data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.50 H34.50 Cl3 Ir O1.50 P S2' _chemical_formula_weight 782.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'O' 'O' 0.0106 0.0060 '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 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 13.1972(7) _cell_length_b 10.2905(5) _cell_length_c 21.7022(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.0332(11) _cell_angle_gamma 90.00 _cell_volume 2935.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6966 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.49 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1546 _exptl_absorpt_coefficient_mu 5.040 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2504 _exptl_absorpt_correction_T_max 0.7867 _exptl_absorpt_process_details ? _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_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20309 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6741 _reflns_number_gt 5593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.2064P] 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 6741 _refine_ls_number_parameters 325 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.759994(9) -0.004468(11) -0.226026(6) 0.01516(5) Uani 1 1 d . . . Cl1 Cl 0.94076(6) -0.01063(8) -0.21882(4) 0.02151(18) Uani 1 1 d . . . Cl2 Cl 0.58078(7) -0.00633(7) -0.23965(4) 0.02172(18) Uani 1 1 d . . . Cl3 Cl 0.76247(6) -0.09747(8) -0.32817(4) 0.02307(18) Uani 1 1 d . . . S1 S 0.75408(6) 0.20457(8) -0.27050(4) 0.02076(19) Uani 1 1 d . . . S2 S 0.75451(7) -0.21582(8) -0.18474(4) 0.02348(19) Uani 1 1 d . . . P1 P 0.76111(6) 0.08652(8) -0.12944(4) 0.01610(18) Uani 1 1 d . . . C1 C 0.8563(3) 0.2217(4) -0.32179(17) 0.0285(8) Uani 1 1 d . . . H1A H 0.8942 0.3035 -0.3128 0.034 Uiso 1 1 calc R . . H1B H 0.9044 0.1480 -0.3160 0.034 Uiso 1 1 calc R . . C2 C 0.8059(3) 0.2232(5) -0.38790(19) 0.0440(11) Uani 1 1 d . . . H2A H 0.8461 0.2768 -0.4148 0.053 Uiso 1 1 calc R . . H2B H 0.8011 0.1339 -0.4049 0.053 Uiso 1 1 calc R . . C3 C 0.7017(3) 0.2799(5) -0.3850(2) 0.0484(12) Uani 1 1 d . . . H3A H 0.6605 0.2672 -0.4250 0.058 Uiso 1 1 calc R . . H3B H 0.7064 0.3742 -0.3763 0.058 Uiso 1 1 calc R . . C4 C 0.6533(3) 0.2103(4) -0.33376(18) 0.0315(9) Uani 1 1 d . . . H4A H 0.6316 0.1216 -0.3468 0.038 Uiso 1 1 calc R . . H4B H 0.5936 0.2589 -0.3214 0.038 Uiso 1 1 calc R . . C5 C 0.6487(3) -0.3063(3) -0.2229(2) 0.0342(10) Uani 1 1 d . . . H5A H 0.5912 -0.3110 -0.1966 0.041 Uiso 1 1 calc R . . H5B H 0.6248 -0.2660 -0.2630 0.041 Uiso 1 1 calc R . . C6 C 0.6936(3) -0.4410(4) -0.2324(3) 0.0456(12) Uani 1 1 d . . . H6A H 0.7015 -0.4890 -0.1927 0.055 Uiso 1 1 calc R . . H6B H 0.6485 -0.4917 -0.2623 0.055 Uiso 1 1 calc R . . C7 C 0.7938(3) -0.4205(4) -0.2564(2) 0.0421(11) Uani 1 1 d . . . H7A H 0.7847 -0.3916 -0.3001 0.051 Uiso 1 1 calc R . . H7B H 0.8330 -0.5027 -0.2545 0.051 Uiso 1 1 calc R . . C8 C 0.8507(3) -0.3171(3) -0.2168(2) 0.0336(10) Uani 1 1 d . . . H8A H 0.8936 -0.2640 -0.2423 0.040 Uiso 1 1 calc R . . H8B H 0.8950 -0.3583 -0.1831 0.040 Uiso 1 1 calc R . . C9 C 0.8141(3) -0.0113(3) -0.06335(17) 0.0197(7) Uani 1 1 d . . . C10 C 0.7784(3) 0.0033(3) -0.00531(19) 0.0269(9) Uani 1 1 d . . . H10 H 0.7239 0.0614 0.0001 0.032 Uiso 1 1 calc R . . C11 C 0.8218(3) -0.0664(4) 0.04438(18) 0.0355(10) Uani 1 1 d . . . H11 H 0.7964 -0.0568 0.0837 0.043 Uiso 1 1 calc R . . C12 C 0.9014(3) -0.1496(4) 0.0377(2) 0.0388(10) Uani 1 1 d . . . H12 H 0.9299 -0.1984 0.0721 0.047 Uiso 1 1 calc R . . C13 C 0.9396(3) -0.1623(4) -0.01894(19) 0.0332(9) Uani 1 1 d . . . H13 H 0.9958 -0.2183 -0.0233 0.040 Uiso 1 1 calc R . . C14 C 0.8965(3) -0.0935(3) -0.06974(17) 0.0258(8) Uani 1 1 d . . . H14 H 0.9232 -0.1024 -0.1088 0.031 Uiso 1 1 calc R . . C15 C 0.8308(2) 0.2397(3) -0.11467(16) 0.0187(7) Uani 1 1 d . . . C16 C 0.9075(2) 0.2806(3) -0.15070(16) 0.0210(7) Uani 1 1 d . . . H16 H 0.9222 0.2314 -0.1859 0.025 Uiso 1 1 calc R . . C17 C 0.9625(3) 0.3929(3) -0.13517(18) 0.0285(8) Uani 1 1 d . . . H17 H 1.0140 0.4209 -0.1601 0.034 Uiso 1 1 calc R . . C18 C 0.9427(3) 0.4640(4) -0.0837(2) 0.0346(10) Uani 1 1 d . . . H18 H 0.9811 0.5400 -0.0730 0.041 Uiso 1 1 calc R . . C19 C 0.8673(3) 0.4250(4) -0.04807(19) 0.0361(10) Uani 1 1 d . . . H19 H 0.8529 0.4751 -0.0131 0.043 Uiso 1 1 calc R . . C20 C 0.8120(3) 0.3126(3) -0.06277(17) 0.0267(8) Uani 1 1 d . . . H20 H 0.7610 0.2853 -0.0373 0.032 Uiso 1 1 calc R . . C21 C 0.6333(2) 0.1278(3) -0.11176(15) 0.0190(7) Uani 1 1 d . . . C22 C 0.5706(3) 0.0369(4) -0.08710(18) 0.0258(8) Uani 1 1 d . . . H22 H 0.5966 -0.0464 -0.0755 0.031 Uiso 1 1 calc R . . C23 C 0.4706(3) 0.0668(5) -0.07936(18) 0.0351(10) Uani 1 1 d . . . H23 H 0.4289 0.0051 -0.0611 0.042 Uiso 1 1 calc R . . C24 C 0.4306(3) 0.1868(4) -0.09822(19) 0.0371(10) Uani 1 1 d . . . H24 H 0.3618 0.2071 -0.0928 0.045 Uiso 1 1 calc R . . C25 C 0.4909(3) 0.2757(4) -0.12466(18) 0.0341(9) Uani 1 1 d . . . H25 H 0.4631 0.3567 -0.1387 0.041 Uiso 1 1 calc R . . C26 C 0.5918(3) 0.2480(4) -0.13103(17) 0.0251(8) Uani 1 1 d . . . H26 H 0.6334 0.3109 -0.1486 0.030 Uiso 1 1 calc R . . O1 O 0.5015(7) 0.6795(9) -0.0517(5) 0.096(3) Uiso 0.50 1 d P A 1 O2 O 0.5276(6) 0.5059(8) 0.0086(4) 0.057(2) Uiso 0.50 1 d PD . 1 C27 C 0.5571(10) 0.6059(12) -0.0234(6) 0.065(3) Uiso 0.50 1 d PD . 1 C28 C 0.6704(8) 0.6257(12) -0.0204(6) 0.067(3) Uiso 0.50 1 d P B 1 H28A H 0.7001 0.5630 -0.0476 0.101 Uiso 0.50 1 calc PR B 1 H28B H 0.6999 0.6128 0.0222 0.101 Uiso 0.50 1 calc PR B 1 H28C H 0.6850 0.7142 -0.0338 0.101 Uiso 0.50 1 calc PR B 1 O3 O 0.5797(11) 0.5130(12) -0.0074(7) 0.120(5) Uiso 0.50 1 d PD C 2 H3 H 0.6313 0.4648 -0.0036 0.180 Uiso 0.50 1 calc PR C 2 C29 C 0.5977(11) 0.6225(13) -0.0505(6) 0.081(4) Uiso 0.50 1 d PD C 2 H29A H 0.5664 0.7020 -0.0361 0.121 Uiso 0.50 1 calc PR C 2 H29B H 0.5675 0.6012 -0.0922 0.121 Uiso 0.50 1 calc PR C 2 H29C H 0.6710 0.6361 -0.0516 0.121 Uiso 0.50 1 calc PR C 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 Ir 0.01451(8) 0.01491(8) 0.01609(8) -0.00026(5) 0.00144(5) 0.00038(5) Cl1 0.0160(4) 0.0237(4) 0.0251(5) -0.0012(3) 0.0030(3) 0.0014(3) Cl2 0.0160(4) 0.0251(4) 0.0239(5) -0.0022(3) 0.0004(3) 0.0003(3) Cl3 0.0235(4) 0.0249(4) 0.0208(4) -0.0047(4) 0.0018(3) -0.0011(3) S1 0.0232(4) 0.0181(4) 0.0211(5) 0.0024(3) 0.0020(4) 0.0011(3) S2 0.0305(5) 0.0174(4) 0.0225(5) 0.0009(4) 0.0016(4) -0.0021(4) P1 0.0169(4) 0.0147(4) 0.0167(4) 0.0001(3) 0.0020(3) 0.0012(3) C1 0.028(2) 0.027(2) 0.032(2) 0.0068(17) 0.0079(16) -0.0008(15) C2 0.050(3) 0.056(3) 0.027(2) 0.015(2) 0.011(2) -0.001(2) C3 0.047(3) 0.067(3) 0.030(2) 0.029(2) -0.003(2) -0.004(2) C4 0.027(2) 0.036(2) 0.030(2) 0.0118(18) -0.0039(16) 0.0043(17) C5 0.0244(19) 0.0219(19) 0.056(3) -0.0064(19) 0.0032(19) -0.0043(15) C6 0.033(2) 0.022(2) 0.082(4) -0.015(2) 0.003(2) -0.0046(17) C7 0.038(2) 0.028(2) 0.060(3) -0.014(2) 0.005(2) 0.0024(18) C8 0.0235(19) 0.0166(18) 0.060(3) 0.0031(18) -0.0011(19) 0.0064(14) C9 0.0206(17) 0.0175(17) 0.0203(18) 0.0045(14) -0.0014(14) -0.0002(12) C10 0.031(2) 0.028(2) 0.022(2) -0.0004(15) -0.0011(16) 0.0030(15) C11 0.043(2) 0.044(2) 0.020(2) 0.0093(19) 0.0024(18) 0.0029(19) C12 0.046(3) 0.036(2) 0.031(2) 0.0139(19) -0.010(2) 0.0068(19) C13 0.031(2) 0.035(2) 0.032(2) 0.0043(18) -0.0061(18) 0.0081(17) C14 0.0262(19) 0.0255(18) 0.026(2) -0.0013(16) 0.0022(15) 0.0039(15) C15 0.0235(17) 0.0142(15) 0.0179(17) 0.0002(13) -0.0006(14) -0.0012(13) C16 0.0218(17) 0.0221(18) 0.0190(17) 0.0036(14) 0.0007(14) -0.0014(14) C17 0.029(2) 0.0249(19) 0.030(2) 0.0094(17) -0.0043(16) -0.0083(15) C18 0.046(3) 0.0217(18) 0.034(2) 0.0014(18) -0.009(2) -0.0126(18) C19 0.055(3) 0.0226(19) 0.030(2) -0.0088(17) -0.003(2) -0.0049(18) C20 0.037(2) 0.0229(18) 0.0204(19) -0.0032(15) 0.0036(16) -0.0018(15) C21 0.0197(17) 0.0215(17) 0.0160(17) -0.0016(14) 0.0026(13) 0.0032(13) C22 0.0258(19) 0.0259(18) 0.026(2) 0.0050(16) 0.0010(16) -0.0014(15) C23 0.0214(19) 0.055(3) 0.030(2) 0.009(2) 0.0068(17) -0.0037(18) C24 0.022(2) 0.059(3) 0.030(2) 0.000(2) 0.0036(17) 0.0123(19) C25 0.034(2) 0.039(2) 0.030(2) 0.0031(19) 0.0043(17) 0.0164(18) C26 0.0252(18) 0.0275(19) 0.0230(19) 0.0028(16) 0.0042(15) 0.0069(15) _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 Ir P1 2.2946(9) . ? Ir S2 2.3557(9) . ? Ir S1 2.3562(9) . ? Ir Cl2 2.3577(9) . ? Ir Cl1 2.3779(9) . ? Ir Cl3 2.4174(8) . ? S1 C4 1.827(4) . ? S1 C1 1.831(4) . ? S2 C5 1.817(4) . ? S2 C8 1.827(4) . ? P1 C21 1.812(3) . ? P1 C15 1.839(3) . ? P1 C9 1.840(3) . ? C1 C2 1.528(5) . ? C2 C3 1.501(6) . ? C3 C4 1.511(6) . ? C5 C6 1.528(5) . ? C6 C7 1.479(6) . ? C7 C8 1.523(5) . ? C9 C10 1.391(6) . ? C9 C14 1.394(5) . ? C10 C11 1.377(5) . ? C11 C12 1.372(6) . ? C12 C13 1.375(6) . ? C13 C14 1.390(5) . ? C15 C20 1.394(5) . ? C15 C16 1.397(5) . ? C16 C17 1.391(5) . ? C17 C18 1.379(6) . ? C18 C19 1.373(6) . ? C19 C20 1.390(5) . ? C21 C22 1.387(5) . ? C21 C26 1.402(5) . ? C22 C23 1.379(5) . ? C23 C24 1.391(6) . ? C24 C25 1.370(6) . ? C25 C26 1.381(5) . ? O1 C27 1.188(14) . ? O2 O2 0.798(14) 3_665 ? O2 C27 1.319(13) . ? O2 C27 1.654(16) 3_665 ? C27 C28 1.506(16) . ? C27 O2 1.654(16) 3_665 ? O3 C29 1.497(14) . ? 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 Ir S2 91.56(3) . . ? P1 Ir S1 89.94(3) . . ? S2 Ir S1 176.07(3) . . ? P1 Ir Cl2 92.51(3) . . ? S2 Ir Cl2 88.64(3) . . ? S1 Ir Cl2 87.66(3) . . ? P1 Ir Cl1 91.42(3) . . ? S2 Ir Cl1 90.83(3) . . ? S1 Ir Cl1 92.77(3) . . ? Cl2 Ir Cl1 176.04(3) . . ? P1 Ir Cl3 178.63(3) . . ? S2 Ir Cl3 89.23(3) . . ? S1 Ir Cl3 89.34(3) . . ? Cl2 Ir Cl3 88.62(3) . . ? Cl1 Ir Cl3 87.45(3) . . ? C4 S1 C1 93.82(18) . . ? C4 S1 Ir 109.46(13) . . ? C1 S1 Ir 109.69(12) . . ? C5 S2 C8 93.78(18) . . ? C5 S2 Ir 110.34(14) . . ? C8 S2 Ir 109.67(13) . . ? C21 P1 C15 102.87(15) . . ? C21 P1 C9 105.10(16) . . ? C15 P1 C9 100.54(15) . . ? C21 P1 Ir 110.95(11) . . ? C15 P1 Ir 118.17(12) . . ? C9 P1 Ir 117.42(12) . . ? C2 C1 S1 106.8(3) . . ? C3 C2 C1 106.9(3) . . ? C2 C3 C4 107.1(3) . . ? C3 C4 S1 104.0(3) . . ? C6 C5 S2 103.5(3) . . ? C7 C6 C5 106.7(3) . . ? C6 C7 C8 108.2(4) . . ? C7 C8 S2 106.8(3) . . ? C10 C9 C14 119.0(3) . . ? C10 C9 P1 120.7(3) . . ? C14 C9 P1 120.1(3) . . ? C11 C10 C9 120.1(4) . . ? C12 C11 C10 120.8(4) . . ? C11 C12 C13 119.9(4) . . ? C12 C13 C14 120.2(4) . . ? C13 C14 C9 119.9(4) . . ? C20 C15 C16 118.7(3) . . ? C20 C15 P1 118.7(3) . . ? C16 C15 P1 122.4(3) . . ? C17 C16 C15 120.2(3) . . ? C18 C17 C16 120.3(4) . . ? C19 C18 C17 120.0(4) . . ? C18 C19 C20 120.4(4) . . ? C19 C20 C15 120.4(4) . . ? C22 C21 C26 118.6(3) . . ? C22 C21 P1 121.4(3) . . ? C26 C21 P1 119.4(3) . . ? C23 C22 C21 120.4(4) . . ? C22 C23 C24 120.3(4) . . ? C25 C24 C23 119.8(4) . . ? C24 C25 C26 120.3(4) . . ? C25 C26 C21 120.5(4) . . ? O2 O2 C27 99.8(15) 3_665 . ? O2 O2 C27 51.8(11) 3_665 3_665 ? C27 O2 C27 151.6(6) . 3_665 ? O1 C27 O2 125.0(12) . . ? O1 C27 C28 120.1(12) . . ? O2 C27 C28 114.9(11) . . ? O1 C27 O2 98.5(10) . 3_665 ? O2 C27 O2 28.4(6) . 3_665 ? C28 C27 O2 140.5(10) . 3_665 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.475 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.137 data_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 Cl2 F2 Ir N P S' _chemical_formula_weight 803.70 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' 'F' 'F' 0.0171 0.0103 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.6610(8) _cell_length_b 13.0231(10) _cell_length_c 21.6671(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3008.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2650 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 24.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 4.776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3814 _exptl_absorpt_correction_T_max 0.4484 _exptl_absorpt_process_details ? _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_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17246 _diffrn_reflns_av_R_equivalents 0.0524 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6851 _reflns_number_gt 5949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+46.4916P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.030(16) _refine_ls_number_reflns 6851 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1580 _refine_ls_wR_factor_gt 0.1508 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 Ir Ir 0.74703(5) -0.01176(3) 0.349676(18) 0.02051(12) Uani 1 1 d . . . Cl1 Cl 0.6904(3) 0.1345(2) 0.28119(15) 0.0297(7) Uani 1 1 d . . . Cl2 Cl 0.5777(3) 0.0221(3) 0.41807(15) 0.0278(6) Uani 1 1 d . . . S1 S 0.6185(3) -0.1092(3) 0.27956(16) 0.0293(7) Uani 1 1 d . . . P1 P 0.8705(3) 0.0894(2) 0.41248(14) 0.0185(6) Uani 1 1 d . . . N1 N 0.8954(10) -0.0564(9) 0.2925(5) 0.028(2) Uani 1 1 d . . . C1 C 0.8039(12) -0.1344(9) 0.3951(6) 0.023(3) Uani 1 1 d . . . C2 C 0.7511(18) -0.1814(8) 0.4462(6) 0.036(3) Uani 1 1 d . . . H2 H 0.6766 -0.1532 0.4632 0.043 Uiso 1 1 calc R . . C3 C 0.8016(16) -0.2663(12) 0.4730(7) 0.045(4) Uani 1 1 d . . . C4 C 0.9113(15) -0.3120(9) 0.4517(7) 0.036(3) Uani 1 1 d . . . H4 H 0.9478 -0.3696 0.4717 0.043 Uiso 1 1 calc R . . C5 C 0.9628(15) -0.2692(11) 0.4005(8) 0.043(4) Uani 1 1 d . . . C6 C 0.9165(12) -0.1834(10) 0.3700(7) 0.030(3) Uani 1 1 d . . . C7 C 0.9617(11) -0.1384(10) 0.3132(6) 0.026(3) Uani 1 1 d . . . C8 C 1.0620(12) -0.1724(12) 0.2755(7) 0.038(4) Uani 1 1 d . . . H8 H 1.1133 -0.2282 0.2880 0.046 Uiso 1 1 calc R . . C9 C 1.0836(13) -0.1241(14) 0.2213(8) 0.045(4) Uani 1 1 d . . . H9 H 1.1524 -0.1461 0.1968 0.054 Uiso 1 1 calc R . . C10 C 1.0132(14) -0.0479(13) 0.2009(7) 0.042(4) Uani 1 1 d . . . H10 H 1.0290 -0.0171 0.1619 0.050 Uiso 1 1 calc R . . C11 C 0.9160(13) -0.0139(12) 0.2379(6) 0.035(3) Uani 1 1 d . . . H11 H 0.8635 0.0403 0.2239 0.042 Uiso 1 1 calc R . . C12 C 0.4679(13) -0.0394(11) 0.2720(8) 0.041(4) Uani 1 1 d . . . H12A H 0.4661 0.0213 0.2995 0.049 Uiso 1 1 calc R . . H12B H 0.4545 -0.0165 0.2290 0.049 Uiso 1 1 calc R . . C13 C 0.3712(15) -0.1154(14) 0.2906(11) 0.061(5) Uani 1 1 d . . . H13A H 0.2960 -0.0789 0.3060 0.074 Uiso 1 1 calc R . . H13B H 0.3462 -0.1568 0.2543 0.074 Uiso 1 1 calc R . . C14 C 0.4200(15) -0.1834(14) 0.3391(8) 0.049(4) Uani 1 1 d . . . H14A H 0.3635 -0.2429 0.3452 0.059 Uiso 1 1 calc R . . H14B H 0.4278 -0.1460 0.3787 0.059 Uiso 1 1 calc R . . C15 C 0.5486(16) -0.2191(12) 0.3166(7) 0.043(4) Uani 1 1 d . . . H15A H 0.5397 -0.2766 0.2870 0.051 Uiso 1 1 calc R . . H15B H 0.6008 -0.2423 0.3517 0.051 Uiso 1 1 calc R . . C16 C 0.8244(11) 0.2241(9) 0.4214(5) 0.019(2) Uani 1 1 d . . . C17 C 0.7027(12) 0.2578(10) 0.4072(6) 0.026(3) Uani 1 1 d . . . H17 H 0.6406 0.2105 0.3937 0.031 Uiso 1 1 calc R . . C18 C 0.6741(12) 0.3639(9) 0.4132(6) 0.025(3) Uani 1 1 d . . . H18 H 0.5920 0.3883 0.4044 0.030 Uiso 1 1 calc R . . C19 C 0.7672(13) 0.4320(9) 0.4323(6) 0.029(3) Uani 1 1 d . . . H19 H 0.7486 0.5032 0.4349 0.035 Uiso 1 1 calc R . . C20 C 0.8846(12) 0.3984(11) 0.4474(6) 0.030(3) Uani 1 1 d . . . H20 H 0.9469 0.4451 0.4614 0.036 Uiso 1 1 calc R . . C21 C 0.9109(13) 0.2946(9) 0.4419(6) 0.028(3) Uani 1 1 d . . . H21 H 0.9923 0.2711 0.4527 0.034 Uiso 1 1 calc R . . C22 C 1.0323(11) 0.1045(9) 0.3844(6) 0.023(2) Uani 1 1 d . . . C23 C 1.0427(12) 0.1452(10) 0.3259(6) 0.027(3) Uani 1 1 d . . . H23 H 0.9703 0.1550 0.3010 0.032 Uiso 1 1 calc R . . C24 C 1.1612(12) 0.1717(10) 0.3039(6) 0.029(3) Uani 1 1 d . . . H24 H 1.1691 0.2014 0.2641 0.035 Uiso 1 1 calc R . . C25 C 1.2664(15) 0.1556(11) 0.3388(6) 0.037(3) Uani 1 1 d . . . H25 H 1.3474 0.1712 0.3230 0.045 Uiso 1 1 calc R . . C26 C 1.2520(16) 0.1164(10) 0.3967(5) 0.035(3) Uani 1 1 d . . . H26 H 1.3246 0.1076 0.4216 0.043 Uiso 1 1 calc R . . C27 C 1.1378(12) 0.0891(11) 0.4208(7) 0.033(3) Uani 1 1 d . . . H27 H 1.1312 0.0606 0.4611 0.040 Uiso 1 1 calc R . . C28 C 0.8786(11) 0.0454(8) 0.4921(5) 0.020(2) Uani 1 1 d . . . C29 C 0.8078(13) 0.0934(10) 0.5373(6) 0.028(3) Uani 1 1 d . . . H29 H 0.7594 0.1522 0.5271 0.034 Uiso 1 1 calc R . . C30 C 0.8068(15) 0.0563(11) 0.5975(7) 0.038(3) Uani 1 1 d . . . H30 H 0.7587 0.0900 0.6283 0.045 Uiso 1 1 calc R . . C31 C 0.8776(15) -0.0319(12) 0.6125(6) 0.041(4) Uani 1 1 d . . . H31 H 0.8763 -0.0594 0.6531 0.049 Uiso 1 1 calc R . . C32 C 0.9473(14) -0.0760(11) 0.5677(6) 0.035(3) Uani 1 1 d . . . H32 H 0.9972 -0.1341 0.5778 0.042 Uiso 1 1 calc R . . C33 C 0.9486(13) -0.0406(10) 0.5094(6) 0.032(3) Uani 1 1 d . . . H33 H 0.9981 -0.0748 0.4793 0.038 Uiso 1 1 calc R . . F1 F 0.7476(12) -0.3085(6) 0.5234(4) 0.055(2) Uani 1 1 d . . . F2 F 1.0693(8) -0.3159(7) 0.3776(5) 0.051(2) 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 Ir 0.01508(19) 0.02141(19) 0.0250(2) -0.00483(15) -0.0022(2) 0.0030(2) Cl1 0.0289(16) 0.0313(16) 0.0288(15) 0.0009(13) -0.0035(13) 0.0008(13) Cl2 0.0146(12) 0.0314(15) 0.0376(15) -0.0047(14) 0.0020(12) 0.0045(12) S1 0.0206(16) 0.0308(17) 0.0365(17) -0.0084(15) 0.0003(14) -0.0039(14) P1 0.0143(14) 0.0176(14) 0.0235(14) -0.0027(12) 0.0006(12) 0.0028(11) N1 0.019(5) 0.035(6) 0.029(6) -0.006(5) 0.000(4) 0.005(5) C1 0.026(6) 0.015(5) 0.029(6) -0.002(5) -0.010(5) 0.005(5) C2 0.034(7) 0.025(5) 0.049(7) -0.008(5) -0.013(9) 0.007(9) C3 0.054(10) 0.033(7) 0.047(9) 0.007(7) -0.008(7) -0.018(7) C4 0.052(9) 0.009(5) 0.046(8) 0.001(5) -0.015(7) 0.012(6) C5 0.039(9) 0.022(6) 0.067(11) -0.002(7) -0.017(8) 0.010(6) C6 0.015(6) 0.028(7) 0.047(8) -0.016(6) -0.006(6) 0.000(5) C7 0.014(6) 0.025(6) 0.038(7) -0.005(5) -0.002(5) 0.003(5) C8 0.015(6) 0.045(8) 0.055(9) -0.018(7) -0.016(6) 0.006(6) C9 0.017(7) 0.066(11) 0.052(9) -0.014(8) 0.005(7) 0.011(7) C10 0.035(8) 0.056(10) 0.034(7) -0.012(7) 0.001(6) -0.010(7) C11 0.030(7) 0.040(8) 0.033(7) -0.011(6) 0.001(5) -0.004(6) C12 0.029(7) 0.036(8) 0.057(9) 0.003(7) -0.008(7) 0.004(6) C13 0.023(8) 0.051(10) 0.110(16) -0.025(11) -0.007(10) -0.008(8) C14 0.034(9) 0.052(10) 0.061(11) -0.004(8) 0.024(8) -0.008(7) C15 0.050(10) 0.035(8) 0.044(9) 0.012(7) -0.010(8) 0.003(7) C16 0.021(6) 0.023(6) 0.012(5) 0.002(5) 0.005(5) 0.000(5) C17 0.028(7) 0.024(6) 0.024(6) 0.001(5) -0.004(5) 0.006(5) C18 0.024(6) 0.024(6) 0.027(6) 0.006(5) -0.002(5) 0.006(5) C19 0.027(7) 0.018(5) 0.042(7) 0.001(4) 0.008(6) 0.004(5) C20 0.025(7) 0.043(8) 0.023(6) -0.008(6) 0.008(5) 0.000(6) C21 0.031(7) 0.017(6) 0.038(7) 0.000(5) 0.009(6) 0.003(5) C22 0.015(6) 0.017(5) 0.036(7) -0.007(5) -0.004(5) 0.006(5) C23 0.020(6) 0.029(7) 0.032(6) 0.000(5) 0.002(5) 0.007(5) C24 0.022(7) 0.032(7) 0.033(7) 0.004(5) 0.010(6) 0.008(5) C25 0.023(8) 0.049(7) 0.040(7) 0.001(6) 0.008(7) 0.004(7) C26 0.019(6) 0.058(7) 0.029(6) -0.001(5) -0.007(7) -0.003(10) C27 0.022(7) 0.036(7) 0.041(8) 0.001(6) -0.007(6) 0.002(6) C28 0.023(6) 0.013(5) 0.025(6) -0.002(4) 0.004(5) 0.006(4) C29 0.030(7) 0.025(6) 0.030(7) 0.000(5) -0.003(5) 0.000(5) C30 0.040(8) 0.037(8) 0.037(8) -0.001(6) 0.015(6) -0.010(6) C31 0.052(9) 0.043(8) 0.027(7) 0.019(6) -0.005(6) -0.021(8) C32 0.038(8) 0.032(7) 0.036(8) 0.004(6) -0.007(6) -0.008(6) C33 0.034(7) 0.025(7) 0.036(7) -0.008(5) -0.010(6) 0.002(6) F1 0.062(6) 0.052(5) 0.051(5) 0.021(4) -0.021(6) -0.008(8) F2 0.036(5) 0.040(5) 0.078(7) -0.004(5) -0.012(5) 0.022(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 Ir C1 1.972(12) . ? Ir N1 2.091(10) . ? Ir P1 2.306(3) . ? Ir Cl2 2.377(3) . ? Ir S1 2.407(3) . ? Ir Cl1 2.489(3) . ? S1 C15 1.803(16) . ? S1 C12 1.852(14) . ? P1 C28 1.820(12) . ? P1 C16 1.832(13) . ? P1 C22 1.840(13) . ? N1 C11 1.326(17) . ? N1 C7 1.358(16) . ? C1 C2 1.384(19) . ? C1 C6 1.464(18) . ? C2 C3 1.36(2) . ? C3 F1 1.352(18) . ? C3 C4 1.39(2) . ? C4 C5 1.36(2) . ? C5 F2 1.381(18) . ? C5 C6 1.39(2) . ? C6 C7 1.445(19) . ? C7 C8 1.417(19) . ? C8 C9 1.35(2) . ? C9 C10 1.32(2) . ? C10 C11 1.382(19) . ? C12 C13 1.48(2) . ? C13 C14 1.47(3) . ? C14 C15 1.53(2) . ? C16 C21 1.375(18) . ? C16 C17 1.404(17) . ? C17 C18 1.422(17) . ? C18 C19 1.394(18) . ? C19 C20 1.366(19) . ? C20 C21 1.386(18) . ? C22 C23 1.377(18) . ? C22 C27 1.390(17) . ? C23 C24 1.394(18) . ? C24 C25 1.368(19) . ? C25 C26 1.364(17) . ? C26 C27 1.37(2) . ? C28 C29 1.386(17) . ? C28 C33 1.396(17) . ? C29 C30 1.391(19) . ? C30 C31 1.41(2) . ? C31 C32 1.35(2) . ? C32 C33 1.346(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 C1 Ir N1 80.7(5) . . ? C1 Ir P1 89.6(3) . . ? N1 Ir P1 94.4(3) . . ? C1 Ir Cl2 94.2(4) . . ? N1 Ir Cl2 174.4(3) . . ? P1 Ir Cl2 87.68(11) . . ? C1 Ir S1 93.6(3) . . ? N1 Ir S1 84.9(3) . . ? P1 Ir S1 176.55(12) . . ? Cl2 Ir S1 93.39(11) . . ? C1 Ir Cl1 172.8(4) . . ? N1 Ir Cl1 92.5(3) . . ? P1 Ir Cl1 93.05(11) . . ? Cl2 Ir Cl1 92.60(11) . . ? S1 Ir Cl1 83.62(11) . . ? C15 S1 C12 94.0(7) . . ? C15 S1 Ir 111.9(6) . . ? C12 S1 Ir 106.9(5) . . ? C28 P1 C16 102.4(5) . . ? C28 P1 C22 107.6(6) . . ? C16 P1 C22 100.6(5) . . ? C28 P1 Ir 114.0(4) . . ? C16 P1 Ir 117.1(4) . . ? C22 P1 Ir 113.6(4) . . ? C11 N1 C7 122.5(12) . . ? C11 N1 Ir 122.6(9) . . ? C7 N1 Ir 114.7(9) . . ? C2 C1 C6 115.9(12) . . ? C2 C1 Ir 129.2(10) . . ? C6 C1 Ir 114.8(9) . . ? C3 C2 C1 122.7(16) . . ? F1 C3 C2 120.5(16) . . ? F1 C3 C4 116.9(14) . . ? C2 C3 C4 122.6(15) . . ? C5 C4 C3 115.8(13) . . ? C4 C5 F2 116.5(13) . . ? C4 C5 C6 125.2(15) . . ? F2 C5 C6 118.3(15) . . ? C5 C6 C7 127.8(13) . . ? C5 C6 C1 117.7(14) . . ? C7 C6 C1 114.4(12) . . ? N1 C7 C8 116.6(13) . . ? N1 C7 C6 115.2(11) . . ? C8 C7 C6 128.1(13) . . ? C9 C8 C7 119.1(14) . . ? C10 C9 C8 122.9(14) . . ? C9 C10 C11 118.3(15) . . ? N1 C11 C10 120.5(14) . . ? C13 C12 S1 104.5(11) . . ? C14 C13 C12 110.5(14) . . ? C13 C14 C15 105.8(13) . . ? C14 C15 S1 105.8(11) . . ? C21 C16 C17 118.8(11) . . ? C21 C16 P1 119.6(9) . . ? C17 C16 P1 121.6(10) . . ? C16 C17 C18 118.8(12) . . ? C19 C18 C17 119.5(11) . . ? C20 C19 C18 121.3(11) . . ? C19 C20 C21 118.5(13) . . ? C16 C21 C20 123.0(13) . . ? C23 C22 C27 120.9(12) . . ? C23 C22 P1 114.9(9) . . ? C27 C22 P1 123.7(11) . . ? C22 C23 C24 118.8(12) . . ? C25 C24 C23 121.1(13) . . ? C26 C25 C24 118.2(15) . . ? C25 C26 C27 123.3(15) . . ? C26 C27 C22 117.6(13) . . ? C29 C28 C33 117.6(11) . . ? C29 C28 P1 120.1(9) . . ? C33 C28 P1 122.1(9) . . ? C28 C29 C30 120.7(13) . . ? C29 C30 C31 119.6(13) . . ? C32 C31 C30 118.4(13) . . ? C33 C32 C31 122.3(14) . . ? C32 C33 C28 121.4(13) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 9.205 _refine_diff_density_min -3.713 _refine_diff_density_rms 0.239 data_8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H82 Cl4 Ir2 P4 S2' _chemical_formula_weight 1805.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 43.3581(17) _cell_length_b 8.8949(3) _cell_length_c 19.2344(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.151(2) _cell_angle_gamma 90.00 _cell_volume 7223.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6069 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 4.022 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3989 _exptl_absorpt_correction_T_max 0.4329 _exptl_absorpt_process_details ? _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_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27074 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -56 _diffrn_reflns_limit_h_max 56 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8308 _reflns_number_gt 7696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+10.3881P] 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 8308 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.012 _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 Ir Ir 0.603572(2) 0.527266(13) 0.579310(6) 0.01427(4) Uani 1 1 d . . . Cl1 Cl 0.626074(17) 0.40963(9) 0.48667(4) 0.02188(15) Uani 1 1 d . . . Cl2 Cl 0.601041(17) 0.27470(8) 0.62663(4) 0.02184(15) Uani 1 1 d . . . S1 S 0.550195(18) 0.49515(9) 0.50547(4) 0.02024(16) Uani 1 1 d . . . P1 P 0.604700(17) 0.75607(9) 0.53102(4) 0.01522(15) Uani 1 1 d . . . P2 P 0.649080(17) 0.56593(9) 0.66722(4) 0.01623(15) Uani 1 1 d . . . C1 C 0.57809(7) 0.6358(4) 0.64282(15) 0.0193(6) Uani 1 1 d . . . C2 C 0.56258(8) 0.5592(4) 0.68862(17) 0.0248(7) Uani 1 1 d . . . H2 H 0.5651 0.4534 0.6937 0.030 Uiso 1 1 calc R . . C3 C 0.54370(9) 0.6339(5) 0.7267(2) 0.0362(9) Uani 1 1 d . . . H3 H 0.5332 0.5788 0.7569 0.043 Uiso 1 1 calc R . . C4 C 0.53998(9) 0.7880(5) 0.7210(2) 0.0388(9) Uani 1 1 d . . . H4 H 0.5276 0.8396 0.7483 0.047 Uiso 1 1 calc R . . C5 C 0.55448(8) 0.8658(4) 0.67534(18) 0.0288(7) Uani 1 1 d . . . H5 H 0.5516 0.9715 0.6703 0.035 Uiso 1 1 calc R . . C6 C 0.57325(7) 0.7916(4) 0.63650(15) 0.0201(6) Uani 1 1 d . . . C7 C 0.59001(7) 0.8844(3) 0.58998(16) 0.0204(6) Uani 1 1 d . . . H7A H 0.6078 0.9406 0.6201 0.024 Uiso 1 1 calc R . . H7B H 0.5751 0.9575 0.5615 0.024 Uiso 1 1 calc R . . C8 C 0.64057(7) 0.8405(3) 0.51477(15) 0.0173(6) Uani 1 1 d . . . C9 C 0.66529(7) 0.7530(4) 0.50120(16) 0.0219(6) Uani 1 1 d . . . H9 H 0.6653 0.6471 0.5077 0.026 Uiso 1 1 calc R . . C10 C 0.68984(7) 0.8227(4) 0.47815(18) 0.0262(7) Uani 1 1 d . . . H10 H 0.7069 0.7643 0.4696 0.031 Uiso 1 1 calc R . . C11 C 0.68959(8) 0.9755(4) 0.46762(18) 0.0262(7) Uani 1 1 d . . . H11 H 0.7062 1.0215 0.4503 0.031 Uiso 1 1 calc R . . C12 C 0.66531(8) 1.0628(4) 0.48204(17) 0.0244(7) Uani 1 1 d . . . H12 H 0.6654 1.1686 0.4754 0.029 Uiso 1 1 calc R . . C13 C 0.64103(8) 0.9954(3) 0.50609(17) 0.0215(7) Uani 1 1 d . . . H13 H 0.6246 1.0553 0.5168 0.026 Uiso 1 1 calc R . . C14 C 0.57916(7) 0.7796(3) 0.44194(15) 0.0182(6) Uani 1 1 d . . . C15 C 0.59151(8) 0.7522(4) 0.38199(17) 0.0251(7) Uani 1 1 d . . . H15 H 0.6128 0.7199 0.3878 0.030 Uiso 1 1 calc R . . C16 C 0.57263(9) 0.7722(4) 0.31412(18) 0.0327(8) Uani 1 1 d . . . H16 H 0.5812 0.7557 0.2734 0.039 Uiso 1 1 calc R . . C17 C 0.54152(9) 0.8159(5) 0.30554(19) 0.0381(9) Uani 1 1 d . . . H17 H 0.5286 0.8288 0.2589 0.046 Uiso 1 1 calc R . . C18 C 0.52887(8) 0.8412(5) 0.3643(2) 0.0378(9) Uani 1 1 d . . . H18 H 0.5073 0.8704 0.3580 0.045 Uiso 1 1 calc R . . C19 C 0.54770(7) 0.8238(4) 0.43268(18) 0.0260(7) Uani 1 1 d . . . H19 H 0.5391 0.8421 0.4731 0.031 Uiso 1 1 calc R . . C20 C 0.70723(7) 0.4013(4) 0.80901(16) 0.0233(7) Uani 1 1 d . . . H20 H 0.7097 0.3423 0.7695 0.028 Uiso 1 1 calc R . . C21 C 0.73275(8) 0.4222(4) 0.86632(18) 0.0290(7) Uani 1 1 d . . . H21 H 0.7527 0.3795 0.8654 0.035 Uiso 1 1 calc R . . C22 C 0.72926(8) 0.5048(4) 0.92467(18) 0.0274(8) Uani 1 1 d . . . H22 H 0.7469 0.5199 0.9637 0.033 Uiso 1 1 calc R . . C23 C 0.70023(8) 0.5653(4) 0.92631(17) 0.0279(7) Uani 1 1 d . . . H23 H 0.6976 0.6201 0.9670 0.033 Uiso 1 1 calc R . . C24 C 0.67479(8) 0.5464(4) 0.86868(17) 0.0230(7) Uani 1 1 d . . . H24 H 0.6549 0.5891 0.8702 0.028 Uiso 1 1 calc R . . C25 C 0.67789(7) 0.4660(3) 0.80866(16) 0.0188(6) Uani 1 1 d . . . C26 C 0.64994(7) 0.4460(3) 0.74652(16) 0.0194(6) Uani 1 1 d . . . H26A H 0.6304 0.4655 0.7635 0.023 Uiso 1 1 calc R . . H26B H 0.6493 0.3395 0.7312 0.023 Uiso 1 1 calc R . . C27 C 0.68702(7) 0.5086(4) 0.64931(17) 0.0196(6) Uani 1 1 d . . . C28 C 0.68761(7) 0.3660(4) 0.61978(16) 0.0222(7) Uani 1 1 d . . . H28 H 0.6683 0.3132 0.6025 0.027 Uiso 1 1 calc R . . C29 C 0.71622(8) 0.3004(4) 0.61552(17) 0.0277(7) Uani 1 1 d . . . H29 H 0.7164 0.2024 0.5959 0.033 Uiso 1 1 calc R . . C30 C 0.74426(8) 0.3763(4) 0.63946(19) 0.0337(8) Uani 1 1 d . . . H30 H 0.7637 0.3306 0.6365 0.040 Uiso 1 1 calc R . . C31 C 0.74411(8) 0.5184(4) 0.6676(2) 0.0347(9) Uani 1 1 d . . . H31 H 0.7634 0.5721 0.6829 0.042 Uiso 1 1 calc R . . C32 C 0.71562(7) 0.5836(4) 0.67374(19) 0.0276(7) Uani 1 1 d . . . H32 H 0.7157 0.6803 0.6948 0.033 Uiso 1 1 calc R . . C33 C 0.65358(7) 0.7540(3) 0.70557(16) 0.0195(6) Uani 1 1 d . . . C34 C 0.63660(8) 0.7875(4) 0.75732(16) 0.0247(7) Uani 1 1 d . . . H34 H 0.6233 0.7131 0.7706 0.030 Uiso 1 1 calc R . . C35 C 0.63890(9) 0.9271(4) 0.78938(18) 0.0331(8) Uani 1 1 d . . . H35 H 0.6272 0.9482 0.8245 0.040 Uiso 1 1 calc R . . C36 C 0.65799(10) 1.0354(4) 0.7707(2) 0.0376(9) Uani 1 1 d . . . H36 H 0.6602 1.1300 0.7943 0.045 Uiso 1 1 calc R . . C37 C 0.67409(10) 1.0072(4) 0.7177(2) 0.0336(9) Uani 1 1 d . . . H37 H 0.6867 1.0839 0.7037 0.040 Uiso 1 1 calc R . . C38 C 0.67194(8) 0.8677(4) 0.68498(17) 0.0246(7) Uani 1 1 d . . . H38 H 0.6830 0.8491 0.6484 0.029 Uiso 1 1 calc R . . C39 C 0.54940(8) 0.4075(4) 0.41965(17) 0.0296(8) Uani 1 1 d . . . H39A H 0.5316 0.4468 0.3825 0.036 Uiso 1 1 calc R . . H39B H 0.5694 0.4265 0.4047 0.036 Uiso 1 1 calc R . . C40 C 0.54521(10) 0.2408(5) 0.4316(2) 0.0437(10) Uani 1 1 d . . . H40A H 0.5654 0.1956 0.4578 0.052 Uiso 1 1 calc R . . H40B H 0.5381 0.1879 0.3854 0.052 Uiso 1 1 calc R . . C41 C 0.52013(9) 0.2300(5) 0.4754(2) 0.0429(10) Uani 1 1 d . . . H41A H 0.4991 0.2568 0.4457 0.051 Uiso 1 1 calc R . . H41B H 0.5191 0.1263 0.4934 0.051 Uiso 1 1 calc R . . C42 C 0.52951(7) 0.3387(4) 0.53710(18) 0.0278(7) Uani 1 1 d . . . H42A H 0.5436 0.2887 0.5784 0.033 Uiso 1 1 calc R . . H42B H 0.5105 0.3757 0.5521 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 Ir 0.01427(6) 0.01291(7) 0.01579(6) 0.00008(4) 0.00377(4) 0.00016(4) Cl1 0.0227(3) 0.0211(4) 0.0232(4) -0.0033(3) 0.0079(3) 0.0018(3) Cl2 0.0225(3) 0.0158(4) 0.0259(4) 0.0033(3) 0.0028(3) -0.0025(3) S1 0.0168(3) 0.0202(4) 0.0224(4) 0.0004(3) 0.0016(3) -0.0011(3) P1 0.0155(3) 0.0140(4) 0.0163(3) 0.0002(3) 0.0039(3) 0.0007(3) P2 0.0158(3) 0.0138(4) 0.0186(4) 0.0006(3) 0.0029(3) -0.0004(3) C1 0.0162(14) 0.0228(16) 0.0187(14) -0.0018(12) 0.0038(11) -0.0003(12) C2 0.0275(17) 0.0259(18) 0.0222(16) 0.0012(13) 0.0083(13) -0.0002(13) C3 0.036(2) 0.045(2) 0.0347(19) 0.0021(17) 0.0229(16) -0.0018(17) C4 0.041(2) 0.046(2) 0.038(2) -0.0026(18) 0.0263(17) 0.0096(18) C5 0.0302(18) 0.0275(19) 0.0304(18) -0.0039(15) 0.0105(14) 0.0056(14) C6 0.0180(14) 0.0240(17) 0.0181(14) -0.0015(12) 0.0033(11) 0.0050(12) C7 0.0231(15) 0.0162(16) 0.0225(15) 0.0002(12) 0.0065(12) 0.0039(12) C8 0.0167(14) 0.0188(16) 0.0162(13) -0.0002(11) 0.0034(11) -0.0027(11) C9 0.0217(15) 0.0198(16) 0.0243(15) -0.0009(13) 0.0056(12) 0.0007(12) C10 0.0216(15) 0.0259(18) 0.0336(18) -0.0020(14) 0.0115(13) 0.0013(13) C11 0.0208(16) 0.0304(19) 0.0275(17) -0.0004(14) 0.0057(13) -0.0077(13) C12 0.0282(17) 0.0184(16) 0.0256(16) 0.0030(13) 0.0041(13) -0.0051(13) C13 0.0215(15) 0.0189(16) 0.0239(16) -0.0009(12) 0.0048(13) 0.0010(12) C14 0.0199(14) 0.0149(15) 0.0183(14) 0.0030(11) 0.0012(11) -0.0028(11) C15 0.0253(16) 0.0254(18) 0.0239(16) -0.0028(13) 0.0041(13) -0.0028(13) C16 0.040(2) 0.038(2) 0.0195(16) -0.0027(15) 0.0049(14) -0.0077(16) C17 0.034(2) 0.050(3) 0.0234(17) 0.0097(16) -0.0061(15) -0.0085(17) C18 0.0245(17) 0.046(2) 0.037(2) 0.0105(18) -0.0044(15) -0.0009(16) C19 0.0211(15) 0.0272(18) 0.0290(17) 0.0024(14) 0.0045(13) 0.0000(13) C20 0.0252(16) 0.0231(17) 0.0213(15) 0.0027(13) 0.0044(12) 0.0046(13) C21 0.0201(16) 0.035(2) 0.0314(18) 0.0064(15) 0.0060(13) 0.0035(14) C22 0.0242(17) 0.0291(19) 0.0253(17) 0.0029(14) -0.0017(13) -0.0026(13) C23 0.0362(19) 0.0251(18) 0.0210(16) -0.0018(13) 0.0035(14) 0.0037(15) C24 0.0217(15) 0.0267(18) 0.0211(15) 0.0049(13) 0.0058(12) 0.0048(13) C25 0.0185(14) 0.0173(16) 0.0202(15) 0.0046(12) 0.0033(12) -0.0021(11) C26 0.0190(14) 0.0190(16) 0.0189(14) 0.0032(12) 0.0018(12) -0.0019(12) C27 0.0153(14) 0.0220(16) 0.0216(15) 0.0040(12) 0.0040(12) 0.0018(12) C28 0.0198(14) 0.0260(17) 0.0204(15) 0.0027(13) 0.0040(12) 0.0019(13) C29 0.0297(17) 0.031(2) 0.0238(16) 0.0014(14) 0.0092(13) 0.0090(14) C30 0.0215(16) 0.044(2) 0.038(2) 0.0088(17) 0.0121(15) 0.0103(15) C31 0.0179(16) 0.035(2) 0.050(2) 0.0083(17) 0.0058(16) 0.0004(14) C32 0.0205(15) 0.0217(17) 0.0405(19) 0.0042(15) 0.0066(14) -0.0001(13) C33 0.0203(14) 0.0146(15) 0.0199(14) -0.0006(12) -0.0033(12) 0.0022(12) C34 0.0291(17) 0.0207(17) 0.0218(15) 0.0024(13) 0.0009(13) 0.0037(13) C35 0.046(2) 0.0276(19) 0.0225(17) -0.0016(14) 0.0009(15) 0.0111(16) C36 0.056(3) 0.0164(18) 0.033(2) -0.0049(15) -0.0044(18) 0.0048(16) C37 0.043(2) 0.0158(17) 0.036(2) 0.0021(14) -0.0029(17) -0.0078(15) C38 0.0259(16) 0.0200(17) 0.0237(15) 0.0038(13) -0.0029(13) -0.0018(13) C39 0.0294(17) 0.039(2) 0.0179(15) -0.0050(14) -0.0001(13) -0.0033(15) C40 0.045(2) 0.035(2) 0.054(3) -0.0163(19) 0.019(2) -0.0082(18) C41 0.038(2) 0.032(2) 0.062(3) -0.0118(19) 0.0190(19) -0.0142(17) C42 0.0183(15) 0.0304(19) 0.0348(18) 0.0049(15) 0.0061(13) -0.0058(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 Ir C1 2.064(3) . ? Ir P1 2.2423(8) . ? Ir P2 2.3136(7) . ? Ir Cl2 2.4358(7) . ? Ir S1 2.4411(8) . ? Ir Cl1 2.4521(7) . ? S1 C39 1.819(3) . ? S1 C42 1.833(3) . ? P1 C8 1.817(3) . ? P1 C7 1.823(3) . ? P1 C14 1.828(3) . ? P2 C33 1.821(3) . ? P2 C27 1.828(3) . ? P2 C26 1.855(3) . ? C1 C2 1.401(4) . ? C1 C6 1.403(4) . ? C2 C3 1.386(5) . ? C3 C4 1.381(6) . ? C4 C5 1.378(5) . ? C5 C6 1.390(4) . ? C6 C7 1.518(4) . ? C8 C13 1.389(4) . ? C8 C9 1.396(4) . ? C9 C10 1.389(4) . ? C10 C11 1.373(5) . ? C11 C12 1.386(5) . ? C12 C13 1.379(5) . ? C14 C19 1.392(4) . ? C14 C15 1.399(4) . ? C15 C16 1.385(4) . ? C16 C17 1.377(5) . ? C17 C18 1.383(5) . ? C18 C19 1.389(4) . ? C20 C21 1.385(4) . ? C20 C25 1.395(4) . ? C21 C22 1.378(5) . ? C22 C23 1.376(5) . ? C23 C24 1.385(4) . ? C24 C25 1.390(4) . ? C25 C26 1.507(4) . ? C27 C32 1.392(4) . ? C27 C28 1.393(5) . ? C28 C29 1.390(4) . ? C29 C30 1.375(5) . ? C30 C31 1.376(6) . ? C31 C32 1.393(5) . ? C33 C34 1.398(5) . ? C33 C38 1.399(4) . ? C34 C35 1.380(5) . ? C35 C36 1.370(6) . ? C36 C37 1.383(6) . ? C37 C38 1.386(5) . ? C39 C40 1.517(5) . ? C40 C41 1.523(5) . ? C41 C42 1.513(5) . ? 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 Ir P1 83.44(9) . . ? C1 Ir P2 88.87(8) . . ? P1 Ir P2 94.16(3) . . ? C1 Ir Cl2 97.73(9) . . ? P1 Ir Cl2 177.45(3) . . ? P2 Ir Cl2 88.13(3) . . ? C1 Ir S1 80.49(8) . . ? P1 Ir S1 88.42(3) . . ? P2 Ir S1 168.70(3) . . ? Cl2 Ir S1 89.55(3) . . ? C1 Ir Cl1 170.01(8) . . ? P1 Ir Cl1 92.09(3) . . ? P2 Ir Cl1 100.39(3) . . ? Cl2 Ir Cl1 86.40(3) . . ? S1 Ir Cl1 90.49(3) . . ? C39 S1 C42 93.79(16) . . ? C39 S1 Ir 113.45(12) . . ? C42 S1 Ir 111.50(11) . . ? C8 P1 C7 106.39(14) . . ? C8 P1 C14 98.69(13) . . ? C7 P1 C14 106.78(14) . . ? C8 P1 Ir 123.13(10) . . ? C7 P1 Ir 105.47(10) . . ? C14 P1 Ir 115.24(10) . . ? C33 P2 C27 108.32(14) . . ? C33 P2 C26 102.43(14) . . ? C27 P2 C26 98.29(14) . . ? C33 P2 Ir 115.31(9) . . ? C27 P2 Ir 118.37(10) . . ? C26 P2 Ir 111.70(10) . . ? C2 C1 C6 116.8(3) . . ? C2 C1 Ir 122.9(2) . . ? C6 C1 Ir 120.0(2) . . ? C3 C2 C1 121.7(3) . . ? C4 C3 C2 120.4(3) . . ? C5 C4 C3 119.1(3) . . ? C4 C5 C6 120.8(3) . . ? C5 C6 C1 121.1(3) . . ? C5 C6 C7 118.4(3) . . ? C1 C6 C7 120.4(3) . . ? C6 C7 P1 108.0(2) . . ? C13 C8 C9 119.9(3) . . ? C13 C8 P1 117.9(2) . . ? C9 C8 P1 121.7(2) . . ? C10 C9 C8 119.2(3) . . ? C11 C10 C9 120.5(3) . . ? C10 C11 C12 120.4(3) . . ? C13 C12 C11 119.7(3) . . ? C12 C13 C8 120.3(3) . . ? C19 C14 C15 119.4(3) . . ? C19 C14 P1 121.3(2) . . ? C15 C14 P1 119.3(2) . . ? C16 C15 C14 120.0(3) . . ? C17 C16 C15 120.1(3) . . ? C16 C17 C18 120.5(3) . . ? C17 C18 C19 119.9(3) . . ? C18 C19 C14 120.0(3) . . ? C21 C20 C25 120.7(3) . . ? C22 C21 C20 120.3(3) . . ? C23 C22 C21 119.8(3) . . ? C22 C23 C24 120.0(3) . . ? C23 C24 C25 121.2(3) . . ? C24 C25 C20 117.9(3) . . ? C24 C25 C26 120.5(3) . . ? C20 C25 C26 121.5(3) . . ? C25 C26 P2 116.5(2) . . ? C32 C27 C28 118.4(3) . . ? C32 C27 P2 125.0(3) . . ? C28 C27 P2 115.6(2) . . ? C29 C28 C27 120.4(3) . . ? C30 C29 C28 120.5(3) . . ? C29 C30 C31 120.0(3) . . ? C30 C31 C32 120.0(3) . . ? C27 C32 C31 120.7(3) . . ? C34 C33 C38 118.3(3) . . ? C34 C33 P2 117.3(2) . . ? C38 C33 P2 124.4(3) . . ? C35 C34 C33 120.9(3) . . ? C36 C35 C34 120.1(4) . . ? C35 C36 C37 120.1(3) . . ? C36 C37 C38 120.3(4) . . ? C37 C38 C33 120.2(3) . . ? C40 C39 S1 105.1(3) . . ? C39 C40 C41 105.7(3) . . ? C42 C41 C40 107.2(3) . . ? C41 C42 S1 106.8(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.229 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.119 data_9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H38 Cl F3 Ir N3 P2' _chemical_formula_weight 991.39 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4793(4) _cell_length_b 20.8875(7) _cell_length_c 15.9283(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.143(1) _cell_angle_gamma 90.00 _cell_volume 3922.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8238 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 26.67 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 3.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3567 _exptl_absorpt_correction_T_max 0.6714 _exptl_absorpt_process_details ? _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_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29888 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9005 _reflns_number_gt 7800 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+1.4778P] 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 9005 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 Ir Ir 0.838425(10) 0.222188(5) 0.198447(7) 0.01305(4) Uani 1 1 d . . . Cl1 Cl 0.66151(6) 0.17271(4) 0.10893(5) 0.01996(16) Uani 1 1 d . . . P1 P 1.01569(7) 0.25188(4) 0.28137(5) 0.01472(16) Uani 1 1 d . . . P2 P 0.73250(7) 0.27682(4) 0.26979(5) 0.01548(16) Uani 1 1 d . . . N1 N 0.9027(2) 0.17053(12) 0.11095(15) 0.0156(5) Uani 1 1 d . . . N2 N 0.8210(2) 0.28766(11) 0.09386(16) 0.0159(5) Uani 1 1 d . . . N3 N 0.7946(2) 0.35034(11) 0.08299(15) 0.0159(5) Uani 1 1 d . . . C1 C 0.9341(3) 0.10858(15) 0.1205(2) 0.0218(7) Uani 1 1 d . . . H1 H 0.9268 0.0853 0.1696 0.026 Uiso 1 1 calc R . . C2 C 0.9764(3) 0.07775(16) 0.0617(2) 0.0257(8) Uani 1 1 d . . . H2 H 0.9990 0.0341 0.0705 0.031 Uiso 1 1 calc R . . C3 C 0.9855(3) 0.11135(16) -0.0105(2) 0.0264(8) Uani 1 1 d . . . H3 H 1.0162 0.0914 -0.0512 0.032 Uiso 1 1 calc R . . C4 C 0.9496(3) 0.17418(15) -0.0226(2) 0.0221(7) Uani 1 1 d . . . H4 H 0.9536 0.1977 -0.0726 0.026 Uiso 1 1 calc R . . C5 C 0.9077(3) 0.20270(15) 0.03878(19) 0.0172(6) Uani 1 1 d . . . C6 C 0.8689(3) 0.26842(14) 0.03278(19) 0.0165(6) Uani 1 1 d . . . C7 C 0.8736(3) 0.32028(15) -0.0205(2) 0.0200(7) Uani 1 1 d . . . H7 H 0.9019 0.3216 -0.0690 0.024 Uiso 1 1 calc R . . C8 C 0.8272(3) 0.36930(14) 0.01395(19) 0.0169(6) Uani 1 1 d . . . C9 C 0.8202(3) 0.43811(15) -0.0100(2) 0.0218(7) Uani 1 1 d . . . C10 C 0.8721(2) 0.15232(13) 0.29636(18) 0.0146(6) Uani 1 1 d . . . C11 C 0.8053(3) 0.09711(14) 0.2887(2) 0.0182(6) Uani 1 1 d . . . H11 H 0.7462 0.0890 0.2344 0.022 Uiso 1 1 calc R . . C12 C 0.8236(3) 0.05400(14) 0.3587(2) 0.0204(7) Uani 1 1 d . . . H12 H 0.7755 0.0178 0.3524 0.024 Uiso 1 1 calc R . . C13 C 0.9115(3) 0.06352(15) 0.4373(2) 0.0217(7) Uani 1 1 d . . . H13 H 0.9231 0.0344 0.4853 0.026 Uiso 1 1 calc R . . C14 C 0.9821(3) 0.11543(15) 0.4456(2) 0.0197(7) Uani 1 1 d . . . H14 H 1.0448 0.1210 0.4985 0.024 Uiso 1 1 calc R . . C15 C 0.9619(3) 0.15982(14) 0.37689(19) 0.0169(6) Uani 1 1 d . . . C16 C 1.0330(3) 0.22021(14) 0.39084(19) 0.0179(6) Uani 1 1 d . . . H16A H 1.1137 0.2103 0.4226 0.021 Uiso 1 1 calc R . . H16B H 1.0067 0.2517 0.4263 0.021 Uiso 1 1 calc R . . C17 C 1.1232(3) 0.21105(14) 0.24534(19) 0.0168(6) Uani 1 1 d . . . C18 C 1.1635(3) 0.15123(15) 0.2785(2) 0.0217(7) Uani 1 1 d . . . H18 H 1.1377 0.1320 0.3224 0.026 Uiso 1 1 calc R . . C19 C 1.2410(3) 0.11915(16) 0.2484(2) 0.0237(7) Uani 1 1 d . . . H19 H 1.2675 0.0780 0.2715 0.028 Uiso 1 1 calc R . . C20 C 1.2798(3) 0.14659(16) 0.1852(2) 0.0249(7) Uani 1 1 d . . . H20 H 1.3338 0.1247 0.1653 0.030 Uiso 1 1 calc R . . C21 C 1.2402(3) 0.20577(16) 0.1508(2) 0.0274(8) Uani 1 1 d . . . H21 H 1.2659 0.2244 0.1065 0.033 Uiso 1 1 calc R . . C22 C 1.1627(3) 0.23818(15) 0.1807(2) 0.0228(7) Uani 1 1 d . . . H22 H 1.1361 0.2792 0.1571 0.027 Uiso 1 1 calc R . . C23 C 1.0679(3) 0.33349(14) 0.2967(2) 0.0175(6) Uani 1 1 d . . . C24 C 1.1286(3) 0.35524(15) 0.3818(2) 0.0198(7) Uani 1 1 d . . . H24 H 1.1423 0.3272 0.4312 0.024 Uiso 1 1 calc R . . C25 C 1.1692(3) 0.41753(16) 0.3948(2) 0.0251(7) Uani 1 1 d . . . H25 H 1.2101 0.4321 0.4530 0.030 Uiso 1 1 calc R . . C26 C 1.1503(3) 0.45841(16) 0.3234(2) 0.0267(8) Uani 1 1 d . . . H26 H 1.1780 0.5011 0.3325 0.032 Uiso 1 1 calc R . . C27 C 1.0910(3) 0.43716(16) 0.2385(2) 0.0250(7) Uani 1 1 d . . . H27 H 1.0780 0.4653 0.1893 0.030 Uiso 1 1 calc R . . C28 C 1.0507(3) 0.37526(15) 0.2253(2) 0.0192(7) Uani 1 1 d . . . H28 H 1.0108 0.3609 0.1668 0.023 Uiso 1 1 calc R . . C29 C 0.5448(3) 0.41889(16) 0.1961(2) 0.0242(7) Uani 1 1 d . . . H29 H 0.6038 0.4322 0.1746 0.029 Uiso 1 1 calc R . . C30 C 0.4752(3) 0.46438(16) 0.2143(2) 0.0280(8) Uani 1 1 d . . . H30 H 0.4865 0.5085 0.2054 0.034 Uiso 1 1 calc R . . C31 C 0.3890(3) 0.44557(17) 0.2455(2) 0.0287(8) Uani 1 1 d . . . H31 H 0.3411 0.4767 0.2585 0.034 Uiso 1 1 calc R . . C32 C 0.3727(3) 0.38104(17) 0.2578(2) 0.0269(8) Uani 1 1 d . . . H32 H 0.3131 0.3677 0.2786 0.032 Uiso 1 1 calc R . . C33 C 0.4436(3) 0.33607(16) 0.2396(2) 0.0228(7) Uani 1 1 d . . . H33 H 0.4325 0.2920 0.2487 0.027 Uiso 1 1 calc R . . C34 C 0.5303(3) 0.35425(15) 0.20860(19) 0.0186(7) Uani 1 1 d . . . C35 C 0.6046(3) 0.30646(15) 0.18309(19) 0.0185(6) Uani 1 1 d . . . H35A H 0.6289 0.3260 0.1356 0.022 Uiso 1 1 calc R . . H35B H 0.5570 0.2689 0.1567 0.022 Uiso 1 1 calc R . . C36 C 0.7821(3) 0.35003(15) 0.3322(2) 0.0194(7) Uani 1 1 d . . . C37 C 0.8320(3) 0.39607(15) 0.2938(2) 0.0195(7) Uani 1 1 d . . . H37 H 0.8464 0.3863 0.2402 0.023 Uiso 1 1 calc R . . C38 C 0.8610(3) 0.45576(16) 0.3321(2) 0.0251(7) Uani 1 1 d . . . H38 H 0.8952 0.4865 0.3050 0.030 Uiso 1 1 calc R . . C39 C 0.8402(3) 0.47069(17) 0.4100(2) 0.0360(9) Uani 1 1 d . . . H39 H 0.8618 0.5112 0.4373 0.043 Uiso 1 1 calc R . . C40 C 0.7878(4) 0.42640(18) 0.4476(2) 0.0414(10) Uani 1 1 d . . . H40 H 0.7716 0.4370 0.5002 0.050 Uiso 1 1 calc R . . C41 C 0.7585(3) 0.36653(17) 0.4095(2) 0.0313(8) Uani 1 1 d . . . H41 H 0.7222 0.3365 0.4360 0.038 Uiso 1 1 calc R . . C42 C 0.6859(3) 0.22472(14) 0.3431(2) 0.0183(6) Uani 1 1 d . . . C43 C 0.5893(3) 0.18691(15) 0.3091(2) 0.0216(7) Uani 1 1 d . . . H43 H 0.5416 0.1926 0.2494 0.026 Uiso 1 1 calc R . . C44 C 0.5624(3) 0.14112(16) 0.3616(2) 0.0261(8) Uani 1 1 d . . . H44 H 0.4964 0.1156 0.3379 0.031 Uiso 1 1 calc R . . C45 C 0.6315(3) 0.13253(16) 0.4485(2) 0.0281(8) Uani 1 1 d . . . H45 H 0.6120 0.1016 0.4848 0.034 Uiso 1 1 calc R . . C46 C 0.7286(3) 0.16873(16) 0.4830(2) 0.0254(7) Uani 1 1 d . . . H46 H 0.7766 0.1624 0.5425 0.030 Uiso 1 1 calc R . . C47 C 0.7554(3) 0.21432(14) 0.4302(2) 0.0201(7) Uani 1 1 d . . . H47 H 0.8226 0.2390 0.4538 0.024 Uiso 1 1 calc R . . F1 F 0.8604(2) 0.47585(9) 0.06105(13) 0.0380(5) Uani 1 1 d . . . F2 F 0.87957(19) 0.45174(9) -0.06369(14) 0.0367(5) Uani 1 1 d . . . F3 F 0.71472(18) 0.45871(10) -0.05220(15) 0.0419(6) 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 Ir 0.01531(7) 0.01157(6) 0.01273(6) 0.00016(4) 0.00526(4) 0.00034(5) Cl1 0.0195(4) 0.0202(4) 0.0185(3) -0.0025(3) 0.0040(3) -0.0018(3) P1 0.0162(4) 0.0130(4) 0.0154(4) 0.0008(3) 0.0058(3) 0.0000(3) P2 0.0171(4) 0.0149(4) 0.0154(4) 0.0011(3) 0.0068(3) 0.0010(3) N1 0.0157(13) 0.0146(13) 0.0156(12) 0.0000(10) 0.0038(10) 0.0003(11) N2 0.0167(13) 0.0144(13) 0.0169(12) 0.0006(10) 0.0060(10) 0.0020(10) N3 0.0171(14) 0.0125(13) 0.0166(12) 0.0014(10) 0.0036(10) 0.0001(10) C1 0.0258(18) 0.0182(16) 0.0194(15) -0.0018(13) 0.0050(13) -0.0002(14) C2 0.034(2) 0.0184(17) 0.0241(17) -0.0037(14) 0.0084(15) 0.0059(15) C3 0.0297(19) 0.0281(19) 0.0238(17) -0.0082(14) 0.0121(15) 0.0055(16) C4 0.0292(19) 0.0206(17) 0.0189(15) -0.0019(13) 0.0112(14) 0.0011(14) C5 0.0160(16) 0.0177(15) 0.0169(14) -0.0015(12) 0.0043(12) -0.0003(13) C6 0.0183(16) 0.0145(15) 0.0177(14) 0.0000(12) 0.0072(12) 0.0011(12) C7 0.0223(17) 0.0233(17) 0.0174(15) 0.0017(13) 0.0107(13) -0.0006(14) C8 0.0171(16) 0.0155(15) 0.0184(14) 0.0019(12) 0.0063(12) -0.0002(13) C9 0.0228(18) 0.0214(17) 0.0218(16) 0.0040(13) 0.0082(14) 0.0020(14) C10 0.0165(16) 0.0124(15) 0.0161(14) -0.0005(11) 0.0071(12) 0.0026(12) C11 0.0175(16) 0.0160(16) 0.0209(15) 0.0009(12) 0.0059(13) 0.0039(13) C12 0.0224(18) 0.0113(15) 0.0314(17) 0.0023(13) 0.0142(14) 0.0007(13) C13 0.0264(18) 0.0174(16) 0.0251(16) 0.0091(13) 0.0135(14) 0.0067(14) C14 0.0194(17) 0.0219(17) 0.0177(15) 0.0015(13) 0.0057(13) 0.0052(14) C15 0.0176(16) 0.0146(15) 0.0209(15) 0.0014(12) 0.0097(13) 0.0022(13) C16 0.0181(16) 0.0188(16) 0.0155(14) 0.0018(12) 0.0039(12) -0.0002(13) C17 0.0147(16) 0.0175(16) 0.0180(15) -0.0021(12) 0.0052(12) -0.0028(12) C18 0.0228(18) 0.0197(17) 0.0231(16) 0.0009(13) 0.0084(14) -0.0009(13) C19 0.0230(18) 0.0194(17) 0.0269(17) -0.0014(14) 0.0058(14) 0.0009(14) C20 0.0191(18) 0.0263(19) 0.0317(18) -0.0082(14) 0.0117(14) 0.0012(14) C21 0.029(2) 0.0300(19) 0.0299(18) -0.0017(15) 0.0197(16) -0.0016(15) C22 0.0265(19) 0.0165(16) 0.0276(17) 0.0016(13) 0.0120(15) 0.0007(14) C23 0.0138(15) 0.0156(15) 0.0238(15) -0.0006(13) 0.0069(12) -0.0002(13) C24 0.0191(17) 0.0178(16) 0.0241(16) -0.0018(13) 0.0092(13) -0.0007(13) C25 0.0247(19) 0.0227(18) 0.0298(18) -0.0099(14) 0.0118(15) -0.0048(15) C26 0.0255(19) 0.0175(17) 0.042(2) -0.0058(15) 0.0177(16) -0.0053(14) C27 0.0229(18) 0.0184(17) 0.0370(19) 0.0071(14) 0.0141(15) 0.0009(14) C28 0.0139(16) 0.0221(17) 0.0219(15) -0.0006(13) 0.0063(13) -0.0016(13) C29 0.0188(17) 0.0242(18) 0.0294(18) 0.0036(14) 0.0077(14) 0.0008(14) C30 0.029(2) 0.0198(18) 0.0341(19) 0.0028(15) 0.0084(16) 0.0041(15) C31 0.027(2) 0.031(2) 0.0300(18) 0.0016(15) 0.0104(15) 0.0129(16) C32 0.0210(18) 0.032(2) 0.0321(18) 0.0048(15) 0.0146(15) 0.0025(15) C33 0.0230(18) 0.0206(17) 0.0260(17) 0.0063(14) 0.0098(14) 0.0037(14) C34 0.0197(17) 0.0192(16) 0.0156(14) 0.0013(12) 0.0042(12) 0.0039(13) C35 0.0209(17) 0.0198(16) 0.0160(14) 0.0020(12) 0.0078(13) 0.0021(13) C36 0.0213(17) 0.0177(16) 0.0199(15) -0.0005(12) 0.0077(13) 0.0046(13) C37 0.0154(16) 0.0199(16) 0.0236(16) -0.0012(13) 0.0070(13) 0.0025(13) C38 0.0243(19) 0.0195(17) 0.0330(18) -0.0012(14) 0.0113(15) 0.0003(14) C39 0.051(3) 0.0194(18) 0.038(2) -0.0128(16) 0.0156(19) -0.0072(17) C40 0.074(3) 0.026(2) 0.033(2) -0.0092(16) 0.030(2) -0.002(2) C41 0.049(2) 0.0250(19) 0.0276(18) 0.0012(15) 0.0228(17) 0.0006(17) C42 0.0227(17) 0.0149(15) 0.0209(15) 0.0029(13) 0.0120(13) 0.0040(13) C43 0.0199(17) 0.0250(18) 0.0220(16) 0.0007(13) 0.0098(13) 0.0032(14) C44 0.0244(19) 0.0191(17) 0.041(2) -0.0016(15) 0.0192(16) 0.0001(14) C45 0.039(2) 0.0209(18) 0.0344(19) 0.0085(15) 0.0262(17) 0.0071(16) C46 0.033(2) 0.0251(18) 0.0202(16) 0.0027(14) 0.0121(14) 0.0076(16) C47 0.0256(18) 0.0172(16) 0.0215(15) -0.0030(12) 0.0131(14) 0.0017(13) F1 0.0631(16) 0.0195(10) 0.0291(11) -0.0021(9) 0.0120(10) -0.0028(10) F2 0.0546(14) 0.0227(11) 0.0468(13) 0.0080(9) 0.0356(11) 0.0004(10) F3 0.0312(12) 0.0259(12) 0.0619(15) 0.0169(10) 0.0064(11) 0.0090(10) _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 Ir C10 2.076(3) . ? Ir N2 2.111(2) . ? Ir N1 2.118(2) . ? Ir P1 2.2598(8) . ? Ir P2 2.3078(8) . ? Ir Cl1 2.4312(7) . ? P1 C16 1.810(3) . ? P1 C23 1.813(3) . ? P1 C17 1.834(3) . ? P2 C36 1.818(3) . ? P2 C42 1.825(3) . ? P2 C35 1.842(3) . ? N1 C1 1.346(4) . ? N1 C5 1.350(4) . ? N2 N3 1.347(3) . ? N2 C6 1.359(4) . ? N3 C8 1.351(4) . ? C1 C2 1.377(4) . ? C2 C3 1.382(5) . ? C3 C4 1.380(4) . ? C4 C5 1.385(4) . ? C5 C6 1.448(4) . ? C6 C7 1.389(4) . ? C7 C8 1.376(4) . ? C8 C9 1.482(4) . ? C9 F2 1.334(4) . ? C9 F1 1.334(4) . ? C9 F3 1.337(4) . ? C10 C11 1.405(4) . ? C10 C15 1.408(4) . ? C11 C12 1.393(4) . ? C12 C13 1.382(4) . ? C13 C14 1.376(4) . ? C14 C15 1.393(4) . ? C15 C16 1.516(4) . ? C17 C18 1.385(4) . ? C17 C22 1.398(4) . ? C18 C19 1.384(4) . ? C19 C20 1.379(5) . ? C20 C21 1.376(5) . ? C21 C22 1.386(5) . ? C23 C28 1.393(4) . ? C23 C24 1.394(4) . ? C24 C25 1.387(4) . ? C25 C26 1.379(5) . ? C26 C27 1.385(5) . ? C27 C28 1.378(4) . ? C29 C30 1.381(5) . ? C29 C34 1.385(4) . ? C30 C31 1.382(5) . ? C31 C32 1.386(5) . ? C32 C33 1.385(4) . ? C33 C34 1.382(4) . ? C34 C35 1.506(4) . ? C36 C37 1.391(4) . ? C36 C41 1.400(4) . ? C37 C38 1.383(4) . ? C38 C39 1.383(5) . ? C39 C40 1.379(5) . ? C40 C41 1.386(5) . ? C42 C47 1.392(4) . ? C42 C43 1.393(4) . ? C43 C44 1.382(4) . ? C44 C45 1.381(5) . ? C45 C46 1.380(5) . ? C46 C47 1.382(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 C10 Ir N2 172.55(10) . . ? C10 Ir N1 96.26(10) . . ? N2 Ir N1 76.93(9) . . ? C10 Ir P1 80.53(8) . . ? N2 Ir P1 96.39(7) . . ? N1 Ir P1 90.85(7) . . ? C10 Ir P2 89.16(8) . . ? N2 Ir P2 98.10(7) . . ? N1 Ir P2 167.94(7) . . ? P1 Ir P2 100.69(3) . . ? C10 Ir Cl1 93.62(8) . . ? N2 Ir Cl1 88.50(7) . . ? N1 Ir Cl1 82.22(7) . . ? P1 Ir Cl1 170.44(3) . . ? P2 Ir Cl1 86.70(3) . . ? C16 P1 C23 106.83(14) . . ? C16 P1 C17 105.26(14) . . ? C23 P1 C17 102.24(14) . . ? C16 P1 Ir 104.32(10) . . ? C23 P1 Ir 125.23(10) . . ? C17 P1 Ir 111.47(10) . . ? C36 P2 C42 105.96(14) . . ? C36 P2 C35 100.54(14) . . ? C42 P2 C35 107.47(15) . . ? C36 P2 Ir 122.53(11) . . ? C42 P2 Ir 111.98(10) . . ? C35 P2 Ir 107.01(10) . . ? C1 N1 C5 118.8(3) . . ? C1 N1 Ir 125.1(2) . . ? C5 N1 Ir 116.08(19) . . ? N3 N2 C6 110.0(2) . . ? N3 N2 Ir 133.52(19) . . ? C6 N2 Ir 114.69(19) . . ? N2 N3 C8 105.3(2) . . ? N1 C1 C2 122.4(3) . . ? C1 C2 C3 118.9(3) . . ? C4 C3 C2 119.2(3) . . ? C3 C4 C5 119.4(3) . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 114.8(3) . . ? C4 C5 C6 123.8(3) . . ? N2 C6 C7 108.9(3) . . ? N2 C6 C5 116.7(3) . . ? C7 C6 C5 134.3(3) . . ? C8 C7 C6 103.2(3) . . ? N3 C8 C7 112.6(3) . . ? N3 C8 C9 119.0(3) . . ? C7 C8 C9 128.1(3) . . ? F2 C9 F1 106.5(3) . . ? F2 C9 F3 105.7(3) . . ? F1 C9 F3 105.7(3) . . ? F2 C9 C8 111.9(3) . . ? F1 C9 C8 112.4(3) . . ? F3 C9 C8 114.0(3) . . ? C11 C10 C15 116.3(3) . . ? C11 C10 Ir 122.9(2) . . ? C15 C10 Ir 120.7(2) . . ? C12 C11 C10 121.6(3) . . ? C13 C12 C11 120.4(3) . . ? C14 C13 C12 119.5(3) . . ? C13 C14 C15 120.3(3) . . ? C14 C15 C10 121.8(3) . . ? C14 C15 C16 119.5(3) . . ? C10 C15 C16 118.6(3) . . ? C15 C16 P1 106.5(2) . . ? C18 C17 C22 118.3(3) . . ? C18 C17 P1 120.8(2) . . ? C22 C17 P1 120.8(2) . . ? C19 C18 C17 120.8(3) . . ? C20 C19 C18 120.3(3) . . ? C21 C20 C19 119.8(3) . . ? C20 C21 C22 120.2(3) . . ? C21 C22 C17 120.6(3) . . ? C28 C23 C24 118.6(3) . . ? C28 C23 P1 121.8(2) . . ? C24 C23 P1 119.6(2) . . ? C25 C24 C23 120.4(3) . . ? C26 C25 C24 120.2(3) . . ? C25 C26 C27 119.9(3) . . ? C28 C27 C26 120.1(3) . . ? C27 C28 C23 120.8(3) . . ? C30 C29 C34 121.3(3) . . ? C29 C30 C31 119.8(3) . . ? C30 C31 C32 119.7(3) . . ? C33 C32 C31 119.8(3) . . ? C34 C33 C32 121.2(3) . . ? C33 C34 C29 118.3(3) . . ? C33 C34 C35 122.5(3) . . ? C29 C34 C35 119.1(3) . . ? C34 C35 P2 118.6(2) . . ? C37 C36 C41 118.0(3) . . ? C37 C36 P2 117.6(2) . . ? C41 C36 P2 123.8(3) . . ? C38 C37 C36 121.3(3) . . ? C37 C38 C39 120.0(3) . . ? C40 C39 C38 119.6(3) . . ? C39 C40 C41 120.6(3) . . ? C40 C41 C36 120.4(3) . . ? C47 C42 C43 118.4(3) . . ? C47 C42 P2 120.4(2) . . ? C43 C42 P2 120.4(2) . . ? C44 C43 C42 120.6(3) . . ? C43 C44 C45 120.0(3) . . ? C46 C45 C44 120.3(3) . . ? C45 C46 C47 119.5(3) . . ? C46 C47 C42 121.2(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.215 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.102