# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hashimoto, Hisako' _publ_contact_author_email hhashimoto@m.tains.tohoku.ac.jp loop_ _publ_author_name H.Hashimoto T.Suzuki H.Tobita data_the-PcyN-ligand _database_code_depnum_ccdc_archive 'CCDC 772158' #TrackingRef '- ToshiCIFs(ESI).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H34 N P' _chemical_formula_sum 'C21 H34 N P' _chemical_formula_weight 331.46 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 9.2587(4) _cell_length_b 11.4129(4) _cell_length_c 18.1566(8) _cell_angle_alpha 90.00 _cell_angle_beta 91.1041(13) _cell_angle_gamma 90.00 _cell_volume 1918.23(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4309 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.144 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9731 _exptl_absorpt_correction_T_max 0.9815 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15535 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4309 _reflns_number_gt 3732 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0457P)^2^+2.5404P] 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 4309 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1483 _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.18920(7) 0.14184(5) 0.18515(3) 0.01604(17) Uani 1 1 d . . . N1 N -0.0336(2) 0.1495(2) 0.30436(12) 0.0215(5) Uani 1 1 d . . . C1 C 0.2114(3) 0.0798(2) 0.27930(13) 0.0177(5) Uani 1 1 d . . . C2 C 0.0981(3) 0.0941(2) 0.32910(13) 0.0181(5) Uani 1 1 d . . . C3 C 0.1149(3) 0.0523(2) 0.40089(13) 0.0222(5) Uani 1 1 d . . . H1 H 0.0384 0.0620 0.4345 0.027 Uiso 1 1 calc R . . C4 C 0.2408(3) -0.0031(2) 0.42441(14) 0.0224(6) Uani 1 1 d . . . H2 H 0.2491 -0.0313 0.4735 0.027 Uiso 1 1 calc R . . C5 C 0.3548(3) -0.0177(2) 0.37686(13) 0.0198(5) Uani 1 1 d . . . C6 C 0.3377(3) 0.0247(2) 0.30495(13) 0.0181(5) Uani 1 1 d . . . H3 H 0.4153 0.0156 0.2720 0.022 Uiso 1 1 calc R . . C7 C 0.4936(3) -0.0774(3) 0.40076(15) 0.0277(6) Uani 1 1 d . . . H4 H 0.4902 -0.0958 0.4534 0.042 Uiso 1 1 calc R . . H5 H 0.5754 -0.0253 0.3917 0.042 Uiso 1 1 calc R . . H6 H 0.5052 -0.1500 0.3727 0.042 Uiso 1 1 calc R . . C8 C 0.1036(3) 0.0208(2) 0.13074(13) 0.0179(5) Uani 1 1 d . . . H7 H 0.0981 0.0500 0.0788 0.021 Uiso 1 1 calc R . . C9 C 0.1846(3) -0.0959(2) 0.12712(14) 0.0219(5) Uani 1 1 d . . . H8 H 0.1888 -0.1319 0.1767 0.026 Uiso 1 1 calc R . . H9 H 0.2848 -0.0818 0.1113 0.026 Uiso 1 1 calc R . . C10 C 0.1091(3) -0.1803(2) 0.07279(15) 0.0261(6) Uani 1 1 d . . . H10 H 0.1154 -0.1483 0.0223 0.031 Uiso 1 1 calc R . . H11 H 0.1597 -0.2567 0.0739 0.031 Uiso 1 1 calc R . . C11 C -0.0488(3) -0.1989(3) 0.09121(15) 0.0293(6) Uani 1 1 d . . . H12 H -0.0548 -0.2426 0.1381 0.035 Uiso 1 1 calc R . . H13 H -0.0957 -0.2468 0.0521 0.035 Uiso 1 1 calc R . . C12 C -0.1294(3) -0.0831(3) 0.09822(15) 0.0284(6) Uani 1 1 d . . . H14 H -0.2287 -0.0986 0.1150 0.034 Uiso 1 1 calc R . . H15 H -0.1366 -0.0451 0.0493 0.034 Uiso 1 1 calc R . . C13 C -0.0533(3) -0.0001(3) 0.15267(14) 0.0248(6) Uani 1 1 d . . . H16 H -0.0552 -0.0342 0.2028 0.030 Uiso 1 1 calc R . . H17 H -0.1054 0.0756 0.1536 0.030 Uiso 1 1 calc R . . C14 C 0.3774(3) 0.1408(2) 0.15139(12) 0.0182(5) Uani 1 1 d . . . H18 H 0.4226 0.0631 0.1628 0.022 Uiso 1 1 calc R . . C15 C 0.4634(3) 0.2377(2) 0.19171(13) 0.0200(5) Uani 1 1 d . . . H19 H 0.4153 0.3141 0.1830 0.024 Uiso 1 1 calc R . . H20 H 0.4637 0.2221 0.2454 0.024 Uiso 1 1 calc R . . C16 C 0.6190(3) 0.2444(3) 0.16553(15) 0.0261(6) Uani 1 1 d . . . H21 H 0.6697 0.3094 0.1912 0.031 Uiso 1 1 calc R . . H22 H 0.6698 0.1706 0.1781 0.031 Uiso 1 1 calc R . . C17 C 0.6232(3) 0.2641(3) 0.08256(15) 0.0296(6) Uani 1 1 d . . . H23 H 0.7247 0.2627 0.0664 0.035 Uiso 1 1 calc R . . H24 H 0.5824 0.3421 0.0705 0.035 Uiso 1 1 calc R . . C18 C 0.5369(3) 0.1694(3) 0.04141(14) 0.0264(6) Uani 1 1 d . . . H25 H 0.5361 0.1868 -0.0120 0.032 Uiso 1 1 calc R . . H26 H 0.5845 0.0926 0.0490 0.032 Uiso 1 1 calc R . . C19 C 0.3814(3) 0.1624(2) 0.06797(13) 0.0211(5) Uani 1 1 d . . . H27 H 0.3302 0.0981 0.0419 0.025 Uiso 1 1 calc R . . H28 H 0.3307 0.2366 0.0561 0.025 Uiso 1 1 calc R . . C20 C -0.1641(3) 0.1076(3) 0.33851(17) 0.0331(7) Uani 1 1 d . . . H29 H -0.1640 0.0218 0.3390 0.050 Uiso 1 1 calc R . . H30 H -0.2486 0.1358 0.3104 0.050 Uiso 1 1 calc R . . H31 H -0.1678 0.1370 0.3891 0.050 Uiso 1 1 calc R . . C21 C -0.0270(3) 0.2775(2) 0.30547(15) 0.0247(6) Uani 1 1 d . . . H32 H -0.0227 0.3050 0.3566 0.037 Uiso 1 1 calc R . . H33 H -0.1133 0.3096 0.2807 0.037 Uiso 1 1 calc R . . H34 H 0.0594 0.3038 0.2798 0.037 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 P1 0.0157(3) 0.0186(3) 0.0139(3) 0.0002(2) 0.0015(2) 0.0020(2) N1 0.0165(11) 0.0257(11) 0.0223(11) -0.0015(9) 0.0027(8) 0.0015(9) C1 0.0217(13) 0.0176(12) 0.0140(11) -0.0005(9) 0.0007(9) -0.0005(10) C2 0.0167(13) 0.0201(12) 0.0176(12) -0.0022(9) -0.0002(9) -0.0014(9) C3 0.0244(14) 0.0266(14) 0.0157(12) -0.0018(10) 0.0041(10) -0.0043(11) C4 0.0265(15) 0.0247(13) 0.0159(12) 0.0016(10) -0.0019(10) -0.0046(11) C5 0.0212(14) 0.0171(12) 0.0209(12) -0.0007(9) -0.0032(10) -0.0029(10) C6 0.0154(13) 0.0202(12) 0.0188(12) -0.0023(9) 0.0019(9) 0.0021(9) C7 0.0264(16) 0.0320(15) 0.0245(13) 0.0047(11) -0.0070(11) 0.0008(12) C8 0.0165(13) 0.0217(12) 0.0154(11) 0.0002(9) -0.0012(9) -0.0021(10) C9 0.0200(14) 0.0210(13) 0.0247(13) 0.0013(10) -0.0013(10) -0.0005(10) C10 0.0306(16) 0.0202(13) 0.0276(14) -0.0021(10) 0.0010(11) -0.0016(11) C11 0.0360(17) 0.0310(15) 0.0207(13) 0.0008(11) -0.0038(11) -0.0147(12) C12 0.0185(14) 0.0445(17) 0.0220(13) -0.0016(12) -0.0011(10) -0.0072(12) C13 0.0173(14) 0.0367(16) 0.0204(13) -0.0026(11) 0.0003(10) -0.0026(11) C14 0.0178(13) 0.0228(12) 0.0139(11) -0.0019(9) 0.0013(9) 0.0008(10) C15 0.0199(13) 0.0249(13) 0.0153(11) -0.0031(9) 0.0002(9) -0.0036(10) C16 0.0208(14) 0.0339(15) 0.0236(13) -0.0019(11) -0.0002(10) -0.0035(11) C17 0.0240(15) 0.0403(17) 0.0248(14) -0.0019(12) 0.0090(11) -0.0063(12) C18 0.0235(15) 0.0391(16) 0.0169(12) -0.0041(11) 0.0076(10) -0.0037(12) C19 0.0215(14) 0.0282(14) 0.0136(11) -0.0011(9) 0.0009(9) -0.0005(10) C20 0.0220(15) 0.0446(18) 0.0328(15) 0.0051(13) 0.0072(12) 0.0020(13) C21 0.0210(14) 0.0274(14) 0.0257(14) -0.0063(11) -0.0028(10) 0.0073(11) _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 P1 C1 1.858(2) . ? P1 C14 1.859(3) . ? P1 C8 1.866(2) . ? N1 C2 1.438(3) . ? N1 C20 1.450(3) . ? N1 C21 1.462(3) . ? C1 C6 1.400(3) . ? C1 C2 1.407(3) . ? C2 C3 1.394(3) . ? C3 C4 1.386(4) . ? C3 H1 0.9500 . ? C4 C5 1.387(4) . ? C4 H2 0.9500 . ? C5 C6 1.398(3) . ? C5 C7 1.511(4) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C9 1.530(4) . ? C8 C13 1.533(4) . ? C8 H7 1.0000 . ? C9 C10 1.537(4) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.521(4) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.524(4) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.531(4) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C19 1.536(3) . ? C14 C15 1.540(3) . ? C14 H18 1.0000 . ? C15 C16 1.528(4) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.524(4) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.531(4) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.528(4) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 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 C1 P1 C14 102.31(11) . . ? C1 P1 C8 104.07(11) . . ? C14 P1 C8 102.23(11) . . ? C2 N1 C20 115.5(2) . . ? C2 N1 C21 113.6(2) . . ? C20 N1 C21 111.0(2) . . ? C6 C1 C2 117.8(2) . . ? C6 C1 P1 123.66(19) . . ? C2 C1 P1 118.45(18) . . ? C3 C2 C1 119.3(2) . . ? C3 C2 N1 121.4(2) . . ? C1 C2 N1 119.2(2) . . ? C4 C3 C2 121.5(2) . . ? C4 C3 H1 119.3 . . ? C2 C3 H1 119.3 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H2 119.7 . . ? C5 C4 H2 119.7 . . ? C4 C5 C6 117.8(2) . . ? C4 C5 C7 121.9(2) . . ? C6 C5 C7 120.3(2) . . ? C5 C6 C1 123.0(2) . . ? C5 C6 H3 118.5 . . ? C1 C6 H3 118.5 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C9 C8 C13 110.1(2) . . ? C9 C8 P1 117.64(17) . . ? C13 C8 P1 111.87(17) . . ? C9 C8 H7 105.4 . . ? C13 C8 H7 105.4 . . ? P1 C8 H7 105.4 . . ? C8 C9 C10 110.9(2) . . ? C8 C9 H8 109.5 . . ? C10 C9 H8 109.5 . . ? C8 C9 H9 109.5 . . ? C10 C9 H9 109.5 . . ? H8 C9 H9 108.1 . . ? C11 C10 C9 111.9(2) . . ? C11 C10 H10 109.2 . . ? C9 C10 H10 109.2 . . ? C11 C10 H11 109.2 . . ? C9 C10 H11 109.2 . . ? H10 C10 H11 107.9 . . ? C10 C11 C12 111.8(2) . . ? C10 C11 H12 109.2 . . ? C12 C11 H12 109.2 . . ? C10 C11 H13 109.2 . . ? C12 C11 H13 109.2 . . ? H12 C11 H13 107.9 . . ? C11 C12 C13 111.8(2) . . ? C11 C12 H14 109.3 . . ? C13 C12 H14 109.3 . . ? C11 C12 H15 109.3 . . ? C13 C12 H15 109.3 . . ? H14 C12 H15 107.9 . . ? C12 C13 C8 110.8(2) . . ? C12 C13 H16 109.5 . . ? C8 C13 H16 109.5 . . ? C12 C13 H17 109.5 . . ? C8 C13 H17 109.5 . . ? H16 C13 H17 108.1 . . ? C19 C14 C15 109.3(2) . . ? C19 C14 P1 111.39(17) . . ? C15 C14 P1 108.53(16) . . ? C19 C14 H18 109.2 . . ? C15 C14 H18 109.2 . . ? P1 C14 H18 109.2 . . ? C16 C15 C14 111.7(2) . . ? C16 C15 H19 109.3 . . ? C14 C15 H19 109.3 . . ? C16 C15 H20 109.3 . . ? C14 C15 H20 109.3 . . ? H19 C15 H20 107.9 . . ? C17 C16 C15 110.9(2) . . ? C17 C16 H21 109.4 . . ? C15 C16 H21 109.4 . . ? C17 C16 H22 109.4 . . ? C15 C16 H22 109.4 . . ? H21 C16 H22 108.0 . . ? C16 C17 C18 110.8(2) . . ? C16 C17 H23 109.5 . . ? C18 C17 H23 109.5 . . ? C16 C17 H24 109.5 . . ? C18 C17 H24 109.5 . . ? H23 C17 H24 108.1 . . ? C19 C18 C17 111.6(2) . . ? C19 C18 H25 109.3 . . ? C17 C18 H25 109.3 . . ? C19 C18 H26 109.3 . . ? C17 C18 H26 109.3 . . ? H25 C18 H26 108.0 . . ? C18 C19 C14 111.1(2) . . ? C18 C19 H27 109.4 . . ? C14 C19 H27 109.4 . . ? C18 C19 H28 109.4 . . ? C14 C19 H28 109.4 . . ? H27 C19 H28 108.0 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 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 C14 P1 C1 C6 -12.5(2) . . . . ? C8 P1 C1 C6 93.7(2) . . . . ? C14 P1 C1 C2 164.10(19) . . . . ? C8 P1 C1 C2 -89.7(2) . . . . ? C6 C1 C2 C3 -0.7(4) . . . . ? P1 C1 C2 C3 -177.47(19) . . . . ? C6 C1 C2 N1 -179.5(2) . . . . ? P1 C1 C2 N1 3.7(3) . . . . ? C20 N1 C2 C3 -31.3(3) . . . . ? C21 N1 C2 C3 98.6(3) . . . . ? C20 N1 C2 C1 147.4(2) . . . . ? C21 N1 C2 C1 -82.7(3) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? N1 C2 C3 C4 178.8(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 -0.3(4) . . . . ? C3 C4 C5 C7 179.9(2) . . . . ? C4 C5 C6 C1 -0.4(4) . . . . ? C7 C5 C6 C1 179.4(2) . . . . ? C2 C1 C6 C5 0.9(4) . . . . ? P1 C1 C6 C5 177.48(19) . . . . ? C1 P1 C8 C9 -58.4(2) . . . . ? C14 P1 C8 C9 47.8(2) . . . . ? C1 P1 C8 C13 70.5(2) . . . . ? C14 P1 C8 C13 176.73(18) . . . . ? C13 C8 C9 C10 57.3(3) . . . . ? P1 C8 C9 C10 -172.99(18) . . . . ? C8 C9 C10 C11 -55.2(3) . . . . ? C9 C10 C11 C12 53.0(3) . . . . ? C10 C11 C12 C13 -53.4(3) . . . . ? C11 C12 C13 C8 55.9(3) . . . . ? C9 C8 C13 C12 -57.7(3) . . . . ? P1 C8 C13 C12 169.52(19) . . . . ? C1 P1 C14 C19 167.06(18) . . . . ? C8 P1 C14 C19 59.5(2) . . . . ? C1 P1 C14 C15 -72.51(19) . . . . ? C8 P1 C14 C15 179.91(17) . . . . ? C19 C14 C15 C16 -56.9(3) . . . . ? P1 C14 C15 C16 -178.64(18) . . . . ? C14 C15 C16 C17 57.0(3) . . . . ? C15 C16 C17 C18 -55.3(3) . . . . ? C16 C17 C18 C19 55.5(3) . . . . ? C17 C18 C19 C14 -56.5(3) . . . . ? C15 C14 C19 C18 56.4(3) . . . . ? P1 C14 C19 C18 176.31(18) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.322 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.091 #===END data_(PcyN-P,N)RhCl(coe)-(2) _database_code_depnum_ccdc_archive 'CCDC 772159' #TrackingRef '- ToshiCIFs(ESI).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H48 Cl N P Rh' _chemical_formula_sum 'C29 H48 Cl N P Rh' _chemical_formula_weight 580.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6574(8) _cell_length_b 11.9410(8) _cell_length_c 13.8776(11) _cell_angle_alpha 105.204(3) _cell_angle_beta 108.539(3) _cell_angle_gamma 98.699(4) _cell_volume 1415.23(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6414 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9268 _exptl_absorpt_correction_T_max 0.9338 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13492 _diffrn_reflns_av_R_equivalents 0.1127 _diffrn_reflns_av_sigmaI/netI 0.1397 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6414 _reflns_number_gt 4762 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0757P)^2^+13.7475P] 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 6414 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1519 _refine_ls_R_factor_gt 0.1091 _refine_ls_wR_factor_ref 0.2450 _refine_ls_wR_factor_gt 0.2206 _refine_ls_goodness_of_fit_ref 1.232 _refine_ls_restrained_S_all 1.232 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.65074(8) 0.76018(7) 0.67829(6) 0.0130(2) Uani 1 1 d . . . Cl1 Cl 0.8949(3) 0.7596(3) 0.6604(2) 0.0320(6) Uani 1 1 d . . . P1 P 0.4388(3) 0.7975(2) 0.68689(19) 0.0149(5) Uani 1 1 d . . . N1 N 0.5661(9) 0.7784(7) 0.5177(7) 0.0207(17) Uani 1 1 d . . . C1 C 0.3353(11) 0.8033(8) 0.5536(7) 0.0173(19) Uani 1 1 d . . . C2 C 0.4097(10) 0.7879(8) 0.4830(7) 0.0173(19) Uani 1 1 d . . . C3 C 0.3318(11) 0.7821(8) 0.3760(7) 0.020(2) Uani 1 1 d . . . H1 H 0.3791 0.7666 0.3251 0.024 Uiso 1 1 calc R . . C4 C 0.1896(11) 0.7985(8) 0.3448(8) 0.022(2) Uani 1 1 d . . . H2 H 0.1407 0.7964 0.2729 0.026 Uiso 1 1 calc R . . C5 C 0.1143(10) 0.8184(8) 0.4156(8) 0.0176(19) Uani 1 1 d . . . C6 C 0.1875(11) 0.8171(8) 0.5190(8) 0.019(2) Uani 1 1 d . . . H3 H 0.1362 0.8257 0.5676 0.023 Uiso 1 1 calc R . . C7 C -0.0412(12) 0.8406(10) 0.3811(9) 0.029(2) Uani 1 1 d . . . H4 H -0.1077 0.7776 0.3134 0.044 Uiso 1 1 calc R . . H5 H -0.0341 0.9190 0.3707 0.044 Uiso 1 1 calc R . . H6 H -0.0826 0.8395 0.4369 0.044 Uiso 1 1 calc R . . C8 C 0.2901(10) 0.6998(8) 0.7084(7) 0.0171(19) Uani 1 1 d . . . H7 H 0.1986 0.7319 0.6916 0.021 Uiso 1 1 calc R . . C9 C 0.2463(11) 0.5712(8) 0.6276(8) 0.020(2) Uani 1 1 d . . . H8 H 0.2140 0.5738 0.5532 0.024 Uiso 1 1 calc R . . H9 H 0.3352 0.5371 0.6408 0.024 Uiso 1 1 calc R . . C10 C 0.1182(11) 0.4916(9) 0.6399(9) 0.027(2) Uani 1 1 d . . . H10 H 0.0959 0.4083 0.5914 0.033 Uiso 1 1 calc R . . H11 H 0.0260 0.5206 0.6187 0.033 Uiso 1 1 calc R . . C11 C 0.1604(14) 0.4926(10) 0.7564(10) 0.034(3) Uani 1 1 d . . . H12 H 0.0733 0.4441 0.7631 0.041 Uiso 1 1 calc R . . H13 H 0.2458 0.4553 0.7749 0.041 Uiso 1 1 calc R . . C12 C 0.2042(11) 0.6181(9) 0.8341(8) 0.026(2) Uani 1 1 d . . . H14 H 0.2346 0.6156 0.9085 0.031 Uiso 1 1 calc R . . H15 H 0.1156 0.6524 0.8200 0.031 Uiso 1 1 calc R . . C13 C 0.3344(11) 0.6996(9) 0.8248(8) 0.023(2) Uani 1 1 d . . . H16 H 0.4264 0.6701 0.8451 0.027 Uiso 1 1 calc R . . H17 H 0.3566 0.7823 0.8743 0.027 Uiso 1 1 calc R . . C14 C 0.4684(9) 0.9476(8) 0.7859(7) 0.0156(18) Uani 1 1 d . . . H18 H 0.5084 0.9398 0.8591 0.019 Uiso 1 1 calc R . . C15 C 0.3253(11) 0.9937(9) 0.7776(8) 0.022(2) Uani 1 1 d . . . H19 H 0.2811 1.0025 0.7060 0.027 Uiso 1 1 calc R . . H20 H 0.2492 0.9347 0.7853 0.027 Uiso 1 1 calc R . . C16 C 0.3643(12) 1.1144(9) 0.8653(9) 0.029(2) Uani 1 1 d . . . H21 H 0.2722 1.1441 0.8569 0.034 Uiso 1 1 calc R . . H22 H 0.3992 1.1035 0.9367 0.034 Uiso 1 1 calc R . . C17 C 0.4854(12) 1.2067(9) 0.8610(9) 0.027(2) Uani 1 1 d . . . H23 H 0.5115 1.2820 0.9216 0.032 Uiso 1 1 calc R . . H24 H 0.4466 1.2244 0.7930 0.032 Uiso 1 1 calc R . . C18 C 0.6279(11) 1.1616(9) 0.8676(8) 0.023(2) Uani 1 1 d . . . H25 H 0.7023 1.2209 0.8589 0.027 Uiso 1 1 calc R . . H26 H 0.6741 1.1537 0.9394 0.027 Uiso 1 1 calc R . . C19 C 0.5907(11) 1.0409(8) 0.7809(9) 0.024(2) Uani 1 1 d . . . H27 H 0.6833 1.0118 0.7901 0.028 Uiso 1 1 calc R . . H28 H 0.5558 1.0510 0.7092 0.028 Uiso 1 1 calc R . . C20 C 0.5794(12) 0.6679(9) 0.4446(9) 0.029(2) Uani 1 1 d . . . H29 H 0.5016 0.5987 0.4356 0.044 Uiso 1 1 calc R . . H30 H 0.6796 0.6551 0.4758 0.044 Uiso 1 1 calc R . . H31 H 0.5657 0.6772 0.3743 0.044 Uiso 1 1 calc R . . C21 C 0.6635(11) 0.8855(9) 0.5152(8) 0.023(2) Uani 1 1 d . . . H32 H 0.6458 0.8795 0.4403 0.035 Uiso 1 1 calc R . . H33 H 0.7698 0.8897 0.5530 0.035 Uiso 1 1 calc R . . H34 H 0.6392 0.9581 0.5507 0.035 Uiso 1 1 calc R . . C22 C 0.7336(11) 0.7749(9) 0.8450(8) 0.022(2) Uani 1 1 d . . . H35 H 0.6682 0.8061 0.8832 0.026 Uiso 1 1 calc R . . C23 C 0.6726(11) 0.6541(8) 0.7792(8) 0.023(2) Uani 1 1 d . . . H36 H 0.5736 0.6188 0.7818 0.028 Uiso 1 1 calc R . . C24 C 0.7682(11) 0.5652(8) 0.7716(9) 0.025(2) Uani 1 1 d . A . H37 H 0.8718 0.6074 0.7835 0.030 Uiso 1 1 calc R . . H38 H 0.7244 0.5040 0.6989 0.030 Uiso 1 1 calc R . . C25 C 0.7738(14) 0.5050(9) 0.8558(9) 0.034(3) Uani 1 1 d . . . H39 H 0.6754 0.4460 0.8307 0.041 Uiso 0.71(3) 1 calc PR A 1 H40 H 0.8518 0.4595 0.8588 0.041 Uiso 0.71(3) 1 calc PR A 1 H41 H 0.7924 0.4251 0.8313 0.041 Uiso 0.29(3) 1 calc PR A 2 H42 H 0.6748 0.4931 0.8637 0.041 Uiso 0.29(3) 1 calc PR A 2 C26 C 0.806(2) 0.5829(15) 0.9671(14) 0.038(5) Uiso 0.71(3) 1 d P A 1 C27 C 0.960(2) 0.6788(16) 1.0142(14) 0.039(5) Uiso 0.71(3) 1 d P A 1 C28 C 0.9463(11) 0.8101(10) 1.0208(9) 0.030(2) Uani 1 1 d . . . H43 H 0.8707 0.8281 1.0528 0.036 Uiso 0.71(3) 1 calc PR A 1 H44 H 1.0447 0.8676 1.0691 0.036 Uiso 0.71(3) 1 calc PR A 1 H45 H 0.9385 0.8810 1.0730 0.036 Uiso 0.29(3) 1 calc PR A 2 H46 H 1.0541 0.8092 1.0439 0.036 Uiso 0.29(3) 1 calc PR A 2 C29 C 0.8997(11) 0.8279(9) 0.9108(8) 0.025(2) Uani 1 1 d . A . H47 H 0.9248 0.9149 0.9214 0.030 Uiso 1 1 calc R . . H48 H 0.9582 0.7900 0.8706 0.030 Uiso 1 1 calc R . . C30 C 0.911(4) 0.587(3) 0.977(3) 0.021(9) Uiso 0.29(3) 1 d P A 2 C31 C 0.858(3) 0.697(2) 1.029(2) 0.008(8) Uiso 0.29(3) 1 d P A 2 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 Rh1 0.0088(3) 0.0169(4) 0.0148(4) 0.0061(3) 0.0047(3) 0.0058(2) Cl1 0.0167(12) 0.0533(17) 0.0385(15) 0.0261(13) 0.0151(11) 0.0143(11) P1 0.0118(11) 0.0173(11) 0.0164(12) 0.0061(10) 0.0065(10) 0.0024(9) N1 0.014(4) 0.023(4) 0.023(4) 0.006(4) 0.006(3) 0.006(3) C1 0.019(5) 0.012(4) 0.017(5) -0.001(4) 0.007(4) 0.000(4) C2 0.016(4) 0.015(4) 0.018(5) 0.000(4) 0.008(4) 0.000(4) C3 0.018(5) 0.025(5) 0.013(4) 0.003(4) 0.006(4) 0.002(4) C4 0.024(5) 0.023(5) 0.017(5) 0.005(4) 0.008(4) 0.005(4) C5 0.015(4) 0.011(4) 0.020(5) 0.005(4) 0.002(4) 0.000(3) C6 0.019(5) 0.017(5) 0.025(5) 0.007(4) 0.011(4) 0.006(4) C7 0.023(5) 0.029(6) 0.025(5) 0.005(5) 0.000(4) 0.003(4) C8 0.012(4) 0.020(5) 0.019(5) 0.007(4) 0.006(4) 0.003(4) C9 0.019(5) 0.016(5) 0.021(5) 0.003(4) 0.007(4) -0.001(4) C10 0.017(5) 0.024(5) 0.034(6) 0.009(5) 0.006(4) -0.007(4) C11 0.037(7) 0.028(6) 0.043(7) 0.020(5) 0.017(6) 0.002(5) C12 0.017(5) 0.034(6) 0.022(5) 0.006(5) 0.008(4) -0.003(4) C13 0.016(5) 0.030(5) 0.020(5) 0.003(4) 0.012(4) 0.000(4) C14 0.007(4) 0.017(4) 0.020(5) 0.001(4) 0.005(4) 0.004(3) C15 0.015(5) 0.026(5) 0.021(5) 0.001(4) 0.006(4) 0.005(4) C16 0.023(5) 0.032(6) 0.029(6) 0.002(5) 0.013(5) 0.009(5) C17 0.032(6) 0.020(5) 0.022(5) -0.002(4) 0.009(5) 0.007(4) C18 0.020(5) 0.025(5) 0.022(5) 0.006(4) 0.008(4) 0.004(4) C19 0.014(5) 0.021(5) 0.031(6) 0.005(4) 0.007(4) -0.001(4) C20 0.021(5) 0.019(5) 0.039(6) -0.003(5) 0.009(5) 0.006(4) C21 0.014(5) 0.032(6) 0.024(5) 0.010(4) 0.007(4) 0.005(4) C22 0.018(5) 0.025(5) 0.024(5) 0.012(4) 0.005(4) 0.009(4) C23 0.021(5) 0.019(5) 0.025(5) 0.009(4) 0.005(4) -0.001(4) C24 0.014(5) 0.015(5) 0.039(6) 0.003(4) 0.006(4) 0.004(4) C25 0.038(6) 0.020(5) 0.038(7) 0.010(5) 0.005(5) 0.008(5) C28 0.011(5) 0.040(6) 0.025(5) 0.006(5) -0.002(4) -0.003(4) C29 0.018(5) 0.017(5) 0.032(6) 0.003(4) 0.002(4) 0.008(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 Rh1 C23 2.106(10) . ? Rh1 C22 2.142(10) . ? Rh1 P1 2.193(2) . ? Rh1 N1 2.198(9) . ? Rh1 Cl1 2.449(3) . ? P1 C1 1.827(10) . ? P1 C8 1.861(9) . ? P1 C14 1.866(9) . ? N1 C2 1.464(12) . ? N1 C21 1.484(12) . ? N1 C20 1.490(12) . ? C1 C2 1.379(13) . ? C1 C6 1.404(13) . ? C2 C3 1.413(13) . ? C3 C4 1.365(14) . ? C3 H1 0.9500 . ? C4 C5 1.390(13) . ? C4 H2 0.9500 . ? C5 C6 1.389(14) . ? C5 C7 1.511(14) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C13 1.534(13) . ? C8 C9 1.547(12) . ? C8 H7 1.0000 . ? C9 C10 1.526(13) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.533(16) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.503(15) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.530(13) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C19 1.529(12) . ? C14 C15 1.546(12) . ? C14 H18 1.0000 . ? C15 C16 1.525(13) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.509(15) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.537(14) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.520(13) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C22 C23 1.404(14) . ? C22 C29 1.505(13) . ? C22 H35 1.0000 . ? C23 C24 1.514(14) . ? C23 H36 1.0000 . ? C24 C25 1.516(15) . ? C24 H37 0.9900 . ? C24 H38 0.9900 . ? C25 C26 1.48(2) . ? C25 C30 1.69(4) . ? C25 H39 0.9900 . ? C25 H40 0.9900 . ? C25 H41 0.9900 . ? C25 H42 0.9900 . ? C26 C27 1.56(3) . ? C27 C28 1.57(2) . ? C28 C29 1.530(15) . ? C28 C31 1.54(3) . ? C28 H43 0.9900 . ? C28 H44 0.9900 . ? C28 H45 0.9900 . ? C28 H46 0.9900 . ? C29 H47 0.9900 . ? C29 H48 0.9900 . ? C30 C31 1.57(4) . ? 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 C23 Rh1 C22 38.6(4) . . ? C23 Rh1 P1 95.7(3) . . ? C22 Rh1 P1 91.0(3) . . ? C23 Rh1 N1 150.8(3) . . ? C22 Rh1 N1 169.9(3) . . ? P1 Rh1 N1 84.5(2) . . ? C23 Rh1 Cl1 95.6(3) . . ? C22 Rh1 Cl1 94.4(3) . . ? P1 Rh1 Cl1 167.51(9) . . ? N1 Rh1 Cl1 88.3(2) . . ? C1 P1 C8 101.6(4) . . ? C1 P1 C14 106.8(4) . . ? C8 P1 C14 102.8(4) . . ? C1 P1 Rh1 104.3(3) . . ? C8 P1 Rh1 126.8(3) . . ? C14 P1 Rh1 112.7(3) . . ? C2 N1 C21 108.6(8) . . ? C2 N1 C20 110.4(7) . . ? C21 N1 C20 109.4(8) . . ? C2 N1 Rh1 113.8(6) . . ? C21 N1 Rh1 110.1(6) . . ? C20 N1 Rh1 104.4(6) . . ? C2 C1 C6 119.7(9) . . ? C2 C1 P1 115.6(7) . . ? C6 C1 P1 124.7(7) . . ? C1 C2 C3 118.5(9) . . ? C1 C2 N1 121.1(9) . . ? C3 C2 N1 120.4(8) . . ? C4 C3 C2 120.7(9) . . ? C4 C3 H1 119.6 . . ? C2 C3 H1 119.6 . . ? C3 C4 C5 121.7(9) . . ? C3 C4 H2 119.1 . . ? C5 C4 H2 119.1 . . ? C6 C5 C4 117.4(9) . . ? C6 C5 C7 121.4(9) . . ? C4 C5 C7 121.2(9) . . ? C5 C6 C1 121.7(9) . . ? C5 C6 H3 119.1 . . ? C1 C6 H3 119.1 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C13 C8 C9 111.5(8) . . ? C13 C8 P1 113.5(6) . . ? C9 C8 P1 109.5(6) . . ? C13 C8 H7 107.4 . . ? C9 C8 H7 107.4 . . ? P1 C8 H7 107.4 . . ? C10 C9 C8 110.2(8) . . ? C10 C9 H8 109.6 . . ? C8 C9 H8 109.6 . . ? C10 C9 H9 109.6 . . ? C8 C9 H9 109.6 . . ? H8 C9 H9 108.1 . . ? C9 C10 C11 111.0(8) . . ? C9 C10 H10 109.4 . . ? C11 C10 H10 109.4 . . ? C9 C10 H11 109.4 . . ? C11 C10 H11 109.4 . . ? H10 C10 H11 108.0 . . ? C12 C11 C10 111.4(9) . . ? C12 C11 H12 109.3 . . ? C10 C11 H12 109.3 . . ? C12 C11 H13 109.3 . . ? C10 C11 H13 109.3 . . ? H12 C11 H13 108.0 . . ? C11 C12 C13 112.1(8) . . ? C11 C12 H14 109.2 . . ? C13 C12 H14 109.2 . . ? C11 C12 H15 109.2 . . ? C13 C12 H15 109.2 . . ? H14 C12 H15 107.9 . . ? C12 C13 C8 109.3(8) . . ? C12 C13 H16 109.8 . . ? C8 C13 H16 109.8 . . ? C12 C13 H17 109.8 . . ? C8 C13 H17 109.8 . . ? H16 C13 H17 108.3 . . ? C19 C14 C15 110.3(8) . . ? C19 C14 P1 110.4(6) . . ? C15 C14 P1 115.8(6) . . ? C19 C14 H18 106.6 . . ? C15 C14 H18 106.6 . . ? P1 C14 H18 106.6 . . ? C16 C15 C14 110.4(8) . . ? C16 C15 H19 109.6 . . ? C14 C15 H19 109.6 . . ? C16 C15 H20 109.6 . . ? C14 C15 H20 109.6 . . ? H19 C15 H20 108.1 . . ? C17 C16 C15 112.1(8) . . ? C17 C16 H21 109.2 . . ? C15 C16 H21 109.2 . . ? C17 C16 H22 109.2 . . ? C15 C16 H22 109.2 . . ? H21 C16 H22 107.9 . . ? C16 C17 C18 111.1(9) . . ? C16 C17 H23 109.4 . . ? C18 C17 H23 109.4 . . ? C16 C17 H24 109.4 . . ? C18 C17 H24 109.4 . . ? H23 C17 H24 108.0 . . ? C19 C18 C17 111.2(8) . . ? C19 C18 H25 109.4 . . ? C17 C18 H25 109.4 . . ? C19 C18 H26 109.4 . . ? C17 C18 H26 109.4 . . ? H25 C18 H26 108.0 . . ? C18 C19 C14 111.7(8) . . ? C18 C19 H27 109.3 . . ? C14 C19 H27 109.3 . . ? C18 C19 H28 109.3 . . ? C14 C19 H28 109.3 . . ? H27 C19 H28 107.9 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? C23 C22 C29 123.1(9) . . ? C23 C22 Rh1 69.3(6) . . ? C29 C22 Rh1 118.7(7) . . ? C23 C22 H35 113.0 . . ? C29 C22 H35 113.0 . . ? Rh1 C22 H35 113.0 . . ? C22 C23 C24 122.5(9) . . ? C22 C23 Rh1 72.1(6) . . ? C24 C23 Rh1 119.1(7) . . ? C22 C23 H36 112.4 . . ? C24 C23 H36 112.4 . . ? Rh1 C23 H36 112.4 . . ? C23 C24 C25 109.4(9) . . ? C23 C24 H37 109.8 . . ? C25 C24 H37 109.8 . . ? C23 C24 H38 109.8 . . ? C25 C24 H38 109.8 . . ? H37 C24 H38 108.2 . . ? C26 C25 C24 117.7(10) . . ? C26 C25 C30 34.7(13) . . ? C24 C25 C30 112.1(14) . . ? C26 C25 H39 107.9 . . ? C24 C25 H39 107.9 . . ? C30 C25 H39 135.6 . . ? C26 C25 H40 107.9 . . ? C24 C25 H40 107.9 . . ? C30 C25 H40 78.3 . . ? H39 C25 H40 107.2 . . ? C26 C25 H41 128.9 . . ? C24 C25 H41 109.2 . . ? C30 C25 H41 109.2 . . ? H39 C25 H41 73.9 . . ? H40 C25 H41 34.8 . . ? C26 C25 H42 75.4 . . ? C24 C25 H42 109.2 . . ? C30 C25 H42 109.2 . . ? H39 C25 H42 36.9 . . ? H40 C25 H42 135.3 . . ? H41 C25 H42 107.9 . . ? C25 C26 C27 111.7(14) . . ? C26 C27 C28 114.4(14) . . ? C29 C28 C31 117.6(13) . . ? C29 C28 C27 112.9(10) . . ? C31 C28 C27 42.1(12) . . ? C29 C28 H43 109.0 . . ? C31 C28 H43 68.2 . . ? C27 C28 H43 109.0 . . ? C29 C28 H44 109.0 . . ? C31 C28 H44 131.9 . . ? C27 C28 H44 109.0 . . ? H43 C28 H44 107.8 . . ? C29 C28 H45 107.9 . . ? C31 C28 H45 107.9 . . ? C27 C28 H45 137.8 . . ? H43 C28 H45 44.9 . . ? H44 C28 H45 65.9 . . ? C29 C28 H46 107.9 . . ? C31 C28 H46 107.9 . . ? C27 C28 H46 70.4 . . ? H43 C28 H46 139.5 . . ? H44 C28 H46 43.1 . . ? H45 C28 H46 107.2 . . ? C22 C29 C28 112.4(9) . . ? C22 C29 H47 109.1 . . ? C28 C29 H47 109.1 . . ? C22 C29 H48 109.1 . . ? C28 C29 H48 109.1 . . ? H47 C29 H48 107.9 . . ? C31 C30 C25 109(2) . . ? C28 C31 C30 108(2) . . ? 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 C23 Rh1 P1 C1 -145.6(4) . . . . ? C22 Rh1 P1 C1 176.0(4) . . . . ? N1 Rh1 P1 C1 5.1(4) . . . . ? Cl1 Rh1 P1 C1 60.0(6) . . . . ? C23 Rh1 P1 C8 -28.9(5) . . . . ? C22 Rh1 P1 C8 -67.3(5) . . . . ? N1 Rh1 P1 C8 121.8(4) . . . . ? Cl1 Rh1 P1 C8 176.7(5) . . . . ? C23 Rh1 P1 C14 98.9(4) . . . . ? C22 Rh1 P1 C14 60.5(4) . . . . ? N1 Rh1 P1 C14 -110.5(4) . . . . ? Cl1 Rh1 P1 C14 -55.5(6) . . . . ? C23 Rh1 N1 C2 83.4(9) . . . . ? C22 Rh1 N1 C2 -72(2) . . . . ? P1 Rh1 N1 C2 -8.3(6) . . . . ? Cl1 Rh1 N1 C2 -178.1(6) . . . . ? C23 Rh1 N1 C21 -154.4(7) . . . . ? C22 Rh1 N1 C21 50(2) . . . . ? P1 Rh1 N1 C21 113.8(6) . . . . ? Cl1 Rh1 N1 C21 -56.0(6) . . . . ? C23 Rh1 N1 C20 -37.0(10) . . . . ? C22 Rh1 N1 C20 167.3(19) . . . . ? P1 Rh1 N1 C20 -128.8(6) . . . . ? Cl1 Rh1 N1 C20 61.4(6) . . . . ? C8 P1 C1 C2 -134.9(7) . . . . ? C14 P1 C1 C2 117.7(7) . . . . ? Rh1 P1 C1 C2 -1.8(7) . . . . ? C8 P1 C1 C6 42.4(9) . . . . ? C14 P1 C1 C6 -65.0(8) . . . . ? Rh1 P1 C1 C6 175.4(7) . . . . ? C6 C1 C2 C3 -2.3(13) . . . . ? P1 C1 C2 C3 175.2(7) . . . . ? C6 C1 C2 N1 177.4(8) . . . . ? P1 C1 C2 N1 -5.2(11) . . . . ? C21 N1 C2 C1 -113.1(10) . . . . ? C20 N1 C2 C1 126.9(10) . . . . ? Rh1 N1 C2 C1 9.9(11) . . . . ? C21 N1 C2 C3 66.5(11) . . . . ? C20 N1 C2 C3 -53.5(12) . . . . ? Rh1 N1 C2 C3 -170.5(7) . . . . ? C1 C2 C3 C4 3.9(14) . . . . ? N1 C2 C3 C4 -175.8(9) . . . . ? C2 C3 C4 C5 -1.7(14) . . . . ? C3 C4 C5 C6 -2.0(14) . . . . ? C3 C4 C5 C7 177.9(9) . . . . ? C4 C5 C6 C1 3.6(13) . . . . ? C7 C5 C6 C1 -176.3(8) . . . . ? C2 C1 C6 C5 -1.5(13) . . . . ? P1 C1 C6 C5 -178.7(7) . . . . ? C1 P1 C8 C13 -167.8(7) . . . . ? C14 P1 C8 C13 -57.3(8) . . . . ? Rh1 P1 C8 C13 74.3(8) . . . . ? C1 P1 C8 C9 66.9(7) . . . . ? C14 P1 C8 C9 177.4(7) . . . . ? Rh1 P1 C8 C9 -51.0(8) . . . . ? C13 C8 C9 C10 56.8(11) . . . . ? P1 C8 C9 C10 -176.8(7) . . . . ? C8 C9 C10 C11 -55.3(12) . . . . ? C9 C10 C11 C12 55.8(12) . . . . ? C10 C11 C12 C13 -56.6(13) . . . . ? C11 C12 C13 C8 56.6(12) . . . . ? C9 C8 C13 C12 -56.5(11) . . . . ? P1 C8 C13 C12 179.3(7) . . . . ? C1 P1 C14 C19 -74.3(7) . . . . ? C8 P1 C14 C19 179.2(7) . . . . ? Rh1 P1 C14 C19 39.7(7) . . . . ? C1 P1 C14 C15 51.9(8) . . . . ? C8 P1 C14 C15 -54.6(8) . . . . ? Rh1 P1 C14 C15 165.9(6) . . . . ? C19 C14 C15 C16 -55.9(11) . . . . ? P1 C14 C15 C16 177.9(7) . . . . ? C14 C15 C16 C17 56.5(12) . . . . ? C15 C16 C17 C18 -55.8(12) . . . . ? C16 C17 C18 C19 54.7(12) . . . . ? C17 C18 C19 C14 -55.4(12) . . . . ? C15 C14 C19 C18 56.0(11) . . . . ? P1 C14 C19 C18 -174.8(7) . . . . ? P1 Rh1 C22 C23 97.8(6) . . . . ? N1 Rh1 C22 C23 161.2(19) . . . . ? Cl1 Rh1 C22 C23 -93.5(6) . . . . ? C23 Rh1 C22 C29 117.3(10) . . . . ? P1 Rh1 C22 C29 -144.9(7) . . . . ? N1 Rh1 C22 C29 -82(2) . . . . ? Cl1 Rh1 C22 C29 23.8(7) . . . . ? C29 C22 C23 C24 2.1(16) . . . . ? Rh1 C22 C23 C24 113.7(10) . . . . ? C29 C22 C23 Rh1 -111.5(10) . . . . ? P1 Rh1 C23 C22 -84.5(6) . . . . ? N1 Rh1 C23 C22 -173.4(7) . . . . ? Cl1 Rh1 C23 C22 90.1(6) . . . . ? C22 Rh1 C23 C24 -117.9(10) . . . . ? P1 Rh1 C23 C24 157.6(7) . . . . ? N1 Rh1 C23 C24 68.8(11) . . . . ? Cl1 Rh1 C23 C24 -27.8(7) . . . . ? C22 C23 C24 C25 90.3(12) . . . . ? Rh1 C23 C24 C25 176.8(7) . . . . ? C23 C24 C25 C26 -47.1(15) . . . . ? C23 C24 C25 C30 -85.0(16) . . . . ? C24 C25 C26 C27 -58.2(18) . . . . ? C30 C25 C26 C27 31(2) . . . . ? C25 C26 C27 C28 106.0(15) . . . . ? C26 C27 C28 C29 -74.4(16) . . . . ? C26 C27 C28 C31 32.0(18) . . . . ? C23 C22 C29 C28 -86.0(12) . . . . ? Rh1 C22 C29 C28 -168.8(7) . . . . ? C31 C28 C29 C22 30.8(17) . . . . ? C27 C28 C29 C22 77.3(12) . . . . ? C26 C25 C30 C31 -32.8(19) . . . . ? C24 C25 C30 C31 74(2) . . . . ? C29 C28 C31 C30 76(2) . . . . ? C27 C28 C31 C30 -18.6(17) . . . . ? C25 C30 C31 C28 -106(2) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.231 _refine_diff_density_min -2.159 _refine_diff_density_rms 0.241 #===END data_(PcyN-P,N)IrCl(PPh3)(4)?C7H8 _database_code_depnum_ccdc_archive 'CCDC 772160' #TrackingRef '- ToshiCIFs(ESI).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 'C39 H49 Cl Ir N P2, C7 H8' _chemical_formula_moiety ? _chemical_formula_sum 'C46 H57 Cl Ir N P2' _chemical_formula_weight 913.52 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' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.4500(6) _cell_length_b 10.3053(3) _cell_length_c 24.0221(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.5386(16) _cell_angle_gamma 90.00 _cell_volume 4064.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8906 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 27.41 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 3.462 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5443 _exptl_absorpt_correction_T_max 0.6247 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30205 _diffrn_reflns_av_R_equivalents 0.1053 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.41 _reflns_number_total 8906 _reflns_number_gt 7320 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0644P)^2^+29.1808P] 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 8906 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0835 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1611 _refine_ls_wR_factor_gt 0.1440 _refine_ls_goodness_of_fit_ref 1.193 _refine_ls_restrained_S_all 1.193 _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 0.170083(19) 0.20121(3) 0.494108(11) 0.01692(10) Uani 1 1 d . . . Cl1 Cl 0.13396(16) 0.3295(2) 0.57288(8) 0.0312(5) Uani 1 1 d . . . P1 P 0.20326(13) 0.12405(18) 0.41354(8) 0.0159(4) Uani 1 1 d . . . P2 P 0.25428(13) 0.09154(19) 0.55266(8) 0.0194(4) Uani 1 1 d . . . N1 N 0.0731(4) 0.3046(6) 0.4438(3) 0.0190(13) Uani 1 1 d . . . C1 C 0.1258(5) 0.1877(7) 0.3629(3) 0.0171(15) Uani 1 1 d . . . C2 C 0.0691(5) 0.2728(7) 0.3839(3) 0.0202(16) Uani 1 1 d . . . C3 C 0.0094(5) 0.3318(8) 0.3474(3) 0.0241(17) Uani 1 1 d . . . H1 H -0.0289 0.3907 0.3613 0.029 Uiso 1 1 calc R . . C4 C 0.0075(6) 0.3025(8) 0.2913(4) 0.0282(18) Uani 1 1 d . . . H2 H -0.0328 0.3422 0.2669 0.034 Uiso 1 1 calc R . . C5 C 0.0618(5) 0.2180(8) 0.2691(3) 0.0225(17) Uani 1 1 d . . . C6 C 0.1214(5) 0.1634(8) 0.3055(3) 0.0206(16) Uani 1 1 d . . . H3 H 0.1607 0.1076 0.2908 0.025 Uiso 1 1 calc R . . C7 C 0.0601(6) 0.1856(9) 0.2084(3) 0.031(2) Uani 1 1 d . . . H4 H 0.0198 0.2403 0.1879 0.046 Uiso 1 1 calc R . . H5 H 0.0454 0.0941 0.2030 0.046 Uiso 1 1 calc R . . H6 H 0.1141 0.2011 0.1945 0.046 Uiso 1 1 calc R . . C8 C 0.2946(5) 0.1896(8) 0.3825(3) 0.0210(16) Uani 1 1 d . . . H7 H 0.2947 0.1557 0.3435 0.025 Uiso 1 1 calc R . . C9 C 0.2918(6) 0.3395(8) 0.3790(4) 0.0278(19) Uani 1 1 d . . . H8 H 0.2412 0.3667 0.3577 0.033 Uiso 1 1 calc R . . H9 H 0.2908 0.3759 0.4171 0.033 Uiso 1 1 calc R . . C10 C 0.3642(6) 0.3927(9) 0.3513(4) 0.033(2) Uani 1 1 d . . . H10 H 0.3621 0.4887 0.3516 0.040 Uiso 1 1 calc R . . H11 H 0.3621 0.3637 0.3119 0.040 Uiso 1 1 calc R . . C11 C 0.4445(6) 0.3474(9) 0.3809(5) 0.036(2) Uani 1 1 d . . . H12 H 0.4908 0.3783 0.3600 0.043 Uiso 1 1 calc R . . H13 H 0.4500 0.3853 0.4188 0.043 Uiso 1 1 calc R . . C12 C 0.4473(5) 0.2004(9) 0.3850(4) 0.0313(19) Uani 1 1 d . . . H14 H 0.4483 0.1630 0.3471 0.038 Uiso 1 1 calc R . . H15 H 0.4980 0.1739 0.4064 0.038 Uiso 1 1 calc R . . C13 C 0.3748(5) 0.1474(9) 0.4132(4) 0.0271(18) Uani 1 1 d . . . H16 H 0.3763 0.1789 0.4522 0.032 Uiso 1 1 calc R . . H17 H 0.3777 0.0515 0.4141 0.032 Uiso 1 1 calc R . . C14 C 0.2067(5) -0.0550(7) 0.4007(3) 0.0182(15) Uani 1 1 d . . . H18 H 0.2373 -0.0939 0.4339 0.022 Uiso 1 1 calc R . . C15 C 0.2483(6) -0.1041(8) 0.3490(4) 0.0247(17) Uani 1 1 d . . . H19 H 0.2185 -0.0719 0.3147 0.030 Uiso 1 1 calc R . . H20 H 0.3048 -0.0707 0.3496 0.030 Uiso 1 1 calc R . . C16 C 0.2492(7) -0.2526(9) 0.3489(4) 0.035(2) Uani 1 1 d . . . H21 H 0.2753 -0.2839 0.3154 0.042 Uiso 1 1 calc R . . H22 H 0.2819 -0.2842 0.3822 0.042 Uiso 1 1 calc R . . C17 C 0.1638(7) -0.3072(8) 0.3492(4) 0.036(2) Uani 1 1 d . . . H23 H 0.1325 -0.2820 0.3144 0.043 Uiso 1 1 calc R . . H24 H 0.1664 -0.4031 0.3506 0.043 Uiso 1 1 calc R . . C18 C 0.1203(7) -0.2578(8) 0.3988(4) 0.032(2) Uani 1 1 d . . . H25 H 0.1477 -0.2920 0.4336 0.038 Uiso 1 1 calc R . . H26 H 0.0635 -0.2898 0.3964 0.038 Uiso 1 1 calc R . . C19 C 0.1203(6) -0.1077(8) 0.4006(4) 0.0268(18) Uani 1 1 d . . . H27 H 0.0878 -0.0736 0.3678 0.032 Uiso 1 1 calc R . . H28 H 0.0947 -0.0780 0.4346 0.032 Uiso 1 1 calc R . . C20 C 0.0849(6) 0.4472(7) 0.4502(3) 0.0240(18) Uani 1 1 d . . . H29 H 0.1371 0.4722 0.4358 0.036 Uiso 1 1 calc R . . H30 H 0.0849 0.4704 0.4898 0.036 Uiso 1 1 calc R . . H31 H 0.0405 0.4930 0.4294 0.036 Uiso 1 1 calc R . . C21 C -0.0055(6) 0.2672(9) 0.4676(4) 0.0289(19) Uani 1 1 d . . . H32 H -0.0506 0.3122 0.4472 0.043 Uiso 1 1 calc R . . H33 H -0.0040 0.2917 0.5070 0.043 Uiso 1 1 calc R . . H34 H -0.0133 0.1732 0.4640 0.043 Uiso 1 1 calc R . . C22 C 0.3495(5) 0.1709(8) 0.5758(3) 0.0234(17) Uani 1 1 d . . . C23 C 0.3562(6) 0.3066(9) 0.5655(4) 0.0304(19) Uani 1 1 d . . . H35 H 0.3132 0.3508 0.5452 0.036 Uiso 1 1 calc R . . C24 C 0.4247(6) 0.3741(10) 0.5848(4) 0.038(2) Uani 1 1 d . . . H36 H 0.4282 0.4648 0.5782 0.046 Uiso 1 1 calc R . . C25 C 0.4879(7) 0.3108(11) 0.6134(5) 0.043(3) Uani 1 1 d . . . H37 H 0.5352 0.3578 0.6261 0.052 Uiso 1 1 calc R . . C26 C 0.4831(6) 0.1796(12) 0.6239(4) 0.042(3) Uani 1 1 d . . . H38 H 0.5270 0.1363 0.6436 0.050 Uiso 1 1 calc R . . C27 C 0.4142(5) 0.1109(9) 0.6057(3) 0.0263(18) Uani 1 1 d . . . H39 H 0.4111 0.0209 0.6138 0.032 Uiso 1 1 calc R . . C28 C 0.2903(6) -0.0733(8) 0.5365(3) 0.0272(19) Uani 1 1 d . . . C29 C 0.3660(7) -0.0961(10) 0.5137(4) 0.037(2) Uani 1 1 d . . . H40 H 0.4021 -0.0257 0.5084 0.045 Uiso 1 1 calc R . . C30 C 0.3881(9) -0.2212(11) 0.4990(5) 0.050(3) Uani 1 1 d . . . H41 H 0.4389 -0.2342 0.4830 0.060 Uiso 1 1 calc R . . C31 C 0.3397(9) -0.3253(11) 0.5067(5) 0.055(4) Uani 1 1 d . . . H42 H 0.3565 -0.4099 0.4967 0.066 Uiso 1 1 calc R . . C32 C 0.2650(9) -0.3055(10) 0.5294(4) 0.051(3) Uani 1 1 d . . . H43 H 0.2305 -0.3776 0.5351 0.062 Uiso 1 1 calc R . . C33 C 0.2400(8) -0.1809(8) 0.5438(4) 0.038(2) Uani 1 1 d . . . H44 H 0.1883 -0.1691 0.5588 0.046 Uiso 1 1 calc R . . C34 C 0.2068(5) 0.0551(8) 0.6186(3) 0.0196(16) Uani 1 1 d . . . C35 C 0.1261(6) 0.0174(8) 0.6156(4) 0.0293(19) Uani 1 1 d . . . H45 H 0.0965 0.0175 0.5804 0.035 Uiso 1 1 calc R . . C36 C 0.0873(6) -0.0203(8) 0.6619(4) 0.032(2) Uani 1 1 d . . . H46 H 0.0320 -0.0474 0.6584 0.038 Uiso 1 1 calc R . . C37 C 0.1291(6) -0.0187(9) 0.7141(4) 0.033(2) Uani 1 1 d . . . H47 H 0.1028 -0.0465 0.7461 0.040 Uiso 1 1 calc R . . C38 C 0.2076(6) 0.0226(10) 0.7189(4) 0.035(2) Uani 1 1 d . . . H48 H 0.2358 0.0270 0.7546 0.041 Uiso 1 1 calc R . . C39 C 0.2470(6) 0.0586(9) 0.6713(3) 0.031(2) Uani 1 1 d . . . H49 H 0.3022 0.0860 0.6750 0.037 Uiso 1 1 calc R . . C40 C 0.6379(10) 0.3369(16) 0.2828(7) 0.068(4) Uiso 1 1 d . . . C41 C 0.5959(12) 0.4546(17) 0.2651(5) 0.082(5) Uani 1 1 d . . . H50 H 0.5433 0.4546 0.2465 0.098 Uiso 1 1 calc R . . C42 C 0.6404(13) 0.571(2) 0.2781(8) 0.090(5) Uiso 1 1 d . . . H51 H 0.6176 0.6530 0.2680 0.108 Uiso 1 1 calc R . . C43 C 0.7086(13) 0.564(2) 0.3024(7) 0.097(6) Uani 1 1 d . . . H52 H 0.7383 0.6416 0.3102 0.117 Uiso 1 1 calc R . . C44 C 0.7453(15) 0.439(2) 0.3197(9) 0.107(7) Uiso 1 1 d . . . H53 H 0.7975 0.4370 0.3389 0.128 Uiso 1 1 calc R . . C45 C 0.7088(13) 0.335(2) 0.3094(8) 0.092(5) Uiso 1 1 d . . . H54 H 0.7328 0.2547 0.3210 0.111 Uiso 1 1 calc R . . C46 C 0.5908(19) 0.226(3) 0.2698(12) 0.158(11) Uiso 1 1 d . . . H55 H 0.6026 0.1945 0.2326 0.237 Uiso 1 1 calc R . . H56 H 0.5329 0.2476 0.2702 0.237 Uiso 1 1 calc R . . H57 H 0.6042 0.1579 0.2974 0.237 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 0.02341(18) 0.01454(15) 0.01262(14) -0.00104(11) -0.00056(10) 0.00002(13) Cl1 0.0482(14) 0.0266(10) 0.0188(9) -0.0050(8) 0.0021(9) 0.0068(9) P1 0.0190(10) 0.0144(8) 0.0143(8) -0.0007(7) 0.0003(7) 0.0006(7) P2 0.0245(11) 0.0178(9) 0.0153(9) 0.0003(7) -0.0039(7) -0.0014(8) N1 0.028(4) 0.015(3) 0.014(3) 0.004(2) 0.000(2) 0.003(3) C1 0.022(4) 0.015(3) 0.015(3) -0.001(3) 0.003(3) -0.006(3) C2 0.022(4) 0.019(4) 0.019(4) -0.002(3) 0.003(3) -0.005(3) C3 0.025(5) 0.022(4) 0.025(4) -0.002(3) 0.000(3) 0.006(3) C4 0.033(5) 0.026(4) 0.025(4) 0.003(4) -0.007(3) -0.003(4) C5 0.028(5) 0.022(4) 0.017(4) -0.002(3) 0.000(3) -0.004(3) C6 0.019(4) 0.022(4) 0.020(4) -0.002(3) -0.002(3) -0.004(3) C7 0.039(5) 0.031(5) 0.020(4) 0.000(3) -0.005(4) -0.001(4) C8 0.020(4) 0.022(4) 0.021(4) 0.001(3) 0.000(3) 0.000(3) C9 0.029(5) 0.019(4) 0.035(5) 0.003(3) -0.001(4) -0.004(3) C10 0.027(5) 0.028(4) 0.046(5) 0.008(4) 0.005(4) -0.009(4) C11 0.025(5) 0.030(5) 0.053(6) 0.004(4) 0.005(4) -0.009(4) C12 0.019(4) 0.041(5) 0.034(5) 0.000(4) 0.000(3) -0.002(4) C13 0.020(5) 0.027(4) 0.034(5) 0.001(4) -0.004(3) -0.001(3) C14 0.023(4) 0.012(3) 0.019(4) -0.002(3) -0.004(3) 0.007(3) C15 0.028(5) 0.017(4) 0.030(4) -0.006(3) 0.010(3) 0.002(3) C16 0.055(7) 0.020(4) 0.031(5) -0.007(4) 0.006(4) 0.002(4) C17 0.065(7) 0.019(4) 0.024(4) -0.004(3) -0.003(4) -0.005(4) C18 0.045(6) 0.019(4) 0.032(5) -0.004(4) -0.002(4) -0.004(4) C19 0.032(5) 0.018(4) 0.030(4) -0.002(3) -0.002(4) -0.005(3) C20 0.037(5) 0.013(3) 0.023(4) -0.001(3) 0.003(3) -0.005(3) C21 0.024(5) 0.037(5) 0.026(4) -0.010(4) 0.007(3) -0.003(4) C22 0.019(4) 0.032(4) 0.019(4) -0.004(3) 0.002(3) 0.001(3) C23 0.033(5) 0.031(5) 0.026(4) -0.003(4) -0.007(3) -0.006(4) C24 0.032(6) 0.039(5) 0.041(5) -0.002(4) -0.008(4) -0.010(4) C25 0.027(6) 0.055(7) 0.047(6) -0.009(5) -0.001(4) -0.016(5) C26 0.025(5) 0.062(7) 0.037(5) -0.005(5) -0.008(4) -0.007(5) C27 0.022(5) 0.034(4) 0.024(4) 0.003(3) 0.007(3) 0.007(4) C28 0.040(5) 0.024(4) 0.017(4) -0.004(3) -0.010(3) 0.005(4) C29 0.057(7) 0.037(5) 0.018(4) 0.000(4) -0.006(4) 0.016(5) C30 0.070(9) 0.046(6) 0.033(5) -0.005(5) -0.010(5) 0.027(6) C31 0.098(11) 0.031(5) 0.034(5) -0.006(4) -0.018(6) 0.024(6) C32 0.093(10) 0.024(5) 0.034(5) -0.001(4) -0.017(6) 0.004(6) C33 0.067(7) 0.019(4) 0.026(4) 0.001(3) -0.013(4) 0.002(4) C34 0.017(4) 0.023(4) 0.019(4) 0.000(3) 0.002(3) -0.002(3) C35 0.034(5) 0.026(4) 0.028(4) 0.004(4) -0.003(4) -0.008(4) C36 0.037(6) 0.021(4) 0.037(5) 0.012(4) 0.002(4) -0.003(4) C37 0.037(6) 0.030(4) 0.033(5) 0.013(4) 0.006(4) -0.002(4) C38 0.032(5) 0.051(6) 0.021(4) 0.006(4) -0.003(4) 0.004(4) C39 0.031(5) 0.042(5) 0.019(4) 0.004(4) -0.001(3) -0.001(4) C41 0.113(14) 0.103(12) 0.033(6) -0.012(7) 0.029(7) -0.004(11) C43 0.098(15) 0.138(17) 0.060(9) -0.016(11) 0.039(9) 0.023(13) _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 P1 2.1923(19) . ? Ir1 N1 2.215(6) . ? Ir1 P2 2.221(2) . ? Ir1 Cl1 2.412(2) . ? P1 C1 1.828(8) . ? P1 C8 1.846(9) . ? P1 C14 1.872(7) . ? P2 C22 1.823(9) . ? P2 C34 1.847(8) . ? P2 C28 1.848(9) . ? N1 C2 1.473(10) . ? N1 C20 1.490(10) . ? N1 C21 1.495(11) . ? C1 C2 1.396(11) . ? C1 C6 1.400(10) . ? C2 C3 1.413(11) . ? C3 C4 1.382(12) . ? C3 H1 0.9500 . ? C4 C5 1.378(12) . ? C4 H2 0.9500 . ? C5 C6 1.392(11) . ? C5 C7 1.493(11) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C13 1.535(11) . ? C8 C9 1.547(11) . ? C8 H7 1.0000 . ? C9 C10 1.504(13) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.534(14) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.518(14) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.510(13) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C19 1.521(12) . ? C14 C15 1.541(11) . ? C14 H18 1.0000 . ? C15 C16 1.531(12) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.515(15) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.514(13) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.547(12) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C22 C27 1.392(12) . ? C22 C23 1.425(12) . ? C23 C24 1.380(13) . ? C23 H35 0.9500 . ? C24 C25 1.376(15) . ? C24 H36 0.9500 . ? C25 C26 1.379(16) . ? C25 H37 0.9500 . ? C26 C27 1.384(13) . ? C26 H38 0.9500 . ? C27 H39 0.9500 . ? C28 C33 1.401(14) . ? C28 C29 1.411(15) . ? C29 C30 1.391(14) . ? C29 H40 0.9500 . ? C30 C31 1.354(19) . ? C30 H41 0.9500 . ? C31 C32 1.39(2) . ? C31 H42 0.9500 . ? C32 C33 1.399(14) . ? C32 H43 0.9500 . ? C33 H44 0.9500 . ? C34 C35 1.380(12) . ? C34 C39 1.394(11) . ? C35 C36 1.372(13) . ? C35 H45 0.9500 . ? C36 C37 1.391(13) . ? C36 H46 0.9500 . ? C37 C38 1.359(14) . ? C37 H47 0.9500 . ? C38 C39 1.398(13) . ? C38 H48 0.9500 . ? C39 H49 0.9500 . ? C40 C45 1.30(2) . ? C40 C46 1.41(3) . ? C40 C41 1.45(2) . ? C41 C42 1.43(3) . ? C41 H50 0.9500 . ? C42 C43 1.24(2) . ? C42 H51 0.9500 . ? C43 C44 1.48(3) . ? C43 H52 0.9500 . ? C44 C45 1.24(3) . ? C44 H53 0.9500 . ? C45 H54 0.9500 . ? C46 H55 0.9800 . ? C46 H56 0.9800 . ? C46 H57 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 P1 Ir1 N1 84.41(17) . . ? P1 Ir1 P2 101.25(7) . . ? N1 Ir1 P2 172.14(18) . . ? P1 Ir1 Cl1 167.96(7) . . ? N1 Ir1 Cl1 87.75(17) . . ? P2 Ir1 Cl1 87.49(7) . . ? C1 P1 C8 98.7(3) . . ? C1 P1 C14 105.7(3) . . ? C8 P1 C14 105.1(4) . . ? C1 P1 Ir1 104.8(2) . . ? C8 P1 Ir1 118.5(3) . . ? C14 P1 Ir1 120.9(3) . . ? C22 P2 C34 103.4(4) . . ? C22 P2 C28 101.3(4) . . ? C34 P2 C28 98.7(4) . . ? C22 P2 Ir1 117.1(3) . . ? C34 P2 Ir1 111.5(3) . . ? C28 P2 Ir1 122.0(3) . . ? C2 N1 C20 108.6(6) . . ? C2 N1 C21 109.2(6) . . ? C20 N1 C21 108.9(7) . . ? C2 N1 Ir1 114.4(5) . . ? C20 N1 Ir1 109.5(5) . . ? C21 N1 Ir1 106.1(5) . . ? C2 C1 C6 118.2(7) . . ? C2 C1 P1 116.0(6) . . ? C6 C1 P1 125.6(6) . . ? C1 C2 C3 120.1(7) . . ? C1 C2 N1 120.1(7) . . ? C3 C2 N1 119.8(7) . . ? C4 C3 C2 118.9(8) . . ? C4 C3 H1 120.6 . . ? C2 C3 H1 120.6 . . ? C5 C4 C3 122.8(8) . . ? C5 C4 H2 118.6 . . ? C3 C4 H2 118.6 . . ? C4 C5 C6 117.4(7) . . ? C4 C5 C7 123.1(8) . . ? C6 C5 C7 119.5(8) . . ? C5 C6 C1 122.6(8) . . ? C5 C6 H3 118.7 . . ? C1 C6 H3 118.7 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C13 C8 C9 109.3(7) . . ? C13 C8 P1 113.5(6) . . ? C9 C8 P1 111.4(6) . . ? C13 C8 H7 107.5 . . ? C9 C8 H7 107.5 . . ? P1 C8 H7 107.5 . . ? C10 C9 C8 111.5(8) . . ? C10 C9 H8 109.3 . . ? C8 C9 H8 109.3 . . ? C10 C9 H9 109.3 . . ? C8 C9 H9 109.3 . . ? H8 C9 H9 108.0 . . ? C9 C10 C11 111.5(8) . . ? C9 C10 H10 109.3 . . ? C11 C10 H10 109.3 . . ? C9 C10 H11 109.3 . . ? C11 C10 H11 109.3 . . ? H10 C10 H11 108.0 . . ? C12 C11 C10 110.8(8) . . ? C12 C11 H12 109.5 . . ? C10 C11 H12 109.5 . . ? C12 C11 H13 109.5 . . ? C10 C11 H13 109.5 . . ? H12 C11 H13 108.1 . . ? C13 C12 C11 111.6(8) . . ? C13 C12 H14 109.3 . . ? C11 C12 H14 109.3 . . ? C13 C12 H15 109.3 . . ? C11 C12 H15 109.3 . . ? H14 C12 H15 108.0 . . ? C12 C13 C8 111.2(7) . . ? C12 C13 H16 109.4 . . ? C8 C13 H16 109.4 . . ? C12 C13 H17 109.4 . . ? C8 C13 H17 109.4 . . ? H16 C13 H17 108.0 . . ? C19 C14 C15 110.0(6) . . ? C19 C14 P1 108.4(5) . . ? C15 C14 P1 118.4(6) . . ? C19 C14 H18 106.5 . . ? C15 C14 H18 106.5 . . ? P1 C14 H18 106.5 . . ? C16 C15 C14 109.6(7) . . ? C16 C15 H19 109.8 . . ? C14 C15 H19 109.8 . . ? C16 C15 H20 109.8 . . ? C14 C15 H20 109.8 . . ? H19 C15 H20 108.2 . . ? C17 C16 C15 111.2(8) . . ? C17 C16 H21 109.4 . . ? C15 C16 H21 109.4 . . ? C17 C16 H22 109.4 . . ? C15 C16 H22 109.4 . . ? H21 C16 H22 108.0 . . ? C18 C17 C16 111.2(7) . . ? C18 C17 H23 109.4 . . ? C16 C17 H23 109.4 . . ? C18 C17 H24 109.4 . . ? C16 C17 H24 109.4 . . ? H23 C17 H24 108.0 . . ? C17 C18 C19 111.1(8) . . ? C17 C18 H25 109.4 . . ? C19 C18 H25 109.4 . . ? C17 C18 H26 109.4 . . ? C19 C18 H26 109.4 . . ? H25 C18 H26 108.0 . . ? C14 C19 C18 110.8(8) . . ? C14 C19 H27 109.5 . . ? C18 C19 H27 109.5 . . ? C14 C19 H28 109.5 . . ? C18 C19 H28 109.5 . . ? H27 C19 H28 108.1 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? C27 C22 C23 117.4(8) . . ? C27 C22 P2 125.0(7) . . ? C23 C22 P2 117.5(6) . . ? C24 C23 C22 120.4(9) . . ? C24 C23 H35 119.8 . . ? C22 C23 H35 119.8 . . ? C25 C24 C23 120.4(10) . . ? C25 C24 H36 119.8 . . ? C23 C24 H36 119.8 . . ? C24 C25 C26 120.4(9) . . ? C24 C25 H37 119.8 . . ? C26 C25 H37 119.8 . . ? C25 C26 C27 119.9(10) . . ? C25 C26 H38 120.0 . . ? C27 C26 H38 120.0 . . ? C26 C27 C22 121.5(9) . . ? C26 C27 H39 119.3 . . ? C22 C27 H39 119.3 . . ? C33 C28 C29 117.4(9) . . ? C33 C28 P2 120.1(8) . . ? C29 C28 P2 122.4(7) . . ? C30 C29 C28 120.2(11) . . ? C30 C29 H40 119.9 . . ? C28 C29 H40 119.9 . . ? C31 C30 C29 122.3(13) . . ? C31 C30 H41 118.8 . . ? C29 C30 H41 118.8 . . ? C30 C31 C32 118.6(10) . . ? C30 C31 H42 120.7 . . ? C32 C31 H42 120.7 . . ? C31 C32 C33 120.8(12) . . ? C31 C32 H43 119.6 . . ? C33 C32 H43 119.6 . . ? C32 C33 C28 120.7(12) . . ? C32 C33 H44 119.7 . . ? C28 C33 H44 119.7 . . ? C35 C34 C39 117.1(8) . . ? C35 C34 P2 118.0(6) . . ? C39 C34 P2 124.9(7) . . ? C36 C35 C34 122.2(9) . . ? C36 C35 H45 118.9 . . ? C34 C35 H45 118.9 . . ? C35 C36 C37 119.9(9) . . ? C35 C36 H46 120.1 . . ? C37 C36 H46 120.1 . . ? C38 C37 C36 119.7(9) . . ? C38 C37 H47 120.2 . . ? C36 C37 H47 120.2 . . ? C37 C38 C39 120.0(8) . . ? C37 C38 H48 120.0 . . ? C39 C38 H48 120.0 . . ? C34 C39 C38 121.2(9) . . ? C34 C39 H49 119.4 . . ? C38 C39 H49 119.4 . . ? C45 C40 C46 124(2) . . ? C45 C40 C41 123.9(18) . . ? C46 C40 C41 111.8(18) . . ? C42 C41 C40 114.3(17) . . ? C42 C41 H50 122.9 . . ? C40 C41 H50 122.9 . . ? C43 C42 C41 119(2) . . ? C43 C42 H51 120.3 . . ? C41 C42 H51 120.3 . . ? C42 C43 C44 122(2) . . ? C42 C43 H52 119.1 . . ? C44 C43 H52 119.1 . . ? C45 C44 C43 121(2) . . ? C45 C44 H53 119.5 . . ? C43 C44 H53 119.5 . . ? C44 C45 C40 120(2) . . ? C44 C45 H54 120.2 . . ? C40 C45 H54 120.2 . . ? C40 C46 H55 109.5 . . ? C40 C46 H56 109.5 . . ? H55 C46 H56 109.5 . . ? C40 C46 H57 109.5 . . ? H55 C46 H57 109.5 . . ? H56 C46 H57 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 N1 Ir1 P1 C1 -3.8(3) . . . . ? P2 Ir1 P1 C1 170.7(2) . . . . ? Cl1 Ir1 P1 C1 -53.4(5) . . . . ? N1 Ir1 P1 C8 105.0(3) . . . . ? P2 Ir1 P1 C8 -80.5(3) . . . . ? Cl1 Ir1 P1 C8 55.4(5) . . . . ? N1 Ir1 P1 C14 -122.8(3) . . . . ? P2 Ir1 P1 C14 51.7(3) . . . . ? Cl1 Ir1 P1 C14 -172.4(4) . . . . ? P1 Ir1 P2 C22 95.7(3) . . . . ? N1 Ir1 P2 C22 -128.7(13) . . . . ? Cl1 Ir1 P2 C22 -75.9(3) . . . . ? P1 Ir1 P2 C34 -145.6(3) . . . . ? N1 Ir1 P2 C34 -10.0(13) . . . . ? Cl1 Ir1 P2 C34 42.8(3) . . . . ? P1 Ir1 P2 C28 -29.7(4) . . . . ? N1 Ir1 P2 C28 105.9(13) . . . . ? Cl1 Ir1 P2 C28 158.7(4) . . . . ? P1 Ir1 N1 C2 3.9(5) . . . . ? P2 Ir1 N1 C2 -132.6(11) . . . . ? Cl1 Ir1 N1 C2 174.7(5) . . . . ? P1 Ir1 N1 C20 -118.3(5) . . . . ? P2 Ir1 N1 C20 105.3(13) . . . . ? Cl1 Ir1 N1 C20 52.6(5) . . . . ? P1 Ir1 N1 C21 124.3(5) . . . . ? P2 Ir1 N1 C21 -12.1(16) . . . . ? Cl1 Ir1 N1 C21 -64.8(5) . . . . ? C8 P1 C1 C2 -118.7(6) . . . . ? C14 P1 C1 C2 132.8(6) . . . . ? Ir1 P1 C1 C2 3.9(6) . . . . ? C8 P1 C1 C6 57.8(7) . . . . ? C14 P1 C1 C6 -50.7(7) . . . . ? Ir1 P1 C1 C6 -179.5(6) . . . . ? C6 C1 C2 C3 0.1(11) . . . . ? P1 C1 C2 C3 176.9(6) . . . . ? C6 C1 C2 N1 -177.9(7) . . . . ? P1 C1 C2 N1 -1.1(9) . . . . ? C20 N1 C2 C1 120.2(8) . . . . ? C21 N1 C2 C1 -121.2(8) . . . . ? Ir1 N1 C2 C1 -2.4(9) . . . . ? C20 N1 C2 C3 -57.9(10) . . . . ? C21 N1 C2 C3 60.8(9) . . . . ? Ir1 N1 C2 C3 179.5(6) . . . . ? C1 C2 C3 C4 0.8(12) . . . . ? N1 C2 C3 C4 178.9(8) . . . . ? C2 C3 C4 C5 -0.2(13) . . . . ? C3 C4 C5 C6 -1.4(13) . . . . ? C3 C4 C5 C7 179.9(8) . . . . ? C4 C5 C6 C1 2.4(12) . . . . ? C7 C5 C6 C1 -178.9(8) . . . . ? C2 C1 C6 C5 -1.8(12) . . . . ? P1 C1 C6 C5 -178.3(6) . . . . ? C1 P1 C8 C13 -176.5(6) . . . . ? C14 P1 C8 C13 -67.6(6) . . . . ? Ir1 P1 C8 C13 71.3(6) . . . . ? C1 P1 C8 C9 59.6(6) . . . . ? C14 P1 C8 C9 168.6(6) . . . . ? Ir1 P1 C8 C9 -52.6(6) . . . . ? C13 C8 C9 C10 56.5(10) . . . . ? P1 C8 C9 C10 -177.3(6) . . . . ? C8 C9 C10 C11 -56.0(11) . . . . ? C9 C10 C11 C12 54.8(11) . . . . ? C10 C11 C12 C13 -55.3(11) . . . . ? C11 C12 C13 C8 57.3(10) . . . . ? C9 C8 C13 C12 -56.7(10) . . . . ? P1 C8 C13 C12 178.3(6) . . . . ? C1 P1 C14 C19 -51.3(6) . . . . ? C8 P1 C14 C19 -155.1(5) . . . . ? Ir1 P1 C14 C19 67.3(6) . . . . ? C1 P1 C14 C15 74.9(7) . . . . ? C8 P1 C14 C15 -28.9(7) . . . . ? Ir1 P1 C14 C15 -166.5(5) . . . . ? C19 C14 C15 C16 -58.5(9) . . . . ? P1 C14 C15 C16 176.2(6) . . . . ? C14 C15 C16 C17 58.2(10) . . . . ? C15 C16 C17 C18 -56.9(10) . . . . ? C16 C17 C18 C19 55.0(11) . . . . ? C15 C14 C19 C18 57.3(9) . . . . ? P1 C14 C19 C18 -171.8(6) . . . . ? C17 C18 C19 C14 -55.7(10) . . . . ? C34 P2 C22 C27 66.8(8) . . . . ? C28 P2 C22 C27 -35.1(8) . . . . ? Ir1 P2 C22 C27 -170.3(6) . . . . ? C34 P2 C22 C23 -109.2(7) . . . . ? C28 P2 C22 C23 148.9(7) . . . . ? Ir1 P2 C22 C23 13.8(8) . . . . ? C27 C22 C23 C24 -0.1(13) . . . . ? P2 C22 C23 C24 176.2(8) . . . . ? C22 C23 C24 C25 1.1(16) . . . . ? C23 C24 C25 C26 -0.9(17) . . . . ? C24 C25 C26 C27 -0.2(17) . . . . ? C25 C26 C27 C22 1.2(15) . . . . ? C23 C22 C27 C26 -1.1(13) . . . . ? P2 C22 C27 C26 -177.0(7) . . . . ? C22 P2 C28 C33 148.2(7) . . . . ? C34 P2 C28 C33 42.6(7) . . . . ? Ir1 P2 C28 C33 -79.5(7) . . . . ? C22 P2 C28 C29 -35.4(8) . . . . ? C34 P2 C28 C29 -141.0(7) . . . . ? Ir1 P2 C28 C29 96.9(7) . . . . ? C33 C28 C29 C30 0.5(12) . . . . ? P2 C28 C29 C30 -175.9(7) . . . . ? C28 C29 C30 C31 -1.3(15) . . . . ? C29 C30 C31 C32 0.9(16) . . . . ? C30 C31 C32 C33 0.3(16) . . . . ? C31 C32 C33 C28 -1.0(15) . . . . ? C29 C28 C33 C32 0.6(13) . . . . ? P2 C28 C33 C32 177.1(7) . . . . ? C22 P2 C34 C35 167.5(7) . . . . ? C28 P2 C34 C35 -88.6(7) . . . . ? Ir1 P2 C34 C35 40.9(7) . . . . ? C22 P2 C34 C39 -14.7(9) . . . . ? C28 P2 C34 C39 89.2(8) . . . . ? Ir1 P2 C34 C39 -141.3(7) . . . . ? C39 C34 C35 C36 -2.6(13) . . . . ? P2 C34 C35 C36 175.4(7) . . . . ? C34 C35 C36 C37 1.3(14) . . . . ? C35 C36 C37 C38 1.3(14) . . . . ? C36 C37 C38 C39 -2.4(15) . . . . ? C35 C34 C39 C38 1.4(14) . . . . ? P2 C34 C39 C38 -176.4(7) . . . . ? C37 C38 C39 C34 1.0(15) . . . . ? C45 C40 C41 C42 2(2) . . . . ? C46 C40 C41 C42 179.1(19) . . . . ? C40 C41 C42 C43 0(2) . . . . ? C41 C42 C43 C44 -1(3) . . . . ? C42 C43 C44 C45 1(3) . . . . ? C43 C44 C45 C40 1(3) . . . . ? C46 C40 C45 C44 -179(2) . . . . ? C41 C40 C45 C44 -2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.41 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 1.823 _refine_diff_density_min -2.021 _refine_diff_density_rms 0.280 # Attachment '- ToshiCIFs.cif' data_(PcyN-P,N)IrCl(coe)-(1) _database_code_depnum_ccdc_archive 'CCDC 772161' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H48 Cl Ir N P' _chemical_formula_sum 'C29 H48 Cl Ir N P' _chemical_formula_weight 669.30 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' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6406(7) _cell_length_b 12.0199(10) _cell_length_c 13.9025(7) _cell_angle_alpha 104.9995(17) _cell_angle_beta 108.743(4) _cell_angle_gamma 98.988(2) _cell_volume 1422.23(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6450 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 4.862 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5931 _exptl_absorpt_correction_T_max 0.6971 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13631 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0710 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 27.44 _reflns_number_total 6450 _reflns_number_gt 5572 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0597P)^2^+7.7863P] 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 6450 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1271 _refine_ls_goodness_of_fit_ref 1.234 _refine_ls_restrained_S_all 1.234 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.14922(4) 0.25795(3) 0.17698(3) 0.01720(11) Uani 1 1 d . . . Cl1 Cl 0.3890(3) 0.2505(3) 0.1569(2) 0.0343(6) Uani 1 1 d . . . P1 P -0.0618(2) 0.2964(2) 0.18605(16) 0.0158(4) Uani 1 1 d . . . N1 N 0.0656(8) 0.2755(7) 0.0171(6) 0.0197(15) Uani 1 1 d . . . C1 C -0.1663(9) 0.3028(8) 0.0529(6) 0.0171(16) Uani 1 1 d . . . C2 C -0.0914(9) 0.2867(7) -0.0181(6) 0.0166(16) Uani 1 1 d . . . C3 C -0.1676(11) 0.2828(8) -0.1247(7) 0.0236(19) Uani 1 1 d . . . H1 H -0.1197 0.2688 -0.1750 0.028 Uiso 1 1 calc R . . C4 C -0.3105(10) 0.2991(8) -0.1554(7) 0.0231(18) Uani 1 1 d . . . H2 H -0.3596 0.2973 -0.2272 0.028 Uiso 1 1 calc R . . C5 C -0.3860(10) 0.3183(8) -0.0858(7) 0.0217(18) Uani 1 1 d . . . C6 C -0.3114(10) 0.3182(8) 0.0183(7) 0.0215(18) Uani 1 1 d . . . H3 H -0.3620 0.3290 0.0672 0.026 Uiso 1 1 calc R . . C7 C -0.5409(11) 0.3391(9) -0.1207(8) 0.029(2) Uani 1 1 d . . . H4 H -0.5330 0.4243 -0.0915 0.043 Uiso 1 1 calc R . . H5 H -0.6047 0.2937 -0.0940 0.043 Uiso 1 1 calc R . . H6 H -0.5865 0.3128 -0.1995 0.043 Uiso 1 1 calc R . . C8 C -0.2094(10) 0.1973(8) 0.2065(7) 0.0218(18) Uani 1 1 d . . . H7 H -0.3022 0.2274 0.1878 0.026 Uiso 1 1 calc R . . C9 C -0.2521(10) 0.0695(8) 0.1287(7) 0.0241(19) Uani 1 1 d . . . H8 H -0.2843 0.0705 0.0538 0.029 Uiso 1 1 calc R . . H9 H -0.1621 0.0370 0.1434 0.029 Uiso 1 1 calc R . . C10 C -0.3799(11) -0.0109(9) 0.1405(8) 0.030(2) Uani 1 1 d . . . H10 H -0.4730 0.0170 0.1191 0.036 Uiso 1 1 calc R . . H11 H -0.4018 -0.0935 0.0920 0.036 Uiso 1 1 calc R . . C11 C -0.3365(12) -0.0098(9) 0.2559(8) 0.033(2) Uani 1 1 d . . . H12 H -0.2490 -0.0446 0.2750 0.040 Uiso 1 1 calc R . . H13 H -0.4225 -0.0598 0.2626 0.040 Uiso 1 1 calc R . . C12 C -0.2952(12) 0.1166(9) 0.3335(7) 0.030(2) Uani 1 1 d . . . H14 H -0.3857 0.1485 0.3185 0.036 Uiso 1 1 calc R . . H15 H -0.2637 0.1150 0.4081 0.036 Uiso 1 1 calc R . . C13 C -0.1686(10) 0.1976(8) 0.3233(7) 0.0223(18) Uani 1 1 d . . . H16 H -0.0749 0.1708 0.3459 0.027 Uiso 1 1 calc R . . H17 H -0.1488 0.2799 0.3716 0.027 Uiso 1 1 calc R . . C14 C -0.0352(9) 0.4441(7) 0.2853(7) 0.0167(16) Uani 1 1 d . . . H18 H 0.0072 0.4363 0.3583 0.020 Uiso 1 1 calc R . . C15 C -0.1761(10) 0.4878(9) 0.2790(7) 0.026(2) Uani 1 1 d . . . H19 H -0.2516 0.4274 0.2858 0.032 Uiso 1 1 calc R . . H20 H -0.2215 0.4975 0.2079 0.032 Uiso 1 1 calc R . . C16 C -0.1404(12) 0.6058(10) 0.3669(8) 0.035(2) Uani 1 1 d . . . H21 H -0.1030 0.5947 0.4381 0.042 Uiso 1 1 calc R . . H22 H -0.2342 0.6327 0.3589 0.042 Uiso 1 1 calc R . . C17 C -0.0204(12) 0.7014(9) 0.3618(8) 0.035(2) Uani 1 1 d . . . H23 H -0.0617 0.7187 0.2938 0.042 Uiso 1 1 calc R . . H24 H 0.0051 0.7759 0.4224 0.042 Uiso 1 1 calc R . . C18 C 0.1221(11) 0.6599(9) 0.3677(7) 0.029(2) Uani 1 1 d . . . H25 H 0.1699 0.6518 0.4392 0.035 Uiso 1 1 calc R . . H26 H 0.1954 0.7206 0.3592 0.035 Uiso 1 1 calc R . . C19 C 0.0862(10) 0.5393(8) 0.2794(7) 0.0227(18) Uani 1 1 d . . . H27 H 0.1800 0.5122 0.2883 0.027 Uiso 1 1 calc R . . H28 H 0.0493 0.5494 0.2079 0.027 Uiso 1 1 calc R . . C20 C 0.0787(12) 0.1663(9) -0.0580(8) 0.030(2) Uani 1 1 d . . . H29 H 0.0118 0.0952 -0.0591 0.045 Uiso 1 1 calc R . . H30 H 0.1839 0.1607 -0.0332 0.045 Uiso 1 1 calc R . . H31 H 0.0489 0.1718 -0.1306 0.045 Uiso 1 1 calc R . . C21 C 0.1653(10) 0.3842(8) 0.0168(7) 0.0236(18) Uani 1 1 d . . . H32 H 0.1366 0.3866 -0.0568 0.035 Uiso 1 1 calc R . . H33 H 0.2715 0.3814 0.0441 0.035 Uiso 1 1 calc R . . H34 H 0.1531 0.4558 0.0629 0.035 Uiso 1 1 calc R . . C22 C 0.2383(10) 0.2769(9) 0.3439(7) 0.0241(19) Uani 1 1 d . . . H35 H 0.1750 0.3100 0.3827 0.029 Uiso 1 1 calc R . . C23 C 0.1738(11) 0.1554(9) 0.2811(7) 0.0250(19) Uani 1 1 d . . . H36 H 0.0754 0.1228 0.2862 0.030 Uiso 1 1 calc R . . C24 C 0.2656(11) 0.0639(9) 0.2728(8) 0.027(2) Uani 1 1 d . A . H37 H 0.3693 0.1032 0.2817 0.032 Uiso 1 1 calc R . . H38 H 0.2173 0.0017 0.2009 0.032 Uiso 1 1 calc R . . C25 C 0.2737(13) 0.0070(10) 0.3596(9) 0.039(3) Uani 1 1 d . . . H39 H 0.1747 -0.0511 0.3365 0.047 Uiso 0.73(3) 1 calc PR A 1 H40 H 0.3510 -0.0388 0.3627 0.047 Uiso 0.73(3) 1 calc PR A 1 H41 H 0.2970 -0.0709 0.3384 0.047 Uiso 0.27(3) 1 calc PR A 2 H42 H 0.1737 -0.0077 0.3661 0.047 Uiso 0.27(3) 1 calc PR A 2 C26 C 0.310(2) 0.0878(15) 0.4714(13) 0.041(4) Uiso 0.73(3) 1 d P A 1 C27 C 0.4631(17) 0.1792(14) 0.5161(12) 0.036(4) Uiso 0.73(3) 1 d P A 1 C28 C 0.403(5) 0.092(4) 0.476(3) 0.031(10) Uiso 0.27(3) 1 d P A 2 C29 C 0.366(4) 0.203(3) 0.534(2) 0.020(9) Uiso 0.27(3) 1 d P A 2 C30 C 0.4542(13) 0.3122(10) 0.5189(8) 0.039(3) Uani 1 1 d . . . H43 H 0.3809 0.3342 0.5516 0.047 Uiso 0.73(3) 1 calc PR A 1 H44 H 0.5549 0.3680 0.5657 0.047 Uiso 0.73(3) 1 calc PR A 1 H45 H 0.4498 0.3847 0.5703 0.047 Uiso 0.27(3) 1 calc PR A 2 H46 H 0.5619 0.3102 0.5410 0.047 Uiso 0.27(3) 1 calc PR A 2 C31 C 0.4073(10) 0.3281(9) 0.4094(7) 0.028(2) Uani 1 1 d . A . H47 H 0.4641 0.2885 0.3691 0.033 Uiso 1 1 calc R . . H48 H 0.4349 0.4142 0.4190 0.033 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 0.01323(16) 0.02271(18) 0.01876(17) 0.00903(12) 0.00702(11) 0.00738(12) Cl1 0.0210(11) 0.0574(17) 0.0404(13) 0.0277(12) 0.0180(10) 0.0206(11) P1 0.0131(10) 0.0207(11) 0.0169(10) 0.0087(8) 0.0072(8) 0.0057(8) N1 0.019(4) 0.022(4) 0.020(4) 0.007(3) 0.009(3) 0.009(3) C1 0.016(4) 0.024(4) 0.013(4) 0.007(3) 0.005(3) 0.009(3) C2 0.013(4) 0.014(4) 0.020(4) 0.006(3) 0.004(3) 0.000(3) C3 0.030(5) 0.021(5) 0.014(4) 0.000(3) 0.006(3) 0.005(4) C4 0.028(5) 0.016(4) 0.022(4) 0.000(3) 0.012(4) 0.003(4) C5 0.021(4) 0.016(4) 0.027(5) 0.008(3) 0.007(3) 0.005(3) C6 0.022(4) 0.024(5) 0.022(4) 0.008(4) 0.013(3) 0.008(4) C7 0.021(5) 0.035(5) 0.028(5) 0.013(4) 0.002(4) 0.011(4) C8 0.023(4) 0.027(5) 0.020(4) 0.009(4) 0.012(3) 0.007(4) C9 0.025(5) 0.023(5) 0.018(4) 0.003(3) 0.007(3) 0.000(4) C10 0.025(5) 0.025(5) 0.035(5) 0.011(4) 0.009(4) 0.000(4) C11 0.038(6) 0.027(5) 0.031(5) 0.011(4) 0.014(4) -0.007(4) C12 0.034(5) 0.037(6) 0.020(5) 0.010(4) 0.013(4) 0.005(4) C13 0.018(4) 0.022(4) 0.022(4) 0.003(3) 0.007(3) -0.002(3) C14 0.017(4) 0.014(4) 0.022(4) 0.007(3) 0.008(3) 0.007(3) C15 0.023(5) 0.027(5) 0.022(4) -0.001(4) 0.005(3) 0.009(4) C16 0.034(6) 0.038(6) 0.036(6) 0.006(5) 0.016(4) 0.022(5) C17 0.041(6) 0.025(5) 0.031(5) 0.001(4) 0.011(4) 0.009(5) C18 0.031(5) 0.031(5) 0.023(5) 0.006(4) 0.009(4) 0.010(4) C19 0.023(4) 0.021(4) 0.022(4) 0.004(4) 0.009(3) 0.002(4) C20 0.037(5) 0.030(5) 0.024(5) -0.001(4) 0.016(4) 0.021(4) C21 0.021(4) 0.023(5) 0.027(5) 0.008(4) 0.012(4) 0.001(4) C22 0.020(4) 0.035(5) 0.023(4) 0.012(4) 0.009(3) 0.015(4) C23 0.025(5) 0.037(5) 0.020(4) 0.016(4) 0.008(3) 0.016(4) C24 0.026(5) 0.025(5) 0.028(5) 0.008(4) 0.007(4) 0.009(4) C25 0.041(6) 0.032(6) 0.042(6) 0.020(5) 0.006(5) 0.014(5) C30 0.033(6) 0.037(6) 0.029(5) 0.001(5) -0.001(4) 0.000(5) C31 0.022(5) 0.024(5) 0.025(5) -0.002(4) 0.003(4) 0.001(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 C23 2.114(9) . ? Ir1 C22 2.136(9) . ? Ir1 N1 2.186(7) . ? Ir1 P1 2.190(2) . ? Ir1 Cl1 2.428(2) . ? P1 C1 1.830(8) . ? P1 C8 1.853(9) . ? P1 C14 1.866(8) . ? N1 C2 1.473(10) . ? N1 C21 1.498(11) . ? N1 C20 1.502(11) . ? C1 C6 1.385(12) . ? C1 C2 1.391(11) . ? C2 C3 1.412(11) . ? C3 C4 1.367(13) . ? C3 H1 0.9500 . ? C4 C5 1.382(12) . ? C4 H2 0.9500 . ? C5 C6 1.395(12) . ? C5 C7 1.498(12) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C9 1.535(12) . ? C8 C13 1.541(12) . ? C8 H7 1.0000 . ? C9 C10 1.522(13) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.519(13) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.522(14) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.506(13) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C15 1.517(12) . ? C14 C19 1.542(12) . ? C14 H18 1.0000 . ? C15 C16 1.518(13) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.531(16) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.519(14) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.541(12) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C22 C23 1.410(14) . ? C22 C31 1.518(12) . ? C22 H35 1.0000 . ? C23 C24 1.520(13) . ? C23 H36 1.0000 . ? C24 C25 1.521(14) . ? C24 H37 0.9900 . ? C24 H38 0.9900 . ? C25 C26 1.498(19) . ? C25 C28 1.63(4) . ? C25 H39 0.9900 . ? C25 H40 0.9900 . ? C25 H41 0.9900 . ? C25 H42 0.9900 . ? C26 C27 1.52(2) . ? C27 C30 1.606(19) . ? C28 C29 1.53(5) . ? C29 C30 1.55(3) . ? C30 C31 1.514(14) . ? C30 H43 0.9900 . ? C30 H44 0.9900 . ? C30 H45 0.9900 . ? C30 H46 0.9900 . ? C31 H47 0.9900 . ? C31 H48 0.9900 . ? 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 C23 Ir1 C22 38.8(4) . . ? C23 Ir1 N1 151.9(3) . . ? C22 Ir1 N1 169.1(3) . . ? C23 Ir1 P1 95.9(3) . . ? C22 Ir1 P1 91.8(2) . . ? N1 Ir1 P1 84.95(19) . . ? C23 Ir1 Cl1 94.5(3) . . ? C22 Ir1 Cl1 93.6(2) . . ? N1 Ir1 Cl1 87.9(2) . . ? P1 Ir1 Cl1 168.66(8) . . ? C1 P1 C8 101.7(4) . . ? C1 P1 C14 106.7(4) . . ? C8 P1 C14 102.4(4) . . ? C1 P1 Ir1 104.4(3) . . ? C8 P1 Ir1 125.4(3) . . ? C14 P1 Ir1 114.4(3) . . ? C2 N1 C21 107.8(7) . . ? C2 N1 C20 110.8(7) . . ? C21 N1 C20 109.3(7) . . ? C2 N1 Ir1 113.8(5) . . ? C21 N1 Ir1 109.3(5) . . ? C20 N1 Ir1 105.8(6) . . ? C6 C1 C2 119.4(7) . . ? C6 C1 P1 125.4(6) . . ? C2 C1 P1 115.1(6) . . ? C1 C2 C3 118.8(8) . . ? C1 C2 N1 121.0(7) . . ? C3 C2 N1 120.2(7) . . ? C4 C3 C2 119.9(8) . . ? C4 C3 H1 120.0 . . ? C2 C3 H1 120.0 . . ? C3 C4 C5 122.3(8) . . ? C3 C4 H2 118.8 . . ? C5 C4 H2 118.8 . . ? C4 C5 C6 117.2(8) . . ? C4 C5 C7 121.3(8) . . ? C6 C5 C7 121.5(8) . . ? C1 C6 C5 122.2(8) . . ? C1 C6 H3 118.9 . . ? C5 C6 H3 118.9 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C9 C8 C13 110.6(7) . . ? C9 C8 P1 110.9(6) . . ? C13 C8 P1 114.4(6) . . ? C9 C8 H7 106.9 . . ? C13 C8 H7 106.9 . . ? P1 C8 H7 106.9 . . ? C10 C9 C8 111.2(7) . . ? C10 C9 H8 109.4 . . ? C8 C9 H8 109.4 . . ? C10 C9 H9 109.4 . . ? C8 C9 H9 109.4 . . ? H8 C9 H9 108.0 . . ? C11 C10 C9 110.6(8) . . ? C11 C10 H10 109.5 . . ? C9 C10 H10 109.5 . . ? C11 C10 H11 109.5 . . ? C9 C10 H11 109.5 . . ? H10 C10 H11 108.1 . . ? C10 C11 C12 111.1(8) . . ? C10 C11 H12 109.4 . . ? C12 C11 H12 109.4 . . ? C10 C11 H13 109.4 . . ? C12 C11 H13 109.4 . . ? H12 C11 H13 108.0 . . ? C13 C12 C11 111.5(8) . . ? C13 C12 H14 109.3 . . ? C11 C12 H14 109.3 . . ? C13 C12 H15 109.3 . . ? C11 C12 H15 109.3 . . ? H14 C12 H15 108.0 . . ? C12 C13 C8 111.1(7) . . ? C12 C13 H16 109.4 . . ? C8 C13 H16 109.4 . . ? C12 C13 H17 109.4 . . ? C8 C13 H17 109.4 . . ? H16 C13 H17 108.0 . . ? C15 C14 C19 110.0(7) . . ? C15 C14 P1 116.9(6) . . ? C19 C14 P1 109.6(5) . . ? C15 C14 H18 106.6 . . ? C19 C14 H18 106.6 . . ? P1 C14 H18 106.6 . . ? C14 C15 C16 111.7(8) . . ? C14 C15 H19 109.3 . . ? C16 C15 H19 109.3 . . ? C14 C15 H20 109.3 . . ? C16 C15 H20 109.3 . . ? H19 C15 H20 107.9 . . ? C15 C16 C17 111.2(8) . . ? C15 C16 H21 109.4 . . ? C17 C16 H21 109.4 . . ? C15 C16 H22 109.4 . . ? C17 C16 H22 109.4 . . ? H21 C16 H22 108.0 . . ? C18 C17 C16 110.7(9) . . ? C18 C17 H23 109.5 . . ? C16 C17 H23 109.5 . . ? C18 C17 H24 109.5 . . ? C16 C17 H24 109.5 . . ? H23 C17 H24 108.1 . . ? C17 C18 C19 111.4(8) . . ? C17 C18 H25 109.3 . . ? C19 C18 H25 109.3 . . ? C17 C18 H26 109.3 . . ? C19 C18 H26 109.3 . . ? H25 C18 H26 108.0 . . ? C18 C19 C14 111.0(7) . . ? C18 C19 H27 109.4 . . ? C14 C19 H27 109.4 . . ? C18 C19 H28 109.4 . . ? C14 C19 H28 109.4 . . ? H27 C19 H28 108.0 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? C23 C22 C31 122.6(8) . . ? C23 C22 Ir1 69.8(5) . . ? C31 C22 Ir1 120.0(6) . . ? C23 C22 H35 112.6 . . ? C31 C22 H35 112.6 . . ? Ir1 C22 H35 112.6 . . ? C22 C23 C24 123.6(8) . . ? C22 C23 Ir1 71.5(5) . . ? C24 C23 Ir1 119.5(6) . . ? C22 C23 H36 112.2 . . ? C24 C23 H36 112.2 . . ? Ir1 C23 H36 112.2 . . ? C23 C24 C25 109.5(8) . . ? C23 C24 H37 109.8 . . ? C25 C24 H37 109.8 . . ? C23 C24 H38 109.8 . . ? C25 C24 H38 109.8 . . ? H37 C24 H38 108.2 . . ? C26 C25 C24 117.8(10) . . ? C26 C25 C28 31.9(14) . . ? C24 C25 C28 111.6(16) . . ? C26 C25 H39 107.9 . . ? C24 C25 H39 107.9 . . ? C28 C25 H39 134.5 . . ? C26 C25 H40 107.9 . . ? C24 C25 H40 107.9 . . ? C28 C25 H40 81.4 . . ? H39 C25 H40 107.2 . . ? C26 C25 H41 127.4 . . ? C24 C25 H41 109.3 . . ? C28 C25 H41 109.3 . . ? H39 C25 H41 77.0 . . ? H40 C25 H41 31.6 . . ? C26 C25 H42 78.1 . . ? C24 C25 H42 109.3 . . ? C28 C25 H42 109.3 . . ? H39 C25 H42 34.0 . . ? H40 C25 H42 133.4 . . ? H41 C25 H42 108.0 . . ? C25 C26 C27 112.2(13) . . ? C26 C27 C30 114.9(12) . . ? C29 C28 C25 116(3) . . ? C28 C29 C30 108(2) . . ? C31 C30 C29 119.7(14) . . ? C31 C30 C27 114.1(9) . . ? C29 C30 C27 40.9(13) . . ? C31 C30 H43 108.7 . . ? C29 C30 H43 68.9 . . ? C27 C30 H43 108.7 . . ? C31 C30 H44 108.7 . . ? C29 C30 H44 130.1 . . ? C27 C30 H44 108.7 . . ? H43 C30 H44 107.6 . . ? C31 C30 H45 107.4 . . ? C29 C30 H45 107.4 . . ? C27 C30 H45 137.0 . . ? H43 C30 H45 44.4 . . ? H44 C30 H45 66.2 . . ? C31 C30 H46 107.4 . . ? C29 C30 H46 107.4 . . ? C27 C30 H46 71.4 . . ? H43 C30 H46 139.6 . . ? H44 C30 H46 42.3 . . ? H45 C30 H46 106.9 . . ? C30 C31 C22 112.6(8) . . ? C30 C31 H47 109.1 . . ? C22 C31 H47 109.1 . . ? C30 C31 H48 109.1 . . ? C22 C31 H48 109.1 . . ? H47 C31 H48 107.8 . . ? 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 C23 Ir1 P1 C1 -146.9(4) . . . . ? C22 Ir1 P1 C1 174.4(4) . . . . ? N1 Ir1 P1 C1 4.9(4) . . . . ? Cl1 Ir1 P1 C1 56.0(5) . . . . ? C23 Ir1 P1 C8 -30.8(4) . . . . ? C22 Ir1 P1 C8 -69.5(4) . . . . ? N1 Ir1 P1 C8 120.9(4) . . . . ? Cl1 Ir1 P1 C8 172.1(5) . . . . ? C23 Ir1 P1 C14 96.9(4) . . . . ? C22 Ir1 P1 C14 58.2(4) . . . . ? N1 Ir1 P1 C14 -111.4(4) . . . . ? Cl1 Ir1 P1 C14 -60.2(5) . . . . ? C23 Ir1 N1 C2 85.1(8) . . . . ? C22 Ir1 N1 C2 -80.7(18) . . . . ? P1 Ir1 N1 C2 -7.9(5) . . . . ? Cl1 Ir1 N1 C2 -179.1(5) . . . . ? C23 Ir1 N1 C21 -154.4(7) . . . . ? C22 Ir1 N1 C21 39.8(19) . . . . ? P1 Ir1 N1 C21 112.6(5) . . . . ? Cl1 Ir1 N1 C21 -58.6(5) . . . . ? C23 Ir1 N1 C20 -36.8(9) . . . . ? C22 Ir1 N1 C20 157.4(15) . . . . ? P1 Ir1 N1 C20 -129.8(6) . . . . ? Cl1 Ir1 N1 C20 59.0(6) . . . . ? C8 P1 C1 C6 44.4(9) . . . . ? C14 P1 C1 C6 -62.5(9) . . . . ? Ir1 P1 C1 C6 176.0(7) . . . . ? C8 P1 C1 C2 -133.4(7) . . . . ? C14 P1 C1 C2 119.7(7) . . . . ? Ir1 P1 C1 C2 -1.8(7) . . . . ? C6 C1 C2 C3 -1.9(13) . . . . ? P1 C1 C2 C3 176.1(6) . . . . ? C6 C1 C2 N1 177.2(8) . . . . ? P1 C1 C2 N1 -4.9(11) . . . . ? C21 N1 C2 C1 -112.0(9) . . . . ? C20 N1 C2 C1 128.4(9) . . . . ? Ir1 N1 C2 C1 9.3(10) . . . . ? C21 N1 C2 C3 67.1(9) . . . . ? C20 N1 C2 C3 -52.5(10) . . . . ? Ir1 N1 C2 C3 -171.6(6) . . . . ? C1 C2 C3 C4 2.4(13) . . . . ? N1 C2 C3 C4 -176.7(8) . . . . ? C2 C3 C4 C5 -0.8(14) . . . . ? C3 C4 C5 C6 -1.2(13) . . . . ? C3 C4 C5 C7 178.5(9) . . . . ? C2 C1 C6 C5 -0.2(14) . . . . ? P1 C1 C6 C5 -177.9(7) . . . . ? C4 C5 C6 C1 1.7(13) . . . . ? C7 C5 C6 C1 -178.0(9) . . . . ? C1 P1 C8 C9 68.2(7) . . . . ? C14 P1 C8 C9 178.3(6) . . . . ? Ir1 P1 C8 C9 -49.2(7) . . . . ? C1 P1 C8 C13 -166.0(6) . . . . ? C14 P1 C8 C13 -55.8(7) . . . . ? Ir1 P1 C8 C13 76.7(7) . . . . ? C13 C8 C9 C10 55.4(10) . . . . ? P1 C8 C9 C10 -176.6(6) . . . . ? C8 C9 C10 C11 -56.5(11) . . . . ? C9 C10 C11 C12 56.7(11) . . . . ? C10 C11 C12 C13 -56.8(11) . . . . ? C11 C12 C13 C8 55.8(11) . . . . ? C9 C8 C13 C12 -55.0(10) . . . . ? P1 C8 C13 C12 179.0(7) . . . . ? C1 P1 C14 C15 52.4(7) . . . . ? C8 P1 C14 C15 -54.0(7) . . . . ? Ir1 P1 C14 C15 167.3(6) . . . . ? C1 P1 C14 C19 -73.6(6) . . . . ? C8 P1 C14 C19 180.0(6) . . . . ? Ir1 P1 C14 C19 41.3(6) . . . . ? C19 C14 C15 C16 -56.8(10) . . . . ? P1 C14 C15 C16 177.5(7) . . . . ? C14 C15 C16 C17 57.3(11) . . . . ? C15 C16 C17 C18 -55.9(11) . . . . ? C16 C17 C18 C19 55.2(11) . . . . ? C17 C18 C19 C14 -55.5(10) . . . . ? C15 C14 C19 C18 55.5(9) . . . . ? P1 C14 C19 C18 -174.6(6) . . . . ? N1 Ir1 C22 C23 169.4(15) . . . . ? P1 Ir1 C22 C23 97.3(5) . . . . ? Cl1 Ir1 C22 C23 -92.7(5) . . . . ? C23 Ir1 C22 C31 116.8(9) . . . . ? N1 Ir1 C22 C31 -73.8(18) . . . . ? P1 Ir1 C22 C31 -146.0(7) . . . . ? Cl1 Ir1 C22 C31 24.0(7) . . . . ? C31 C22 C23 C24 0.2(14) . . . . ? Ir1 C22 C23 C24 113.6(9) . . . . ? C31 C22 C23 Ir1 -113.4(8) . . . . ? N1 Ir1 C23 C22 -175.8(6) . . . . ? P1 Ir1 C23 C22 -85.4(5) . . . . ? Cl1 Ir1 C23 C22 90.2(5) . . . . ? C22 Ir1 C23 C24 -118.7(10) . . . . ? N1 Ir1 C23 C24 65.6(11) . . . . ? P1 Ir1 C23 C24 155.9(7) . . . . ? Cl1 Ir1 C23 C24 -28.5(7) . . . . ? C22 C23 C24 C25 90.6(11) . . . . ? Ir1 C23 C24 C25 176.9(7) . . . . ? C23 C24 C25 C26 -45.9(14) . . . . ? C23 C24 C25 C28 -80.5(18) . . . . ? C24 C25 C26 C27 -59.2(16) . . . . ? C28 C25 C26 C27 27(3) . . . . ? C25 C26 C27 C30 104.6(14) . . . . ? C26 C25 C28 C29 -35(2) . . . . ? C24 C25 C28 C29 73(3) . . . . ? C25 C28 C29 C30 -103(3) . . . . ? C28 C29 C30 C31 71(3) . . . . ? C28 C29 C30 C27 -22.6(19) . . . . ? C26 C27 C30 C31 -73.2(15) . . . . ? C26 C27 C30 C29 35(2) . . . . ? C29 C30 C31 C22 30.6(19) . . . . ? C27 C30 C31 C22 76.3(12) . . . . ? C23 C22 C31 C30 -84.5(11) . . . . ? Ir1 C22 C31 C30 -168.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.698 _refine_diff_density_min -3.101 _refine_diff_density_rms 0.303 #===END data_(PcyN-P,N)IrCl(PMe3)(3)\/YC7H8 _database_code_depnum_ccdc_archive 'CCDC 772162' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H43 Cl Ir N P2, C7 H8' _chemical_formula_sum 'C31 H51 Cl Ir N P2' _chemical_formula_weight 727.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2063(5) _cell_length_b 18.9042(12) _cell_length_c 18.4783(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.2856(9) _cell_angle_gamma 90.00 _cell_volume 3210.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7012 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 4.361 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5243 _exptl_absorpt_correction_T_max 0.5803 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21422 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.0732 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7012 _reflns_number_gt 5499 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0001P)^2^+72.5522P] 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 7012 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1512 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 0.07599(5) 0.32190(2) 0.73871(2) 0.02324(12) Uani 1 1 d . . . Cl1 Cl 0.0504(4) 0.19599(15) 0.72362(17) 0.0436(8) Uani 1 1 d . . . P1 P 0.0702(3) 0.43538(14) 0.75705(12) 0.0189(5) Uani 1 1 d . . . P2 P 0.2330(3) 0.31545(16) 0.65293(14) 0.0276(6) Uani 1 1 d . . . N1 N -0.0666(9) 0.3156(5) 0.8307(5) 0.0271(19) Uani 1 1 d . . . C1 C -0.0318(11) 0.4460(5) 0.8385(5) 0.022(2) Uani 1 1 d . . . C2 C -0.0886(11) 0.3843(6) 0.8665(5) 0.024(2) Uani 1 1 d . . . C3 C -0.1706(11) 0.3871(6) 0.9280(5) 0.029(2) Uani 1 1 d . . . H1 H -0.2088 0.3449 0.9474 0.035 Uiso 1 1 calc R . . C4 C -0.1958(12) 0.4510(6) 0.9602(5) 0.031(3) Uani 1 1 d . . . H2 H -0.2505 0.4523 1.0022 0.037 Uiso 1 1 calc R . . C5 C -0.1433(11) 0.5136(6) 0.9329(5) 0.026(2) Uani 1 1 d . . . C6 C -0.0653(11) 0.5091(6) 0.8715(5) 0.025(2) Uani 1 1 d . . . H3 H -0.0328 0.5518 0.8506 0.029 Uiso 1 1 calc R . . C7 C -0.1746(13) 0.5827(6) 0.9674(6) 0.036(3) Uani 1 1 d . . . H4 H -0.1307 0.6209 0.9402 0.053 Uiso 1 1 calc R . . H5 H -0.1335 0.5828 1.0175 0.053 Uiso 1 1 calc R . . H6 H -0.2801 0.5898 0.9671 0.053 Uiso 1 1 calc R . . C8 C 0.2429(11) 0.4831(5) 0.7731(5) 0.023(2) Uani 1 1 d . . . H7 H 0.2895 0.4818 0.7256 0.027 Uiso 1 1 calc R . . C9 C 0.2410(12) 0.5610(6) 0.7938(6) 0.032(3) Uani 1 1 d . . . H8 H 0.2074 0.5664 0.8435 0.039 Uiso 1 1 calc R . . H9 H 0.1731 0.5872 0.7601 0.039 Uiso 1 1 calc R . . C10 C 0.3952(13) 0.5911(7) 0.7903(7) 0.041(3) Uani 1 1 d . . . H10 H 0.4261 0.5874 0.7400 0.049 Uiso 1 1 calc R . . H11 H 0.3947 0.6418 0.8036 0.049 Uiso 1 1 calc R . . C11 C 0.5029(14) 0.5521(7) 0.8406(8) 0.048(3) Uani 1 1 d . . . H12 H 0.6020 0.5708 0.8347 0.058 Uiso 1 1 calc R . . H13 H 0.4787 0.5601 0.8915 0.058 Uiso 1 1 calc R . . C12 C 0.4999(15) 0.4748(8) 0.8247(8) 0.050(3) Uani 1 1 d . . . H14 H 0.5644 0.4500 0.8611 0.059 Uiso 1 1 calc R . . H15 H 0.5385 0.4666 0.7765 0.059 Uiso 1 1 calc R . . C13 C 0.3477(12) 0.4435(7) 0.8254(6) 0.037(3) Uani 1 1 d . . . H16 H 0.3129 0.4464 0.8751 0.044 Uiso 1 1 calc R . . H17 H 0.3505 0.3930 0.8115 0.044 Uiso 1 1 calc R . . C14 C -0.0392(10) 0.4951(5) 0.6953(5) 0.020(2) Uani 1 1 d . . . H18 H -0.0507 0.5412 0.7208 0.025 Uiso 1 1 calc R . . C15 C 0.0323(12) 0.5099(6) 0.6236(5) 0.028(2) Uani 1 1 d . . . H19 H 0.1293 0.5316 0.6337 0.034 Uiso 1 1 calc R . . H20 H 0.0454 0.4650 0.5972 0.034 Uiso 1 1 calc R . . C16 C -0.0646(13) 0.5603(6) 0.5771(6) 0.034(3) Uani 1 1 d . . . H21 H -0.0701 0.6064 0.6023 0.040 Uiso 1 1 calc R . . H22 H -0.0195 0.5686 0.5305 0.040 Uiso 1 1 calc R . . C17 C -0.2152(12) 0.5325(7) 0.5620(6) 0.037(3) Uani 1 1 d . . . H23 H -0.2118 0.4896 0.5314 0.045 Uiso 1 1 calc R . . H24 H -0.2750 0.5684 0.5351 0.045 Uiso 1 1 calc R . . C18 C -0.2845(13) 0.5145(8) 0.6326(7) 0.046(3) Uani 1 1 d . . . H25 H -0.3812 0.4930 0.6213 0.055 Uiso 1 1 calc R . . H26 H -0.2991 0.5586 0.6600 0.055 Uiso 1 1 calc R . . C19 C -0.1914(12) 0.4632(7) 0.6800(6) 0.036(3) Uani 1 1 d . . . H27 H -0.1834 0.4173 0.6547 0.043 Uiso 1 1 calc R . . H28 H -0.2380 0.4548 0.7262 0.043 Uiso 1 1 calc R . . C20 C 0.0019(15) 0.2650(6) 0.8852(6) 0.041(3) Uani 1 1 d . . . H29 H 0.0877 0.2871 0.9096 0.061 Uiso 1 1 calc R . . H30 H 0.0312 0.2219 0.8605 0.061 Uiso 1 1 calc R . . H31 H -0.0684 0.2530 0.9211 0.061 Uiso 1 1 calc R . . C21 C -0.2106(14) 0.2869(7) 0.8043(7) 0.045(3) Uani 1 1 d . . . H32 H -0.2748 0.2842 0.8447 0.068 Uiso 1 1 calc R . . H33 H -0.1978 0.2395 0.7842 0.068 Uiso 1 1 calc R . . H34 H -0.2541 0.3180 0.7665 0.068 Uiso 1 1 calc R . . C22 C 0.3522(12) 0.3869(6) 0.6268(6) 0.033(3) Uani 1 1 d . . . H35 H 0.4169 0.4005 0.6685 0.050 Uiso 1 1 calc R . . H36 H 0.2933 0.4277 0.6107 0.050 Uiso 1 1 calc R . . H37 H 0.4106 0.3709 0.5872 0.050 Uiso 1 1 calc R . . C23 C 0.3723(13) 0.2489(7) 0.6725(7) 0.043(3) Uani 1 1 d . . . H38 H 0.4261 0.2404 0.6291 0.064 Uiso 1 1 calc R . . H39 H 0.3264 0.2048 0.6872 0.064 Uiso 1 1 calc R . . H40 H 0.4395 0.2656 0.7119 0.064 Uiso 1 1 calc R . . C24 C 0.1568(13) 0.2882(7) 0.5640(6) 0.038(3) Uani 1 1 d . . . H41 H 0.2355 0.2822 0.5310 0.057 Uiso 1 1 calc R . . H42 H 0.0891 0.3245 0.5448 0.057 Uiso 1 1 calc R . . H43 H 0.1049 0.2433 0.5685 0.057 Uiso 1 1 calc R . . C25 C 0.6419(17) 0.2323(9) 1.0150(8) 0.059(4) Uani 1 1 d . . . C26 C 0.5420(16) 0.2812(8) 0.9909(8) 0.052(4) Uani 1 1 d . . . H44 H 0.5344 0.3251 1.0155 0.062 Uiso 1 1 calc R . . C27 C 0.4487(19) 0.2660(12) 0.9284(11) 0.084(6) Uani 1 1 d . . . H45 H 0.3804 0.3002 0.9101 0.101 Uiso 1 1 calc R . . C28 C 0.459(2) 0.1998(13) 0.8944(10) 0.083(6) Uani 1 1 d . . . H46 H 0.3977 0.1879 0.8532 0.099 Uiso 1 1 calc R . . C29 C 0.565(2) 0.1512(10) 0.9236(11) 0.079(6) Uani 1 1 d . . . H47 H 0.5751 0.1059 0.9022 0.094 Uiso 1 1 calc R . . C30 C 0.651(2) 0.1699(9) 0.9815(10) 0.073(5) Uani 1 1 d . . . H48 H 0.7221 0.1371 0.9997 0.087 Uiso 1 1 calc R . . C31 C 0.743(2) 0.2503(11) 1.0793(9) 0.080(6) Uani 1 1 d . . . H49 H 0.6921 0.2429 1.1240 0.120 Uiso 1 1 calc R . . H50 H 0.7725 0.2999 1.0762 0.120 Uiso 1 1 calc R . . H51 H 0.8286 0.2197 1.0796 0.120 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 0.0280(2) 0.0196(2) 0.02256(18) -0.00067(17) 0.00511(13) -0.0002(2) Cl1 0.062(2) 0.0197(14) 0.0507(19) -0.0052(12) 0.0173(15) -0.0063(13) P1 0.0232(13) 0.0188(12) 0.0149(12) 0.0003(9) 0.0036(9) -0.0019(10) P2 0.0331(15) 0.0268(15) 0.0232(13) -0.0007(11) 0.0058(10) 0.0056(13) N1 0.020(4) 0.022(5) 0.040(5) 0.005(4) 0.008(3) -0.004(4) C1 0.024(5) 0.025(5) 0.018(5) 0.005(4) 0.004(4) 0.009(4) C2 0.031(6) 0.028(6) 0.014(5) -0.002(4) 0.001(4) 0.001(5) C3 0.025(6) 0.038(7) 0.024(5) 0.006(5) -0.001(4) -0.003(5) C4 0.034(6) 0.040(7) 0.020(5) -0.008(5) 0.007(4) 0.006(5) C5 0.025(5) 0.029(6) 0.024(5) -0.005(4) -0.003(4) 0.008(5) C6 0.032(6) 0.023(5) 0.019(5) 0.007(4) 0.004(4) 0.000(5) C7 0.041(7) 0.045(7) 0.021(5) -0.011(5) 0.001(4) 0.011(6) C8 0.029(5) 0.023(5) 0.017(5) 0.004(4) 0.005(4) -0.003(4) C9 0.032(6) 0.022(6) 0.041(7) -0.002(5) -0.005(5) -0.003(5) C10 0.030(6) 0.032(7) 0.061(8) -0.004(6) -0.001(5) -0.009(5) C11 0.033(7) 0.050(9) 0.061(9) -0.005(7) -0.015(6) -0.005(6) C12 0.047(8) 0.052(9) 0.048(8) 0.003(7) -0.012(6) -0.003(7) C13 0.032(6) 0.042(7) 0.036(6) 0.004(5) -0.008(5) 0.004(5) C14 0.024(5) 0.028(5) 0.010(4) 0.005(4) 0.002(3) 0.004(4) C15 0.034(6) 0.027(6) 0.024(5) 0.005(4) 0.002(4) -0.003(5) C16 0.047(7) 0.035(7) 0.020(5) 0.008(5) 0.006(5) 0.001(6) C17 0.032(6) 0.047(8) 0.033(6) 0.010(5) -0.004(5) 0.004(6) C18 0.031(6) 0.064(9) 0.044(7) 0.011(7) -0.001(5) 0.003(6) C19 0.034(6) 0.042(7) 0.030(6) 0.007(5) -0.001(5) -0.005(6) C20 0.054(8) 0.033(7) 0.036(7) 0.009(5) 0.005(6) 0.004(6) C21 0.044(8) 0.045(8) 0.047(8) 0.005(6) 0.003(6) -0.010(6) C22 0.029(6) 0.041(7) 0.032(6) -0.001(5) 0.012(5) 0.001(5) C23 0.034(7) 0.043(7) 0.054(8) 0.010(6) 0.020(6) 0.029(6) C24 0.040(7) 0.042(7) 0.031(6) -0.008(5) 0.002(5) 0.004(6) C25 0.055(10) 0.071(11) 0.055(9) 0.019(8) 0.024(7) -0.009(8) C26 0.047(8) 0.055(9) 0.057(9) 0.015(7) 0.026(7) 0.001(7) C27 0.051(10) 0.116(18) 0.087(14) 0.053(13) 0.020(9) -0.010(11) C28 0.077(13) 0.114(18) 0.060(11) -0.010(11) 0.027(9) -0.052(13) C29 0.094(15) 0.062(12) 0.082(13) -0.008(10) 0.028(11) -0.026(11) C30 0.095(14) 0.039(9) 0.089(13) -0.003(9) 0.046(11) -0.013(9) C31 0.076(12) 0.112(16) 0.052(10) 0.007(10) 0.016(9) -0.010(12) _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 P1 2.173(3) . ? Ir1 N1 2.209(8) . ? Ir1 P2 2.209(3) . ? Ir1 Cl1 2.406(3) . ? P1 C1 1.830(9) . ? P1 C8 1.838(10) . ? P1 C14 1.859(9) . ? P2 C23 1.818(11) . ? P2 C22 1.823(12) . ? P2 C24 1.824(11) . ? N1 C2 1.476(13) . ? N1 C21 1.489(15) . ? N1 C20 1.502(14) . ? C1 C6 1.383(14) . ? C1 C2 1.390(14) . ? C2 C3 1.401(14) . ? C3 C4 1.372(15) . ? C3 H1 0.9500 . ? C4 C5 1.383(16) . ? C4 H2 0.9500 . ? C5 C6 1.381(14) . ? C5 C7 1.488(15) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C9 1.523(14) . ? C8 C13 1.523(14) . ? C8 H7 1.0000 . ? C9 C10 1.535(15) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.512(17) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.492(19) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.522(17) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C19 1.537(14) . ? C14 C15 1.539(13) . ? C14 H18 1.0000 . ? C15 C16 1.535(15) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.494(16) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.522(16) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.534(16) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C22 H35 0.9800 . ? C22 H36 0.9800 . ? C22 H37 0.9800 . ? C23 H38 0.9800 . ? C23 H39 0.9800 . ? C23 H40 0.9800 . ? C24 H41 0.9800 . ? C24 H42 0.9800 . ? C24 H43 0.9800 . ? C25 C30 1.34(2) . ? C25 C26 1.36(2) . ? C25 C31 1.50(2) . ? C26 C27 1.43(2) . ? C26 H44 0.9500 . ? C27 C28 1.41(3) . ? C27 H45 0.9500 . ? C28 C29 1.42(3) . ? C28 H46 0.9500 . ? C29 C30 1.34(3) . ? C29 H47 0.9500 . ? C30 H48 0.9500 . ? C31 H49 0.9800 . ? C31 H50 0.9800 . ? C31 H51 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 P1 Ir1 N1 84.9(2) . . ? P1 Ir1 P2 100.92(10) . . ? N1 Ir1 P2 172.4(2) . . ? P1 Ir1 Cl1 172.48(11) . . ? N1 Ir1 Cl1 88.7(2) . . ? P2 Ir1 Cl1 85.76(11) . . ? C1 P1 C8 107.1(5) . . ? C1 P1 C14 98.8(4) . . ? C8 P1 C14 103.5(5) . . ? C1 P1 Ir1 104.8(3) . . ? C8 P1 Ir1 118.8(3) . . ? C14 P1 Ir1 121.4(3) . . ? C23 P2 C22 97.9(6) . . ? C23 P2 C24 102.4(6) . . ? C22 P2 C24 100.2(6) . . ? C23 P2 Ir1 112.2(4) . . ? C22 P2 Ir1 125.3(4) . . ? C24 P2 Ir1 115.4(4) . . ? C2 N1 C21 109.0(9) . . ? C2 N1 C20 108.8(8) . . ? C21 N1 C20 108.6(9) . . ? C2 N1 Ir1 113.7(6) . . ? C21 N1 Ir1 108.9(7) . . ? C20 N1 Ir1 107.8(7) . . ? C6 C1 C2 117.5(9) . . ? C6 C1 P1 126.5(8) . . ? C2 C1 P1 115.8(7) . . ? C1 C2 C3 120.1(10) . . ? C1 C2 N1 120.4(8) . . ? C3 C2 N1 119.5(9) . . ? C4 C3 C2 119.9(10) . . ? C4 C3 H1 120.1 . . ? C2 C3 H1 120.1 . . ? C3 C4 C5 121.6(10) . . ? C3 C4 H2 119.2 . . ? C5 C4 H2 119.2 . . ? C6 C5 C4 117.1(10) . . ? C6 C5 C7 121.8(10) . . ? C4 C5 C7 121.0(10) . . ? C5 C6 C1 123.7(10) . . ? C5 C6 H3 118.2 . . ? C1 C6 H3 118.2 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C9 C8 C13 109.4(9) . . ? C9 C8 P1 119.6(8) . . ? C13 C8 P1 111.8(7) . . ? C9 C8 H7 104.9 . . ? C13 C8 H7 104.9 . . ? P1 C8 H7 104.9 . . ? C8 C9 C10 108.9(10) . . ? C8 C9 H8 109.9 . . ? C10 C9 H8 109.9 . . ? C8 C9 H9 109.9 . . ? C10 C9 H9 109.9 . . ? H8 C9 H9 108.3 . . ? C11 C10 C9 111.7(11) . . ? C11 C10 H10 109.3 . . ? C9 C10 H10 109.3 . . ? C11 C10 H11 109.3 . . ? C9 C10 H11 109.3 . . ? H10 C10 H11 107.9 . . ? C12 C11 C10 110.6(11) . . ? C12 C11 H12 109.5 . . ? C10 C11 H12 109.5 . . ? C12 C11 H13 109.5 . . ? C10 C11 H13 109.5 . . ? H12 C11 H13 108.1 . . ? C11 C12 C13 112.7(12) . . ? C11 C12 H14 109.1 . . ? C13 C12 H14 109.1 . . ? C11 C12 H15 109.1 . . ? C13 C12 H15 109.1 . . ? H14 C12 H15 107.8 . . ? C12 C13 C8 110.7(10) . . ? C12 C13 H16 109.5 . . ? C8 C13 H16 109.5 . . ? C12 C13 H17 109.5 . . ? C8 C13 H17 109.5 . . ? H16 C13 H17 108.1 . . ? C19 C14 C15 110.0(8) . . ? C19 C14 P1 109.4(7) . . ? C15 C14 P1 113.3(7) . . ? C19 C14 H18 108.0 . . ? C15 C14 H18 108.0 . . ? P1 C14 H18 108.0 . . ? C16 C15 C14 109.4(9) . . ? C16 C15 H19 109.8 . . ? C14 C15 H19 109.8 . . ? C16 C15 H20 109.8 . . ? C14 C15 H20 109.8 . . ? H19 C15 H20 108.2 . . ? C17 C16 C15 112.9(9) . . ? C17 C16 H21 109.0 . . ? C15 C16 H21 109.0 . . ? C17 C16 H22 109.0 . . ? C15 C16 H22 109.0 . . ? H21 C16 H22 107.8 . . ? C16 C17 C18 110.4(9) . . ? C16 C17 H23 109.6 . . ? C18 C17 H23 109.6 . . ? C16 C17 H24 109.6 . . ? C18 C17 H24 109.6 . . ? H23 C17 H24 108.1 . . ? C17 C18 C19 112.5(10) . . ? C17 C18 H25 109.1 . . ? C19 C18 H25 109.1 . . ? C17 C18 H26 109.1 . . ? C19 C18 H26 109.1 . . ? H25 C18 H26 107.8 . . ? C18 C19 C14 109.4(10) . . ? C18 C19 H27 109.8 . . ? C14 C19 H27 109.8 . . ? C18 C19 H28 109.8 . . ? C14 C19 H28 109.8 . . ? H27 C19 H28 108.3 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? P2 C22 H35 109.5 . . ? P2 C22 H36 109.5 . . ? H35 C22 H36 109.5 . . ? P2 C22 H37 109.5 . . ? H35 C22 H37 109.5 . . ? H36 C22 H37 109.5 . . ? P2 C23 H38 109.5 . . ? P2 C23 H39 109.5 . . ? H38 C23 H39 109.5 . . ? P2 C23 H40 109.5 . . ? H38 C23 H40 109.5 . . ? H39 C23 H40 109.5 . . ? P2 C24 H41 109.5 . . ? P2 C24 H42 109.5 . . ? H41 C24 H42 109.5 . . ? P2 C24 H43 109.5 . . ? H41 C24 H43 109.5 . . ? H42 C24 H43 109.5 . . ? C30 C25 C26 120.5(18) . . ? C30 C25 C31 120.9(18) . . ? C26 C25 C31 118.6(17) . . ? C25 C26 C27 119.4(17) . . ? C25 C26 H44 120.3 . . ? C27 C26 H44 120.3 . . ? C28 C27 C26 119.1(19) . . ? C28 C27 H45 120.5 . . ? C26 C27 H45 120.5 . . ? C27 C28 C29 118.0(18) . . ? C27 C28 H46 121.0 . . ? C29 C28 H46 121.0 . . ? C30 C29 C28 119.4(18) . . ? C30 C29 H47 120.3 . . ? C28 C29 H47 120.3 . . ? C25 C30 C29 124(2) . . ? C25 C30 H48 118.2 . . ? C29 C30 H48 118.2 . . ? C25 C31 H49 109.5 . . ? C25 C31 H50 109.5 . . ? H49 C31 H50 109.5 . . ? C25 C31 H51 109.5 . . ? H49 C31 H51 109.5 . . ? H50 C31 H51 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 N1 Ir1 P1 C1 4.9(4) . . . . ? P2 Ir1 P1 C1 -170.2(3) . . . . ? Cl1 Ir1 P1 C1 37.5(9) . . . . ? N1 Ir1 P1 C8 124.2(4) . . . . ? P2 Ir1 P1 C8 -50.8(4) . . . . ? Cl1 Ir1 P1 C8 156.9(8) . . . . ? N1 Ir1 P1 C14 -105.4(4) . . . . ? P2 Ir1 P1 C14 79.6(4) . . . . ? Cl1 Ir1 P1 C14 -72.8(9) . . . . ? P1 Ir1 P2 C23 131.6(5) . . . . ? N1 Ir1 P2 C23 -8.0(19) . . . . ? Cl1 Ir1 P2 C23 -51.8(5) . . . . ? P1 Ir1 P2 C22 13.6(5) . . . . ? N1 Ir1 P2 C22 -126.1(19) . . . . ? Cl1 Ir1 P2 C22 -169.9(5) . . . . ? P1 Ir1 P2 C24 -111.6(5) . . . . ? N1 Ir1 P2 C24 108.8(19) . . . . ? Cl1 Ir1 P2 C24 64.9(5) . . . . ? P1 Ir1 N1 C2 -5.9(6) . . . . ? P2 Ir1 N1 C2 134.4(16) . . . . ? Cl1 Ir1 N1 C2 178.2(6) . . . . ? P1 Ir1 N1 C21 115.8(7) . . . . ? P2 Ir1 N1 C21 -103.8(19) . . . . ? Cl1 Ir1 N1 C21 -60.1(7) . . . . ? P1 Ir1 N1 C20 -126.5(7) . . . . ? P2 Ir1 N1 C20 14(2) . . . . ? Cl1 Ir1 N1 C20 57.5(7) . . . . ? C8 P1 C1 C6 53.6(10) . . . . ? C14 P1 C1 C6 -53.6(10) . . . . ? Ir1 P1 C1 C6 -179.5(9) . . . . ? C8 P1 C1 C2 -131.0(8) . . . . ? C14 P1 C1 C2 121.9(8) . . . . ? Ir1 P1 C1 C2 -4.0(8) . . . . ? C6 C1 C2 C3 -2.9(15) . . . . ? P1 C1 C2 C3 -178.8(8) . . . . ? C6 C1 C2 N1 175.3(9) . . . . ? P1 C1 C2 N1 -0.6(13) . . . . ? C21 N1 C2 C1 -116.7(11) . . . . ? C20 N1 C2 C1 125.1(10) . . . . ? Ir1 N1 C2 C1 5.0(12) . . . . ? C21 N1 C2 C3 61.6(12) . . . . ? C20 N1 C2 C3 -56.7(12) . . . . ? Ir1 N1 C2 C3 -176.7(7) . . . . ? C1 C2 C3 C4 0.5(16) . . . . ? N1 C2 C3 C4 -177.8(9) . . . . ? C2 C3 C4 C5 0.8(16) . . . . ? C3 C4 C5 C6 0.5(16) . . . . ? C3 C4 C5 C7 178.5(10) . . . . ? C4 C5 C6 C1 -3.2(16) . . . . ? C7 C5 C6 C1 178.9(10) . . . . ? C2 C1 C6 C5 4.4(16) . . . . ? P1 C1 C6 C5 179.8(8) . . . . ? C1 P1 C8 C9 -55.4(9) . . . . ? C14 P1 C8 C9 48.3(9) . . . . ? Ir1 P1 C8 C9 -173.6(7) . . . . ? C1 P1 C8 C13 74.2(8) . . . . ? C14 P1 C8 C13 178.0(8) . . . . ? Ir1 P1 C8 C13 -44.0(8) . . . . ? C13 C8 C9 C10 59.6(12) . . . . ? P1 C8 C9 C10 -169.7(8) . . . . ? C8 C9 C10 C11 -59.0(13) . . . . ? C9 C10 C11 C12 55.6(16) . . . . ? C10 C11 C12 C13 -53.6(16) . . . . ? C11 C12 C13 C8 55.5(14) . . . . ? C9 C8 C13 C12 -58.1(13) . . . . ? P1 C8 C13 C12 167.2(9) . . . . ? C1 P1 C14 C19 -67.2(8) . . . . ? C8 P1 C14 C19 -177.3(7) . . . . ? Ir1 P1 C14 C19 46.1(8) . . . . ? C1 P1 C14 C15 169.6(8) . . . . ? C8 P1 C14 C15 59.6(8) . . . . ? Ir1 P1 C14 C15 -77.0(8) . . . . ? C19 C14 C15 C16 58.0(12) . . . . ? P1 C14 C15 C16 -179.2(7) . . . . ? C14 C15 C16 C17 -57.1(12) . . . . ? C15 C16 C17 C18 55.0(14) . . . . ? C16 C17 C18 C19 -54.8(15) . . . . ? C17 C18 C19 C14 56.7(14) . . . . ? C15 C14 C19 C18 -58.1(12) . . . . ? P1 C14 C19 C18 176.8(8) . . . . ? C30 C25 C26 C27 -1(2) . . . . ? C31 C25 C26 C27 177.9(13) . . . . ? C25 C26 C27 C28 2(2) . . . . ? C26 C27 C28 C29 -1(2) . . . . ? C27 C28 C29 C30 0(2) . . . . ? C26 C25 C30 C29 0(2) . . . . ? C31 C25 C30 C29 -179.4(15) . . . . ? C28 C29 C30 C25 1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.222 _refine_diff_density_min -3.526 _refine_diff_density_rms 0.326 #===END data_(PcyN-P,N)2Ir2H2(m-Cl)(m-H)(m-SiClMes)-(5) _database_code_depnum_ccdc_archive 'CCDC 772163' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H82 Cl2 Ir2 N2 P2 Si' _chemical_formula_sum 'C51 H86 Cl2 Ir2 N2 P2 Si' _chemical_formula_weight 1272.55 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' 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 14.6736(9) _cell_length_b 10.0455(7) _cell_length_c 19.8282(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.567(3) _cell_angle_gamma 90.00 _cell_volume 2770.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12190 _cell_measurement_theta_min 1.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 5.007 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5622 _exptl_absorpt_correction_T_max 0.6089 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24195 _diffrn_reflns_av_R_equivalents 0.1045 _diffrn_reflns_av_sigmaI/netI 0.1007 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12190 _reflns_number_gt 9069 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0769P)^2^+123.4034P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'no H-Atom' _refine_ls_hydrogen_treatment constr _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 0.47(2) _refine_ls_number_reflns 12190 _refine_ls_number_parameters 234 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0896 _refine_ls_wR_factor_ref 0.2353 _refine_ls_wR_factor_gt 0.2060 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.104 _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 0.94602(4) 0.482(3) 0.76270(3) 0.01659(16) Uani 1 1 d D . . Ir2 Ir 1.12199(4) 0.482(3) 0.87825(3) 0.01977(17) Uani 1 1 d D . . Cl1 Cl 1.0016(4) 0.300(3) 0.8555(3) 0.0283(11) Uani 1 1 d . . . Cl2 Cl 1.1291(4) 0.701(3) 0.7369(3) 0.0323(12) Uani 1 1 d . . . P1 P 0.8547(4) 0.391(3) 0.6632(3) 0.0248(12) Uani 1 1 d D . . P2 P 1.2654(4) 0.407(3) 0.9325(3) 0.0203(11) Uani 1 1 d D . . Si1 Si 1.1012(3) 0.471(3) 0.7587(3) 0.0228(11) Uiso 1 1 d . . . N1 N 0.7976(14) 0.521(3) 0.7801(9) 0.031(5) Uiso 1 1 d D . . N2 N 1.1252(15) 0.544(3) 0.9980(12) 0.042(5) Uiso 1 1 d D . . C1 C 0.7289(9) 0.415(3) 0.6604(7) 0.041(6) Uiso 1 1 d GD . . C2 C 0.7154(8) 0.471(3) 0.7206(6) 0.021(4) Uiso 1 1 d G . . C3 C 0.6234(9) 0.505(3) 0.7203(6) 0.034(6) Uiso 1 1 d G . . C4 C 0.5450(7) 0.483(4) 0.6599(8) 0.050(6) Uiso 1 1 d G . . C5 C 0.5585(9) 0.426(4) 0.5998(7) 0.051(7) Uiso 1 1 d G . . C6 C 0.6505(12) 0.393(3) 0.6000(6) 0.036(6) Uiso 1 1 d G . . C7 C 0.470(2) 0.393(4) 0.5333(17) 0.052(8) Uiso 1 1 d . . . C8 C 0.8608(16) 0.446(4) 0.5750(12) 0.031(5) Uiso 1 1 d . . . C9 C 0.8497(19) 0.595(4) 0.5681(14) 0.035(6) Uiso 1 1 d . . . C10 C 0.853(2) 0.631(4) 0.4924(17) 0.051(7) Uiso 1 1 d . . . C11 C 0.948(2) 0.582(4) 0.4777(16) 0.043(7) Uiso 1 1 d . . . C12 C 0.960(2) 0.431(4) 0.4912(15) 0.037(6) Uiso 1 1 d . . . C13 C 0.9598(18) 0.404(4) 0.5664(13) 0.032(5) Uiso 1 1 d . . . C14 C 0.8587(18) 0.201(4) 0.6602(13) 0.031(5) Uiso 1 1 d . . . C15 C 0.8061(17) 0.137(4) 0.5864(13) 0.032(5) Uiso 1 1 d . . . C16 C 0.8300(17) -0.020(6) 0.5932(12) 0.047(5) Uiso 1 1 d . . . C17 C 0.795(2) -0.073(4) 0.6495(17) 0.053(8) Uiso 1 1 d . . . C18 C 0.8476(16) -0.012(4) 0.7218(12) 0.045(5) Uiso 1 1 d D . . C19 C 0.8262(18) 0.142(4) 0.7167(13) 0.033(5) Uiso 1 1 d D . . C20 C 0.790(2) 0.664(4) 0.7983(17) 0.053(8) Uiso 1 1 d D . . C21 C 0.790(2) 0.520(4) 0.8505(11) 0.044(7) Uiso 1 1 d D . . C22 C 1.2922(9) 0.449(3) 1.0277(5) 0.016(4) Uiso 1 1 d GD . . C23 C 1.2209(7) 0.511(3) 1.0486(7) 0.029(5) Uiso 1 1 d G . . C24 C 1.2402(10) 0.553(3) 1.1185(8) 0.043(7) Uiso 1 1 d G . . C25 C 1.3308(11) 0.533(3) 1.1676(6) 0.042(6) Uiso 1 1 d G . . C26 C 1.4021(8) 0.471(3) 1.1468(7) 0.037(5) Uiso 1 1 d G . . C27 C 1.3827(8) 0.428(3) 1.0769(7) 0.040(6) Uiso 1 1 d G . . C28 C 1.498(2) 0.444(4) 1.2037(16) 0.049(7) Uiso 1 1 d . . . C29 C 1.3752(13) 0.462(3) 0.9132(8) 0.023(4) Uiso 1 1 d D . . C30 C 1.3678(16) 0.412(4) 0.8363(10) 0.025(5) Uiso 1 1 d D . . C31 C 1.4587(13) 0.455(3) 0.8203(10) 0.022(5) Uiso 1 1 d . . . C32 C 1.4734(17) 0.604(4) 0.8241(13) 0.030(5) Uiso 1 1 d . . . C33 C 1.4751(17) 0.657(4) 0.8978(12) 0.029(5) Uiso 1 1 d . . . C34 C 1.3834(18) 0.618(3) 0.9151(13) 0.033(5) Uiso 1 1 d D . . C35 C 1.2679(16) 0.219(4) 0.9317(12) 0.025(5) Uiso 1 1 d . . . C36 C 1.3691(18) 0.150(4) 0.9562(14) 0.035(6) Uiso 1 1 d D . . C37 C 1.3561(14) -0.003(4) 0.9382(10) 0.034(5) Uiso 1 1 d D . . C38 C 1.2897(16) -0.057(4) 0.9786(14) 0.051(8) Uiso 1 1 d D . . C39 C 1.1912(17) 0.010(4) 0.9544(14) 0.048(7) Uiso 1 1 d D . . C40 C 1.2078(18) 0.163(4) 0.9714(14) 0.035(6) Uiso 1 1 d D . . C41 C 1.100(3) 0.687(4) 0.9973(19) 0.059(9) Uiso 1 1 d D . . C42 C 1.0534(15) 0.455(4) 1.0147(12) 0.034(6) Uiso 1 1 d D . . C43 C 1.1629(10) 0.384(3) 0.7045(8) 0.022(4) Uiso 1 1 d G . . C44 C 1.2204(11) 0.428(3) 0.6653(8) 0.027(5) Uiso 1 1 d G . . C45 C 1.2736(12) 0.338(3) 0.6403(9) 0.040(6) Uiso 1 1 d G . . C46 C 1.2693(12) 0.203(3) 0.6545(10) 0.047(7) Uiso 1 1 d G . . C47 C 1.2118(13) 0.159(3) 0.6936(9) 0.037(6) Uiso 1 1 d G . . C48 C 1.1586(11) 0.249(3) 0.7187(8) 0.029(5) Uiso 1 1 d G . . C49 C 1.2313(17) 0.571(4) 0.6415(13) 0.029(5) Uiso 1 1 d . . . C50 C 1.333(3) 0.108(5) 0.6286(19) 0.060(9) Uiso 1 1 d . . . C51 C 1.1034 0.1890 0.7577 0.059(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0165(3) 0.0178(3) 0.0182(3) -0.0011(6) 0.0094(2) -0.0070(6) Ir2 0.0160(3) 0.0276(4) 0.0187(3) -0.0046(7) 0.0097(2) -0.0024(6) Cl1 0.024(3) 0.036(3) 0.026(3) 0.005(2) 0.010(2) -0.003(2) Cl2 0.034(3) 0.035(3) 0.032(3) 0.002(2) 0.017(3) -0.003(2) P1 0.019(3) 0.033(3) 0.026(3) 0.007(2) 0.013(2) 0.004(2) P2 0.026(3) 0.020(3) 0.022(3) -0.006(2) 0.017(2) -0.002(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 P1 2.198(6) . ? Ir1 Si1 2.306(5) . ? Ir1 N1 2.345(19) . ? Ir1 Cl1 2.539(6) . ? Ir1 Ir2 2.8547(9) . ? Ir2 P2 2.170(6) . ? Ir2 Si1 2.294(5) . ? Ir2 N2 2.44(2) . ? Ir2 Cl1 2.481(6) . ? Cl2 Si1 2.409(11) . ? P1 C1 1.844(12) . ? P1 C8 1.86(2) . ? P1 C14 1.92(3) . ? P2 C22 1.851(11) . ? P2 C29 1.856(19) . ? P2 C35 1.89(2) . ? Si1 C43 1.831(13) . ? N1 C21 1.436(17) . ? N1 C2 1.48(2) . ? N1 C20 1.490(18) . ? N2 C23 1.48(2) . ? N2 C41 1.480(18) . ? N2 C42 1.498(17) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C5 C7 1.56(3) . ? C8 C9 1.51(4) . ? C8 C13 1.57(3) . ? C9 C10 1.56(4) . ? C10 C11 1.59(4) . ? C11 C12 1.54(4) . ? C12 C13 1.52(4) . ? C14 C19 1.47(3) . ? C14 C15 1.56(3) . ? C15 C16 1.61(6) . ? C16 C17 1.47(4) . ? C17 C18 1.52(4) . ? C18 C19 1.577(19) . ? C22 C23 1.3900 . ? C22 C27 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C26 C28 1.52(3) . ? C29 C34 1.566(17) . ? C29 C30 1.578(16) . ? C30 C31 1.53(3) . ? C31 C32 1.52(3) . ? C32 C33 1.55(3) . ? C33 C34 1.54(3) . ? C35 C40 1.47(3) . ? C35 C36 1.57(3) . ? C36 C37 1.572(18) . ? C37 C38 1.545(18) . ? C38 C39 1.526(18) . ? C39 C40 1.579(18) . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 C49 1.53(3) . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C46 C50 1.54(4) . ? C47 C48 1.3900 . ? C48 C51 1.421(16) . ? 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 P1 Ir1 Si1 106.0(2) . . ? P1 Ir1 N1 82.7(5) . . ? Si1 Ir1 N1 170.7(5) . . ? P1 Ir1 Cl1 108.3(2) . . ? Si1 Ir1 Cl1 84.0(2) . . ? N1 Ir1 Cl1 96.5(4) . . ? P1 Ir1 Ir2 148.94(16) . . ? Si1 Ir1 Ir2 51.44(12) . . ? N1 Ir1 Ir2 121.8(4) . . ? Cl1 Ir1 Ir2 54.39(13) . . ? P2 Ir2 Si1 106.5(2) . . ? P2 Ir2 N2 83.7(5) . . ? Si1 Ir2 N2 166.5(5) . . ? P2 Ir2 Cl1 110.9(2) . . ? Si1 Ir2 Cl1 85.6(2) . . ? N2 Ir2 Cl1 99.0(4) . . ? P2 Ir2 Ir1 152.22(14) . . ? Si1 Ir2 Ir1 51.84(12) . . ? N2 Ir2 Ir1 120.9(5) . . ? Cl1 Ir2 Ir1 56.31(13) . . ? Ir2 Cl1 Ir1 69.30(15) . . ? C1 P1 C8 106.3(9) . . ? C1 P1 C14 99.7(9) . . ? C8 P1 C14 104.8(10) . . ? C1 P1 Ir1 107.0(5) . . ? C8 P1 Ir1 121.4(7) . . ? C14 P1 Ir1 115.2(8) . . ? C22 P2 C29 103.1(7) . . ? C22 P2 C35 103.7(8) . . ? C29 P2 C35 106.0(9) . . ? C22 P2 Ir2 106.6(5) . . ? C29 P2 Ir2 124.3(6) . . ? C35 P2 Ir2 111.2(7) . . ? C43 Si1 Ir2 134.6(6) . . ? C43 Si1 Ir1 136.2(6) . . ? Ir2 Si1 Ir1 76.72(15) . . ? C43 Si1 Cl2 102.0(5) . . ? Ir2 Si1 Cl2 99.5(3) . . ? Ir1 Si1 Cl2 100.6(3) . . ? C21 N1 C2 118.3(17) . . ? C21 N1 C20 74.8(18) . . ? C2 N1 C20 114.3(18) . . ? C21 N1 Ir1 120.5(15) . . ? C2 N1 Ir1 112.6(10) . . ? C20 N1 Ir1 110.1(16) . . ? C23 N2 C41 113(2) . . ? C23 N2 C42 107.5(16) . . ? C41 N2 C42 113(2) . . ? C23 N2 Ir2 108.8(12) . . ? C41 N2 Ir2 108.0(17) . . ? C42 N2 Ir2 105.4(14) . . ? C2 C1 C6 120.0 . . ? C2 C1 P1 116.2(8) . . ? C6 C1 P1 123.4(8) . . ? C3 C2 C1 120.0 . . ? C3 C2 N1 117.6(11) . . ? C1 C2 N1 121.3(11) . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 C7 120.3(16) . . ? C6 C5 C7 119.6(16) . . ? C5 C6 C1 120.0 . . ? C9 C8 C13 110(2) . . ? C9 C8 P1 110.1(17) . . ? C13 C8 P1 110.0(15) . . ? C8 C9 C10 106(2) . . ? C9 C10 C11 114(2) . . ? C12 C11 C10 109(3) . . ? C13 C12 C11 108(2) . . ? C12 C13 C8 110(2) . . ? C19 C14 C15 111(2) . . ? C19 C14 P1 111.0(17) . . ? C15 C14 P1 115.5(17) . . ? C14 C15 C16 107.2(19) . . ? C17 C16 C15 107(3) . . ? C16 C17 C18 112(3) . . ? C17 C18 C19 108(2) . . ? C14 C19 C18 110(2) . . ? C23 C22 C27 120.0 . . ? C23 C22 P2 118.0(8) . . ? C27 C22 P2 121.8(8) . . ? C22 C23 C24 120.0 . . ? C22 C23 N2 122.7(12) . . ? C24 C23 N2 117.2(12) . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C27 C26 C28 122.1(15) . . ? C25 C26 C28 117.8(15) . . ? C26 C27 C22 120.0 . . ? C34 C29 C30 109.0(17) . . ? C34 C29 P2 111.0(14) . . ? C30 C29 P2 107.8(13) . . ? C31 C30 C29 108.3(16) . . ? C32 C31 C30 112.9(18) . . ? C31 C32 C33 110.2(19) . . ? C34 C33 C32 111.7(19) . . ? C33 C34 C29 108.3(18) . . ? C40 C35 C36 109.8(19) . . ? C40 C35 P2 111.1(16) . . ? C36 C35 P2 117.2(15) . . ? C35 C36 C37 109.0(19) . . ? C38 C37 C36 106.1(19) . . ? C39 C38 C37 112(2) . . ? C38 C39 C40 107(2) . . ? C35 C40 C39 110(2) . . ? C44 C43 C48 120.0 . . ? C44 C43 Si1 132.7(9) . . ? C48 C43 Si1 106.4(9) . . ? C45 C44 C43 120.0 . . ? C45 C44 C49 112.1(13) . . ? C43 C44 C49 127.9(13) . . ? C44 C45 C46 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 C50 117.7(17) . . ? C47 C46 C50 122.2(17) . . ? C46 C47 C48 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 C51 113.4(14) . . ? C43 C48 C51 126.6(14) . . ? 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 P1 Ir1 Ir2 P2 5.8(5) . . . . ? Si1 Ir1 Ir2 P2 -44.3(4) . . . . ? N1 Ir1 Ir2 P2 143.4(5) . . . . ? Cl1 Ir1 Ir2 P2 69.7(4) . . . . ? P1 Ir1 Ir2 Si1 50.1(4) . . . . ? N1 Ir1 Ir2 Si1 -172.2(5) . . . . ? Cl1 Ir1 Ir2 Si1 114.1(3) . . . . ? P1 Ir1 Ir2 N2 -143.7(5) . . . . ? Si1 Ir1 Ir2 N2 166.2(5) . . . . ? N1 Ir1 Ir2 N2 -6.0(6) . . . . ? Cl1 Ir1 Ir2 N2 -79.7(5) . . . . ? P1 Ir1 Ir2 Cl1 -63.9(3) . . . . ? Si1 Ir1 Ir2 Cl1 -114.1(3) . . . . ? N1 Ir1 Ir2 Cl1 73.7(5) . . . . ? P2 Ir2 Cl1 Ir1 -152.10(16) . . . . ? Si1 Ir2 Cl1 Ir1 -46.1(2) . . . . ? N2 Ir2 Cl1 Ir1 121.2(5) . . . . ? P1 Ir1 Cl1 Ir2 150.77(17) . . . . ? Si1 Ir1 Cl1 Ir2 45.9(2) . . . . ? N1 Ir1 Cl1 Ir2 -124.8(4) . . . . ? Si1 Ir1 P1 C1 -174.1(5) . . . . ? N1 Ir1 P1 C1 2.6(5) . . . . ? Cl1 Ir1 P1 C1 97.0(5) . . . . ? Ir2 Ir1 P1 C1 147.3(5) . . . . ? Si1 Ir1 P1 C8 -52.1(9) . . . . ? N1 Ir1 P1 C8 124.6(10) . . . . ? Cl1 Ir1 P1 C8 -141.0(9) . . . . ? Ir2 Ir1 P1 C8 -90.7(9) . . . . ? Si1 Ir1 P1 C14 76.2(9) . . . . ? N1 Ir1 P1 C14 -107.2(10) . . . . ? Cl1 Ir1 P1 C14 -12.7(9) . . . . ? Ir2 Ir1 P1 C14 37.6(10) . . . . ? Si1 Ir2 P2 C22 168.2(5) . . . . ? N2 Ir2 P2 C22 -2.9(5) . . . . ? Cl1 Ir2 P2 C22 -100.2(4) . . . . ? Ir1 Ir2 P2 C22 -156.9(4) . . . . ? Si1 Ir2 P2 C29 49.0(7) . . . . ? N2 Ir2 P2 C29 -122.1(8) . . . . ? Cl1 Ir2 P2 C29 140.6(7) . . . . ? Ir1 Ir2 P2 C29 83.9(8) . . . . ? Si1 Ir2 P2 C35 -79.5(8) . . . . ? N2 Ir2 P2 C35 109.4(9) . . . . ? Cl1 Ir2 P2 C35 12.1(8) . . . . ? Ir1 Ir2 P2 C35 -44.5(9) . . . . ? P2 Ir2 Si1 C43 16.3(9) . . . . ? N2 Ir2 Si1 C43 155(2) . . . . ? Cl1 Ir2 Si1 C43 -94.2(8) . . . . ? Ir1 Ir2 Si1 C43 -143.9(9) . . . . ? P2 Ir2 Si1 Ir1 160.1(2) . . . . ? N2 Ir2 Si1 Ir1 -61(2) . . . . ? Cl1 Ir2 Si1 Ir1 49.6(2) . . . . ? P2 Ir2 Si1 Cl2 -101.1(3) . . . . ? N2 Ir2 Si1 Cl2 37(2) . . . . ? Cl1 Ir2 Si1 Cl2 148.4(3) . . . . ? Ir1 Ir2 Si1 Cl2 98.8(3) . . . . ? P1 Ir1 Si1 C43 -13.0(9) . . . . ? N1 Ir1 Si1 C43 -172(3) . . . . ? Cl1 Ir1 Si1 C43 94.4(9) . . . . ? Ir2 Ir1 Si1 C43 142.6(10) . . . . ? P1 Ir1 Si1 Ir2 -155.7(2) . . . . ? N1 Ir1 Si1 Ir2 46(3) . . . . ? Cl1 Ir1 Si1 Ir2 -48.3(2) . . . . ? P1 Ir1 Si1 Cl2 107.0(3) . . . . ? N1 Ir1 Si1 Cl2 -52(3) . . . . ? Cl1 Ir1 Si1 Cl2 -145.6(3) . . . . ? Ir2 Ir1 Si1 Cl2 -97.4(3) . . . . ? P1 Ir1 N1 C21 147.1(16) . . . . ? Si1 Ir1 N1 C21 -53(3) . . . . ? Cl1 Ir1 N1 C21 39.4(16) . . . . ? Ir2 Ir1 N1 C21 -12.4(17) . . . . ? P1 Ir1 N1 C2 -0.2(9) . . . . ? Si1 Ir1 N1 C2 159(2) . . . . ? Cl1 Ir1 N1 C2 -108.0(10) . . . . ? Ir2 Ir1 N1 C2 -159.7(8) . . . . ? P1 Ir1 N1 C20 -129.1(16) . . . . ? Si1 Ir1 N1 C20 30(4) . . . . ? Cl1 Ir1 N1 C20 123.2(16) . . . . ? Ir2 Ir1 N1 C20 71.4(16) . . . . ? P2 Ir2 N2 C23 3.5(9) . . . . ? Si1 Ir2 N2 C23 -136.8(18) . . . . ? Cl1 Ir2 N2 C23 113.8(9) . . . . ? Ir1 Ir2 N2 C23 169.7(8) . . . . ? P2 Ir2 N2 C41 127.2(18) . . . . ? Si1 Ir2 N2 C41 -13(3) . . . . ? Cl1 Ir2 N2 C41 -122.6(18) . . . . ? Ir1 Ir2 N2 C41 -66.6(18) . . . . ? P2 Ir2 N2 C42 -111.6(14) . . . . ? Si1 Ir2 N2 C42 108.1(19) . . . . ? Cl1 Ir2 N2 C42 -1.3(14) . . . . ? Ir1 Ir2 N2 C42 54.7(15) . . . . ? C8 P1 C1 C2 -136.4(11) . . . . ? C14 P1 C1 C2 114.9(11) . . . . ? Ir1 P1 C1 C2 -5.3(9) . . . . ? C8 P1 C1 C6 36.8(13) . . . . ? C14 P1 C1 C6 -71.8(12) . . . . ? Ir1 P1 C1 C6 167.9(9) . . . . ? C6 C1 C2 C3 0.0 . . . . ? P1 C1 C2 C3 173.5(12) . . . . ? C6 C1 C2 N1 -167.7(15) . . . . ? P1 C1 C2 N1 5.8(15) . . . . ? C21 N1 C2 C3 40.6(19) . . . . ? C20 N1 C2 C3 -45(2) . . . . ? Ir1 N1 C2 C3 -171.3(9) . . . . ? C21 N1 C2 C1 -151.5(16) . . . . ? C20 N1 C2 C1 123.3(19) . . . . ? Ir1 N1 C2 C1 -3.3(16) . . . . ? C1 C2 C3 C4 0.0 . . . . ? N1 C2 C3 C4 168.1(14) . . . . ? C2 C3 C4 C5 0.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? C3 C4 C5 C7 176(2) . . . . ? C4 C5 C6 C1 0.0 . . . . ? C7 C5 C6 C1 -176(2) . . . . ? C2 C1 C6 C5 0.0 . . . . ? P1 C1 C6 C5 -173.0(13) . . . . ? C1 P1 C8 C9 70.2(18) . . . . ? C14 P1 C8 C9 175.1(17) . . . . ? Ir1 P1 C8 C9 -52.1(19) . . . . ? C1 P1 C8 C13 -168.8(14) . . . . ? C14 P1 C8 C13 -63.9(17) . . . . ? Ir1 P1 C8 C13 68.8(17) . . . . ? C13 C8 C9 C10 60(3) . . . . ? P1 C8 C9 C10 -178.5(17) . . . . ? C8 C9 C10 C11 -57(3) . . . . ? C9 C10 C11 C12 55(3) . . . . ? C10 C11 C12 C13 -56(3) . . . . ? C11 C12 C13 C8 62(3) . . . . ? C9 C8 C13 C12 -67(3) . . . . ? P1 C8 C13 C12 172.3(17) . . . . ? C1 P1 C14 C19 -53.5(18) . . . . ? C8 P1 C14 C19 -163.3(17) . . . . ? Ir1 P1 C14 C19 60.6(18) . . . . ? C1 P1 C14 C15 74.5(18) . . . . ? C8 P1 C14 C15 -35(2) . . . . ? Ir1 P1 C14 C15 -171.5(15) . . . . ? C19 C14 C15 C16 -60(3) . . . . ? P1 C14 C15 C16 172.6(16) . . . . ? C14 C15 C16 C17 60(3) . . . . ? C15 C16 C17 C18 -64(3) . . . . ? C16 C17 C18 C19 63(3) . . . . ? C15 C14 C19 C18 60(3) . . . . ? P1 C14 C19 C18 -169.9(16) . . . . ? C17 C18 C19 C14 -59(3) . . . . ? C29 P2 C22 C23 134.7(10) . . . . ? C35 P2 C22 C23 -114.9(11) . . . . ? Ir2 P2 C22 C23 2.5(9) . . . . ? C29 P2 C22 C27 -40.4(11) . . . . ? C35 P2 C22 C27 70.0(11) . . . . ? Ir2 P2 C22 C27 -172.6(8) . . . . ? C27 C22 C23 C24 0.0 . . . . ? P2 C22 C23 C24 -175.2(9) . . . . ? C27 C22 C23 N2 175.8(15) . . . . ? P2 C22 C23 N2 0.7(16) . . . . ? C41 N2 C23 C22 -123(2) . . . . ? C42 N2 C23 C22 110.6(18) . . . . ? Ir2 N2 C23 C22 -3.1(16) . . . . ? C41 N2 C23 C24 52(2) . . . . ? C42 N2 C23 C24 -73.4(17) . . . . ? Ir2 N2 C23 C24 172.8(8) . . . . ? C22 C23 C24 C25 0.0 . . . . ? N2 C23 C24 C25 -176.1(14) . . . . ? C23 C24 C25 C26 0.0 . . . . ? C24 C25 C26 C27 0.0 . . . . ? C24 C25 C26 C28 -176.6(19) . . . . ? C25 C26 C27 C22 0.0 . . . . ? C28 C26 C27 C22 176(2) . . . . ? C23 C22 C27 C26 0.0 . . . . ? P2 C22 C27 C26 175.0(10) . . . . ? C22 P2 C29 C34 -69.3(14) . . . . ? C35 P2 C29 C34 -178.0(14) . . . . ? Ir2 P2 C29 C34 51.5(15) . . . . ? C22 P2 C29 C30 171.4(12) . . . . ? C35 P2 C29 C30 62.8(15) . . . . ? Ir2 P2 C29 C30 -67.8(14) . . . . ? C34 C29 C30 C31 60(2) . . . . ? P2 C29 C30 C31 -179.1(14) . . . . ? C29 C30 C31 C32 -59(2) . . . . ? C30 C31 C32 C33 56(2) . . . . ? C31 C32 C33 C34 -56(2) . . . . ? C32 C33 C34 C29 59(2) . . . . ? C30 C29 C34 C33 -61(2) . . . . ? P2 C29 C34 C33 -179.3(14) . . . . ? C22 P2 C35 C40 50.4(18) . . . . ? C29 P2 C35 C40 158.6(16) . . . . ? Ir2 P2 C35 C40 -63.7(17) . . . . ? C22 P2 C35 C36 -76.8(18) . . . . ? C29 P2 C35 C36 31.4(19) . . . . ? Ir2 P2 C35 C36 169.0(15) . . . . ? C40 C35 C36 C37 63(2) . . . . ? P2 C35 C36 C37 -169.5(15) . . . . ? C35 C36 C37 C38 -59(2) . . . . ? C36 C37 C38 C39 61(3) . . . . ? C37 C38 C39 C40 -61(3) . . . . ? C36 C35 C40 C39 -62(2) . . . . ? P2 C35 C40 C39 166.4(15) . . . . ? C38 C39 C40 C35 61(3) . . . . ? Ir2 Si1 C43 C44 -110.4(12) . . . . ? Ir1 Si1 C43 C44 125.6(10) . . . . ? Cl2 Si1 C43 C44 6.1(12) . . . . ? Ir2 Si1 C43 C48 58.2(11) . . . . ? Ir1 Si1 C43 C48 -65.9(10) . . . . ? Cl2 Si1 C43 C48 174.6(6) . . . . ? C48 C43 C44 C45 0.0 . . . . ? Si1 C43 C44 C45 167.3(14) . . . . ? C48 C43 C44 C49 177.0(19) . . . . ? Si1 C43 C44 C49 -16(2) . . . . ? C43 C44 C45 C46 0.0 . . . . ? C49 C44 C45 C46 -177.5(16) . . . . ? C44 C45 C46 C47 0.0 . . . . ? C44 C45 C46 C50 -177(2) . . . . ? C45 C46 C47 C48 0.0 . . . . ? C50 C46 C47 C48 177(2) . . . . ? C46 C47 C48 C43 0.0 . . . . ? C46 C47 C48 C51 180.0(13) . . . . ? C44 C43 C48 C47 0.0 . . . . ? Si1 C43 C48 C47 -170.3(11) . . . . ? C44 C43 C48 C51 -180.0(15) . . . . ? Si1 C43 C48 C51 9.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.447 _refine_diff_density_min -3.511 _refine_diff_density_rms 0.502 #===END data_(PcyN-P,N)2Ir2H(m-Cl)(m-H)[m-SiMeCl(C6H3-2,4,-Me2-6-CH)-Si,C,C]-(7)?C7H8 _database_code_depnum_ccdc_archive 'CCDC 772164' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H81 Cl2 Ir2 N2 P2 Si, C7 H8' _chemical_formula_sum 'C59 H89 Cl2 Ir2 N2 P2 Si' _chemical_formula_weight 1371.65 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' 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1763(8) _cell_length_b 15.2748(8) _cell_length_c 17.6511(12) _cell_angle_alpha 71.710(2) _cell_angle_beta 80.573(2) _cell_angle_gamma 69.440(2) _cell_volume 2913.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12585 _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1378 _exptl_absorpt_coefficient_mu 4.769 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.4978 _exptl_absorpt_correction_T_max 0.6220 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26343 _diffrn_reflns_av_R_equivalents 0.0539 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 27.42 _reflns_number_total 12585 _reflns_number_gt 9998 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0674P)^2^+16.5323P] 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 12585 _refine_ls_number_parameters 614 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.1565 _refine_ls_wR_factor_gt 0.1426 _refine_ls_goodness_of_fit_ref 1.255 _refine_ls_restrained_S_all 1.255 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.23755(3) 0.30318(2) 0.24462(2) 0.01583(10) Uani 1 1 d . . . Ir2 Ir 0.16212(3) 0.49761(3) 0.17276(2) 0.01804(11) Uani 1 1 d . . . Cl1 Cl 0.0362(2) 0.39298(17) 0.17157(15) 0.0246(5) Uani 1 1 d . . . Cl2 Cl 0.5272(2) 0.17633(19) 0.34186(17) 0.0318(6) Uani 1 1 d . . . P1 P 0.2137(2) 0.18069(17) 0.35066(14) 0.0166(5) Uani 1 1 d . A . P2 P 0.0443(2) 0.64651(17) 0.16828(14) 0.0184(5) Uani 1 1 d . . . Si1 Si 0.4046(2) 0.31138(19) 0.28045(16) 0.0202(5) Uani 1 1 d . . . N1 N 0.3149(7) 0.1823(6) 0.1813(5) 0.0193(16) Uani 1 1 d . . . N2 N 0.1915(7) 0.5613(6) 0.0378(5) 0.0215(17) Uani 1 1 d . . . C1 C 0.2984(8) 0.0688(7) 0.3206(6) 0.0198(19) Uiso 1 1 d . . . C2 C 0.3435(9) 0.0835(7) 0.2398(6) 0.021(2) Uani 1 1 d . . . C3 C 0.4099(9) 0.0021(8) 0.2129(7) 0.029(2) Uani 1 1 d . . . H1 H 0.4391 0.0102 0.1587 0.035 Uiso 1 1 calc R . . C4 C 0.4330(9) -0.0908(7) 0.2660(6) 0.028(2) Uani 1 1 d . . . H2 H 0.4776 -0.1452 0.2467 0.033 Uiso 1 1 calc R . . C5 C 0.3937(10) -0.1072(9) 0.3461(8) 0.037(3) Uani 1 1 d . . . C6 C 0.3208(9) -0.0235(7) 0.3709(6) 0.027(2) Uani 1 1 d . . . H3 H 0.2868 -0.0322 0.4241 0.033 Uiso 1 1 calc R . . C7 C 0.4122(11) -0.2071(7) 0.4008(8) 0.038(3) Uani 1 1 d . . . H4 H 0.3841 -0.2447 0.3769 0.057 Uiso 1 1 calc R . . H5 H 0.3686 -0.2032 0.4521 0.057 Uiso 1 1 calc R . . H6 H 0.4962 -0.2393 0.4094 0.057 Uiso 1 1 calc R . . C8 C 0.2645(8) 0.1741(6) 0.4472(5) 0.0148(17) Uani 1 1 d . . . H7 H 0.3276 0.2054 0.4303 0.018 Uiso 1 1 calc R . . C9 C 0.3234(8) 0.0766(7) 0.5050(6) 0.023(2) Uani 1 1 d . . . H8 H 0.3857 0.0352 0.4759 0.028 Uiso 1 1 calc R . . H9 H 0.2649 0.0428 0.5299 0.028 Uiso 1 1 calc R . . C10 C 0.3769(9) 0.0939(7) 0.5700(6) 0.025(2) Uani 1 1 d . . . H10 H 0.4130 0.0307 0.6088 0.030 Uiso 1 1 calc R . . H11 H 0.4396 0.1230 0.5450 0.030 Uiso 1 1 calc R . . C11 C 0.2854(9) 0.1604(8) 0.6134(6) 0.027(2) Uani 1 1 d . . . H12 H 0.3238 0.1732 0.6523 0.032 Uiso 1 1 calc R . . H13 H 0.2277 0.1279 0.6435 0.032 Uiso 1 1 calc R . . C12 C 0.2222(9) 0.2558(7) 0.5562(6) 0.026(2) Uani 1 1 d . . . H14 H 0.1589 0.2953 0.5862 0.031 Uiso 1 1 calc R . . H15 H 0.2781 0.2923 0.5317 0.031 Uiso 1 1 calc R . . C13 C 0.1700(9) 0.2416(7) 0.4912(6) 0.023(2) Uani 1 1 d . . . H16 H 0.1353 0.3055 0.4526 0.028 Uiso 1 1 calc R . . H17 H 0.1065 0.2130 0.5147 0.028 Uiso 1 1 calc R . . C14 C 0.0641(9) 0.1678(8) 0.3766(6) 0.027(2) Uani 1 1 d . . . H18 H 0.0650 0.1215 0.4312 0.032 Uiso 0.517(15) 1 calc PR A 1 H19 H 0.0199 0.2311 0.3889 0.032 Uiso 0.483(15) 1 calc PR A 2 C15 C -0.0304(18) 0.2551(15) 0.3776(12) 0.028(5) Uiso 0.517(15) 1 d P A 1 C16 C -0.146(2) 0.2316(17) 0.4063(14) 0.037(6) Uiso 0.517(15) 1 d P A 1 C17 C -0.175(3) 0.184(2) 0.352(2) 0.054(8) Uiso 0.517(15) 1 d P A 1 C18 C -0.0736(18) 0.0924(15) 0.3420(13) 0.030(5) Uiso 0.517(15) 1 d P A 1 C19 C 0.0426(16) 0.1172(14) 0.3139(11) 0.021(4) Uiso 0.517(15) 1 d P A 1 C20 C -0.0019(18) 0.1787(15) 0.3058(12) 0.022(5) Uiso 0.483(15) 1 d P A 2 C21 C -0.144(2) 0.1960(17) 0.3275(15) 0.026(5) Uiso 0.483(15) 1 d P A 2 C22 C -0.162(2) 0.118(2) 0.3995(17) 0.042(6) Uiso 0.483(15) 1 d P A 2 C23 C -0.097(2) 0.1173(16) 0.4719(14) 0.030(5) Uiso 0.483(15) 1 d P A 2 C24 C 0.0345(19) 0.0978(15) 0.4527(13) 0.026(5) Uiso 0.483(15) 1 d P A 2 C25 C 0.4224(9) 0.1955(8) 0.1318(6) 0.030(2) Uani 1 1 d . . . H20 H 0.4857 0.1787 0.1669 0.044 Uiso 1 1 calc R . . H21 H 0.4055 0.2634 0.0997 0.044 Uiso 1 1 calc R . . H22 H 0.4466 0.1530 0.0964 0.044 Uiso 1 1 calc R . . C26 C 0.2264(10) 0.1902(7) 0.1284(7) 0.032(3) Uani 1 1 d . . . H23 H 0.1597 0.1734 0.1612 0.048 Uiso 1 1 calc R . . H24 H 0.2623 0.1453 0.0952 0.048 Uiso 1 1 calc R . . H25 H 0.1990 0.2570 0.0940 0.048 Uiso 1 1 calc R . . C27 C 0.0573(9) 0.7164(7) 0.0645(5) 0.0204(19) Uani 1 1 d . . . C28 C 0.1228(9) 0.6650(7) 0.0097(6) 0.022(2) Uani 1 1 d . . . C29 C 0.1229(9) 0.7116(8) -0.0713(6) 0.027(2) Uani 1 1 d . . . H26 H 0.1653 0.6763 -0.1084 0.032 Uiso 1 1 calc R . . C30 C 0.0604(9) 0.8108(8) -0.0986(6) 0.029(2) Uani 1 1 d . . . H27 H 0.0605 0.8422 -0.1543 0.035 Uiso 1 1 calc R . . C31 C -0.0016(9) 0.8643(7) -0.0456(6) 0.023(2) Uani 1 1 d . . . C32 C -0.0039(9) 0.8153(7) 0.0350(6) 0.024(2) Uani 1 1 d . . . H28 H -0.0489 0.8504 0.0717 0.029 Uiso 1 1 calc R . . C33 C -0.0662(11) 0.9712(8) -0.0760(7) 0.039(3) Uani 1 1 d . . . H29 H -0.1199 0.9815 -0.1160 0.059 Uiso 1 1 calc R . . H30 H -0.0096 1.0060 -0.1004 0.059 Uiso 1 1 calc R . . H31 H -0.1112 0.9958 -0.0314 0.059 Uiso 1 1 calc R . . C34 C 0.0820(8) 0.7068(7) 0.2314(6) 0.022(2) Uani 1 1 d . . . H32 H 0.0976 0.6572 0.2844 0.026 Uiso 1 1 calc R . . C35 C 0.1975(9) 0.7290(8) 0.2022(7) 0.030(2) Uani 1 1 d . . . H33 H 0.1860 0.7829 0.1522 0.035 Uiso 1 1 calc R . . H34 H 0.2582 0.6709 0.1905 0.035 Uiso 1 1 calc R . . C36 C 0.2397(10) 0.7575(9) 0.2657(8) 0.037(3) Uani 1 1 d . . . H35 H 0.2580 0.7013 0.3140 0.044 Uiso 1 1 calc R . . H36 H 0.3129 0.7736 0.2448 0.044 Uiso 1 1 calc R . . C37 C 0.1490(10) 0.8434(8) 0.2886(7) 0.035(3) Uani 1 1 d . . . H37 H 0.1399 0.9024 0.2427 0.042 Uiso 1 1 calc R . . H38 H 0.1758 0.8547 0.3336 0.042 Uiso 1 1 calc R . . C38 C 0.0303(10) 0.8257(8) 0.3129(7) 0.032(2) Uani 1 1 d . . . H39 H -0.0290 0.8855 0.3226 0.038 Uiso 1 1 calc R . . H40 H 0.0370 0.7731 0.3636 0.038 Uiso 1 1 calc R . . C39 C -0.0120(9) 0.7975(7) 0.2496(6) 0.028(2) Uani 1 1 d . . . H41 H -0.0265 0.8522 0.2002 0.033 Uiso 1 1 calc R . . H42 H -0.0866 0.7835 0.2694 0.033 Uiso 1 1 calc R . . C40 C -0.1168(8) 0.6703(7) 0.1853(6) 0.020(2) Uani 1 1 d . . . H43 H -0.1542 0.7407 0.1831 0.024 Uiso 1 1 calc R . . C41 C -0.1467(9) 0.6119(8) 0.2666(6) 0.029(2) Uani 1 1 d . . . H44 H -0.1160 0.6276 0.3075 0.035 Uiso 1 1 calc R . . H45 H -0.1081 0.5418 0.2711 0.035 Uiso 1 1 calc R . . C42 C -0.2817(9) 0.6326(9) 0.2832(7) 0.038(3) Uani 1 1 d . . . H46 H -0.2978 0.5902 0.3361 0.045 Uiso 1 1 calc R . . H47 H -0.3200 0.7012 0.2841 0.045 Uiso 1 1 calc R . . C43 C -0.3311(11) 0.6138(10) 0.2200(9) 0.047(3) Uani 1 1 d . . . H48 H -0.4175 0.6310 0.2297 0.056 Uiso 1 1 calc R . . H49 H -0.2991 0.5436 0.2234 0.056 Uiso 1 1 calc R . . C44 C -0.3025(10) 0.6717(10) 0.1368(8) 0.042(3) Uani 1 1 d . . . H50 H -0.3417 0.7420 0.1312 0.050 Uiso 1 1 calc R . . H51 H -0.3329 0.6542 0.0969 0.050 Uiso 1 1 calc R . . C45 C -0.1683(9) 0.6514(8) 0.1203(7) 0.032(2) Uani 1 1 d . . . H52 H -0.1299 0.5829 0.1191 0.038 Uiso 1 1 calc R . . H53 H -0.1524 0.6939 0.0674 0.038 Uiso 1 1 calc R . . C46 C 0.3180(9) 0.5519(8) 0.0201(7) 0.034(3) Uani 1 1 d . . . H54 H 0.3334 0.5758 -0.0376 0.052 Uiso 1 1 calc R . . H55 H 0.3656 0.4833 0.0389 0.052 Uiso 1 1 calc R . . H56 H 0.3386 0.5903 0.0475 0.052 Uiso 1 1 calc R . . C47 C 0.1631(11) 0.5023(8) -0.0051(6) 0.031(2) Uani 1 1 d . . . H57 H 0.0787 0.5114 0.0024 0.047 Uiso 1 1 calc R . . H58 H 0.2072 0.4334 0.0165 0.047 Uiso 1 1 calc R . . H59 H 0.1849 0.5235 -0.0622 0.047 Uiso 1 1 calc R . . C48 C 0.5116(8) 0.3591(8) 0.1982(6) 0.023(2) Uani 1 1 d . . . H60 H 0.4683 0.4219 0.1631 0.035 Uiso 1 1 calc R . . H61 H 0.5484 0.3124 0.1668 0.035 Uiso 1 1 calc R . . H62 H 0.5724 0.3674 0.2230 0.035 Uiso 1 1 calc R . . C49 C 0.3493(8) 0.3939(7) 0.3477(6) 0.022(2) Uani 1 1 d . . . C50 C 0.2255(9) 0.4364(7) 0.3470(5) 0.0197(19) Uani 1 1 d . . . C51 C 0.1672(9) 0.4934(7) 0.3986(6) 0.024(2) Uani 1 1 d . . . H63 H 0.0838 0.5187 0.4003 0.029 Uiso 1 1 calc R . . C52 C 0.2276(9) 0.5145(7) 0.4480(6) 0.022(2) Uani 1 1 d . . . C53 C 0.3486(10) 0.4774(8) 0.4445(7) 0.033(3) Uani 1 1 d . . . H64 H 0.3908 0.4925 0.4767 0.039 Uiso 1 1 calc R . . C54 C 0.4108(9) 0.4186(7) 0.3951(6) 0.026(2) Uani 1 1 d . . . C55 C 0.1577(8) 0.4200(6) 0.2924(5) 0.0190(19) Uani 1 1 d . . . H65 H 0.0759 0.4232 0.3148 0.023 Uiso 1 1 calc R . . C56 C 0.5443(9) 0.3822(9) 0.3927(7) 0.033(3) Uani 1 1 d . . . H66 H 0.5709 0.4013 0.4327 0.050 Uiso 1 1 calc R . . H67 H 0.5756 0.4107 0.3394 0.050 Uiso 1 1 calc R . . H68 H 0.5725 0.3111 0.4043 0.050 Uiso 1 1 calc R . . C57 C 0.1623(11) 0.5756(9) 0.5039(7) 0.038(3) Uani 1 1 d . . . H69 H 0.1597 0.5333 0.5585 0.056 Uiso 1 1 calc R . . H70 H 0.0820 0.6118 0.4873 0.056 Uiso 1 1 calc R . . H71 H 0.2028 0.6215 0.5024 0.056 Uiso 1 1 calc R . . C58 C 0.7072(10) 0.0563(9) 0.1117(7) 0.039(3) Uani 1 1 d . . . C59 C 0.6906(10) 0.1434(9) 0.0507(8) 0.038(3) Uani 1 1 d . . . H72 H 0.7093 0.1952 0.0587 0.045 Uiso 1 1 calc R . . C60 C 0.6476(11) 0.1559(13) -0.0212(9) 0.056(4) Uani 1 1 d . . . H73 H 0.6343 0.2162 -0.0616 0.067 Uiso 1 1 calc R . . C61 C 0.6247(13) 0.0800(15) -0.0331(11) 0.066(5) Uani 1 1 d . . . H74 H 0.5953 0.0876 -0.0822 0.079 Uiso 1 1 calc R . . C62 C 0.6439(14) -0.0085(15) 0.0258(14) 0.080(6) Uani 1 1 d . . . H75 H 0.6283 -0.0610 0.0167 0.096 Uiso 1 1 calc R . . C63 C 0.6858(12) -0.0198(11) 0.0974(11) 0.057(4) Uani 1 1 d . . . H76 H 0.7000 -0.0805 0.1372 0.068 Uiso 1 1 calc R . . C64 C 0.7438(13) 0.0450(12) 0.1921(8) 0.059(4) Uani 1 1 d . . . H77 H 0.6820 0.0323 0.2330 0.089 Uiso 1 1 calc R . . H78 H 0.7565 0.1049 0.1922 0.089 Uiso 1 1 calc R . . H79 H 0.8169 -0.0096 0.2038 0.089 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 0.01615(18) 0.01535(18) 0.01538(19) -0.00641(14) -0.00089(13) -0.00245(14) Ir2 0.02006(19) 0.01784(18) 0.01563(19) -0.00516(14) -0.00170(14) -0.00461(15) Cl1 0.0225(11) 0.0264(11) 0.0256(12) -0.0082(9) -0.0062(9) -0.0056(10) Cl2 0.0222(12) 0.0291(12) 0.0380(15) -0.0096(11) -0.0028(10) -0.0002(11) P1 0.0171(11) 0.0173(11) 0.0160(11) -0.0079(9) -0.0014(9) -0.0030(9) P2 0.0202(12) 0.0172(11) 0.0166(11) -0.0046(9) -0.0017(9) -0.0041(10) Si1 0.0192(13) 0.0210(12) 0.0212(13) -0.0092(10) 0.0014(10) -0.0057(11) N1 0.025(4) 0.020(4) 0.016(4) -0.007(3) -0.001(3) -0.008(3) N2 0.032(5) 0.020(4) 0.014(4) -0.001(3) 0.000(3) -0.013(4) C2 0.029(5) 0.023(5) 0.015(4) -0.011(4) 0.000(4) -0.009(4) C3 0.031(6) 0.029(5) 0.029(6) -0.017(4) 0.007(4) -0.007(5) C4 0.028(5) 0.023(5) 0.027(5) -0.011(4) 0.003(4) -0.001(4) C5 0.035(6) 0.040(6) 0.045(7) -0.012(5) -0.025(5) -0.012(5) C6 0.032(6) 0.021(5) 0.029(6) -0.015(4) -0.011(4) 0.001(4) C7 0.047(7) 0.018(5) 0.046(7) -0.002(5) -0.023(6) -0.002(5) C8 0.019(4) 0.020(4) 0.006(4) -0.004(3) -0.002(3) -0.007(4) C9 0.017(5) 0.025(5) 0.027(5) -0.012(4) -0.007(4) 0.001(4) C10 0.024(5) 0.027(5) 0.019(5) -0.006(4) -0.005(4) -0.003(4) C11 0.035(6) 0.034(5) 0.016(5) -0.009(4) -0.008(4) -0.011(5) C12 0.032(5) 0.028(5) 0.019(5) -0.012(4) -0.001(4) -0.005(4) C13 0.024(5) 0.017(4) 0.021(5) -0.003(4) 0.001(4) 0.000(4) C14 0.027(5) 0.042(6) 0.017(5) -0.004(4) -0.003(4) -0.022(5) C25 0.031(6) 0.029(5) 0.030(6) -0.022(5) 0.010(4) -0.005(5) C26 0.042(6) 0.023(5) 0.030(6) -0.011(4) -0.015(5) 0.000(5) C27 0.028(5) 0.025(5) 0.010(4) 0.000(4) -0.005(4) -0.013(4) C28 0.025(5) 0.025(5) 0.018(5) -0.001(4) -0.004(4) -0.013(4) C29 0.028(5) 0.036(6) 0.019(5) -0.009(4) 0.000(4) -0.011(5) C30 0.034(6) 0.035(6) 0.018(5) 0.001(4) -0.007(4) -0.014(5) C31 0.026(5) 0.022(5) 0.025(5) 0.000(4) -0.005(4) -0.016(4) C32 0.028(5) 0.021(5) 0.024(5) -0.008(4) -0.001(4) -0.006(4) C33 0.048(7) 0.023(5) 0.035(6) 0.003(5) -0.011(5) -0.005(5) C34 0.022(5) 0.019(4) 0.019(5) 0.000(4) -0.003(4) -0.003(4) C35 0.034(6) 0.028(5) 0.036(6) -0.014(5) 0.005(5) -0.020(5) C36 0.034(6) 0.042(7) 0.045(7) -0.020(6) -0.001(5) -0.019(5) C37 0.042(7) 0.027(5) 0.044(7) -0.014(5) -0.008(5) -0.015(5) C38 0.034(6) 0.034(6) 0.032(6) -0.020(5) 0.000(5) -0.008(5) C39 0.033(6) 0.023(5) 0.028(5) -0.016(4) 0.000(4) -0.004(4) C40 0.012(4) 0.020(4) 0.030(5) -0.015(4) -0.005(4) 0.002(4) C41 0.019(5) 0.038(6) 0.029(6) -0.009(5) -0.001(4) -0.008(5) C42 0.025(5) 0.047(7) 0.036(7) -0.008(5) 0.005(5) -0.012(5) C43 0.027(6) 0.051(8) 0.069(10) -0.020(7) -0.006(6) -0.016(6) C44 0.030(6) 0.049(7) 0.050(8) -0.018(6) -0.016(5) -0.007(6) C45 0.030(6) 0.030(5) 0.036(6) -0.009(5) -0.012(5) -0.006(5) C46 0.028(6) 0.035(6) 0.026(6) 0.003(5) 0.002(4) -0.005(5) C47 0.050(7) 0.031(5) 0.014(5) -0.006(4) -0.005(4) -0.013(5) C48 0.010(4) 0.034(5) 0.031(5) -0.009(4) 0.006(4) -0.015(4) C49 0.021(5) 0.023(5) 0.022(5) -0.009(4) 0.000(4) -0.006(4) C50 0.030(5) 0.019(4) 0.012(4) -0.004(3) -0.006(4) -0.009(4) C51 0.030(5) 0.020(4) 0.018(5) -0.005(4) 0.000(4) -0.002(4) C52 0.031(5) 0.017(4) 0.018(5) -0.005(4) -0.003(4) -0.005(4) C53 0.044(7) 0.028(5) 0.028(6) -0.013(4) -0.010(5) -0.006(5) C54 0.026(5) 0.028(5) 0.024(5) -0.005(4) -0.004(4) -0.009(4) C55 0.018(4) 0.016(4) 0.016(4) -0.001(3) -0.002(3) 0.000(4) C56 0.025(5) 0.045(7) 0.035(6) -0.018(5) -0.009(5) -0.009(5) C57 0.044(7) 0.038(6) 0.027(6) -0.019(5) -0.002(5) -0.001(5) C58 0.030(6) 0.042(6) 0.035(6) -0.013(5) 0.012(5) -0.005(5) C59 0.028(6) 0.042(7) 0.045(7) -0.014(6) 0.007(5) -0.015(5) C60 0.036(7) 0.092(12) 0.040(8) -0.022(8) 0.011(6) -0.022(8) C61 0.052(9) 0.113(15) 0.063(11) -0.058(11) 0.014(8) -0.042(10) C62 0.054(10) 0.091(14) 0.134(19) -0.090(14) 0.042(11) -0.041(10) C63 0.050(8) 0.049(8) 0.081(12) -0.039(8) 0.028(8) -0.024(7) C64 0.055(9) 0.067(10) 0.038(8) -0.013(7) 0.000(6) -0.002(8) _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 C55 2.073(9) . ? Ir1 P1 2.257(2) . ? Ir1 Si1 2.281(3) . ? Ir1 N1 2.297(8) . ? Ir1 Cl1 2.668(2) . ? Ir1 Ir2 2.7155(5) . ? Ir2 C55 2.075(9) . ? Ir2 P2 2.207(2) . ? Ir2 N2 2.294(8) . ? Ir2 Cl1 2.581(3) . ? Cl2 Si1 2.150(4) . ? P1 C1 1.848(9) . ? P1 C14 1.868(10) . ? P1 C8 1.868(8) . ? P2 C27 1.821(9) . ? P2 C34 1.846(10) . ? P2 C40 1.856(9) . ? Si1 C49 1.880(10) . ? Si1 C48 1.929(10) . ? N1 C26 1.488(12) . ? N1 C25 1.488(13) . ? N1 C2 1.495(12) . ? N2 C28 1.472(12) . ? N2 C46 1.485(13) . ? N2 C47 1.496(13) . ? C1 C6 1.369(14) . ? C1 C2 1.420(13) . ? C2 C3 1.401(13) . ? C3 C4 1.394(15) . ? C3 H1 0.9500 . ? C4 C5 1.388(16) . ? C4 H2 0.9500 . ? C5 C6 1.429(15) . ? C5 C7 1.490(16) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C9 1.519(12) . ? C8 C13 1.538(12) . ? C8 H7 1.0000 . ? C9 C10 1.538(13) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.509(13) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.510(13) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.503(13) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C15 1.43(2) . ? C14 C24 1.51(2) . ? C14 C20 1.53(2) . ? C14 C19 1.63(2) . ? C14 H18 1.0000 . ? C14 H19 1.0000 . ? C15 C16 1.54(3) . ? C16 C17 1.52(4) . ? C17 C18 1.54(4) . ? C18 C19 1.56(3) . ? C20 C21 1.65(3) . ? C21 C22 1.49(4) . ? C22 C23 1.60(3) . ? C23 C24 1.53(3) . ? C25 H20 0.9800 . ? C25 H21 0.9800 . ? C25 H22 0.9800 . ? C26 H23 0.9800 . ? C26 H24 0.9800 . ? C26 H25 0.9800 . ? C27 C32 1.397(13) . ? C27 C28 1.404(14) . ? C28 C29 1.383(13) . ? C29 C30 1.400(15) . ? C29 H26 0.9500 . ? C30 C31 1.388(15) . ? C30 H27 0.9500 . ? C31 C32 1.384(14) . ? C31 C33 1.504(14) . ? C32 H28 0.9500 . ? C33 H29 0.9800 . ? C33 H30 0.9800 . ? C33 H31 0.9800 . ? C34 C35 1.532(14) . ? C34 C39 1.542(13) . ? C34 H32 1.0000 . ? C35 C36 1.538(15) . ? C35 H33 0.9900 . ? C35 H34 0.9900 . ? C36 C37 1.508(15) . ? C36 H35 0.9900 . ? C36 H36 0.9900 . ? C37 C38 1.530(16) . ? C37 H37 0.9900 . ? C37 H38 0.9900 . ? C38 C39 1.532(14) . ? C38 H39 0.9900 . ? C38 H40 0.9900 . ? C39 H41 0.9900 . ? C39 H42 0.9900 . ? C40 C41 1.497(14) . ? C40 C45 1.538(13) . ? C40 H43 1.0000 . ? C41 C42 1.556(14) . ? C41 H44 0.9900 . ? C41 H45 0.9900 . ? C42 C43 1.494(17) . ? C42 H46 0.9900 . ? C42 H47 0.9900 . ? C43 C44 1.513(19) . ? C43 H48 0.9900 . ? C43 H49 0.9900 . ? C44 C45 1.547(16) . ? C44 H50 0.9900 . ? C44 H51 0.9900 . ? C45 H52 0.9900 . ? C45 H53 0.9900 . ? C46 H54 0.9800 . ? C46 H55 0.9800 . ? C46 H56 0.9800 . ? C47 H57 0.9800 . ? C47 H58 0.9800 . ? C47 H59 0.9800 . ? C48 H60 0.9800 . ? C48 H61 0.9800 . ? C48 H62 0.9800 . ? C49 C54 1.415(14) . ? C49 C50 1.418(13) . ? C50 C51 1.394(13) . ? C50 C55 1.493(13) . ? C51 C52 1.399(14) . ? C51 H63 0.9500 . ? C52 C53 1.379(15) . ? C52 C57 1.509(13) . ? C53 C54 1.393(14) . ? C53 H64 0.9500 . ? C54 C56 1.520(14) . ? C55 H65 1.0000 . ? C56 H66 0.9800 . ? C56 H67 0.9800 . ? C56 H68 0.9800 . ? C57 H69 0.9800 . ? C57 H70 0.9800 . ? C57 H71 0.9800 . ? C58 C63 1.380(19) . ? C58 C59 1.398(17) . ? C58 C64 1.497(18) . ? C59 C60 1.385(18) . ? C59 H72 0.9500 . ? C60 C61 1.37(2) . ? C60 H73 0.9500 . ? C61 C62 1.39(3) . ? C61 H74 0.9500 . ? C62 C63 1.38(3) . ? C62 H75 0.9500 . ? C63 H76 0.9500 . ? C64 H77 0.9800 . ? C64 H78 0.9800 . ? C64 H79 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 C55 Ir1 P1 99.9(3) . . ? C55 Ir1 Si1 83.0(3) . . ? P1 Ir1 Si1 97.75(9) . . ? C55 Ir1 N1 174.4(3) . . ? P1 Ir1 N1 83.7(2) . . ? Si1 Ir1 N1 100.9(2) . . ? C55 Ir1 Cl1 77.0(3) . . ? P1 Ir1 Cl1 108.64(8) . . ? Si1 Ir1 Cl1 149.08(9) . . ? N1 Ir1 Cl1 97.9(2) . . ? C55 Ir1 Ir2 49.1(2) . . ? P1 Ir1 Ir2 146.24(6) . . ? Si1 Ir1 Ir2 91.81(7) . . ? N1 Ir1 Ir2 126.24(19) . . ? Cl1 Ir1 Ir2 57.28(5) . . ? C55 Ir2 P2 105.1(2) . . ? C55 Ir2 N2 170.6(3) . . ? P2 Ir2 N2 84.2(2) . . ? C55 Ir2 Cl1 79.0(3) . . ? P2 Ir2 Cl1 108.47(8) . . ? N2 Ir2 Cl1 99.7(2) . . ? C55 Ir2 Ir1 49.1(2) . . ? P2 Ir2 Ir1 151.65(7) . . ? N2 Ir2 Ir1 122.2(2) . . ? Cl1 Ir2 Ir1 60.44(5) . . ? Ir2 Cl1 Ir1 62.28(5) . . ? C1 P1 C14 102.4(5) . . ? C1 P1 C8 109.7(4) . . ? C14 P1 C8 104.7(4) . . ? C1 P1 Ir1 104.6(3) . . ? C14 P1 Ir1 118.4(3) . . ? C8 P1 Ir1 116.0(3) . . ? C27 P2 C34 107.8(4) . . ? C27 P2 C40 101.9(4) . . ? C34 P2 C40 105.7(4) . . ? C27 P2 Ir2 104.8(3) . . ? C34 P2 Ir2 115.5(3) . . ? C40 P2 Ir2 119.7(3) . . ? C49 Si1 C48 108.7(5) . . ? C49 Si1 Cl2 109.3(3) . . ? C48 Si1 Cl2 98.8(3) . . ? C49 Si1 Ir1 104.0(3) . . ? C48 Si1 Ir1 119.1(3) . . ? Cl2 Si1 Ir1 116.71(15) . . ? C26 N1 C25 109.2(8) . . ? C26 N1 C2 108.1(8) . . ? C25 N1 C2 110.2(8) . . ? C26 N1 Ir1 108.7(6) . . ? C25 N1 Ir1 109.0(6) . . ? C2 N1 Ir1 111.5(5) . . ? C28 N2 C46 108.1(8) . . ? C28 N2 C47 111.2(7) . . ? C46 N2 C47 108.0(9) . . ? C28 N2 Ir2 112.6(6) . . ? C46 N2 Ir2 108.0(6) . . ? C47 N2 Ir2 108.8(6) . . ? C6 C1 C2 120.0(9) . . ? C6 C1 P1 124.4(8) . . ? C2 C1 P1 115.5(7) . . ? C3 C2 C1 118.8(9) . . ? C3 C2 N1 119.1(9) . . ? C1 C2 N1 122.0(8) . . ? C4 C3 C2 119.7(10) . . ? C4 C3 H1 120.1 . . ? C2 C3 H1 120.1 . . ? C5 C4 C3 122.8(10) . . ? C5 C4 H2 118.6 . . ? C3 C4 H2 118.6 . . ? C4 C5 C6 116.3(10) . . ? C4 C5 C7 122.2(11) . . ? C6 C5 C7 121.0(12) . . ? C1 C6 C5 122.1(11) . . ? C1 C6 H3 118.9 . . ? C5 C6 H3 118.9 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C9 C8 C13 111.1(7) . . ? C9 C8 P1 120.9(6) . . ? C13 C8 P1 111.6(6) . . ? C9 C8 H7 103.7 . . ? C13 C8 H7 103.7 . . ? P1 C8 H7 103.7 . . ? C8 C9 C10 109.0(8) . . ? C8 C9 H8 109.9 . . ? C10 C9 H8 109.9 . . ? C8 C9 H9 109.9 . . ? C10 C9 H9 109.9 . . ? H8 C9 H9 108.3 . . ? C11 C10 C9 111.6(8) . . ? C11 C10 H10 109.3 . . ? C9 C10 H10 109.3 . . ? C11 C10 H11 109.3 . . ? C9 C10 H11 109.3 . . ? H10 C10 H11 108.0 . . ? C10 C11 C12 111.5(8) . . ? C10 C11 H12 109.3 . . ? C12 C11 H12 109.3 . . ? C10 C11 H13 109.3 . . ? C12 C11 H13 109.3 . . ? H12 C11 H13 108.0 . . ? C13 C12 C11 112.3(8) . . ? C13 C12 H14 109.1 . . ? C11 C12 H14 109.1 . . ? C13 C12 H15 109.1 . . ? C11 C12 H15 109.1 . . ? H14 C12 H15 107.9 . . ? C12 C13 C8 110.6(8) . . ? C12 C13 H16 109.5 . . ? C8 C13 H16 109.5 . . ? C12 C13 H17 109.5 . . ? C8 C13 H17 109.5 . . ? H16 C13 H17 108.1 . . ? C15 C14 C24 101.3(13) . . ? C15 C14 C20 79.6(12) . . ? C24 C14 C20 112.9(13) . . ? C15 C14 C19 110.6(12) . . ? C24 C14 C19 97.4(12) . . ? C20 C14 C19 32.2(9) . . ? C15 C14 P1 115.9(11) . . ? C24 C14 P1 122.7(10) . . ? C20 C14 P1 115.4(10) . . ? C19 C14 P1 107.3(9) . . ? C15 C14 H18 107.6 . . ? C24 C14 H18 15.6 . . ? C20 C14 H18 127.6 . . ? C19 C14 H18 107.6 . . ? P1 C14 H18 107.6 . . ? C15 C14 H19 21.8 . . ? C24 C14 H19 100.1 . . ? C20 C14 H19 100.1 . . ? C19 C14 H19 131.9 . . ? P1 C14 H19 100.1 . . ? H18 C14 H19 100.6 . . ? C14 C15 C16 109.8(17) . . ? C17 C16 C15 111(2) . . ? C16 C17 C18 112(2) . . ? C17 C18 C19 110(2) . . ? C18 C19 C14 107.9(14) . . ? C14 C20 C21 113.3(16) . . ? C22 C21 C20 109.9(18) . . ? C21 C22 C23 109(2) . . ? C24 C23 C22 112.0(19) . . ? C14 C24 C23 113.4(16) . . ? N1 C25 H20 109.5 . . ? N1 C25 H21 109.5 . . ? H20 C25 H21 109.5 . . ? N1 C25 H22 109.5 . . ? H20 C25 H22 109.5 . . ? H21 C25 H22 109.5 . . ? N1 C26 H23 109.5 . . ? N1 C26 H24 109.5 . . ? H23 C26 H24 109.5 . . ? N1 C26 H25 109.5 . . ? H23 C26 H25 109.5 . . ? H24 C26 H25 109.5 . . ? C32 C27 C28 118.3(8) . . ? C32 C27 P2 123.9(8) . . ? C28 C27 P2 117.4(7) . . ? C29 C28 C27 120.1(9) . . ? C29 C28 N2 119.4(9) . . ? C27 C28 N2 120.5(8) . . ? C28 C29 C30 120.0(10) . . ? C28 C29 H26 120.0 . . ? C30 C29 H26 120.0 . . ? C31 C30 C29 121.2(9) . . ? C31 C30 H27 119.4 . . ? C29 C30 H27 119.4 . . ? C32 C31 C30 117.8(9) . . ? C32 C31 C33 121.8(10) . . ? C30 C31 C33 120.4(9) . . ? C31 C32 C27 122.7(9) . . ? C31 C32 H28 118.7 . . ? C27 C32 H28 118.7 . . ? C31 C33 H29 109.5 . . ? C31 C33 H30 109.5 . . ? H29 C33 H30 109.5 . . ? C31 C33 H31 109.5 . . ? H29 C33 H31 109.5 . . ? H30 C33 H31 109.5 . . ? C35 C34 C39 109.2(9) . . ? C35 C34 P2 112.5(7) . . ? C39 C34 P2 118.4(7) . . ? C35 C34 H32 105.2 . . ? C39 C34 H32 105.2 . . ? P2 C34 H32 105.2 . . ? C34 C35 C36 110.7(9) . . ? C34 C35 H33 109.5 . . ? C36 C35 H33 109.5 . . ? C34 C35 H34 109.5 . . ? C36 C35 H34 109.5 . . ? H33 C35 H34 108.1 . . ? C37 C36 C35 112.1(9) . . ? C37 C36 H35 109.2 . . ? C35 C36 H35 109.2 . . ? C37 C36 H36 109.2 . . ? C35 C36 H36 109.2 . . ? H35 C36 H36 107.9 . . ? C36 C37 C38 110.9(9) . . ? C36 C37 H37 109.5 . . ? C38 C37 H37 109.5 . . ? C36 C37 H38 109.5 . . ? C38 C37 H38 109.5 . . ? H37 C37 H38 108.0 . . ? C37 C38 C39 112.9(9) . . ? C37 C38 H39 109.0 . . ? C39 C38 H39 109.0 . . ? C37 C38 H40 109.0 . . ? C39 C38 H40 109.0 . . ? H39 C38 H40 107.8 . . ? C38 C39 C34 109.6(8) . . ? C38 C39 H41 109.8 . . ? C34 C39 H41 109.8 . . ? C38 C39 H42 109.8 . . ? C34 C39 H42 109.8 . . ? H41 C39 H42 108.2 . . ? C41 C40 C45 110.7(9) . . ? C41 C40 P2 110.9(6) . . ? C45 C40 P2 112.2(7) . . ? C41 C40 H43 107.6 . . ? C45 C40 H43 107.6 . . ? P2 C40 H43 107.6 . . ? C40 C41 C42 111.9(8) . . ? C40 C41 H44 109.2 . . ? C42 C41 H44 109.2 . . ? C40 C41 H45 109.2 . . ? C42 C41 H45 109.2 . . ? H44 C41 H45 107.9 . . ? C43 C42 C41 110.2(10) . . ? C43 C42 H46 109.6 . . ? C41 C42 H46 109.6 . . ? C43 C42 H47 109.6 . . ? C41 C42 H47 109.6 . . ? H46 C42 H47 108.1 . . ? C42 C43 C44 112.3(11) . . ? C42 C43 H48 109.1 . . ? C44 C43 H48 109.1 . . ? C42 C43 H49 109.1 . . ? C44 C43 H49 109.1 . . ? H48 C43 H49 107.9 . . ? C43 C44 C45 111.1(9) . . ? C43 C44 H50 109.4 . . ? C45 C44 H50 109.4 . . ? C43 C44 H51 109.4 . . ? C45 C44 H51 109.4 . . ? H50 C44 H51 108.0 . . ? C40 C45 C44 110.6(9) . . ? C40 C45 H52 109.5 . . ? C44 C45 H52 109.5 . . ? C40 C45 H53 109.5 . . ? C44 C45 H53 109.5 . . ? H52 C45 H53 108.1 . . ? N2 C46 H54 109.5 . . ? N2 C46 H55 109.5 . . ? H54 C46 H55 109.5 . . ? N2 C46 H56 109.5 . . ? H54 C46 H56 109.5 . . ? H55 C46 H56 109.5 . . ? N2 C47 H57 109.5 . . ? N2 C47 H58 109.5 . . ? H57 C47 H58 109.5 . . ? N2 C47 H59 109.5 . . ? H57 C47 H59 109.5 . . ? H58 C47 H59 109.5 . . ? Si1 C48 H60 109.5 . . ? Si1 C48 H61 109.5 . . ? H60 C48 H61 109.5 . . ? Si1 C48 H62 109.5 . . ? H60 C48 H62 109.5 . . ? H61 C48 H62 109.5 . . ? C54 C49 C50 118.7(9) . . ? C54 C49 Si1 130.6(7) . . ? C50 C49 Si1 110.7(7) . . ? C51 C50 C49 119.1(9) . . ? C51 C50 C55 120.2(9) . . ? C49 C50 C55 120.8(8) . . ? C50 C51 C52 122.1(9) . . ? C50 C51 H63 119.0 . . ? C52 C51 H63 119.0 . . ? C53 C52 C51 118.1(9) . . ? C53 C52 C57 120.9(9) . . ? C51 C52 C57 121.0(9) . . ? C52 C53 C54 122.1(10) . . ? C52 C53 H64 119.0 . . ? C54 C53 H64 119.0 . . ? C53 C54 C49 119.8(10) . . ? C53 C54 C56 119.2(10) . . ? C49 C54 C56 121.0(9) . . ? C50 C55 Ir1 118.0(6) . . ? C50 C55 Ir2 117.5(7) . . ? Ir1 C55 Ir2 81.8(3) . . ? C50 C55 H65 112.1 . . ? Ir1 C55 H65 112.1 . . ? Ir2 C55 H65 112.1 . . ? C54 C56 H66 109.5 . . ? C54 C56 H67 109.5 . . ? H66 C56 H67 109.5 . . ? C54 C56 H68 109.5 . . ? H66 C56 H68 109.5 . . ? H67 C56 H68 109.5 . . ? C52 C57 H69 109.5 . . ? C52 C57 H70 109.5 . . ? H69 C57 H70 109.5 . . ? C52 C57 H71 109.5 . . ? H69 C57 H71 109.5 . . ? H70 C57 H71 109.5 . . ? C63 C58 C59 118.5(13) . . ? C63 C58 C64 119.7(14) . . ? C59 C58 C64 121.8(13) . . ? C60 C59 C58 121.4(13) . . ? C60 C59 H72 119.3 . . ? C58 C59 H72 119.3 . . ? C61 C60 C59 118.8(16) . . ? C61 C60 H73 120.6 . . ? C59 C60 H73 120.6 . . ? C60 C61 C62 120.9(16) . . ? C60 C61 H74 119.5 . . ? C62 C61 H74 119.5 . . ? C63 C62 C61 119.8(15) . . ? C63 C62 H75 120.1 . . ? C61 C62 H75 120.1 . . ? C62 C63 C58 120.6(16) . . ? C62 C63 H76 119.7 . . ? C58 C63 H76 119.7 . . ? C58 C64 H77 109.5 . . ? C58 C64 H78 109.5 . . ? H77 C64 H78 109.5 . . ? C58 C64 H79 109.5 . . ? H77 C64 H79 109.5 . . ? H78 C64 H79 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 P1 Ir1 Ir2 C55 27.8(4) . . . . ? Si1 Ir1 Ir2 C55 -79.1(4) . . . . ? N1 Ir1 Ir2 C55 176.0(4) . . . . ? Cl1 Ir1 Ir2 C55 101.6(4) . . . . ? C55 Ir1 Ir2 P2 -28.2(4) . . . . ? P1 Ir1 Ir2 P2 -0.38(18) . . . . ? Si1 Ir1 Ir2 P2 -107.24(15) . . . . ? N1 Ir1 Ir2 P2 147.9(3) . . . . ? Cl1 Ir1 Ir2 P2 73.49(15) . . . . ? C55 Ir1 Ir2 N2 175.8(4) . . . . ? P1 Ir1 Ir2 N2 -156.5(3) . . . . ? Si1 Ir1 Ir2 N2 96.7(3) . . . . ? N1 Ir1 Ir2 N2 -8.2(3) . . . . ? Cl1 Ir1 Ir2 N2 -82.6(3) . . . . ? C55 Ir1 Ir2 Cl1 -101.6(4) . . . . ? P1 Ir1 Ir2 Cl1 -73.87(13) . . . . ? Si1 Ir1 Ir2 Cl1 179.27(9) . . . . ? N1 Ir1 Ir2 Cl1 74.4(3) . . . . ? C55 Ir2 Cl1 Ir1 -48.9(2) . . . . ? P2 Ir2 Cl1 Ir1 -151.31(7) . . . . ? N2 Ir2 Cl1 Ir1 121.7(2) . . . . ? C55 Ir1 Cl1 Ir2 49.5(3) . . . . ? P1 Ir1 Cl1 Ir2 145.71(7) . . . . ? Si1 Ir1 Cl1 Ir2 -1.42(18) . . . . ? N1 Ir1 Cl1 Ir2 -128.4(2) . . . . ? C55 Ir1 P1 C1 -172.9(4) . . . . ? Si1 Ir1 P1 C1 -88.8(3) . . . . ? N1 Ir1 P1 C1 11.4(4) . . . . ? Cl1 Ir1 P1 C1 107.6(3) . . . . ? Ir2 Ir1 P1 C1 166.1(3) . . . . ? C55 Ir1 P1 C14 74.0(5) . . . . ? Si1 Ir1 P1 C14 158.1(4) . . . . ? N1 Ir1 P1 C14 -101.7(4) . . . . ? Cl1 Ir1 P1 C14 -5.5(4) . . . . ? Ir2 Ir1 P1 C14 53.0(4) . . . . ? C55 Ir1 P1 C8 -51.9(4) . . . . ? Si1 Ir1 P1 C8 32.2(3) . . . . ? N1 Ir1 P1 C8 132.4(4) . . . . ? Cl1 Ir1 P1 C8 -131.4(3) . . . . ? Ir2 Ir1 P1 C8 -72.9(3) . . . . ? C55 Ir2 P2 C27 175.8(4) . . . . ? N2 Ir2 P2 C27 -2.7(4) . . . . ? Cl1 Ir2 P2 C27 -101.0(3) . . . . ? Ir1 Ir2 P2 C27 -162.5(3) . . . . ? C55 Ir2 P2 C34 57.3(5) . . . . ? N2 Ir2 P2 C34 -121.2(4) . . . . ? Cl1 Ir2 P2 C34 140.6(4) . . . . ? Ir1 Ir2 P2 C34 79.0(4) . . . . ? C55 Ir2 P2 C40 -70.8(5) . . . . ? N2 Ir2 P2 C40 110.7(4) . . . . ? Cl1 Ir2 P2 C40 12.4(4) . . . . ? Ir1 Ir2 P2 C40 -49.1(4) . . . . ? C55 Ir1 Si1 C49 13.2(4) . . . . ? P1 Ir1 Si1 C49 -85.9(3) . . . . ? N1 Ir1 Si1 C49 -170.9(4) . . . . ? Cl1 Ir1 Si1 C49 62.8(4) . . . . ? Ir2 Ir1 Si1 C49 61.6(3) . . . . ? C55 Ir1 Si1 C48 -107.9(5) . . . . ? P1 Ir1 Si1 C48 152.9(4) . . . . ? N1 Ir1 Si1 C48 67.9(4) . . . . ? Cl1 Ir1 Si1 C48 -58.3(4) . . . . ? Ir2 Ir1 Si1 C48 -59.5(4) . . . . ? C55 Ir1 Si1 Cl2 133.7(3) . . . . ? P1 Ir1 Si1 Cl2 34.56(16) . . . . ? N1 Ir1 Si1 Cl2 -50.4(2) . . . . ? Cl1 Ir1 Si1 Cl2 -176.70(13) . . . . ? Ir2 Ir1 Si1 Cl2 -177.90(14) . . . . ? C55 Ir1 N1 C26 -27(4) . . . . ? P1 Ir1 N1 C26 103.7(7) . . . . ? Si1 Ir1 N1 C26 -159.6(6) . . . . ? Cl1 Ir1 N1 C26 -4.3(7) . . . . ? Ir2 Ir1 N1 C26 -59.2(7) . . . . ? C55 Ir1 N1 C25 92(4) . . . . ? P1 Ir1 N1 C25 -137.3(6) . . . . ? Si1 Ir1 N1 C25 -40.5(6) . . . . ? Cl1 Ir1 N1 C25 114.7(6) . . . . ? Ir2 Ir1 N1 C25 59.8(7) . . . . ? C55 Ir1 N1 C2 -146(3) . . . . ? P1 Ir1 N1 C2 -15.3(6) . . . . ? Si1 Ir1 N1 C2 81.4(6) . . . . ? Cl1 Ir1 N1 C2 -123.4(6) . . . . ? Ir2 Ir1 N1 C2 -178.2(5) . . . . ? C55 Ir2 N2 C28 -171.9(19) . . . . ? P2 Ir2 N2 C28 -0.8(6) . . . . ? Cl1 Ir2 N2 C28 107.0(6) . . . . ? Ir1 Ir2 N2 C28 168.0(5) . . . . ? C55 Ir2 N2 C46 -53(2) . . . . ? P2 Ir2 N2 C46 118.5(6) . . . . ? Cl1 Ir2 N2 C46 -133.7(6) . . . . ? Ir1 Ir2 N2 C46 -72.7(7) . . . . ? C55 Ir2 N2 C47 64(2) . . . . ? P2 Ir2 N2 C47 -124.5(6) . . . . ? Cl1 Ir2 N2 C47 -16.7(7) . . . . ? Ir1 Ir2 N2 C47 44.4(7) . . . . ? C14 P1 C1 C6 -64.8(10) . . . . ? C8 P1 C1 C6 46.0(10) . . . . ? Ir1 P1 C1 C6 171.2(8) . . . . ? C14 P1 C1 C2 116.6(8) . . . . ? C8 P1 C1 C2 -132.6(7) . . . . ? Ir1 P1 C1 C2 -7.5(8) . . . . ? C6 C1 C2 C3 0.5(15) . . . . ? P1 C1 C2 C3 179.2(8) . . . . ? C6 C1 C2 N1 175.9(9) . . . . ? P1 C1 C2 N1 -5.4(12) . . . . ? C26 N1 C2 C3 71.6(11) . . . . ? C25 N1 C2 C3 -47.7(12) . . . . ? Ir1 N1 C2 C3 -169.0(8) . . . . ? C26 N1 C2 C1 -103.8(10) . . . . ? C25 N1 C2 C1 136.9(9) . . . . ? Ir1 N1 C2 C1 15.6(11) . . . . ? C1 C2 C3 C4 -1.7(16) . . . . ? N1 C2 C3 C4 -177.3(9) . . . . ? C2 C3 C4 C5 -0.6(17) . . . . ? C3 C4 C5 C6 3.9(16) . . . . ? C3 C4 C5 C7 175.8(11) . . . . ? C2 C1 C6 C5 3.1(15) . . . . ? P1 C1 C6 C5 -175.6(8) . . . . ? C4 C5 C6 C1 -5.2(15) . . . . ? C7 C5 C6 C1 -177.2(10) . . . . ? C1 P1 C8 C9 -24.1(9) . . . . ? C14 P1 C8 C9 85.1(8) . . . . ? Ir1 P1 C8 C9 -142.3(7) . . . . ? C1 P1 C8 C13 -157.6(7) . . . . ? C14 P1 C8 C13 -48.3(8) . . . . ? Ir1 P1 C8 C13 84.2(7) . . . . ? C13 C8 C9 C10 -57.5(10) . . . . ? P1 C8 C9 C10 168.8(7) . . . . ? C8 C9 C10 C11 57.1(11) . . . . ? C9 C10 C11 C12 -55.5(12) . . . . ? C10 C11 C12 C13 54.4(12) . . . . ? C11 C12 C13 C8 -54.6(11) . . . . ? C9 C8 C13 C12 56.9(11) . . . . ? P1 C8 C13 C12 -165.0(7) . . . . ? C1 P1 C14 C15 -160.6(11) . . . . ? C8 P1 C14 C15 84.9(11) . . . . ? Ir1 P1 C14 C15 -46.3(12) . . . . ? C1 P1 C14 C24 74.6(13) . . . . ? C8 P1 C14 C24 -39.9(13) . . . . ? Ir1 P1 C14 C24 -171.1(11) . . . . ? C1 P1 C14 C20 -70.1(11) . . . . ? C8 P1 C14 C20 175.4(11) . . . . ? Ir1 P1 C14 C20 44.3(12) . . . . ? C1 P1 C14 C19 -36.5(9) . . . . ? C8 P1 C14 C19 -151.0(9) . . . . ? Ir1 P1 C14 C19 77.9(9) . . . . ? C24 C14 C15 C16 -40.3(19) . . . . ? C20 C14 C15 C16 71.2(17) . . . . ? C19 C14 C15 C16 62.1(19) . . . . ? P1 C14 C15 C16 -175.5(12) . . . . ? C14 C15 C16 C17 -60(2) . . . . ? C15 C16 C17 C18 55(3) . . . . ? C16 C17 C18 C19 -54(3) . . . . ? C17 C18 C19 C14 54(2) . . . . ? C15 C14 C19 C18 -60.7(18) . . . . ? C24 C14 C19 C18 44.4(16) . . . . ? C20 C14 C19 C18 -78(2) . . . . ? P1 C14 C19 C18 172.0(11) . . . . ? C15 C14 C20 C21 -50.7(17) . . . . ? C24 C14 C20 C21 47(2) . . . . ? C19 C14 C20 C21 113(3) . . . . ? P1 C14 C20 C21 -164.6(13) . . . . ? C14 C20 C21 C22 -53(2) . . . . ? C20 C21 C22 C23 57(2) . . . . ? C21 C22 C23 C24 -60(3) . . . . ? C15 C14 C24 C23 34(2) . . . . ? C20 C14 C24 C23 -49(2) . . . . ? C19 C14 C24 C23 -78.8(18) . . . . ? P1 C14 C24 C23 165.2(13) . . . . ? C22 C23 C24 C14 55(2) . . . . ? C34 P2 C27 C32 -56.8(9) . . . . ? C40 P2 C27 C32 54.2(9) . . . . ? Ir2 P2 C27 C32 179.6(8) . . . . ? C34 P2 C27 C28 130.3(8) . . . . ? C40 P2 C27 C28 -118.7(8) . . . . ? Ir2 P2 C27 C28 6.7(8) . . . . ? C32 C27 C28 C29 -1.9(15) . . . . ? P2 C27 C28 C29 171.4(8) . . . . ? C32 C27 C28 N2 178.3(9) . . . . ? P2 C27 C28 N2 -8.4(12) . . . . ? C46 N2 C28 C29 66.5(11) . . . . ? C47 N2 C28 C29 -51.9(12) . . . . ? Ir2 N2 C28 C29 -174.2(7) . . . . ? C46 N2 C28 C27 -113.7(10) . . . . ? C47 N2 C28 C27 127.9(10) . . . . ? Ir2 N2 C28 C27 5.6(11) . . . . ? C27 C28 C29 C30 1.9(15) . . . . ? N2 C28 C29 C30 -178.2(9) . . . . ? C28 C29 C30 C31 0.4(16) . . . . ? C29 C30 C31 C32 -2.7(15) . . . . ? C29 C30 C31 C33 178.8(10) . . . . ? C30 C31 C32 C27 2.7(15) . . . . ? C33 C31 C32 C27 -178.8(10) . . . . ? C28 C27 C32 C31 -0.4(15) . . . . ? P2 C27 C32 C31 -173.3(8) . . . . ? C27 P2 C34 C35 -49.4(8) . . . . ? C40 P2 C34 C35 -157.9(7) . . . . ? Ir2 P2 C34 C35 67.4(7) . . . . ? C27 P2 C34 C39 79.5(9) . . . . ? C40 P2 C34 C39 -28.9(9) . . . . ? Ir2 P2 C34 C39 -163.6(7) . . . . ? C39 C34 C35 C36 59.1(11) . . . . ? P2 C34 C35 C36 -167.3(7) . . . . ? C34 C35 C36 C37 -57.0(13) . . . . ? C35 C36 C37 C38 52.9(14) . . . . ? C36 C37 C38 C39 -53.4(13) . . . . ? C37 C38 C39 C34 56.4(12) . . . . ? C35 C34 C39 C38 -58.5(11) . . . . ? P2 C34 C39 C38 171.0(7) . . . . ? C27 P2 C40 C41 175.2(7) . . . . ? C34 P2 C40 C41 -72.3(8) . . . . ? Ir2 P2 C40 C41 60.2(8) . . . . ? C27 P2 C40 C45 50.8(8) . . . . ? C34 P2 C40 C45 163.4(7) . . . . ? Ir2 P2 C40 C45 -64.1(8) . . . . ? C45 C40 C41 C42 -56.2(12) . . . . ? P2 C40 C41 C42 178.6(8) . . . . ? C40 C41 C42 C43 56.3(13) . . . . ? C41 C42 C43 C44 -55.6(14) . . . . ? C42 C43 C44 C45 55.9(14) . . . . ? C41 C40 C45 C44 55.3(11) . . . . ? P2 C40 C45 C44 179.8(8) . . . . ? C43 C44 C45 C40 -54.7(13) . . . . ? C48 Si1 C49 C54 -59.7(11) . . . . ? Cl2 Si1 C49 C54 47.2(11) . . . . ? Ir1 Si1 C49 C54 172.5(9) . . . . ? C48 Si1 C49 C50 119.6(7) . . . . ? Cl2 Si1 C49 C50 -133.6(6) . . . . ? Ir1 Si1 C49 C50 -8.3(8) . . . . ? C54 C49 C50 C51 -6.2(14) . . . . ? Si1 C49 C50 C51 174.5(8) . . . . ? C54 C49 C50 C55 174.4(9) . . . . ? Si1 C49 C50 C55 -5.0(12) . . . . ? C49 C50 C51 C52 3.7(15) . . . . ? C55 C50 C51 C52 -176.9(9) . . . . ? C50 C51 C52 C53 0.2(15) . . . . ? C50 C51 C52 C57 -179.4(10) . . . . ? C51 C52 C53 C54 -1.5(16) . . . . ? C57 C52 C53 C54 178.1(11) . . . . ? C52 C53 C54 C49 -1.2(17) . . . . ? C52 C53 C54 C56 178.5(10) . . . . ? C50 C49 C54 C53 5.0(15) . . . . ? Si1 C49 C54 C53 -175.8(9) . . . . ? C50 C49 C54 C56 -174.7(10) . . . . ? Si1 C49 C54 C56 4.5(16) . . . . ? C51 C50 C55 Ir1 -160.9(7) . . . . ? C49 C50 C55 Ir1 18.5(12) . . . . ? C51 C50 C55 Ir2 103.7(9) . . . . ? C49 C50 C55 Ir2 -76.9(10) . . . . ? P1 Ir1 C55 C50 78.4(7) . . . . ? Si1 Ir1 C55 C50 -18.3(7) . . . . ? N1 Ir1 C55 C50 -152(3) . . . . ? Cl1 Ir1 C55 C50 -174.6(7) . . . . ? Ir2 Ir1 C55 C50 -116.8(8) . . . . ? P1 Ir1 C55 Ir2 -164.8(2) . . . . ? Si1 Ir1 C55 Ir2 98.6(3) . . . . ? N1 Ir1 C55 Ir2 -35(4) . . . . ? Cl1 Ir1 C55 Ir2 -57.8(2) . . . . ? P2 Ir2 C55 C50 -76.0(7) . . . . ? N2 Ir2 C55 C50 95(2) . . . . ? Cl1 Ir2 C55 C50 177.6(7) . . . . ? Ir1 Ir2 C55 C50 117.4(8) . . . . ? P2 Ir2 C55 Ir1 166.58(18) . . . . ? N2 Ir2 C55 Ir1 -23(2) . . . . ? Cl1 Ir2 C55 Ir1 60.2(2) . . . . ? C63 C58 C59 C60 3.5(18) . . . . ? C64 C58 C59 C60 -174.7(12) . . . . ? C58 C59 C60 C61 -2.1(19) . . . . ? C59 C60 C61 C62 0(2) . . . . ? C60 C61 C62 C63 1(2) . . . . ? C61 C62 C63 C58 1(2) . . . . ? C59 C58 C63 C62 -2.9(19) . . . . ? C64 C58 C63 C62 175.4(13) . . . . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 27.42 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 1.231 _refine_diff_density_min -2.298 _refine_diff_density_rms 0.366 #===END data_(PcyN-P,N)IrHCl[SiMe2??O(Me)??SiMe2-Si,Si]-(8)?C7H8 _database_code_depnum_ccdc_archive 'CCDC 772165' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H580 Cl Ir N O P Si2, C7 H8' _chemical_formula_sum 'C33 H58 Cl Ir N O P Si2' _chemical_formula_weight 799.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0805(5) _cell_length_b 16.3211(8) _cell_length_c 18.1653(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.365(2) _cell_angle_gamma 90.00 _cell_volume 3578.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8173 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 3.943 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6282 _exptl_absorpt_correction_T_max 0.7698 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31899 _diffrn_reflns_av_R_equivalents 0.1691 _diffrn_reflns_av_sigmaI/netI 0.1100 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8173 _reflns_number_gt 6128 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0607P)^2^+5.5304P] 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 8173 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1335 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.227 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.11612(3) 0.225077(19) 0.129442(16) 0.01323(10) Uani 1 1 d . . . H1 H 0.156(13) 0.181(10) 0.067(8) 0.09(5) Uiso 1 1 d . . . Cl1 Cl 0.00023(19) 0.30190(13) 0.21684(11) 0.0213(4) Uani 1 1 d . . . P1 P 0.27146(19) 0.21150(12) 0.20674(11) 0.0137(4) Uani 1 1 d . . . Si1 Si -0.0129(2) 0.23549(15) 0.03048(12) 0.0188(5) Uani 1 1 d . . . Si2 Si 0.1597(2) 0.33601(15) 0.06137(12) 0.0173(5) Uani 1 1 d . . . O1 O 0.0701(5) 0.3088(4) -0.0171(3) 0.0185(13) Uani 1 1 d . . . N1 N 0.0725(6) 0.1006(4) 0.1826(3) 0.0158(15) Uani 1 1 d . . . C1 C 0.2523(8) 0.1153(5) 0.2548(4) 0.0174(18) Uani 1 1 d . . . C2 C 0.1547(8) 0.0714(5) 0.2390(4) 0.0199(19) Uani 1 1 d . . . C3 C 0.1381(9) -0.0041(5) 0.2738(5) 0.024(2) Uani 1 1 d . . . H2 H 0.0721 -0.0342 0.2633 0.028 Uiso 1 1 calc R . . C4 C 0.2173(9) -0.0345(5) 0.3232(5) 0.028(2) Uani 1 1 d . . . H3 H 0.2042 -0.0853 0.3468 0.033 Uiso 1 1 calc R . . C5 C 0.3160(9) 0.0070(5) 0.3396(4) 0.022(2) Uani 1 1 d . . . C6 C 0.3309(8) 0.0821(6) 0.3059(5) 0.0223(19) Uani 1 1 d . . . H4 H 0.3964 0.1123 0.3177 0.027 Uiso 1 1 calc R . . C7 C 0.4026(9) -0.0298(6) 0.3920(5) 0.031(2) Uani 1 1 d . . . H5 H 0.4595 -0.0569 0.3638 0.046 Uiso 1 1 calc R . . H6 H 0.3677 -0.0699 0.4238 0.046 Uiso 1 1 calc R . . H7 H 0.4367 0.0137 0.4225 0.046 Uiso 1 1 calc R . . C8 C 0.4004(7) 0.1989(5) 0.1555(4) 0.0167(17) Uani 1 1 d . . . H8 H 0.3904 0.2340 0.1106 0.020 Uiso 1 1 calc R . . C9 C 0.4140(8) 0.1113(6) 0.1269(5) 0.0238(19) Uani 1 1 d . . . H9 H 0.4315 0.0742 0.1688 0.029 Uiso 1 1 calc R . . H10 H 0.3434 0.0929 0.1026 0.029 Uiso 1 1 calc R . . C10 C 0.5062(8) 0.1064(7) 0.0720(5) 0.030(2) Uani 1 1 d . . . H11 H 0.5165 0.0486 0.0571 0.036 Uiso 1 1 calc R . . H12 H 0.4847 0.1384 0.0274 0.036 Uiso 1 1 calc R . . C11 C 0.6139(8) 0.1393(6) 0.1053(5) 0.027(2) Uani 1 1 d . . . H13 H 0.6412 0.1021 0.1452 0.032 Uiso 1 1 calc R . . H14 H 0.6700 0.1406 0.0671 0.032 Uiso 1 1 calc R . . C12 C 0.6006(7) 0.2234(6) 0.1360(5) 0.026(2) Uani 1 1 d . . . H15 H 0.5810 0.2617 0.0952 0.031 Uiso 1 1 calc R . . H16 H 0.6720 0.2416 0.1592 0.031 Uiso 1 1 calc R . . C13 C 0.5102(8) 0.2267(6) 0.1934(5) 0.0241(19) Uani 1 1 d . . . H17 H 0.5301 0.1901 0.2354 0.029 Uiso 1 1 calc R . . H18 H 0.5030 0.2832 0.2124 0.029 Uiso 1 1 calc R . . C14 C 0.3094(8) 0.2857(5) 0.2804(4) 0.0169(17) Uani 1 1 d . . . H19 H 0.3875 0.2746 0.2979 0.020 Uiso 1 1 calc R . . C15 C 0.3047(9) 0.3713(5) 0.2469(5) 0.022(2) Uani 1 1 d . . . H20 H 0.2291 0.3815 0.2258 0.027 Uiso 1 1 calc R . . H21 H 0.3567 0.3742 0.2063 0.027 Uiso 1 1 calc R . . C16 C 0.3346(10) 0.4383(6) 0.3038(5) 0.032(2) Uani 1 1 d . . . H22 H 0.4138 0.4333 0.3195 0.038 Uiso 1 1 calc R . . H23 H 0.3233 0.4929 0.2809 0.038 Uiso 1 1 calc R . . C17 C 0.2638(10) 0.4309(6) 0.3705(5) 0.030(2) Uani 1 1 d . . . H24 H 0.1858 0.4434 0.3559 0.036 Uiso 1 1 calc R . . H25 H 0.2889 0.4714 0.4081 0.036 Uiso 1 1 calc R . . C18 C 0.2707(8) 0.3453(6) 0.4034(4) 0.024(2) Uani 1 1 d . . . H26 H 0.2224 0.3421 0.4460 0.029 Uiso 1 1 calc R . . H27 H 0.3478 0.3344 0.4214 0.029 Uiso 1 1 calc R . . C19 C 0.2353(8) 0.2806(5) 0.3469(4) 0.0208(18) Uani 1 1 d . . . H28 H 0.1570 0.2896 0.3306 0.025 Uiso 1 1 calc R . . H29 H 0.2415 0.2255 0.3694 0.025 Uiso 1 1 calc R . . C20 C 0.0652(8) 0.0371(5) 0.1228(5) 0.0219(19) Uani 1 1 d . . . H30 H 0.1345 0.0364 0.0967 0.033 Uiso 1 1 calc R . . H31 H 0.0035 0.0504 0.0881 0.033 Uiso 1 1 calc R . . H32 H 0.0528 -0.0168 0.1447 0.033 Uiso 1 1 calc R . . C21 C -0.0404(7) 0.1054(6) 0.2147(5) 0.0209(19) Uani 1 1 d . . . H33 H -0.0569 0.0534 0.2388 0.031 Uiso 1 1 calc R . . H34 H -0.0963 0.1160 0.1752 0.031 Uiso 1 1 calc R . . H35 H -0.0413 0.1499 0.2509 0.031 Uiso 1 1 calc R . . C22 C -0.0395(9) 0.1535(6) -0.0402(5) 0.028(2) Uani 1 1 d . . . H36 H -0.0630 0.1787 -0.0872 0.042 Uiso 1 1 calc R . . H37 H -0.0980 0.1169 -0.0238 0.042 Uiso 1 1 calc R . . H38 H 0.0285 0.1220 -0.0464 0.042 Uiso 1 1 calc R . . C23 C -0.1459(8) 0.2923(6) 0.0355(5) 0.027(2) Uani 1 1 d . . . H39 H -0.1334 0.3433 0.0631 0.040 Uiso 1 1 calc R . . H40 H -0.1998 0.2585 0.0605 0.040 Uiso 1 1 calc R . . H41 H -0.1745 0.3051 -0.0145 0.040 Uiso 1 1 calc R . . C24 C 0.2987(8) 0.3517(6) 0.0189(5) 0.026(2) Uani 1 1 d . . . H42 H 0.3270 0.2989 0.0022 0.039 Uiso 1 1 calc R . . H43 H 0.3510 0.3753 0.0558 0.039 Uiso 1 1 calc R . . H44 H 0.2900 0.3891 -0.0231 0.039 Uiso 1 1 calc R . . C25 C 0.1105(9) 0.4409(6) 0.0834(5) 0.026(2) Uani 1 1 d . . . H45 H 0.1143 0.4758 0.0397 0.039 Uiso 1 1 calc R . . H46 H 0.1575 0.4640 0.1235 0.039 Uiso 1 1 calc R . . H47 H 0.0337 0.4382 0.0987 0.039 Uiso 1 1 calc R . . C26 C 0.0388(9) 0.3563(6) -0.0812(5) 0.027(2) Uani 1 1 d . . . H48 H 0.0176 0.3195 -0.1220 0.041 Uiso 1 1 calc R . . H49 H 0.1014 0.3904 -0.0950 0.041 Uiso 1 1 calc R . . H50 H -0.0242 0.3916 -0.0703 0.041 Uiso 1 1 calc R . . C27 C 0.6712(9) 0.2843(7) 0.3600(5) 0.034(2) Uani 1 1 d . . . C28 C 0.5958(9) 0.2498(7) 0.4044(5) 0.035(3) Uani 1 1 d . . . H51 H 0.5470 0.2850 0.4293 0.042 Uiso 1 1 calc R . . C29 C 0.5865(9) 0.1655(7) 0.4152(6) 0.034(2) Uani 1 1 d . . . H52 H 0.5329 0.1438 0.4468 0.041 Uiso 1 1 calc R . . C30 C 0.6563(11) 0.1151(8) 0.3793(6) 0.045(3) Uani 1 1 d . . . H53 H 0.6506 0.0574 0.3850 0.054 Uiso 1 1 calc R . . C31 C 0.7350(10) 0.1473(9) 0.3348(6) 0.046(3) Uani 1 1 d . . . H54 H 0.7841 0.1120 0.3103 0.055 Uiso 1 1 calc R . . C32 C 0.7424(9) 0.2326(9) 0.3259(5) 0.044(3) Uani 1 1 d . . . H55 H 0.7975 0.2548 0.2959 0.052 Uiso 1 1 calc R . . C33 C 0.6788(12) 0.3740(8) 0.3501(8) 0.059(4) Uani 1 1 d . . . H56 H 0.6659 0.4014 0.3969 0.088 Uiso 1 1 calc R . . H57 H 0.6228 0.3918 0.3129 0.088 Uiso 1 1 calc R . . H58 H 0.7527 0.3882 0.3338 0.088 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 0.01334(16) 0.01354(15) 0.01276(14) -0.00209(14) -0.00024(10) -0.00075(15) Cl1 0.0197(11) 0.0225(10) 0.0218(9) -0.0058(8) 0.0014(8) 0.0039(9) P1 0.0163(11) 0.0107(10) 0.0142(9) -0.0013(8) 0.0009(8) -0.0009(8) Si1 0.0177(12) 0.0207(12) 0.0179(10) -0.0031(10) -0.0018(9) -0.0008(11) Si2 0.0169(12) 0.0186(11) 0.0162(10) 0.0014(9) -0.0004(9) 0.0000(10) O1 0.018(3) 0.023(3) 0.015(3) 0.002(2) 0.001(2) 0.003(3) N1 0.009(4) 0.023(4) 0.016(3) -0.004(3) 0.002(3) -0.001(3) C1 0.021(5) 0.018(4) 0.014(4) -0.004(3) -0.001(3) -0.007(4) C2 0.030(5) 0.011(4) 0.020(4) 0.002(3) 0.006(4) 0.000(4) C3 0.027(5) 0.011(4) 0.033(5) 0.001(4) 0.003(4) -0.007(4) C4 0.040(6) 0.012(4) 0.032(5) 0.006(4) 0.006(4) -0.005(4) C5 0.034(6) 0.016(4) 0.016(4) 0.001(3) 0.002(4) 0.007(4) C6 0.023(5) 0.022(5) 0.022(4) 0.000(4) 0.002(4) -0.004(4) C7 0.034(6) 0.027(5) 0.030(5) 0.014(4) -0.003(4) 0.002(5) C8 0.017(5) 0.015(4) 0.018(4) 0.002(3) 0.002(3) -0.003(3) C9 0.020(5) 0.024(5) 0.028(4) -0.001(4) 0.005(4) 0.001(4) C10 0.022(5) 0.035(5) 0.034(5) -0.014(4) 0.013(4) 0.004(4) C11 0.019(5) 0.025(5) 0.038(5) 0.000(4) 0.009(4) 0.004(4) C12 0.015(5) 0.029(5) 0.035(5) 0.007(5) 0.003(4) 0.008(4) C13 0.019(5) 0.027(5) 0.027(4) 0.003(4) 0.007(3) -0.007(4) C14 0.020(4) 0.011(4) 0.019(4) -0.001(3) -0.002(3) -0.004(3) C15 0.034(6) 0.010(4) 0.023(4) -0.006(3) -0.002(4) -0.007(4) C16 0.049(7) 0.022(5) 0.025(4) -0.005(4) 0.007(5) -0.017(5) C17 0.040(7) 0.021(5) 0.029(5) -0.007(4) -0.004(4) 0.005(5) C18 0.025(5) 0.029(5) 0.017(4) -0.002(4) -0.001(4) -0.002(4) C19 0.028(5) 0.018(4) 0.017(4) 0.001(4) 0.004(3) 0.004(4) C20 0.024(5) 0.017(4) 0.023(4) -0.007(4) -0.008(4) 0.001(4) C21 0.011(4) 0.022(4) 0.030(4) -0.002(4) 0.006(4) -0.006(4) C22 0.031(6) 0.025(5) 0.026(4) -0.005(4) -0.012(4) -0.001(4) C23 0.019(5) 0.027(5) 0.034(5) -0.002(4) 0.000(4) -0.002(4) C24 0.015(5) 0.029(5) 0.034(5) 0.008(4) 0.004(4) 0.002(4) C25 0.035(6) 0.022(5) 0.021(4) 0.002(4) -0.005(4) -0.006(4) C26 0.027(6) 0.036(5) 0.018(4) 0.005(4) -0.003(4) 0.009(5) C27 0.026(5) 0.049(7) 0.027(4) 0.000(5) -0.008(4) -0.010(5) C28 0.027(6) 0.049(7) 0.028(5) -0.006(4) -0.006(4) 0.006(5) C29 0.017(5) 0.047(7) 0.039(5) 0.002(5) 0.000(4) -0.008(5) C30 0.035(7) 0.048(7) 0.051(7) -0.010(6) -0.012(6) -0.006(6) C31 0.021(6) 0.071(9) 0.044(6) -0.011(6) -0.003(5) -0.001(6) C32 0.024(6) 0.081(10) 0.026(5) 0.004(6) 0.004(4) -0.020(7) C33 0.041(8) 0.050(8) 0.084(9) 0.026(8) -0.014(7) -0.010(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 Si2 2.267(2) . ? Ir1 P1 2.308(2) . ? Ir1 N1 2.319(7) . ? Ir1 Si1 2.336(2) . ? Ir1 Cl1 2.497(2) . ? Ir1 H1 1.44(15) . ? P1 C1 1.816(9) . ? P1 C14 1.849(8) . ? P1 C8 1.859(9) . ? Si1 O1 1.804(7) . ? Si1 C23 1.861(10) . ? Si1 C22 1.873(9) . ? Si1 Si2 2.694(3) . ? Si2 O1 1.810(6) . ? Si2 C25 1.861(10) . ? Si2 C24 1.893(10) . ? O1 C26 1.437(10) . ? N1 C2 1.476(11) . ? N1 C20 1.500(10) . ? N1 C21 1.507(11) . ? C1 C2 1.399(13) . ? C1 C6 1.408(12) . ? C2 C3 1.402(11) . ? C3 C4 1.377(14) . ? C3 H2 0.9500 . ? C4 C5 1.393(14) . ? C4 H3 0.9500 . ? C5 C6 1.384(12) . ? C5 C7 1.510(13) . ? C6 H4 0.9500 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C8 C9 1.532(12) . ? C8 C13 1.538(12) . ? C8 H8 1.0000 . ? C9 C10 1.526(13) . ? C9 H9 0.9900 . ? C9 H10 0.9900 . ? C10 C11 1.511(14) . ? C10 H11 0.9900 . ? C10 H12 0.9900 . ? C11 C12 1.492(13) . ? C11 H13 0.9900 . ? C11 H14 0.9900 . ? C12 C13 1.542(12) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 H17 0.9900 . ? C13 H18 0.9900 . ? C14 C15 1.524(11) . ? C14 C19 1.534(12) . ? C14 H19 1.0000 . ? C15 C16 1.537(12) . ? C15 H20 0.9900 . ? C15 H21 0.9900 . ? C16 C17 1.517(14) . ? C16 H22 0.9900 . ? C16 H23 0.9900 . ? C17 C18 1.520(13) . ? C17 H24 0.9900 . ? C17 H25 0.9900 . ? C18 C19 1.521(12) . ? C18 H26 0.9900 . ? C18 H27 0.9900 . ? C19 H28 0.9900 . ? C19 H29 0.9900 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C20 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C21 H35 0.9800 . ? C22 H36 0.9800 . ? C22 H37 0.9800 . ? C22 H38 0.9800 . ? C23 H39 0.9800 . ? C23 H40 0.9800 . ? C23 H41 0.9800 . ? C24 H42 0.9800 . ? C24 H43 0.9800 . ? C24 H44 0.9800 . ? C25 H45 0.9800 . ? C25 H46 0.9800 . ? C25 H47 0.9800 . ? C26 H48 0.9800 . ? C26 H49 0.9800 . ? C26 H50 0.9800 . ? C27 C28 1.363(16) . ? C27 C32 1.371(17) . ? C27 C33 1.479(16) . ? C28 C29 1.395(16) . ? C28 H51 0.9500 . ? C29 C30 1.363(17) . ? C29 H52 0.9500 . ? C30 C31 1.377(18) . ? C30 H53 0.9500 . ? C31 C32 1.405(19) . ? C31 H54 0.9500 . ? C32 H55 0.9500 . ? C33 H56 0.9800 . ? C33 H57 0.9800 . ? C33 H58 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 Si2 Ir1 P1 101.96(8) . . ? Si2 Ir1 N1 171.35(17) . . ? P1 Ir1 N1 81.70(18) . . ? Si2 Ir1 Si1 71.63(9) . . ? P1 Ir1 Si1 167.19(8) . . ? N1 Ir1 Si1 103.19(18) . . ? Si2 Ir1 Cl1 95.44(8) . . ? P1 Ir1 Cl1 97.16(7) . . ? N1 Ir1 Cl1 91.85(18) . . ? Si1 Ir1 Cl1 94.53(8) . . ? Si2 Ir1 H1 83(6) . . ? P1 Ir1 H1 98(6) . . ? N1 Ir1 H1 89(6) . . ? Si1 Ir1 H1 71(6) . . ? Cl1 Ir1 H1 165(6) . . ? C1 P1 C14 104.6(3) . . ? C1 P1 C8 105.7(4) . . ? C14 P1 C8 104.3(4) . . ? C1 P1 Ir1 105.0(3) . . ? C14 P1 Ir1 123.3(3) . . ? C8 P1 Ir1 112.5(3) . . ? O1 Si1 C23 101.0(4) . . ? O1 Si1 C22 103.2(4) . . ? C23 Si1 C22 105.4(5) . . ? O1 Si1 Ir1 92.9(2) . . ? C23 Si1 Ir1 123.3(3) . . ? C22 Si1 Ir1 124.4(3) . . ? O1 Si1 Si2 41.88(19) . . ? C23 Si1 Si2 110.4(3) . . ? C22 Si1 Si2 133.4(4) . . ? Ir1 Si1 Si2 52.99(7) . . ? O1 Si2 C25 102.1(4) . . ? O1 Si2 C24 103.0(4) . . ? C25 Si2 C24 105.0(5) . . ? O1 Si2 Ir1 95.1(2) . . ? C25 Si2 Ir1 122.2(3) . . ? C24 Si2 Ir1 124.1(3) . . ? O1 Si2 Si1 41.7(2) . . ? C25 Si2 Si1 110.7(3) . . ? C24 Si2 Si1 133.6(3) . . ? Ir1 Si2 Si1 55.38(7) . . ? C26 O1 Si1 127.9(6) . . ? C26 O1 Si2 129.4(6) . . ? Si1 O1 Si2 96.4(3) . . ? C2 N1 C20 107.2(7) . . ? C2 N1 C21 110.0(6) . . ? C20 N1 C21 106.8(7) . . ? C2 N1 Ir1 114.5(5) . . ? C20 N1 Ir1 108.1(5) . . ? C21 N1 Ir1 109.9(5) . . ? C2 C1 C6 118.5(8) . . ? C2 C1 P1 117.9(6) . . ? C6 C1 P1 123.6(7) . . ? C1 C2 C3 119.5(8) . . ? C1 C2 N1 120.9(7) . . ? C3 C2 N1 119.5(8) . . ? C4 C3 C2 120.2(9) . . ? C4 C3 H2 119.9 . . ? C2 C3 H2 119.9 . . ? C3 C4 C5 121.9(8) . . ? C3 C4 H3 119.0 . . ? C5 C4 H3 119.0 . . ? C6 C5 C4 117.5(8) . . ? C6 C5 C7 122.1(9) . . ? C4 C5 C7 120.4(8) . . ? C5 C6 C1 122.4(9) . . ? C5 C6 H4 118.8 . . ? C1 C6 H4 118.8 . . ? C5 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C5 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? C9 C8 C13 109.0(8) . . ? C9 C8 P1 112.1(6) . . ? C13 C8 P1 117.9(6) . . ? C9 C8 H8 105.6 . . ? C13 C8 H8 105.6 . . ? P1 C8 H8 105.6 . . ? C10 C9 C8 111.2(8) . . ? C10 C9 H9 109.4 . . ? C8 C9 H9 109.4 . . ? C10 C9 H10 109.4 . . ? C8 C9 H10 109.4 . . ? H9 C9 H10 108.0 . . ? C11 C10 C9 111.1(8) . . ? C11 C10 H11 109.4 . . ? C9 C10 H11 109.4 . . ? C11 C10 H12 109.4 . . ? C9 C10 H12 109.4 . . ? H11 C10 H12 108.0 . . ? C12 C11 C10 111.8(8) . . ? C12 C11 H13 109.2 . . ? C10 C11 H13 109.2 . . ? C12 C11 H14 109.2 . . ? C10 C11 H14 109.2 . . ? H13 C11 H14 107.9 . . ? C11 C12 C13 112.0(8) . . ? C11 C12 H15 109.2 . . ? C13 C12 H15 109.2 . . ? C11 C12 H16 109.2 . . ? C13 C12 H16 109.2 . . ? H15 C12 H16 107.9 . . ? C8 C13 C12 108.0(7) . . ? C8 C13 H17 110.1 . . ? C12 C13 H17 110.1 . . ? C8 C13 H18 110.1 . . ? C12 C13 H18 110.1 . . ? H17 C13 H18 108.4 . . ? C15 C14 C19 110.6(7) . . ? C15 C14 P1 107.9(5) . . ? C19 C14 P1 113.5(6) . . ? C15 C14 H19 108.2 . . ? C19 C14 H19 108.2 . . ? P1 C14 H19 108.2 . . ? C14 C15 C16 112.3(7) . . ? C14 C15 H20 109.1 . . ? C16 C15 H20 109.1 . . ? C14 C15 H21 109.1 . . ? C16 C15 H21 109.1 . . ? H20 C15 H21 107.9 . . ? C17 C16 C15 110.8(8) . . ? C17 C16 H22 109.5 . . ? C15 C16 H22 109.5 . . ? C17 C16 H23 109.5 . . ? C15 C16 H23 109.5 . . ? H22 C16 H23 108.1 . . ? C16 C17 C18 111.3(8) . . ? C16 C17 H24 109.4 . . ? C18 C17 H24 109.4 . . ? C16 C17 H25 109.4 . . ? C18 C17 H25 109.4 . . ? H24 C17 H25 108.0 . . ? C17 C18 C19 111.3(7) . . ? C17 C18 H26 109.4 . . ? C19 C18 H26 109.4 . . ? C17 C18 H27 109.4 . . ? C19 C18 H27 109.4 . . ? H26 C18 H27 108.0 . . ? C18 C19 C14 109.6(8) . . ? C18 C19 H28 109.7 . . ? C14 C19 H28 109.7 . . ? C18 C19 H29 109.7 . . ? C14 C19 H29 109.7 . . ? H28 C19 H29 108.2 . . ? N1 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C20 H32 109.5 . . ? H30 C20 H32 109.5 . . ? H31 C20 H32 109.5 . . ? N1 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? N1 C21 H35 109.5 . . ? H33 C21 H35 109.5 . . ? H34 C21 H35 109.5 . . ? Si1 C22 H36 109.5 . . ? Si1 C22 H37 109.5 . . ? H36 C22 H37 109.5 . . ? Si1 C22 H38 109.5 . . ? H36 C22 H38 109.5 . . ? H37 C22 H38 109.5 . . ? Si1 C23 H39 109.5 . . ? Si1 C23 H40 109.5 . . ? H39 C23 H40 109.5 . . ? Si1 C23 H41 109.5 . . ? H39 C23 H41 109.5 . . ? H40 C23 H41 109.5 . . ? Si2 C24 H42 109.5 . . ? Si2 C24 H43 109.5 . . ? H42 C24 H43 109.5 . . ? Si2 C24 H44 109.5 . . ? H42 C24 H44 109.5 . . ? H43 C24 H44 109.5 . . ? Si2 C25 H45 109.5 . . ? Si2 C25 H46 109.5 . . ? H45 C25 H46 109.5 . . ? Si2 C25 H47 109.5 . . ? H45 C25 H47 109.5 . . ? H46 C25 H47 109.5 . . ? O1 C26 H48 109.5 . . ? O1 C26 H49 109.5 . . ? H48 C26 H49 109.5 . . ? O1 C26 H50 109.5 . . ? H48 C26 H50 109.5 . . ? H49 C26 H50 109.5 . . ? C28 C27 C32 117.5(11) . . ? C28 C27 C33 121.8(12) . . ? C32 C27 C33 120.7(11) . . ? C27 C28 C29 123.4(11) . . ? C27 C28 H51 118.3 . . ? C29 C28 H51 118.3 . . ? C30 C29 C28 118.2(11) . . ? C30 C29 H52 120.9 . . ? C28 C29 H52 120.9 . . ? C29 C30 C31 120.5(13) . . ? C29 C30 H53 119.8 . . ? C31 C30 H53 119.8 . . ? C30 C31 C32 119.6(12) . . ? C30 C31 H54 120.2 . . ? C32 C31 H54 120.2 . . ? C27 C32 C31 120.9(10) . . ? C27 C32 H55 119.6 . . ? C31 C32 H55 119.6 . . ? C27 C33 H56 109.5 . . ? C27 C33 H57 109.5 . . ? H56 C33 H57 109.5 . . ? C27 C33 H58 109.5 . . ? H56 C33 H58 109.5 . . ? H57 C33 H58 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 Si2 Ir1 P1 C1 -172.2(3) . . . . ? N1 Ir1 P1 C1 -0.2(3) . . . . ? Si1 Ir1 P1 C1 -113.7(4) . . . . ? Cl1 Ir1 P1 C1 90.6(3) . . . . ? Si2 Ir1 P1 C14 68.6(3) . . . . ? N1 Ir1 P1 C14 -119.3(4) . . . . ? Si1 Ir1 P1 C14 127.2(5) . . . . ? Cl1 Ir1 P1 C14 -28.5(3) . . . . ? Si2 Ir1 P1 C8 -57.7(3) . . . . ? N1 Ir1 P1 C8 114.3(3) . . . . ? Si1 Ir1 P1 C8 0.8(5) . . . . ? Cl1 Ir1 P1 C8 -154.9(3) . . . . ? Si2 Ir1 Si1 O1 13.6(2) . . . . ? P1 Ir1 Si1 O1 -48.0(4) . . . . ? N1 Ir1 Si1 O1 -159.2(3) . . . . ? Cl1 Ir1 Si1 O1 107.8(2) . . . . ? Si2 Ir1 Si1 C23 -91.6(4) . . . . ? P1 Ir1 Si1 C23 -153.2(5) . . . . ? N1 Ir1 Si1 C23 95.6(4) . . . . ? Cl1 Ir1 Si1 C23 2.6(4) . . . . ? Si2 Ir1 Si1 C22 121.8(4) . . . . ? P1 Ir1 Si1 C22 60.2(6) . . . . ? N1 Ir1 Si1 C22 -51.0(5) . . . . ? Cl1 Ir1 Si1 C22 -144.0(4) . . . . ? P1 Ir1 Si1 Si2 -61.6(4) . . . . ? N1 Ir1 Si1 Si2 -172.80(19) . . . . ? Cl1 Ir1 Si1 Si2 94.23(9) . . . . ? P1 Ir1 Si2 O1 154.9(2) . . . . ? N1 Ir1 Si2 O1 40.6(13) . . . . ? Si1 Ir1 Si2 O1 -13.6(2) . . . . ? Cl1 Ir1 Si2 O1 -106.6(2) . . . . ? P1 Ir1 Si2 C25 -97.3(4) . . . . ? N1 Ir1 Si2 C25 148.4(13) . . . . ? Si1 Ir1 Si2 C25 94.2(4) . . . . ? Cl1 Ir1 Si2 C25 1.2(4) . . . . ? P1 Ir1 Si2 C24 45.5(4) . . . . ? N1 Ir1 Si2 C24 -68.8(13) . . . . ? Si1 Ir1 Si2 C24 -123.0(4) . . . . ? Cl1 Ir1 Si2 C24 144.0(4) . . . . ? P1 Ir1 Si2 Si1 168.50(8) . . . . ? N1 Ir1 Si2 Si1 54.2(12) . . . . ? Cl1 Ir1 Si2 Si1 -92.98(8) . . . . ? C23 Si1 Si2 O1 -83.7(4) . . . . ? C22 Si1 Si2 O1 54.3(5) . . . . ? Ir1 Si1 Si2 O1 159.4(3) . . . . ? O1 Si1 Si2 C25 85.0(4) . . . . ? C23 Si1 Si2 C25 1.3(5) . . . . ? C22 Si1 Si2 C25 139.2(5) . . . . ? Ir1 Si1 Si2 C25 -115.6(3) . . . . ? O1 Si1 Si2 C24 -53.0(5) . . . . ? C23 Si1 Si2 C24 -136.7(5) . . . . ? C22 Si1 Si2 C24 1.2(6) . . . . ? Ir1 Si1 Si2 C24 106.4(4) . . . . ? O1 Si1 Si2 Ir1 -159.4(3) . . . . ? C23 Si1 Si2 Ir1 116.9(3) . . . . ? C22 Si1 Si2 Ir1 -105.2(4) . . . . ? C23 Si1 O1 C26 -45.3(8) . . . . ? C22 Si1 O1 C26 63.6(8) . . . . ? Ir1 Si1 O1 C26 -170.0(7) . . . . ? Si2 Si1 O1 C26 -153.7(8) . . . . ? C23 Si1 O1 Si2 108.4(4) . . . . ? C22 Si1 O1 Si2 -142.7(4) . . . . ? Ir1 Si1 O1 Si2 -16.3(2) . . . . ? C25 Si2 O1 C26 45.4(8) . . . . ? C24 Si2 O1 C26 -63.4(8) . . . . ? Ir1 Si2 O1 C26 169.9(7) . . . . ? Si1 Si2 O1 C26 153.1(9) . . . . ? C25 Si2 O1 Si1 -107.7(4) . . . . ? C24 Si2 O1 Si1 143.6(4) . . . . ? Ir1 Si2 O1 Si1 16.9(3) . . . . ? Si2 Ir1 N1 C2 117.2(12) . . . . ? P1 Ir1 N1 C2 1.5(5) . . . . ? Si1 Ir1 N1 C2 169.5(5) . . . . ? Cl1 Ir1 N1 C2 -95.5(5) . . . . ? Si2 Ir1 N1 C20 -2.3(16) . . . . ? P1 Ir1 N1 C20 -117.9(5) . . . . ? Si1 Ir1 N1 C20 50.0(5) . . . . ? Cl1 Ir1 N1 C20 145.1(5) . . . . ? Si2 Ir1 N1 C21 -118.5(12) . . . . ? P1 Ir1 N1 C21 125.8(5) . . . . ? Si1 Ir1 N1 C21 -66.2(5) . . . . ? Cl1 Ir1 N1 C21 28.9(5) . . . . ? C14 P1 C1 C2 129.8(7) . . . . ? C8 P1 C1 C2 -120.4(7) . . . . ? Ir1 P1 C1 C2 -1.2(7) . . . . ? C14 P1 C1 C6 -51.2(8) . . . . ? C8 P1 C1 C6 58.6(8) . . . . ? Ir1 P1 C1 C6 177.8(7) . . . . ? C6 C1 C2 C3 -0.4(13) . . . . ? P1 C1 C2 C3 178.6(7) . . . . ? C6 C1 C2 N1 -176.3(7) . . . . ? P1 C1 C2 N1 2.8(11) . . . . ? C20 N1 C2 C1 117.1(9) . . . . ? C21 N1 C2 C1 -127.1(8) . . . . ? Ir1 N1 C2 C1 -2.9(10) . . . . ? C20 N1 C2 C3 -58.8(10) . . . . ? C21 N1 C2 C3 57.0(10) . . . . ? Ir1 N1 C2 C3 -178.7(7) . . . . ? C1 C2 C3 C4 0.1(14) . . . . ? N1 C2 C3 C4 176.0(8) . . . . ? C2 C3 C4 C5 -0.9(15) . . . . ? C3 C4 C5 C6 1.9(14) . . . . ? C3 C4 C5 C7 -177.9(9) . . . . ? C4 C5 C6 C1 -2.3(14) . . . . ? C7 C5 C6 C1 177.5(9) . . . . ? C2 C1 C6 C5 1.6(13) . . . . ? P1 C1 C6 C5 -177.4(7) . . . . ? C1 P1 C8 C9 35.2(7) . . . . ? C14 P1 C8 C9 145.2(6) . . . . ? Ir1 P1 C8 C9 -78.8(6) . . . . ? C1 P1 C8 C13 -92.6(7) . . . . ? C14 P1 C8 C13 17.4(8) . . . . ? Ir1 P1 C8 C13 153.4(6) . . . . ? C13 C8 C9 C10 -59.4(9) . . . . ? P1 C8 C9 C10 168.2(6) . . . . ? C8 C9 C10 C11 55.3(11) . . . . ? C9 C10 C11 C12 -53.3(11) . . . . ? C10 C11 C12 C13 56.3(11) . . . . ? C9 C8 C13 C12 59.9(9) . . . . ? P1 C8 C13 C12 -170.8(6) . . . . ? C11 C12 C13 C8 -59.3(10) . . . . ? C1 P1 C14 C15 -169.0(7) . . . . ? C8 P1 C14 C15 80.2(7) . . . . ? Ir1 P1 C14 C15 -49.6(7) . . . . ? C1 P1 C14 C19 -46.1(7) . . . . ? C8 P1 C14 C19 -156.9(6) . . . . ? Ir1 P1 C14 C19 73.3(6) . . . . ? C19 C14 C15 C16 55.2(11) . . . . ? P1 C14 C15 C16 179.8(7) . . . . ? C14 C15 C16 C17 -53.5(12) . . . . ? C15 C16 C17 C18 54.1(12) . . . . ? C16 C17 C18 C19 -57.8(11) . . . . ? C17 C18 C19 C14 58.6(11) . . . . ? C15 C14 C19 C18 -57.1(9) . . . . ? P1 C14 C19 C18 -178.4(6) . . . . ? C32 C27 C28 C29 -1.4(15) . . . . ? C33 C27 C28 C29 -179.8(10) . . . . ? C27 C28 C29 C30 -0.2(16) . . . . ? C28 C29 C30 C31 1.3(16) . . . . ? C29 C30 C31 C32 -0.7(17) . . . . ? C28 C27 C32 C31 2.0(15) . . . . ? C33 C27 C32 C31 -179.6(11) . . . . ? C30 C31 C32 C27 -1.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.573 _refine_diff_density_min -2.089 _refine_diff_density_rms 0.298 #===END data_(PcyN-P,N)IrH3[SiMe2C(SiMe3)2SiClMe-Si,Si]-(9) _database_code_depnum_ccdc_archive 'CCDC 772166' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H64 Cl Ir N P Si4' _chemical_formula_sum 'C31 H64 Cl Ir N P Si4' _chemical_formula_weight 821.81 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' 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5618(3) _cell_length_b 18.3157(4) _cell_length_c 17.9750(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.0413(11) _cell_angle_gamma 90.00 _cell_volume 3785.29(17) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8508 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellowish-white _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 3.788 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6593 _exptl_absorpt_correction_T_max 0.7268 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33309 _diffrn_reflns_av_R_equivalents 0.0986 _diffrn_reflns_av_sigmaI/netI 0.0739 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8508 _reflns_number_gt 6769 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0665P)^2^+20.9692P] 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 8508 _refine_ls_number_parameters 359 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1634 _refine_ls_goodness_of_fit_ref 1.298 _refine_ls_restrained_S_all 1.298 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.08803(3) 0.11375(2) 0.32586(2) 0.02044(12) Uani 1 1 d . A . Cl1 Cl 0.2393(3) 0.2522(2) 0.21851(19) 0.0575(10) Uani 1 1 d . A 1 P1 P -0.0042(2) 0.10556(13) 0.20550(13) 0.0201(5) Uani 1 1 d . A . Si1 Si 0.2077(2) 0.21450(15) 0.32565(16) 0.0235(6) Uani 1 1 d . . . Si2 Si 0.2907(2) 0.08224(15) 0.36416(15) 0.0228(6) Uani 1 1 d . A . Si3 Si 0.3700(3) 0.20646(18) 0.47854(17) 0.0353(7) Uani 1 1 d . . . Si4 Si 0.4842(3) 0.20504(16) 0.32889(18) 0.0300(7) Uani 1 1 d . . . N1 N -0.0593(7) 0.0337(4) 0.3506(4) 0.0231(18) Uani 1 1 d . . . C1 C -0.1382(8) 0.0553(5) 0.2177(5) 0.0192(19) Uani 1 1 d . . . C2 C -0.1506(9) 0.0259(5) 0.2878(5) 0.024(2) Uani 1 1 d . A . C3 C -0.2504(9) -0.0145(5) 0.2969(6) 0.028(2) Uani 1 1 d . . . H1 H -0.2586 -0.0378 0.3433 0.034 Uiso 1 1 calc R A . C4 C -0.3377(9) -0.0208(6) 0.2381(7) 0.033(3) Uani 1 1 d . A . H2 H -0.4067 -0.0464 0.2460 0.040 Uiso 1 1 calc R . . C5 C -0.3280(9) 0.0085(5) 0.1695(7) 0.030(2) Uani 1 1 d . . . C6 C -0.2285(9) 0.0459(5) 0.1586(6) 0.026(2) Uani 1 1 d . A . H3 H -0.2198 0.0658 0.1107 0.032 Uiso 1 1 calc R . . C7 C -0.4231(9) 0.0017(6) 0.1063(6) 0.035(3) Uani 1 1 d . A . H4 H -0.3920 0.0129 0.0589 0.053 Uiso 1 1 calc R . . H5 H -0.4858 0.0361 0.1140 0.053 Uiso 1 1 calc R . . H6 H -0.4538 -0.0482 0.1047 0.053 Uiso 1 1 calc R . . C8 C -0.0551(9) 0.1926(5) 0.1601(5) 0.021(2) Uani 1 1 d . . . H7 H 0.0108 0.2276 0.1714 0.025 Uiso 1 1 calc R A . C9 C -0.1559(10) 0.2254(6) 0.1963(7) 0.035(3) Uani 1 1 d . A . H8 H -0.1359 0.2274 0.2512 0.042 Uiso 1 1 calc R . . H9 H -0.2253 0.1939 0.1859 0.042 Uiso 1 1 calc R . . C10 C -0.1836(12) 0.3020(6) 0.1665(9) 0.053(4) Uani 1 1 d . . . H10 H -0.2536 0.3205 0.1878 0.064 Uiso 1 1 calc R A . H11 H -0.1180 0.3350 0.1829 0.064 Uiso 1 1 calc R . . C11 C -0.2049(11) 0.3029(7) 0.0819(8) 0.050(4) Uani 1 1 d . A . H12 H -0.2764 0.2749 0.0659 0.060 Uiso 1 1 calc R . . H13 H -0.2173 0.3539 0.0645 0.060 Uiso 1 1 calc R . . C12 C -0.1049(12) 0.2707(6) 0.0466(8) 0.050(4) Uani 1 1 d . . . H14 H -0.0348 0.3011 0.0589 0.060 Uiso 1 1 calc R A . H15 H -0.1231 0.2704 -0.0085 0.060 Uiso 1 1 calc R . . C13 C -0.0804(10) 0.1930(6) 0.0742(6) 0.034(2) Uani 1 1 d . A . H16 H -0.0127 0.1731 0.0514 0.040 Uiso 1 1 calc R . . H17 H -0.1485 0.1616 0.0589 0.040 Uiso 1 1 calc R . . C14 C 0.0569(8) 0.0500(5) 0.1333(5) 0.0206(19) Uani 1 1 d . . . H18 H 0.0006 0.0511 0.0871 0.025 Uiso 1 1 calc R A . C15 C 0.1733(8) 0.0803(5) 0.1133(6) 0.024(2) Uani 1 1 d . A . H19 H 0.1615 0.1307 0.0941 0.028 Uiso 1 1 calc R . . H20 H 0.2289 0.0824 0.1590 0.028 Uiso 1 1 calc R . . C16 C 0.2253(10) 0.0338(6) 0.0544(6) 0.034(3) Uani 1 1 d . . . H21 H 0.1745 0.0364 0.0065 0.041 Uiso 1 1 calc R A . H22 H 0.3026 0.0533 0.0458 0.041 Uiso 1 1 calc R . . C17 C 0.2373(10) -0.0443(6) 0.0795(7) 0.039(3) Uani 1 1 d . A . H23 H 0.2961 -0.0473 0.1236 0.047 Uiso 1 1 calc R . . H24 H 0.2656 -0.0739 0.0390 0.047 Uiso 1 1 calc R . . C18 C 0.1229(10) -0.0763(6) 0.0998(6) 0.034(3) Uani 1 1 d . . . H25 H 0.0668 -0.0794 0.0543 0.040 Uiso 1 1 calc R A . H26 H 0.1364 -0.1263 0.1197 0.040 Uiso 1 1 calc R . . C19 C 0.0725(9) -0.0292(5) 0.1578(6) 0.025(2) Uani 1 1 d . A . H27 H 0.1247 -0.0312 0.2051 0.030 Uiso 1 1 calc R . . H28 H -0.0038 -0.0494 0.1677 0.030 Uiso 1 1 calc R . . C20 C -0.1110(11) 0.0648(8) 0.4162(6) 0.044(3) Uani 1 1 d . A . H29 H -0.1494 0.1112 0.4020 0.066 Uiso 1 1 calc R . . H30 H -0.0495 0.0732 0.4571 0.066 Uiso 1 1 calc R . . H31 H -0.1682 0.0305 0.4326 0.066 Uiso 1 1 calc R . . C21 C -0.0087(11) -0.0395(6) 0.3707(7) 0.044(3) Uani 1 1 d . A . H32 H -0.0699 -0.0719 0.3853 0.066 Uiso 1 1 calc R . . H33 H 0.0524 -0.0345 0.4125 0.066 Uiso 1 1 calc R . . H34 H 0.0246 -0.0603 0.3274 0.066 Uiso 1 1 calc R . . C22 C 0.1531(11) 0.3046(7) 0.3635(7) 0.041(3) Uiso 1 1 d . A 1 C23 C 0.3068(10) 0.0241(6) 0.4510(6) 0.036(3) Uani 1 1 d . . . H35 H 0.3895 0.0163 0.4670 0.054 Uiso 1 1 calc R A . H36 H 0.2688 -0.0232 0.4403 0.054 Uiso 1 1 calc R . . H37 H 0.2704 0.0487 0.4909 0.054 Uiso 1 1 calc R . . C24 C 0.3782(9) 0.0255(6) 0.2984(7) 0.036(3) Uani 1 1 d . . . H38 H 0.4606 0.0253 0.3179 0.054 Uiso 1 1 calc R A . H39 H 0.3694 0.0472 0.2483 0.054 Uiso 1 1 calc R . . H40 H 0.3489 -0.0248 0.2957 0.054 Uiso 1 1 calc R . . C25 C 0.3521(8) 0.1803(5) 0.3766(5) 0.0191(19) Uani 1 1 d . A . C26 C 0.2332(13) 0.2023(9) 0.5268(7) 0.059(4) Uani 1 1 d . A . H41 H 0.1730 0.2325 0.4995 0.089 Uiso 1 1 calc R . . H42 H 0.2494 0.2204 0.5781 0.089 Uiso 1 1 calc R . . H43 H 0.2061 0.1516 0.5278 0.089 Uiso 1 1 calc R . . C27 C 0.4767(12) 0.1484(8) 0.5389(7) 0.053(4) Uani 1 1 d . A . H44 H 0.4343 0.1152 0.5691 0.080 Uiso 1 1 calc R . . H45 H 0.5276 0.1799 0.5721 0.080 Uiso 1 1 calc R . . H46 H 0.5237 0.1200 0.5071 0.080 Uiso 1 1 calc R . . C28 C 0.4258(15) 0.3028(8) 0.4939(8) 0.062(4) Uani 1 1 d . A . H47 H 0.5057 0.3058 0.4807 0.092 Uiso 1 1 calc R . . H48 H 0.4242 0.3161 0.5466 0.092 Uiso 1 1 calc R . . H49 H 0.3763 0.3364 0.4623 0.092 Uiso 1 1 calc R . . C29 C 0.6218(11) 0.1745(8) 0.3812(9) 0.060(4) Uani 1 1 d . A . H50 H 0.6329 0.1999 0.4294 0.090 Uiso 1 1 calc R . . H51 H 0.6867 0.1858 0.3522 0.090 Uiso 1 1 calc R . . H52 H 0.6186 0.1218 0.3896 0.090 Uiso 1 1 calc R . . C30 C 0.4980(12) 0.3065(6) 0.3176(8) 0.047(3) Uani 1 1 d . A . H53 H 0.5513 0.3260 0.3588 0.071 Uiso 1 1 calc R . . H54 H 0.4214 0.3293 0.3181 0.071 Uiso 1 1 calc R . . H55 H 0.5286 0.3171 0.2699 0.071 Uiso 1 1 calc R . . C31 C 0.4961(13) 0.1672(7) 0.2326(7) 0.053(4) Uani 1 1 d . A . H56 H 0.5333 0.1190 0.2368 0.079 Uiso 1 1 calc R . . H57 H 0.5431 0.2002 0.2051 0.079 Uiso 1 1 calc R . . H58 H 0.4183 0.1626 0.2056 0.079 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 0.01814(19) 0.02355(19) 0.01982(18) 0.00274(16) 0.00285(12) 0.00003(17) Cl1 0.054(2) 0.071(2) 0.0445(18) 0.0258(16) -0.0099(15) -0.0243(18) P1 0.0175(12) 0.0197(12) 0.0232(12) 0.0028(9) 0.0028(9) -0.0014(10) Si1 0.0194(14) 0.0236(13) 0.0267(14) 0.0015(10) -0.0010(11) 0.0003(11) Si2 0.0197(14) 0.0223(13) 0.0266(14) 0.0037(10) 0.0037(11) 0.0004(11) Si3 0.0396(19) 0.0413(18) 0.0240(15) -0.0059(12) -0.0012(13) -0.0010(14) Si4 0.0244(16) 0.0283(15) 0.0384(17) 0.0003(12) 0.0090(13) 0.0003(12) N1 0.019(4) 0.027(4) 0.023(4) 0.010(3) 0.000(3) 0.000(3) C1 0.020(5) 0.017(4) 0.022(5) 0.001(3) 0.010(4) 0.000(4) C2 0.020(5) 0.027(5) 0.026(5) 0.003(4) 0.008(4) 0.006(4) C3 0.028(6) 0.022(5) 0.036(6) 0.000(4) 0.011(5) -0.007(4) C4 0.022(6) 0.027(5) 0.053(7) -0.007(5) 0.021(5) -0.006(4) C5 0.015(5) 0.023(5) 0.051(7) -0.008(4) 0.005(4) 0.000(4) C6 0.020(5) 0.023(5) 0.036(6) -0.004(4) 0.000(4) -0.004(4) C7 0.022(6) 0.044(6) 0.041(7) -0.017(5) 0.005(5) -0.012(5) C8 0.023(5) 0.009(4) 0.029(5) 0.012(3) 0.001(4) -0.005(4) C9 0.036(7) 0.025(6) 0.047(7) 0.001(5) 0.013(5) 0.009(5) C10 0.037(8) 0.024(6) 0.099(12) 0.008(6) 0.013(7) 0.003(5) C11 0.033(7) 0.043(7) 0.072(10) 0.030(7) -0.004(6) 0.008(6) C12 0.045(8) 0.034(7) 0.066(9) 0.030(6) -0.016(7) -0.005(6) C13 0.029(6) 0.032(6) 0.038(6) 0.009(5) -0.004(5) -0.006(5) C14 0.016(5) 0.023(5) 0.023(5) 0.001(4) 0.002(4) -0.004(4) C15 0.016(5) 0.025(5) 0.030(5) -0.002(4) 0.004(4) -0.003(4) C16 0.024(6) 0.043(6) 0.037(6) 0.001(5) 0.012(5) 0.003(5) C17 0.033(7) 0.042(7) 0.045(7) -0.017(5) 0.016(5) 0.001(5) C18 0.035(7) 0.027(5) 0.040(6) -0.010(5) 0.010(5) 0.003(5) C19 0.024(5) 0.023(5) 0.029(5) 0.000(4) 0.009(4) -0.002(4) C20 0.040(7) 0.074(9) 0.019(5) -0.004(5) 0.012(5) -0.011(6) C21 0.041(7) 0.042(7) 0.049(7) 0.023(6) 0.001(6) 0.003(6) C23 0.035(7) 0.031(6) 0.039(6) 0.021(5) -0.007(5) -0.008(5) C24 0.012(5) 0.025(5) 0.069(8) -0.018(5) 0.000(5) 0.002(4) C25 0.020(5) 0.017(4) 0.020(5) 0.001(3) 0.004(4) 0.003(4) C26 0.062(10) 0.099(12) 0.018(6) -0.016(6) 0.013(6) 0.010(8) C27 0.046(8) 0.073(9) 0.039(7) 0.006(7) -0.006(6) -0.010(7) C28 0.080(11) 0.057(9) 0.046(8) -0.015(7) -0.006(8) -0.017(8) C29 0.030(8) 0.069(10) 0.084(11) 0.017(8) 0.015(7) 0.004(7) C30 0.047(8) 0.038(7) 0.057(8) -0.002(6) 0.007(6) -0.005(6) C31 0.073(10) 0.045(7) 0.047(8) -0.009(6) 0.042(7) 0.000(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 Si1 2.307(3) . ? Ir1 P1 2.314(2) . ? Ir1 N1 2.325(8) . ? Ir1 Si2 2.440(3) . ? Cl1 Si1 2.113(4) . ? P1 C1 1.835(9) . ? P1 C14 1.848(10) . ? P1 C8 1.859(9) . ? Si1 C22 1.918(12) . ? Si1 C25 1.923(10) . ? Si1 Si2 2.670(4) . ? Si2 C23 1.883(10) . ? Si2 C25 1.935(9) . ? Si2 C24 1.938(11) . ? Si3 C26 1.883(14) . ? Si3 C25 1.884(9) . ? Si3 C27 1.884(14) . ? Si3 C28 1.889(14) . ? Si4 C29 1.847(14) . ? Si4 C30 1.877(12) . ? Si4 C31 1.884(12) . ? Si4 C25 1.884(10) . ? N1 C2 1.469(13) . ? N1 C20 1.490(13) . ? N1 C21 1.493(13) . ? C1 C2 1.392(13) . ? C1 C6 1.420(14) . ? C2 C3 1.395(14) . ? C3 C4 1.387(16) . ? C3 H1 0.9500 . ? C4 C5 1.360(16) . ? C4 H2 0.9500 . ? C5 C6 1.370(14) . ? C5 C7 1.500(15) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C9 1.517(14) . ? C8 C13 1.541(14) . ? C8 H7 1.0000 . ? C9 C10 1.525(15) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.51(2) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.498(19) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.523(14) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C19 1.521(13) . ? C14 C15 1.533(13) . ? C14 H18 1.0000 . ? C15 C16 1.530(14) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.503(16) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.525(15) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.516(13) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C23 H35 0.9800 . ? C23 H36 0.9800 . ? C23 H37 0.9800 . ? C24 H38 0.9800 . ? C24 H39 0.9800 . ? C24 H40 0.9800 . ? C26 H41 0.9800 . ? C26 H42 0.9800 . ? C26 H43 0.9800 . ? C27 H44 0.9800 . ? C27 H45 0.9800 . ? C27 H46 0.9800 . ? C28 H47 0.9800 . ? C28 H48 0.9800 . ? C28 H49 0.9800 . ? C29 H50 0.9800 . ? C29 H51 0.9800 . ? C29 H52 0.9800 . ? C30 H53 0.9800 . ? C30 H54 0.9800 . ? C30 H55 0.9800 . ? C31 H56 0.9800 . ? C31 H57 0.9800 . ? C31 H58 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 Si1 Ir1 P1 105.54(9) . . ? Si1 Ir1 N1 163.0(2) . . ? P1 Ir1 N1 82.1(2) . . ? Si1 Ir1 Si2 68.37(9) . . ? P1 Ir1 Si2 125.64(9) . . ? N1 Ir1 Si2 119.8(2) . . ? C1 P1 C14 101.4(4) . . ? C1 P1 C8 104.5(4) . . ? C14 P1 C8 106.9(4) . . ? C1 P1 Ir1 103.5(3) . . ? C14 P1 Ir1 121.3(3) . . ? C8 P1 Ir1 116.6(3) . . ? C22 Si1 C25 114.4(5) . . ? C22 Si1 Cl1 97.9(4) . . ? C25 Si1 Cl1 108.5(3) . . ? C22 Si1 Ir1 117.9(4) . . ? C25 Si1 Ir1 103.3(3) . . ? Cl1 Si1 Ir1 115.09(16) . . ? C22 Si1 Si2 144.3(4) . . ? C25 Si1 Si2 46.4(3) . . ? Cl1 Si1 Si2 116.18(17) . . ? Ir1 Si1 Si2 58.19(9) . . ? C23 Si2 C25 115.2(5) . . ? C23 Si2 C24 100.9(6) . . ? C25 Si2 C24 111.1(4) . . ? C23 Si2 Ir1 112.1(4) . . ? C25 Si2 Ir1 98.2(3) . . ? C24 Si2 Ir1 120.2(4) . . ? C23 Si2 Si1 136.9(4) . . ? C25 Si2 Si1 46.0(3) . . ? C24 Si2 Si1 121.7(4) . . ? Ir1 Si2 Si1 53.44(8) . . ? C26 Si3 C25 115.2(5) . . ? C26 Si3 C27 104.0(7) . . ? C25 Si3 C27 114.5(5) . . ? C26 Si3 C28 105.1(7) . . ? C25 Si3 C28 112.4(5) . . ? C27 Si3 C28 104.5(7) . . ? C29 Si4 C30 106.0(7) . . ? C29 Si4 C31 102.4(7) . . ? C30 Si4 C31 104.4(6) . . ? C29 Si4 C25 113.0(5) . . ? C30 Si4 C25 111.7(5) . . ? C31 Si4 C25 118.1(5) . . ? C2 N1 C20 109.2(8) . . ? C2 N1 C21 109.2(8) . . ? C20 N1 C21 109.4(9) . . ? C2 N1 Ir1 113.4(6) . . ? C20 N1 Ir1 105.9(7) . . ? C21 N1 Ir1 109.7(7) . . ? C2 C1 C6 119.6(9) . . ? C2 C1 P1 118.1(8) . . ? C6 C1 P1 122.3(7) . . ? C1 C2 C3 118.4(10) . . ? C1 C2 N1 121.6(9) . . ? C3 C2 N1 119.9(9) . . ? C4 C3 C2 120.0(10) . . ? C4 C3 H1 120.0 . . ? C2 C3 H1 120.0 . . ? C5 C4 C3 122.4(10) . . ? C5 C4 H2 118.8 . . ? C3 C4 H2 118.8 . . ? C4 C5 C6 118.5(10) . . ? C4 C5 C7 122.0(10) . . ? C6 C5 C7 119.5(10) . . ? C5 C6 C1 121.1(10) . . ? C5 C6 H3 119.5 . . ? C1 C6 H3 119.5 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C9 C8 C13 110.8(9) . . ? C9 C8 P1 111.9(7) . . ? C13 C8 P1 117.5(7) . . ? C9 C8 H7 105.2 . . ? C13 C8 H7 105.2 . . ? P1 C8 H7 105.2 . . ? C8 C9 C10 110.9(9) . . ? C8 C9 H8 109.5 . . ? C10 C9 H8 109.5 . . ? C8 C9 H9 109.5 . . ? C10 C9 H9 109.5 . . ? H8 C9 H9 108.1 . . ? C11 C10 C9 111.6(11) . . ? C11 C10 H10 109.3 . . ? C9 C10 H10 109.3 . . ? C11 C10 H11 109.3 . . ? C9 C10 H11 109.3 . . ? H10 C10 H11 108.0 . . ? C12 C11 C10 111.7(10) . . ? C12 C11 H12 109.3 . . ? C10 C11 H12 109.3 . . ? C12 C11 H13 109.3 . . ? C10 C11 H13 109.3 . . ? H12 C11 H13 107.9 . . ? C11 C12 C13 110.8(10) . . ? C11 C12 H14 109.5 . . ? C13 C12 H14 109.5 . . ? C11 C12 H15 109.5 . . ? C13 C12 H15 109.5 . . ? H14 C12 H15 108.1 . . ? C12 C13 C8 109.9(9) . . ? C12 C13 H16 109.7 . . ? C8 C13 H16 109.7 . . ? C12 C13 H17 109.7 . . ? C8 C13 H17 109.7 . . ? H16 C13 H17 108.2 . . ? C19 C14 C15 109.5(8) . . ? C19 C14 P1 111.4(6) . . ? C15 C14 P1 112.0(6) . . ? C19 C14 H18 107.9 . . ? C15 C14 H18 107.9 . . ? P1 C14 H18 107.9 . . ? C16 C15 C14 112.3(8) . . ? C16 C15 H19 109.2 . . ? C14 C15 H19 109.2 . . ? C16 C15 H20 109.2 . . ? C14 C15 H20 109.2 . . ? H19 C15 H20 107.9 . . ? C17 C16 C15 110.7(9) . . ? C17 C16 H21 109.5 . . ? C15 C16 H21 109.5 . . ? C17 C16 H22 109.5 . . ? C15 C16 H22 109.5 . . ? H21 C16 H22 108.1 . . ? C16 C17 C18 112.5(10) . . ? C16 C17 H23 109.1 . . ? C18 C17 H23 109.1 . . ? C16 C17 H24 109.1 . . ? C18 C17 H24 109.1 . . ? H23 C17 H24 107.8 . . ? C19 C18 C17 110.6(9) . . ? C19 C18 H25 109.5 . . ? C17 C18 H25 109.5 . . ? C19 C18 H26 109.5 . . ? C17 C18 H26 109.5 . . ? H25 C18 H26 108.1 . . ? C18 C19 C14 112.7(8) . . ? C18 C19 H27 109.1 . . ? C14 C19 H27 109.1 . . ? C18 C19 H28 109.1 . . ? C14 C19 H28 109.1 . . ? H27 C19 H28 107.8 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? Si2 C23 H35 109.5 . . ? Si2 C23 H36 109.5 . . ? H35 C23 H36 109.5 . . ? Si2 C23 H37 109.5 . . ? H35 C23 H37 109.5 . . ? H36 C23 H37 109.5 . . ? Si2 C24 H38 109.5 . . ? Si2 C24 H39 109.5 . . ? H38 C24 H39 109.5 . . ? Si2 C24 H40 109.5 . . ? H38 C24 H40 109.5 . . ? H39 C24 H40 109.5 . . ? Si3 C25 Si4 111.7(5) . . ? Si3 C25 Si1 112.4(5) . . ? Si4 C25 Si1 114.1(5) . . ? Si3 C25 Si2 110.5(5) . . ? Si4 C25 Si2 118.4(5) . . ? Si1 C25 Si2 87.6(4) . . ? Si3 C26 H41 109.5 . . ? Si3 C26 H42 109.5 . . ? H41 C26 H42 109.5 . . ? Si3 C26 H43 109.5 . . ? H41 C26 H43 109.5 . . ? H42 C26 H43 109.5 . . ? Si3 C27 H44 109.5 . . ? Si3 C27 H45 109.5 . . ? H44 C27 H45 109.5 . . ? Si3 C27 H46 109.5 . . ? H44 C27 H46 109.5 . . ? H45 C27 H46 109.5 . . ? Si3 C28 H47 109.5 . . ? Si3 C28 H48 109.5 . . ? H47 C28 H48 109.5 . . ? Si3 C28 H49 109.5 . . ? H47 C28 H49 109.5 . . ? H48 C28 H49 109.5 . . ? Si4 C29 H50 109.5 . . ? Si4 C29 H51 109.5 . . ? H50 C29 H51 109.5 . . ? Si4 C29 H52 109.5 . . ? H50 C29 H52 109.5 . . ? H51 C29 H52 109.5 . . ? Si4 C30 H53 109.5 . . ? Si4 C30 H54 109.5 . . ? H53 C30 H54 109.5 . . ? Si4 C30 H55 109.5 . . ? H53 C30 H55 109.5 . . ? H54 C30 H55 109.5 . . ? Si4 C31 H56 109.5 . . ? Si4 C31 H57 109.5 . . ? H56 C31 H57 109.5 . . ? Si4 C31 H58 109.5 . . ? H56 C31 H58 109.5 . . ? H57 C31 H58 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 Si1 Ir1 P1 C1 -155.6(3) . . . . ? N1 Ir1 P1 C1 8.9(4) . . . . ? Si2 Ir1 P1 C1 130.1(3) . . . . ? Si1 Ir1 P1 C14 91.9(4) . . . . ? N1 Ir1 P1 C14 -103.7(4) . . . . ? Si2 Ir1 P1 C14 17.6(4) . . . . ? Si1 Ir1 P1 C8 -41.5(4) . . . . ? N1 Ir1 P1 C8 123.0(4) . . . . ? Si2 Ir1 P1 C8 -115.7(4) . . . . ? P1 Ir1 Si1 C22 98.5(4) . . . . ? N1 Ir1 Si1 C22 -16.5(8) . . . . ? Si2 Ir1 Si1 C22 -138.8(5) . . . . ? P1 Ir1 Si1 C25 -134.3(3) . . . . ? N1 Ir1 Si1 C25 110.7(7) . . . . ? Si2 Ir1 Si1 C25 -11.6(3) . . . . ? P1 Ir1 Si1 Cl1 -16.27(19) . . . . ? N1 Ir1 Si1 Cl1 -131.3(7) . . . . ? Si2 Ir1 Si1 Cl1 106.43(19) . . . . ? P1 Ir1 Si1 Si2 -122.70(10) . . . . ? N1 Ir1 Si1 Si2 122.3(7) . . . . ? Si1 Ir1 Si2 C23 132.8(4) . . . . ? P1 Ir1 Si2 C23 -133.1(4) . . . . ? N1 Ir1 Si2 C23 -30.6(5) . . . . ? Si1 Ir1 Si2 C25 11.3(3) . . . . ? P1 Ir1 Si2 C25 105.3(3) . . . . ? N1 Ir1 Si2 C25 -152.1(4) . . . . ? Si1 Ir1 Si2 C24 -109.0(4) . . . . ? P1 Ir1 Si2 C24 -14.9(4) . . . . ? N1 Ir1 Si2 C24 87.6(5) . . . . ? P1 Ir1 Si2 Si1 94.03(12) . . . . ? N1 Ir1 Si2 Si1 -163.4(2) . . . . ? C22 Si1 Si2 C23 10.8(9) . . . . ? C25 Si1 Si2 C23 80.5(7) . . . . ? Cl1 Si1 Si2 C23 171.6(5) . . . . ? Ir1 Si1 Si2 C23 -83.9(5) . . . . ? C22 Si1 Si2 C25 -69.8(8) . . . . ? Cl1 Si1 Si2 C25 91.1(4) . . . . ? Ir1 Si1 Si2 C25 -164.4(4) . . . . ? C22 Si1 Si2 C24 -159.3(8) . . . . ? C25 Si1 Si2 C24 -89.5(5) . . . . ? Cl1 Si1 Si2 C24 1.6(4) . . . . ? Ir1 Si1 Si2 C24 106.1(4) . . . . ? C22 Si1 Si2 Ir1 94.6(7) . . . . ? C25 Si1 Si2 Ir1 164.4(4) . . . . ? Cl1 Si1 Si2 Ir1 -104.54(17) . . . . ? Si1 Ir1 N1 C2 107.5(8) . . . . ? P1 Ir1 N1 C2 -10.7(6) . . . . ? Si2 Ir1 N1 C2 -137.5(5) . . . . ? Si1 Ir1 N1 C20 -12.2(12) . . . . ? P1 Ir1 N1 C20 -130.4(7) . . . . ? Si2 Ir1 N1 C20 102.8(7) . . . . ? Si1 Ir1 N1 C21 -130.2(8) . . . . ? P1 Ir1 N1 C21 111.7(7) . . . . ? Si2 Ir1 N1 C21 -15.1(8) . . . . ? C14 P1 C1 C2 118.6(8) . . . . ? C8 P1 C1 C2 -130.4(8) . . . . ? Ir1 P1 C1 C2 -7.8(8) . . . . ? C14 P1 C1 C6 -61.7(9) . . . . ? C8 P1 C1 C6 49.3(9) . . . . ? Ir1 P1 C1 C6 171.9(7) . . . . ? C6 C1 C2 C3 2.4(14) . . . . ? P1 C1 C2 C3 -177.8(7) . . . . ? C6 C1 C2 N1 179.6(8) . . . . ? P1 C1 C2 N1 -0.6(12) . . . . ? C20 N1 C2 C1 127.0(10) . . . . ? C21 N1 C2 C1 -113.4(10) . . . . ? Ir1 N1 C2 C1 9.2(11) . . . . ? C20 N1 C2 C3 -55.8(12) . . . . ? C21 N1 C2 C3 63.8(12) . . . . ? Ir1 N1 C2 C3 -173.6(7) . . . . ? C1 C2 C3 C4 -4.0(14) . . . . ? N1 C2 C3 C4 178.7(9) . . . . ? C2 C3 C4 C5 3.1(16) . . . . ? C3 C4 C5 C6 -0.4(16) . . . . ? C3 C4 C5 C7 -179.8(10) . . . . ? C4 C5 C6 C1 -1.3(15) . . . . ? C7 C5 C6 C1 178.1(9) . . . . ? C2 C1 C6 C5 0.3(14) . . . . ? P1 C1 C6 C5 -179.5(8) . . . . ? C1 P1 C8 C9 44.3(8) . . . . ? C14 P1 C8 C9 151.3(8) . . . . ? Ir1 P1 C8 C9 -69.2(8) . . . . ? C1 P1 C8 C13 -85.5(8) . . . . ? C14 P1 C8 C13 21.5(9) . . . . ? Ir1 P1 C8 C13 161.0(6) . . . . ? C13 C8 C9 C10 -55.6(12) . . . . ? P1 C8 C9 C10 171.1(9) . . . . ? C8 C9 C10 C11 54.3(14) . . . . ? C9 C10 C11 C12 -55.1(14) . . . . ? C10 C11 C12 C13 57.0(14) . . . . ? C11 C12 C13 C8 -57.7(13) . . . . ? C9 C8 C13 C12 57.3(11) . . . . ? P1 C8 C13 C12 -172.4(8) . . . . ? C1 P1 C14 C19 -56.1(8) . . . . ? C8 P1 C14 C19 -165.3(7) . . . . ? Ir1 P1 C14 C19 57.5(8) . . . . ? C1 P1 C14 C15 -179.1(7) . . . . ? C8 P1 C14 C15 71.7(8) . . . . ? Ir1 P1 C14 C15 -65.5(7) . . . . ? C19 C14 C15 C16 55.0(11) . . . . ? P1 C14 C15 C16 179.1(7) . . . . ? C14 C15 C16 C17 -55.2(12) . . . . ? C15 C16 C17 C18 54.7(13) . . . . ? C16 C17 C18 C19 -54.8(13) . . . . ? C17 C18 C19 C14 55.4(13) . . . . ? C15 C14 C19 C18 -55.4(11) . . . . ? P1 C14 C19 C18 -179.8(7) . . . . ? C26 Si3 C25 Si4 167.9(6) . . . . ? C27 Si3 C25 Si4 -71.5(7) . . . . ? C28 Si3 C25 Si4 47.5(8) . . . . ? C26 Si3 C25 Si1 38.1(8) . . . . ? C27 Si3 C25 Si1 158.7(6) . . . . ? C28 Si3 C25 Si1 -82.3(7) . . . . ? C26 Si3 C25 Si2 -58.0(8) . . . . ? C27 Si3 C25 Si2 62.6(7) . . . . ? C28 Si3 C25 Si2 -178.4(7) . . . . ? C29 Si4 C25 Si3 48.8(8) . . . . ? C30 Si4 C25 Si3 -70.7(7) . . . . ? C31 Si4 C25 Si3 168.2(6) . . . . ? C29 Si4 C25 Si1 177.7(7) . . . . ? C30 Si4 C25 Si1 58.3(7) . . . . ? C31 Si4 C25 Si1 -62.9(7) . . . . ? C29 Si4 C25 Si2 -81.3(8) . . . . ? C30 Si4 C25 Si2 159.2(6) . . . . ? C31 Si4 C25 Si2 38.0(8) . . . . ? C22 Si1 C25 Si3 31.8(7) . . . . ? Cl1 Si1 C25 Si3 139.9(4) . . . . ? Ir1 Si1 C25 Si3 -97.6(4) . . . . ? Si2 Si1 C25 Si3 -111.2(6) . . . . ? C22 Si1 C25 Si4 -96.8(6) . . . . ? Cl1 Si1 C25 Si4 11.3(5) . . . . ? Ir1 Si1 C25 Si4 133.8(4) . . . . ? Si2 Si1 C25 Si4 120.2(6) . . . . ? C22 Si1 C25 Si2 143.0(5) . . . . ? Cl1 Si1 C25 Si2 -108.9(3) . . . . ? Ir1 Si1 C25 Si2 13.6(3) . . . . ? C23 Si2 C25 Si3 -18.8(7) . . . . ? C24 Si2 C25 Si3 -132.7(5) . . . . ? Ir1 Si2 C25 Si3 100.4(4) . . . . ? Si1 Si2 C25 Si3 113.0(6) . . . . ? C23 Si2 C25 Si4 111.9(6) . . . . ? C24 Si2 C25 Si4 -2.0(7) . . . . ? Ir1 Si2 C25 Si4 -128.9(5) . . . . ? Si1 Si2 C25 Si4 -116.3(6) . . . . ? C23 Si2 C25 Si1 -131.8(5) . . . . ? C24 Si2 C25 Si1 114.2(5) . . . . ? Ir1 Si2 C25 Si1 -12.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.197 _refine_diff_density_min -2.692 _refine_diff_density_rms 0.253 #===END data_(PcyN-P,N)RhH[SiMe2C(SiMe3)2SiClMe-Si,Si]-(10)-?C7H8 _database_code_depnum_ccdc_archive 'CCDC 772167' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H62 Cl N P Rh Si4, C7 H8' _chemical_formula_sum 'C38 H70 Cl N P Rh Si4' _chemical_formula_weight 822.64 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.53940(10) _cell_length_b 13.1147(2) _cell_length_c 19.6455(5) _cell_angle_alpha 70.960(4) _cell_angle_beta 77.3979(19) _cell_angle_gamma 71.675(3) _cell_volume 2187.11(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9660 _cell_measurement_theta_min 1.11 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8854 _exptl_absorpt_correction_T_max 0.9014 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19687 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9660 _reflns_number_gt 7779 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0554P)^2^+4.7362P] 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 9660 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1448 _refine_ls_wR_factor_gt 0.1351 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.167 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.03537(4) 0.20851(3) 0.218961(17) 0.01835(10) Uani 1 1 d . A . H1 H 0.070(8) 0.087(6) 0.203(4) 0.08(2) Uiso 1 1 d . . . Cl1 Cl 0.4132(7) 0.2057(5) 0.1679(3) 0.0374(12) Uani 0.589(6) 1 d P A 1 Cl2 Cl 0.3367(6) 0.0136(5) 0.1297(3) 0.0488(16) Uiso 0.411(6) 1 d P A 2 P1 P -0.03569(11) 0.39045(9) 0.22765(5) 0.0163(2) Uani 1 1 d . A . Si1 Si 0.27049(14) 0.09866(10) 0.20724(6) 0.0237(3) Uani 1 1 d . . . Si2 Si 0.11156(14) 0.10320(10) 0.33143(6) 0.0225(3) Uani 1 1 d . A . Si3 Si 0.27686(15) -0.14052(10) 0.31604(7) 0.0274(3) Uani 1 1 d . . . Si4 Si 0.47674(15) -0.00631(12) 0.33466(8) 0.0318(3) Uani 1 1 d . . . N1 N -0.1025(4) 0.2894(3) 0.12335(19) 0.0222(7) Uani 1 1 d . . . C1 C -0.1521(4) 0.4679(4) 0.1542(2) 0.0188(8) Uani 1 1 d . . . C2 C -0.1715(4) 0.4089(4) 0.1107(2) 0.0204(8) Uani 1 1 d . A . C3 C -0.2590(5) 0.4674(4) 0.0539(2) 0.0290(10) Uani 1 1 d . . . H2 H -0.2741 0.4281 0.0243 0.035 Uiso 1 1 calc R A . C4 C -0.3238(5) 0.5818(5) 0.0403(2) 0.0329(11) Uani 1 1 d . A . H3 H -0.3820 0.6197 0.0014 0.040 Uiso 1 1 calc R . . C5 C -0.3046(5) 0.6407(4) 0.0825(2) 0.0307(11) Uani 1 1 d . . . C6 C -0.2187(5) 0.5841(4) 0.1387(2) 0.0237(9) Uani 1 1 d . A . H4 H -0.2043 0.6246 0.1676 0.028 Uiso 1 1 calc R . . C7 C -0.3766(7) 0.7657(5) 0.0685(3) 0.0478(15) Uani 1 1 d . A . H5 H -0.3762 0.8006 0.0161 0.072 Uiso 1 1 calc R . . H6 H -0.3206 0.7988 0.0878 0.072 Uiso 1 1 calc R . . H7 H -0.4795 0.7781 0.0926 0.072 Uiso 1 1 calc R . . C8 C -0.1618(4) 0.4023(3) 0.3127(2) 0.0177(8) Uani 1 1 d . . . H8 H -0.1021 0.3536 0.3531 0.021 Uiso 1 1 calc R A . C9 C -0.2876(5) 0.3490(4) 0.3194(2) 0.0222(9) Uani 1 1 d . A . H9 H -0.2447 0.2740 0.3113 0.027 Uiso 1 1 calc R . . H10 H -0.3529 0.3955 0.2816 0.027 Uiso 1 1 calc R . . C10 C -0.4383(5) 0.4501(4) 0.4128(2) 0.0274(10) Uani 1 1 d . A . H11 H -0.5133 0.5011 0.3806 0.033 Uiso 1 1 calc R . . H12 H -0.4878 0.4381 0.4636 0.033 Uiso 1 1 calc R . . C11 C -0.3799(5) 0.3383(4) 0.3945(2) 0.0264(9) Uani 1 1 d . . . H13 H -0.4651 0.3095 0.3959 0.032 Uiso 1 1 calc R A . H14 H -0.3177 0.2835 0.4317 0.032 Uiso 1 1 calc R . . C12 C -0.3131(5) 0.5042(4) 0.4038(2) 0.0262(9) Uani 1 1 d . . . H15 H -0.2450 0.4578 0.4404 0.031 Uiso 1 1 calc R A . H16 H -0.3558 0.5787 0.4126 0.031 Uiso 1 1 calc R . . C13 C -0.2244(5) 0.5172(4) 0.3277(2) 0.0227(9) Uani 1 1 d . A . H17 H -0.1417 0.5498 0.3243 0.027 Uiso 1 1 calc R . . H18 H -0.2900 0.5684 0.2909 0.027 Uiso 1 1 calc R . . C14 C 0.0882(4) 0.4807(3) 0.2146(2) 0.0177(8) Uani 1 1 d . . . H19 H 0.0244 0.5554 0.2195 0.021 Uiso 1 1 calc R A . C15 C 0.1910(5) 0.4317(4) 0.2740(2) 0.0228(9) Uani 1 1 d . A . H20 H 0.1299 0.4268 0.3220 0.027 Uiso 1 1 calc R . . H21 H 0.2493 0.3549 0.2727 0.027 Uiso 1 1 calc R . . C16 C 0.2974(5) 0.5026(5) 0.2642(3) 0.0319(11) Uani 1 1 d . . . H22 H 0.3663 0.4657 0.3014 0.038 Uiso 1 1 calc R A . H23 H 0.2397 0.5765 0.2713 0.038 Uiso 1 1 calc R . . C17 C 0.3871(5) 0.5190(5) 0.1887(3) 0.0371(12) Uani 1 1 d . A . H24 H 0.4511 0.5686 0.1829 0.045 Uiso 1 1 calc R . . H25 H 0.4525 0.4459 0.1832 0.045 Uiso 1 1 calc R . . C18 C 0.2840(6) 0.5704(5) 0.1299(3) 0.0357(12) Uani 1 1 d . . . H26 H 0.3443 0.5773 0.0815 0.043 Uiso 1 1 calc R A . H27 H 0.2251 0.6464 0.1326 0.043 Uiso 1 1 calc R . . C19 C 0.1779(5) 0.4983(4) 0.1389(2) 0.0247(9) Uani 1 1 d . A . H28 H 0.1089 0.5354 0.1017 0.030 Uiso 1 1 calc R . . H29 H 0.2363 0.4248 0.1314 0.030 Uiso 1 1 calc R . . C20 C -0.2207(6) 0.2285(5) 0.1418(3) 0.0390(12) Uani 1 1 d . A . H30 H -0.2866 0.2435 0.1852 0.059 Uiso 1 1 calc R . . H31 H -0.1742 0.1480 0.1510 0.059 Uiso 1 1 calc R . . H32 H -0.2789 0.2542 0.1011 0.059 Uiso 1 1 calc R . . C21 C -0.0014(6) 0.2644(5) 0.0581(3) 0.0353(11) Uani 1 1 d . A . H33 H -0.0588 0.2883 0.0173 0.053 Uiso 1 1 calc R . . H34 H 0.0455 0.1838 0.0685 0.053 Uiso 1 1 calc R . . H35 H 0.0758 0.3046 0.0455 0.053 Uiso 1 1 calc R . . C22 C 0.3717(13) 0.0114(9) 0.1287(5) 0.021(2) Uiso 0.589(6) 1 d P A 1 C23 C 0.411(4) 0.187(3) 0.1690(19) 0.026(7) Uiso 0.411(6) 1 d P A 2 C24 C -0.0425(5) 0.0329(4) 0.3841(3) 0.0353(11) Uani 1 1 d . . . H36 H -0.0096 -0.0207 0.4295 0.053 Uiso 1 1 calc R A . H37 H -0.0645 -0.0065 0.3547 0.053 Uiso 1 1 calc R . . H38 H -0.1323 0.0897 0.3952 0.053 Uiso 1 1 calc R . . C25 C 0.1336(5) 0.1662(4) 0.4032(2) 0.0245(9) Uani 1 1 d . . . H39 H 0.0350 0.1991 0.4261 0.037 Uiso 1 1 calc R A . H40 H 0.1866 0.2242 0.3797 0.037 Uiso 1 1 calc R . . H41 H 0.1903 0.1072 0.4402 0.037 Uiso 1 1 calc R . . C26 C 0.2999(5) 0.0035(4) 0.3017(2) 0.0221(8) Uani 1 1 d . A . C27 C 0.1281(7) -0.1463(5) 0.2694(3) 0.0425(13) Uani 1 1 d . A . H42 H 0.1598 -0.1299 0.2169 0.064 Uiso 1 1 calc R . . H43 H 0.0354 -0.0909 0.2792 0.064 Uiso 1 1 calc R . . H44 H 0.1115 -0.2212 0.2877 0.064 Uiso 1 1 calc R . . C28 C 0.2350(7) -0.2138(5) 0.4147(3) 0.0451(14) Uani 1 1 d . A . H45 H 0.1441 -0.2379 0.4222 0.068 Uiso 1 1 calc R . . H46 H 0.2208 -0.1625 0.4439 0.068 Uiso 1 1 calc R . . H47 H 0.3183 -0.2792 0.4294 0.068 Uiso 1 1 calc R . . C29 C 0.4497(6) -0.2354(4) 0.2805(3) 0.0442(13) Uani 1 1 d . A . H48 H 0.4273 -0.3035 0.2807 0.066 Uiso 1 1 calc R . . H49 H 0.5274 -0.2552 0.3115 0.066 Uiso 1 1 calc R . . H50 H 0.4845 -0.1971 0.2308 0.066 Uiso 1 1 calc R . . C30 C 0.4966(7) 0.1265(5) 0.3434(3) 0.0456(14) Uani 1 1 d . A . H51 H 0.4586 0.1890 0.3025 0.068 Uiso 1 1 calc R . . H52 H 0.6019 0.1198 0.3433 0.068 Uiso 1 1 calc R . . H53 H 0.4397 0.1402 0.3890 0.068 Uiso 1 1 calc R . . C31 C 0.5020(7) -0.1055(6) 0.4278(3) 0.0542(17) Uani 1 1 d . A . H54 H 0.5954 -0.1070 0.4416 0.081 Uiso 1 1 calc R . . H55 H 0.5051 -0.1807 0.4274 0.081 Uiso 1 1 calc R . . H56 H 0.4185 -0.0805 0.4629 0.081 Uiso 1 1 calc R . . C32 C 0.6468(6) -0.0544(6) 0.2712(4) 0.0508(15) Uani 1 1 d . A . H57 H 0.6277 -0.0168 0.2208 0.076 Uiso 1 1 calc R . . H58 H 0.6691 -0.1355 0.2800 0.076 Uiso 1 1 calc R . . H59 H 0.7318 -0.0357 0.2800 0.076 Uiso 1 1 calc R . . C33 C 0.271(3) -0.054(2) -0.0319(13) 0.112(7) Uiso 0.50 1 d P . . C34 C 0.1077(7) -0.0212(10) -0.0092(6) 0.059(3) Uiso 0.50 1 d PG . . C35 C 0.0575(12) -0.0804(8) 0.0598(5) 0.064(4) Uiso 0.50 1 d PG . . C36 C -0.0942(13) -0.0600(10) 0.0841(5) 0.083(5) Uiso 0.50 1 d PG . . C37 C -0.1956(8) 0.0195(11) 0.0395(7) 0.084(5) Uiso 0.50 1 d PG . . C38 C -0.1454(10) 0.0786(9) -0.0295(6) 0.071(4) Uiso 0.50 1 d PG . . C39 C 0.0063(11) 0.0583(9) -0.0538(4) 0.061(4) Uiso 0.50 1 d PG . . C40 C -0.1327(16) 0.7008(12) 0.4414(8) 0.057(3) Uiso 0.50 1 d P . . C41 C -0.0506(8) 0.5802(4) 0.4766(4) 0.041(2) Uiso 0.50 1 d PG . . C42 C -0.1085(7) 0.5228(6) 0.5444(4) 0.035(2) Uiso 0.50 1 d PG . . C43 C -0.0350(9) 0.4127(6) 0.5763(3) 0.047(3) Uiso 0.50 1 d PG . . C44 C 0.0964(9) 0.3602(4) 0.5404(4) 0.049(3) Uiso 0.50 1 d PG . . C45 C 0.1543(6) 0.4176(5) 0.4726(4) 0.041(2) Uiso 0.50 1 d PG . . C46 C 0.0808(8) 0.5276(5) 0.4407(3) 0.0250(18) Uiso 0.50 1 d PG . . 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 Rh1 0.02150(17) 0.01556(16) 0.01792(16) -0.00496(11) -0.00401(11) -0.00346(12) Cl1 0.0275(15) 0.028(2) 0.0476(19) -0.0020(16) 0.0061(9) -0.0109(16) P1 0.0151(5) 0.0174(5) 0.0159(5) -0.0043(4) -0.0024(4) -0.0037(4) Si1 0.0266(6) 0.0191(6) 0.0199(6) -0.0036(4) 0.0010(4) -0.0030(5) Si2 0.0250(6) 0.0198(6) 0.0180(6) -0.0028(4) -0.0017(4) -0.0028(5) Si3 0.0368(7) 0.0174(6) 0.0278(6) -0.0022(5) -0.0107(5) -0.0067(5) Si4 0.0273(7) 0.0314(7) 0.0368(7) -0.0057(6) -0.0100(5) -0.0077(6) N1 0.0226(18) 0.027(2) 0.0195(17) -0.0072(14) -0.0013(14) -0.0102(15) C1 0.0152(19) 0.023(2) 0.0150(18) -0.0018(15) 0.0001(14) -0.0064(16) C2 0.0162(19) 0.024(2) 0.0182(19) -0.0036(16) -0.0003(15) -0.0058(17) C3 0.024(2) 0.045(3) 0.017(2) -0.0066(19) -0.0041(16) -0.010(2) C4 0.025(2) 0.047(3) 0.017(2) 0.000(2) -0.0049(17) -0.003(2) C5 0.021(2) 0.034(3) 0.020(2) 0.0053(18) 0.0024(16) -0.0005(19) C6 0.021(2) 0.023(2) 0.022(2) -0.0045(17) -0.0007(16) -0.0023(17) C7 0.053(4) 0.036(3) 0.029(3) 0.007(2) -0.009(2) 0.008(3) C8 0.0171(19) 0.020(2) 0.0154(18) -0.0037(15) -0.0014(14) -0.0053(16) C9 0.022(2) 0.025(2) 0.019(2) -0.0061(16) 0.0023(16) -0.0088(17) C10 0.025(2) 0.040(3) 0.020(2) -0.0140(19) 0.0046(16) -0.011(2) C11 0.030(2) 0.031(2) 0.020(2) -0.0081(18) 0.0035(17) -0.014(2) C12 0.027(2) 0.029(2) 0.025(2) -0.0151(18) 0.0030(17) -0.0074(19) C13 0.022(2) 0.026(2) 0.024(2) -0.0115(17) 0.0032(16) -0.0104(18) C14 0.0166(19) 0.019(2) 0.0181(19) -0.0042(15) -0.0009(14) -0.0069(16) C15 0.024(2) 0.029(2) 0.0167(19) -0.0050(16) -0.0011(15) -0.0118(18) C16 0.027(2) 0.049(3) 0.028(2) -0.014(2) -0.0013(18) -0.020(2) C17 0.025(2) 0.062(4) 0.033(3) -0.015(2) -0.0002(19) -0.023(2) C18 0.036(3) 0.052(3) 0.023(2) 0.000(2) 0.0007(19) -0.030(2) C19 0.024(2) 0.034(3) 0.018(2) -0.0012(17) -0.0030(16) -0.0153(19) C20 0.042(3) 0.042(3) 0.045(3) -0.009(2) -0.010(2) -0.026(3) C21 0.038(3) 0.038(3) 0.025(2) -0.012(2) 0.000(2) -0.003(2) C24 0.027(3) 0.034(3) 0.033(3) 0.000(2) 0.0043(19) -0.008(2) C25 0.036(2) 0.021(2) 0.0120(19) -0.0031(15) -0.0105(16) 0.0028(18) C26 0.020(2) 0.019(2) 0.024(2) -0.0034(16) -0.0026(16) -0.0039(17) C27 0.062(4) 0.029(3) 0.046(3) -0.007(2) -0.022(3) -0.017(3) C28 0.059(4) 0.038(3) 0.039(3) 0.005(2) -0.016(3) -0.026(3) C29 0.048(3) 0.023(3) 0.057(4) -0.014(2) -0.014(3) 0.004(2) C30 0.044(3) 0.049(4) 0.057(4) -0.016(3) -0.014(3) -0.024(3) C31 0.058(4) 0.053(4) 0.056(4) 0.002(3) -0.036(3) -0.018(3) C32 0.027(3) 0.050(4) 0.068(4) -0.013(3) -0.003(3) -0.004(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 Rh1 Si1 2.2624(13) . ? Rh1 N1 2.299(3) . ? Rh1 P1 2.3196(11) . ? Rh1 Si2 2.3230(12) . ? Rh1 H1 1.65(8) . ? Cl1 Si1 2.111(6) . ? Cl2 Si1 2.052(5) . ? P1 C1 1.839(4) . ? P1 C14 1.847(4) . ? P1 C8 1.854(4) . ? Si1 C26 1.891(4) . ? Si1 C23 1.91(3) . ? Si1 C22 2.104(10) . ? Si1 Si2 2.5843(16) . ? Si1 H1 1.99(7) . ? Si2 C24 1.910(5) . ? Si2 C25 1.926(4) . ? Si2 C26 1.959(4) . ? Si3 C28 1.878(5) . ? Si3 C29 1.879(6) . ? Si3 C27 1.882(5) . ? Si3 C26 1.893(5) . ? Si4 C30 1.876(6) . ? Si4 C31 1.881(6) . ? Si4 C26 1.889(4) . ? Si4 C32 1.889(6) . ? N1 C2 1.456(6) . ? N1 C21 1.489(6) . ? N1 C20 1.497(6) . ? C1 C2 1.397(6) . ? C1 C6 1.410(6) . ? C2 C3 1.406(6) . ? C3 C4 1.390(7) . ? C3 H2 0.9500 . ? C4 C5 1.376(8) . ? C4 H3 0.9500 . ? C5 C6 1.384(6) . ? C5 C7 1.521(7) . ? C6 H4 0.9500 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C8 C9 1.531(6) . ? C8 C13 1.537(6) . ? C8 H8 1.0000 . ? C9 C11 1.533(6) . ? C9 H9 0.9900 . ? C9 H10 0.9900 . ? C10 C12 1.523(6) . ? C10 C11 1.527(6) . ? C10 H11 0.9900 . ? C10 H12 0.9900 . ? C11 H13 0.9900 . ? C11 H14 0.9900 . ? C12 C13 1.534(6) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 H17 0.9900 . ? C13 H18 0.9900 . ? C14 C19 1.530(5) . ? C14 C15 1.533(6) . ? C14 H19 1.0000 . ? C15 C16 1.525(6) . ? C15 H20 0.9900 . ? C15 H21 0.9900 . ? C16 C17 1.527(6) . ? C16 H22 0.9900 . ? C16 H23 0.9900 . ? C17 C18 1.525(7) . ? C17 H24 0.9900 . ? C17 H25 0.9900 . ? C18 C19 1.538(6) . ? C18 H26 0.9900 . ? C18 H27 0.9900 . ? C19 H28 0.9900 . ? C19 H29 0.9900 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C20 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C21 H35 0.9800 . ? C24 H36 0.9800 . ? C24 H37 0.9800 . ? C24 H38 0.9800 . ? C25 H39 0.9800 . ? C25 H40 0.9800 . ? C25 H41 0.9800 . ? C27 H42 0.9800 . ? C27 H43 0.9800 . ? C27 H44 0.9800 . ? C28 H45 0.9800 . ? C28 H46 0.9800 . ? C28 H47 0.9800 . ? C29 H48 0.9800 . ? C29 H49 0.9800 . ? C29 H50 0.9800 . ? C30 H51 0.9800 . ? C30 H52 0.9800 . ? C30 H53 0.9800 . ? C31 H54 0.9800 . ? C31 H55 0.9800 . ? C31 H56 0.9800 . ? C32 H57 0.9800 . ? C32 H58 0.9800 . ? C32 H59 0.9800 . ? C33 C34 1.49(3) . ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C40 C41 1.528(16) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? 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 Si1 Rh1 N1 121.94(10) . . ? Si1 Rh1 P1 126.88(4) . . ? N1 Rh1 P1 82.29(10) . . ? Si1 Rh1 Si2 68.60(4) . . ? N1 Rh1 Si2 162.02(9) . . ? P1 Rh1 Si2 103.17(4) . . ? Si1 Rh1 H1 59(3) . . ? N1 Rh1 H1 89(3) . . ? P1 Rh1 H1 171(3) . . ? Si2 Rh1 H1 85(3) . . ? C1 P1 C14 102.36(18) . . ? C1 P1 C8 105.33(18) . . ? C14 P1 C8 105.68(18) . . ? C1 P1 Rh1 103.37(14) . . ? C14 P1 Rh1 126.71(14) . . ? C8 P1 Rh1 111.18(14) . . ? C26 Si1 C23 112.5(11) . . ? C26 Si1 Cl2 112.7(2) . . ? C23 Si1 Cl2 95.7(11) . . ? C26 Si1 C22 110.8(3) . . ? C23 Si1 C22 88.8(11) . . ? Cl2 Si1 C22 8.8(3) . . ? C26 Si1 Cl1 112.8(2) . . ? C23 Si1 Cl1 4.3(13) . . ? Cl2 Si1 Cl1 99.3(2) . . ? C22 Si1 Cl1 92.6(4) . . ? C26 Si1 Rh1 104.99(14) . . ? C23 Si1 Rh1 110.9(11) . . ? Cl2 Si1 Rh1 120.06(16) . . ? C22 Si1 Rh1 128.0(3) . . ? Cl1 Si1 Rh1 106.95(18) . . ? C26 Si1 Si2 48.98(13) . . ? C23 Si1 Si2 119.7(11) . . ? Cl2 Si1 Si2 143.74(17) . . ? C22 Si1 Si2 148.7(3) . . ? Cl1 Si1 Si2 116.40(19) . . ? Rh1 Si1 Si2 56.81(4) . . ? C26 Si1 H1 99(2) . . ? C23 Si1 H1 145(2) . . ? Cl2 Si1 H1 83(2) . . ? C22 Si1 H1 92(2) . . ? Cl1 Si1 H1 143(2) . . ? Rh1 Si1 H1 45(2) . . ? Si2 Si1 H1 72(2) . . ? C24 Si2 C25 99.4(2) . . ? C24 Si2 C26 115.8(2) . . ? C25 Si2 C26 111.41(19) . . ? C24 Si2 Rh1 106.31(17) . . ? C25 Si2 Rh1 124.10(14) . . ? C26 Si2 Rh1 100.60(13) . . ? C24 Si2 Si1 131.54(18) . . ? C25 Si2 Si1 128.67(16) . . ? C26 Si2 Si1 46.74(13) . . ? Rh1 Si2 Si1 54.59(4) . . ? C28 Si3 C29 105.9(3) . . ? C28 Si3 C27 106.1(3) . . ? C29 Si3 C27 103.3(3) . . ? C28 Si3 C26 112.3(2) . . ? C29 Si3 C26 112.3(2) . . ? C27 Si3 C26 116.0(2) . . ? C30 Si4 C31 103.1(3) . . ? C30 Si4 C26 116.4(2) . . ? C31 Si4 C26 113.4(2) . . ? C30 Si4 C32 104.5(3) . . ? C31 Si4 C32 107.1(3) . . ? C26 Si4 C32 111.4(3) . . ? C2 N1 C21 111.2(3) . . ? C2 N1 C20 109.6(4) . . ? C21 N1 C20 109.1(4) . . ? C2 N1 Rh1 115.1(2) . . ? C21 N1 Rh1 106.6(3) . . ? C20 N1 Rh1 104.9(3) . . ? C2 C1 C6 118.9(4) . . ? C2 C1 P1 118.1(3) . . ? C6 C1 P1 123.1(3) . . ? C1 C2 C3 118.6(4) . . ? C1 C2 N1 121.1(4) . . ? C3 C2 N1 120.2(4) . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H2 119.5 . . ? C2 C3 H2 119.5 . . ? C5 C4 C3 120.7(4) . . ? C5 C4 H3 119.6 . . ? C3 C4 H3 119.6 . . ? C4 C5 C6 118.8(5) . . ? C4 C5 C7 121.0(4) . . ? C6 C5 C7 120.2(5) . . ? C5 C6 C1 122.0(4) . . ? C5 C6 H4 119.0 . . ? C1 C6 H4 119.0 . . ? C5 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C5 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? C9 C8 C13 110.7(3) . . ? C9 C8 P1 108.8(3) . . ? C13 C8 P1 119.2(3) . . ? C9 C8 H8 105.8 . . ? C13 C8 H8 105.8 . . ? P1 C8 H8 105.8 . . ? C8 C9 C11 111.1(3) . . ? C8 C9 H9 109.4 . . ? C11 C9 H9 109.4 . . ? C8 C9 H10 109.4 . . ? C11 C9 H10 109.4 . . ? H9 C9 H10 108.0 . . ? C12 C10 C11 111.5(4) . . ? C12 C10 H11 109.3 . . ? C11 C10 H11 109.3 . . ? C12 C10 H12 109.3 . . ? C11 C10 H12 109.3 . . ? H11 C10 H12 108.0 . . ? C10 C11 C9 111.9(4) . . ? C10 C11 H13 109.2 . . ? C9 C11 H13 109.2 . . ? C10 C11 H14 109.2 . . ? C9 C11 H14 109.2 . . ? H13 C11 H14 107.9 . . ? C10 C12 C13 111.9(4) . . ? C10 C12 H15 109.2 . . ? C13 C12 H15 109.2 . . ? C10 C12 H16 109.2 . . ? C13 C12 H16 109.2 . . ? H15 C12 H16 107.9 . . ? C12 C13 C8 109.6(4) . . ? C12 C13 H17 109.8 . . ? C8 C13 H17 109.8 . . ? C12 C13 H18 109.8 . . ? C8 C13 H18 109.8 . . ? H17 C13 H18 108.2 . . ? C19 C14 C15 111.1(3) . . ? C19 C14 P1 111.7(3) . . ? C15 C14 P1 110.1(3) . . ? C19 C14 H19 107.9 . . ? C15 C14 H19 107.9 . . ? P1 C14 H19 107.9 . . ? C16 C15 C14 111.7(4) . . ? C16 C15 H20 109.3 . . ? C14 C15 H20 109.3 . . ? C16 C15 H21 109.3 . . ? C14 C15 H21 109.3 . . ? H20 C15 H21 107.9 . . ? C15 C16 C17 111.3(4) . . ? C15 C16 H22 109.4 . . ? C17 C16 H22 109.4 . . ? C15 C16 H23 109.4 . . ? C17 C16 H23 109.4 . . ? H22 C16 H23 108.0 . . ? C18 C17 C16 110.8(4) . . ? C18 C17 H24 109.5 . . ? C16 C17 H24 109.5 . . ? C18 C17 H25 109.5 . . ? C16 C17 H25 109.5 . . ? H24 C17 H25 108.1 . . ? C17 C18 C19 111.1(4) . . ? C17 C18 H26 109.4 . . ? C19 C18 H26 109.4 . . ? C17 C18 H27 109.4 . . ? C19 C18 H27 109.4 . . ? H26 C18 H27 108.0 . . ? C14 C19 C18 111.0(4) . . ? C14 C19 H28 109.4 . . ? C18 C19 H28 109.4 . . ? C14 C19 H29 109.4 . . ? C18 C19 H29 109.4 . . ? H28 C19 H29 108.0 . . ? N1 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C20 H32 109.5 . . ? H30 C20 H32 109.5 . . ? H31 C20 H32 109.5 . . ? N1 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? N1 C21 H35 109.5 . . ? H33 C21 H35 109.5 . . ? H34 C21 H35 109.5 . . ? Si2 C24 H36 109.5 . . ? Si2 C24 H37 109.5 . . ? H36 C24 H37 109.5 . . ? Si2 C24 H38 109.5 . . ? H36 C24 H38 109.5 . . ? H37 C24 H38 109.5 . . ? Si2 C25 H39 109.5 . . ? Si2 C25 H40 109.5 . . ? H39 C25 H40 109.5 . . ? Si2 C25 H41 109.5 . . ? H39 C25 H41 109.5 . . ? H40 C25 H41 109.5 . . ? Si4 C26 Si1 115.6(2) . . ? Si4 C26 Si3 110.9(2) . . ? Si1 C26 Si3 113.1(2) . . ? Si4 C26 Si2 119.9(2) . . ? Si1 C26 Si2 84.29(17) . . ? Si3 C26 Si2 110.7(2) . . ? Si3 C27 H42 109.5 . . ? Si3 C27 H43 109.5 . . ? H42 C27 H43 109.5 . . ? Si3 C27 H44 109.5 . . ? H42 C27 H44 109.5 . . ? H43 C27 H44 109.5 . . ? Si3 C28 H45 109.5 . . ? Si3 C28 H46 109.5 . . ? H45 C28 H46 109.5 . . ? Si3 C28 H47 109.5 . . ? H45 C28 H47 109.5 . . ? H46 C28 H47 109.5 . . ? Si3 C29 H48 109.5 . . ? Si3 C29 H49 109.5 . . ? H48 C29 H49 109.5 . . ? Si3 C29 H50 109.5 . . ? H48 C29 H50 109.5 . . ? H49 C29 H50 109.5 . . ? Si4 C30 H51 109.5 . . ? Si4 C30 H52 109.5 . . ? H51 C30 H52 109.5 . . ? Si4 C30 H53 109.5 . . ? H51 C30 H53 109.5 . . ? H52 C30 H53 109.5 . . ? Si4 C31 H54 109.5 . . ? Si4 C31 H55 109.5 . . ? H54 C31 H55 109.5 . . ? Si4 C31 H56 109.5 . . ? H54 C31 H56 109.5 . . ? H55 C31 H56 109.5 . . ? Si4 C32 H57 109.5 . . ? Si4 C32 H58 109.5 . . ? H57 C32 H58 109.5 . . ? Si4 C32 H59 109.5 . . ? H57 C32 H59 109.5 . . ? H58 C32 H59 109.5 . . ? C35 C34 C39 120.0 . . ? C35 C34 C33 115.8(12) . . ? C39 C34 C33 124.0(12) . . ? C36 C35 C34 120.0 . . ? C35 C36 C37 120.0 . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C34 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 C40 119.8(7) . . ? C46 C41 C40 120.2(7) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C41 120.0 . . ? 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 Si1 Rh1 P1 C1 125.37(13) . . . . ? N1 Rh1 P1 C1 0.90(16) . . . . ? Si2 Rh1 P1 C1 -161.67(13) . . . . ? Si1 Rh1 P1 C14 8.51(17) . . . . ? N1 Rh1 P1 C14 -115.95(18) . . . . ? Si2 Rh1 P1 C14 81.48(16) . . . . ? Si1 Rh1 P1 C8 -122.08(14) . . . . ? N1 Rh1 P1 C8 113.45(16) . . . . ? Si2 Rh1 P1 C8 -49.12(14) . . . . ? N1 Rh1 Si1 C26 -154.45(18) . . . . ? P1 Rh1 Si1 C26 99.88(15) . . . . ? Si2 Rh1 Si1 C26 9.19(14) . . . . ? N1 Rh1 Si1 C23 83.8(11) . . . . ? P1 Rh1 Si1 C23 -21.9(11) . . . . ? Si2 Rh1 Si1 C23 -112.6(11) . . . . ? N1 Rh1 Si1 Cl2 -26.4(2) . . . . ? P1 Rh1 Si1 Cl2 -132.04(19) . . . . ? Si2 Rh1 Si1 Cl2 137.28(19) . . . . ? N1 Rh1 Si1 C22 -21.9(4) . . . . ? P1 Rh1 Si1 C22 -127.6(4) . . . . ? Si2 Rh1 Si1 C22 141.7(4) . . . . ? N1 Rh1 Si1 Cl1 85.5(2) . . . . ? P1 Rh1 Si1 Cl1 -20.2(2) . . . . ? Si2 Rh1 Si1 Cl1 -110.9(2) . . . . ? N1 Rh1 Si1 Si2 -163.64(11) . . . . ? P1 Rh1 Si1 Si2 90.68(5) . . . . ? Si1 Rh1 Si2 C24 -129.78(19) . . . . ? N1 Rh1 Si2 C24 -0.5(4) . . . . ? P1 Rh1 Si2 C24 105.45(18) . . . . ? Si1 Rh1 Si2 C25 116.39(19) . . . . ? N1 Rh1 Si2 C25 -114.3(4) . . . . ? P1 Rh1 Si2 C25 -8.38(19) . . . . ? Si1 Rh1 Si2 C26 -8.72(14) . . . . ? N1 Rh1 Si2 C26 120.6(3) . . . . ? P1 Rh1 Si2 C26 -133.49(14) . . . . ? N1 Rh1 Si2 Si1 129.3(3) . . . . ? P1 Rh1 Si2 Si1 -124.77(5) . . . . ? C26 Si1 Si2 C24 -88.0(3) . . . . ? C23 Si1 Si2 C24 177.0(13) . . . . ? Cl2 Si1 Si2 C24 -16.7(4) . . . . ? C22 Si1 Si2 C24 -29.7(6) . . . . ? Cl1 Si1 Si2 C24 173.9(3) . . . . ? Rh1 Si1 Si2 C24 80.2(2) . . . . ? C26 Si1 Si2 C25 83.6(2) . . . . ? C23 Si1 Si2 C25 -11.4(13) . . . . ? Cl2 Si1 Si2 C25 154.9(3) . . . . ? C22 Si1 Si2 C25 141.9(6) . . . . ? Cl1 Si1 Si2 C25 -14.5(3) . . . . ? Rh1 Si1 Si2 C25 -108.19(18) . . . . ? C23 Si1 Si2 C26 -95.0(13) . . . . ? Cl2 Si1 Si2 C26 71.3(3) . . . . ? C22 Si1 Si2 C26 58.3(6) . . . . ? Cl1 Si1 Si2 C26 -98.1(3) . . . . ? Rh1 Si1 Si2 C26 168.19(18) . . . . ? C26 Si1 Si2 Rh1 -168.19(18) . . . . ? C23 Si1 Si2 Rh1 96.8(13) . . . . ? Cl2 Si1 Si2 Rh1 -96.9(3) . . . . ? C22 Si1 Si2 Rh1 -109.9(6) . . . . ? Cl1 Si1 Si2 Rh1 93.7(2) . . . . ? Si1 Rh1 N1 C2 -129.9(2) . . . . ? P1 Rh1 N1 C2 -0.9(3) . . . . ? Si2 Rh1 N1 C2 108.2(4) . . . . ? Si1 Rh1 N1 C21 -6.0(3) . . . . ? P1 Rh1 N1 C21 123.0(3) . . . . ? Si2 Rh1 N1 C21 -127.9(3) . . . . ? Si1 Rh1 N1 C20 109.6(3) . . . . ? P1 Rh1 N1 C20 -121.4(3) . . . . ? Si2 Rh1 N1 C20 -12.3(5) . . . . ? C14 P1 C1 C2 131.9(3) . . . . ? C8 P1 C1 C2 -117.8(3) . . . . ? Rh1 P1 C1 C2 -1.0(3) . . . . ? C14 P1 C1 C6 -46.3(4) . . . . ? C8 P1 C1 C6 64.1(4) . . . . ? Rh1 P1 C1 C6 -179.2(3) . . . . ? C6 C1 C2 C3 -1.1(6) . . . . ? P1 C1 C2 C3 -179.4(3) . . . . ? C6 C1 C2 N1 178.6(4) . . . . ? P1 C1 C2 N1 0.3(5) . . . . ? C21 N1 C2 C1 -120.9(4) . . . . ? C20 N1 C2 C1 118.4(4) . . . . ? Rh1 N1 C2 C1 0.6(5) . . . . ? C21 N1 C2 C3 58.8(5) . . . . ? C20 N1 C2 C3 -61.9(5) . . . . ? Rh1 N1 C2 C3 -179.7(3) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? N1 C2 C3 C4 -178.9(4) . . . . ? C2 C3 C4 C5 -0.4(7) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? C3 C4 C5 C7 -179.3(5) . . . . ? C4 C5 C6 C1 -0.7(7) . . . . ? C7 C5 C6 C1 178.9(4) . . . . ? C2 C1 C6 C5 1.1(6) . . . . ? P1 C1 C6 C5 179.2(3) . . . . ? C1 P1 C8 C9 60.9(3) . . . . ? C14 P1 C8 C9 168.8(3) . . . . ? Rh1 P1 C8 C9 -50.4(3) . . . . ? C1 P1 C8 C13 -67.2(3) . . . . ? C14 P1 C8 C13 40.7(4) . . . . ? Rh1 P1 C8 C13 -178.5(3) . . . . ? C13 C8 C9 C11 -57.0(5) . . . . ? P1 C8 C9 C11 170.3(3) . . . . ? C12 C10 C11 C9 -52.9(5) . . . . ? C8 C9 C11 C10 54.2(5) . . . . ? C11 C10 C12 C13 54.8(5) . . . . ? C10 C12 C13 C8 -57.2(5) . . . . ? C9 C8 C13 C12 58.0(4) . . . . ? P1 C8 C13 C12 -174.7(3) . . . . ? C1 P1 C14 C19 -58.5(3) . . . . ? C8 P1 C14 C19 -168.5(3) . . . . ? Rh1 P1 C14 C19 58.8(3) . . . . ? C1 P1 C14 C15 177.5(3) . . . . ? C8 P1 C14 C15 67.5(3) . . . . ? Rh1 P1 C14 C15 -65.2(3) . . . . ? C19 C14 C15 C16 54.5(5) . . . . ? P1 C14 C15 C16 178.8(3) . . . . ? C14 C15 C16 C17 -55.2(6) . . . . ? C15 C16 C17 C18 56.2(6) . . . . ? C16 C17 C18 C19 -56.7(6) . . . . ? C15 C14 C19 C18 -54.7(5) . . . . ? P1 C14 C19 C18 -178.2(3) . . . . ? C17 C18 C19 C14 56.2(6) . . . . ? C30 Si4 C26 Si1 62.3(3) . . . . ? C31 Si4 C26 Si1 -178.3(3) . . . . ? C32 Si4 C26 Si1 -57.3(3) . . . . ? C30 Si4 C26 Si3 -167.2(3) . . . . ? C31 Si4 C26 Si3 -47.8(4) . . . . ? C32 Si4 C26 Si3 73.2(3) . . . . ? C30 Si4 C26 Si2 -36.1(4) . . . . ? C31 Si4 C26 Si2 83.3(3) . . . . ? C32 Si4 C26 Si2 -155.8(3) . . . . ? C23 Si1 C26 Si4 -9.9(12) . . . . ? Cl2 Si1 C26 Si4 96.9(3) . . . . ? C22 Si1 C26 Si4 87.7(4) . . . . ? Cl1 Si1 C26 Si4 -14.6(3) . . . . ? Rh1 Si1 C26 Si4 -130.7(2) . . . . ? Si2 Si1 C26 Si4 -120.5(3) . . . . ? C23 Si1 C26 Si3 -139.3(12) . . . . ? Cl2 Si1 C26 Si3 -32.5(3) . . . . ? C22 Si1 C26 Si3 -41.7(4) . . . . ? Cl1 Si1 C26 Si3 -144.0(3) . . . . ? Rh1 Si1 C26 Si3 99.9(2) . . . . ? Si2 Si1 C26 Si3 110.1(3) . . . . ? C23 Si1 C26 Si2 110.5(12) . . . . ? Cl2 Si1 C26 Si2 -142.6(2) . . . . ? C22 Si1 C26 Si2 -151.8(3) . . . . ? Cl1 Si1 C26 Si2 105.9(2) . . . . ? Rh1 Si1 C26 Si2 -10.21(16) . . . . ? C28 Si3 C26 Si4 69.7(3) . . . . ? C29 Si3 C26 Si4 -49.6(3) . . . . ? C27 Si3 C26 Si4 -168.1(3) . . . . ? C28 Si3 C26 Si1 -158.6(3) . . . . ? C29 Si3 C26 Si1 82.2(3) . . . . ? C27 Si3 C26 Si1 -36.3(3) . . . . ? C28 Si3 C26 Si2 -65.9(3) . . . . ? C29 Si3 C26 Si2 174.8(2) . . . . ? C27 Si3 C26 Si2 56.3(3) . . . . ? C24 Si2 C26 Si4 -119.9(3) . . . . ? C25 Si2 C26 Si4 -7.3(3) . . . . ? Rh1 Si2 C26 Si4 126.1(2) . . . . ? Si1 Si2 C26 Si4 116.3(3) . . . . ? C24 Si2 C26 Si1 123.8(2) . . . . ? C25 Si2 C26 Si1 -123.55(19) . . . . ? Rh1 Si2 C26 Si1 9.77(15) . . . . ? C24 Si2 C26 Si3 11.2(3) . . . . ? C25 Si2 C26 Si3 123.8(2) . . . . ? Rh1 Si2 C26 Si3 -102.84(19) . . . . ? Si1 Si2 C26 Si3 -112.6(3) . . . . ? C39 C34 C35 C36 0.0 . . . . ? C33 C34 C35 C36 -176.1(15) . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C39 0.0 . . . . ? C37 C38 C39 C34 0.0 . . . . ? C35 C34 C39 C38 0.0 . . . . ? C33 C34 C39 C38 175.7(16) . . . . ? C46 C41 C42 C43 0.0 . . . . ? C40 C41 C42 C43 179.3(9) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? C40 C41 C46 C45 -179.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.955 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.164 #===END data_(PcyN-P,N)IrH2(PMe3)(SiHClDmp)-(11)\/Y0.5C4H8O _database_code_depnum_ccdc_archive 'CCDC 772168' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H71 Cl Ir N P2 Si, C2 H4 O0.5' _chemical_formula_sum 'C50 H75 Cl Ir N O0.50 P2 Si' _chemical_formula_weight 1015.79 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' 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9670(4) _cell_length_b 12.5030(3) _cell_length_c 18.2016(5) _cell_angle_alpha 80.8548(13) _cell_angle_beta 77.1201(17) _cell_angle_gamma 68.214(2) _cell_volume 2456.49(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11141 _cell_measurement_theta_min 1.15 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 2.896 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6873 _exptl_absorpt_correction_T_max 0.7226 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22679 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0756 _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 -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11141 _reflns_number_gt 9520 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0717P)^2^+7.4083P] 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 11141 _refine_ls_number_parameters 519 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.215 _refine_ls_restrained_S_all 1.215 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.02638(2) 0.24654(2) 0.211458(15) 0.01336(9) Uani 1 1 d . . . Cl1 Cl -0.15615(19) 0.56337(17) 0.16242(12) 0.0314(4) Uani 1 1 d . . . P1 P 0.14399(16) 0.05811(15) 0.18819(10) 0.0163(4) Uani 1 1 d . . . P2 P 0.15271(17) 0.31249(17) 0.25878(11) 0.0211(4) Uani 1 1 d . . . Si1 Si -0.13601(18) 0.41555(17) 0.24415(12) 0.0202(4) Uani 1 1 d . . . N1 N 0.0951(5) 0.2787(5) 0.0840(3) 0.0184(12) Uani 1 1 d . . . C1 C 0.2267(6) 0.0696(6) 0.0909(4) 0.0154(13) Uani 1 1 d . . . C2 C 0.1931(6) 0.1773(7) 0.0509(4) 0.0213(15) Uani 1 1 d . . . C3 C 0.2504(7) 0.1893(7) -0.0246(4) 0.0239(16) Uani 1 1 d . . . H1 H 0.2283 0.2630 -0.0522 0.029 Uiso 1 1 calc R . . C4 C 0.3379(7) 0.0962(7) -0.0588(4) 0.0242(16) Uani 1 1 d . . . H2 H 0.3758 0.1070 -0.1098 0.029 Uiso 1 1 calc R . . C5 C 0.3728(7) -0.0134(6) -0.0215(4) 0.0191(14) Uani 1 1 d . . . C6 C 0.3138(7) -0.0238(6) 0.0546(4) 0.0191(14) Uani 1 1 d . . . H3 H 0.3347 -0.0978 0.0818 0.023 Uiso 1 1 calc R . . C7 C 0.4668(7) -0.1137(7) -0.0599(5) 0.0255(17) Uani 1 1 d . . . H4 H 0.4466 -0.1162 -0.1088 0.038 Uiso 1 1 calc R . . H5 H 0.4686 -0.1853 -0.0283 0.038 Uiso 1 1 calc R . . H6 H 0.5471 -0.1057 -0.0681 0.038 Uiso 1 1 calc R . . C8 C 0.2606(7) -0.0249(6) 0.2478(4) 0.0215(15) Uani 1 1 d . . . H7 H 0.3261 0.0101 0.2332 0.026 Uiso 1 1 calc R . . C9 C 0.3270(8) -0.1562(7) 0.2409(5) 0.0318(19) Uani 1 1 d . . . H8 H 0.2673 -0.1966 0.2579 0.038 Uiso 1 1 calc R . . H9 H 0.3635 -0.1703 0.1873 0.038 Uiso 1 1 calc R . . C10 C 0.4270(9) -0.2040(8) 0.2888(5) 0.041(2) Uani 1 1 d . . . H10 H 0.4662 -0.2884 0.2852 0.049 Uiso 1 1 calc R . . H11 H 0.4904 -0.1685 0.2685 0.049 Uiso 1 1 calc R . . C11 C 0.3776(9) -0.1803(8) 0.3713(5) 0.039(2) Uani 1 1 d . . . H12 H 0.4465 -0.2066 0.3994 0.047 Uiso 1 1 calc R . . H13 H 0.3230 -0.2247 0.3938 0.047 Uiso 1 1 calc R . . C12 C 0.3072(9) -0.0522(8) 0.3794(5) 0.039(2) Uani 1 1 d . . . H14 H 0.2691 -0.0403 0.4330 0.047 Uiso 1 1 calc R . . H15 H 0.3644 -0.0089 0.3640 0.047 Uiso 1 1 calc R . . C13 C 0.2097(8) -0.0063(7) 0.3314(4) 0.0271(17) Uani 1 1 d . . . H16 H 0.1671 0.0774 0.3368 0.032 Uiso 1 1 calc R . . H17 H 0.1488 -0.0451 0.3499 0.032 Uiso 1 1 calc R . . C14 C 0.0723(7) -0.0449(6) 0.1792(4) 0.0204(15) Uani 1 1 d . . . H18 H 0.1403 -0.1189 0.1659 0.024 Uiso 1 1 calc R . . C15 C -0.0077(8) -0.0730(7) 0.2524(4) 0.0267(17) Uani 1 1 d . . . H19 H 0.0412 -0.1006 0.2933 0.032 Uiso 1 1 calc R . . H20 H -0.0768 -0.0017 0.2672 0.032 Uiso 1 1 calc R . . C16 C -0.0574(9) -0.1644(8) 0.2434(5) 0.036(2) Uani 1 1 d . . . H21 H -0.1108 -0.1778 0.2912 0.043 Uiso 1 1 calc R . . H22 H 0.0114 -0.2378 0.2334 0.043 Uiso 1 1 calc R . . C17 C -0.1305(8) -0.1292(7) 0.1788(5) 0.0299(18) Uani 1 1 d . . . H23 H -0.1535 -0.1945 0.1712 0.036 Uiso 1 1 calc R . . H24 H -0.2066 -0.0631 0.1924 0.036 Uiso 1 1 calc R . . C18 C -0.0564(8) -0.0960(8) 0.1065(5) 0.0316(19) Uani 1 1 d . . . H25 H -0.1095 -0.0637 0.0678 0.038 Uiso 1 1 calc R . . H26 H 0.0104 -0.1663 0.0879 0.038 Uiso 1 1 calc R . . C19 C -0.0009(8) -0.0070(7) 0.1155(4) 0.0239(16) Uani 1 1 d . . . H27 H 0.0530 0.0048 0.0675 0.029 Uiso 1 1 calc R . . H28 H -0.0675 0.0678 0.1256 0.029 Uiso 1 1 calc R . . C20 C 0.1355(7) 0.3800(7) 0.0694(5) 0.0249(16) Uani 1 1 d . . . H29 H 0.2126 0.3597 0.0875 0.037 Uiso 1 1 calc R . . H30 H 0.0730 0.4445 0.0960 0.037 Uiso 1 1 calc R . . H31 H 0.1476 0.4026 0.0149 0.037 Uiso 1 1 calc R . . C21 C -0.0111(7) 0.3093(7) 0.0440(4) 0.0221(15) Uani 1 1 d . . . H32 H 0.0148 0.3270 -0.0101 0.033 Uiso 1 1 calc R . . H33 H -0.0774 0.3770 0.0649 0.033 Uiso 1 1 calc R . . H34 H -0.0400 0.2440 0.0511 0.033 Uiso 1 1 calc R . . C22 C 0.1412(9) 0.4625(8) 0.2375(5) 0.035(2) Uani 1 1 d . . . H35 H 0.0554 0.5126 0.2494 0.052 Uiso 1 1 calc R . . H36 H 0.1728 0.4759 0.1837 0.052 Uiso 1 1 calc R . . H37 H 0.1893 0.4801 0.2679 0.052 Uiso 1 1 calc R . . C23 C 0.3194(8) 0.2431(8) 0.2400(6) 0.036(2) Uani 1 1 d . . . H38 H 0.3494 0.2472 0.1854 0.054 Uiso 1 1 calc R . . H39 H 0.3418 0.1620 0.2604 0.054 Uiso 1 1 calc R . . H40 H 0.3562 0.2831 0.2644 0.054 Uiso 1 1 calc R . . C24 C 0.1245(9) 0.3097(9) 0.3619(5) 0.038(2) Uani 1 1 d . . . H41 H 0.1689 0.3522 0.3769 0.057 Uiso 1 1 calc R . . H42 H 0.1527 0.2294 0.3837 0.057 Uiso 1 1 calc R . . H43 H 0.0367 0.3459 0.3805 0.057 Uiso 1 1 calc R . . C25 C -0.3026(7) 0.4257(6) 0.2836(4) 0.0210(15) Uani 1 1 d . . . C26 C -0.3424(7) 0.4279(7) 0.3624(5) 0.0266(17) Uani 1 1 d . . . C27 C -0.4659(8) 0.4490(9) 0.3932(5) 0.037(2) Uani 1 1 d . . . H44 H -0.4916 0.4504 0.4464 0.045 Uiso 1 1 calc R . . C28 C -0.5511(8) 0.4677(10) 0.3484(5) 0.041(2) Uani 1 1 d . . . H45 H -0.6351 0.4847 0.3701 0.049 Uiso 1 1 calc R . . C29 C -0.5129(7) 0.4616(8) 0.2719(5) 0.0306(18) Uani 1 1 d . . . H46 H -0.5713 0.4735 0.2409 0.037 Uiso 1 1 calc R . . C30 C -0.3903(7) 0.4383(6) 0.2385(4) 0.0205(15) Uani 1 1 d . . . C31 C -0.2573(8) 0.4027(8) 0.4164(4) 0.0298(18) Uani 1 1 d . . . C32 C -0.2418(7) 0.4928(8) 0.4458(4) 0.0296(18) Uani 1 1 d . . . C33 C -0.1672(8) 0.4652(9) 0.4989(5) 0.037(2) Uani 1 1 d . . . H47 H -0.1556 0.5257 0.5185 0.044 Uiso 1 1 calc R . . C34 C -0.1077(10) 0.3496(10) 0.5249(5) 0.044(3) Uani 1 1 d . . . C35 C -0.1254(10) 0.2647(10) 0.4970(6) 0.046(3) Uani 1 1 d . . . H48 H -0.0859 0.1869 0.5149 0.055 Uiso 1 1 calc R . . C36 C -0.1989(9) 0.2863(9) 0.4433(5) 0.038(2) Uani 1 1 d . . . C37 C -0.3015(9) 0.6156(8) 0.4192(6) 0.043(2) Uani 1 1 d . . . H49 H -0.3905 0.6350 0.4292 0.065 Uiso 1 1 calc R . . H50 H -0.2731 0.6272 0.3647 0.065 Uiso 1 1 calc R . . H51 H -0.2804 0.6655 0.4459 0.065 Uiso 1 1 calc R . . C38 C -0.0283(12) 0.3247(12) 0.5837(6) 0.061(3) Uani 1 1 d . . . H52 H -0.0717 0.3037 0.6330 0.092 Uiso 1 1 calc R . . H53 H -0.0096 0.3936 0.5869 0.092 Uiso 1 1 calc R . . H54 H 0.0479 0.2605 0.5696 0.092 Uiso 1 1 calc R . . C39 C -0.2190(10) 0.1881(9) 0.4162(6) 0.050(3) Uani 1 1 d . . . H55 H -0.1562 0.1149 0.4294 0.074 Uiso 1 1 calc R . . H56 H -0.2140 0.1996 0.3612 0.074 Uiso 1 1 calc R . . H57 H -0.3000 0.1859 0.4405 0.074 Uiso 1 1 calc R . . C40 C -0.3599(6) 0.4205(6) 0.1566(4) 0.0186(14) Uani 1 1 d . . . C41 C -0.3204(7) 0.3069(7) 0.1357(4) 0.0219(15) Uani 1 1 d . . . C42 C -0.2922(7) 0.2867(7) 0.0590(5) 0.0236(16) Uani 1 1 d . . . H58 H -0.2620 0.2096 0.0450 0.028 Uiso 1 1 calc R . . C43 C -0.3082(7) 0.3785(7) 0.0029(4) 0.0231(16) Uani 1 1 d . . . C44 C -0.3536(7) 0.4894(7) 0.0247(4) 0.0237(16) Uani 1 1 d . . . H59 H -0.3671 0.5523 -0.0131 0.028 Uiso 1 1 calc R . . C45 C -0.3805(6) 0.5123(6) 0.1000(4) 0.0218(15) Uani 1 1 d . . . C46 C -0.3140(7) 0.2059(7) 0.1944(5) 0.0271(17) Uani 1 1 d . . . H60 H -0.2942 0.1357 0.1692 0.041 Uiso 1 1 calc R . . H61 H -0.3932 0.2210 0.2284 0.041 Uiso 1 1 calc R . . H62 H -0.2505 0.1953 0.2235 0.041 Uiso 1 1 calc R . . C47 C -0.2757(8) 0.3562(9) -0.0796(5) 0.035(2) Uani 1 1 d . . . H63 H -0.3272 0.4217 -0.1085 0.053 Uiso 1 1 calc R . . H64 H -0.2894 0.2857 -0.0855 0.053 Uiso 1 1 calc R . . H65 H -0.1895 0.3467 -0.0984 0.053 Uiso 1 1 calc R . . C48 C -0.4370(7) 0.6367(7) 0.1213(5) 0.0279(17) Uani 1 1 d . . . H66 H -0.4371 0.6895 0.0753 0.042 Uiso 1 1 calc R . . H67 H -0.3890 0.6494 0.1541 0.042 Uiso 1 1 calc R . . H68 H -0.5212 0.6512 0.1482 0.042 Uiso 1 1 calc R . . O1 O -0.467(4) 0.965(4) 0.488(3) 0.190(17) Uiso 0.50 1 d PD . . C49 C -0.355(3) 0.936(3) 0.4296(17) 0.089(10) Uiso 0.50 1 d PD . . C50 C -0.387(3) 1.013(3) 0.3620(17) 0.092(10) Uiso 0.50 1 d PD . . C51 C -0.487(4) 1.101(4) 0.408(2) 0.139(17) Uiso 0.50 1 d PD . . C52 C -0.551(4) 1.090(3) 0.488(2) 0.121(15) Uiso 0.50 1 d PD . . 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 0.01343(13) 0.01280(13) 0.01307(13) -0.00123(9) -0.00316(9) -0.00315(9) Cl1 0.0310(10) 0.0257(9) 0.0345(10) 0.0067(8) -0.0072(8) -0.0093(8) P1 0.0173(8) 0.0150(8) 0.0155(8) -0.0008(7) -0.0032(7) -0.0045(7) P2 0.0189(9) 0.0220(9) 0.0232(9) -0.0059(8) -0.0043(7) -0.0060(8) Si1 0.0163(9) 0.0164(9) 0.0266(10) -0.0038(8) -0.0001(8) -0.0055(8) N1 0.018(3) 0.022(3) 0.017(3) 0.008(2) -0.007(2) -0.010(3) C1 0.014(3) 0.021(3) 0.011(3) -0.001(3) -0.008(2) -0.003(3) C2 0.015(3) 0.031(4) 0.021(4) -0.009(3) -0.007(3) -0.007(3) C3 0.022(4) 0.031(4) 0.018(4) 0.003(3) -0.007(3) -0.010(3) C4 0.019(4) 0.041(5) 0.011(3) -0.006(3) 0.001(3) -0.010(3) C5 0.018(3) 0.025(4) 0.016(3) -0.007(3) -0.004(3) -0.007(3) C6 0.024(4) 0.021(3) 0.017(3) -0.003(3) -0.005(3) -0.012(3) C7 0.016(3) 0.034(4) 0.027(4) -0.009(3) 0.000(3) -0.009(3) C8 0.019(3) 0.016(3) 0.024(4) -0.002(3) -0.009(3) 0.003(3) C9 0.036(5) 0.024(4) 0.027(4) -0.010(3) -0.016(4) 0.009(4) C10 0.036(5) 0.031(5) 0.038(5) -0.001(4) -0.009(4) 0.007(4) C11 0.044(5) 0.034(5) 0.022(4) 0.000(4) -0.017(4) 0.011(4) C12 0.046(5) 0.038(5) 0.027(4) -0.003(4) -0.017(4) -0.002(4) C13 0.033(4) 0.022(4) 0.021(4) -0.003(3) -0.008(3) -0.001(3) C14 0.022(4) 0.016(3) 0.022(4) 0.001(3) -0.006(3) -0.005(3) C15 0.030(4) 0.033(4) 0.022(4) 0.003(3) -0.010(3) -0.016(4) C16 0.047(5) 0.031(5) 0.037(5) 0.005(4) -0.015(4) -0.022(4) C17 0.037(5) 0.022(4) 0.036(5) 0.006(3) -0.016(4) -0.014(4) C18 0.040(5) 0.031(4) 0.033(4) -0.003(4) -0.017(4) -0.017(4) C19 0.034(4) 0.024(4) 0.021(4) -0.001(3) -0.008(3) -0.017(3) C20 0.027(4) 0.022(4) 0.027(4) -0.007(3) -0.001(3) -0.009(3) C21 0.018(3) 0.027(4) 0.018(3) 0.001(3) -0.007(3) -0.004(3) C22 0.041(5) 0.031(4) 0.040(5) -0.003(4) -0.012(4) -0.018(4) C23 0.025(4) 0.033(5) 0.054(6) -0.016(4) -0.012(4) -0.007(4) C24 0.045(5) 0.052(6) 0.028(4) -0.015(4) -0.002(4) -0.027(5) C25 0.020(4) 0.018(3) 0.022(4) -0.003(3) -0.003(3) -0.004(3) C26 0.025(4) 0.027(4) 0.028(4) 0.001(3) -0.006(3) -0.009(3) C27 0.026(4) 0.064(6) 0.021(4) -0.006(4) 0.004(3) -0.019(4) C28 0.015(4) 0.069(7) 0.039(5) -0.019(5) 0.006(3) -0.016(4) C29 0.019(4) 0.042(5) 0.031(4) -0.004(4) 0.000(3) -0.013(4) C30 0.019(3) 0.019(3) 0.023(4) -0.002(3) -0.003(3) -0.007(3) C31 0.031(4) 0.041(5) 0.016(4) -0.006(3) -0.004(3) -0.010(4) C32 0.023(4) 0.043(5) 0.016(4) -0.009(3) -0.001(3) -0.004(4) C33 0.037(5) 0.062(6) 0.019(4) -0.012(4) -0.002(3) -0.023(5) C34 0.048(6) 0.076(7) 0.016(4) 0.007(4) -0.007(4) -0.034(6) C35 0.048(6) 0.055(6) 0.038(5) 0.022(5) -0.013(4) -0.030(5) C36 0.049(6) 0.046(5) 0.028(4) 0.013(4) -0.009(4) -0.032(5) C37 0.041(5) 0.032(5) 0.054(6) -0.017(4) -0.016(5) -0.002(4) C38 0.066(8) 0.087(9) 0.041(6) 0.015(6) -0.034(6) -0.033(7) C39 0.055(6) 0.046(6) 0.052(6) 0.014(5) -0.013(5) -0.028(5) C40 0.009(3) 0.020(3) 0.025(4) -0.002(3) 0.003(3) -0.008(3) C41 0.019(4) 0.025(4) 0.023(4) 0.000(3) -0.003(3) -0.010(3) C42 0.020(4) 0.021(4) 0.031(4) -0.006(3) -0.003(3) -0.008(3) C43 0.020(4) 0.033(4) 0.022(4) -0.008(3) -0.004(3) -0.013(3) C44 0.017(3) 0.033(4) 0.023(4) 0.007(3) -0.003(3) -0.014(3) C45 0.012(3) 0.023(4) 0.030(4) 0.000(3) -0.007(3) -0.004(3) C46 0.027(4) 0.020(4) 0.038(5) -0.003(3) -0.008(3) -0.011(3) C47 0.035(5) 0.047(5) 0.026(4) -0.014(4) -0.002(4) -0.014(4) C48 0.026(4) 0.024(4) 0.032(4) 0.002(3) -0.011(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 P1 2.3023(18) . ? Ir1 N1 2.306(6) . ? Ir1 Si1 2.331(2) . ? Ir1 P2 2.332(2) . ? Cl1 Si1 2.155(3) . ? P1 C14 1.836(8) . ? P1 C1 1.838(7) . ? P1 C8 1.856(7) . ? P2 C22 1.813(9) . ? P2 C24 1.829(9) . ? P2 C23 1.831(9) . ? Si1 C25 1.925(8) . ? N1 C2 1.474(10) . ? N1 C20 1.483(9) . ? N1 C21 1.500(9) . ? C1 C6 1.386(10) . ? C1 C2 1.387(10) . ? C2 C3 1.404(10) . ? C3 C4 1.369(11) . ? C3 H1 0.9500 . ? C4 C5 1.385(11) . ? C4 H2 0.9500 . ? C5 C6 1.416(10) . ? C5 C7 1.486(10) . ? C6 H3 0.9500 . ? C7 H4 0.9800 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C8 C13 1.528(10) . ? C8 C9 1.548(10) . ? C8 H7 1.0000 . ? C9 C10 1.523(12) . ? C9 H8 0.9900 . ? C9 H9 0.9900 . ? C10 C11 1.520(12) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 C12 1.522(13) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? C12 C13 1.500(12) . ? C12 H14 0.9900 . ? C12 H15 0.9900 . ? C13 H16 0.9900 . ? C13 H17 0.9900 . ? C14 C19 1.519(10) . ? C14 C15 1.532(10) . ? C14 H18 1.0000 . ? C15 C16 1.514(11) . ? C15 H19 0.9900 . ? C15 H20 0.9900 . ? C16 C17 1.532(12) . ? C16 H21 0.9900 . ? C16 H22 0.9900 . ? C17 C18 1.507(12) . ? C17 H23 0.9900 . ? C17 H24 0.9900 . ? C18 C19 1.536(10) . ? C18 H25 0.9900 . ? C18 H26 0.9900 . ? C19 H27 0.9900 . ? C19 H28 0.9900 . ? C20 H29 0.9800 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C21 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C22 H35 0.9800 . ? C22 H36 0.9800 . ? C22 H37 0.9800 . ? C23 H38 0.9800 . ? C23 H39 0.9800 . ? C23 H40 0.9800 . ? C24 H41 0.9800 . ? C24 H42 0.9800 . ? C24 H43 0.9800 . ? C25 C26 1.409(11) . ? C25 C30 1.422(11) . ? C26 C27 1.398(11) . ? C26 C31 1.488(12) . ? C27 C28 1.376(13) . ? C27 H44 0.9500 . ? C28 C29 1.369(12) . ? C28 H45 0.9500 . ? C29 C30 1.396(10) . ? C29 H46 0.9500 . ? C30 C40 1.485(10) . ? C31 C32 1.408(13) . ? C31 C36 1.420(13) . ? C32 C33 1.378(12) . ? C32 C37 1.486(13) . ? C33 C34 1.411(15) . ? C33 H47 0.9500 . ? C34 C35 1.348(15) . ? C34 C38 1.507(13) . ? C35 C36 1.387(14) . ? C35 H48 0.9500 . ? C36 C39 1.509(14) . ? C37 H49 0.9800 . ? C37 H50 0.9800 . ? C37 H51 0.9800 . ? C38 H52 0.9800 . ? C38 H53 0.9800 . ? C38 H54 0.9800 . ? C39 H55 0.9800 . ? C39 H56 0.9800 . ? C39 H57 0.9800 . ? C40 C45 1.402(10) . ? C40 C41 1.406(10) . ? C41 C42 1.402(11) . ? C41 C46 1.510(10) . ? C42 C43 1.395(11) . ? C42 H58 0.9500 . ? C43 C44 1.376(11) . ? C43 C47 1.510(11) . ? C44 C45 1.388(11) . ? C44 H59 0.9500 . ? C45 C48 1.523(11) . ? C46 H60 0.9800 . ? C46 H61 0.9800 . ? C46 H62 0.9800 . ? C47 H63 0.9800 . ? C47 H64 0.9800 . ? C47 H65 0.9800 . ? C48 H66 0.9800 . ? C48 H67 0.9800 . ? C48 H68 0.9800 . ? O1 C49 1.475(19) . ? O1 C52 1.51(2) . ? C49 C50 1.461(19) . ? C50 C51 1.493(19) . ? C51 C52 1.499(19) . ? 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 P1 Ir1 N1 82.21(16) . . ? P1 Ir1 Si1 163.97(7) . . ? N1 Ir1 Si1 105.10(16) . . ? P1 Ir1 P2 104.25(7) . . ? N1 Ir1 P2 98.77(16) . . ? Si1 Ir1 P2 88.92(7) . . ? C14 P1 C1 100.3(3) . . ? C14 P1 C8 104.1(3) . . ? C1 P1 C8 106.9(3) . . ? C14 P1 Ir1 120.6(2) . . ? C1 P1 Ir1 103.9(2) . . ? C8 P1 Ir1 118.8(2) . . ? C22 P2 C24 97.7(4) . . ? C22 P2 C23 99.5(4) . . ? C24 P2 C23 100.3(5) . . ? C22 P2 Ir1 119.2(3) . . ? C24 P2 Ir1 114.4(3) . . ? C23 P2 Ir1 121.6(3) . . ? C25 Si1 Cl1 102.9(2) . . ? C25 Si1 Ir1 125.3(2) . . ? Cl1 Si1 Ir1 116.68(10) . . ? C2 N1 C20 110.3(6) . . ? C2 N1 C21 108.0(6) . . ? C20 N1 C21 106.5(6) . . ? C2 N1 Ir1 113.5(4) . . ? C20 N1 Ir1 110.5(5) . . ? C21 N1 Ir1 107.8(4) . . ? C6 C1 C2 118.9(6) . . ? C6 C1 P1 123.8(5) . . ? C2 C1 P1 117.1(5) . . ? C1 C2 C3 119.2(7) . . ? C1 C2 N1 122.0(6) . . ? C3 C2 N1 118.8(7) . . ? C4 C3 C2 120.8(7) . . ? C4 C3 H1 119.6 . . ? C2 C3 H1 119.6 . . ? C3 C4 C5 122.1(7) . . ? C3 C4 H2 119.0 . . ? C5 C4 H2 119.0 . . ? C4 C5 C6 116.3(7) . . ? C4 C5 C7 121.2(7) . . ? C6 C5 C7 122.5(7) . . ? C1 C6 C5 122.8(7) . . ? C1 C6 H3 118.6 . . ? C5 C6 H3 118.6 . . ? C5 C7 H4 109.5 . . ? C5 C7 H5 109.5 . . ? H4 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H4 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C13 C8 C9 108.0(6) . . ? C13 C8 P1 111.3(5) . . ? C9 C8 P1 119.4(6) . . ? C13 C8 H7 105.7 . . ? C9 C8 H7 105.7 . . ? P1 C8 H7 105.7 . . ? C10 C9 C8 110.4(7) . . ? C10 C9 H8 109.6 . . ? C8 C9 H8 109.6 . . ? C10 C9 H9 109.6 . . ? C8 C9 H9 109.6 . . ? H8 C9 H9 108.1 . . ? C11 C10 C9 112.1(8) . . ? C11 C10 H10 109.2 . . ? C9 C10 H10 109.2 . . ? C11 C10 H11 109.2 . . ? C9 C10 H11 109.2 . . ? H10 C10 H11 107.9 . . ? C10 C11 C12 111.2(7) . . ? C10 C11 H12 109.4 . . ? C12 C11 H12 109.4 . . ? C10 C11 H13 109.4 . . ? C12 C11 H13 109.4 . . ? H12 C11 H13 108.0 . . ? C13 C12 C11 111.0(8) . . ? C13 C12 H14 109.4 . . ? C11 C12 H14 109.4 . . ? C13 C12 H15 109.4 . . ? C11 C12 H15 109.4 . . ? H14 C12 H15 108.0 . . ? C12 C13 C8 112.7(7) . . ? C12 C13 H16 109.0 . . ? C8 C13 H16 109.0 . . ? C12 C13 H17 109.0 . . ? C8 C13 H17 109.0 . . ? H16 C13 H17 107.8 . . ? C19 C14 C15 109.4(6) . . ? C19 C14 P1 112.8(5) . . ? C15 C14 P1 114.0(5) . . ? C19 C14 H18 106.7 . . ? C15 C14 H18 106.7 . . ? P1 C14 H18 106.7 . . ? C16 C15 C14 111.8(7) . . ? C16 C15 H19 109.2 . . ? C14 C15 H19 109.2 . . ? C16 C15 H20 109.2 . . ? C14 C15 H20 109.2 . . ? H19 C15 H20 107.9 . . ? C15 C16 C17 112.1(7) . . ? C15 C16 H21 109.2 . . ? C17 C16 H21 109.2 . . ? C15 C16 H22 109.2 . . ? C17 C16 H22 109.2 . . ? H21 C16 H22 107.9 . . ? C18 C17 C16 110.8(7) . . ? C18 C17 H23 109.5 . . ? C16 C17 H23 109.5 . . ? C18 C17 H24 109.5 . . ? C16 C17 H24 109.5 . . ? H23 C17 H24 108.1 . . ? C17 C18 C19 113.4(7) . . ? C17 C18 H25 108.9 . . ? C19 C18 H25 108.9 . . ? C17 C18 H26 108.9 . . ? C19 C18 H26 108.9 . . ? H25 C18 H26 107.7 . . ? C14 C19 C18 112.3(6) . . ? C14 C19 H27 109.1 . . ? C18 C19 H27 109.1 . . ? C14 C19 H28 109.1 . . ? C18 C19 H28 109.1 . . ? H27 C19 H28 107.9 . . ? N1 C20 H29 109.5 . . ? N1 C20 H30 109.5 . . ? H29 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H29 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C21 H32 109.5 . . ? N1 C21 H33 109.5 . . ? H32 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H32 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? P2 C22 H35 109.5 . . ? P2 C22 H36 109.5 . . ? H35 C22 H36 109.5 . . ? P2 C22 H37 109.5 . . ? H35 C22 H37 109.5 . . ? H36 C22 H37 109.5 . . ? P2 C23 H38 109.5 . . ? P2 C23 H39 109.5 . . ? H38 C23 H39 109.5 . . ? P2 C23 H40 109.5 . . ? H38 C23 H40 109.5 . . ? H39 C23 H40 109.5 . . ? P2 C24 H41 109.5 . . ? P2 C24 H42 109.5 . . ? H41 C24 H42 109.5 . . ? P2 C24 H43 109.5 . . ? H41 C24 H43 109.5 . . ? H42 C24 H43 109.5 . . ? C26 C25 C30 117.6(7) . . ? C26 C25 Si1 117.6(6) . . ? C30 C25 Si1 124.7(5) . . ? C27 C26 C25 120.0(8) . . ? C27 C26 C31 117.2(7) . . ? C25 C26 C31 122.8(7) . . ? C28 C27 C26 121.7(8) . . ? C28 C27 H44 119.1 . . ? C26 C27 H44 119.1 . . ? C29 C28 C27 118.9(7) . . ? C29 C28 H45 120.6 . . ? C27 C28 H45 120.6 . . ? C28 C29 C30 121.7(8) . . ? C28 C29 H46 119.1 . . ? C30 C29 H46 119.1 . . ? C29 C30 C25 119.9(7) . . ? C29 C30 C40 115.7(7) . . ? C25 C30 C40 124.2(6) . . ? C32 C31 C36 119.6(8) . . ? C32 C31 C26 120.9(8) . . ? C36 C31 C26 119.3(8) . . ? C33 C32 C31 118.8(9) . . ? C33 C32 C37 120.0(9) . . ? C31 C32 C37 121.2(8) . . ? C32 C33 C34 121.7(9) . . ? C32 C33 H47 119.2 . . ? C34 C33 H47 119.2 . . ? C35 C34 C33 118.6(9) . . ? C35 C34 C38 122.0(11) . . ? C33 C34 C38 119.4(10) . . ? C34 C35 C36 122.7(10) . . ? C34 C35 H48 118.6 . . ? C36 C35 H48 118.6 . . ? C35 C36 C31 118.6(9) . . ? C35 C36 C39 120.4(9) . . ? C31 C36 C39 121.0(9) . . ? C32 C37 H49 109.5 . . ? C32 C37 H50 109.5 . . ? H49 C37 H50 109.5 . . ? C32 C37 H51 109.5 . . ? H49 C37 H51 109.5 . . ? H50 C37 H51 109.5 . . ? C34 C38 H52 109.5 . . ? C34 C38 H53 109.5 . . ? H52 C38 H53 109.5 . . ? C34 C38 H54 109.5 . . ? H52 C38 H54 109.5 . . ? H53 C38 H54 109.5 . . ? C36 C39 H55 109.5 . . ? C36 C39 H56 109.5 . . ? H55 C39 H56 109.5 . . ? C36 C39 H57 109.5 . . ? H55 C39 H57 109.5 . . ? H56 C39 H57 109.5 . . ? C45 C40 C41 118.7(7) . . ? C45 C40 C30 122.8(7) . . ? C41 C40 C30 118.2(6) . . ? C42 C41 C40 119.9(7) . . ? C42 C41 C46 118.7(7) . . ? C40 C41 C46 121.3(7) . . ? C43 C42 C41 120.7(7) . . ? C43 C42 H58 119.6 . . ? C41 C42 H58 119.6 . . ? C44 C43 C42 118.5(7) . . ? C44 C43 C47 121.0(7) . . ? C42 C43 C47 120.5(7) . . ? C43 C44 C45 122.2(7) . . ? C43 C44 H59 118.9 . . ? C45 C44 H59 118.9 . . ? C44 C45 C40 119.7(7) . . ? C44 C45 C48 120.0(7) . . ? C40 C45 C48 120.2(7) . . ? C41 C46 H60 109.5 . . ? C41 C46 H61 109.5 . . ? H60 C46 H61 109.5 . . ? C41 C46 H62 109.5 . . ? H60 C46 H62 109.5 . . ? H61 C46 H62 109.5 . . ? C43 C47 H63 109.5 . . ? C43 C47 H64 109.5 . . ? H63 C47 H64 109.5 . . ? C43 C47 H65 109.5 . . ? H63 C47 H65 109.5 . . ? H64 C47 H65 109.5 . . ? C45 C48 H66 109.5 . . ? C45 C48 H67 109.5 . . ? H66 C48 H67 109.5 . . ? C45 C48 H68 109.5 . . ? H66 C48 H68 109.5 . . ? H67 C48 H68 109.5 . . ? C49 O1 C52 117(4) . . ? C50 C49 O1 107(3) . . ? C49 C50 C51 92(3) . . ? C50 C51 C52 130(4) . . ? C51 C52 O1 85(3) . . ? 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 N1 Ir1 P1 C14 -102.4(3) . . . . ? Si1 Ir1 P1 C14 16.0(4) . . . . ? P2 Ir1 P1 C14 160.4(3) . . . . ? N1 Ir1 P1 C1 8.6(3) . . . . ? Si1 Ir1 P1 C1 127.1(3) . . . . ? P2 Ir1 P1 C1 -88.5(2) . . . . ? N1 Ir1 P1 C8 127.2(3) . . . . ? Si1 Ir1 P1 C8 -114.3(4) . . . . ? P2 Ir1 P1 C8 30.1(3) . . . . ? P1 Ir1 P2 C22 146.2(4) . . . . ? N1 Ir1 P2 C22 62.1(4) . . . . ? Si1 Ir1 P2 C22 -43.0(4) . . . . ? P1 Ir1 P2 C24 -98.7(4) . . . . ? N1 Ir1 P2 C24 177.2(4) . . . . ? Si1 Ir1 P2 C24 72.0(4) . . . . ? P1 Ir1 P2 C23 21.9(4) . . . . ? N1 Ir1 P2 C23 -62.2(4) . . . . ? Si1 Ir1 P2 C23 -167.4(4) . . . . ? P1 Ir1 Si1 C25 3.2(4) . . . . ? N1 Ir1 Si1 C25 118.7(3) . . . . ? P2 Ir1 Si1 C25 -142.5(3) . . . . ? P1 Ir1 Si1 Cl1 -128.3(2) . . . . ? N1 Ir1 Si1 Cl1 -12.8(2) . . . . ? P2 Ir1 Si1 Cl1 86.04(12) . . . . ? P1 Ir1 N1 C2 -10.2(4) . . . . ? Si1 Ir1 N1 C2 -175.7(4) . . . . ? P2 Ir1 N1 C2 93.1(4) . . . . ? P1 Ir1 N1 C20 -134.7(5) . . . . ? Si1 Ir1 N1 C20 59.9(5) . . . . ? P2 Ir1 N1 C20 -31.4(5) . . . . ? P1 Ir1 N1 C21 109.3(5) . . . . ? Si1 Ir1 N1 C21 -56.2(5) . . . . ? P2 Ir1 N1 C21 -147.4(4) . . . . ? C14 P1 C1 C6 -58.2(7) . . . . ? C8 P1 C1 C6 50.1(7) . . . . ? Ir1 P1 C1 C6 176.5(6) . . . . ? C14 P1 C1 C2 117.5(6) . . . . ? C8 P1 C1 C2 -134.2(6) . . . . ? Ir1 P1 C1 C2 -7.7(6) . . . . ? C6 C1 C2 C3 -1.7(10) . . . . ? P1 C1 C2 C3 -177.6(6) . . . . ? C6 C1 C2 N1 175.6(6) . . . . ? P1 C1 C2 N1 -0.3(9) . . . . ? C20 N1 C2 C1 133.3(7) . . . . ? C21 N1 C2 C1 -110.8(7) . . . . ? Ir1 N1 C2 C1 8.7(8) . . . . ? C20 N1 C2 C3 -49.4(9) . . . . ? C21 N1 C2 C3 66.5(8) . . . . ? Ir1 N1 C2 C3 -174.0(5) . . . . ? C1 C2 C3 C4 0.5(11) . . . . ? N1 C2 C3 C4 -176.9(7) . . . . ? C2 C3 C4 C5 0.6(12) . . . . ? C3 C4 C5 C6 -0.5(11) . . . . ? C3 C4 C5 C7 179.2(7) . . . . ? C2 C1 C6 C5 1.8(11) . . . . ? P1 C1 C6 C5 177.5(6) . . . . ? C4 C5 C6 C1 -0.7(11) . . . . ? C7 C5 C6 C1 179.5(7) . . . . ? C14 P1 C8 C13 -93.3(6) . . . . ? C1 P1 C8 C13 161.1(5) . . . . ? Ir1 P1 C8 C13 44.1(6) . . . . ? C14 P1 C8 C9 33.6(7) . . . . ? C1 P1 C8 C9 -71.9(7) . . . . ? Ir1 P1 C8 C9 171.1(5) . . . . ? C13 C8 C9 C10 -57.2(9) . . . . ? P1 C8 C9 C10 174.3(6) . . . . ? C8 C9 C10 C11 56.7(11) . . . . ? C9 C10 C11 C12 -54.1(12) . . . . ? C10 C11 C12 C13 53.4(12) . . . . ? C11 C12 C13 C8 -57.3(10) . . . . ? C9 C8 C13 C12 58.6(9) . . . . ? P1 C8 C13 C12 -168.5(6) . . . . ? C1 P1 C14 C19 -53.6(6) . . . . ? C8 P1 C14 C19 -164.0(5) . . . . ? Ir1 P1 C14 C19 59.5(6) . . . . ? C1 P1 C14 C15 -179.1(5) . . . . ? C8 P1 C14 C15 70.4(6) . . . . ? Ir1 P1 C14 C15 -66.1(6) . . . . ? C19 C14 C15 C16 56.7(9) . . . . ? P1 C14 C15 C16 -176.0(6) . . . . ? C14 C15 C16 C17 -56.9(10) . . . . ? C15 C16 C17 C18 53.0(10) . . . . ? C16 C17 C18 C19 -51.0(10) . . . . ? C15 C14 C19 C18 -54.2(9) . . . . ? P1 C14 C19 C18 177.8(6) . . . . ? C17 C18 C19 C14 53.1(10) . . . . ? Cl1 Si1 C25 C26 -124.6(6) . . . . ? Ir1 Si1 C25 C26 98.8(6) . . . . ? Cl1 Si1 C25 C30 51.3(7) . . . . ? Ir1 Si1 C25 C30 -85.2(7) . . . . ? C30 C25 C26 C27 -3.8(12) . . . . ? Si1 C25 C26 C27 172.4(7) . . . . ? C30 C25 C26 C31 173.0(7) . . . . ? Si1 C25 C26 C31 -10.8(10) . . . . ? C25 C26 C27 C28 0.1(15) . . . . ? C31 C26 C27 C28 -176.9(9) . . . . ? C26 C27 C28 C29 2.3(16) . . . . ? C27 C28 C29 C30 -0.8(15) . . . . ? C28 C29 C30 C25 -3.0(13) . . . . ? C28 C29 C30 C40 173.0(9) . . . . ? C26 C25 C30 C29 5.2(11) . . . . ? Si1 C25 C30 C29 -170.7(6) . . . . ? C26 C25 C30 C40 -170.5(7) . . . . ? Si1 C25 C30 C40 13.6(10) . . . . ? C27 C26 C31 C32 -84.0(10) . . . . ? C25 C26 C31 C32 99.0(10) . . . . ? C27 C26 C31 C36 90.6(10) . . . . ? C25 C26 C31 C36 -86.3(10) . . . . ? C36 C31 C32 C33 1.8(12) . . . . ? C26 C31 C32 C33 176.4(7) . . . . ? C36 C31 C32 C37 -180.0(8) . . . . ? C26 C31 C32 C37 -5.3(12) . . . . ? C31 C32 C33 C34 -0.9(12) . . . . ? C37 C32 C33 C34 -179.2(8) . . . . ? C32 C33 C34 C35 -0.3(14) . . . . ? C32 C33 C34 C38 -179.3(9) . . . . ? C33 C34 C35 C36 0.6(15) . . . . ? C38 C34 C35 C36 179.5(10) . . . . ? C34 C35 C36 C31 0.3(15) . . . . ? C34 C35 C36 C39 -177.7(9) . . . . ? C32 C31 C36 C35 -1.5(13) . . . . ? C26 C31 C36 C35 -176.2(8) . . . . ? C32 C31 C36 C39 176.5(8) . . . . ? C26 C31 C36 C39 1.8(13) . . . . ? C29 C30 C40 C45 80.5(9) . . . . ? C25 C30 C40 C45 -103.6(9) . . . . ? C29 C30 C40 C41 -92.9(9) . . . . ? C25 C30 C40 C41 82.9(9) . . . . ? C45 C40 C41 C42 5.5(10) . . . . ? C30 C40 C41 C42 179.2(7) . . . . ? C45 C40 C41 C46 -171.1(7) . . . . ? C30 C40 C41 C46 2.6(10) . . . . ? C40 C41 C42 C43 -2.9(11) . . . . ? C46 C41 C42 C43 173.8(7) . . . . ? C41 C42 C43 C44 -0.8(11) . . . . ? C41 C42 C43 C47 178.9(7) . . . . ? C42 C43 C44 C45 1.9(11) . . . . ? C47 C43 C44 C45 -177.8(7) . . . . ? C43 C44 C45 C40 0.8(11) . . . . ? C43 C44 C45 C48 -176.7(7) . . . . ? C41 C40 C45 C44 -4.5(10) . . . . ? C30 C40 C45 C44 -177.9(7) . . . . ? C41 C40 C45 C48 173.0(7) . . . . ? C30 C40 C45 C48 -0.3(10) . . . . ? C52 O1 C49 C50 -34(5) . . . . ? O1 C49 C50 C51 25(4) . . . . ? C49 C50 C51 C52 -17(6) . . . . ? C50 C51 C52 O1 -1(6) . . . . ? C49 O1 C52 C51 20(4) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.919 _refine_diff_density_min -3.495 _refine_diff_density_rms 0.316 #===END data_(PcyN-P,N)IrHCl(DMAP)(SiH2Trip)-(12)\/YCH2Cl2?-C5H12 _database_code_depnum_ccdc_archive 'CCDC 772169' #TrackingRef '- ToshiCIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H70 Cl Ir N3 P Si, C H Cl2, C5 H12' _chemical_formula_sum 'C49 H84 Cl3 Ir N3 P Si' _chemical_formula_weight 1072.80 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' 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' N N 0.0061 0.0033 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7958(7) _cell_length_b 12.2790(7) _cell_length_c 18.9266(8) _cell_angle_alpha 104.795(3) _cell_angle_beta 99.527(4) _cell_angle_gamma 92.1081(15) _cell_volume 2604.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11632 _cell_measurement_theta_min 1.13 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.805 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5774 _exptl_absorpt_correction_T_max 0.6178 _exptl_absorpt_process_details 'NUMABS (Higashi, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23832 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 27.43 _reflns_number_total 11632 _reflns_number_gt 10517 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _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^)+(0.0592P)^2^+5.7423P] 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 11632 _refine_ls_number_parameters 513 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.1113 _refine_ls_goodness_of_fit_ref 1.218 _refine_ls_restrained_S_all 1.227 _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 0.090446(16) 0.199231(16) 0.231535(10) 0.01786(7) Uani 1 1 d . . . H1 H 0.118(5) 0.325(5) 0.277(3) 0.025(15) Uiso 1 1 d . . . Cl1 Cl 0.07337(13) -0.00171(11) 0.15832(7) 0.0301(3) Uani 1 1 d . . . Cl2 Cl 0.2701(2) 0.7258(2) 0.17248(15) 0.0709(6) Uani 1 1 d . . . Cl3 Cl 0.2903(3) 0.7679(2) 0.02959(14) 0.0795(7) Uani 1 1 d . . . P1 P 0.05098(11) 0.17489(11) 0.33743(7) 0.0192(2) Uani 1 1 d . . . Si1 Si 0.28912(12) 0.19666(13) 0.26100(8) 0.0242(3) Uani 1 1 d . . . N1 N -0.1089(4) 0.2179(4) 0.2054(2) 0.0272(10) Uani 1 1 d . . . N2 N 0.1078(4) 0.2503(4) 0.1330(2) 0.0215(8) Uani 1 1 d . . . N3 N 0.0928(5) 0.3782(4) -0.0533(3) 0.0333(11) Uani 1 1 d . . . C1 C -0.1005(4) 0.2048(4) 0.3353(3) 0.0211(10) Uani 1 1 d . . . C2 C -0.1635(4) 0.2232(4) 0.2709(3) 0.0232(10) Uani 1 1 d . . . C3 C -0.2797(5) 0.2419(5) 0.2672(3) 0.0297(12) Uani 1 1 d . . . H2 H -0.3223 0.2545 0.2232 0.036 Uiso 1 1 calc R . . C4 C -0.3340(5) 0.2425(5) 0.3267(3) 0.0297(12) Uani 1 1 d . . . H3 H -0.4132 0.2563 0.3232 0.036 Uiso 1 1 calc R . . C5 C -0.2741(5) 0.2233(4) 0.3914(3) 0.0254(11) Uani 1 1 d . . . C6 C -0.1583(5) 0.2045(4) 0.3945(3) 0.0246(10) Uani 1 1 d . . . H4 H -0.1164 0.1910 0.4384 0.029 Uiso 1 1 calc R . . C7 C -0.3341(5) 0.2241(6) 0.4555(4) 0.0395(14) Uani 1 1 d . . . H5 H -0.2927 0.2797 0.5001 0.059 Uiso 1 1 calc R . . H6 H -0.3355 0.1489 0.4644 0.059 Uiso 1 1 calc R . . H7 H -0.4134 0.2443 0.4439 0.059 Uiso 1 1 calc R . . C8 C 0.0510(5) 0.0366(4) 0.3594(3) 0.0237(10) Uani 1 1 d . . . H8 H 0.0364 0.0496 0.4113 0.028 Uiso 1 1 calc R . . C9 C -0.0442(5) -0.0522(5) 0.3085(3) 0.0278(11) Uani 1 1 d . . . H9 H -0.1205 -0.0216 0.3099 0.033 Uiso 1 1 calc R . . H10 H -0.0311 -0.0694 0.2566 0.033 Uiso 1 1 calc R . . C10 C -0.0422(6) -0.1603(5) 0.3349(4) 0.0358(13) Uani 1 1 d . . . H11 H -0.0612 -0.1436 0.3854 0.043 Uiso 1 1 calc R . . H12 H -0.1017 -0.2177 0.3014 0.043 Uiso 1 1 calc R . . C11 C 0.0754(7) -0.2078(5) 0.3362(4) 0.0444(16) Uani 1 1 d . . . H13 H 0.0753 -0.2748 0.3563 0.053 Uiso 1 1 calc R . . H14 H 0.0910 -0.2321 0.2849 0.053 Uiso 1 1 calc R . . C12 C 0.1701(6) -0.1194(6) 0.3840(4) 0.0417(15) Uani 1 1 d . . . H15 H 0.2459 -0.1510 0.3821 0.050 Uiso 1 1 calc R . . H16 H 0.1586 -0.1009 0.4363 0.050 Uiso 1 1 calc R . . C13 C 0.1705(5) -0.0108(5) 0.3579(3) 0.0324(12) Uani 1 1 d . . . H17 H 0.1873 -0.0275 0.3068 0.039 Uiso 1 1 calc R . . H18 H 0.2312 0.0458 0.3910 0.039 Uiso 1 1 calc R . . C14 C 0.1339(5) 0.2755(4) 0.4236(3) 0.0233(10) Uani 1 1 d . . . H19 H 0.2156 0.2792 0.4158 0.028 Uiso 1 1 calc R . . C15 C 0.1383(5) 0.2442(5) 0.4978(3) 0.0306(12) Uani 1 1 d . . . H20 H 0.0597 0.2421 0.5096 0.037 Uiso 1 1 calc R . . H21 H 0.1660 0.1680 0.4930 0.037 Uiso 1 1 calc R . . C16 C 0.2184(6) 0.3299(6) 0.5608(3) 0.0373(14) Uani 1 1 d . . . H22 H 0.2173 0.3094 0.6080 0.045 Uiso 1 1 calc R . . H23 H 0.2982 0.3267 0.5510 0.045 Uiso 1 1 calc R . . C17 C 0.1833(6) 0.4494(6) 0.5689(3) 0.0386(14) Uani 1 1 d . . . H24 H 0.2405 0.5028 0.6076 0.046 Uiso 1 1 calc R . . H25 H 0.1074 0.4554 0.5847 0.046 Uiso 1 1 calc R . . C18 C 0.1763(6) 0.4803(5) 0.4955(3) 0.0349(13) Uani 1 1 d . . . H26 H 0.2546 0.4838 0.4833 0.042 Uiso 1 1 calc R . . H27 H 0.1477 0.5563 0.5008 0.042 Uiso 1 1 calc R . . C19 C 0.0968(5) 0.3954(5) 0.4320(3) 0.0285(11) Uani 1 1 d . . . H28 H 0.0978 0.4167 0.3851 0.034 Uiso 1 1 calc R . . H29 H 0.0168 0.3976 0.4417 0.034 Uiso 1 1 calc R . . C20 C -0.1683(5) 0.1208(6) 0.1432(3) 0.0382(15) Uani 1 1 d . . . H30 H -0.1571 0.0499 0.1573 0.057 Uiso 1 1 calc R . . H31 H -0.1358 0.1183 0.0985 0.057 Uiso 1 1 calc R . . H32 H -0.2510 0.1306 0.1332 0.057 Uiso 1 1 calc R . . C21 C -0.1241(5) 0.3234(6) 0.1820(4) 0.0415(15) Uani 1 1 d . . . H33 H -0.2066 0.3317 0.1686 0.062 Uiso 1 1 calc R . . H34 H -0.0870 0.3202 0.1390 0.062 Uiso 1 1 calc R . . H35 H -0.0888 0.3881 0.2230 0.062 Uiso 1 1 calc R . . C22 C 0.3780(4) 0.2952(4) 0.2228(3) 0.0231(10) Uani 1 1 d . . . C23 C 0.4162(4) 0.2579(5) 0.1545(3) 0.0248(10) Uani 1 1 d . . . C24 C 0.4876(5) 0.3291(5) 0.1314(3) 0.0278(11) Uani 1 1 d . . . H36 H 0.5138 0.3012 0.0858 0.033 Uiso 1 1 calc R . . C25 C 0.5220(5) 0.4396(5) 0.1725(3) 0.0304(12) Uani 1 1 d . . . C26 C 0.4785(5) 0.4792(5) 0.2371(3) 0.0297(12) Uani 1 1 d . . . H37 H 0.4979 0.5556 0.2650 0.036 Uiso 1 1 calc R . . C27 C 0.4069(4) 0.4103(4) 0.2627(3) 0.0235(10) Uani 1 1 d . . . C28 C 0.3827(5) 0.1389(5) 0.1029(3) 0.0329(13) Uani 1 1 d . . . H38 H 0.3138 0.1069 0.1176 0.039 Uiso 1 1 calc R . . C29 C 0.4800(6) 0.0630(6) 0.1131(4) 0.0464(17) Uani 1 1 d . . . H39 H 0.5502 0.0951 0.1019 0.070 Uiso 1 1 calc R . . H40 H 0.4581 -0.0125 0.0793 0.070 Uiso 1 1 calc R . . H41 H 0.4944 0.0576 0.1645 0.070 Uiso 1 1 calc R . . C30 C 0.3502(6) 0.1379(7) 0.0209(4) 0.0477(18) Uani 1 1 d . . . H42 H 0.2917 0.1912 0.0155 0.072 Uiso 1 1 calc R . . H43 H 0.3194 0.0617 -0.0085 0.072 Uiso 1 1 calc R . . H44 H 0.4189 0.1602 0.0034 0.072 Uiso 1 1 calc R . . C31 C 0.6017(6) 0.5152(6) 0.1456(4) 0.0426(16) Uani 1 1 d . . . H45 H 0.6425 0.4645 0.1096 0.051 Uiso 1 1 calc R . . C32 C 0.6945(7) 0.5851(6) 0.2096(5) 0.056(2) Uani 1 1 d . . . H46 H 0.6578 0.6391 0.2447 0.084 Uiso 1 1 calc R . . H47 H 0.7487 0.6261 0.1896 0.084 Uiso 1 1 calc R . . H48 H 0.7361 0.5345 0.2353 0.084 Uiso 1 1 calc R . . C33 C 0.5320(9) 0.5882(8) 0.1039(6) 0.070(3) Uani 1 1 d . . . H49 H 0.4789 0.5397 0.0612 0.105 Uiso 1 1 calc R . . H50 H 0.5842 0.6354 0.0866 0.105 Uiso 1 1 calc R . . H51 H 0.4878 0.6367 0.1371 0.105 Uiso 1 1 calc R . . C34 C 0.3621(5) 0.4629(5) 0.3340(3) 0.0263(11) Uani 1 1 d . . . H52 H 0.3049 0.4064 0.3411 0.032 Uiso 1 1 calc R . . C35 C 0.4619(5) 0.4891(6) 0.4014(3) 0.0377(14) Uani 1 1 d . . . H53 H 0.4957 0.4189 0.4058 0.057 Uiso 1 1 calc R . . H54 H 0.4324 0.5235 0.4467 0.057 Uiso 1 1 calc R . . H55 H 0.5211 0.5416 0.3944 0.057 Uiso 1 1 calc R . . C36 C 0.3015(6) 0.5699(5) 0.3305(3) 0.0371(14) Uani 1 1 d . . . H56 H 0.3578 0.6293 0.3286 0.056 Uiso 1 1 calc R . . H57 H 0.2664 0.5954 0.3747 0.056 Uiso 1 1 calc R . . H58 H 0.2413 0.5535 0.2859 0.056 Uiso 1 1 calc R . . C37 C 0.0682(5) 0.1850(5) 0.0630(3) 0.0249(11) Uani 1 1 d . . . H59 H 0.0435 0.1081 0.0569 0.030 Uiso 1 1 calc R . . C38 C 0.0617(5) 0.2232(5) 0.0003(3) 0.0261(11) Uani 1 1 d . . . H60 H 0.0322 0.1735 -0.0472 0.031 Uiso 1 1 calc R . . C39 C 0.0988(5) 0.3358(5) 0.0066(3) 0.0252(11) Uani 1 1 d . . . C40 C 0.1429(5) 0.4030(4) 0.0791(3) 0.0255(11) Uani 1 1 d . . . H61 H 0.1710 0.4794 0.0869 0.031 Uiso 1 1 calc R . . C41 C 0.1451(5) 0.3575(4) 0.1384(3) 0.0245(10) Uani 1 1 d . . . H62 H 0.1751 0.4049 0.1866 0.029 Uiso 1 1 calc R . . C42 C 0.0557(6) 0.3046(6) -0.1276(3) 0.0445(17) Uani 1 1 d . . . H63 H 0.1117 0.2485 -0.1383 0.067 Uiso 1 1 calc R . . H64 H 0.0502 0.3497 -0.1638 0.067 Uiso 1 1 calc R . . H65 H -0.0200 0.2660 -0.1310 0.067 Uiso 1 1 calc R . . C43 C 0.1453(5) 0.4904(5) -0.0447(3) 0.0341(13) Uani 1 1 d . . . H66 H 0.1079 0.5461 -0.0111 0.051 Uiso 1 1 calc R . . H67 H 0.1360 0.5068 -0.0933 0.051 Uiso 1 1 calc R . . H68 H 0.2276 0.4942 -0.0240 0.051 Uiso 1 1 calc R . . C44 C 0.3004(8) 0.8272(7) 0.1247(5) 0.061(2) Uani 1 1 d . . . H69 H 0.2456 0.8864 0.1326 0.074 Uiso 1 1 calc R . . H70 H 0.3792 0.8638 0.1458 0.074 Uiso 1 1 calc R . . C45 C 0.6466(13) 0.8920(13) 0.2119(8) 0.115(5) Uiso 1 1 d D . . C46 C 0.5884(8) 0.9056(8) 0.2699(5) 0.058(2) Uiso 1 1 d D . . C47 C 0.6287(18) 0.8969(18) 0.3396(9) 0.159(7) Uiso 1 1 d D . . C48 C 0.502(2) 0.910(3) 0.3412(15) 0.286(16) Uiso 1 1 d D . . C49 C 0.5335(11) 0.8792(11) 0.4131(7) 0.091(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01976(10) 0.01629(10) 0.01621(10) 0.00368(6) 0.00099(6) -0.00069(6) Cl1 0.0451(8) 0.0181(6) 0.0244(6) 0.0026(5) 0.0045(5) -0.0027(5) Cl2 0.0682(14) 0.0593(13) 0.0967(18) 0.0264(12) 0.0375(13) 0.0071(10) Cl3 0.108(2) 0.0532(13) 0.0627(14) 0.0078(10) -0.0086(13) -0.0149(13) P1 0.0190(6) 0.0186(6) 0.0191(6) 0.0055(5) 0.0004(4) 0.0005(5) Si1 0.0215(7) 0.0248(7) 0.0263(7) 0.0065(6) 0.0045(5) 0.0020(5) N1 0.028(2) 0.033(3) 0.020(2) 0.0102(18) -0.0001(17) 0.0016(19) N2 0.025(2) 0.019(2) 0.021(2) 0.0054(16) 0.0036(16) 0.0006(16) N3 0.043(3) 0.032(3) 0.028(2) 0.013(2) 0.009(2) -0.001(2) C1 0.022(2) 0.019(2) 0.020(2) 0.0030(18) 0.0018(18) 0.0012(19) C2 0.019(2) 0.025(3) 0.024(3) 0.0060(19) 0.0011(19) 0.0011(19) C3 0.022(3) 0.034(3) 0.033(3) 0.010(2) 0.001(2) 0.005(2) C4 0.023(3) 0.031(3) 0.033(3) 0.004(2) 0.006(2) 0.005(2) C5 0.025(3) 0.022(3) 0.026(3) 0.000(2) 0.006(2) 0.002(2) C6 0.026(3) 0.025(3) 0.021(2) 0.0036(19) 0.0010(19) -0.001(2) C7 0.031(3) 0.050(4) 0.036(3) 0.005(3) 0.011(3) 0.007(3) C8 0.028(3) 0.019(2) 0.027(3) 0.0109(19) 0.004(2) 0.004(2) C9 0.036(3) 0.023(3) 0.025(3) 0.010(2) 0.002(2) 0.000(2) C10 0.051(4) 0.024(3) 0.035(3) 0.013(2) 0.011(3) -0.004(3) C11 0.062(5) 0.024(3) 0.051(4) 0.016(3) 0.011(3) 0.012(3) C12 0.048(4) 0.036(4) 0.046(4) 0.021(3) 0.006(3) 0.017(3) C13 0.030(3) 0.034(3) 0.036(3) 0.016(2) 0.004(2) 0.012(2) C14 0.024(2) 0.025(3) 0.020(2) 0.0046(19) 0.0026(19) -0.002(2) C15 0.033(3) 0.034(3) 0.022(3) 0.007(2) -0.002(2) -0.005(2) C16 0.038(3) 0.043(4) 0.025(3) 0.005(2) -0.002(2) -0.007(3) C17 0.043(4) 0.040(4) 0.026(3) -0.002(2) 0.006(2) -0.010(3) C18 0.046(4) 0.027(3) 0.027(3) -0.003(2) 0.011(2) -0.007(3) C19 0.037(3) 0.024(3) 0.023(3) 0.003(2) 0.009(2) 0.001(2) C20 0.025(3) 0.060(4) 0.020(3) -0.002(3) -0.003(2) -0.004(3) C21 0.030(3) 0.051(4) 0.056(4) 0.035(3) 0.008(3) 0.011(3) C22 0.018(2) 0.025(3) 0.025(3) 0.003(2) 0.0050(19) 0.0031(19) C23 0.023(3) 0.026(3) 0.021(2) -0.0008(19) 0.0028(19) 0.000(2) C24 0.023(3) 0.036(3) 0.025(3) 0.005(2) 0.009(2) 0.004(2) C25 0.030(3) 0.032(3) 0.032(3) 0.009(2) 0.012(2) 0.001(2) C26 0.030(3) 0.029(3) 0.026(3) 0.000(2) 0.007(2) 0.000(2) C27 0.021(2) 0.026(3) 0.020(2) 0.0008(19) 0.0014(19) 0.002(2) C28 0.024(3) 0.034(3) 0.032(3) -0.009(2) 0.013(2) -0.004(2) C29 0.032(3) 0.030(3) 0.068(5) -0.007(3) 0.015(3) 0.005(3) C30 0.036(3) 0.063(5) 0.028(3) -0.014(3) 0.004(3) -0.001(3) C31 0.045(4) 0.039(4) 0.051(4) 0.012(3) 0.028(3) 0.004(3) C32 0.048(4) 0.039(4) 0.074(5) -0.004(3) 0.029(4) -0.017(3) C33 0.077(6) 0.069(6) 0.089(7) 0.049(5) 0.040(5) 0.020(5) C34 0.026(3) 0.029(3) 0.021(2) 0.001(2) 0.006(2) -0.001(2) C35 0.035(3) 0.052(4) 0.018(3) -0.003(2) 0.001(2) 0.008(3) C36 0.046(4) 0.034(3) 0.026(3) -0.004(2) 0.008(2) 0.008(3) C37 0.027(3) 0.022(3) 0.024(3) 0.003(2) 0.007(2) -0.004(2) C38 0.029(3) 0.029(3) 0.018(2) 0.004(2) 0.003(2) -0.004(2) C39 0.027(3) 0.028(3) 0.022(3) 0.008(2) 0.008(2) 0.000(2) C40 0.031(3) 0.020(3) 0.025(3) 0.0049(19) 0.004(2) -0.004(2) C41 0.029(3) 0.021(3) 0.021(2) 0.0018(19) 0.003(2) -0.001(2) C42 0.054(4) 0.061(4) 0.019(3) 0.014(3) 0.006(3) -0.017(3) C43 0.039(3) 0.037(3) 0.035(3) 0.019(3) 0.015(3) 0.006(3) C44 0.069(5) 0.037(4) 0.080(6) 0.012(4) 0.023(5) 0.008(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 N2 2.150(4) . ? Ir1 P1 2.2199(13) . ? Ir1 Si1 2.3207(15) . ? Ir1 N1 2.353(5) . ? Ir1 Cl1 2.4846(13) . ? Ir1 H1 1.55(6) . ? Cl2 C44 1.774(9) . ? Cl3 C44 1.743(9) . ? P1 C1 1.834(5) . ? P1 C8 1.848(5) . ? P1 C14 1.870(5) . ? Si1 C22 1.921(5) . ? N1 C2 1.476(7) . ? N1 C21 1.481(7) . ? N1 C20 1.500(7) . ? N2 C41 1.346(7) . ? N2 C37 1.358(7) . ? N3 C39 1.357(7) . ? N3 C43 1.448(8) . ? N3 C42 1.450(8) . ? C1 C2 1.395(7) . ? C1 C6 1.404(7) . ? C2 C3 1.392(7) . ? C3 C4 1.384(8) . ? C3 H2 0.9500 . ? C4 C5 1.389(8) . ? C4 H3 0.9500 . ? C5 C6 1.388(7) . ? C5 C7 1.500(8) . ? C6 H4 0.9500 . ? C7 H5 0.9800 . ? C7 H6 0.9800 . ? C7 H7 0.9800 . ? C8 C13 1.546(7) . ? C8 C9 1.547(7) . ? C8 H8 1.0000 . ? C9 C10 1.534(7) . ? C9 H9 0.9900 . ? C9 H10 0.9900 . ? C10 C11 1.524(10) . ? C10 H11 0.9900 . ? C10 H12 0.9900 . ? C11 C12 1.523(10) . ? C11 H13 0.9900 . ? C11 H14 0.9900 . ? C12 C13 1.536(8) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 H17 0.9900 . ? C13 H18 0.9900 . ? C14 C19 1.529(7) . ? C14 C15 1.540(7) . ? C14 H19 1.0000 . ? C15 C16 1.528(8) . ? C15 H20 0.9900 . ? C15 H21 0.9900 . ? C16 C17 1.515(9) . ? C16 H22 0.9900 . ? C16 H23 0.9900 . ? C17 C18 1.521(9) . ? C17 H24 0.9900 . ? C17 H25 0.9900 . ? C18 C19 1.525(8) . ? C18 H26 0.9900 . ? C18 H27 0.9900 . ? C19 H28 0.9900 . ? C19 H29 0.9900 . ? C20 H30 0.9800 . ? C20 H31 0.9800 . ? C20 H32 0.9800 . ? C21 H33 0.9800 . ? C21 H34 0.9800 . ? C21 H35 0.9800 . ? C22 C23 1.411(7) . ? C22 C27 1.421(7) . ? C23 C24 1.388(8) . ? C23 C28 1.531(7) . ? C24 C25 1.388(8) . ? C24 H36 0.9500 . ? C25 C26 1.385(8) . ? C25 C31 1.531(8) . ? C26 C27 1.398(8) . ? C26 H37 0.9500 . ? C27 C34 1.527(7) . ? C28 C29 1.523(9) . ? C28 C30 1.531(9) . ? C28 H38 1.0000 . ? C29 H39 0.9800 . ? C29 H40 0.9800 . ? C29 H41 0.9800 . ? C30 H42 0.9800 . ? C30 H43 0.9800 . ? C30 H44 0.9800 . ? C31 C33 1.518(11) . ? C31 C32 1.536(11) . ? C31 H45 1.0000 . ? C32 H46 0.9800 . ? C32 H47 0.9800 . ? C32 H48 0.9800 . ? C33 H49 0.9800 . ? C33 H50 0.9800 . ? C33 H51 0.9800 . ? C34 C36 1.529(8) . ? C34 C35 1.543(8) . ? C34 H52 1.0000 . ? C35 H53 0.9800 . ? C35 H54 0.9800 . ? C35 H55 0.9800 . ? C36 H56 0.9800 . ? C36 H57 0.9800 . ? C36 H58 0.9800 . ? C37 C38 1.374(7) . ? C37 H59 0.9500 . ? C38 C39 1.404(8) . ? C38 H60 0.9500 . ? C39 C40 1.411(7) . ? C40 C41 1.372(7) . ? C40 H61 0.9500 . ? C41 H62 0.9500 . ? C42 H63 0.9800 . ? C42 H64 0.9800 . ? C42 H65 0.9800 . ? C43 H66 0.9800 . ? C43 H67 0.9800 . ? C43 H68 0.9800 . ? C44 H69 0.9900 . ? C44 H70 0.9900 . ? C45 C46 1.367(13) . ? C46 C47 1.359(15) . ? C47 C48 1.514(18) . ? C48 C49 1.495(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 N2 Ir1 P1 168.70(12) . . ? N2 Ir1 Si1 90.39(12) . . ? P1 Ir1 Si1 96.85(5) . . ? N2 Ir1 N1 88.70(16) . . ? P1 Ir1 N1 83.39(11) . . ? Si1 Ir1 N1 175.35(12) . . ? N2 Ir1 Cl1 89.45(12) . . ? P1 Ir1 Cl1 99.11(5) . . ? Si1 Ir1 Cl1 90.58(5) . . ? N1 Ir1 Cl1 93.97(12) . . ? N2 Ir1 H1 89(2) . . ? P1 Ir1 H1 84(2) . . ? Si1 Ir1 H1 82(2) . . ? N1 Ir1 H1 93(2) . . ? Cl1 Ir1 H1 173(2) . . ? C1 P1 C8 101.7(2) . . ? C1 P1 C14 106.0(2) . . ? C8 P1 C14 104.2(2) . . ? C1 P1 Ir1 104.63(16) . . ? C8 P1 Ir1 123.13(18) . . ? C14 P1 Ir1 115.26(17) . . ? C22 Si1 Ir1 115.46(17) . . ? C2 N1 C21 109.5(5) . . ? C2 N1 C20 108.3(4) . . ? C21 N1 C20 108.5(5) . . ? C2 N1 Ir1 111.9(3) . . ? C21 N1 Ir1 107.6(3) . . ? C20 N1 Ir1 111.0(4) . . ? C41 N2 C37 115.6(4) . . ? C41 N2 Ir1 120.0(3) . . ? C37 N2 Ir1 123.8(3) . . ? C39 N3 C43 119.8(5) . . ? C39 N3 C42 120.1(5) . . ? C43 N3 C42 118.8(5) . . ? C2 C1 C6 118.0(5) . . ? C2 C1 P1 118.9(4) . . ? C6 C1 P1 123.0(4) . . ? C3 C2 C1 119.8(5) . . ? C3 C2 N1 119.8(5) . . ? C1 C2 N1 120.3(4) . . ? C4 C3 C2 120.9(5) . . ? C4 C3 H2 119.6 . . ? C2 C3 H2 119.6 . . ? C3 C4 C5 120.8(5) . . ? C3 C4 H3 119.6 . . ? C5 C4 H3 119.6 . . ? C6 C5 C4 117.8(5) . . ? C6 C5 C7 122.0(5) . . ? C4 C5 C7 120.2(5) . . ? C5 C6 C1 122.7(5) . . ? C5 C6 H4 118.7 . . ? C1 C6 H4 118.7 . . ? C5 C7 H5 109.5 . . ? C5 C7 H6 109.5 . . ? H5 C7 H6 109.5 . . ? C5 C7 H7 109.5 . . ? H5 C7 H7 109.5 . . ? H6 C7 H7 109.5 . . ? C13 C8 C9 110.1(5) . . ? C13 C8 P1 110.9(4) . . ? C9 C8 P1 113.8(3) . . ? C13 C8 H8 107.2 . . ? C9 C8 H8 107.2 . . ? P1 C8 H8 107.2 . . ? C10 C9 C8 109.6(4) . . ? C10 C9 H9 109.8 . . ? C8 C9 H9 109.8 . . ? C10 C9 H10 109.8 . . ? C8 C9 H10 109.8 . . ? H9 C9 H10 108.2 . . ? C11 C10 C9 111.5(5) . . ? C11 C10 H11 109.3 . . ? C9 C10 H11 109.3 . . ? C11 C10 H12 109.3 . . ? C9 C10 H12 109.3 . . ? H11 C10 H12 108.0 . . ? C12 C11 C10 110.8(5) . . ? C12 C11 H13 109.5 . . ? C10 C11 H13 109.5 . . ? C12 C11 H14 109.5 . . ? C10 C11 H14 109.5 . . ? H13 C11 H14 108.1 . . ? C11 C12 C13 111.8(5) . . ? C11 C12 H15 109.2 . . ? C13 C12 H15 109.2 . . ? C11 C12 H16 109.2 . . ? C13 C12 H16 109.2 . . ? H15 C12 H16 107.9 . . ? C12 C13 C8 109.0(5) . . ? C12 C13 H17 109.9 . . ? C8 C13 H17 109.9 . . ? C12 C13 H18 109.9 . . ? C8 C13 H18 109.9 . . ? H17 C13 H18 108.3 . . ? C19 C14 C15 109.5(4) . . ? C19 C14 P1 111.4(4) . . ? C15 C14 P1 118.0(4) . . ? C19 C14 H19 105.6 . . ? C15 C14 H19 105.6 . . ? P1 C14 H19 105.6 . . ? C16 C15 C14 110.9(5) . . ? C16 C15 H20 109.5 . . ? C14 C15 H20 109.5 . . ? C16 C15 H21 109.5 . . ? C14 C15 H21 109.5 . . ? H20 C15 H21 108.0 . . ? C17 C16 C15 112.1(5) . . ? C17 C16 H22 109.2 . . ? C15 C16 H22 109.2 . . ? C17 C16 H23 109.2 . . ? C15 C16 H23 109.2 . . ? H22 C16 H23 107.9 . . ? C16 C17 C18 110.3(5) . . ? C16 C17 H24 109.6 . . ? C18 C17 H24 109.6 . . ? C16 C17 H25 109.6 . . ? C18 C17 H25 109.6 . . ? H24 C17 H25 108.1 . . ? C17 C18 C19 112.1(5) . . ? C17 C18 H26 109.2 . . ? C19 C18 H26 109.2 . . ? C17 C18 H27 109.2 . . ? C19 C18 H27 109.2 . . ? H26 C18 H27 107.9 . . ? C18 C19 C14 111.4(5) . . ? C18 C19 H28 109.4 . . ? C14 C19 H28 109.4 . . ? C18 C19 H29 109.4 . . ? C14 C19 H29 109.4 . . ? H28 C19 H29 108.0 . . ? N1 C20 H30 109.5 . . ? N1 C20 H31 109.5 . . ? H30 C20 H31 109.5 . . ? N1 C20 H32 109.5 . . ? H30 C20 H32 109.5 . . ? H31 C20 H32 109.5 . . ? N1 C21 H33 109.5 . . ? N1 C21 H34 109.5 . . ? H33 C21 H34 109.5 . . ? N1 C21 H35 109.5 . . ? H33 C21 H35 109.5 . . ? H34 C21 H35 109.5 . . ? C23 C22 C27 117.2(5) . . ? C23 C22 Si1 122.2(4) . . ? C27 C22 Si1 120.6(4) . . ? C24 C23 C22 120.5(5) . . ? C24 C23 C28 116.9(5) . . ? C22 C23 C28 122.6(5) . . ? C23 C24 C25 122.3(5) . . ? C23 C24 H36 118.8 . . ? C25 C24 H36 118.8 . . ? C26 C25 C24 117.5(5) . . ? C26 C25 C31 121.7(5) . . ? C24 C25 C31 120.9(5) . . ? C25 C26 C27 122.1(5) . . ? C25 C26 H37 119.0 . . ? C27 C26 H37 119.0 . . ? C26 C27 C22 120.1(5) . . ? C26 C27 C34 117.9(5) . . ? C22 C27 C34 122.0(5) . . ? C29 C28 C30 110.1(5) . . ? C29 C28 C23 110.2(5) . . ? C30 C28 C23 113.1(6) . . ? C29 C28 H38 107.8 . . ? C30 C28 H38 107.8 . . ? C23 C28 H38 107.8 . . ? C28 C29 H39 109.5 . . ? C28 C29 H40 109.5 . . ? H39 C29 H40 109.5 . . ? C28 C29 H41 109.5 . . ? H39 C29 H41 109.5 . . ? H40 C29 H41 109.5 . . ? C28 C30 H42 109.5 . . ? C28 C30 H43 109.5 . . ? H42 C30 H43 109.5 . . ? C28 C30 H44 109.5 . . ? H42 C30 H44 109.5 . . ? H43 C30 H44 109.5 . . ? C33 C31 C25 110.5(6) . . ? C33 C31 C32 112.5(7) . . ? C25 C31 C32 111.8(6) . . ? C33 C31 H45 107.2 . . ? C25 C31 H45 107.2 . . ? C32 C31 H45 107.2 . . ? C31 C32 H46 109.5 . . ? C31 C32 H47 109.5 . . ? H46 C32 H47 109.5 . . ? C31 C32 H48 109.5 . . ? H46 C32 H48 109.5 . . ? H47 C32 H48 109.5 . . ? C31 C33 H49 109.5 . . ? C31 C33 H50 109.5 . . ? H49 C33 H50 109.5 . . ? C31 C33 H51 109.5 . . ? H49 C33 H51 109.5 . . ? H50 C33 H51 109.5 . . ? C27 C34 C36 112.5(5) . . ? C27 C34 C35 110.2(4) . . ? C36 C34 C35 110.1(5) . . ? C27 C34 H52 108.0 . . ? C36 C34 H52 108.0 . . ? C35 C34 H52 108.0 . . ? C34 C35 H53 109.5 . . ? C34 C35 H54 109.5 . . ? H53 C35 H54 109.5 . . ? C34 C35 H55 109.5 . . ? H53 C35 H55 109.5 . . ? H54 C35 H55 109.5 . . ? C34 C36 H56 109.5 . . ? C34 C36 H57 109.5 . . ? H56 C36 H57 109.5 . . ? C34 C36 H58 109.5 . . ? H56 C36 H58 109.5 . . ? H57 C36 H58 109.5 . . ? N2 C37 C38 124.1(5) . . ? N2 C37 H59 118.0 . . ? C38 C37 H59 118.0 . . ? C37 C38 C39 119.9(5) . . ? C37 C38 H60 120.0 . . ? C39 C38 H60 120.0 . . ? N3 C39 C38 122.3(5) . . ? N3 C39 C40 121.5(5) . . ? C38 C39 C40 116.2(5) . . ? C41 C40 C39 119.7(5) . . ? C41 C40 H61 120.2 . . ? C39 C40 H61 120.2 . . ? N2 C41 C40 124.6(5) . . ? N2 C41 H62 117.7 . . ? C40 C41 H62 117.7 . . ? N3 C42 H63 109.5 . . ? N3 C42 H64 109.5 . . ? H63 C42 H64 109.5 . . ? N3 C42 H65 109.5 . . ? H63 C42 H65 109.5 . . ? H64 C42 H65 109.5 . . ? N3 C43 H66 109.5 . . ? N3 C43 H67 109.5 . . ? H66 C43 H67 109.5 . . ? N3 C43 H68 109.5 . . ? H66 C43 H68 109.5 . . ? H67 C43 H68 109.5 . . ? Cl3 C44 Cl2 112.5(5) . . ? Cl3 C44 H69 109.1 . . ? Cl2 C44 H69 109.1 . . ? Cl3 C44 H70 109.1 . . ? Cl2 C44 H70 109.1 . . ? H69 C44 H70 107.8 . . ? C47 C46 C45 127.7(14) . . ? C46 C47 C48 78.1(14) . . ? C49 C48 C47 82.0(15) . . ? 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 N2 Ir1 P1 C1 38.6(6) . . . . ? Si1 Ir1 P1 C1 168.06(17) . . . . ? N1 Ir1 P1 C1 -7.3(2) . . . . ? Cl1 Ir1 P1 C1 -100.25(17) . . . . ? N2 Ir1 P1 C8 153.4(6) . . . . ? Si1 Ir1 P1 C8 -77.1(2) . . . . ? N1 Ir1 P1 C8 107.6(2) . . . . ? Cl1 Ir1 P1 C8 14.6(2) . . . . ? N2 Ir1 P1 C14 -77.3(6) . . . . ? Si1 Ir1 P1 C14 52.1(2) . . . . ? N1 Ir1 P1 C14 -123.2(2) . . . . ? Cl1 Ir1 P1 C14 143.81(19) . . . . ? N2 Ir1 Si1 C22 26.4(2) . . . . ? P1 Ir1 Si1 C22 -144.88(18) . . . . ? N1 Ir1 Si1 C22 -52.2(14) . . . . ? Cl1 Ir1 Si1 C22 115.87(18) . . . . ? N2 Ir1 N1 C2 -163.3(4) . . . . ? P1 Ir1 N1 C2 8.6(3) . . . . ? Si1 Ir1 N1 C2 -84.6(14) . . . . ? Cl1 Ir1 N1 C2 107.4(3) . . . . ? N2 Ir1 N1 C21 -42.9(4) . . . . ? P1 Ir1 N1 C21 129.0(4) . . . . ? Si1 Ir1 N1 C21 35.8(16) . . . . ? Cl1 Ir1 N1 C21 -132.3(4) . . . . ? N2 Ir1 N1 C20 75.6(4) . . . . ? P1 Ir1 N1 C20 -112.5(4) . . . . ? Si1 Ir1 N1 C20 154.3(12) . . . . ? Cl1 Ir1 N1 C20 -13.8(4) . . . . ? P1 Ir1 N2 C41 54.5(8) . . . . ? Si1 Ir1 N2 C41 -75.5(4) . . . . ? N1 Ir1 N2 C41 100.0(4) . . . . ? Cl1 Ir1 N2 C41 -166.1(4) . . . . ? P1 Ir1 N2 C37 -116.0(6) . . . . ? Si1 Ir1 N2 C37 114.0(4) . . . . ? N1 Ir1 N2 C37 -70.5(4) . . . . ? Cl1 Ir1 N2 C37 23.4(4) . . . . ? C8 P1 C1 C2 -122.5(4) . . . . ? C14 P1 C1 C2 128.9(4) . . . . ? Ir1 P1 C1 C2 6.6(4) . . . . ? C8 P1 C1 C6 54.2(5) . . . . ? C14 P1 C1 C6 -54.4(5) . . . . ? Ir1 P1 C1 C6 -176.7(4) . . . . ? C6 C1 C2 C3 0.8(8) . . . . ? P1 C1 C2 C3 177.7(4) . . . . ? C6 C1 C2 N1 -176.5(5) . . . . ? P1 C1 C2 N1 0.4(7) . . . . ? C21 N1 C2 C3 56.4(7) . . . . ? C20 N1 C2 C3 -61.7(7) . . . . ? Ir1 N1 C2 C3 175.6(4) . . . . ? C21 N1 C2 C1 -126.3(6) . . . . ? C20 N1 C2 C1 115.6(5) . . . . ? Ir1 N1 C2 C1 -7.0(6) . . . . ? C1 C2 C3 C4 -0.1(8) . . . . ? N1 C2 C3 C4 177.3(5) . . . . ? C2 C3 C4 C5 -0.7(9) . . . . ? C3 C4 C5 C6 0.6(8) . . . . ? C3 C4 C5 C7 -180.0(6) . . . . ? C4 C5 C6 C1 0.2(8) . . . . ? C7 C5 C6 C1 -179.2(5) . . . . ? C2 C1 C6 C5 -0.9(8) . . . . ? P1 C1 C6 C5 -177.6(4) . . . . ? C1 P1 C8 C13 175.5(4) . . . . ? C14 P1 C8 C13 -74.5(4) . . . . ? Ir1 P1 C8 C13 59.2(4) . . . . ? C1 P1 C8 C9 50.7(4) . . . . ? C14 P1 C8 C9 160.7(4) . . . . ? Ir1 P1 C8 C9 -65.6(4) . . . . ? C13 C8 C9 C10 59.0(6) . . . . ? P1 C8 C9 C10 -175.8(4) . . . . ? C8 C9 C10 C11 -57.3(7) . . . . ? C9 C10 C11 C12 55.9(7) . . . . ? C10 C11 C12 C13 -56.3(7) . . . . ? C11 C12 C13 C8 57.7(7) . . . . ? C9 C8 C13 C12 -58.8(6) . . . . ? P1 C8 C13 C12 174.3(4) . . . . ? C1 P1 C14 C19 -45.9(4) . . . . ? C8 P1 C14 C19 -152.7(4) . . . . ? Ir1 P1 C14 C19 69.3(4) . . . . ? C1 P1 C14 C15 82.1(5) . . . . ? C8 P1 C14 C15 -24.8(5) . . . . ? Ir1 P1 C14 C15 -162.7(4) . . . . ? C19 C14 C15 C16 -56.4(6) . . . . ? P1 C14 C15 C16 174.8(4) . . . . ? C14 C15 C16 C17 56.8(7) . . . . ? C15 C16 C17 C18 -55.0(7) . . . . ? C16 C17 C18 C19 54.6(7) . . . . ? C17 C18 C19 C14 -56.3(7) . . . . ? C15 C14 C19 C18 56.2(6) . . . . ? P1 C14 C19 C18 -171.3(4) . . . . ? Ir1 Si1 C22 C23 -93.6(4) . . . . ? Ir1 Si1 C22 C27 85.8(4) . . . . ? C27 C22 C23 C24 5.5(8) . . . . ? Si1 C22 C23 C24 -175.1(4) . . . . ? C27 C22 C23 C28 -174.8(5) . . . . ? Si1 C22 C23 C28 4.6(7) . . . . ? C22 C23 C24 C25 -1.6(9) . . . . ? C28 C23 C24 C25 178.6(5) . . . . ? C23 C24 C25 C26 -2.6(9) . . . . ? C23 C24 C25 C31 179.4(6) . . . . ? C24 C25 C26 C27 2.9(9) . . . . ? C31 C25 C26 C27 -179.1(6) . . . . ? C25 C26 C27 C22 1.0(9) . . . . ? C25 C26 C27 C34 -179.1(5) . . . . ? C23 C22 C27 C26 -5.2(8) . . . . ? Si1 C22 C27 C26 175.4(4) . . . . ? C23 C22 C27 C34 174.9(5) . . . . ? Si1 C22 C27 C34 -4.5(7) . . . . ? C24 C23 C28 C29 80.3(7) . . . . ? C22 C23 C28 C29 -99.4(6) . . . . ? C24 C23 C28 C30 -43.4(7) . . . . ? C22 C23 C28 C30 136.9(6) . . . . ? C26 C25 C31 C33 -82.1(8) . . . . ? C24 C25 C31 C33 95.8(8) . . . . ? C26 C25 C31 C32 44.0(9) . . . . ? C24 C25 C31 C32 -138.1(6) . . . . ? C26 C27 C34 C36 53.9(7) . . . . ? C22 C27 C34 C36 -126.2(6) . . . . ? C26 C27 C34 C35 -69.4(7) . . . . ? C22 C27 C34 C35 110.5(6) . . . . ? C41 N2 C37 C38 -2.0(8) . . . . ? Ir1 N2 C37 C38 168.9(4) . . . . ? N2 C37 C38 C39 0.9(9) . . . . ? C43 N3 C39 C38 -172.3(5) . . . . ? C42 N3 C39 C38 -5.0(9) . . . . ? C43 N3 C39 C40 7.8(8) . . . . ? C42 N3 C39 C40 175.0(6) . . . . ? C37 C38 C39 N3 -179.1(5) . . . . ? C37 C38 C39 C40 0.9(8) . . . . ? N3 C39 C40 C41 178.5(5) . . . . ? C38 C39 C40 C41 -1.4(8) . . . . ? C37 N2 C41 C40 1.5(8) . . . . ? Ir1 N2 C41 C40 -169.8(4) . . . . ? C39 C40 C41 N2 0.2(9) . . . . ? C45 C46 C47 C48 -173.1(19) . . . . ? C46 C47 C48 C49 169.7(18) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.204 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.235