Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Haiping Xia' _publ_contact_author_address ; Chemistry and Chemical Engineering Xiamen University Xiamen 361005 CHINA ; _publ_contact_author_email HPXIA@XMU.EDU.CN _publ_section_title ; Synthesis and characterization of a bimetallic iridium complex with a bridge of ten sp2-carbon chain ; loop_ _publ_author_name 'Haiping Xia' 'Lei Gong' 'Yumei Lin' 'Tingbin Wen' 'Liqiong Wu' ; Fang-zu Yang ; 'Hong Zang' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 633228' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C59 H50 Cl2 P3 O Ir, 2 CH2Cl2' _chemical_formula_sum 'C61 H54 Cl6 Ir O P3' _chemical_formula_weight 1300.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 12.8331(19) _cell_length_b 32.704(5) _cell_length_c 13.692(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.703(2) _cell_angle_gamma 90.00 _cell_volume 5339.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9407 _cell_measurement_theta_min 0 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2608 _exptl_absorpt_coefficient_mu 2.934 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.557 _exptl_absorpt_correction_T_max 0.814 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38479 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0705 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9407 _reflns_number_gt 8156 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+200.2098P] 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 9407 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.002 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 -0.06939(4) 0.132827(14) 0.18481(4) 0.02213(15) Uani 1 1 d . . . Cl1 Cl -0.0773(3) 0.20796(9) 0.1642(2) 0.0295(7) Uani 1 1 d . . . Cl2 Cl -0.1570(3) 0.11186(10) -0.0018(2) 0.0348(7) Uani 1 1 d . . . P1 P -0.2418(3) 0.13986(10) 0.2025(2) 0.0259(7) Uani 1 1 d . . . P2 P 0.0980(3) 0.13334(10) 0.1537(2) 0.0250(7) Uani 1 1 d . . . P3 P 0.0996(3) 0.10583(10) 0.5344(2) 0.0284(7) Uani 1 1 d . . . O1 O 0.0033(14) 0.0338(4) 0.3920(10) 0.085(5) Uani 1 1 d . . . H1B H -0.0415 0.0153 0.3624 0.102 Uiso 1 1 calc R . . C1 C 0.0059(10) 0.1400(4) 0.3392(9) 0.024(3) Uani 1 1 d . . . H1A H 0.0313 0.1658 0.3688 0.029 Uiso 1 1 calc R . . C2 C 0.0188(10) 0.1069(4) 0.3990(9) 0.027(3) Uani 1 1 d . . . C3 C -0.0332(13) 0.0690(4) 0.3425(11) 0.038(3) Uani 1 1 d . . . H3A H -0.1106 0.0707 0.3415 0.046 Uiso 1 1 calc R . . C4 C -0.0508(10) 0.0732(4) 0.2282(10) 0.026(3) Uani 1 1 d . . . C5 C -0.0507(11) 0.0407(4) 0.1763(12) 0.041(4) Uani 1 1 d . . . H5A H -0.0399 0.0151 0.2098 0.049 Uiso 1 1 calc R . . H5B H -0.0615 0.0424 0.1046 0.049 Uiso 1 1 calc R . . C111 C -0.3416(10) 0.1745(4) 0.1097(10) 0.030(3) Uani 1 1 d . . . C112 C -0.3352(11) 0.1832(4) 0.0150(11) 0.039(3) Uani 1 1 d . . . H11C H -0.2745 0.1737 -0.0015 0.047 Uiso 1 1 calc R . . C113 C -0.4189(12) 0.2059(5) -0.0563(12) 0.044(4) Uani 1 1 d . . . H11D H -0.4149 0.2120 -0.1219 0.053 Uiso 1 1 calc R . . C114 C -0.5078(14) 0.2199(5) -0.0342(13) 0.059(5) Uani 1 1 d . . . H11E H -0.5658 0.2347 -0.0847 0.070 Uiso 1 1 calc R . . C115 C -0.5111(12) 0.2123(5) 0.0593(14) 0.054(4) Uani 1 1 d . . . H11A H -0.5708 0.2230 0.0755 0.065 Uiso 1 1 calc R . . C116 C -0.4305(13) 0.1892(5) 0.1341(12) 0.046(4) Uani 1 1 d . . . H11B H -0.4355 0.1837 0.1995 0.055 Uiso 1 1 calc R . . C121 C -0.2306(10) 0.1611(4) 0.3280(10) 0.030(3) Uani 1 1 d . . . C122 C -0.2155(11) 0.2031(4) 0.3411(11) 0.038(3) Uani 1 1 d . . . H12A H -0.2139 0.2195 0.2853 0.046 Uiso 1 1 calc R . . C123 C -0.2029(11) 0.2204(5) 0.4361(12) 0.042(3) Uani 1 1 d . . . H12B H -0.1945 0.2489 0.4448 0.050 Uiso 1 1 calc R . . C124 C -0.2025(12) 0.1967(5) 0.5172(12) 0.043(4) Uani 1 1 d . . . H12E H -0.1927 0.2087 0.5823 0.052 Uiso 1 1 calc R . . C125 C -0.2159(13) 0.1566(5) 0.5053(12) 0.048(4) Uani 1 1 d . . . H12C H -0.2158 0.1404 0.5621 0.057 Uiso 1 1 calc R . . C126 C -0.2298(11) 0.1386(4) 0.4122(11) 0.036(3) Uani 1 1 d . . . H12D H -0.2392 0.1101 0.4054 0.044 Uiso 1 1 calc R . . C131 C -0.3322(10) 0.0953(4) 0.1846(10) 0.030(3) Uani 1 1 d . . . C132 C -0.4185(10) 0.0935(4) 0.2216(12) 0.039(3) Uani 1 1 d . . . H13E H -0.4280 0.1150 0.2631 0.047 Uiso 1 1 calc R . . C133 C -0.4899(12) 0.0611(5) 0.1987(13) 0.049(4) Uani 1 1 d . . . H13A H -0.5490 0.0607 0.2237 0.059 Uiso 1 1 calc R . . C134 C -0.4775(11) 0.0298(5) 0.1412(13) 0.046(4) Uani 1 1 d . . . H13B H -0.5274 0.0076 0.1262 0.055 Uiso 1 1 calc R . . C135 C -0.3915(13) 0.0302(5) 0.1041(13) 0.049(4) Uani 1 1 d . . . H13C H -0.3816 0.0079 0.0651 0.059 Uiso 1 1 calc R . . C136 C -0.3193(11) 0.0634(4) 0.1242(11) 0.040(3) Uani 1 1 d . . . H13D H -0.2620 0.0642 0.0969 0.048 Uiso 1 1 calc R . . C211 C 0.0958(12) 0.1629(4) 0.0394(10) 0.033(3) Uani 1 1 d . . . C212 C 0.1941(12) 0.1649(4) 0.0181(12) 0.041(3) Uani 1 1 d . . . H21B H 0.2597 0.1516 0.0620 0.050 Uiso 1 1 calc R . . C213 C 0.1931(14) 0.1863(5) -0.0673(13) 0.050(4) Uani 1 1 d . . . H21D H 0.2588 0.1869 -0.0825 0.059 Uiso 1 1 calc R . . C214 C 0.1032(13) 0.2065(4) -0.1304(12) 0.044(4) Uani 1 1 d . . . H21A H 0.1060 0.2213 -0.1882 0.053 Uiso 1 1 calc R . . C215 C 0.0070(13) 0.2053(4) -0.1097(11) 0.041(3) Uani 1 1 d . . . H21E H -0.0571 0.2194 -0.1537 0.049 Uiso 1 1 calc R . . C216 C 0.0032(12) 0.1836(4) -0.0246(10) 0.035(3) Uani 1 1 d . . . H21C H -0.0632 0.1831 -0.0106 0.042 Uiso 1 1 calc R . . C221 C 0.2207(10) 0.1548(4) 0.2596(9) 0.024(3) Uani 1 1 d . . . C222 C 0.2048(11) 0.1865(4) 0.3179(10) 0.030(3) Uani 1 1 d . . . H22C H 0.1333 0.1983 0.2998 0.037 Uiso 1 1 calc R . . C223 C 0.2913(12) 0.2008(4) 0.4010(11) 0.038(3) Uani 1 1 d . . . H22D H 0.2794 0.2230 0.4394 0.046 Uiso 1 1 calc R . . C224 C 0.3957(12) 0.1841(5) 0.4308(11) 0.044(4) Uani 1 1 d . . . H22A H 0.4542 0.1935 0.4914 0.053 Uiso 1 1 calc R . . C225 C 0.4137(11) 0.1532(5) 0.3703(13) 0.045(4) Uani 1 1 d . . . H22E H 0.4859 0.1419 0.3887 0.055 Uiso 1 1 calc R . . C226 C 0.3271(12) 0.1386(5) 0.2831(12) 0.043(4) Uani 1 1 d . . . H22B H 0.3401 0.1182 0.2405 0.052 Uiso 1 1 calc R . . C231 C 0.1495(10) 0.0837(4) 0.1327(10) 0.028(3) Uani 1 1 d . . . C232 C 0.1990(11) 0.0582(4) 0.2168(11) 0.036(3) Uani 1 1 d . . . H23C H 0.2089 0.0673 0.2849 0.044 Uiso 1 1 calc R . . C233 C 0.2340(11) 0.0199(4) 0.2030(13) 0.040(3) Uani 1 1 d . . . H23D H 0.2697 0.0030 0.2613 0.048 Uiso 1 1 calc R . . C234 C 0.2170(14) 0.0066(5) 0.1053(15) 0.054(4) Uani 1 1 d . . . H23E H 0.2400 -0.0197 0.0949 0.065 Uiso 1 1 calc R . . C235 C 0.1667(17) 0.0314(5) 0.0224(14) 0.062(5) Uani 1 1 d . . . H23B H 0.1554 0.0221 -0.0457 0.074 Uiso 1 1 calc R . . C236 C 0.1325(14) 0.0694(5) 0.0357(12) 0.047(4) Uani 1 1 d . . . H23A H 0.0965 0.0859 -0.0233 0.057 Uiso 1 1 calc R . . C311 C 0.2086(11) 0.0691(4) 0.5550(9) 0.032(3) Uani 1 1 d . . . C312 C 0.2146(13) 0.0343(4) 0.6125(12) 0.047(4) Uani 1 1 d . . . H31D H 0.1648 0.0301 0.6475 0.056 Uiso 1 1 calc R . . C313 C 0.2939(16) 0.0059(5) 0.6178(15) 0.065(5) Uani 1 1 d . . . H31E H 0.2977 -0.0184 0.6556 0.077 Uiso 1 1 calc R . . C314 C 0.3671(17) 0.0120(6) 0.5698(16) 0.071(6) Uani 1 1 d . . . H31A H 0.4226 -0.0077 0.5759 0.085 Uiso 1 1 calc R . . C315 C 0.3614(16) 0.0465(6) 0.5126(14) 0.065(5) Uani 1 1 d . . . H31B H 0.4121 0.0508 0.4785 0.078 Uiso 1 1 calc R . . C316 C 0.2806(13) 0.0750(5) 0.5053(12) 0.046(4) Uani 1 1 d . . . H31C H 0.2752 0.0988 0.4653 0.055 Uiso 1 1 calc R . . C321 C 0.0202(11) 0.0921(4) 0.6150(9) 0.028(3) Uani 1 1 d . . . C322 C -0.0555(12) 0.0606(4) 0.5851(11) 0.039(3) Uani 1 1 d . . . H32A H -0.0670 0.0458 0.5232 0.047 Uiso 1 1 calc R . . C323 C -0.1142(14) 0.0515(5) 0.6479(12) 0.049(4) Uani 1 1 d . . . H32E H -0.1660 0.0298 0.6294 0.059 Uiso 1 1 calc R . . C324 C -0.0984(14) 0.0731(5) 0.7361(12) 0.046(4) Uani 1 1 d . . . H32D H -0.1392 0.0663 0.7785 0.056 Uiso 1 1 calc R . . C325 C -0.0251(14) 0.1042(4) 0.7638(11) 0.044(4) Uani 1 1 d . . . H32C H -0.0154 0.1192 0.8250 0.053 Uiso 1 1 calc R . . C326 C 0.0358(12) 0.1141(4) 0.7032(10) 0.038(3) Uani 1 1 d . . . H32B H 0.0874 0.1358 0.7226 0.046 Uiso 1 1 calc R . . C331 C 0.1608(11) 0.1546(4) 0.5809(9) 0.028(3) Uani 1 1 d . . . C332 C 0.2765(12) 0.1581(4) 0.6367(12) 0.042(3) Uani 1 1 d . . . H33B H 0.3232 0.1351 0.6465 0.051 Uiso 1 1 calc R . . C333 C 0.3209(13) 0.1949(5) 0.6764(11) 0.045(4) Uani 1 1 d . . . H33E H 0.3985 0.1973 0.7140 0.055 Uiso 1 1 calc R . . C334 C 0.2535(14) 0.2288(4) 0.6623(11) 0.045(4) Uani 1 1 d . . . H33C H 0.2851 0.2543 0.6895 0.053 Uiso 1 1 calc R . . C335 C 0.1411(12) 0.2255(4) 0.6090(11) 0.037(3) Uani 1 1 d . . . H33A H 0.0948 0.2486 0.6003 0.044 Uiso 1 1 calc R . . C336 C 0.0947(11) 0.1882(4) 0.5674(10) 0.032(3) Uani 1 1 d . . . H33D H 0.0170 0.1861 0.5297 0.039 Uiso 1 1 calc R . . C1S C -0.3133(18) 0.1473(7) -0.2570(14) 0.086(7) Uani 1 1 d . . . H1SA H -0.3271 0.1424 -0.1922 0.104 Uiso 1 1 calc R . . H1SB H -0.2335 0.1423 -0.2419 0.104 Uiso 1 1 calc R . . Cl1B Cl -0.3436(6) 0.1969(2) -0.2940(5) 0.0941(18) Uani 1 1 d . . . Cl1A Cl -0.3929(6) 0.1131(2) -0.3531(5) 0.104(2) Uani 1 1 d . . . C2S C 0.4400(18) 0.1050(6) -0.0844(17) 0.080(6) Uani 1 1 d . . . H2SA H 0.4862 0.0964 -0.0128 0.096 Uiso 1 1 calc R . . H2SB H 0.4386 0.1349 -0.0860 0.096 Uiso 1 1 calc R . . Cl2B Cl 0.4992(6) 0.0877(2) -0.1687(6) 0.0998(19) Uani 1 1 d . . . Cl2A Cl 0.3068(5) 0.0872(2) -0.1148(7) 0.110(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 Ir1 0.0192(2) 0.0222(2) 0.0214(2) 0.00068(19) 0.00331(17) -0.00137(19) Cl1 0.0274(15) 0.0273(15) 0.0300(16) 0.0039(12) 0.0062(13) 0.0014(12) Cl2 0.0329(17) 0.0387(18) 0.0249(15) -0.0041(13) 0.0015(13) -0.0010(14) P1 0.0209(16) 0.0256(17) 0.0279(16) -0.0001(13) 0.0051(13) 0.0003(12) P2 0.0215(15) 0.0294(16) 0.0233(15) -0.0004(13) 0.0074(12) -0.0011(13) P3 0.0313(18) 0.0262(17) 0.0236(16) 0.0020(13) 0.0054(13) 0.0007(14) O1 0.142(14) 0.043(7) 0.055(8) 0.004(6) 0.020(8) -0.017(8) C1 0.030(6) 0.025(6) 0.019(6) 0.000(5) 0.012(5) 0.000(5) C2 0.026(6) 0.034(7) 0.026(6) 0.006(5) 0.015(5) 0.001(5) C3 0.051(9) 0.020(7) 0.040(8) 0.008(6) 0.013(7) -0.005(6) C4 0.020(6) 0.021(6) 0.031(6) 0.007(5) 0.001(5) -0.003(5) C5 0.039(8) 0.019(7) 0.056(9) -0.002(6) 0.006(7) -0.002(6) C111 0.025(7) 0.022(6) 0.038(7) -0.003(5) 0.004(6) 0.001(5) C112 0.028(7) 0.038(8) 0.041(8) 0.004(6) 0.000(6) -0.001(6) C113 0.043(9) 0.051(9) 0.036(8) 0.011(7) 0.012(7) 0.003(7) C114 0.051(10) 0.049(10) 0.050(10) -0.004(8) -0.012(8) 0.029(8) C115 0.024(8) 0.067(11) 0.060(11) -0.002(9) 0.001(7) 0.024(7) C116 0.044(9) 0.050(9) 0.044(9) 0.000(7) 0.016(7) 0.013(7) C121 0.017(6) 0.038(7) 0.032(7) -0.003(6) 0.007(5) 0.006(5) C122 0.027(7) 0.044(8) 0.043(8) -0.002(6) 0.012(6) -0.003(6) C123 0.030(7) 0.043(8) 0.052(9) -0.013(7) 0.015(7) -0.005(6) C124 0.036(8) 0.062(10) 0.039(8) -0.016(7) 0.022(7) -0.005(7) C125 0.044(9) 0.063(11) 0.037(8) 0.001(7) 0.017(7) 0.005(8) C126 0.031(7) 0.035(8) 0.042(8) 0.006(6) 0.013(6) 0.006(6) C131 0.020(6) 0.032(7) 0.032(7) 0.004(5) 0.003(5) -0.007(5) C132 0.019(6) 0.037(8) 0.063(10) -0.003(7) 0.016(6) -0.003(5) C133 0.024(7) 0.053(10) 0.072(11) 0.011(8) 0.020(7) -0.009(7) C134 0.023(7) 0.039(8) 0.068(11) 0.003(7) 0.008(7) -0.011(6) C135 0.046(9) 0.034(8) 0.054(10) -0.014(7) 0.002(7) -0.008(7) C136 0.027(7) 0.049(9) 0.036(8) -0.011(7) 0.001(6) -0.006(6) C211 0.046(8) 0.025(7) 0.031(7) -0.005(5) 0.017(6) -0.004(6) C212 0.038(8) 0.041(8) 0.047(9) 0.001(7) 0.018(7) -0.006(6) C213 0.047(9) 0.049(9) 0.059(10) -0.003(8) 0.027(8) -0.009(8) C214 0.053(10) 0.037(8) 0.048(9) 0.001(7) 0.025(8) -0.016(7) C215 0.055(9) 0.036(8) 0.028(7) 0.001(6) 0.010(7) -0.001(7) C216 0.043(8) 0.033(7) 0.027(7) 0.004(6) 0.011(6) -0.002(6) C221 0.019(6) 0.032(7) 0.023(6) 0.003(5) 0.010(5) -0.005(5) C222 0.025(7) 0.029(7) 0.032(7) 0.000(5) 0.005(5) -0.002(5) C223 0.040(8) 0.029(7) 0.043(8) -0.010(6) 0.012(7) -0.007(6) C224 0.033(8) 0.055(10) 0.037(8) -0.007(7) 0.002(6) -0.014(7) C225 0.013(6) 0.047(9) 0.067(10) -0.011(8) 0.004(6) -0.003(6) C226 0.031(8) 0.049(9) 0.047(9) -0.004(7) 0.010(6) 0.004(6) C231 0.020(6) 0.029(7) 0.036(7) 0.001(5) 0.012(5) -0.002(5) C232 0.026(7) 0.039(8) 0.045(8) -0.001(6) 0.014(6) -0.004(6) C233 0.028(7) 0.033(8) 0.059(10) 0.007(7) 0.017(7) 0.000(6) C234 0.056(10) 0.036(9) 0.080(13) -0.001(9) 0.037(9) -0.004(7) C235 0.097(15) 0.043(10) 0.056(11) -0.025(8) 0.040(10) -0.019(9) C236 0.062(10) 0.037(8) 0.040(8) -0.005(7) 0.015(7) -0.012(7) C311 0.032(7) 0.032(7) 0.022(6) 0.003(5) -0.001(5) 0.007(6) C312 0.042(9) 0.038(8) 0.048(9) 0.009(7) 0.002(7) 0.003(7) C313 0.058(12) 0.043(10) 0.073(13) 0.009(9) 0.002(10) 0.011(9) C314 0.060(12) 0.058(12) 0.077(13) 0.011(10) 0.005(10) 0.037(10) C315 0.058(11) 0.079(13) 0.057(11) -0.014(10) 0.021(9) 0.020(10) C316 0.043(9) 0.054(10) 0.038(8) -0.005(7) 0.011(7) 0.002(7) C321 0.032(7) 0.029(7) 0.025(6) 0.008(5) 0.013(5) 0.002(5) C322 0.047(9) 0.032(7) 0.036(8) -0.002(6) 0.013(7) -0.003(6) C323 0.057(10) 0.046(9) 0.044(9) 0.006(7) 0.021(8) -0.008(8) C324 0.059(10) 0.048(9) 0.041(9) 0.014(7) 0.028(8) -0.004(8) C325 0.067(11) 0.033(8) 0.026(7) 0.004(6) 0.011(7) 0.002(7) C326 0.044(8) 0.041(8) 0.026(7) 0.002(6) 0.007(6) -0.004(6) C331 0.031(7) 0.033(7) 0.015(6) 0.003(5) 0.003(5) 0.001(5) C332 0.039(8) 0.038(8) 0.046(9) -0.006(7) 0.011(7) 0.005(6) C333 0.036(8) 0.054(10) 0.035(8) -0.014(7) 0.001(6) -0.014(7) C334 0.067(11) 0.033(8) 0.032(8) -0.012(6) 0.017(7) -0.013(7) C335 0.050(9) 0.026(7) 0.036(8) -0.002(6) 0.018(7) 0.006(6) C336 0.033(7) 0.034(7) 0.028(7) 0.001(6) 0.008(6) 0.005(6) C1S 0.071(14) 0.13(2) 0.037(10) -0.006(11) -0.005(9) 0.012(13) Cl1B 0.098(4) 0.116(5) 0.077(4) 0.006(3) 0.044(3) -0.002(4) Cl1A 0.092(4) 0.139(6) 0.077(4) -0.015(4) 0.029(3) -0.041(4) C2S 0.084(15) 0.064(13) 0.073(14) -0.002(10) 0.005(11) -0.006(11) Cl2B 0.086(4) 0.116(5) 0.112(5) 0.009(4) 0.053(4) 0.008(4) Cl2A 0.061(3) 0.110(5) 0.167(7) -0.017(5) 0.052(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.986(11) . ? Ir1 C4 2.026(11) . ? Ir1 P1 2.324(3) . ? Ir1 P2 2.339(3) . ? Ir1 Cl1 2.471(3) . ? Ir1 Cl2 2.477(3) . ? P1 C121 1.809(13) . ? P1 C131 1.822(12) . ? P1 C111 1.827(13) . ? P2 C231 1.816(13) . ? P2 C211 1.833(13) . ? P2 C221 1.840(12) . ? P3 C2 1.759(12) . ? P3 C311 1.785(13) . ? P3 C331 1.788(13) . ? P3 C321 1.813(12) . ? O1 C3 1.331(17) . ? C1 C2 1.329(16) . ? C2 C3 1.482(18) . ? C3 C4 1.502(18) . ? C4 C5 1.281(18) . ? C111 C112 1.36(2) . ? C111 C116 1.39(2) . ? C112 C113 1.373(19) . ? C113 C114 1.36(2) . ? C114 C115 1.32(2) . ? C115 C116 1.38(2) . ? C121 C126 1.364(18) . ? C121 C122 1.389(19) . ? C122 C123 1.37(2) . ? C123 C124 1.35(2) . ? C124 C125 1.33(2) . ? C125 C126 1.35(2) . ? C131 C132 1.379(19) . ? C131 C136 1.377(19) . ? C132 C133 1.361(19) . ? C133 C134 1.34(2) . ? C134 C135 1.38(2) . ? C135 C136 1.39(2) . ? C211 C216 1.367(19) . ? C211 C212 1.40(2) . ? C212 C213 1.36(2) . ? C213 C214 1.33(2) . ? C214 C215 1.37(2) . ? C215 C216 1.380(19) . ? C221 C222 1.369(17) . ? C221 C226 1.386(18) . ? C222 C223 1.347(18) . ? C223 C224 1.36(2) . ? C224 C225 1.38(2) . ? C225 C226 1.381(19) . ? C231 C236 1.348(19) . ? C231 C232 1.371(18) . ? C232 C233 1.368(19) . ? C233 C234 1.34(2) . ? C234 C235 1.35(2) . ? C235 C236 1.35(2) . ? C311 C316 1.35(2) . ? C311 C312 1.371(19) . ? C312 C313 1.36(2) . ? C313 C314 1.35(3) . ? C314 C315 1.36(3) . ? C315 C316 1.37(2) . ? C321 C326 1.357(18) . ? C321 C322 1.368(18) . ? C322 C323 1.37(2) . ? C323 C324 1.35(2) . ? C324 C325 1.34(2) . ? C325 C326 1.37(2) . ? C331 C336 1.359(18) . ? C331 C332 1.400(19) . ? C332 C333 1.36(2) . ? C333 C334 1.37(2) . ? C334 C335 1.36(2) . ? C335 C336 1.383(18) . ? C1S Cl1B 1.70(2) . ? C1S Cl1A 1.74(2) . ? C2S Cl2A 1.70(2) . ? C2S Cl2B 1.70(2) . ? 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 Ir1 C4 81.0(5) . . ? C1 Ir1 P1 89.1(3) . . ? C4 Ir1 P1 94.5(4) . . ? C1 Ir1 P2 94.3(3) . . ? C4 Ir1 P2 92.5(4) . . ? P1 Ir1 P2 172.64(11) . . ? C1 Ir1 Cl1 89.3(3) . . ? C4 Ir1 Cl1 170.2(4) . . ? P1 Ir1 Cl1 85.02(11) . . ? P2 Ir1 Cl1 88.49(11) . . ? C1 Ir1 Cl2 170.6(3) . . ? C4 Ir1 Cl2 89.8(4) . . ? P1 Ir1 Cl2 92.78(11) . . ? P2 Ir1 Cl2 84.91(11) . . ? Cl1 Ir1 Cl2 100.01(10) . . ? C121 P1 C131 105.0(6) . . ? C121 P1 C111 102.2(6) . . ? C131 P1 C111 99.0(6) . . ? C121 P1 Ir1 113.1(4) . . ? C131 P1 Ir1 119.3(4) . . ? C111 P1 Ir1 116.0(5) . . ? C231 P2 C211 103.2(6) . . ? C231 P2 C221 102.1(6) . . ? C211 P2 C221 102.1(6) . . ? C231 P2 Ir1 115.8(4) . . ? C211 P2 Ir1 115.8(5) . . ? C221 P2 Ir1 115.8(4) . . ? C2 P3 C311 107.5(6) . . ? C2 P3 C331 111.5(6) . . ? C311 P3 C331 109.1(6) . . ? C2 P3 C321 113.7(6) . . ? C311 P3 C321 108.7(6) . . ? C331 P3 C321 106.1(6) . . ? C2 C1 Ir1 117.4(9) . . ? C1 C2 C3 115.4(11) . . ? C1 C2 P3 123.9(10) . . ? C3 C2 P3 120.6(9) . . ? O1 C3 C2 116.9(12) . . ? O1 C3 C4 119.9(13) . . ? C2 C3 C4 109.4(10) . . ? C5 C4 C3 118.2(12) . . ? C5 C4 Ir1 131.4(11) . . ? C3 C4 Ir1 110.5(8) . . ? C112 C111 C116 120.2(13) . . ? C112 C111 P1 121.2(10) . . ? C116 C111 P1 118.4(11) . . ? C111 C112 C113 118.9(14) . . ? C114 C113 C112 121.6(15) . . ? C115 C114 C113 118.8(14) . . ? C114 C115 C116 122.5(15) . . ? C115 C116 C111 118.0(15) . . ? C126 C121 C122 117.8(13) . . ? C126 C121 P1 124.7(11) . . ? C122 C121 P1 117.4(10) . . ? C123 C122 C121 119.5(14) . . ? C124 C123 C122 120.3(14) . . ? C125 C124 C123 120.4(14) . . ? C124 C125 C126 120.7(15) . . ? C125 C126 C121 121.3(14) . . ? C132 C131 C136 118.7(12) . . ? C132 C131 P1 122.8(11) . . ? C136 C131 P1 118.3(10) . . ? C133 C132 C131 120.8(14) . . ? C134 C133 C132 121.0(14) . . ? C133 C134 C135 119.9(13) . . ? C134 C135 C136 120.1(15) . . ? C131 C136 C135 119.5(14) . . ? C216 C211 C212 118.8(13) . . ? C216 C211 P2 123.0(11) . . ? C212 C211 P2 118.2(11) . . ? C213 C212 C211 118.7(14) . . ? C214 C213 C212 122.9(15) . . ? C213 C214 C215 119.0(14) . . ? C214 C215 C216 120.4(14) . . ? C211 C216 C215 120.1(14) . . ? C222 C221 C226 120.0(12) . . ? C222 C221 P2 118.6(9) . . ? C226 C221 P2 121.4(10) . . ? C223 C222 C221 120.2(13) . . ? C222 C223 C224 121.7(13) . . ? C223 C224 C225 118.6(13) . . ? C224 C225 C226 120.8(13) . . ? C225 C226 C221 118.5(14) . . ? C236 C231 C232 118.2(13) . . ? C236 C231 P2 122.1(11) . . ? C232 C231 P2 119.5(10) . . ? C233 C232 C231 120.9(14) . . ? C234 C233 C232 119.5(15) . . ? C233 C234 C235 119.6(15) . . ? C236 C235 C234 121.1(16) . . ? C231 C236 C235 120.6(15) . . ? C316 C311 C312 120.3(14) . . ? C316 C311 P3 117.9(11) . . ? C312 C311 P3 121.6(12) . . ? C313 C312 C311 118.7(17) . . ? C314 C313 C312 121.1(17) . . ? C313 C314 C315 120.3(17) . . ? C314 C315 C316 118.9(19) . . ? C311 C316 C315 120.6(16) . . ? C326 C321 C322 121.3(13) . . ? C326 C321 P3 118.6(10) . . ? C322 C321 P3 120.1(10) . . ? C323 C322 C321 118.1(14) . . ? C324 C323 C322 120.8(15) . . ? C325 C324 C323 120.5(14) . . ? C324 C325 C326 120.3(14) . . ? C321 C326 C325 118.9(14) . . ? C336 C331 C332 119.4(12) . . ? C336 C331 P3 120.2(10) . . ? C332 C331 P3 120.4(10) . . ? C333 C332 C331 119.7(14) . . ? C332 C333 C334 120.7(14) . . ? C335 C334 C333 119.9(13) . . ? C334 C335 C336 120.1(13) . . ? C331 C336 C335 120.3(13) . . ? Cl1B C1S Cl1A 112.4(11) . . ? Cl2A C2S Cl2B 112.4(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.528 _refine_diff_density_min -5.329 _refine_diff_density_rms 0.190 # Attachment 'complex 3.cif' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 633229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H72 Cl2 P3 O Ir, C4H10O' _chemical_formula_sum 'C51 H82 Cl2 Ir O2 P3' _chemical_formula_weight 1083.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 21.421(4) _cell_length_b 14.267(3) _cell_length_c 18.226(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.765(3) _cell_angle_gamma 90.00 _cell_volume 5333.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8087 _cell_measurement_theta_min 0 _cell_measurement_theta_max 25 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 2.729 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.793468 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20742 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9151 _reflns_number_gt 8087 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0058P)^2^+8.3517P] 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 0.020(9) _refine_ls_number_reflns 9151 _refine_ls_number_parameters 532 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.008 _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 0.331330(13) 0.249460(5) 0.205840(14) 0.02900(2) Uani 1 1 d . . . P1 P 0.25483(3) 0.36694(4) 0.20075(3) 0.03942(17) Uani 1 1 d . . . P2 P 0.41505(3) 0.14127(4) 0.21233(3) 0.03535(17) Uani 1 1 d . . . P3 P 0.18207(3) 0.02365(4) 0.09407(3) 0.02760(14) Uani 1 1 d . . . Cl1 Cl 0.40778(3) 0.38058(4) 0.21553(3) 0.04072(16) Uani 1 1 d . . . Cl2 Cl 0.35322(3) 0.24384(4) 0.34716(3) 0.03922(18) Uani 1 1 d . . . O1 O 0.23445(8) 0.15102(11) -0.01100(8) 0.0440(5) Uani 1 1 d . . . C1 C 0.26625(9) 0.14866(13) 0.18958(10) 0.0233(5) Uani 1 1 d . . . H1A H 0.2554 0.1215 0.2313 0.028 Uiso 1 1 calc R . . C2 C 0.23733(9) 0.11912(15) 0.11737(10) 0.0277(6) Uani 1 1 d . . . C3 C 0.25671(10) 0.16800(15) 0.05764(11) 0.0301(6) Uani 1 1 d . . . C4 C 0.30715(12) 0.24305(12) 0.08784(13) 0.0259(6) Uani 1 1 d . . . C5 C 0.32718(12) 0.2912(2) 0.03943(13) 0.0432(7) Uani 1 1 d . . . H5A H 0.3104 0.2792 -0.0133 0.052 Uiso 1 1 calc R . . H5B H 0.3586 0.3384 0.0568 0.052 Uiso 1 1 calc R . . C111 C 0.28012(14) 0.45366(18) 0.27729(15) 0.0550(9) Uani 1 1 d . . . H11E H 0.2884 0.4208 0.3264 0.066 Uiso 1 1 calc R . . H11I H 0.3217 0.4806 0.2752 0.066 Uiso 1 1 calc R . . C112 C 0.23398(18) 0.5330(2) 0.2771(2) 0.0889(13) Uani 1 1 d . . . H11A H 0.2212 0.5617 0.2261 0.107 Uiso 1 1 calc R . . H11B H 0.1945 0.5075 0.2866 0.107 Uiso 1 1 calc R . . C113 C 0.26059(19) 0.6060(2) 0.3339(2) 0.0937(14) Uani 1 1 d D . . H11C H 0.3021 0.6282 0.3279 0.112 Uiso 1 1 calc R . . H11D H 0.2690 0.5796 0.3855 0.112 Uiso 1 1 calc R . . C114 C 0.21238(17) 0.6902(3) 0.3246(2) 0.0852(13) Uani 1 1 d D . . H11F H 0.2326 0.7397 0.3600 0.128 Uiso 1 1 calc R . . H11G H 0.1729 0.6696 0.3356 0.128 Uiso 1 1 calc R . . H11H H 0.2017 0.7137 0.2725 0.128 Uiso 1 1 calc R . . C121 C 0.17484(12) 0.3316(2) 0.20486(14) 0.0515(8) Uani 1 1 d . . . H12E H 0.1462 0.3865 0.1942 0.062 Uiso 1 1 calc R . . H12I H 0.1573 0.2859 0.1639 0.062 Uiso 1 1 calc R . . C122 C 0.17201(14) 0.2893(3) 0.27942(16) 0.0608(9) Uani 1 1 d . . . H12C H 0.1887 0.3347 0.3208 0.073 Uiso 1 1 calc R . . H12D H 0.2002 0.2338 0.2906 0.073 Uiso 1 1 calc R . . C123 C 0.1021(2) 0.2611(3) 0.2770(2) 0.0897(17) Uani 1 1 d . . . H12A H 0.0729 0.3148 0.2602 0.108 Uiso 1 1 calc R . . H12B H 0.0872 0.2104 0.2397 0.108 Uiso 1 1 calc R . . C124 C 0.09848(19) 0.2293(2) 0.3538(2) 0.0708(12) Uani 1 1 d . . . H12F H 0.0541 0.2106 0.3501 0.106 Uiso 1 1 calc R . . H12G H 0.1115 0.2802 0.3903 0.106 Uiso 1 1 calc R . . H12H H 0.1275 0.1764 0.3707 0.106 Uiso 1 1 calc R . . C131 C 0.23919(14) 0.4414(2) 0.11437(15) 0.0581(9) Uani 1 1 d . . . H13A H 0.2325 0.5059 0.1290 0.070 Uiso 1 1 calc R . . H13B H 0.2783 0.4411 0.0968 0.070 Uiso 1 1 calc R . . C132 C 0.18256(15) 0.4142(3) 0.04883(17) 0.0830(12) Uani 1 1 d . . . H13E H 0.1435 0.4089 0.0663 0.100 Uiso 1 1 calc R . . H13F H 0.1908 0.3529 0.0293 0.100 Uiso 1 1 calc R . . C133 C 0.17098(16) 0.4865(2) -0.01497(18) 0.0783(12) Uani 1 1 d D . . H13C H 0.1648 0.5481 0.0055 0.094 Uiso 1 1 calc R . . H13D H 0.2096 0.4899 -0.0333 0.094 Uiso 1 1 calc R . . C134 C 0.11191(17) 0.4633(3) -0.0818(2) 0.0925(14) Uani 1 1 d D . . H13G H 0.1059 0.5118 -0.1206 0.139 Uiso 1 1 calc R . . H13H H 0.0735 0.4599 -0.0640 0.139 Uiso 1 1 calc R . . H13I H 0.1186 0.4035 -0.1037 0.139 Uiso 1 1 calc R . . C211 C 0.39387(11) 0.04917(17) 0.13952(12) 0.0397(7) Uani 1 1 d . . . H21E H 0.3572 0.0135 0.1472 0.048 Uiso 1 1 calc R . . H21F H 0.3786 0.0793 0.0892 0.048 Uiso 1 1 calc R . . C212 C 0.44697(12) -0.01920(18) 0.13746(14) 0.0479(8) Uani 1 1 d . . . H21A H 0.4631 -0.0500 0.1875 0.057 Uiso 1 1 calc R . . H21B H 0.4834 0.0148 0.1274 0.057 Uiso 1 1 calc R . . C213 C 0.42215(13) -0.0929(2) 0.07577(15) 0.0565(9) Uani 1 1 d . . . H21C H 0.3886 -0.1304 0.0890 0.068 Uiso 1 1 calc R . . H21D H 0.4015 -0.0612 0.0271 0.068 Uiso 1 1 calc R . . C214 C 0.47388(15) -0.1575(2) 0.06485(18) 0.0784(11) Uani 1 1 d . . . H21G H 0.4545 -0.2020 0.0245 0.118 Uiso 1 1 calc R . . H21H H 0.4936 -0.1910 0.1122 0.118 Uiso 1 1 calc R . . H21I H 0.5070 -0.1213 0.0508 0.118 Uiso 1 1 calc R . . C221 C 0.49267(11) 0.1875(2) 0.20550(14) 0.0499(8) Uani 1 1 d . . . H22C H 0.5064 0.2385 0.2426 0.060 Uiso 1 1 calc R . . H22D H 0.5256 0.1379 0.2200 0.060 Uiso 1 1 calc R . . C222 C 0.49139(14) 0.2237(2) 0.12717(19) 0.0622(9) Uani 1 1 d . . . H22A H 0.4659 0.1803 0.0883 0.075 Uiso 1 1 calc R . . H22B H 0.4690 0.2844 0.1190 0.075 Uiso 1 1 calc R . . C223 C 0.55688(18) 0.2355(2) 0.1156(2) 0.0755(13) Uani 1 1 d D . . H22J H 0.5845 0.2696 0.1598 0.091 Uiso 1 1 calc R . . H22K H 0.5521 0.2750 0.0703 0.091 Uiso 1 1 calc R . . C224 C 0.59201(17) 0.1481(2) 0.1055(2) 0.0871(13) Uani 1 1 d D . . H22L H 0.6338 0.1644 0.0983 0.131 Uiso 1 1 calc R . . H22M H 0.5662 0.1142 0.0610 0.131 Uiso 1 1 calc R . . H22N H 0.5989 0.1090 0.1507 0.131 Uiso 1 1 calc R . . C231 C 0.44302(11) 0.07468(17) 0.30208(12) 0.0406(7) Uani 1 1 d . . . H23A H 0.4818 0.0389 0.3010 0.049 Uiso 1 1 calc R . . H23B H 0.4564 0.1194 0.3445 0.049 Uiso 1 1 calc R . . C232 C 0.39461(12) 0.00786(19) 0.31901(13) 0.0469(8) Uani 1 1 d . . . H23H H 0.3588 0.0438 0.3286 0.056 Uiso 1 1 calc R . . H23I H 0.3763 -0.0318 0.2740 0.056 Uiso 1 1 calc R . . C233 C 0.42457(13) -0.0531(2) 0.38681(15) 0.0649(10) Uani 1 1 d . . . H23F H 0.4449 -0.0132 0.4310 0.078 Uiso 1 1 calc R . . H23G H 0.4590 -0.0911 0.3760 0.078 Uiso 1 1 calc R . . C234 C 0.37587(15) -0.1176(2) 0.40715(16) 0.0769(11) Uani 1 1 d . . . H23C H 0.3978 -0.1544 0.4519 0.115 Uiso 1 1 calc R . . H23D H 0.3569 -0.1591 0.3644 0.115 Uiso 1 1 calc R . . H23E H 0.3417 -0.0804 0.4182 0.115 Uiso 1 1 calc R . . C311 C 0.10924(10) 0.05676(16) 0.02048(11) 0.0327(6) Uani 1 1 d . . . C312 C 0.09094(11) 0.14798(18) 0.01052(12) 0.0437(7) Uani 1 1 d . . . H31C H 0.1165 0.1951 0.0410 0.052 Uiso 1 1 calc R . . C313 C 0.03380(13) 0.1704(2) -0.04553(14) 0.0619(9) Uani 1 1 d . . . H31E H 0.0208 0.2335 -0.0527 0.074 Uiso 1 1 calc R . . C314 C -0.00331(12) 0.1046(2) -0.08972(14) 0.0653(10) Uani 1 1 d . . . H31D H -0.0423 0.1209 -0.1269 0.078 Uiso 1 1 calc R . . C315 C 0.01642(12) 0.0141(2) -0.07974(15) 0.0658(10) Uani 1 1 d . . . H31B H -0.0086 -0.0322 -0.1118 0.079 Uiso 1 1 calc R . . C316 C 0.07174(11) -0.01181(19) -0.02436(12) 0.0459(8) Uani 1 1 d . . . H31A H 0.0839 -0.0752 -0.0171 0.055 Uiso 1 1 calc R . . C321 C 0.21643(9) -0.07508(16) 0.05803(11) 0.0315(6) Uani 1 1 d . . . C322 C 0.22242(12) -0.16221(18) 0.09221(14) 0.0478(8) Uani 1 1 d . . . H32E H 0.2079 -0.1719 0.1356 0.057 Uiso 1 1 calc R . . C323 C 0.24968(18) -0.23470(18) 0.0624(2) 0.0606(11) Uani 1 1 d . . . H32C H 0.2563 -0.2929 0.0877 0.073 Uiso 1 1 calc R . . C324 C 0.26723(13) -0.2235(2) -0.00296(17) 0.0559(8) Uani 1 1 d . . . H32B H 0.2845 -0.2742 -0.0237 0.067 Uiso 1 1 calc R . . C325 C 0.25961(12) -0.13857(19) -0.03823(14) 0.0534(8) Uani 1 1 d . . . H32A H 0.2715 -0.1306 -0.0836 0.064 Uiso 1 1 calc R . . C326 C 0.23469(11) -0.06460(18) -0.00791(13) 0.0432(7) Uani 1 1 d . . . H32D H 0.2300 -0.0060 -0.0324 0.052 Uiso 1 1 calc R . . C331 C 0.16017(10) -0.01203(15) 0.17787(10) 0.0297(6) Uani 1 1 d . . . C332 C 0.20800(11) -0.04405(16) 0.24231(11) 0.0352(6) Uani 1 1 d . . . H33A H 0.2519 -0.0460 0.2423 0.042 Uiso 1 1 calc R . . C333 C 0.19094(12) -0.07255(17) 0.30533(12) 0.0436(7) Uani 1 1 d . . . H33D H 0.2233 -0.0936 0.3489 0.052 Uiso 1 1 calc R . . C334 C 0.12750(12) -0.07088(19) 0.30577(13) 0.0507(8) Uani 1 1 d . . . H33B H 0.1162 -0.0916 0.3492 0.061 Uiso 1 1 calc R . . C335 C 0.07997(11) -0.03892(19) 0.24265(14) 0.0505(8) Uani 1 1 d . . . H33C H 0.0363 -0.0361 0.2435 0.061 Uiso 1 1 calc R . . C336 C 0.09621(11) -0.01131(17) 0.17872(12) 0.0390(7) Uani 1 1 d . . . H33E H 0.0634 0.0083 0.1350 0.047 Uiso 1 1 calc R . . O2 O 0.38842(11) -0.36345(17) 0.12044(12) 0.0827(8) Uani 1 1 d . . . C21B C 0.39657(19) -0.2833(3) 0.2338(2) 0.0856(13) Uani 1 1 d . . . H21J H 0.4233 -0.2767 0.2865 0.128 Uiso 1 1 calc R . . H21K H 0.3529 -0.3022 0.2330 0.128 Uiso 1 1 calc R . . H21L H 0.3947 -0.2237 0.2076 0.128 Uiso 1 1 calc R . . C21A C 0.4247(2) -0.3534(3) 0.1957(2) 0.0945(15) Uani 1 1 d . . . H21M H 0.4693 -0.3352 0.1980 0.113 Uiso 1 1 calc R . . H21N H 0.4267 -0.4136 0.2223 0.113 Uiso 1 1 calc R . . C22B C 0.37306(16) -0.4452(3) 0.00292(19) 0.0836(12) Uani 1 1 d . . . H22E H 0.3933 -0.4890 -0.0240 0.125 Uiso 1 1 calc R . . H22F H 0.3642 -0.3867 -0.0253 0.125 Uiso 1 1 calc R . . H22G H 0.3325 -0.4715 0.0073 0.125 Uiso 1 1 calc R . . C22A C 0.41643(16) -0.4280(2) 0.0784(2) 0.0789(11) Uani 1 1 d . . . H22H H 0.4259 -0.4874 0.1065 0.095 Uiso 1 1 calc R . . H22I H 0.4576 -0.4025 0.0739 0.095 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 0.03004(3) 0.03236(4) 0.02341(3) 0.00059(3) 0.00583(2) -0.00514(3) P1 0.0422(3) 0.0396(3) 0.0328(3) -0.0034(3) 0.0048(2) 0.0014(3) P2 0.0299(3) 0.0431(3) 0.0323(3) 0.0022(3) 0.0079(2) -0.0013(3) P3 0.0249(2) 0.0320(3) 0.0240(2) -0.0021(2) 0.00395(17) -0.0013(2) Cl1 0.0418(3) 0.0407(3) 0.0381(3) 0.0019(2) 0.0090(2) -0.0145(3) Cl2 0.0459(3) 0.0461(4) 0.0237(2) -0.0008(2) 0.0070(2) -0.0096(2) O1 0.0548(9) 0.0490(9) 0.0280(7) 0.0016(7) 0.0116(6) -0.0075(8) C1 0.0229(8) 0.0225(10) 0.0262(8) 0.0082(7) 0.0100(7) -0.0078(8) C2 0.0262(9) 0.0340(11) 0.0190(8) -0.0050(8) 0.0003(7) -0.0021(9) C3 0.0314(9) 0.0365(12) 0.0245(8) -0.0036(8) 0.0116(7) -0.0001(9) C4 0.0336(11) 0.0250(11) 0.0173(9) -0.0002(7) 0.0043(8) -0.0024(8) C5 0.0485(13) 0.0479(14) 0.0312(11) -0.0034(11) 0.0084(10) -0.0016(13) C111 0.0609(15) 0.0438(15) 0.0548(14) -0.0108(12) 0.0077(12) 0.0018(13) C112 0.093(2) 0.068(2) 0.091(2) -0.0233(18) 0.0034(19) 0.0135(19) C113 0.126(3) 0.0532(18) 0.085(2) -0.0245(16) 0.005(2) 0.017(2) C114 0.085(2) 0.085(3) 0.085(2) 0.000(2) 0.0241(17) 0.000(2) C121 0.0515(13) 0.0515(15) 0.0515(13) 0.0000(12) 0.0149(11) 0.0000(13) C122 0.0535(15) 0.0761(18) 0.0486(15) -0.0027(15) 0.0077(13) 0.0045(16) C123 0.068(2) 0.141(4) 0.059(2) 0.0131(18) 0.0160(18) -0.0038(19) C124 0.071(2) 0.071(2) 0.071(2) 0.0004(16) 0.0204(16) -0.0001(16) C131 0.0589(15) 0.0572(17) 0.0557(14) 0.0002(13) 0.0124(12) 0.0100(14) C132 0.0605(17) 0.116(3) 0.0681(17) 0.0387(17) 0.0119(14) 0.0228(19) C133 0.0782(19) 0.078(2) 0.0782(19) 0.0001(18) 0.0225(16) 0.0000(18) C134 0.092(2) 0.093(3) 0.092(2) 0.000(2) 0.0263(18) 0.000(2) C211 0.0430(12) 0.0446(14) 0.0311(10) 0.0022(10) 0.0100(9) 0.0059(11) C212 0.0382(12) 0.0507(15) 0.0541(13) -0.0098(12) 0.0122(10) 0.0022(11) C213 0.0539(14) 0.0613(17) 0.0553(13) -0.0054(13) 0.0174(11) 0.0030(13) C214 0.0841(19) 0.072(2) 0.0863(18) -0.0227(16) 0.0353(15) 0.0164(16) C221 0.0338(11) 0.0587(17) 0.0563(14) -0.0028(13) 0.0117(10) 0.0010(12) C222 0.0472(14) 0.0744(18) 0.0713(17) 0.0146(15) 0.0272(12) -0.0047(14) C223 0.0574(17) 0.098(3) 0.081(2) 0.0067(16) 0.0359(15) -0.0103(15) C224 0.087(2) 0.087(3) 0.087(2) 0.000(2) 0.0251(18) 0.000(2) C231 0.0352(11) 0.0518(14) 0.0300(10) 0.0118(10) 0.0018(9) 0.0054(11) C232 0.0446(12) 0.0581(16) 0.0361(11) 0.0030(11) 0.0085(10) 0.0014(12) C233 0.0574(15) 0.082(2) 0.0537(14) 0.0189(14) 0.0138(12) -0.0041(15) C234 0.0719(18) 0.096(2) 0.0604(15) 0.0339(15) 0.0157(14) 0.0007(18) C311 0.0268(10) 0.0454(13) 0.0229(9) -0.0025(9) 0.0027(8) 0.0034(9) C312 0.0489(12) 0.0435(14) 0.0375(11) -0.0028(10) 0.0106(10) 0.0099(11) C313 0.0585(15) 0.0807(19) 0.0431(13) 0.0137(13) 0.0092(12) 0.0330(14) C314 0.0339(12) 0.121(2) 0.0347(12) 0.0043(15) -0.0007(10) 0.0300(15) C315 0.0371(13) 0.105(2) 0.0452(14) -0.0178(15) -0.0049(11) 0.0126(15) C316 0.0406(13) 0.0549(15) 0.0337(11) -0.0084(10) -0.0029(10) -0.0054(12) C321 0.0229(9) 0.0369(12) 0.0333(10) -0.0062(9) 0.0057(8) -0.0028(9) C322 0.0531(13) 0.0428(14) 0.0472(12) -0.0044(11) 0.0142(10) 0.0074(12) C323 0.0643(19) 0.0403(15) 0.072(2) -0.0056(12) 0.0111(16) 0.0142(12) C324 0.0428(13) 0.0670(15) 0.0581(14) -0.0223(13) 0.0148(11) 0.0195(12) C325 0.0543(14) 0.0582(16) 0.0510(13) -0.0146(12) 0.0206(11) -0.0020(13) C326 0.0479(12) 0.0424(14) 0.0420(11) -0.0031(10) 0.0172(9) 0.0007(11) C331 0.0340(10) 0.0303(11) 0.0238(9) -0.0017(8) 0.0066(8) -0.0029(9) C332 0.0365(11) 0.0383(12) 0.0302(10) -0.0016(9) 0.0086(8) -0.0018(10) C333 0.0542(14) 0.0452(14) 0.0282(10) 0.0014(10) 0.0069(10) -0.0030(12) C334 0.0587(13) 0.0587(16) 0.0392(11) -0.0007(11) 0.0212(10) -0.0063(13) C335 0.0378(11) 0.0663(17) 0.0528(12) -0.0077(12) 0.0217(9) -0.0053(12) C336 0.0365(10) 0.0436(13) 0.0380(10) 0.0019(10) 0.0125(8) 0.0047(10) O2 0.0684(12) 0.1032(17) 0.0726(12) 0.0122(12) 0.0142(10) 0.0208(12) C21B 0.086(2) 0.086(2) 0.086(2) 0.000(2) 0.0246(19) 0.000(2) C21A 0.093(3) 0.073(2) 0.101(3) 0.011(2) 0.002(2) 0.007(2) C22B 0.0769(19) 0.089(2) 0.090(2) 0.0199(19) 0.0312(16) 0.0086(19) C22A 0.0650(18) 0.073(2) 0.096(2) 0.0378(17) 0.0188(16) 0.0080(17) _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 1.9650(19) . ? Ir C4 2.064(2) . ? Ir P1 2.3271(7) . ? Ir P2 2.3432(7) . ? Ir Cl1 2.4588(7) . ? Ir Cl2 2.4827(8) . ? P1 C121 1.808(3) . ? P1 C111 1.826(3) . ? P1 C131 1.848(3) . ? P2 C221 1.826(3) . ? P2 C211 1.829(2) . ? P2 C231 1.836(2) . ? P3 C2 1.774(2) . ? P3 C331 1.796(2) . ? P3 C321 1.799(2) . ? P3 C311 1.8025(19) . ? O1 C3 1.228(2) . ? C1 C2 1.350(2) . ? C2 C3 1.451(3) . ? C3 C4 1.508(3) . ? C4 C5 1.285(4) . ? C111 C112 1.502(4) . ? C112 C113 1.463(4) . ? C113 C114 1.561(5) . ? C121 C122 1.504(4) . ? C122 C123 1.540(6) . ? C123 C124 1.493(6) . ? C131 C132 1.488(4) . ? C132 C133 1.520(5) . ? C133 C134 1.518(4) . ? C211 C212 1.507(3) . ? C212 C213 1.519(4) . ? C213 C214 1.498(4) . ? C221 C222 1.511(4) . ? C222 C223 1.487(5) . ? C223 C224 1.495(5) . ? C231 C232 1.505(4) . ? C232 C233 1.496(4) . ? C233 C234 1.515(5) . ? C311 C312 1.356(3) . ? C311 C316 1.375(3) . ? C312 C313 1.387(3) . ? C313 C314 1.339(4) . ? C314 C315 1.355(5) . ? C315 C316 1.367(3) . ? C321 C326 1.375(3) . ? C321 C322 1.380(3) . ? C322 C323 1.374(4) . ? C323 C324 1.359(5) . ? C324 C325 1.359(4) . ? C325 C326 1.369(4) . ? C331 C336 1.375(3) . ? C331 C332 1.394(3) . ? C332 C333 1.364(3) . ? C333 C334 1.362(4) . ? C334 C335 1.376(3) . ? C335 C336 1.367(4) . ? O2 C21A 1.376(4) . ? O2 C22A 1.436(4) . ? C21B C21A 1.446(6) . ? C22B C22A 1.442(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 C1 Ir C4 81.75(8) . . ? C1 Ir P1 93.46(6) . . ? C4 Ir P1 91.62(6) . . ? C1 Ir P2 91.43(6) . . ? C4 Ir P2 88.96(7) . . ? P1 Ir P2 175.12(2) . . ? C1 Ir Cl1 175.21(5) . . ? C4 Ir Cl1 94.03(6) . . ? P1 Ir Cl1 84.36(3) . . ? P2 Ir Cl1 90.76(3) . . ? C1 Ir Cl2 92.65(6) . . ? C4 Ir Cl2 174.39(6) . . ? P1 Ir Cl2 89.12(2) . . ? P2 Ir Cl2 90.78(2) . . ? Cl1 Ir Cl2 91.57(2) . . ? C121 P1 C111 103.49(13) . . ? C121 P1 C131 104.75(12) . . ? C111 P1 C131 101.67(13) . . ? C121 P1 Ir 117.52(9) . . ? C111 P1 Ir 114.03(9) . . ? C131 P1 Ir 113.61(10) . . ? C221 P2 C211 104.48(12) . . ? C221 P2 C231 100.25(11) . . ? C211 P2 C231 102.92(11) . . ? C221 P2 Ir 117.22(10) . . ? C211 P2 Ir 114.24(7) . . ? C231 P2 Ir 115.73(8) . . ? C2 P3 C331 109.51(9) . . ? C2 P3 C321 111.94(10) . . ? C331 P3 C321 108.87(10) . . ? C2 P3 C311 110.58(10) . . ? C331 P3 C311 108.95(10) . . ? C321 P3 C311 106.92(9) . . ? C2 C1 Ir 118.78(15) . . ? C1 C2 C3 115.55(18) . . ? C1 C2 P3 124.05(16) . . ? C3 C2 P3 120.34(13) . . ? O1 C3 C2 123.97(19) . . ? O1 C3 C4 122.6(2) . . ? C2 C3 C4 113.42(16) . . ? C5 C4 C3 118.3(2) . . ? C5 C4 Ir 131.19(17) . . ? C3 C4 Ir 110.48(15) . . ? C112 C111 P1 117.33(19) . . ? C113 C112 C111 114.4(3) . . ? C112 C113 C114 111.1(3) . . ? C122 C121 P1 115.78(17) . . ? C121 C122 C123 111.8(2) . . ? C124 C123 C122 111.4(3) . . ? C132 C131 P1 116.1(2) . . ? C131 C132 C133 110.7(3) . . ? C134 C133 C132 112.4(3) . . ? C212 C211 P2 116.87(15) . . ? C211 C212 C213 111.16(19) . . ? C214 C213 C212 114.2(2) . . ? C222 C221 P2 114.79(17) . . ? C223 C222 C221 114.3(2) . . ? C222 C223 C224 116.9(3) . . ? C232 C231 P2 116.32(14) . . ? C233 C232 C231 112.4(2) . . ? C232 C233 C234 113.2(2) . . ? C312 C311 C316 120.42(19) . . ? C312 C311 P3 120.39(16) . . ? C316 C311 P3 119.18(18) . . ? C311 C312 C313 118.7(2) . . ? C314 C313 C312 121.8(3) . . ? C313 C314 C315 118.7(2) . . ? C314 C315 C316 121.8(3) . . ? C315 C316 C311 118.7(3) . . ? C326 C321 C322 118.7(2) . . ? C326 C321 P3 118.91(17) . . ? C322 C321 P3 122.35(18) . . ? C323 C322 C321 119.6(3) . . ? C324 C323 C322 121.0(3) . . ? C323 C324 C325 119.6(3) . . ? C324 C325 C326 120.3(3) . . ? C325 C326 C321 120.8(2) . . ? C336 C331 C332 119.1(2) . . ? C336 C331 P3 120.87(15) . . ? C332 C331 P3 120.04(17) . . ? C333 C332 C331 119.8(2) . . ? C334 C333 C332 120.7(2) . . ? C333 C334 C335 120.0(2) . . ? C336 C335 C334 120.0(2) . . ? C335 C336 C331 120.47(19) . . ? C21A O2 C22A 113.3(3) . . ? O2 C21A C21B 110.9(3) . . ? O2 C22A C22B 111.4(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.955 _refine_diff_density_min -0.975 _refine_diff_density_rms 0.084 # Attachment 'complex 4.cif' data_complex4 _database_code_depnum_ccdc_archive 'CCDC 633230' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C94 H142 Cl4 P6 O4 Ir2, 3CHCl3' _chemical_formula_sum 'C99 H147 Cl19 Ir2 O4 P6' _chemical_formula_weight 2644.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 14.197(2) _cell_length_b 19.240(3) _cell_length_c 23.412(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.442(3) _cell_angle_gamma 90.00 _cell_volume 6308.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 0 _cell_measurement_theta_max 26 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 2.628 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.696441 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48083 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12327 _reflns_number_gt 10822 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+6.8448P] 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 12327 _refine_ls_number_parameters 604 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.005 _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 0.068430(11) 0.280465(8) 0.063715(7) 0.02888(8) Uani 1 1 d . . . P1 P 0.18128(8) 0.33431(6) 0.13493(5) 0.0344(2) Uani 1 1 d . . . P2 P -0.04039(9) 0.23177(7) -0.01261(5) 0.0375(3) Uani 1 1 d . . . P3 P -0.18209(8) 0.33805(6) 0.15996(5) 0.0352(2) Uani 1 1 d . . . Cl1 Cl 0.10905(9) 0.16866(6) 0.10308(5) 0.0451(3) Uani 1 1 d . . . Cl2 Cl 0.19513(9) 0.26895(6) 0.00353(5) 0.0410(3) Uani 1 1 d . . . O1 O -0.1357(2) 0.45673(17) 0.10478(16) 0.0460(8) Uani 1 1 d . . . O2 O 0.0355(2) 0.37645(15) 0.02891(13) 0.0322(6) Uani 1 1 d . . . C1 C -0.0335(3) 0.2860(2) 0.10990(19) 0.0308(9) Uani 1 1 d . . . H1A H -0.0449 0.2457 0.1304 0.037 Uiso 1 1 calc R . . C2 C -0.0898(3) 0.3414(2) 0.11581(18) 0.0312(9) Uani 1 1 d . . . C3 C -0.0851(3) 0.4108(2) 0.08977(19) 0.0334(9) Uani 1 1 d . . . C4 C -0.0211(3) 0.4238(2) 0.04555(18) 0.0311(9) Uani 1 1 d . . . C5 C -0.0269(3) 0.4892(2) 0.02185(18) 0.0320(9) Uani 1 1 d . . . H5A H -0.0683 0.5215 0.0349 0.038 Uiso 1 1 calc R . . C111 C 0.2965(3) 0.2898(2) 0.1492(2) 0.0394(10) Uani 1 1 d . . . H11A H 0.2850 0.2413 0.1589 0.047 Uiso 1 1 calc R . . H11B H 0.3235 0.2895 0.1133 0.047 Uiso 1 1 calc R . . C112 C 0.3714(4) 0.3198(3) 0.1973(2) 0.0518(13) Uani 1 1 d . . . H11C H 0.3864 0.3675 0.1872 0.062 Uiso 1 1 calc R . . H11D H 0.3449 0.3214 0.2334 0.062 Uiso 1 1 calc R . . C113 C 0.4617(5) 0.2777(4) 0.2069(3) 0.0708(19) Uani 1 1 d . . . H11E H 0.4907 0.2792 0.1717 0.085 Uiso 1 1 calc R . . H11F H 0.4458 0.2291 0.2137 0.085 Uiso 1 1 calc R . . C114 C 0.5337(5) 0.3032(5) 0.2576(4) 0.092(3) Uani 1 1 d . . . H11G H 0.5904 0.2743 0.2617 0.138 Uiso 1 1 calc R . . H11H H 0.5059 0.3007 0.2928 0.138 Uiso 1 1 calc R . . H11I H 0.5508 0.3510 0.2508 0.138 Uiso 1 1 calc R . . C121 C 0.1469(4) 0.3438(3) 0.2065(2) 0.0429(11) Uani 1 1 d . . . H12A H 0.1928 0.3749 0.2297 0.052 Uiso 1 1 calc R . . H12B H 0.0843 0.3664 0.2018 0.052 Uiso 1 1 calc R . . C122 C 0.1418(4) 0.2777(3) 0.2399(2) 0.0500(13) Uani 1 1 d . . . H12C H 0.2033 0.2537 0.2435 0.060 Uiso 1 1 calc R . . H12D H 0.0932 0.2473 0.2182 0.060 Uiso 1 1 calc R . . C123 C 0.1178(5) 0.2895(3) 0.2998(3) 0.0634(16) Uani 1 1 d . . . H12E H 0.0538 0.3099 0.2961 0.076 Uiso 1 1 calc R . . H12F H 0.1632 0.3229 0.3204 0.076 Uiso 1 1 calc R . . C124 C 0.1205(6) 0.2232(4) 0.3353(3) 0.076(2) Uani 1 1 d . . . H12G H 0.1050 0.2339 0.3732 0.113 Uiso 1 1 calc R . . H12H H 0.1839 0.2031 0.3397 0.113 Uiso 1 1 calc R . . H12I H 0.0744 0.1904 0.3157 0.113 Uiso 1 1 calc R . . C131 C 0.2085(3) 0.4244(2) 0.1185(2) 0.0424(11) Uani 1 1 d . . . H13A H 0.1486 0.4508 0.1121 0.051 Uiso 1 1 calc R . . H13B H 0.2490 0.4443 0.1525 0.051 Uiso 1 1 calc R . . C132 C 0.2580(4) 0.4347(3) 0.0663(2) 0.0499(12) Uani 1 1 d . . . H13C H 0.2214 0.4105 0.0331 0.060 Uiso 1 1 calc R . . H13D H 0.3213 0.4130 0.0744 0.060 Uiso 1 1 calc R . . C133 C 0.2698(4) 0.5107(3) 0.0499(3) 0.0561(14) Uani 1 1 d . . . H13E H 0.2978 0.5123 0.0143 0.067 Uiso 1 1 calc R . . H13F H 0.2064 0.5322 0.0414 0.067 Uiso 1 1 calc R . . C135 C 0.3313(5) 0.5532(3) 0.0958(3) 0.0663(16) Uani 1 1 d . . . H13G H 0.3347 0.6007 0.0824 0.099 Uiso 1 1 calc R . . H13H H 0.3950 0.5335 0.1035 0.099 Uiso 1 1 calc R . . H13I H 0.3036 0.5527 0.1310 0.099 Uiso 1 1 calc R . . C211 C -0.1010(4) 0.2985(3) -0.0615(2) 0.0517(13) Uani 1 1 d . . . H21A H -0.1560 0.2774 -0.0862 0.062 Uiso 1 1 calc R . . H21B H -0.1251 0.3349 -0.0384 0.062 Uiso 1 1 calc R . . C212 C -0.0355(4) 0.3319(4) -0.1001(3) 0.0612(15) Uani 1 1 d . . . H21C H 0.0176 0.3551 -0.0753 0.073 Uiso 1 1 calc R . . H21D H -0.0085 0.2951 -0.1215 0.073 Uiso 1 1 calc R . . C213 C -0.0842(6) 0.3820(5) -0.1411(4) 0.102(3) Uani 1 1 d . . . H21E H -0.1089 0.4196 -0.1195 0.122 Uiso 1 1 calc R . . H21F H -0.1390 0.3591 -0.1646 0.122 Uiso 1 1 calc R . . C214 C -0.0220(6) 0.4132(5) -0.1811(4) 0.101(3) Uani 1 1 d . . . H21G H -0.0591 0.4462 -0.2070 0.152 Uiso 1 1 calc R . . H21H H 0.0011 0.3766 -0.2037 0.152 Uiso 1 1 calc R . . H21I H 0.0318 0.4369 -0.1584 0.152 Uiso 1 1 calc R . . C221 C -0.1384(4) 0.1855(3) 0.0125(2) 0.0448(11) Uani 1 1 d . . . H22A H -0.1104 0.1483 0.0385 0.054 Uiso 1 1 calc R . . H22I H -0.1695 0.2179 0.0357 0.054 Uiso 1 1 calc R . . C222 C -0.2156(4) 0.1532(3) -0.0324(3) 0.0567(14) Uani 1 1 d . . . H22B H -0.2350 0.1872 -0.0632 0.068 Uiso 1 1 calc R . . H22C H -0.1885 0.1131 -0.0497 0.068 Uiso 1 1 calc R . . C223 C -0.3026(4) 0.1300(4) -0.0088(3) 0.0717(18) Uani 1 1 d . . . H22D H -0.3288 0.1699 0.0094 0.086 Uiso 1 1 calc R . . H22E H -0.2834 0.0952 0.0214 0.086 Uiso 1 1 calc R . . C224 C -0.3810(5) 0.0991(5) -0.0542(4) 0.087(2) Uani 1 1 d . . . H22F H -0.4345 0.0851 -0.0358 0.131 Uiso 1 1 calc R . . H22G H -0.3562 0.0589 -0.0719 0.131 Uiso 1 1 calc R . . H22H H -0.4021 0.1337 -0.0837 0.131 Uiso 1 1 calc R . . C231 C 0.0059(4) 0.1736(3) -0.0635(2) 0.0558(14) Uani 1 1 d . . . H23A H -0.0446 0.1672 -0.0970 0.067 Uiso 1 1 calc R . . H23I H 0.0587 0.1976 -0.0773 0.067 Uiso 1 1 calc R . . C232 C 0.0402(5) 0.1043(3) -0.0434(3) 0.0694(17) Uani 1 1 d . . . H23B H -0.0135 0.0762 -0.0350 0.083 Uiso 1 1 calc R . . H23C H 0.0866 0.1086 -0.0076 0.083 Uiso 1 1 calc R . . C233 C 0.0867(6) 0.0688(4) -0.0897(4) 0.087(2) Uani 1 1 d . . . H23D H 0.0430 0.0712 -0.1267 0.105 Uiso 1 1 calc R . . H23E H 0.1449 0.0941 -0.0941 0.105 Uiso 1 1 calc R . . C234 C 0.1105(8) -0.0027(6) -0.0767(5) 0.123(3) Uani 1 1 d U . . H23F H 0.1393 -0.0227 -0.1078 0.148 Uiso 1 1 calc R . . H23G H 0.0530 -0.0283 -0.0729 0.148 Uiso 1 1 calc R . . H23H H 0.1553 -0.0054 -0.0408 0.148 Uiso 1 1 calc R . . C311 C -0.2012(3) 0.2481(3) 0.1779(2) 0.0401(10) Uani 1 1 d . . . C312 C -0.1321(4) 0.2148(3) 0.2179(3) 0.0519(13) Uani 1 1 d . . . H31A H -0.0775 0.2389 0.2357 0.062 Uiso 1 1 calc R . . C313 C -0.1453(5) 0.1452(3) 0.2312(3) 0.0628(16) Uani 1 1 d . . . H31B H -0.0984 0.1219 0.2574 0.075 Uiso 1 1 calc R . . C314 C -0.2268(6) 0.1101(3) 0.2062(3) 0.078(2) Uani 1 1 d . . . H31C H -0.2345 0.0629 0.2147 0.094 Uiso 1 1 calc R . . C315 C -0.2965(6) 0.1442(4) 0.1690(3) 0.079(2) Uani 1 1 d . . . H31D H -0.3531 0.1209 0.1536 0.095 Uiso 1 1 calc R . . C316 C -0.2837(5) 0.2130(3) 0.1540(3) 0.0585(15) Uani 1 1 d . . . H31E H -0.3308 0.2357 0.1276 0.070 Uiso 1 1 calc R . . C321 C -0.1527(4) 0.3832(3) 0.2294(2) 0.0419(11) Uani 1 1 d . . . C322 C -0.0882(5) 0.4387(3) 0.2366(3) 0.0594(15) Uani 1 1 d . . . H32A H -0.0609 0.4545 0.2050 0.071 Uiso 1 1 calc R . . C323 C -0.0650(5) 0.4694(4) 0.2888(3) 0.0709(18) Uani 1 1 d . . . H32B H -0.0217 0.5067 0.2931 0.085 Uiso 1 1 calc R . . C324 C -0.1041(5) 0.4470(4) 0.3361(3) 0.0696(17) Uani 1 1 d . . . H32C H -0.0878 0.4693 0.3720 0.084 Uiso 1 1 calc R . . C325 C -0.1662(6) 0.3925(4) 0.3303(3) 0.0740(19) Uani 1 1 d . . . H32D H -0.1927 0.3767 0.3622 0.089 Uiso 1 1 calc R . . C326 C -0.1907(5) 0.3594(3) 0.2749(3) 0.0617(15) Uani 1 1 d . . . H32E H -0.2329 0.3214 0.2703 0.074 Uiso 1 1 calc R . . C331 C -0.2942(3) 0.3685(3) 0.1209(2) 0.0467(12) Uani 1 1 d . . . C332 C -0.3557(4) 0.4083(4) 0.1484(3) 0.0669(17) Uani 1 1 d . . . H33A H -0.3379 0.4219 0.1872 0.080 Uiso 1 1 calc R . . C333 C -0.4423(5) 0.4273(5) 0.1178(4) 0.090(3) Uani 1 1 d . . . H33B H -0.4847 0.4536 0.1360 0.109 Uiso 1 1 calc R . . C334 C -0.4683(5) 0.4082(5) 0.0602(4) 0.100(3) Uani 1 1 d . . . H33C H -0.5283 0.4215 0.0399 0.120 Uiso 1 1 calc R . . C335 C -0.4079(4) 0.3702(4) 0.0328(3) 0.077(2) Uani 1 1 d . . . H33D H -0.4253 0.3577 -0.0064 0.092 Uiso 1 1 calc R . . C336 C -0.3202(4) 0.3507(4) 0.0640(3) 0.0620(16) Uani 1 1 d . . . H33E H -0.2778 0.3246 0.0456 0.074 Uiso 1 1 calc R . . C1S C 0.3656(5) 0.1466(4) 0.0515(3) 0.0727(18) Uani 1 1 d . . . H1SA H 0.3060 0.1735 0.0511 0.087 Uiso 1 1 calc R . . Cl11 Cl 0.45652(19) 0.20505(16) 0.04603(14) 0.1161(8) Uani 1 1 d . . . Cl12 Cl 0.3896(2) 0.10175(14) 0.11729(11) 0.1186(9) Uani 1 1 d . . . Cl13 Cl 0.3466(2) 0.08773(15) -0.00634(11) 0.1225(9) Uani 1 1 d . . . C2S C 0.1499(6) 0.0323(4) 0.1961(3) 0.078(2) Uani 1 1 d . . . H2SA H 0.1248 0.0673 0.1665 0.093 Uiso 1 1 calc R . . Cl21 Cl 0.2454(2) 0.06786(17) 0.24135(10) 0.1291(10) Uani 1 1 d . . . Cl22 Cl 0.0588(2) 0.01101(17) 0.23613(12) 0.1250(9) Uani 1 1 d . . . Cl23 Cl 0.1811(2) -0.04038(15) 0.16155(13) 0.1297(10) Uani 1 1 d . . . C3S C 0.3000(6) 0.3382(4) -0.0985(3) 0.0277(16) Uani 0.50 1 d P . . H3SA H 0.2890 0.3209 -0.0603 0.033 Uiso 0.50 1 calc PR . . Cl31 Cl 0.2212(3) 0.2945(2) -0.15287(15) 0.0811(11) Uani 0.50 1 d P . . Cl32 Cl 0.4134(3) 0.3142(5) -0.10819(18) 0.151(3) Uani 0.50 1 d P . . Cl33 Cl 0.2744(6) 0.42220(19) -0.1028(2) 0.150(3) Uani 0.50 1 d P . . 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 0.02819(11) 0.02965(11) 0.02909(12) 0.00215(6) 0.00556(7) 0.00196(6) P1 0.0299(6) 0.0379(6) 0.0348(6) -0.0009(5) 0.0032(4) 0.0019(5) P2 0.0353(6) 0.0433(6) 0.0338(6) -0.0020(5) 0.0053(5) -0.0039(5) P3 0.0313(6) 0.0406(6) 0.0356(6) 0.0037(5) 0.0110(5) -0.0002(5) Cl1 0.0547(7) 0.0331(6) 0.0477(7) 0.0071(5) 0.0089(5) 0.0080(5) Cl2 0.0365(6) 0.0475(6) 0.0415(6) -0.0009(5) 0.0137(5) 0.0045(5) O1 0.0463(19) 0.0403(18) 0.057(2) 0.0068(16) 0.0258(16) 0.0092(15) O2 0.0344(15) 0.0300(15) 0.0336(16) 0.0050(12) 0.0096(12) 0.0048(12) C1 0.027(2) 0.036(2) 0.029(2) 0.0027(16) 0.0048(17) -0.0032(16) C2 0.029(2) 0.035(2) 0.030(2) 0.0021(17) 0.0080(16) -0.0016(17) C3 0.030(2) 0.036(2) 0.035(2) 0.0046(18) 0.0072(17) -0.0009(17) C4 0.025(2) 0.037(2) 0.031(2) 0.0016(17) 0.0048(16) 0.0001(17) C5 0.027(2) 0.036(2) 0.032(2) 0.0036(18) 0.0044(17) 0.0037(17) C111 0.033(2) 0.043(3) 0.040(3) 0.000(2) 0.000(2) 0.0043(19) C112 0.040(3) 0.064(3) 0.049(3) -0.005(3) -0.001(2) 0.001(2) C113 0.046(3) 0.088(5) 0.070(4) -0.001(3) -0.015(3) 0.006(3) C114 0.052(4) 0.138(7) 0.076(5) 0.012(5) -0.020(4) -0.010(4) C121 0.042(3) 0.052(3) 0.035(2) -0.006(2) 0.006(2) 0.000(2) C122 0.046(3) 0.064(4) 0.041(3) 0.003(2) 0.008(2) 0.002(2) C123 0.074(4) 0.079(4) 0.037(3) -0.002(3) 0.008(3) -0.009(3) C124 0.082(5) 0.088(5) 0.058(4) 0.013(3) 0.017(4) -0.013(4) C131 0.037(2) 0.038(2) 0.051(3) -0.005(2) 0.003(2) -0.0011(19) C132 0.049(3) 0.046(3) 0.056(3) -0.004(2) 0.014(2) -0.010(2) C133 0.059(3) 0.053(3) 0.058(3) 0.004(3) 0.012(3) -0.010(3) C135 0.067(4) 0.057(4) 0.074(4) -0.004(3) 0.010(3) -0.014(3) C211 0.050(3) 0.059(3) 0.042(3) 0.006(2) -0.006(2) -0.007(3) C212 0.058(3) 0.075(4) 0.047(3) 0.014(3) -0.002(3) -0.012(3) C213 0.078(5) 0.130(7) 0.091(6) 0.051(5) -0.010(4) -0.028(5) C214 0.086(5) 0.127(7) 0.083(5) 0.052(5) -0.007(4) -0.037(5) C221 0.042(3) 0.047(3) 0.046(3) -0.004(2) 0.010(2) -0.010(2) C222 0.049(3) 0.069(4) 0.053(3) -0.015(3) 0.011(2) -0.020(3) C223 0.051(3) 0.094(5) 0.072(4) -0.009(4) 0.014(3) -0.023(3) C224 0.064(4) 0.110(6) 0.088(5) -0.017(5) 0.012(4) -0.039(4) C231 0.059(3) 0.063(4) 0.045(3) -0.020(3) 0.009(3) -0.007(3) C232 0.069(4) 0.065(4) 0.073(4) -0.018(3) 0.007(3) 0.005(3) C233 0.099(6) 0.081(5) 0.081(5) -0.011(4) 0.012(4) 0.015(4) C234 0.123(4) 0.123(4) 0.123(4) -0.0005(10) 0.0202(11) 0.0005(10) C311 0.040(3) 0.044(3) 0.039(3) 0.009(2) 0.015(2) -0.001(2) C312 0.050(3) 0.055(3) 0.051(3) 0.008(2) 0.010(3) -0.007(2) C313 0.075(4) 0.052(3) 0.064(4) 0.018(3) 0.020(3) 0.010(3) C314 0.116(6) 0.041(3) 0.083(5) -0.002(3) 0.030(5) -0.021(4) C315 0.086(5) 0.062(4) 0.084(5) 0.005(4) -0.002(4) -0.033(4) C316 0.061(4) 0.054(3) 0.061(4) 0.000(3) 0.011(3) -0.014(3) C321 0.041(3) 0.045(3) 0.042(3) -0.003(2) 0.013(2) 0.001(2) C322 0.076(4) 0.058(3) 0.047(3) -0.003(3) 0.017(3) -0.012(3) C323 0.090(5) 0.062(4) 0.063(4) -0.013(3) 0.018(3) -0.023(3) C324 0.091(5) 0.068(4) 0.050(3) -0.013(3) 0.013(3) 0.005(4) C325 0.097(5) 0.085(5) 0.044(3) -0.002(3) 0.021(3) -0.008(4) C326 0.074(4) 0.065(4) 0.050(3) -0.005(3) 0.023(3) -0.016(3) C331 0.034(2) 0.054(3) 0.055(3) 0.016(2) 0.015(2) -0.002(2) C332 0.047(3) 0.077(4) 0.081(4) 0.011(3) 0.020(3) 0.017(3) C333 0.053(4) 0.124(7) 0.099(6) 0.033(5) 0.028(4) 0.036(4) C334 0.040(4) 0.146(8) 0.114(7) 0.068(6) 0.011(4) 0.016(4) C335 0.040(3) 0.123(6) 0.065(4) 0.027(4) 0.003(3) -0.002(4) C336 0.045(3) 0.091(5) 0.050(3) 0.004(3) 0.006(2) -0.002(3) C1S 0.072(4) 0.068(4) 0.075(4) -0.005(3) 0.006(3) 0.019(3) Cl11 0.0822(15) 0.136(2) 0.139(2) -0.0106(17) 0.0422(15) -0.0067(14) Cl12 0.168(3) 0.0964(16) 0.0837(15) 0.0145(12) -0.0015(15) 0.0381(16) Cl13 0.155(2) 0.120(2) 0.0859(15) -0.0271(14) 0.0021(15) 0.0176(17) C2S 0.112(6) 0.062(4) 0.050(4) 0.011(3) -0.014(4) -0.001(4) Cl21 0.149(2) 0.153(2) 0.0733(13) -0.0128(14) -0.0162(14) -0.0544(19) Cl22 0.128(2) 0.146(2) 0.1015(18) -0.0072(17) 0.0216(16) 0.0034(18) Cl23 0.157(2) 0.1129(19) 0.118(2) -0.0443(16) 0.0185(18) 0.0166(17) C3S 0.032(4) 0.033(4) 0.023(4) -0.002(3) 0.018(3) -0.007(3) Cl31 0.0630(19) 0.130(3) 0.0561(18) -0.0444(19) 0.0258(15) -0.0331(19) Cl32 0.0451(19) 0.351(9) 0.057(2) -0.006(4) 0.0081(16) 0.067(3) Cl33 0.329(9) 0.0326(17) 0.082(3) -0.0103(17) 0.018(4) 0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.947(4) . ? Ir1 O2 2.042(3) . ? Ir1 P1 2.3545(12) . ? Ir1 P2 2.3563(13) . ? Ir1 Cl1 2.3739(12) . ? Ir1 Cl2 2.4702(12) . ? P1 C111 1.828(5) . ? P1 C121 1.830(5) . ? P1 C131 1.831(5) . ? P2 C221 1.828(5) . ? P2 C231 1.833(5) . ? P2 C211 1.837(6) . ? P3 C2 1.798(4) . ? P3 C331 1.799(5) . ? P3 C311 1.812(5) . ? P3 C321 1.829(5) . ? O1 C3 1.226(5) . ? O2 C4 1.314(5) . ? C1 C2 1.352(6) . ? C2 C3 1.474(6) . ? C3 C4 1.507(6) . ? C4 C5 1.373(6) . ? C5 C5 1.436(8) 3_565 ? C111 C112 1.529(7) . ? C112 C113 1.501(8) . ? C113 C114 1.516(9) . ? C121 C122 1.500(7) . ? C122 C123 1.512(8) . ? C123 C124 1.519(9) . ? C131 C132 1.519(7) . ? C132 C133 1.529(7) . ? C133 C135 1.510(8) . ? C211 C212 1.539(8) . ? C212 C213 1.454(10) . ? C213 C214 1.513(10) . ? C221 C222 1.520(7) . ? C222 C223 1.501(8) . ? C223 C224 1.528(9) . ? C231 C232 1.470(9) . ? C232 C233 1.522(10) . ? C233 C234 1.437(12) . ? C311 C316 1.387(8) . ? C311 C312 1.397(8) . ? C312 C313 1.394(8) . ? C313 C314 1.384(10) . ? C314 C315 1.373(11) . ? C315 C316 1.389(9) . ? C321 C326 1.351(7) . ? C321 C322 1.398(8) . ? C322 C323 1.349(8) . ? C323 C324 1.387(9) . ? C324 C325 1.362(10) . ? C325 C326 1.436(9) . ? C331 C336 1.366(8) . ? C331 C332 1.396(8) . ? C332 C333 1.366(9) . ? C333 C334 1.388(13) . ? C334 C335 1.365(12) . ? C335 C336 1.388(9) . ? C1S Cl11 1.732(8) . ? C1S Cl12 1.751(8) . ? C1S Cl13 1.752(7) . ? C2S Cl23 1.710(8) . ? C2S Cl21 1.720(7) . ? C2S Cl22 1.766(9) . ? C3S Cl33 1.656(9) . ? C3S Cl32 1.726(8) . ? C3S Cl31 1.763(9) . ? 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 Ir1 O2 91.68(15) . . ? C1 Ir1 P1 93.68(13) . . ? O2 Ir1 P1 88.25(9) . . ? C1 Ir1 P2 89.32(13) . . ? O2 Ir1 P2 88.75(9) . . ? P1 Ir1 P2 175.81(4) . . ? C1 Ir1 Cl1 89.40(13) . . ? O2 Ir1 Cl1 178.92(9) . . ? P1 Ir1 Cl1 91.72(4) . . ? P2 Ir1 Cl1 91.23(5) . . ? C1 Ir1 Cl2 177.71(13) . . ? O2 Ir1 Cl2 89.67(8) . . ? P1 Ir1 Cl2 88.21(4) . . ? P2 Ir1 Cl2 88.85(4) . . ? Cl1 Ir1 Cl2 89.25(4) . . ? C111 P1 C121 104.1(2) . . ? C111 P1 C131 105.6(2) . . ? C121 P1 C131 101.3(2) . . ? C111 P1 Ir1 114.08(16) . . ? C121 P1 Ir1 116.09(17) . . ? C131 P1 Ir1 114.21(17) . . ? C221 P2 C231 106.5(3) . . ? C221 P2 C211 103.7(3) . . ? C231 P2 C211 101.7(3) . . ? C221 P2 Ir1 112.90(17) . . ? C231 P2 Ir1 118.36(19) . . ? C211 P2 Ir1 112.10(19) . . ? C2 P3 C331 111.3(2) . . ? C2 P3 C311 108.6(2) . . ? C331 P3 C311 106.0(2) . . ? C2 P3 C321 114.3(2) . . ? C331 P3 C321 110.6(3) . . ? C311 P3 C321 105.6(2) . . ? C4 O2 Ir1 128.3(3) . . ? C2 C1 Ir1 127.3(3) . . ? C1 C2 C3 127.2(4) . . ? C1 C2 P3 122.0(3) . . ? C3 C2 P3 110.9(3) . . ? O1 C3 C2 117.8(4) . . ? O1 C3 C4 121.7(4) . . ? C2 C3 C4 120.5(4) . . ? O2 C4 C5 121.0(4) . . ? O2 C4 C3 123.8(4) . . ? C5 C4 C3 115.2(4) . . ? C4 C5 C5 123.4(5) . 3_565 ? C112 C111 P1 116.9(4) . . ? C113 C112 C111 112.3(5) . . ? C112 C113 C114 113.0(6) . . ? C122 C121 P1 115.9(4) . . ? C121 C122 C123 113.2(5) . . ? C122 C123 C124 113.1(6) . . ? C132 C131 P1 115.7(3) . . ? C131 C132 C133 114.2(5) . . ? C135 C133 C132 114.4(5) . . ? C212 C211 P2 113.0(4) . . ? C213 C212 C211 113.4(6) . . ? C212 C213 C214 114.2(7) . . ? C222 C221 P2 118.5(4) . . ? C223 C222 C221 114.3(5) . . ? C222 C223 C224 114.1(6) . . ? C232 C231 P2 118.7(4) . . ? C231 C232 C233 109.8(6) . . ? C234 C233 C232 113.2(8) . . ? C316 C311 C312 120.0(5) . . ? C316 C311 P3 121.3(4) . . ? C312 C311 P3 118.6(4) . . ? C313 C312 C311 119.1(6) . . ? C314 C313 C312 120.4(6) . . ? C315 C314 C313 120.1(6) . . ? C314 C315 C316 120.4(6) . . ? C311 C316 C315 119.9(6) . . ? C326 C321 C322 120.2(5) . . ? C326 C321 P3 118.5(4) . . ? C322 C321 P3 121.3(4) . . ? C323 C322 C321 120.1(6) . . ? C322 C323 C324 121.1(6) . . ? C325 C324 C323 119.9(6) . . ? C324 C325 C326 119.2(6) . . ? C321 C326 C325 119.6(6) . . ? C336 C331 C332 119.9(6) . . ? C336 C331 P3 119.3(4) . . ? C332 C331 P3 120.8(5) . . ? C333 C332 C331 118.9(7) . . ? C332 C333 C334 120.7(7) . . ? C335 C334 C333 120.8(7) . . ? C334 C335 C336 118.4(7) . . ? C331 C336 C335 121.3(6) . . ? Cl11 C1S Cl12 110.2(4) . . ? Cl11 C1S Cl13 112.7(4) . . ? Cl12 C1S Cl13 110.1(4) . . ? Cl23 C2S Cl21 112.2(5) . . ? Cl23 C2S Cl22 109.3(4) . . ? Cl21 C2S Cl22 109.7(4) . . ? Cl33 C3S Cl32 116.9(6) . . ? Cl33 C3S Cl31 108.3(6) . . ? Cl32 C3S Cl31 105.8(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.363 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.140