024(2) -0.0056(17) -0.0029(15) -0.0055(16) C34 0.0117(16) 0.0177(18) 0.0182(18) -0.0050(15) -0.0001(13) -0.0045(14) C35 0.0153(17) 0.026(2) 0.0176(19) -0.0011(16) -0.0027(14) -0.0057(15) C36 0.024(2) 0.018(2) 0.023(2) 0.0000(17) -0.0012(16) -0.0036(16) C37 0.024(2) 0.025(2) 0.024(2) -0.0079(17) 0.0000(16) -0.0100(17) C38 0.0180(19) 0.038(2) 0.024(2) -0.0097(18) -0.0044(16) -0.0093(17) C39 0.0166(18) 0.027(2) 0.0189(19) -0.0031(17) -0.0034(15) -0.0029(16) C40 0.0144(17) 0.0199(19) 0.0152(18) -0.0004(15) 0.0021(13) -0.0020(14) C41 0.0185(18) 0.022(2) 0.027(2) -0.0032(17) -0.0064(16) -0.0013(16) C42 0.025(2) 0.022(2) 0.032(2) 0.0040(18) -0.0064(18) 0.0041(17) C43 0.032(2) 0.014(2) 0.032(2) -0.0039(18) 0.0018(18) -0.0004(17) C44 0.031(2) 0.023(2) 0.031(2) -0.0044(18) -0.0057(18) -0.0069(18) C45 0.0193(19) 0.024(2) 0.025(2) -0.0021(17) -0.0076(16) -0.0021(16) C46 0.0178(17) 0.023(2) 0.0150(18) 0.0025(15) -0.0076(14) -0.0053(15) C47 0.026(2) 0.029(2) 0.028(2) -0.0090(19) 0.0050(16) -0.0108(18) C48 0.025(2) 0.042(3) 0.025(2) -0.012(2) 0.0076(17) -0.0104(19) C49 0.020(2) 0.041(3) 0.025(2) 0.0006(19) -0.0025(16) -0.0138(19) C50 0.023(2) 0.026(2) 0.035(2) -0.0008(19) -0.0052(17) -0.0099(18) C51 0.0195(19) 0.023(2) 0.030(2) -0.0021(18) -0.0056(16) -0.0023(16) O3 0.0315(16) 0.0432(19) 0.0338(17) -0.0030(14) 0.0015(13) -0.0139(14) C52 0.035(3) 0.050(3) 0.088(5) 0.022(3) -0.022(3) -0.011(3) C53 0.029(2) 0.024(2) 0.036(2) -0.0047(18) -0.0095(18) -0.0077(18) C54 0.033(2) 0.036(3) 0.037(3) -0.005(2) -0.0010(19) -0.010(2) O4 0.0408(19) 0.046(2) 0.057(2) -0.0263(18) -0.0091(16) -0.0019(16) C55 0.074(4) 0.071(4) 0.051(3) 0.011(3) -0.026(3) -0.035(4) C56 0.019(2) 0.038(3) 0.043(3) -0.013(2) -0.0076(18) -0.0005(18) C57 0.032(2) 0.034(3) 0.034(3) -0.010(2) -0.0109(19) 0.0053(19) O5 0.0436(19) 0.0302(18) 0.0405(19) 0.0082(15) 0.0027(15) 0.0012(14) C58 0.046(3) 0.053(3) 0.055(3) 0.009(3) -0.029(3) -0.017(3) C59 0.027(2) 0.028(2) 0.018(2) -0.0021(17) -0.0002(16) -0.0027(17) C60 0.032(2) 0.039(3) 0.041(3) 0.003(2) -0.008(2) -0.012(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 P3 2.3206(9) . ? Ir1 P2 2.3340(9) . ? Ir1 P4 2.3405(9) . ? Ir1 P1 2.3463(9) . ? Ir1 Cl1 2.4806(9) . ? Ir1 H0 1.45(3) . ? P1 C1 1.763(4) . ? P1 C4 1.820(4) . ? P1 C10 1.821(4) . ? P2 C1 1.764(4) . ? P2 C16 1.823(4) . ? P2 C22 1.824(4) . ? P3 C34 1.818(3) . ? P3 C28 1.822(4) . ? P3 C3 1.840(4) . ? P4 C40 1.811(4) . ? P4 C46 1.826(4) . ? P4 C3 1.853(4) . ? O1 C2 1.296(4) . ? O1 H1 1.12(7) . ? O2 C2 1.295(4) . ? C1 C2 1.421(5) . ? C3 H3A 0.92(4) . ? C3 H3B 0.94(4) . ? C4 C5 1.395(5) . ? C4 C9 1.402(5) . ? C5 C6 1.376(6) . ? C5 H5 0.84(4) . ? C6 C7 1.384(6) . ? C6 H6 0.97(5) . ? C7 C8 1.386(7) . ? C7 H7 0.93(4) . ? C8 C9 1.377(6) . ? C8 H8 1.00(4) . ? C9 H9 0.91(4) . ? C10 C11 1.378(5) . ? C10 C15 1.389(5) . ? C11 C12 1.387(6) . ? C11 H11 0.84(4) . ? C12 C13 1.374(6) . ? C12 H12 0.96(6) . ? C13 C14 1.366(6) . ? C13 H13 0.88(5) . ? C14 C15 1.383(5) . ? C14 H14 0.99(4) . ? C15 H15 0.84(5) . ? C16 C21 1.389(5) . ? C16 C17 1.397(5) . ? C17 C18 1.393(5) . ? C17 H17 0.95(4) . ? C18 C19 1.387(6) . ? C18 H18 0.95(4) . ? C19 C20 1.382(6) . ? C19 H19 0.85(4) . ? C20 C21 1.391(5) . ? C20 H20 0.96(4) . ? C21 H21 0.99(4) . ? C22 C27 1.387(5) . ? C22 C23 1.388(5) . ? C23 C24 1.388(6) . ? C23 H23 0.87(4) . ? C24 C25 1.370(7) . ? C24 H24 0.87(5) . ? C25 C26 1.382(7) . ? C25 H25 0.92(4) . ? C26 C27 1.392(6) . ? C26 H26 0.96(5) . ? C27 H27 0.94(4) . ? C28 C33 1.386(5) . ? C28 C29 1.389(5) . ? C29 C30 1.386(5) . ? C29 H29 0.92(4) . ? C30 C31 1.374(6) . ? C30 H30 0.86(3) . ? C31 C32 1.372(6) . ? C31 H31 0.98(4) . ? C32 C33 1.384(5) . ? C32 H32 0.92(4) . ? C33 H33 0.92(4) . ? C34 C35 1.386(5) . ? C34 C39 1.399(5) . ? C35 C36 1.389(5) . ? C35 H35 0.92(3) . ? C36 C37 1.387(5) . ? C36 H36 0.88(3) . ? C37 C38 1.370(6) . ? C37 H37 0.97(4) . ? C38 C39 1.388(5) . ? C38 H38 0.85(3) . ? C39 H39 0.90(4) . ? C40 C41 1.388(5) . ? C40 C45 1.389(5) . ? C41 C42 1.381(5) . ? C41 H41 0.90(4) . ? C42 C43 1.377(6) . ? C42 H42 0.90(4) . ? C43 C44 1.380(6) . ? C43 H43 0.86(4) . ? C44 C45 1.380(5) . ? C44 H44 0.90(4) . ? C45 H45 0.82(4) . ? C46 C51 1.386(5) . ? C46 C47 1.397(5) . ? C47 C48 1.384(5) . ? C47 H47 0.88(4) . ? C48 C49 1.378(6) . ? C48 H48 0.98(4) . ? C49 C50 1.379(6) . ? C49 H49 0.89(4) . ? C50 C51 1.383(5) . ? C50 H50 0.90(4) . ? C51 H51 0.87(4) . ? O3 C53 1.213(5) . ? C52 C53 1.497(6) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.483(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O4 C56 1.214(5) . ? C55 C56 1.489(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.493(6) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? O5 C59 1.201(5) . ? C58 C59 1.489(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.483(5) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? 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 P3 Ir1 P2 107.53(3) . . ? P3 Ir1 P4 71.92(3) . . ? P2 Ir1 P4 177.22(3) . . ? P3 Ir1 P1 172.25(3) . . ? P2 Ir1 P1 70.63(3) . . ? P4 Ir1 P1 109.53(3) . . ? P3 Ir1 Cl1 91.93(3) . . ? P2 Ir1 Cl1 95.11(3) . . ? P4 Ir1 Cl1 87.65(3) . . ? P1 Ir1 Cl1 95.72(3) . . ? P3 Ir1 H0 88.6(15) . . ? P2 Ir1 H0 80.5(15) . . ? P4 Ir1 H0 96.8(15) . . ? P1 Ir1 H0 83.7(15) . . ? Cl1 Ir1 H0 175.5(15) . . ? C1 P1 C4 111.24(17) . . ? C1 P1 C10 112.52(17) . . ? C4 P1 C10 102.78(17) . . ? C1 P1 Ir1 94.38(12) . . ? C4 P1 Ir1 119.84(12) . . ? C10 P1 Ir1 116.32(12) . . ? C1 P2 C16 113.31(16) . . ? C1 P2 C22 111.15(17) . . ? C16 P2 C22 101.29(16) . . ? C1 P2 Ir1 94.79(12) . . ? C16 P2 Ir1 120.77(12) . . ? C22 P2 Ir1 115.94(11) . . ? C34 P3 C28 103.81(16) . . ? C34 P3 C3 105.42(17) . . ? C28 P3 C3 108.48(17) . . ? C34 P3 Ir1 119.18(12) . . ? C28 P3 Ir1 122.54(11) . . ? C3 P3 Ir1 95.48(12) . . ? C40 P4 C46 103.65(16) . . ? C40 P4 C3 105.84(17) . . ? C46 P4 C3 106.17(16) . . ? C40 P4 Ir1 122.26(11) . . ? C46 P4 Ir1 121.75(12) . . ? C3 P4 Ir1 94.47(12) . . ? C2 O1 H1 120(3) . . ? C2 C1 P1 129.1(3) . . ? C2 C1 P2 130.0(3) . . ? P1 C1 P2 100.17(18) . . ? O2 C2 O1 120.1(3) . . ? O2 C2 C1 119.6(3) . . ? O1 C2 C1 120.3(3) . . ? P3 C3 P4 95.65(17) . . ? P3 C3 H3A 117(2) . . ? P4 C3 H3A 115(2) . . ? P3 C3 H3B 107(2) . . ? P4 C3 H3B 109(2) . . ? H3A C3 H3B 112(3) . . ? C5 C4 C9 118.4(4) . . ? C5 C4 P1 122.3(3) . . ? C9 C4 P1 118.9(3) . . ? C6 C5 C4 121.0(4) . . ? C6 C5 H5 118(3) . . ? C4 C5 H5 121(3) . . ? C5 C6 C7 119.8(4) . . ? C5 C6 H6 124(3) . . ? C7 C6 H6 116(3) . . ? C6 C7 C8 120.3(4) . . ? C6 C7 H7 121(2) . . ? C8 C7 H7 118(2) . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8 118(3) . . ? C7 C8 H8 122(3) . . ? C8 C9 C4 120.6(4) . . ? C8 C9 H9 121(2) . . ? C4 C9 H9 119(2) . . ? C11 C10 C15 117.9(4) . . ? C11 C10 P1 119.9(3) . . ? C15 C10 P1 122.2(3) . . ? C10 C11 C12 121.1(4) . . ? C10 C11 H11 119(3) . . ? C12 C11 H11 119(3) . . ? C13 C12 C11 120.0(4) . . ? C13 C12 H12 117(4) . . ? C11 C12 H12 122(4) . . ? C14 C13 C12 119.8(4) . . ? C14 C13 H13 116(3) . . ? C12 C13 H13 124(3) . . ? C13 C14 C15 120.2(4) . . ? C13 C14 H14 118(3) . . ? C15 C14 H14 121(3) . . ? C14 C15 C10 121.0(4) . . ? C14 C15 H15 121(4) . . ? C10 C15 H15 118(4) . . ? C21 C16 C17 118.9(3) . . ? C21 C16 P2 120.5(3) . . ? C17 C16 P2 120.5(3) . . ? C18 C17 C16 120.4(3) . . ? C18 C17 H17 122(2) . . ? C16 C17 H17 117(2) . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 114(2) . . ? C17 C18 H18 126(2) . . ? C20 C19 C18 119.9(4) . . ? C20 C19 H19 121(3) . . ? C18 C19 H19 119(3) . . ? C19 C20 C21 120.2(4) . . ? C19 C20 H20 122(2) . . ? C21 C20 H20 118(2) . . ? C16 C21 C20 120.6(4) . . ? C16 C21 H21 120(2) . . ? C20 C21 H21 120(2) . . ? C27 C22 C23 118.7(4) . . ? C27 C22 P2 121.4(3) . . ? C23 C22 P2 119.7(3) . . ? C22 C23 C24 120.0(4) . . ? C22 C23 H23 117(2) . . ? C24 C23 H23 122(2) . . ? C25 C24 C23 120.9(4) . . ? C25 C24 H24 122(3) . . ? C23 C24 H24 117(3) . . ? C24 C25 C26 119.8(4) . . ? C24 C25 H25 120(3) . . ? C26 C25 H25 120(3) . . ? C25 C26 C27 119.5(5) . . ? C25 C26 H26 122(3) . . ? C27 C26 H26 118(3) . . ? C22 C27 C26 121.1(4) . . ? C22 C27 H27 117(3) . . ? C26 C27 H27 121(3) . . ? C33 C28 C29 118.8(3) . . ? C33 C28 P3 120.8(3) . . ? C29 C28 P3 120.1(3) . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 120(2) . . ? C28 C29 H29 120(2) . . ? C31 C30 C29 120.1(4) . . ? C31 C30 H30 121(2) . . ? C29 C30 H30 119(2) . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 122(2) . . ? C30 C31 H31 118(2) . . ? C31 C32 C33 120.2(4) . . ? C31 C32 H32 121(3) . . ? C33 C32 H32 119(3) . . ? C32 C33 C28 120.5(4) . . ? C32 C33 H33 117(2) . . ? C28 C33 H33 122(2) . . ? C35 C34 C39 119.7(3) . . ? C35 C34 P3 121.1(3) . . ? C39 C34 P3 119.2(3) . . ? C34 C35 C36 120.0(3) . . ? C34 C35 H35 118(2) . . ? C36 C35 H35 122(2) . . ? C37 C36 C35 120.1(4) . . ? C37 C36 H36 121(2) . . ? C35 C36 H36 118(2) . . ? C38 C37 C36 120.1(4) . . ? C38 C37 H37 121(2) . . ? C36 C37 H37 119(2) . . ? C37 C38 C39 120.7(4) . . ? C37 C38 H38 118(2) . . ? C39 C38 H38 121(2) . . ? C38 C39 C34 119.5(4) . . ? C38 C39 H39 122(2) . . ? C34 C39 H39 118(2) . . ? C41 C40 C45 119.8(3) . . ? C41 C40 P4 119.6(3) . . ? C45 C40 P4 120.6(3) . . ? C42 C41 C40 119.4(4) . . ? C42 C41 H41 119(2) . . ? C40 C41 H41 121(2) . . ? C43 C42 C41 120.5(4) . . ? C43 C42 H42 121(2) . . ? C41 C42 H42 118(2) . . ? C42 C43 C44 120.4(4) . . ? C42 C43 H43 118(2) . . ? C44 C43 H43 122(2) . . ? C43 C44 C45 119.6(4) . . ? C43 C44 H44 119(3) . . ? C45 C44 H44 122(3) . . ? C44 C45 C40 120.3(4) . . ? C44 C45 H45 121(3) . . ? C40 C45 H45 119(3) . . ? C51 C46 C47 118.0(3) . . ? C51 C46 P4 120.4(3) . . ? C47 C46 P4 121.6(3) . . ? C48 C47 C46 120.7(4) . . ? C48 C47 H47 117(3) . . ? C46 C47 H47 123(3) . . ? C49 C48 C47 120.5(4) . . ? C49 C48 H48 118(2) . . ? C47 C48 H48 121(2) . . ? C48 C49 C50 119.1(4) . . ? C48 C49 H49 124(3) . . ? C50 C49 H49 117(3) . . ? C49 C50 C51 120.7(4) . . ? C49 C50 H50 119(3) . . ? C51 C50 H50 120(3) . . ? C50 C51 C46 120.8(4) . . ? C50 C51 H51 120(3) . . ? C46 C51 H51 119(3) . . ? C53 C52 H52A 109.5 . . ? C53 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O3 C53 C54 122.2(4) . . ? O3 C53 C52 122.4(4) . . ? C54 C53 C52 115.3(4) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O4 C56 C55 122.1(5) . . ? O4 C56 C57 122.1(4) . . ? C55 C56 C57 115.8(4) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 H58A 109.5 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C59 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O5 C59 C60 121.8(4) . . ? O5 C59 C58 121.8(4) . . ? C60 C59 C58 116.4(4) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Ir1 P1 C1 1.29(12) . . . . ? P4 Ir1 P1 C1 -175.77(12) . . . . ? Cl1 Ir1 P1 C1 94.70(12) . . . . ? P2 Ir1 P1 C4 -116.29(14) . . . . ? P4 Ir1 P1 C4 66.66(14) . . . . ? Cl1 Ir1 P1 C4 -22.87(14) . . . . ? P2 Ir1 P1 C10 119.08(14) . . . . ? P4 Ir1 P1 C10 -57.97(14) . . . . ? Cl1 Ir1 P1 C10 -147.50(13) . . . . ? P3 Ir1 P2 C1 170.78(12) . . . . ? P1 Ir1 P2 C1 -1.29(12) . . . . ? Cl1 Ir1 P2 C1 -95.57(12) . . . . ? P3 Ir1 P2 C16 -68.43(14) . . . . ? P1 Ir1 P2 C16 119.51(14) . . . . ? Cl1 Ir1 P2 C16 25.23(13) . . . . ? P3 Ir1 P2 C22 54.46(14) . . . . ? P1 Ir1 P2 C22 -117.61(14) . . . . ? Cl1 Ir1 P2 C22 148.11(14) . . . . ? P2 Ir1 P3 C34 -76.94(13) . . . . ? P4 Ir1 P3 C34 100.19(13) . . . . ? Cl1 Ir1 P3 C34 -172.92(13) . . . . ? P2 Ir1 P3 C28 55.95(15) . . . . ? P4 Ir1 P3 C28 -126.92(15) . . . . ? Cl1 Ir1 P3 C28 -40.03(15) . . . . ? P2 Ir1 P3 C3 171.98(13) . . . . ? P4 Ir1 P3 C3 -10.88(13) . . . . ? Cl1 Ir1 P3 C3 76.01(13) . . . . ? P3 Ir1 P4 C40 122.69(14) . . . . ? P1 Ir1 P4 C40 -65.35(14) . . . . ? Cl1 Ir1 P4 C40 29.89(14) . . . . ? P3 Ir1 P4 C46 -101.35(14) . . . . ? P1 Ir1 P4 C46 70.61(14) . . . . ? Cl1 Ir1 P4 C46 165.84(14) . . . . ? P3 Ir1 P4 C3 10.79(13) . . . . ? P1 Ir1 P4 C3 -177.25(13) . . . . ? Cl1 Ir1 P4 C3 -82.02(13) . . . . ? C4 P1 C1 C2 -66.4(4) . . . . ? C10 P1 C1 C2 48.3(4) . . . . ? Ir1 P1 C1 C2 169.2(3) . . . . ? C4 P1 C1 P2 122.79(17) . . . . ? C10 P1 C1 P2 -122.50(18) . . . . ? Ir1 P1 C1 P2 -1.63(15) . . . . ? C16 P2 C1 C2 64.5(4) . . . . ? C22 P2 C1 C2 -48.8(4) . . . . ? Ir1 P2 C1 C2 -169.0(3) . . . . ? C16 P2 C1 P1 -124.88(18) . . . . ? C22 P2 C1 P1 121.84(17) . . . . ? Ir1 P2 C1 P1 1.64(15) . . . . ? P1 C1 C2 O2 13.0(5) . . . . ? P2 C1 C2 O2 -178.9(3) . . . . ? P1 C1 C2 O1 -166.9(3) . . . . ? P2 C1 C2 O1 1.2(5) . . . . ? C34 P3 C3 P4 -109.15(17) . . . . ? C28 P3 C3 P4 140.16(16) . . . . ? Ir1 P3 C3 P4 13.16(15) . . . . ? C40 P4 C3 P3 -138.39(16) . . . . ? C46 P4 C3 P3 111.87(18) . . . . ? Ir1 P4 C3 P3 -13.03(15) . . . . ? C1 P1 C4 C5 147.0(3) . . . . ? C10 P1 C4 C5 26.4(3) . . . . ? Ir1 P1 C4 C5 -104.5(3) . . . . ? C1 P1 C4 C9 -40.3(3) . . . . ? C10 P1 C4 C9 -161.0(3) . . . . ? Ir1 P1 C4 C9 68.2(3) . . . . ? C9 C4 C5 C6 -0.3(6) . . . . ? P1 C4 C5 C6 172.4(3) . . . . ? C4 C5 C6 C7 0.1(6) . . . . ? C5 C6 C7 C8 0.3(7) . . . . ? C6 C7 C8 C9 -0.6(7) . . . . ? C7 C8 C9 C4 0.4(6) . . . . ? C5 C4 C9 C8 0.0(6) . . . . ? P1 C4 C9 C8 -172.9(3) . . . . ? C1 P1 C10 C11 120.0(4) . . . . ? C4 P1 C10 C11 -120.2(4) . . . . ? Ir1 P1 C10 C11 12.7(4) . . . . ? C1 P1 C10 C15 -59.8(4) . . . . ? C4 P1 C10 C15 60.0(4) . . . . ? Ir1 P1 C10 C15 -167.1(3) . . . . ? C15 C10 C11 C12 0.7(9) . . . . ? P1 C10 C11 C12 -179.2(5) . . . . ? C10 C11 C12 C13 0.3(11) . . . . ? C11 C12 C13 C14 -1.0(11) . . . . ? C12 C13 C14 C15 0.6(8) . . . . ? C13 C14 C15 C10 0.4(7) . . . . ? C11 C10 C15 C14 -1.0(7) . . . . ? P1 C10 C15 C14 178.8(3) . . . . ? C1 P2 C16 C21 -46.4(4) . . . . ? C22 P2 C16 C21 72.8(3) . . . . ? Ir1 P2 C16 C21 -157.6(3) . . . . ? C1 P2 C16 C17 136.9(3) . . . . ? C22 P2 C16 C17 -103.9(3) . . . . ? Ir1 P2 C16 C17 25.7(3) . . . . ? C21 C16 C17 C18 0.0(6) . . . . ? P2 C16 C17 C18 176.7(3) . . . . ? C16 C17 C18 C19 0.9(6) . . . . ? C17 C18 C19 C20 -1.2(6) . . . . ? C18 C19 C20 C21 0.7(6) . . . . ? C17 C16 C21 C20 -0.5(6) . . . . ? P2 C16 C21 C20 -177.3(3) . . . . ? C19 C20 C21 C16 0.2(6) . . . . ? C1 P2 C22 C27 159.0(3) . . . . ? C16 P2 C22 C27 38.4(3) . . . . ? Ir1 P2 C22 C27 -94.2(3) . . . . ? C1 P2 C22 C23 -26.2(3) . . . . ? C16 P2 C22 C23 -146.9(3) . . . . ? Ir1 P2 C22 C23 80.5(3) . . . . ? C27 C22 C23 C24 0.7(5) . . . . ? P2 C22 C23 C24 -174.1(3) . . . . ? C22 C23 C24 C25 0.4(6) . . . . ? C23 C24 C25 C26 -0.7(7) . . . . ? C24 C25 C26 C27 -0.3(7) . . . . ? C23 C22 C27 C26 -1.7(5) . . . . ? P2 C22 C27 C26 173.1(3) . . . . ? C25 C26 C27 C22 1.5(6) . . . . ? C34 P3 C28 C33 34.7(3) . . . . ? C3 P3 C28 C33 146.5(3) . . . . ? Ir1 P3 C28 C33 -104.1(3) . . . . ? C34 P3 C28 C29 -151.5(3) . . . . ? C3 P3 C28 C29 -39.7(3) . . . . ? Ir1 P3 C28 C29 69.7(3) . . . . ? C33 C28 C29 C30 -1.8(5) . . . . ? P3 C28 C29 C30 -175.8(3) . . . . ? C28 C29 C30 C31 1.7(6) . . . . ? C29 C30 C31 C32 -0.6(6) . . . . ? C30 C31 C32 C33 -0.5(6) . . . . ? C31 C32 C33 C28 0.4(6) . . . . ? C29 C28 C33 C32 0.7(5) . . . . ? P3 C28 C33 C32 174.6(3) . . . . ? C28 P3 C34 C35 -109.2(3) . . . . ? C3 P3 C34 C35 136.9(3) . . . . ? Ir1 P3 C34 C35 31.4(3) . . . . ? C28 P3 C34 C39 69.8(3) . . . . ? C3 P3 C34 C39 -44.2(3) . . . . ? Ir1 P3 C34 C39 -149.7(2) . . . . ? C39 C34 C35 C36 0.0(5) . . . . ? P3 C34 C35 C36 179.0(3) . . . . ? C34 C35 C36 C37 1.3(6) . . . . ? C35 C36 C37 C38 -1.7(6) . . . . ? C36 C37 C38 C39 0.7(6) . . . . ? C37 C38 C39 C34 0.6(6) . . . . ? C35 C34 C39 C38 -0.9(5) . . . . ? P3 C34 C39 C38 -179.9(3) . . . . ? C46 P4 C40 C41 69.2(3) . . . . ? C3 P4 C40 C41 -42.3(3) . . . . ? Ir1 P4 C40 C41 -148.2(2) . . . . ? C46 P4 C40 C45 -109.4(3) . . . . ? C3 P4 C40 C45 139.1(3) . . . . ? Ir1 P4 C40 C45 33.1(3) . . . . ? C45 C40 C41 C42 0.7(6) . . . . ? P4 C40 C41 C42 -178.0(3) . . . . ? C40 C41 C42 C43 0.9(6) . . . . ? C41 C42 C43 C44 -1.4(6) . . . . ? C42 C43 C44 C45 0.3(6) . . . . ? C43 C44 C45 C40 1.2(6) . . . . ? C41 C40 C45 C44 -1.7(6) . . . . ? P4 C40 C45 C44 176.9(3) . . . . ? C40 P4 C46 C51 -169.5(3) . . . . ? C3 P4 C46 C51 -58.2(3) . . . . ? Ir1 P4 C46 C51 47.7(3) . . . . ? C40 P4 C46 C47 12.8(3) . . . . ? C3 P4 C46 C47 124.1(3) . . . . ? Ir1 P4 C46 C47 -130.0(3) . . . . ? C51 C46 C47 C48 1.1(6) . . . . ? P4 C46 C47 C48 178.9(3) . . . . ? C46 C47 C48 C49 -0.2(7) . . . . ? C47 C48 C49 C50 -0.2(6) . . . . ? C48 C49 C50 C51 -0.4(6) . . . . ? C49 C50 C51 C46 1.4(6) . . . . ? C47 C46 C51 C50 -1.7(6) . . . . ? P4 C46 C51 C50 -179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.729 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.114