# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kenneth Caulton' _publ_contact_author_email CAULTON@INDIANA.EDU _publ_section_title ; Surprising Isomer Preference on IrIII, Favoring Facile H-C(sp3) Bond Cleavage ; loop_ _publ_author_name 'Kenneth Caulton' 'Hongjun Fan.' 'Matthew F. Laird' 'Maren Pink' 'Nikolai P. Tsvetkov' # Attachment '07139_CCDC_730042.cif' data_07139 _database_code_depnum_ccdc_archive 'CCDC 730042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H52 I2 Ir N P2 Si2' _chemical_formula_sum 'C22 H52 I2 Ir N P2 Si2' _chemical_formula_weight 894.77 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 16.4974(9) _cell_length_b 12.9874(7) _cell_length_c 30.8640(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.0520(10) _cell_angle_gamma 90.00 _cell_volume 6386.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 6.302 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.4516 _exptl_absorpt_correction_T_max 0.5185 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 15 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81937 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.51 _reflns_number_total 14579 _reflns_number_gt 11532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2003)' _computing_publication_material 'SHELXTL (Bruker, 2003)' _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^)+(0.0233P)^2^+42.8246P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14579 _refine_ls_number_parameters 571 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0522 _refine_ls_R_factor_gt 0.0363 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1A Ir 0.858049(12) 0.904285(16) 0.133620(7) 0.02115(5) Uani 1 1 d . . . I1A I 0.90804(3) 0.77887(4) 0.070399(16) 0.04877(12) Uani 1 1 d . . . I2A I 1.01021(2) 0.90681(3) 0.190577(14) 0.03691(10) Uani 1 1 d . . . P1A P 0.88684(10) 1.06801(12) 0.10225(5) 0.0315(3) Uani 1 1 d . . . P2A P 0.81065(8) 0.76564(11) 0.16776(5) 0.0221(3) Uani 1 1 d . . . Si1A Si 0.71910(11) 0.99061(14) 0.03663(6) 0.0389(4) Uani 1 1 d . . . Si2A Si 0.65175(9) 0.83084(13) 0.09341(6) 0.0289(3) Uani 1 1 d . . . N1A N 0.7372(3) 0.9002(4) 0.08149(18) 0.0385(12) Uani 1 1 d . . . H1NA H 0.7531 0.8471 0.0652 0.046 Uiso 1 1 calc R . . C1A C 0.6208(5) 1.0649(6) 0.0319(3) 0.069(3) Uani 1 1 d . . . H1A H 0.6181 1.0876 0.0618 0.103 Uiso 1 1 calc R . . H1B H 0.5723 1.0211 0.0187 0.103 Uiso 1 1 calc R . . H1C H 0.6202 1.1251 0.0126 0.103 Uiso 1 1 calc R . . C2A C 0.7078(6) 0.9187(7) -0.0173(3) 0.072(3) Uani 1 1 d . . . H2A H 0.7532 0.8683 -0.0137 0.109 Uiso 1 1 calc R . . H2B H 0.7105 0.9673 -0.0412 0.109 Uiso 1 1 calc R . . H2C H 0.6536 0.8830 -0.0253 0.109 Uiso 1 1 calc R . . C3A C 0.8167(4) 1.0686(5) 0.0455(2) 0.0396(15) Uani 1 1 d . . . H3A H 0.8487 1.0434 0.0245 0.048 Uiso 1 1 calc R . . H3B H 0.8005 1.1408 0.0372 0.048 Uiso 1 1 calc R . . C4A C 0.8549(5) 1.1861(5) 0.1289(3) 0.0518(19) Uani 1 1 d . . . C5A C 0.9032(6) 1.1933(6) 0.1789(2) 0.058(2) Uani 1 1 d . . . H5A H 0.8750 1.2426 0.1942 0.087 Uiso 1 1 calc R . . H5B H 0.9608 1.2164 0.1814 0.087 Uiso 1 1 calc R . . H5C H 0.9044 1.1254 0.1930 0.087 Uiso 1 1 calc R . . C6A C 0.8662(7) 1.2892(6) 0.1056(3) 0.075(3) Uani 1 1 d . . . H6A H 0.8383 1.3447 0.1177 0.113 Uiso 1 1 calc R . . H6B H 0.8413 1.2832 0.0732 0.113 Uiso 1 1 calc R . . H6C H 0.9262 1.3048 0.1112 0.113 Uiso 1 1 calc R . . C7A C 0.7609(5) 1.1777(6) 0.1248(3) 0.063(2) Uani 1 1 d . . . H7A H 0.7446 1.2297 0.1440 0.095 Uiso 1 1 calc R . . H7B H 0.7482 1.1089 0.1344 0.095 Uiso 1 1 calc R . . H7C H 0.7296 1.1891 0.0936 0.095 Uiso 1 1 calc R . . C8A C 0.9934(5) 1.0994(6) 0.0907(3) 0.056(2) Uani 1 1 d . . . C9A C 1.0319(5) 0.9985(7) 0.0776(3) 0.066(2) Uani 1 1 d . . . H9A H 1.0860 1.0139 0.0714 0.098 Uiso 1 1 calc R . . H9B H 0.9937 0.9690 0.0507 0.098 Uiso 1 1 calc R . . H9C H 1.0403 0.9491 0.1023 0.098 Uiso 1 1 calc R . . C10A C 0.9843(5) 1.1718(7) 0.0507(3) 0.071(3) Uani 1 1 d . . . H10A H 1.0397 1.1848 0.0457 0.106 Uiso 1 1 calc R . . H10B H 0.9597 1.2371 0.0570 0.106 Uiso 1 1 calc R . . H10C H 0.9477 1.1401 0.0239 0.106 Uiso 1 1 calc R . . C11A C 1.0569(5) 1.1450(7) 0.1311(3) 0.070(3) Uani 1 1 d . . . H11A H 1.1115 1.1513 0.1243 0.105 Uiso 1 1 calc R . . H11B H 1.0622 1.0998 0.1571 0.105 Uiso 1 1 calc R . . H11C H 1.0378 1.2132 0.1378 0.105 Uiso 1 1 calc R . . C12A C 0.5960(4) 0.7653(5) 0.0404(2) 0.0437(16) Uani 1 1 d . . . H12A H 0.5685 0.8169 0.0183 0.066 Uiso 1 1 calc R . . H12B H 0.5537 0.7183 0.0464 0.066 Uiso 1 1 calc R . . H12C H 0.6364 0.7262 0.0287 0.066 Uiso 1 1 calc R . . C13A C 0.5772(4) 0.9124(6) 0.1137(3) 0.054(2) Uani 1 1 d . . . H13A H 0.6085 0.9625 0.1354 0.081 Uiso 1 1 calc R . . H13B H 0.5433 0.8690 0.1282 0.081 Uiso 1 1 calc R . . H13C H 0.5404 0.9488 0.0883 0.081 Uiso 1 1 calc R . . C14A C 0.7065(3) 0.7301(4) 0.13349(19) 0.0277(12) Uani 1 1 d . . . H14A H 0.6708 0.7125 0.1537 0.033 Uiso 1 1 calc R . . H14B H 0.7119 0.6674 0.1162 0.033 Uiso 1 1 calc R . . C15A C 0.7952(4) 0.8503(5) 0.2130(2) 0.0383(14) Uani 1 1 d . . . C16A C 0.7087(4) 0.8433(6) 0.2228(2) 0.0447(16) Uani 1 1 d . . . H16A H 0.7017 0.9012 0.2419 0.067 Uiso 1 1 calc R . . H16B H 0.7045 0.7784 0.2382 0.067 Uiso 1 1 calc R . . H16C H 0.6648 0.8460 0.1945 0.067 Uiso 1 1 calc R . . C17A C 0.8627(4) 0.8463(6) 0.2574(2) 0.0439(16) Uani 1 1 d . . . H17A H 0.8547 0.9035 0.2765 0.066 Uiso 1 1 calc R . . H17B H 0.9182 0.8518 0.2516 0.066 Uiso 1 1 calc R . . H17C H 0.8586 0.7809 0.2725 0.066 Uiso 1 1 calc R . . C18A C 0.8053(4) 0.9507(5) 0.1862(2) 0.0367(14) Uani 1 1 d . . . H18A H 0.8426 1.0005 0.2061 0.044 Uiso 1 1 calc R . . H18B H 0.7500 0.9837 0.1739 0.044 Uiso 1 1 calc R . . C19A C 0.8587(4) 0.6358(5) 0.1866(2) 0.0358(14) Uani 1 1 d . . . C20A C 0.8112(5) 0.5890(6) 0.2200(3) 0.055(2) Uani 1 1 d . . . H20A H 0.8343 0.5209 0.2298 0.083 Uiso 1 1 calc R . . H20B H 0.7513 0.5827 0.2049 0.083 Uiso 1 1 calc R . . H20C H 0.8184 0.6344 0.2461 0.083 Uiso 1 1 calc R . . C21A C 0.9515(4) 0.6451(5) 0.2113(3) 0.0454(17) Uani 1 1 d . . . H21A H 0.9734 0.5772 0.2224 0.068 Uiso 1 1 calc R . . H21B H 0.9579 0.6926 0.2366 0.068 Uiso 1 1 calc R . . H21C H 0.9829 0.6714 0.1907 0.068 Uiso 1 1 calc R . . C22A C 0.8482(5) 0.5632(5) 0.1472(3) 0.0500(18) Uani 1 1 d . . . H22A H 0.8801 0.5000 0.1571 0.075 Uiso 1 1 calc R . . H22B H 0.8692 0.5963 0.1237 0.075 Uiso 1 1 calc R . . H22C H 0.7887 0.5464 0.1354 0.075 Uiso 1 1 calc R . . Ir1B Ir 0.356473(11) 0.593692(16) 0.130584(7) 0.02060(5) Uani 1 1 d . . . I1B I 0.37520(3) 0.70207(4) 0.052914(16) 0.04504(11) Uani 1 1 d . . . I2B I 0.50435(2) 0.64796(3) 0.184863(14) 0.03657(10) Uani 1 1 d . . . P1B P 0.41756(8) 0.43141(11) 0.11496(5) 0.0267(3) Uani 1 1 d . . . P2B P 0.28298(8) 0.72811(11) 0.15297(5) 0.0244(3) Uani 1 1 d . . . Si1B Si 0.24040(10) 0.44059(13) 0.04562(5) 0.0292(3) Uani 1 1 d . . . Si2B Si 0.14261(9) 0.60160(14) 0.08757(6) 0.0316(4) Uani 1 1 d . . . N1B N 0.2388(3) 0.5491(4) 0.08121(19) 0.0385(13) Uani 1 1 d . . . H1NB H 0.2445 0.5974 0.0600 0.046 Uiso 1 1 calc R . . C1B C 0.1611(4) 0.3436(5) 0.0511(2) 0.0403(15) Uani 1 1 d . . . H1D H 0.1050 0.3681 0.0354 0.060 Uiso 1 1 calc R . . H1E H 0.1640 0.3332 0.0829 0.060 Uiso 1 1 calc R . . H1F H 0.1725 0.2783 0.0379 0.060 Uiso 1 1 calc R . . C2B C 0.2169(4) 0.4821(6) -0.0142(2) 0.0452(16) Uani 1 1 d . . . H2D H 0.1579 0.5028 -0.0245 0.068 Uiso 1 1 calc R . . H2E H 0.2276 0.4248 -0.0327 0.068 Uiso 1 1 calc R . . H2F H 0.2530 0.5404 -0.0169 0.068 Uiso 1 1 calc R . . C3B C 0.3503(3) 0.3906(5) 0.06081(19) 0.0290(12) Uani 1 1 d . . . H3C H 0.3480 0.3144 0.0605 0.035 Uiso 1 1 calc R . . H3D H 0.3774 0.4119 0.0371 0.035 Uiso 1 1 calc R . . C4B C 0.4095(4) 0.3199(5) 0.1542(2) 0.0392(15) Uani 1 1 d . . . C5B C 0.4439(5) 0.2152(5) 0.1427(3) 0.0516(18) Uani 1 1 d . . . H5D H 0.4297 0.1612 0.1616 0.077 Uiso 1 1 calc R . . H5E H 0.5051 0.2194 0.1482 0.077 Uiso 1 1 calc R . . H5F H 0.4188 0.1988 0.1111 0.077 Uiso 1 1 calc R . . C6B C 0.3170(4) 0.3004(6) 0.1502(3) 0.0473(17) Uani 1 1 d . . . H6D H 0.3113 0.2528 0.1739 0.071 Uiso 1 1 calc R . . H6E H 0.2907 0.2701 0.1209 0.071 Uiso 1 1 calc R . . H6F H 0.2892 0.3656 0.1534 0.071 Uiso 1 1 calc R . . C7B C 0.4550(4) 0.3485(6) 0.2025(2) 0.0451(16) Uani 1 1 d . . . H7D H 0.4443 0.2956 0.2230 0.068 Uiso 1 1 calc R . . H7E H 0.4344 0.4151 0.2101 0.068 Uiso 1 1 calc R . . H7F H 0.5155 0.3531 0.2054 0.068 Uiso 1 1 calc R . . C8B C 0.5270(4) 0.4204(5) 0.1043(2) 0.0360(14) Uani 1 1 d . . . C9B C 0.5337(4) 0.3305(6) 0.0733(2) 0.0466(17) Uani 1 1 d . . . H9D H 0.5919 0.3242 0.0714 0.070 Uiso 1 1 calc R . . H9E H 0.4968 0.3432 0.0434 0.070 Uiso 1 1 calc R . . H9F H 0.5168 0.2667 0.0855 0.070 Uiso 1 1 calc R . . C10B C 0.5979(4) 0.4091(6) 0.1477(3) 0.0482(18) Uani 1 1 d . . . H10D H 0.6524 0.4144 0.1407 0.072 Uiso 1 1 calc R . . H10E H 0.5934 0.3418 0.1613 0.072 Uiso 1 1 calc R . . H10F H 0.5930 0.4637 0.1688 0.072 Uiso 1 1 calc R . . C11B C 0.5439(4) 0.5194(5) 0.0809(2) 0.0439(16) Uani 1 1 d . . . H11D H 0.5979 0.5136 0.0735 0.066 Uiso 1 1 calc R . . H11E H 0.5454 0.5782 0.1010 0.066 Uiso 1 1 calc R . . H11F H 0.4991 0.5296 0.0534 0.066 Uiso 1 1 calc R . . C12B C 0.0827(5) 0.5129(7) 0.1153(3) 0.062(2) Uani 1 1 d . . . H12D H 0.0507 0.4640 0.0932 0.093 Uiso 1 1 calc R . . H12E H 0.0441 0.5529 0.1281 0.093 Uiso 1 1 calc R . . H12F H 0.1219 0.4750 0.1394 0.093 Uiso 1 1 calc R . . C13B C 0.0781(5) 0.6291(7) 0.0298(3) 0.067(3) Uani 1 1 d . . . H13D H 0.1114 0.6689 0.0136 0.100 Uiso 1 1 calc R . . H13E H 0.0284 0.6687 0.0313 0.100 Uiso 1 1 calc R . . H13F H 0.0606 0.5641 0.0140 0.100 Uiso 1 1 calc R . . C14B C 0.1760(3) 0.7263(5) 0.1171(2) 0.0306(13) Uani 1 1 d . . . H14C H 0.1705 0.7813 0.0943 0.037 Uiso 1 1 calc R . . H14D H 0.1370 0.7429 0.1357 0.037 Uiso 1 1 calc R . . C15B C 0.2800(4) 0.6585(5) 0.2047(2) 0.0363(14) Uani 1 1 d . . . C16B C 0.3451(4) 0.6901(5) 0.2474(2) 0.0406(15) Uani 1 1 d . . . H16D H 0.3435 0.6418 0.2716 0.061 Uiso 1 1 calc R . . H16E H 0.3327 0.7597 0.2561 0.061 Uiso 1 1 calc R . . H16F H 0.4011 0.6890 0.2421 0.061 Uiso 1 1 calc R . . C17B C 0.1948(4) 0.6483(6) 0.2143(2) 0.0458(17) Uani 1 1 d . . . H17D H 0.1980 0.5973 0.2381 0.069 Uiso 1 1 calc R . . H17E H 0.1534 0.6259 0.1870 0.069 Uiso 1 1 calc R . . H17F H 0.1779 0.7150 0.2239 0.069 Uiso 1 1 calc R . . C18B C 0.3097(4) 0.5545(5) 0.1865(2) 0.0363(14) Uani 1 1 d . . . H18C H 0.2621 0.5060 0.1773 0.044 Uiso 1 1 calc R . . H18D H 0.3543 0.5214 0.2102 0.044 Uiso 1 1 calc R . . C19B C 0.3071(4) 0.8705(5) 0.1608(2) 0.0344(14) Uani 1 1 d . . . C20B C 0.3971(4) 0.8905(6) 0.1870(3) 0.056(2) Uani 1 1 d . . . H20D H 0.4069 0.9649 0.1899 0.083 Uiso 1 1 calc R . . H20E H 0.4354 0.8599 0.1711 0.083 Uiso 1 1 calc R . . H20F H 0.4071 0.8597 0.2169 0.083 Uiso 1 1 calc R . . C21B C 0.2472(5) 0.9170(6) 0.1869(3) 0.062(2) Uani 1 1 d . . . H21D H 0.2540 0.9920 0.1885 0.092 Uiso 1 1 calc R . . H21E H 0.2607 0.8884 0.2173 0.092 Uiso 1 1 calc R . . H21F H 0.1890 0.8999 0.1714 0.092 Uiso 1 1 calc R . . C22B C 0.2902(7) 0.9234(6) 0.1160(3) 0.069(2) Uani 1 1 d . . . H22D H 0.3030 0.9969 0.1205 0.104 Uiso 1 1 calc R . . H22E H 0.2310 0.9147 0.1000 0.104 Uiso 1 1 calc R . . H22F H 0.3257 0.8930 0.0983 0.104 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 Ir1A 0.02249(9) 0.02112(11) 0.01992(11) -0.00366(8) 0.00561(8) -0.00279(8) I1A 0.0605(3) 0.0495(3) 0.0429(3) -0.0165(2) 0.0252(2) -0.0002(2) I2A 0.02697(17) 0.0389(2) 0.0391(2) 0.00197(18) -0.00161(16) -0.00530(16) P1A 0.0389(8) 0.0235(8) 0.0292(8) 0.0011(6) 0.0039(6) -0.0100(6) P2A 0.0253(6) 0.0220(7) 0.0189(7) 0.0005(5) 0.0055(5) -0.0004(5) Si1A 0.0453(9) 0.0346(10) 0.0281(9) 0.0093(7) -0.0062(7) -0.0128(8) Si2A 0.0214(7) 0.0321(9) 0.0312(9) 0.0052(7) 0.0034(6) -0.0017(6) N1A 0.033(3) 0.041(3) 0.036(3) 0.012(2) -0.002(2) -0.011(2) C1A 0.050(4) 0.045(5) 0.092(7) 0.035(5) -0.017(4) -0.002(3) C2A 0.106(7) 0.073(6) 0.030(4) -0.005(4) 0.003(4) -0.049(5) C3A 0.055(4) 0.030(3) 0.031(3) 0.005(3) 0.006(3) -0.011(3) C4A 0.072(5) 0.026(3) 0.048(4) -0.008(3) -0.001(4) 0.001(3) C5A 0.089(6) 0.036(4) 0.040(4) -0.010(3) 0.000(4) -0.007(4) C6A 0.119(8) 0.027(4) 0.067(6) 0.000(4) 0.002(5) -0.009(4) C7A 0.083(6) 0.047(5) 0.060(5) 0.005(4) 0.016(4) 0.029(4) C8A 0.048(4) 0.058(5) 0.058(5) 0.020(4) 0.009(4) -0.023(4) C9A 0.047(4) 0.079(6) 0.077(6) 0.018(5) 0.028(4) -0.008(4) C10A 0.065(5) 0.081(6) 0.066(6) 0.028(5) 0.014(4) -0.027(5) C11A 0.055(5) 0.071(6) 0.072(6) 0.018(5) -0.007(4) -0.032(4) C12A 0.038(3) 0.047(4) 0.038(4) 0.008(3) -0.005(3) -0.011(3) C13A 0.044(4) 0.072(5) 0.048(4) 0.018(4) 0.017(3) 0.020(4) C14A 0.027(3) 0.029(3) 0.027(3) 0.002(2) 0.005(2) -0.006(2) C15A 0.043(3) 0.044(4) 0.028(3) -0.007(3) 0.009(3) 0.002(3) C16A 0.047(4) 0.056(4) 0.038(4) -0.006(3) 0.024(3) 0.000(3) C17A 0.060(4) 0.047(4) 0.024(3) -0.002(3) 0.010(3) -0.008(3) C18A 0.043(3) 0.032(3) 0.036(4) -0.008(3) 0.012(3) 0.003(3) C19A 0.040(3) 0.027(3) 0.035(4) 0.002(3) -0.001(3) 0.002(2) C20A 0.061(4) 0.047(4) 0.052(5) 0.022(4) 0.004(4) -0.008(4) C21A 0.039(3) 0.030(3) 0.057(5) 0.008(3) -0.005(3) 0.007(3) C22A 0.056(4) 0.025(3) 0.063(5) -0.004(3) 0.003(4) 0.007(3) Ir1B 0.01891(9) 0.02191(11) 0.01997(11) 0.00044(8) 0.00323(7) -0.00277(7) I1B 0.0579(3) 0.0428(3) 0.0401(3) 0.0121(2) 0.0228(2) 0.0033(2) I2B 0.02185(16) 0.0441(2) 0.0404(2) -0.01693(19) 0.00198(15) -0.00509(15) P1B 0.0239(6) 0.0265(8) 0.0282(8) -0.0039(6) 0.0043(6) -0.0013(5) P2B 0.0251(6) 0.0231(7) 0.0256(7) 0.0024(6) 0.0075(6) -0.0016(5) Si1B 0.0288(7) 0.0305(9) 0.0247(8) -0.0037(7) 0.0003(6) -0.0046(6) Si2B 0.0193(7) 0.0410(10) 0.0308(9) -0.0033(7) 0.0000(6) -0.0002(6) N1B 0.025(2) 0.042(3) 0.042(3) -0.018(3) -0.002(2) 0.001(2) C1B 0.033(3) 0.040(4) 0.043(4) -0.009(3) 0.002(3) -0.010(3) C2B 0.047(4) 0.056(4) 0.028(3) -0.001(3) 0.002(3) 0.002(3) C3B 0.034(3) 0.031(3) 0.022(3) -0.004(2) 0.008(2) -0.001(2) C4B 0.042(3) 0.036(4) 0.035(4) 0.008(3) 0.003(3) 0.003(3) C5B 0.069(5) 0.031(4) 0.053(5) 0.005(3) 0.013(4) 0.003(3) C6B 0.054(4) 0.040(4) 0.050(4) 0.005(3) 0.018(3) -0.013(3) C7B 0.050(4) 0.049(4) 0.032(4) 0.005(3) 0.002(3) 0.013(3) C8B 0.029(3) 0.036(4) 0.043(4) -0.004(3) 0.010(3) 0.004(2) C9B 0.037(3) 0.053(4) 0.051(4) -0.016(4) 0.014(3) 0.003(3) C10B 0.030(3) 0.052(4) 0.058(5) -0.015(4) 0.004(3) 0.002(3) C11B 0.037(3) 0.049(4) 0.050(4) -0.002(3) 0.020(3) -0.004(3) C12B 0.055(4) 0.078(6) 0.064(5) -0.034(4) 0.033(4) -0.040(4) C13B 0.061(5) 0.076(6) 0.048(5) -0.009(4) -0.013(4) 0.035(4) C14B 0.024(2) 0.036(3) 0.030(3) 0.003(3) 0.003(2) 0.007(2) C15B 0.032(3) 0.045(4) 0.032(3) 0.009(3) 0.008(3) -0.006(3) C16B 0.047(4) 0.049(4) 0.027(3) -0.002(3) 0.010(3) -0.003(3) C17B 0.048(4) 0.060(5) 0.034(4) 0.008(3) 0.020(3) -0.007(3) C18B 0.040(3) 0.037(4) 0.034(4) 0.005(3) 0.014(3) -0.003(3) C19B 0.045(3) 0.023(3) 0.037(4) -0.002(3) 0.014(3) -0.003(2) C20B 0.042(4) 0.036(4) 0.087(6) -0.006(4) 0.013(4) -0.011(3) C21B 0.061(5) 0.044(5) 0.089(7) -0.021(4) 0.038(5) -0.003(4) C22B 0.109(7) 0.038(4) 0.058(5) 0.012(4) 0.018(5) -0.010(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 Ir1A C18A 2.119(6) . ? Ir1A N1A 2.213(5) . ? Ir1A P2A 2.3221(14) . ? Ir1A P1A 2.4337(15) . ? Ir1A I2A 2.6647(4) . ? Ir1A I1A 2.8243(5) . ? P1A C3A 1.833(6) . ? P1A C4A 1.879(7) . ? P1A C8A 1.926(7) . ? P2A C14A 1.828(5) . ? P2A C15A 1.847(6) . ? P2A C19A 1.890(6) . ? Si1A N1A 1.781(5) . ? Si1A C1A 1.860(8) . ? Si1A C3A 1.861(6) . ? Si1A C2A 1.876(8) . ? Si2A N1A 1.790(5) . ? Si2A C13A 1.851(7) . ? Si2A C12A 1.862(7) . ? Si2A C14A 1.865(6) . ? N1A H1NA 0.9300 . ? C1A H1A 0.9800 . ? C1A H1B 0.9800 . ? C1A H1C 0.9800 . ? C2A H2A 0.9800 . ? C2A H2B 0.9800 . ? C2A H2C 0.9800 . ? C3A H3A 0.9900 . ? C3A H3B 0.9900 . ? C4A C7A 1.526(11) . ? C4A C5A 1.547(10) . ? C4A C6A 1.553(11) . ? C5A H5A 0.9800 . ? C5A H5B 0.9800 . ? C5A H5C 0.9800 . ? C6A H6A 0.9800 . ? C6A H6B 0.9800 . ? C6A H6C 0.9800 . ? C7A H7A 0.9800 . ? C7A H7B 0.9800 . ? C7A H7C 0.9800 . ? C8A C11A 1.524(11) . ? C8A C10A 1.527(10) . ? C8A C9A 1.555(12) . ? C9A H9A 0.9800 . ? C9A H9B 0.9800 . ? C9A H9C 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 0.9800 . ? C14A H14A 0.9900 . ? C14A H14B 0.9900 . ? C15A C17A 1.526(9) . ? C15A C16A 1.535(9) . ? C15A C18A 1.575(9) . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C18A H18A 0.9900 . ? C18A H18B 0.9900 . ? C19A C22A 1.511(9) . ? C19A C21A 1.529(8) . ? C19A C20A 1.569(10) . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? Ir1B C18B 2.128(6) . ? Ir1B N1B 2.212(5) . ? Ir1B P2B 2.3303(14) . ? Ir1B P1B 2.4377(15) . ? Ir1B I2B 2.6706(4) . ? Ir1B I1B 2.8650(5) . ? P1B C3B 1.828(6) . ? P1B C4B 1.913(7) . ? P1B C8B 1.923(6) . ? P2B C14B 1.824(5) . ? P2B C15B 1.847(6) . ? P2B C19B 1.894(6) . ? Si1B N1B 1.792(5) . ? Si1B C1B 1.855(6) . ? Si1B C2B 1.865(7) . ? Si1B C3B 1.868(6) . ? Si2B N1B 1.783(5) . ? Si2B C13B 1.859(8) . ? Si2B C12B 1.865(7) . ? Si2B C14B 1.870(6) . ? N1B H1NB 0.9300 . ? C1B H1D 0.9800 . ? C1B H1E 0.9800 . ? C1B H1F 0.9800 . ? C2B H2D 0.9800 . ? C2B H2E 0.9800 . ? C2B H2F 0.9800 . ? C3B H3C 0.9900 . ? C3B H3D 0.9900 . ? C4B C6B 1.522(9) . ? C4B C7B 1.532(9) . ? C4B C5B 1.550(9) . ? C5B H5D 0.9800 . ? C5B H5E 0.9800 . ? C5B H5F 0.9800 . ? C6B H6D 0.9800 . ? C6B H6E 0.9800 . ? C6B H6F 0.9800 . ? C7B H7D 0.9800 . ? C7B H7E 0.9800 . ? C7B H7F 0.9800 . ? C8B C9B 1.530(9) . ? C8B C11B 1.534(9) . ? C8B C10B 1.539(9) . ? C9B H9D 0.9800 . ? C9B H9E 0.9800 . ? C9B H9F 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12B H12D 0.9800 . ? C12B H12E 0.9800 . ? C12B H12F 0.9800 . ? C13B H13D 0.9800 . ? C13B H13E 0.9800 . ? C13B H13F 0.9800 . ? C14B H14C 0.9900 . ? C14B H14D 0.9900 . ? C15B C17B 1.515(8) . ? C15B C16B 1.525(9) . ? C15B C18B 1.589(9) . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C18B H18C 0.9900 . ? C18B H18D 0.9900 . ? C19B C22B 1.503(10) . ? C19B C20B 1.518(9) . ? C19B C21B 1.550(9) . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 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 C18A Ir1A N1A 95.3(2) . . ? C18A Ir1A P2A 67.62(18) . . ? N1A Ir1A P2A 88.02(13) . . ? C18A Ir1A P1A 102.57(18) . . ? N1A Ir1A P1A 87.92(13) . . ? P2A Ir1A P1A 168.97(5) . . ? C18A Ir1A I2A 89.72(18) . . ? N1A Ir1A I2A 174.94(15) . . ? P2A Ir1A I2A 94.63(4) . . ? P1A Ir1A I2A 90.23(4) . . ? C18A Ir1A I1A 160.92(18) . . ? N1A Ir1A I1A 81.58(16) . . ? P2A Ir1A I1A 93.41(4) . . ? P1A Ir1A I1A 96.13(4) . . ? I2A Ir1A I1A 93.945(16) . . ? C3A P1A C4A 103.6(3) . . ? C3A P1A C8A 101.7(3) . . ? C4A P1A C8A 106.3(4) . . ? C3A P1A Ir1A 104.1(2) . . ? C4A P1A Ir1A 115.7(3) . . ? C8A P1A Ir1A 122.7(3) . . ? C14A P2A C15A 107.1(3) . . ? C14A P2A C19A 102.0(3) . . ? C15A P2A C19A 115.4(3) . . ? C14A P2A Ir1A 108.06(18) . . ? C15A P2A Ir1A 90.6(2) . . ? C19A P2A Ir1A 131.9(2) . . ? N1A Si1A C1A 111.7(3) . . ? N1A Si1A C3A 106.3(3) . . ? C1A Si1A C3A 115.6(3) . . ? N1A Si1A C2A 108.7(4) . . ? C1A Si1A C2A 107.7(5) . . ? C3A Si1A C2A 106.5(4) . . ? N1A Si2A C13A 114.2(3) . . ? N1A Si2A C12A 106.6(3) . . ? C13A Si2A C12A 109.8(3) . . ? N1A Si2A C14A 102.6(2) . . ? C13A Si2A C14A 115.3(3) . . ? C12A Si2A C14A 107.8(3) . . ? Si1A N1A Si2A 120.6(3) . . ? Si1A N1A Ir1A 119.2(2) . . ? Si2A N1A Ir1A 118.1(3) . . ? Si1A N1A H1NA 94.8 . . ? Si2A N1A H1NA 94.8 . . ? Ir1A N1A H1NA 94.8 . . ? Si1A C1A H1A 109.5 . . ? Si1A C1A H1B 109.5 . . ? H1A C1A H1B 109.5 . . ? Si1A C1A H1C 109.5 . . ? H1A C1A H1C 109.5 . . ? H1B C1A H1C 109.5 . . ? Si1A C2A H2A 109.5 . . ? Si1A C2A H2B 109.5 . . ? H2A C2A H2B 109.5 . . ? Si1A C2A H2C 109.5 . . ? H2A C2A H2C 109.5 . . ? H2B C2A H2C 109.5 . . ? P1A C3A Si1A 116.4(3) . . ? P1A C3A H3A 108.2 . . ? Si1A C3A H3A 108.2 . . ? P1A C3A H3B 108.2 . . ? Si1A C3A H3B 108.2 . . ? H3A C3A H3B 107.3 . . ? C7A C4A C5A 109.6(7) . . ? C7A C4A C6A 105.4(7) . . ? C5A C4A C6A 108.5(6) . . ? C7A C4A P1A 107.5(5) . . ? C5A C4A P1A 110.8(5) . . ? C6A C4A P1A 114.9(6) . . ? C4A C5A H5A 109.5 . . ? C4A C5A H5B 109.5 . . ? H5A C5A H5B 109.5 . . ? C4A C5A H5C 109.5 . . ? H5A C5A H5C 109.5 . . ? H5B C5A H5C 109.5 . . ? C4A C6A H6A 109.5 . . ? C4A C6A H6B 109.5 . . ? H6A C6A H6B 109.5 . . ? C4A C6A H6C 109.5 . . ? H6A C6A H6C 109.5 . . ? H6B C6A H6C 109.5 . . ? C4A C7A H7A 109.5 . . ? C4A C7A H7B 109.5 . . ? H7A C7A H7B 109.5 . . ? C4A C7A H7C 109.5 . . ? H7A C7A H7C 109.5 . . ? H7B C7A H7C 109.5 . . ? C11A C8A C10A 108.9(6) . . ? C11A C8A C9A 107.4(7) . . ? C10A C8A C9A 105.6(7) . . ? C11A C8A P1A 113.4(6) . . ? C10A C8A P1A 112.2(5) . . ? C9A C8A P1A 108.9(5) . . ? C8A C9A H9A 109.5 . . ? C8A C9A H9B 109.5 . . ? H9A C9A H9B 109.5 . . ? C8A C9A H9C 109.5 . . ? H9A C9A H9C 109.5 . . ? H9B C9A H9C 109.5 . . ? C8A C10A H10A 109.5 . . ? C8A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C8A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C8A C11A H11A 109.5 . . ? C8A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? C8A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? Si2A C12A H12A 109.5 . . ? Si2A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? Si2A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? Si2A C13A H13A 109.5 . . ? Si2A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? Si2A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 109.5 . . ? P2A C14A Si2A 115.3(3) . . ? P2A C14A H14A 108.5 . . ? Si2A C14A H14A 108.5 . . ? P2A C14A H14B 108.5 . . ? Si2A C14A H14B 108.5 . . ? H14A C14A H14B 107.5 . . ? C17A C15A C16A 108.7(5) . . ? C17A C15A C18A 110.3(5) . . ? C16A C15A C18A 112.5(5) . . ? C17A C15A P2A 116.5(5) . . ? C16A C15A P2A 115.5(5) . . ? C18A C15A P2A 92.4(4) . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15A C17A H17A 109.5 . . ? C15A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C15A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C15A C18A Ir1A 106.7(4) . . ? C15A C18A H18A 110.4 . . ? Ir1A C18A H18A 110.4 . . ? C15A C18A H18B 110.4 . . ? Ir1A C18A H18B 110.4 . . ? H18A C18A H18B 108.6 . . ? C22A C19A C21A 109.9(6) . . ? C22A C19A C20A 108.3(6) . . ? C21A C19A C20A 108.0(6) . . ? C22A C19A P2A 111.0(4) . . ? C21A C19A P2A 111.6(4) . . ? C20A C19A P2A 107.8(5) . . ? C19A C20A H20A 109.5 . . ? C19A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C19A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C19A C21A H21A 109.5 . . ? C19A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C19A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C19A C22A H22A 109.5 . . ? C19A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C19A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C18B Ir1B N1B 93.3(2) . . ? C18B Ir1B P2B 67.20(18) . . ? N1B Ir1B P2B 88.22(13) . . ? C18B Ir1B P1B 102.08(18) . . ? N1B Ir1B P1B 88.38(14) . . ? P2B Ir1B P1B 168.52(5) . . ? C18B Ir1B I2B 91.06(18) . . ? N1B Ir1B I2B 175.49(15) . . ? P2B Ir1B I2B 94.43(4) . . ? P1B Ir1B I2B 89.71(3) . . ? C18B Ir1B I1B 159.59(17) . . ? N1B Ir1B I1B 79.53(16) . . ? P2B Ir1B I1B 93.30(4) . . ? P1B Ir1B I1B 96.85(4) . . ? I2B Ir1B I1B 96.647(15) . . ? C3B P1B C4B 103.5(3) . . ? C3B P1B C8B 101.3(3) . . ? C4B P1B C8B 105.9(3) . . ? C3B P1B Ir1B 104.35(19) . . ? C4B P1B Ir1B 115.4(2) . . ? C8B P1B Ir1B 123.6(2) . . ? C14B P2B C15B 106.2(3) . . ? C14B P2B C19B 103.2(3) . . ? C15B P2B C19B 114.8(3) . . ? C14B P2B Ir1B 107.8(2) . . ? C15B P2B Ir1B 91.3(2) . . ? C19B P2B Ir1B 131.4(2) . . ? N1B Si1B C1B 110.8(3) . . ? N1B Si1B C2B 110.3(3) . . ? C1B Si1B C2B 108.5(3) . . ? N1B Si1B C3B 106.7(2) . . ? C1B Si1B C3B 113.7(3) . . ? C2B Si1B C3B 106.7(3) . . ? N1B Si2B C13B 105.7(3) . . ? N1B Si2B C12B 114.0(4) . . ? C13B Si2B C12B 108.7(4) . . ? N1B Si2B C14B 103.1(2) . . ? C13B Si2B C14B 108.9(3) . . ? C12B Si2B C14B 115.8(3) . . ? Si2B N1B Si1B 121.6(3) . . ? Si2B N1B Ir1B 118.1(3) . . ? Si1B N1B Ir1B 118.5(2) . . ? Si2B N1B H1NB 94.4 . . ? Si1B N1B H1NB 94.4 . . ? Ir1B N1B H1NB 94.4 . . ? Si1B C1B H1D 109.5 . . ? Si1B C1B H1E 109.5 . . ? H1D C1B H1E 109.5 . . ? Si1B C1B H1F 109.5 . . ? H1D C1B H1F 109.5 . . ? H1E C1B H1F 109.5 . . ? Si1B C2B H2D 109.5 . . ? Si1B C2B H2E 109.5 . . ? H2D C2B H2E 109.5 . . ? Si1B C2B H2F 109.5 . . ? H2D C2B H2F 109.5 . . ? H2E C2B H2F 109.5 . . ? P1B C3B Si1B 116.6(3) . . ? P1B C3B H3C 108.1 . . ? Si1B C3B H3C 108.1 . . ? P1B C3B H3D 108.1 . . ? Si1B C3B H3D 108.1 . . ? H3C C3B H3D 107.3 . . ? C6B C4B C7B 110.2(6) . . ? C6B C4B C5B 104.8(6) . . ? C7B C4B C5B 108.6(5) . . ? C6B C4B P1B 108.0(4) . . ? C7B C4B P1B 109.6(5) . . ? C5B C4B P1B 115.5(5) . . ? C4B C5B H5D 109.5 . . ? C4B C5B H5E 109.5 . . ? H5D C5B H5E 109.5 . . ? C4B C5B H5F 109.5 . . ? H5D C5B H5F 109.5 . . ? H5E C5B H5F 109.5 . . ? C4B C6B H6D 109.5 . . ? C4B C6B H6E 109.5 . . ? H6D C6B H6E 109.5 . . ? C4B C6B H6F 109.5 . . ? H6D C6B H6F 109.5 . . ? H6E C6B H6F 109.5 . . ? C4B C7B H7D 109.5 . . ? C4B C7B H7E 109.5 . . ? H7D C7B H7E 109.5 . . ? C4B C7B H7F 109.5 . . ? H7D C7B H7F 109.5 . . ? H7E C7B H7F 109.5 . . ? C9B C8B C11B 107.1(6) . . ? C9B C8B C10B 108.0(5) . . ? C11B C8B C10B 107.4(5) . . ? C9B C8B P1B 112.8(4) . . ? C11B C8B P1B 108.1(4) . . ? C10B C8B P1B 113.1(5) . . ? C8B C9B H9D 109.5 . . ? C8B C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C8B C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C8B C10B H10D 109.5 . . ? C8B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C8B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C8B C11B H11D 109.5 . . ? C8B C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C8B C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? Si2B C12B H12D 109.5 . . ? Si2B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? Si2B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? Si2B C13B H13D 109.5 . . ? Si2B C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? Si2B C13B H13F 109.5 . . ? H13D C13B H13F 109.5 . . ? H13E C13B H13F 109.5 . . ? P2B C14B Si2B 115.0(3) . . ? P2B C14B H14C 108.5 . . ? Si2B C14B H14C 108.5 . . ? P2B C14B H14D 108.5 . . ? Si2B C14B H14D 108.5 . . ? H14C C14B H14D 107.5 . . ? C17B C15B C16B 109.7(5) . . ? C17B C15B C18B 112.4(5) . . ? C16B C15B C18B 108.7(5) . . ? C17B C15B P2B 116.5(5) . . ? C16B C15B P2B 116.4(4) . . ? C18B C15B P2B 91.7(4) . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15B C17B H17D 109.5 . . ? C15B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C15B C18B Ir1B 107.1(4) . . ? C15B C18B H18C 110.3 . . ? Ir1B C18B H18C 110.3 . . ? C15B C18B H18D 110.3 . . ? Ir1B C18B H18D 110.3 . . ? H18C C18B H18D 108.6 . . ? C22B C19B C20B 109.5(6) . . ? C22B C19B C21B 108.0(7) . . ? C20B C19B C21B 108.9(6) . . ? C22B C19B P2B 110.3(5) . . ? C20B C19B P2B 112.3(5) . . ? C21B C19B P2B 107.8(4) . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C19B C21B H21D 109.5 . . ? C19B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C19B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C19B C22B H22D 109.5 . . ? C19B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C19B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 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 C18A Ir1A P1A C3A -114.7(3) . . . . ? N1A Ir1A P1A C3A -19.7(3) . . . . ? P2A Ir1A P1A C3A -88.2(4) . . . . ? I2A Ir1A P1A C3A 155.5(2) . . . . ? I1A Ir1A P1A C3A 61.5(2) . . . . ? C18A Ir1A P1A C4A -1.7(3) . . . . ? N1A Ir1A P1A C4A 93.2(3) . . . . ? P2A Ir1A P1A C4A 24.8(4) . . . . ? I2A Ir1A P1A C4A -91.5(3) . . . . ? I1A Ir1A P1A C4A 174.5(3) . . . . ? C18A Ir1A P1A C8A 131.2(4) . . . . ? N1A Ir1A P1A C8A -133.9(4) . . . . ? P2A Ir1A P1A C8A 157.6(4) . . . . ? I2A Ir1A P1A C8A 41.4(3) . . . . ? I1A Ir1A P1A C8A -52.6(3) . . . . ? C18A Ir1A P2A C14A 98.0(3) . . . . ? N1A Ir1A P2A C14A 1.4(3) . . . . ? P1A Ir1A P2A C14A 69.9(3) . . . . ? I2A Ir1A P2A C14A -174.3(2) . . . . ? I1A Ir1A P2A C14A -80.0(2) . . . . ? C18A Ir1A P2A C15A -10.3(3) . . . . ? N1A Ir1A P2A C15A -106.8(3) . . . . ? P1A Ir1A P2A C15A -38.4(3) . . . . ? I2A Ir1A P2A C15A 77.5(2) . . . . ? I1A Ir1A P2A C15A 171.7(2) . . . . ? C18A Ir1A P2A C19A -136.1(3) . . . . ? N1A Ir1A P2A C19A 127.4(3) . . . . ? P1A Ir1A P2A C19A -164.1(3) . . . . ? I2A Ir1A P2A C19A -48.3(3) . . . . ? I1A Ir1A P2A C19A 46.0(3) . . . . ? C1A Si1A N1A Si2A 38.1(5) . . . . ? C3A Si1A N1A Si2A 165.2(4) . . . . ? C2A Si1A N1A Si2A -80.6(5) . . . . ? C1A Si1A N1A Ir1A -125.1(4) . . . . ? C3A Si1A N1A Ir1A 1.9(4) . . . . ? C2A Si1A N1A Ir1A 116.2(4) . . . . ? C13A Si2A N1A Si1A -66.4(5) . . . . ? C12A Si2A N1A Si1A 55.1(5) . . . . ? C14A Si2A N1A Si1A 168.2(4) . . . . ? C13A Si2A N1A Ir1A 97.1(4) . . . . ? C12A Si2A N1A Ir1A -141.5(3) . . . . ? C14A Si2A N1A Ir1A -28.3(4) . . . . ? C18A Ir1A N1A Si1A 113.3(4) . . . . ? P2A Ir1A N1A Si1A -179.4(3) . . . . ? P1A Ir1A N1A Si1A 10.9(3) . . . . ? I2A Ir1A N1A Si1A -57.7(18) . . . . ? I1A Ir1A N1A Si1A -85.7(3) . . . . ? C18A Ir1A N1A Si2A -50.4(4) . . . . ? P2A Ir1A N1A Si2A 16.9(3) . . . . ? P1A Ir1A N1A Si2A -152.8(3) . . . . ? I2A Ir1A N1A Si2A 138.6(14) . . . . ? I1A Ir1A N1A Si2A 110.7(3) . . . . ? C4A P1A C3A Si1A -94.8(4) . . . . ? C8A P1A C3A Si1A 155.0(4) . . . . ? Ir1A P1A C3A Si1A 26.6(4) . . . . ? N1A Si1A C3A P1A -19.8(5) . . . . ? C1A Si1A C3A P1A 104.8(5) . . . . ? C2A Si1A C3A P1A -135.6(5) . . . . ? C3A P1A C4A C7A 55.6(6) . . . . ? C8A P1A C4A C7A 162.3(5) . . . . ? Ir1A P1A C4A C7A -57.7(6) . . . . ? C3A P1A C4A C5A 175.3(5) . . . . ? C8A P1A C4A C5A -78.0(6) . . . . ? Ir1A P1A C4A C5A 62.0(6) . . . . ? C3A P1A C4A C6A -61.4(7) . . . . ? C8A P1A C4A C6A 45.4(7) . . . . ? Ir1A P1A C4A C6A -174.6(5) . . . . ? C3A P1A C8A C11A 157.4(6) . . . . ? C4A P1A C8A C11A 49.2(7) . . . . ? Ir1A P1A C8A C11A -87.3(6) . . . . ? C3A P1A C8A C10A 33.5(7) . . . . ? C4A P1A C8A C10A -74.6(7) . . . . ? Ir1A P1A C8A C10A 148.9(5) . . . . ? C3A P1A C8A C9A -83.1(6) . . . . ? C4A P1A C8A C9A 168.8(5) . . . . ? Ir1A P1A C8A C9A 32.3(7) . . . . ? C15A P2A C14A Si2A 78.0(4) . . . . ? C19A P2A C14A Si2A -160.4(3) . . . . ? Ir1A P2A C14A Si2A -18.4(4) . . . . ? N1A Si2A C14A P2A 28.7(4) . . . . ? C13A Si2A C14A P2A -95.9(4) . . . . ? C12A Si2A C14A P2A 141.0(3) . . . . ? C14A P2A C15A C17A 149.5(5) . . . . ? C19A P2A C15A C17A 36.7(6) . . . . ? Ir1A P2A C15A C17A -101.3(5) . . . . ? C14A P2A C15A C16A 20.1(6) . . . . ? C19A P2A C15A C16A -92.7(5) . . . . ? Ir1A P2A C15A C16A 129.2(5) . . . . ? C14A P2A C15A C18A -96.3(4) . . . . ? C19A P2A C15A C18A 150.9(4) . . . . ? Ir1A P2A C15A C18A 12.8(3) . . . . ? C17A C15A C18A Ir1A 104.7(5) . . . . ? C16A C15A C18A Ir1A -133.7(5) . . . . ? P2A C15A C18A Ir1A -14.7(4) . . . . ? N1A Ir1A C18A C15A 98.3(4) . . . . ? P2A Ir1A C18A C15A 12.6(3) . . . . ? P1A Ir1A C18A C15A -172.7(4) . . . . ? I2A Ir1A C18A C15A -82.5(4) . . . . ? I1A Ir1A C18A C15A 18.8(8) . . . . ? C14A P2A C19A C22A 49.7(5) . . . . ? C15A P2A C19A C22A 165.4(5) . . . . ? Ir1A P2A C19A C22A -78.4(5) . . . . ? C14A P2A C19A C21A 172.7(5) . . . . ? C15A P2A C19A C21A -71.6(6) . . . . ? Ir1A P2A C19A C21A 44.5(6) . . . . ? C14A P2A C19A C20A -68.8(5) . . . . ? C15A P2A C19A C20A 46.9(5) . . . . ? Ir1A P2A C19A C20A 163.0(3) . . . . ? C18B Ir1B P1B C3B 112.3(3) . . . . ? N1B Ir1B P1B C3B 19.2(3) . . . . ? P2B Ir1B P1B C3B 92.0(3) . . . . ? I2B Ir1B P1B C3B -156.7(2) . . . . ? I1B Ir1B P1B C3B -60.0(2) . . . . ? C18B Ir1B P1B C4B -0.6(3) . . . . ? N1B Ir1B P1B C4B -93.6(3) . . . . ? P2B Ir1B P1B C4B -20.8(4) . . . . ? I2B Ir1B P1B C4B 90.5(2) . . . . ? I1B Ir1B P1B C4B -172.9(2) . . . . ? C18B Ir1B P1B C8B -133.4(3) . . . . ? N1B Ir1B P1B C8B 133.5(3) . . . . ? P2B Ir1B P1B C8B -153.7(3) . . . . ? I2B Ir1B P1B C8B -42.4(3) . . . . ? I1B Ir1B P1B C8B 54.3(3) . . . . ? C18B Ir1B P2B C14B -97.2(3) . . . . ? N1B Ir1B P2B C14B -2.9(3) . . . . ? P1B Ir1B P2B C14B -75.7(3) . . . . ? I2B Ir1B P2B C14B 173.5(2) . . . . ? I1B Ir1B P2B C14B 76.5(2) . . . . ? C18B Ir1B P2B C15B 10.3(3) . . . . ? N1B Ir1B P2B C15B 104.6(2) . . . . ? P1B Ir1B P2B C15B 31.8(3) . . . . ? I2B Ir1B P2B C15B -79.02(19) . . . . ? I1B Ir1B P2B C15B -175.96(19) . . . . ? C18B Ir1B P2B C19B 135.7(3) . . . . ? N1B Ir1B P2B C19B -129.9(3) . . . . ? P1B Ir1B P2B C19B 157.3(3) . . . . ? I2B Ir1B P2B C19B 46.4(3) . . . . ? I1B Ir1B P2B C19B -50.5(3) . . . . ? C13B Si2B N1B Si1B -53.9(5) . . . . ? C12B Si2B N1B Si1B 65.5(5) . . . . ? C14B Si2B N1B Si1B -168.2(4) . . . . ? C13B Si2B N1B Ir1B 141.5(4) . . . . ? C12B Si2B N1B Ir1B -99.2(4) . . . . ? C14B Si2B N1B Ir1B 27.2(4) . . . . ? C1B Si1B N1B Si2B -40.6(5) . . . . ? C2B Si1B N1B Si2B 79.5(5) . . . . ? C3B Si1B N1B Si2B -164.9(4) . . . . ? C1B Si1B N1B Ir1B 124.0(3) . . . . ? C2B Si1B N1B Ir1B -115.9(4) . . . . ? C3B Si1B N1B Ir1B -0.4(4) . . . . ? C18B Ir1B N1B Si2B 51.7(4) . . . . ? P2B Ir1B N1B Si2B -15.3(3) . . . . ? P1B Ir1B N1B Si2B 153.7(3) . . . . ? I2B Ir1B N1B Si2B -141.2(16) . . . . ? I1B Ir1B N1B Si2B -109.0(3) . . . . ? C18B Ir1B N1B Si1B -113.4(4) . . . . ? P2B Ir1B N1B Si1B 179.6(3) . . . . ? P1B Ir1B N1B Si1B -11.4(3) . . . . ? I2B Ir1B N1B Si1B 54(2) . . . . ? I1B Ir1B N1B Si1B 85.9(3) . . . . ? C4B P1B C3B Si1B 96.3(4) . . . . ? C8B P1B C3B Si1B -154.1(3) . . . . ? Ir1B P1B C3B Si1B -24.8(4) . . . . ? N1B Si1B C3B P1B 17.8(4) . . . . ? C1B Si1B C3B P1B -104.7(4) . . . . ? C2B Si1B C3B P1B 135.7(4) . . . . ? C3B P1B C4B C6B -53.4(5) . . . . ? C8B P1B C4B C6B -159.5(5) . . . . ? Ir1B P1B C4B C6B 59.9(5) . . . . ? C3B P1B C4B C7B -173.5(4) . . . . ? C8B P1B C4B C7B 80.4(5) . . . . ? Ir1B P1B C4B C7B -60.2(5) . . . . ? C3B P1B C4B C5B 63.5(5) . . . . ? C8B P1B C4B C5B -42.6(6) . . . . ? Ir1B P1B C4B C5B 176.8(4) . . . . ? C3B P1B C8B C9B -34.8(5) . . . . ? C4B P1B C8B C9B 72.9(5) . . . . ? Ir1B P1B C8B C9B -150.6(4) . . . . ? C3B P1B C8B C11B 83.4(5) . . . . ? C4B P1B C8B C11B -168.8(4) . . . . ? Ir1B P1B C8B C11B -32.4(5) . . . . ? C3B P1B C8B C10B -157.7(5) . . . . ? C4B P1B C8B C10B -50.0(5) . . . . ? Ir1B P1B C8B C10B 86.5(5) . . . . ? C15B P2B C14B Si2B -77.3(4) . . . . ? C19B P2B C14B Si2B 161.5(3) . . . . ? Ir1B P2B C14B Si2B 19.5(4) . . . . ? N1B Si2B C14B P2B -28.9(4) . . . . ? C13B Si2B C14B P2B -140.9(4) . . . . ? C12B Si2B C14B P2B 96.3(4) . . . . ? C14B P2B C15B C17B -19.9(6) . . . . ? C19B P2B C15B C17B 93.4(6) . . . . ? Ir1B P2B C15B C17B -128.9(5) . . . . ? C14B P2B C15B C16B -151.8(5) . . . . ? C19B P2B C15B C16B -38.5(6) . . . . ? Ir1B P2B C15B C16B 99.2(5) . . . . ? C14B P2B C15B C18B 96.3(4) . . . . ? C19B P2B C15B C18B -150.4(3) . . . . ? Ir1B P2B C15B C18B -12.7(3) . . . . ? C17B C15B C18B Ir1B 134.3(5) . . . . ? C16B C15B C18B Ir1B -104.1(5) . . . . ? P2B C15B C18B Ir1B 14.6(4) . . . . ? N1B Ir1B C18B C15B -99.2(4) . . . . ? P2B Ir1B C18B C15B -12.5(3) . . . . ? P1B Ir1B C18B C15B 171.8(3) . . . . ? I2B Ir1B C18B C15B 81.8(4) . . . . ? I1B Ir1B C18B C15B -30.6(8) . . . . ? C14B P2B C19B C22B -53.0(6) . . . . ? C15B P2B C19B C22B -168.1(5) . . . . ? Ir1B P2B C19B C22B 75.7(6) . . . . ? C14B P2B C19B C20B -175.3(5) . . . . ? C15B P2B C19B C20B 69.6(6) . . . . ? Ir1B P2B C19B C20B -46.6(6) . . . . ? C14B P2B C19B C21B 64.7(5) . . . . ? C15B P2B C19B C21B -50.4(6) . . . . ? Ir1B P2B C19B C21B -166.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 4.621 _refine_diff_density_min -2.624 _refine_diff_density_rms 0.151 # Attachment '08119_CCDC_730044.cif' data_08119 _database_code_depnum_ccdc_archive 'CCDC 730044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H52 Cl Ir N P2 Si2, C F3 O3 S' _chemical_formula_sum 'C23 H52 Cl F3 Ir N O3 P2 S Si2' _chemical_formula_weight 825.49 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9232(9) _cell_length_b 20.6668(15) _cell_length_c 13.5066(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.5730(10) _cell_angle_gamma 90.00 _cell_volume 3474.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9506 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 25.8 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 4.181 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.5728 _exptl_absorpt_correction_T_max 0.6799 _exptl_absorpt_process_details 'TWINABS, G. Sheldrick, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 10 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 28585 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.68 _reflns_number_total 6581 _reflns_number_gt 5559 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 2008)' _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^)+(0.0410P)^2^+6.7209P] 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 6581 _refine_ls_number_parameters 338 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0815 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.768879(13) 0.872241(8) 0.320329(12) 0.02428(7) Uani 1 1 d . . . Cl1 Cl 0.87573(11) 0.77840(7) 0.34989(9) 0.0419(3) Uani 1 1 d . . . P1 P 0.72834(10) 0.86529(6) 0.47823(9) 0.0272(3) Uani 1 1 d . . . P2 P 0.78181(10) 0.87709(6) 0.14888(9) 0.0256(2) Uani 1 1 d . . . Si1 Si 0.70211(11) 1.00477(6) 0.41908(10) 0.0301(3) Uani 1 1 d . . . Si2 Si 0.68926(10) 1.01110(6) 0.18426(10) 0.0277(3) Uani 1 1 d . . . N1 N 0.6837(3) 0.96418(18) 0.2963(3) 0.0260(8) Uani 1 1 d . . . H1N H 0.623(4) 0.957(2) 0.284(3) 0.016(12) Uiso 1 1 d . . . C1 C 0.6143(4) 1.0768(2) 0.4080(4) 0.0386(12) Uani 1 1 d . . . H1A H 0.6381 1.1102 0.3674 0.058 Uiso 1 1 calc R . . H1B H 0.6185 1.0938 0.4767 0.058 Uiso 1 1 calc R . . H1C H 0.5400 1.0647 0.3740 0.058 Uiso 1 1 calc R . . C2 C 0.8452(4) 1.0289(3) 0.4687(4) 0.0446(13) Uani 1 1 d . . . H2A H 0.8620 1.0627 0.4245 0.067 Uiso 1 1 calc R . . H2B H 0.8913 0.9912 0.4687 0.067 Uiso 1 1 calc R . . H2C H 0.8579 1.0454 0.5389 0.067 Uiso 1 1 calc R . . C3 C 0.6606(4) 0.9403(2) 0.4968(4) 0.0347(11) Uani 1 1 d . . . H3A H 0.6811 0.9525 0.5704 0.042 Uiso 1 1 calc R . . H3B H 0.5817 0.9344 0.4743 0.042 Uiso 1 1 calc R . . C4 C 0.8150(4) 0.8440(3) 0.6088(4) 0.0369(12) Uani 1 1 d . . . C5 C 0.7417(5) 0.8257(4) 0.6793(4) 0.0584(17) Uani 1 1 d . . . H5A H 0.7865 0.8147 0.7480 0.088 Uiso 1 1 calc R . . H5B H 0.6971 0.7884 0.6501 0.088 Uiso 1 1 calc R . . H5C H 0.6955 0.8625 0.6840 0.088 Uiso 1 1 calc R . . C6 C 0.8906(5) 0.7874(3) 0.6052(4) 0.0532(16) Uani 1 1 d . . . H6A H 0.9345 0.7778 0.6750 0.080 Uiso 1 1 calc R . . H6B H 0.9375 0.7990 0.5618 0.080 Uiso 1 1 calc R . . H6C H 0.8482 0.7492 0.5767 0.080 Uiso 1 1 calc R . . C7 C 0.8833(5) 0.9026(3) 0.6539(5) 0.0573(17) Uani 1 1 d . . . H7A H 0.9287 0.8919 0.7225 0.086 Uiso 1 1 calc R . . H7B H 0.8364 0.9390 0.6589 0.086 Uiso 1 1 calc R . . H7C H 0.9289 0.9146 0.6093 0.086 Uiso 1 1 calc R . . C8 C 0.6216(4) 0.8026(2) 0.4180(4) 0.0379(12) Uani 1 1 d . . . C9 C 0.6574(5) 0.7322(2) 0.4398(5) 0.0486(14) Uani 1 1 d . . . H9A H 0.5983 0.7033 0.4060 0.073 Uiso 1 1 calc R . . H9B H 0.6771 0.7245 0.5141 0.073 Uiso 1 1 calc R . . H9C H 0.7195 0.7237 0.4132 0.073 Uiso 1 1 calc R . . C10 C 0.5114(4) 0.8111(3) 0.4345(4) 0.0452(13) Uani 1 1 d . . . H10A H 0.4644 0.7759 0.4002 0.068 Uiso 1 1 calc R . . H10B H 0.4812 0.8527 0.4058 0.068 Uiso 1 1 calc R . . H10C H 0.5169 0.8101 0.5083 0.068 Uiso 1 1 calc R . . C11 C 0.6252(4) 0.8210(2) 0.3065(4) 0.0362(11) Uani 1 1 d . . . H11A H 0.5626 0.8482 0.2728 0.043 Uiso 1 1 calc R . . H11B H 0.6237 0.7814 0.2647 0.043 Uiso 1 1 calc R . . C12 C 0.5589(4) 1.0533(3) 0.1316(4) 0.0418(13) Uani 1 1 d . . . H12A H 0.5005 1.0215 0.1160 0.063 Uiso 1 1 calc R . . H12B H 0.5604 1.0764 0.0687 0.063 Uiso 1 1 calc R . . H12C H 0.5472 1.0843 0.1825 0.063 Uiso 1 1 calc R . . C13 C 0.7958(4) 1.0744(2) 0.2120(4) 0.0427(13) Uani 1 1 d . . . H13A H 0.8660 1.0540 0.2398 0.064 Uiso 1 1 calc R . . H13B H 0.7821 1.1051 0.2624 0.064 Uiso 1 1 calc R . . H13C H 0.7952 1.0975 0.1485 0.064 Uiso 1 1 calc R . . C14 C 0.7051(4) 0.9483(2) 0.0904(3) 0.0289(10) Uani 1 1 d . . . H14A H 0.6329 0.9341 0.0502 0.035 Uiso 1 1 calc R . . H14B H 0.7413 0.9680 0.0419 0.035 Uiso 1 1 calc R . . C15 C 0.9273(4) 0.8955(3) 0.1559(4) 0.0383(12) Uani 1 1 d . . . C16 C 0.9396(5) 0.9438(3) 0.0734(5) 0.0583(17) Uani 1 1 d . . . H16A H 1.0161 0.9515 0.0805 0.087 Uiso 1 1 calc R . . H16B H 0.9046 0.9847 0.0819 0.087 Uiso 1 1 calc R . . H16C H 0.9061 0.9259 0.0051 0.087 Uiso 1 1 calc R . . C17 C 0.9731(4) 0.9271(3) 0.2633(5) 0.0523(15) Uani 1 1 d . . . H17A H 1.0489 0.9380 0.2727 0.079 Uiso 1 1 calc R . . H17B H 0.9666 0.8966 0.3169 0.079 Uiso 1 1 calc R . . H17C H 0.9326 0.9665 0.2680 0.079 Uiso 1 1 calc R . . C18 C 0.9946(5) 0.8348(3) 0.1537(5) 0.0496(15) Uani 1 1 d . . . H18A H 1.0687 0.8474 0.1574 0.074 Uiso 1 1 calc R . . H18B H 0.9642 0.8110 0.0897 0.074 Uiso 1 1 calc R . . H18C H 0.9940 0.8072 0.2125 0.074 Uiso 1 1 calc R . . C19 C 0.7249(4) 0.8109(2) 0.0541(4) 0.0350(11) Uani 1 1 d . . . C20 C 0.6030(4) 0.8087(3) 0.0369(5) 0.0488(15) Uani 1 1 d . . . H20A H 0.5727 0.7743 -0.0123 0.073 Uiso 1 1 calc R . . H20B H 0.5719 0.8504 0.0096 0.073 Uiso 1 1 calc R . . H20C H 0.5865 0.8000 0.1023 0.073 Uiso 1 1 calc R . . C21 C 0.7483(6) 0.8234(3) -0.0504(4) 0.0540(16) Uani 1 1 d . . . H21A H 0.7182 0.7881 -0.0979 0.081 Uiso 1 1 calc R . . H21B H 0.8262 0.8255 -0.0409 0.081 Uiso 1 1 calc R . . H21C H 0.7156 0.8644 -0.0789 0.081 Uiso 1 1 calc R . . C22 C 0.7694(5) 0.7438(2) 0.0945(4) 0.0452(14) Uani 1 1 d . . . H22A H 0.7382 0.7108 0.0431 0.068 Uiso 1 1 calc R . . H22B H 0.7505 0.7344 0.1586 0.068 Uiso 1 1 calc R . . H22C H 0.8477 0.7437 0.1073 0.068 Uiso 1 1 calc R . . S1 S 0.33501(11) 0.96610(6) 0.24257(10) 0.0378(3) Uani 1 1 d . . . F1 F 0.3046(3) 0.84512(17) 0.1896(3) 0.0712(11) Uani 1 1 d . . . F2 F 0.2116(3) 0.9101(2) 0.0788(3) 0.0711(11) Uani 1 1 d . . . F3 F 0.3796(3) 0.9013(2) 0.0933(3) 0.0771(12) Uani 1 1 d . . . C23 C 0.3059(5) 0.9029(3) 0.1468(4) 0.0464(14) Uani 1 1 d . . . O1 O 0.4456(3) 0.95475(18) 0.2944(3) 0.0478(9) Uani 1 1 d . . . O2 O 0.3144(3) 1.02416(19) 0.1819(4) 0.0605(12) Uani 1 1 d . . . O3 O 0.2610(3) 0.9522(2) 0.3030(3) 0.0566(11) Uani 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 0.02494(10) 0.02951(11) 0.01799(10) 0.00069(7) 0.00503(7) 0.00467(7) Cl1 0.0483(8) 0.0484(8) 0.0315(7) 0.0116(6) 0.0151(6) 0.0238(6) P1 0.0316(6) 0.0316(6) 0.0199(6) 0.0004(5) 0.0095(5) 0.0024(5) P2 0.0291(6) 0.0287(6) 0.0192(6) 0.0016(5) 0.0067(5) 0.0030(5) Si1 0.0310(7) 0.0306(7) 0.0279(7) -0.0074(5) 0.0067(5) 0.0004(5) Si2 0.0301(7) 0.0245(6) 0.0275(7) 0.0017(5) 0.0062(5) 0.0020(5) N1 0.023(2) 0.028(2) 0.026(2) -0.0010(16) 0.0045(16) 0.0005(17) C1 0.045(3) 0.029(3) 0.045(3) -0.010(2) 0.017(2) 0.001(2) C2 0.038(3) 0.057(4) 0.034(3) -0.012(3) 0.001(2) -0.005(3) C3 0.036(3) 0.042(3) 0.027(3) -0.001(2) 0.011(2) 0.009(2) C4 0.044(3) 0.044(3) 0.022(2) 0.006(2) 0.007(2) 0.013(2) C5 0.074(5) 0.075(4) 0.032(3) 0.010(3) 0.023(3) 0.017(3) C6 0.068(4) 0.056(4) 0.036(3) 0.011(3) 0.014(3) 0.024(3) C7 0.053(4) 0.066(4) 0.040(3) -0.004(3) -0.010(3) 0.007(3) C8 0.043(3) 0.035(3) 0.040(3) 0.006(2) 0.018(2) 0.006(2) C9 0.062(4) 0.029(3) 0.060(4) 0.005(3) 0.024(3) -0.002(3) C10 0.047(3) 0.044(3) 0.050(3) 0.005(3) 0.022(3) -0.002(3) C11 0.040(3) 0.029(3) 0.039(3) 0.000(2) 0.010(2) -0.004(2) C12 0.045(3) 0.042(3) 0.036(3) 0.007(2) 0.006(2) 0.014(2) C13 0.050(3) 0.033(3) 0.045(3) 0.002(2) 0.013(3) -0.006(2) C14 0.032(3) 0.028(2) 0.025(2) 0.0042(19) 0.0048(19) 0.0015(19) C15 0.032(3) 0.041(3) 0.045(3) 0.003(2) 0.015(2) 0.001(2) C16 0.052(4) 0.057(4) 0.079(5) 0.022(3) 0.039(3) 0.004(3) C17 0.036(3) 0.056(4) 0.059(4) -0.004(3) 0.000(3) 0.000(3) C18 0.040(3) 0.055(4) 0.060(4) 0.007(3) 0.024(3) 0.013(3) C19 0.048(3) 0.026(3) 0.028(3) 0.000(2) 0.005(2) 0.002(2) C20 0.049(3) 0.036(3) 0.051(4) 0.000(3) -0.004(3) -0.009(2) C21 0.089(5) 0.046(3) 0.025(3) -0.002(2) 0.012(3) -0.002(3) C22 0.064(4) 0.025(3) 0.045(3) 0.000(2) 0.012(3) 0.002(2) S1 0.0402(7) 0.0309(7) 0.0421(7) -0.0056(5) 0.0108(6) -0.0011(5) F1 0.099(3) 0.0353(19) 0.082(3) -0.0140(18) 0.029(2) -0.0108(19) F2 0.057(2) 0.096(3) 0.051(2) -0.014(2) -0.0014(18) -0.012(2) F3 0.078(3) 0.100(3) 0.070(3) -0.024(2) 0.048(2) -0.004(2) C23 0.047(3) 0.049(3) 0.044(3) -0.006(3) 0.014(3) 0.000(3) O1 0.042(2) 0.047(2) 0.050(2) 0.0009(18) 0.0040(18) -0.0062(17) O2 0.063(3) 0.035(2) 0.082(3) 0.016(2) 0.018(2) 0.0103(19) O3 0.059(3) 0.070(3) 0.052(3) -0.017(2) 0.033(2) -0.009(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 C11 2.103(5) . ? Ir1 N1 2.176(4) . ? Ir1 P1 2.3331(12) . ? Ir1 Cl1 2.3519(12) . ? Ir1 P2 2.3682(12) . ? P1 C3 1.831(5) . ? P1 C4 1.869(5) . ? P1 C8 1.908(6) . ? P2 C14 1.830(4) . ? P2 C19 1.883(5) . ? P2 C15 1.896(5) . ? Si1 N1 1.817(4) . ? Si1 C1 1.854(5) . ? Si1 C2 1.858(5) . ? Si1 C3 1.862(5) . ? Si2 N1 1.815(4) . ? Si2 C12 1.860(5) . ? Si2 C13 1.863(5) . ? Si2 C14 1.864(5) . ? N1 H1N 0.77(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.526(8) . ? C4 C6 1.534(7) . ? C4 C5 1.559(8) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.510(7) . ? C8 C9 1.531(7) . ? C8 C11 1.566(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.532(7) . ? C15 C16 1.535(7) . ? C15 C17 1.555(8) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.530(8) . ? C19 C22 1.543(7) . ? C19 C21 1.543(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? S1 O1 1.432(4) . ? S1 O2 1.437(4) . ? S1 O3 1.443(4) . ? S1 C23 1.805(6) . ? F1 C23 1.329(7) . ? F2 C23 1.323(7) . ? F3 C23 1.342(7) . ? 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 C11 Ir1 N1 91.57(18) . . ? C11 Ir1 P1 68.94(14) . . ? N1 Ir1 P1 87.79(11) . . ? C11 Ir1 Cl1 93.65(14) . . ? N1 Ir1 Cl1 174.73(11) . . ? P1 Ir1 Cl1 93.42(4) . . ? C11 Ir1 P2 103.10(14) . . ? N1 Ir1 P2 89.01(10) . . ? P1 Ir1 P2 171.33(4) . . ? Cl1 Ir1 P2 90.49(4) . . ? C3 P1 C4 104.9(2) . . ? C3 P1 C8 108.4(2) . . ? C4 P1 C8 115.1(2) . . ? C3 P1 Ir1 107.84(16) . . ? C4 P1 Ir1 130.69(17) . . ? C8 P1 Ir1 88.05(16) . . ? C14 P2 C19 102.9(2) . . ? C14 P2 C15 106.0(2) . . ? C19 P2 C15 112.4(2) . . ? C14 P2 Ir1 106.48(16) . . ? C19 P2 Ir1 121.11(16) . . ? C15 P2 Ir1 106.79(17) . . ? N1 Si1 C1 111.7(2) . . ? N1 Si1 C2 109.1(2) . . ? C1 Si1 C2 110.0(3) . . ? N1 Si1 C3 101.4(2) . . ? C1 Si1 C3 110.9(2) . . ? C2 Si1 C3 113.5(2) . . ? N1 Si2 C12 109.5(2) . . ? N1 Si2 C13 113.6(2) . . ? C12 Si2 C13 107.0(3) . . ? N1 Si2 C14 103.35(19) . . ? C12 Si2 C14 108.7(2) . . ? C13 Si2 C14 114.6(2) . . ? Si2 N1 Si1 119.3(2) . . ? Si2 N1 Ir1 117.3(2) . . ? Si1 N1 Ir1 109.25(18) . . ? Si2 N1 H1N 101(3) . . ? Si1 N1 H1N 100(3) . . ? Ir1 N1 H1N 107(3) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 Si1 107.9(2) . . ? P1 C3 H3A 110.1 . . ? Si1 C3 H3A 110.1 . . ? P1 C3 H3B 110.1 . . ? Si1 C3 H3B 110.1 . . ? H3A C3 H3B 108.4 . . ? C7 C4 C6 108.2(5) . . ? C7 C4 C5 109.2(5) . . ? C6 C4 C5 109.3(5) . . ? C7 C4 P1 109.1(4) . . ? C6 C4 P1 112.1(4) . . ? C5 C4 P1 109.0(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C9 109.2(4) . . ? C10 C8 C11 112.7(4) . . ? C9 C8 C11 109.3(4) . . ? C10 C8 P1 117.4(4) . . ? C9 C8 P1 114.7(4) . . ? C11 C8 P1 92.4(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 Ir1 106.8(3) . . ? C8 C11 H11A 110.4 . . ? Ir1 C11 H11A 110.4 . . ? C8 C11 H11B 110.4 . . ? Ir1 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 Si2 114.3(2) . . ? P2 C14 H14A 108.7 . . ? Si2 C14 H14A 108.7 . . ? P2 C14 H14B 108.7 . . ? Si2 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C18 C15 C16 110.4(5) . . ? C18 C15 C17 106.7(5) . . ? C16 C15 C17 108.5(5) . . ? C18 C15 P2 113.2(4) . . ? C16 C15 P2 112.9(4) . . ? C17 C15 P2 104.8(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 107.3(4) . . ? C20 C19 C21 108.2(4) . . ? C22 C19 C21 109.1(4) . . ? C20 C19 P2 108.9(4) . . ? C22 C19 P2 111.9(3) . . ? C21 C19 P2 111.3(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 S1 O2 115.0(2) . . ? O1 S1 O3 114.7(3) . . ? O2 S1 O3 116.0(3) . . ? O1 S1 C23 102.7(3) . . ? O2 S1 C23 103.0(3) . . ? O3 S1 C23 102.7(3) . . ? F2 C23 F1 106.6(5) . . ? F2 C23 F3 106.5(5) . . ? F1 C23 F3 107.7(5) . . ? F2 C23 S1 113.1(4) . . ? F1 C23 S1 111.3(4) . . ? F3 C23 S1 111.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Ir1 P1 C3 -96.8(2) . . . . ? N1 Ir1 P1 C3 -4.3(2) . . . . ? Cl1 Ir1 P1 C3 170.57(18) . . . . ? C11 Ir1 P1 C4 133.9(3) . . . . ? N1 Ir1 P1 C4 -133.5(3) . . . . ? Cl1 Ir1 P1 C4 41.3(2) . . . . ? C11 Ir1 P1 C8 11.9(2) . . . . ? N1 Ir1 P1 C8 104.44(19) . . . . ? Cl1 Ir1 P1 C8 -80.70(16) . . . . ? C11 Ir1 P2 C14 86.3(2) . . . . ? N1 Ir1 P2 C14 -5.10(19) . . . . ? Cl1 Ir1 P2 C14 -179.86(16) . . . . ? C11 Ir1 P2 C19 -30.5(2) . . . . ? N1 Ir1 P2 C19 -121.9(2) . . . . ? Cl1 Ir1 P2 C19 63.35(19) . . . . ? C11 Ir1 P2 C15 -160.9(2) . . . . ? N1 Ir1 P2 C15 107.8(2) . . . . ? Cl1 Ir1 P2 C15 -66.99(18) . . . . ? C12 Si2 N1 Si1 -79.6(3) . . . . ? C13 Si2 N1 Si1 39.9(3) . . . . ? C14 Si2 N1 Si1 164.7(2) . . . . ? C12 Si2 N1 Ir1 144.7(2) . . . . ? C13 Si2 N1 Ir1 -95.8(3) . . . . ? C14 Si2 N1 Ir1 28.9(3) . . . . ? C1 Si1 N1 Si2 50.3(3) . . . . ? C2 Si1 N1 Si2 -71.5(3) . . . . ? C3 Si1 N1 Si2 168.5(3) . . . . ? C1 Si1 N1 Ir1 -170.8(2) . . . . ? C2 Si1 N1 Ir1 67.4(3) . . . . ? C3 Si1 N1 Ir1 -52.5(2) . . . . ? C11 Ir1 N1 Si2 -117.8(2) . . . . ? P1 Ir1 N1 Si2 173.3(2) . . . . ? P2 Ir1 N1 Si2 -14.7(2) . . . . ? C11 Ir1 N1 Si1 102.3(2) . . . . ? P1 Ir1 N1 Si1 33.47(18) . . . . ? P2 Ir1 N1 Si1 -154.60(19) . . . . ? C4 P1 C3 Si1 117.9(3) . . . . ? C8 P1 C3 Si1 -118.6(3) . . . . ? Ir1 P1 C3 Si1 -24.7(3) . . . . ? N1 Si1 C3 P1 47.8(3) . . . . ? C1 Si1 C3 P1 166.5(2) . . . . ? C2 Si1 C3 P1 -69.0(3) . . . . ? C3 P1 C4 C7 -51.9(4) . . . . ? C8 P1 C4 C7 -170.9(4) . . . . ? Ir1 P1 C4 C7 78.4(4) . . . . ? C3 P1 C4 C6 -171.7(4) . . . . ? C8 P1 C4 C6 69.3(5) . . . . ? Ir1 P1 C4 C6 -41.4(5) . . . . ? C3 P1 C4 C5 67.3(4) . . . . ? C8 P1 C4 C5 -51.8(5) . . . . ? Ir1 P1 C4 C5 -162.4(3) . . . . ? C3 P1 C8 C10 -24.0(5) . . . . ? C4 P1 C8 C10 93.0(4) . . . . ? Ir1 P1 C8 C10 -132.2(4) . . . . ? C3 P1 C8 C9 -154.3(4) . . . . ? C4 P1 C8 C9 -37.3(5) . . . . ? Ir1 P1 C8 C9 97.5(4) . . . . ? C3 P1 C8 C11 93.2(3) . . . . ? C4 P1 C8 C11 -149.8(3) . . . . ? Ir1 P1 C8 C11 -15.0(3) . . . . ? C10 C8 C11 Ir1 138.6(4) . . . . ? C9 C8 C11 Ir1 -99.7(4) . . . . ? P1 C8 C11 Ir1 17.4(3) . . . . ? N1 Ir1 C11 C8 -102.2(3) . . . . ? P1 Ir1 C11 C8 -15.2(3) . . . . ? Cl1 Ir1 C11 C8 77.1(3) . . . . ? P2 Ir1 C11 C8 168.4(3) . . . . ? C19 P2 C14 Si2 151.7(3) . . . . ? C15 P2 C14 Si2 -90.1(3) . . . . ? Ir1 P2 C14 Si2 23.4(3) . . . . ? N1 Si2 C14 P2 -32.7(3) . . . . ? C12 Si2 C14 P2 -149.0(3) . . . . ? C13 Si2 C14 P2 91.4(3) . . . . ? C14 P2 C15 C18 -152.8(4) . . . . ? C19 P2 C15 C18 -41.2(5) . . . . ? Ir1 P2 C15 C18 93.9(4) . . . . ? C14 P2 C15 C16 -26.5(5) . . . . ? C19 P2 C15 C16 85.1(5) . . . . ? Ir1 P2 C15 C16 -139.8(4) . . . . ? C14 P2 C15 C17 91.3(4) . . . . ? C19 P2 C15 C17 -157.0(3) . . . . ? Ir1 P2 C15 C17 -21.9(4) . . . . ? C14 P2 C19 C20 -54.9(4) . . . . ? C15 P2 C19 C20 -168.5(3) . . . . ? Ir1 P2 C19 C20 63.7(4) . . . . ? C14 P2 C19 C22 -173.3(4) . . . . ? C15 P2 C19 C22 73.1(4) . . . . ? Ir1 P2 C19 C22 -54.8(4) . . . . ? C14 P2 C19 C21 64.3(4) . . . . ? C15 P2 C19 C21 -49.3(4) . . . . ? Ir1 P2 C19 C21 -177.1(3) . . . . ? O1 S1 C23 F2 -170.1(4) . . . . ? O2 S1 C23 F2 -50.3(5) . . . . ? O3 S1 C23 F2 70.6(5) . . . . ? O1 S1 C23 F1 69.9(4) . . . . ? O2 S1 C23 F1 -170.3(4) . . . . ? O3 S1 C23 F1 -49.4(5) . . . . ? O1 S1 C23 F3 -50.3(5) . . . . ? O2 S1 C23 F3 69.5(5) . . . . ? O3 S1 C23 F3 -169.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O1 0.77(5) 2.33(5) 3.076(6) 161(4) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.462 _refine_diff_density_min -1.320 _refine_diff_density_rms 0.110