# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2036 data_oct298 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[HIr4(CO)8(PPh2)(PPh3)(PPhCPhCPh)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H41 Ir4 O8 P3' _chemical_formula_weight 1727.62 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' '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 12.575(4) _cell_length_b 20.875(5) _cell_length_c 21.202(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.35(2) _cell_angle_gamma 90.00 _cell_volume 5415(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.119 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 9.941 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6977 _diffrn_reflns_av_R_equivalents 0.0835 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 21.99 _reflns_number_total 6628 _reflns_number_gt 4589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; All phenyl groups were refined as rigid bodies.Ir and P atoms were anisotropic, C atoms isotropic,and H atoms in riding mode with Uiso(H) equal to 1.2Ueq(C). The C(11) and C(47) phenyl groups were disordered 0.63:0.37 and 0.75:0.25 respectively over two orientations. For the lower occupancy C(47a) ring carbon atoms Uiso was fixed at 0.05. 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^)+(0.0692P)^2^+34.4168P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6628 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0981 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1502 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Ir1 Ir 0.53985(7) 0.28886(3) 0.16030(4) 0.0370(2) Uani 1 1 d . A . Ir2 Ir 0.50263(7) 0.18470(3) 0.07498(4) 0.0346(2) Uani 1 1 d . . . Ir3 Ir 0.54767(7) 0.16652(4) 0.20958(4) 0.0418(3) Uani 1 1 d . A . Ir4 Ir 0.70500(7) 0.20920(4) 0.15083(4) 0.0431(3) Uani 1 1 d . A . P1 P 0.3719(5) 0.3370(2) 0.1584(3) 0.0430(14) Uani 1 1 d . . . P2 P 0.5094(5) 0.0895(2) 0.1295(3) 0.0405(13) Uani 1 1 d . . . P3 P 0.7718(5) 0.2678(3) 0.0754(3) 0.0461(14) Uani 1 1 d . . . O1 O 0.6483(13) 0.4152(7) 0.1564(7) 0.062(4) Uiso 1 1 d . B . O2 O 0.5846(14) 0.1646(8) -0.0443(8) 0.072(5) Uiso 1 1 d . . . O3 O 0.2644(13) 0.1906(7) 0.0055(8) 0.064(4) Uiso 1 1 d . . . O4 O 0.3695(16) 0.1396(9) 0.2804(9) 0.085(5) Uiso 1 1 d . . . O5 O 0.7276(18) 0.1054(10) 0.3070(10) 0.101(6) Uiso 1 1 d . . . O6 O 0.8474(18) 0.2639(10) 0.2718(10) 0.104(6) Uiso 1 1 d . A . O7 O 0.843(2) 0.0912(13) 0.1496(13) 0.142(9) Uiso 1 1 d . A . O8 O 0.5914(14) 0.2822(8) 0.3043(9) 0.077(5) Uiso 1 1 d . B . C1 C 0.6040(15) 0.3658(9) 0.1555(9) 0.034(5) Uiso 1 1 d . . . C2 C 0.5555(17) 0.1724(10) 0.0030(10) 0.047(5) Uiso 1 1 d . . . C3 C 0.3553(18) 0.1863(10) 0.0361(10) 0.049(6) Uiso 1 1 d . . . C4 C 0.440(2) 0.1503(11) 0.2553(12) 0.062(6) Uiso 1 1 d . . . C5 C 0.656(2) 0.1310(13) 0.2734(13) 0.078(8) Uiso 1 1 d . . . C6 C 0.789(2) 0.2425(13) 0.2217(14) 0.082(8) Uiso 1 1 d . . . C7 C 0.784(2) 0.1356(14) 0.1454(14) 0.085(8) Uiso 1 1 d . . . C8 C 0.569(2) 0.2664(12) 0.2491(13) 0.068(7) Uiso 1 1 d . . . C9 C 0.8115(18) 0.3478(10) 0.0834(10) 0.048(5) Uiso 1 1 d . A . C10 C 0.7259(19) 0.3408(10) 0.0357(11) 0.057(6) Uiso 1 1 d . A . C17 C 0.8943(12) 0.3915(7) 0.1220(7) 0.052(6) Uiso 1 1 d G . . C18 C 0.9064(14) 0.4543(8) 0.1031(7) 0.092(9) Uiso 1 1 d G A . H18 H 0.8626 0.4698 0.0646 0.110 Uiso 1 1 calc R . . C19 C 0.9838(16) 0.4939(6) 0.1416(9) 0.102(10) Uiso 1 1 d G A . H19 H 0.9919 0.5359 0.1290 0.122 Uiso 1 1 calc R . . C20 C 1.0492(14) 0.4706(8) 0.1990(9) 0.100(10) Uiso 1 1 d G A . H20 H 1.1010 0.4971 0.2248 0.120 Uiso 1 1 calc R . . C21 C 1.0371(14) 0.4078(9) 0.2179(7) 0.087(9) Uiso 1 1 d G A . H21 H 1.0809 0.3923 0.2564 0.104 Uiso 1 1 calc R . . C22 C 0.9597(14) 0.3682(6) 0.1794(8) 0.087(8) Uiso 1 1 d G A . H22 H 0.9516 0.3262 0.1921 0.104 Uiso 1 1 calc R . . C23 C 0.6431(11) 0.3722(6) -0.0130(6) 0.049(6) Uiso 1 1 d G . . C24 C 0.6294(11) 0.4382(6) -0.0114(6) 0.060(6) Uiso 1 1 d G A . H24 H 0.6727 0.4623 0.0217 0.072 Uiso 1 1 calc R . . C25 C 0.5510(13) 0.4683(5) -0.0592(7) 0.067(7) Uiso 1 1 d G A . H25 H 0.5418 0.5125 -0.0581 0.080 Uiso 1 1 calc R . . C26 C 0.4862(11) 0.4323(7) -0.1087(6) 0.066(7) Uiso 1 1 d G A . H26 H 0.4337 0.4525 -0.1406 0.079 Uiso 1 1 calc R . . C27 C 0.4999(12) 0.3663(7) -0.1103(7) 0.079(8) Uiso 1 1 d G A . H27 H 0.4565 0.3423 -0.1434 0.095 Uiso 1 1 calc R . . C28 C 0.5783(13) 0.3363(5) -0.0625(8) 0.073(7) Uiso 1 1 d G A . H28 H 0.5874 0.2921 -0.0636 0.088 Uiso 1 1 calc R . . C29 C 0.6061(11) 0.0258(5) 0.1261(7) 0.044(5) Uiso 1 1 d G . . C30 C 0.6346(12) 0.0121(6) 0.0680(6) 0.056(6) Uiso 1 1 d G . . H30 H 0.6091 0.0379 0.0319 0.067 Uiso 1 1 calc R . . C31 C 0.7011(13) -0.0402(7) 0.0638(6) 0.077(8) Uiso 1 1 d G . . H31 H 0.7202 -0.0494 0.0249 0.092 Uiso 1 1 calc R . . C32 C 0.7392(12) -0.0787(6) 0.1178(7) 0.064(7) Uiso 1 1 d G . . H32 H 0.7837 -0.1137 0.1150 0.077 Uiso 1 1 calc R . . C33 C 0.7108(12) -0.0650(6) 0.1759(6) 0.072(7) Uiso 1 1 d G . . H33 H 0.7362 -0.0908 0.2120 0.086 Uiso 1 1 calc R . . C34 C 0.6442(12) -0.0128(7) 0.1801(5) 0.049(5) Uiso 1 1 d G . . H34 H 0.6251 -0.0036 0.2189 0.059 Uiso 1 1 calc R . . C35 C 0.3820(9) 0.0447(6) 0.1220(7) 0.047(5) Uiso 1 1 d G . . C36 C 0.3763(11) -0.0207(6) 0.1093(7) 0.053(6) Uiso 1 1 d G . . H36 H 0.4389 -0.0431 0.1064 0.064 Uiso 1 1 calc R . . C37 C 0.2769(13) -0.0525(5) 0.1008(8) 0.084(8) Uiso 1 1 d G . . H37 H 0.2730 -0.0963 0.0923 0.101 Uiso 1 1 calc R . . C38 C 0.1833(10) -0.0190(8) 0.1050(8) 0.086(8) Uiso 1 1 d G . . H38 H 0.1168 -0.0403 0.0994 0.103 Uiso 1 1 calc R . . C39 C 0.1891(10) 0.0464(8) 0.1178(8) 0.083(8) Uiso 1 1 d G . . H39 H 0.1264 0.0688 0.1206 0.099 Uiso 1 1 calc R . . C40 C 0.2884(12) 0.0783(5) 0.1263(7) 0.056(6) Uiso 1 1 d G . . H40 H 0.2923 0.1220 0.1348 0.067 Uiso 1 1 calc R . . C41 C 0.3846(12) 0.4160(6) 0.1951(7) 0.052(6) Uiso 1 1 d G B . C42 C 0.4706(11) 0.4268(7) 0.2484(7) 0.061(6) Uiso 1 1 d G . . H42 H 0.5171 0.3934 0.2657 0.073 Uiso 1 1 calc R B . C43 C 0.4869(12) 0.4876(8) 0.2757(7) 0.099(10) Uiso 1 1 d G B . H43 H 0.5444 0.4948 0.3114 0.118 Uiso 1 1 calc R . . C44 C 0.4174(15) 0.5375(6) 0.2498(8) 0.094(9) Uiso 1 1 d G . . H44 H 0.4283 0.5781 0.2681 0.113 Uiso 1 1 calc R B . C45 C 0.3314(13) 0.5267(6) 0.1965(8) 0.087(9) Uiso 1 1 d G B . H45 H 0.2849 0.5601 0.1791 0.105 Uiso 1 1 calc R . . C46 C 0.3151(11) 0.4659(7) 0.1691(6) 0.062(7) Uiso 1 1 d G . . H46 H 0.2576 0.4586 0.1334 0.075 Uiso 1 1 calc R B . C53 C 0.2821(13) 0.3517(7) 0.0779(6) 0.046(5) Uiso 1 1 d G B . C54 C 0.3301(11) 0.3563(7) 0.0253(7) 0.051(6) Uiso 1 1 d G . . H54 H 0.4056 0.3528 0.0314 0.061 Uiso 1 1 calc R B . C55 C 0.2655(16) 0.3662(8) -0.0366(6) 0.082(8) Uiso 1 1 d G B . H55 H 0.2976 0.3693 -0.0718 0.098 Uiso 1 1 calc R . . C56 C 0.1527(15) 0.3715(10) -0.0458(7) 0.125(12) Uiso 1 1 d G . . H56 H 0.1095 0.3781 -0.0872 0.150 Uiso 1 1 calc R B . C57 C 0.1047(10) 0.3668(10) 0.0068(11) 0.133(13) Uiso 1 1 d G B . H57 H 0.0292 0.3704 0.0006 0.160 Uiso 1 1 calc R . . C58 C 0.1693(13) 0.3569(9) 0.0687(9) 0.093(9) Uiso 1 1 d G . . H58 H 0.1372 0.3538 0.1039 0.112 Uiso 1 1 calc R B . C11 C 0.858(2) 0.2341(15) 0.0217(14) 0.10(3) Uiso 0.63(3) 1 d PG A 1 C12 C 0.846(2) 0.2547(12) -0.0419(14) 0.062(12) Uiso 0.63(3) 1 d PG A 1 H12 H 0.7933 0.2848 -0.0593 0.075 Uiso 0.63(3) 1 calc PR A 1 C13 C 0.914(2) 0.2302(13) -0.0795(11) 0.081(14) Uiso 0.63(3) 1 d PG A 1 H13 H 0.9061 0.2439 -0.1220 0.098 Uiso 0.63(3) 1 calc PR A 1 C14 C 0.993(2) 0.1851(14) -0.0535(13) 0.067(12) Uiso 0.63(3) 1 d PG A 1 H14 H 1.0387 0.1687 -0.0786 0.080 Uiso 0.63(3) 1 calc PR A 1 C15 C 1.005(2) 0.1646(13) 0.0102(13) 0.090(15) Uiso 0.63(3) 1 d PG A 1 H15 H 1.0585 0.1344 0.0276 0.108 Uiso 0.63(3) 1 calc PR A 1 C16 C 0.938(3) 0.1891(15) 0.0477(11) 0.082(14) Uiso 0.63(3) 1 d PG A 1 H16 H 0.9457 0.1753 0.0903 0.098 Uiso 0.63(3) 1 calc PR A 1 C47 C 0.285(2) 0.2935(11) 0.2016(11) 0.046(8) Uiso 0.75(5) 1 d PG B 1 C48 C 0.287(2) 0.3035(16) 0.2666(12) 0.061(10) Uiso 0.75(5) 1 d PG B 1 H48 H 0.3363 0.3325 0.2908 0.073 Uiso 0.75(5) 1 calc PR B 1 C49 C 0.215(3) 0.2703(18) 0.2956(10) 0.103(15) Uiso 0.75(5) 1 d PG B 1 H49 H 0.2164 0.2770 0.3391 0.124 Uiso 0.75(5) 1 calc PR B 1 C50 C 0.142(2) 0.2269(14) 0.2595(16) 0.119(18) Uiso 0.75(5) 1 d PG B 1 H50 H 0.0935 0.2047 0.2789 0.142 Uiso 0.75(5) 1 calc PR B 1 C51 C 0.140(2) 0.2169(14) 0.1945(16) 0.083(13) Uiso 0.75(5) 1 d PG B 1 H51 H 0.0906 0.1879 0.1704 0.100 Uiso 0.75(5) 1 calc PR B 1 C52 C 0.212(2) 0.2502(15) 0.1655(10) 0.066(11) Uiso 0.75(5) 1 d PG B 1 H52 H 0.2105 0.2435 0.1220 0.079 Uiso 0.75(5) 1 calc PR B 1 C11A C 0.856(3) 0.2271(16) 0.0303(19) 0.012(16) Uiso 0.37(3) 1 d PG A 2 C12A C 0.919(4) 0.2623(14) -0.003(3) 0.09(3) Uiso 0.37(3) 1 d PG A 2 H12A H 0.9152 0.3068 -0.0035 0.105 Uiso 0.37(3) 1 calc PR A 2 C13A C 0.987(4) 0.231(2) -0.036(3) 0.14(4) Uiso 0.37(3) 1 d PG A 2 H13A H 1.0295 0.2544 -0.0584 0.166 Uiso 0.37(3) 1 calc PR A 2 C14A C 0.993(3) 0.164(2) -0.035(2) 0.07(2) Uiso 0.37(3) 1 d PG A 2 H14A H 1.0383 0.1434 -0.0574 0.079 Uiso 0.37(3) 1 calc PR A 2 C15A C 0.929(4) 0.1292(15) -0.002(2) 0.06(2) Uiso 0.37(3) 1 d PG A 2 H15A H 0.9329 0.0847 -0.0015 0.077 Uiso 0.37(3) 1 calc PR A 2 C16A C 0.861(3) 0.1606(16) 0.0309(19) 0.060(19) Uiso 0.37(3) 1 d PG A 2 H16A H 0.8186 0.1371 0.0533 0.072 Uiso 0.37(3) 1 calc PR A 2 C47A C 0.259(7) 0.299(3) 0.194(3) 0.050 Uiso 0.25(5) 1 d PG B 2 C48A C 0.246(7) 0.325(3) 0.252(4) 0.050 Uiso 0.25(5) 1 d PG B 2 H48A H 0.2735 0.3659 0.2643 0.060 Uiso 0.25(5) 1 calc PR B 2 C49A C 0.191(6) 0.291(3) 0.291(3) 0.050 Uiso 0.25(5) 1 d PG B 2 H49A H 0.1827 0.3088 0.3297 0.060 Uiso 0.25(5) 1 calc PR B 2 C50A C 0.150(6) 0.231(3) 0.272(3) 0.050 Uiso 0.25(5) 1 d PG B 2 H50A H 0.1137 0.2076 0.2984 0.060 Uiso 0.25(5) 1 calc PR B 2 C51A C 0.163(6) 0.204(3) 0.214(4) 0.050 Uiso 0.25(5) 1 d PG B 2 H51A H 0.1356 0.1637 0.2017 0.060 Uiso 0.25(5) 1 calc PR B 2 C52A C 0.218(6) 0.238(3) 0.175(3) 0.050 Uiso 0.25(5) 1 d PG B 2 H52A H 0.2264 0.2208 0.1363 0.060 Uiso 0.25(5) 1 calc PR B 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 Ir1 0.0414(5) 0.0292(4) 0.0412(5) -0.0032(4) 0.0109(4) -0.0018(4) Ir2 0.0365(5) 0.0293(4) 0.0376(5) -0.0002(3) 0.0079(4) 0.0034(3) Ir3 0.0548(6) 0.0334(4) 0.0373(5) 0.0017(4) 0.0104(4) -0.0025(4) Ir4 0.0357(5) 0.0379(5) 0.0522(6) 0.0081(4) 0.0032(4) 0.0039(4) P1 0.047(4) 0.035(3) 0.054(4) -0.006(3) 0.027(3) -0.004(3) P2 0.048(4) 0.035(3) 0.038(3) 0.002(2) 0.011(3) 0.003(2) P3 0.037(3) 0.042(3) 0.059(4) 0.004(3) 0.011(3) 0.006(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 1.810(19) . ? Ir1 C8 1.89(3) . ? Ir1 P1 2.331(6) . ? Ir1 Ir4 2.7039(13) . ? Ir1 Ir3 2.7525(12) . ? Ir1 Ir2 2.7978(11) . ? Ir2 C2 1.82(2) . ? Ir2 C3 1.85(2) . ? Ir2 P2 2.291(5) . ? Ir2 Ir4 2.7265(14) . ? Ir2 Ir3 2.8040(13) . ? Ir3 C5 1.84(3) . ? Ir3 C4 1.87(3) . ? Ir3 C8 2.24(2) . ? Ir3 P2 2.308(5) . ? Ir3 Ir4 2.7198(14) . ? Ir4 C6 1.77(3) . ? Ir4 C7 1.85(3) . ? Ir4 P3 2.319(6) . ? P1 C41 1.814(12) . ? P1 C47 1.82(2) . ? P1 C53 1.841(13) . ? P1 C47A 1.92(5) . ? P2 C29 1.814(11) . ? P2 C35 1.830(12) . ? P3 C9 1.74(2) . ? P3 C10 1.77(2) . ? P3 C11A 1.79(3) . ? P3 C11 1.88(2) . ? O1 C1 1.17(2) . ? O2 C2 1.16(2) . ? O3 C3 1.18(2) . ? O4 C4 1.16(3) . ? O5 C5 1.14(3) . ? O6 C6 1.23(3) . ? O7 C7 1.18(3) . ? O8 C8 1.18(3) . ? C9 C10 1.30(3) . ? C9 C17 1.48(2) . ? C10 C23 1.44(2) . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C11A C12A 1.3900 . ? C11A C16A 1.3900 . ? C12A C13A 1.3900 . ? C13A C14A 1.3900 . ? C14A C15A 1.3900 . ? C15A C16A 1.3900 . ? C47A C48A 1.3900 . ? C47A C52A 1.3900 . ? C48A C49A 1.3900 . ? C49A C50A 1.3900 . ? C50A C51A 1.3900 . ? C51A C52A 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C8 106.8(9) . . ? C1 Ir1 P1 91.7(6) . . ? C8 Ir1 P1 95.3(8) . . ? C1 Ir1 Ir4 100.5(6) . . ? C8 Ir1 Ir4 86.8(8) . . ? P1 Ir1 Ir4 166.48(13) . . ? C1 Ir1 Ir3 150.1(6) . . ? C8 Ir1 Ir3 53.9(7) . . ? P1 Ir1 Ir3 111.08(13) . . ? Ir4 Ir1 Ir3 59.79(3) . . ? C1 Ir1 Ir2 131.5(6) . . ? C8 Ir1 Ir2 114.6(7) . . ? P1 Ir1 Ir2 107.95(14) . . ? Ir4 Ir1 Ir2 59.39(3) . . ? Ir3 Ir1 Ir2 60.68(3) . . ? C2 Ir2 C3 98.7(9) . . ? C2 Ir2 P2 108.8(6) . . ? C3 Ir2 P2 99.1(7) . . ? C2 Ir2 Ir4 92.8(7) . . ? C3 Ir2 Ir4 164.5(6) . . ? P2 Ir2 Ir4 86.80(14) . . ? C2 Ir2 Ir1 127.9(6) . . ? C3 Ir2 Ir1 106.0(6) . . ? P2 Ir2 Ir1 111.55(14) . . ? Ir4 Ir2 Ir1 58.59(3) . . ? C2 Ir2 Ir3 143.9(7) . . ? C3 Ir2 Ir3 113.8(7) . . ? P2 Ir2 Ir3 52.71(13) . . ? Ir4 Ir2 Ir3 58.89(3) . . ? Ir1 Ir2 Ir3 58.86(3) . . ? C5 Ir3 C4 92.8(11) . . ? C5 Ir3 C8 95.4(11) . . ? C4 Ir3 C8 90.8(10) . . ? C5 Ir3 P2 104.7(8) . . ? C4 Ir3 P2 101.7(7) . . ? C8 Ir3 P2 155.6(7) . . ? C5 Ir3 Ir4 88.5(9) . . ? C4 Ir3 Ir4 171.0(7) . . ? C8 Ir3 Ir4 80.1(7) . . ? P2 Ir3 Ir4 86.62(14) . . ? C5 Ir3 Ir1 127.4(8) . . ? C4 Ir3 Ir1 113.5(7) . . ? C8 Ir3 Ir1 43.0(7) . . ? P2 Ir3 Ir1 112.59(13) . . ? Ir4 Ir3 Ir1 59.22(3) . . ? C5 Ir3 Ir2 138.0(9) . . ? C4 Ir3 Ir2 123.5(7) . . ? C8 Ir3 Ir2 103.5(7) . . ? P2 Ir3 Ir2 52.16(13) . . ? Ir4 Ir3 Ir2 59.13(3) . . ? Ir1 Ir3 Ir2 60.46(3) . . ? C6 Ir4 C7 99.0(13) . . ? C6 Ir4 P3 97.9(9) . . ? C7 Ir4 P3 96.3(9) . . ? C6 Ir4 Ir1 90.8(9) . . ? C7 Ir4 Ir1 161.7(9) . . ? P3 Ir4 Ir1 97.65(14) . . ? C6 Ir4 Ir3 95.5(9) . . ? C7 Ir4 Ir3 102.4(9) . . ? P3 Ir4 Ir3 154.96(14) . . ? Ir1 Ir4 Ir3 60.99(3) . . ? C6 Ir4 Ir2 150.3(9) . . ? C7 Ir4 Ir2 104.5(9) . . ? P3 Ir4 Ir2 97.45(15) . . ? Ir1 Ir4 Ir2 62.02(3) . . ? Ir3 Ir4 Ir2 61.97(4) . . ? C41 P1 C47 103.9(9) . . ? C41 P1 C53 102.8(7) . . ? C47 P1 C53 103.8(10) . . ? C41 P1 C47A 102(2) . . ? C47 P1 C47A 10(3) . . ? C53 P1 C47A 95(3) . . ? C41 P1 Ir1 113.2(5) . . ? C47 P1 Ir1 114.9(9) . . ? C53 P1 Ir1 116.6(5) . . ? C47A P1 Ir1 124(3) . . ? C29 P2 C35 101.8(7) . . ? C29 P2 Ir2 124.3(5) . . ? C35 P2 Ir2 118.0(5) . . ? C29 P2 Ir3 120.8(5) . . ? C35 P2 Ir3 116.6(5) . . ? Ir2 P2 Ir3 75.13(16) . . ? C9 P3 C10 43.6(9) . . ? C9 P3 C11A 108.4(14) . . ? C10 P3 C11A 108.7(15) . . ? C9 P3 C11 103.0(12) . . ? C10 P3 C11 101.8(12) . . ? C11A P3 C11 7.0(17) . . ? C9 P3 Ir4 125.5(8) . . ? C10 P3 Ir4 130.7(8) . . ? C11A P3 Ir4 117.9(13) . . ? C11 P3 Ir4 124.8(10) . . ? O1 C1 Ir1 175.8(17) . . ? O2 C2 Ir2 177.2(19) . . ? O3 C3 Ir2 172.6(19) . . ? O4 C4 Ir3 176(2) . . ? O5 C5 Ir3 172(3) . . ? O6 C6 Ir4 178(2) . . ? O7 C7 Ir4 171(3) . . ? O8 C8 Ir1 149(2) . . ? O8 C8 Ir3 127.5(19) . . ? Ir1 C8 Ir3 83.0(10) . . ? C10 C9 C17 148(2) . . ? C10 C9 P3 69.5(14) . . ? C17 C9 P3 142.6(16) . . ? C9 C10 C23 146(2) . . ? C9 C10 P3 66.9(13) . . ? C23 C10 P3 146.4(17) . . ? C18 C17 C22 120.0 . . ? C18 C17 C9 122.1(14) . . ? C22 C17 C9 117.9(14) . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C24 C23 C28 120.0 . . ? C24 C23 C10 120.3(13) . . ? C28 C23 C10 119.6(13) . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C27 C26 C25 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C23 120.0 . . ? C30 C29 C34 120.0 . . ? C30 C29 P2 119.8(8) . . ? C34 C29 P2 119.9(8) . . ? C31 C30 C29 120.0 . . ? C30 C31 C32 120.0 . . ? C33 C32 C31 120.0 . . ? C34 C33 C32 120.0 . . ? C33 C34 C29 120.0 . . ? C36 C35 C40 120.0 . . ? C36 C35 P2 121.5(8) . . ? C40 C35 P2 118.4(8) . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C37 C38 C39 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P1 118.1(9) . . ? C46 C41 P1 121.8(9) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C54 C53 C58 120.0 . . ? C54 C53 P1 117.9(10) . . ? C58 C53 P1 122.1(10) . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C56 C57 C58 120.0 . . ? C57 C58 C53 120.0 . . ? C12 C11 C16 120.0 . . ? C12 C11 P3 121.6(17) . . ? C16 C11 P3 118.4(17) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 P1 123.4(16) . . ? C52 C47 P1 116.6(16) . . ? C47 C48 C49 120.0 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C52 120.0 . . ? C51 C52 C47 120.0 . . ? C12A C11A C16A 120.0 . . ? C12A C11A P3 120(2) . . ? C16A C11A P3 120(2) . . ? C11A C12A C13A 120.0 . . ? C14A C13A C12A 120.0 . . ? C15A C14A C13A 120.0 . . ? C14A C15A C16A 120.0 . . ? C15A C16A C11A 120.0 . . ? C48A C47A C52A 120.0 . . ? C48A C47A P1 116(4) . . ? C52A C47A P1 122(4) . . ? C49A C48A C47A 120.0 . . ? C48A C49A C50A 120.0 . . ? C51A C50A C49A 120.0 . . ? C52A C51A C50A 120.0 . . ? C51A C52A C47A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 21.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.511 _refine_diff_density_min -1.824 _refine_diff_density_rms 0.234 #===END data_nov998 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[HIr4(CO)7(PPH2)(PPh3)(PPhCPhCPh)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H41 Ir4 O7 P3' _chemical_formula_weight 1699.61 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' '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 15.174(6) _cell_length_b 20.952(5) _cell_length_c 17.733(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.27(3) _cell_angle_gamma 90.00 _cell_volume 5322(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.121 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3168 _exptl_absorpt_coefficient_mu 10.112 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6770 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.2130 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 21.97 _reflns_number_total 6485 _reflns_number_gt 3292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6485 _refine_ls_number_parameters 224 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1798 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.16449(9) -0.02122(7) 0.23429(7) 0.0296(4) Uani 1 1 d . . . Ir2 Ir 0.07758(9) -0.07982(6) 0.34129(7) 0.0297(4) Uani 1 1 d . . . Ir3 Ir 0.07842(10) -0.13704(6) 0.19416(8) 0.0341(4) Uani 1 1 d . . . Ir4 Ir -0.02100(9) -0.02866(7) 0.19712(7) 0.0321(4) Uani 1 1 d . . . P1 P 0.3245(6) -0.0404(4) 0.2578(5) 0.037(2) Uani 1 1 d . . . P2 P 0.0147(6) -0.1774(4) 0.2842(5) 0.033(2) Uani 1 1 d . . . P3 P 0.1368(6) 0.0235(4) 0.3397(5) 0.031(2) Uani 1 1 d . . . O1 O 0.1523(19) 0.0975(13) 0.1376(15) 0.077(9) Uiso 1 1 d . . . O2 O -0.0755(18) -0.0286(13) 0.3955(14) 0.066(8) Uiso 1 1 d . . . O3 O 0.2145(18) -0.1305(12) 0.4963(14) 0.062(7) Uiso 1 1 d . . . O4 O 0.211(2) -0.2443(15) 0.1944(17) 0.093(10) Uiso 1 1 d . . . O5 O -0.069(2) -0.1557(13) 0.0357(16) 0.082(9) Uiso 1 1 d . . . O6 O -0.064(2) 0.0314(14) 0.0320(17) 0.084(9) Uiso 1 1 d . . . O7 O -0.228(2) -0.0594(13) 0.1690(16) 0.084(9) Uiso 1 1 d . . . C1 C 0.154(3) 0.0525(18) 0.179(2) 0.051(11) Uiso 1 1 d . . . C2 C -0.018(3) -0.054(2) 0.378(3) 0.083(15) Uiso 1 1 d . . . C3 C 0.165(2) -0.1120(15) 0.4349(19) 0.038(9) Uiso 1 1 d . . . C4 C 0.162(3) -0.2010(18) 0.195(2) 0.051(11) Uiso 1 1 d . . . C5 C -0.013(2) -0.1500(16) 0.099(2) 0.044(10) Uiso 1 1 d . . . C6 C -0.044(3) 0.0058(19) 0.095(2) 0.069(13) Uiso 1 1 d . . . C7 C -0.146(3) -0.0503(16) 0.180(2) 0.046(10) Uiso 1 1 d . . . C9 C 0.040(2) 0.0776(15) 0.3120(17) 0.035(8) Uiso 1 1 d . . . C10 C -0.032(2) 0.0641(13) 0.2477(15) 0.022(7) Uiso 1 1 d . . . C11 C 0.2237(14) 0.0575(10) 0.4261(11) 0.031(8) Uiso 1 1 d G . . C12 C 0.2180(15) 0.0446(10) 0.5013(13) 0.059(11) Uiso 1 1 d G . . H12 H 0.1731 0.0164 0.5066 0.071 Uiso 1 1 calc R . . C13 C 0.2795(18) 0.0738(12) 0.5685(10) 0.076(13) Uiso 1 1 d G . . H13 H 0.2757 0.0652 0.6188 0.092 Uiso 1 1 calc R . . C14 C 0.3467(16) 0.1160(12) 0.5606(11) 0.072(13) Uiso 1 1 d G . . H14 H 0.3878 0.1355 0.6055 0.087 Uiso 1 1 calc R . . C15 C 0.3523(14) 0.1289(10) 0.4854(14) 0.065(12) Uiso 1 1 d G . . H15 H 0.3973 0.1571 0.4801 0.078 Uiso 1 1 calc R . . C16 C 0.2908(16) 0.0997(11) 0.4182(10) 0.051(10) Uiso 1 1 d G . . H16 H 0.2946 0.1083 0.3679 0.061 Uiso 1 1 calc R . . C17 C 0.0435(15) 0.1380(9) 0.3618(12) 0.030(8) Uiso 1 1 d G . . C18 C 0.1001(14) 0.1889(11) 0.3570(12) 0.055(11) Uiso 1 1 d G . . H18 H 0.1375 0.1858 0.3248 0.067 Uiso 1 1 calc R . . C19 C 0.1009(15) 0.2443(9) 0.4002(14) 0.060(11) Uiso 1 1 d G . . H19 H 0.1388 0.2784 0.3969 0.071 Uiso 1 1 calc R . . C20 C 0.0450(17) 0.2489(9) 0.4483(13) 0.051(10) Uiso 1 1 d G . . H20 H 0.0455 0.2860 0.4772 0.062 Uiso 1 1 calc R . . C21 C -0.0116(15) 0.1980(11) 0.4531(12) 0.068(13) Uiso 1 1 d G . . H21 H -0.0490 0.2010 0.4853 0.082 Uiso 1 1 calc R . . C22 C -0.0123(14) 0.1425(9) 0.4099(13) 0.050(10) Uiso 1 1 d G . . H22 H -0.0502 0.1085 0.4132 0.060 Uiso 1 1 calc R . . C23 C -0.1108(15) 0.1000(11) 0.2102(13) 0.055(11) Uiso 1 1 d G . . C24 C -0.1079(15) 0.1440(12) 0.1524(14) 0.054(11) Uiso 1 1 d G . . H24 H -0.0533 0.1495 0.1402 0.065 Uiso 1 1 calc R . . C25 C -0.187(2) 0.1799(10) 0.1128(12) 0.077(13) Uiso 1 1 d G . . H25 H -0.1848 0.2093 0.0742 0.092 Uiso 1 1 calc R . . C26 C -0.2683(16) 0.1717(12) 0.1311(15) 0.092(15) Uiso 1 1 d G . . H26 H -0.3210 0.1957 0.1047 0.111 Uiso 1 1 calc R . . C27 C -0.2711(15) 0.1277(13) 0.1889(16) 0.080(14) Uiso 1 1 d G . . H27 H -0.3257 0.1223 0.2012 0.096 Uiso 1 1 calc R . . C28 C -0.1924(19) 0.0919(11) 0.2285(13) 0.072(13) Uiso 1 1 d G . . H28 H -0.1943 0.0624 0.2672 0.086 Uiso 1 1 calc R . . C29 C -0.1096(12) -0.1932(10) 0.2539(13) 0.032(8) Uiso 1 1 d G . . C30 C -0.1635(17) -0.1760(11) 0.3006(11) 0.066(12) Uiso 1 1 d G . . H30 H -0.1356 -0.1567 0.3500 0.079 Uiso 1 1 calc R . . C31 C -0.2590(16) -0.1877(12) 0.2736(15) 0.082(14) Uiso 1 1 d G . . H31 H -0.2950 -0.1762 0.3049 0.098 Uiso 1 1 calc R . . C32 C -0.3006(12) -0.2167(12) 0.1999(16) 0.077(14) Uiso 1 1 d G . . H32 H -0.3645 -0.2245 0.1818 0.092 Uiso 1 1 calc R . . C33 C -0.2468(16) -0.2339(11) 0.1531(11) 0.069(13) Uiso 1 1 d G . . H33 H -0.2746 -0.2532 0.1038 0.083 Uiso 1 1 calc R . . C34 C -0.1513(15) -0.2221(10) 0.1801(12) 0.043(10) Uiso 1 1 d G . . H34 H -0.1152 -0.2336 0.1489 0.052 Uiso 1 1 calc R . . C35 C 0.0649(15) -0.2492(9) 0.3423(11) 0.038(9) Uiso 1 1 d G . . C36 C 0.0089(12) -0.2958(11) 0.3590(13) 0.051(10) Uiso 1 1 d G . . H36 H -0.0557 -0.2911 0.3409 0.061 Uiso 1 1 calc R . . C37 C 0.0493(17) -0.3495(10) 0.4028(14) 0.075(13) Uiso 1 1 d G . . H37 H 0.0118 -0.3807 0.4140 0.090 Uiso 1 1 calc R . . C38 C 0.1458(17) -0.3566(9) 0.4299(13) 0.075(13) Uiso 1 1 d G . . H38 H 0.1728 -0.3926 0.4593 0.090 Uiso 1 1 calc R . . C39 C 0.2018(12) -0.3100(11) 0.4132(13) 0.054(11) Uiso 1 1 d G . . H39 H 0.2664 -0.3148 0.4313 0.065 Uiso 1 1 calc R . . C40 C 0.1614(14) -0.2563(9) 0.3694(12) 0.045(10) Uiso 1 1 d G . . H40 H 0.1989 -0.2251 0.3582 0.054 Uiso 1 1 calc R . . C41 C 0.4045(14) 0.0196(9) 0.3150(12) 0.033(8) Uiso 1 1 d G . . C42 C 0.3970(13) 0.0808(10) 0.2835(10) 0.031(8) Uiso 1 1 d G . . H42 H 0.3466 0.0914 0.2386 0.037 Uiso 1 1 calc R . . C43 C 0.4647(16) 0.1263(8) 0.3190(13) 0.051(10) Uiso 1 1 d G . . H43 H 0.4596 0.1673 0.2978 0.062 Uiso 1 1 calc R . . C44 C 0.5400(14) 0.1104(11) 0.3860(13) 0.088(15) Uiso 1 1 d G . . H44 H 0.5853 0.1408 0.4098 0.106 Uiso 1 1 calc R . . C45 C 0.5475(14) 0.0492(12) 0.4176(11) 0.064(12) Uiso 1 1 d G . . H45 H 0.5978 0.0386 0.4625 0.077 Uiso 1 1 calc R . . C46 C 0.4798(17) 0.0037(9) 0.3821(13) 0.074(13) Uiso 1 1 d G . . H46 H 0.4848 -0.0373 0.4032 0.089 Uiso 1 1 calc R . . C47 C 0.3716(15) -0.1157(8) 0.3085(12) 0.035(9) Uiso 1 1 d G . . C48 C 0.3564(15) -0.1306(10) 0.3795(12) 0.052(10) Uiso 1 1 d G . . H48 H 0.3254 -0.1018 0.4019 0.062 Uiso 1 1 calc R . . C49 C 0.3875(16) -0.1884(11) 0.4172(10) 0.062(12) Uiso 1 1 d G . . H49 H 0.3773 -0.1984 0.4648 0.075 Uiso 1 1 calc R . . C50 C 0.4338(16) -0.2315(8) 0.3839(12) 0.045(10) Uiso 1 1 d G . . H50 H 0.4546 -0.2702 0.4091 0.054 Uiso 1 1 calc R . . C51 C 0.4490(15) -0.2166(9) 0.3128(13) 0.054(11) Uiso 1 1 d G . . H51 H 0.4800 -0.2454 0.2904 0.064 Uiso 1 1 calc R . . C52 C 0.4180(16) -0.1587(10) 0.2751(10) 0.050(10) Uiso 1 1 d G . . H52 H 0.4282 -0.1488 0.2275 0.060 Uiso 1 1 calc R . . C53 C 0.3564(16) -0.0438(11) 0.1672(11) 0.045(10) Uiso 1 1 d G . . C54 C 0.2885(12) -0.0497(11) 0.0925(14) 0.064(12) Uiso 1 1 d G . . H54 H 0.2258 -0.0519 0.0882 0.077 Uiso 1 1 calc R . . C55 C 0.3143(16) -0.0523(11) 0.0243(11) 0.070(13) Uiso 1 1 d G . . H55 H 0.2688 -0.0563 -0.0257 0.084 Uiso 1 1 calc R . . C56 C 0.4080(19) -0.0490(12) 0.0308(12) 0.083(14) Uiso 1 1 d G . . H56 H 0.4252 -0.0508 -0.0148 0.100 Uiso 1 1 calc R . . C57 C 0.4759(13) -0.0431(12) 0.1055(15) 0.068(12) Uiso 1 1 d G . . H57 H 0.5386 -0.0409 0.1099 0.081 Uiso 1 1 calc R . . C58 C 0.4501(14) -0.0405(10) 0.1738(11) 0.054(11) Uiso 1 1 d G . . H58 H 0.4955 -0.0365 0.2238 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0274(8) 0.0339(8) 0.0259(7) -0.0011(7) 0.0066(6) -0.0028(7) Ir2 0.0270(8) 0.0327(8) 0.0279(7) -0.0022(7) 0.0069(6) -0.0038(7) Ir3 0.0309(8) 0.0360(8) 0.0339(8) -0.0082(7) 0.0085(7) -0.0026(8) Ir4 0.0252(8) 0.0365(8) 0.0305(7) -0.0039(7) 0.0034(6) -0.0012(8) P1 0.030(6) 0.035(6) 0.037(5) 0.009(5) -0.002(4) -0.002(5) P2 0.029(5) 0.029(5) 0.040(6) -0.004(4) 0.008(4) -0.003(5) P3 0.031(5) 0.024(5) 0.035(5) -0.017(4) 0.008(4) -0.005(5) _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 1.81(4) . ? Ir1 P3 2.250(8) . ? Ir1 P1 2.359(9) . ? Ir1 Ir4 2.675(2) . ? Ir1 Ir3 2.736(2) . ? Ir1 Ir2 2.915(2) . ? Ir2 C2 1.85(5) . ? Ir2 C3 1.88(3) . ? Ir2 P2 2.340(9) . ? Ir2 P3 2.347(9) . ? Ir2 Ir4 2.720(2) . ? Ir2 Ir3 2.875(2) . ? Ir3 C5 1.82(3) . ? Ir3 C4 1.84(4) . ? Ir3 P2 2.284(9) . ? Ir3 Ir4 2.736(2) . ? Ir4 C7 1.87(4) . ? Ir4 C6 1.87(4) . ? Ir4 C10 2.17(3) . ? P1 C41 1.808(18) . ? P1 C53 1.825(19) . ? P1 C47 1.839(17) . ? P2 C29 1.813(18) . ? P2 C35 1.841(18) . ? P3 C9 1.79(3) . ? P3 C11 1.806(17) . ? O1 C1 1.19(4) . ? O2 C2 1.15(5) . ? O3 C3 1.17(3) . ? O4 C4 1.18(4) . ? O5 C5 1.17(4) . ? O6 C6 1.18(4) . ? O7 C7 1.21(4) . ? C9 C10 1.32(4) . ? C9 C17 1.54(3) . ? C10 C23 1.39(3) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 P3 95.0(11) . . ? C1 Ir1 P1 98.0(12) . . ? P3 Ir1 P1 112.8(3) . . ? C1 Ir1 Ir4 91.3(12) . . ? P3 Ir1 Ir4 76.1(2) . . ? P1 Ir1 Ir4 166.3(2) . . ? C1 Ir1 Ir3 132.1(11) . . ? P3 Ir1 Ir3 112.4(2) . . ? P1 Ir1 Ir3 105.7(2) . . ? Ir4 Ir1 Ir3 60.74(5) . . ? C1 Ir1 Ir2 137.4(12) . . ? P3 Ir1 Ir2 52.1(2) . . ? P1 Ir1 Ir2 118.3(2) . . ? Ir4 Ir1 Ir2 58.04(5) . . ? Ir3 Ir1 Ir2 61.07(5) . . ? C2 Ir2 C3 101.8(16) . . ? C2 Ir2 P2 98.8(14) . . ? C3 Ir2 P2 97.9(10) . . ? C2 Ir2 P3 94.5(14) . . ? C3 Ir2 P3 100.4(10) . . ? P2 Ir2 P3 154.6(3) . . ? C2 Ir2 Ir4 87.7(13) . . ? C3 Ir2 Ir4 169.3(10) . . ? P2 Ir2 Ir4 85.3(2) . . ? P3 Ir2 Ir4 73.7(2) . . ? C2 Ir2 Ir3 132.6(13) . . ? C3 Ir2 Ir3 116.1(10) . . ? P2 Ir2 Ir3 50.7(2) . . ? P3 Ir2 Ir3 104.9(2) . . ? Ir4 Ir2 Ir3 58.48(5) . . ? C2 Ir2 Ir1 132.6(13) . . ? C3 Ir2 Ir1 112.8(10) . . ? P2 Ir2 Ir1 107.1(2) . . ? P3 Ir2 Ir1 49.2(2) . . ? Ir4 Ir2 Ir1 56.55(5) . . ? Ir3 Ir2 Ir1 56.40(5) . . ? C5 Ir3 C4 102.2(15) . . ? C5 Ir3 P2 103.2(11) . . ? C4 Ir3 P2 99.9(11) . . ? C5 Ir3 Ir1 121.7(11) . . ? C4 Ir3 Ir1 112.1(11) . . ? P2 Ir3 Ir1 115.0(2) . . ? C5 Ir3 Ir4 83.5(11) . . ? C4 Ir3 Ir4 170.5(11) . . ? P2 Ir3 Ir4 86.0(2) . . ? Ir1 Ir3 Ir4 58.52(5) . . ? C5 Ir3 Ir2 132.6(11) . . ? C4 Ir3 Ir2 120.2(11) . . ? P2 Ir3 Ir2 52.4(2) . . ? Ir1 Ir3 Ir2 62.54(5) . . ? Ir4 Ir3 Ir2 57.92(5) . . ? C7 Ir4 C6 94.6(16) . . ? C7 Ir4 C10 94.3(13) . . ? C6 Ir4 C10 92.2(14) . . ? C7 Ir4 Ir1 168.5(11) . . ? C6 Ir4 Ir1 93.5(13) . . ? C10 Ir4 Ir1 93.5(8) . . ? C7 Ir4 Ir2 105.7(10) . . ? C6 Ir4 Ir2 158.5(13) . . ? C10 Ir4 Ir2 93.3(7) . . ? Ir1 Ir4 Ir2 65.41(6) . . ? C7 Ir4 Ir3 109.3(11) . . ? C6 Ir4 Ir3 103.3(12) . . ? C10 Ir4 Ir3 150.2(7) . . ? Ir1 Ir4 Ir3 60.74(5) . . ? Ir2 Ir4 Ir3 63.60(5) . . ? C41 P1 C53 101.4(11) . . ? C41 P1 C47 104.0(10) . . ? C53 P1 C47 102.9(11) . . ? C41 P1 Ir1 116.2(8) . . ? C53 P1 Ir1 114.0(8) . . ? C47 P1 Ir1 116.4(8) . . ? C29 P2 C35 102.4(11) . . ? C29 P2 Ir3 120.0(8) . . ? C35 P2 Ir3 120.1(8) . . ? C29 P2 Ir2 121.6(9) . . ? C35 P2 Ir2 116.0(8) . . ? Ir3 P2 Ir2 76.9(3) . . ? C9 P3 C11 106.5(13) . . ? C9 P3 Ir1 113.3(10) . . ? C11 P3 Ir1 125.8(8) . . ? C9 P3 Ir2 107.8(11) . . ? C11 P3 Ir2 121.9(8) . . ? Ir1 P3 Ir2 78.7(3) . . ? O1 C1 Ir1 173(3) . . ? O2 C2 Ir2 170(4) . . ? O3 C3 Ir2 174(3) . . ? O4 C4 Ir3 176(3) . . ? O5 C5 Ir3 176(3) . . ? O6 C6 Ir4 174(4) . . ? O7 C7 Ir4 175(3) . . ? C10 C9 C17 122(3) . . ? C10 C9 P3 118(2) . . ? C17 C9 P3 120(2) . . ? C9 C10 C23 129(3) . . ? C9 C10 Ir4 113(2) . . ? C23 C10 Ir4 117.3(18) . . ? C12 C11 C16 120.0 . . ? C12 C11 P3 118.6(14) . . ? C16 C11 P3 121.3(14) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C11 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 C9 119.9(19) . . ? C22 C17 C9 120.0(19) . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C20 C21 C22 120.0 . . ? C21 C22 C17 120.0 . . ? C10 C23 C24 119(2) . . ? C10 C23 C28 121(2) . . ? C24 C23 C28 120.0 . . ? C25 C24 C23 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C23 120.0 . . ? C30 C29 C34 120.0 . . ? C30 C29 P2 122.3(14) . . ? C34 C29 P2 117.6(14) . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C29 120.0 . . ? C36 C35 C40 120.0 . . ? C36 C35 P2 121.6(14) . . ? C40 C35 P2 118.4(14) . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 P1 117.7(13) . . ? C46 C41 P1 121.6(13) . . ? C43 C42 C41 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 P1 118.7(13) . . ? C52 C47 P1 121.2(13) . . ? C49 C48 C47 120.0 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C52 120.0 . . ? C51 C52 C47 120.0 . . ? C54 C53 C58 120.0 . . ? C54 C53 P1 120.9(14) . . ? C58 C53 P1 119.1(14) . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C57 120.0 . . ? C56 C57 C58 120.0 . . ? C57 C58 C53 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.375 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.303 #===END data_oct898 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Ir4(CO)8(PPh2)(PHPCPhCPh)(PhPCPhCHPh)]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H41 Ir4 O8 P3' _chemical_formula_weight 1751.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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 22.206(4) _cell_length_b 17.563(2) _cell_length_c 35.748(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.08(2) _cell_angle_gamma 90.00 _cell_volume 13727(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6544 _exptl_absorpt_coefficient_mu 7.845 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.57 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19632 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.1747 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 23.00 _reflns_number_total 19075 _reflns_number_gt 8760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Two independent molecules, equivalently labelled. Ir,P anisotropic, C,O isotropic, phenyl groups as rigid bodies. H atoms riding. 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^)+(0.0882P)^2^+61.9906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19075 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1980 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2466 _refine_ls_wR_factor_gt 0.1923 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.08737(6) 0.78934(7) 0.11329(4) 0.0491(4) Uani 1 1 d . . . Ir2 Ir -0.04010(6) 0.83136(7) 0.12287(4) 0.0514(4) Uani 1 1 d . . . Ir3 Ir 0.00187(6) 0.66176(6) 0.13735(4) 0.0482(4) Uani 1 1 d . . . Ir4 Ir 0.04942(6) 0.78899(6) 0.18196(4) 0.0463(3) Uani 1 1 d . . . P1 P 0.0957(4) 0.6558(4) 0.1182(2) 0.047(2) Uani 1 1 d . . . P2 P -0.0930(3) 0.7200(4) 0.1342(2) 0.047(2) Uani 1 1 d . . . P3 P 0.0439(4) 0.9070(4) 0.1200(3) 0.052(2) Uani 1 1 d . . . O1 O 0.2122(12) 0.8434(13) 0.1484(7) 0.089(8) Uiso 1 1 d . . . O2 O 0.0844(13) 0.7969(15) 0.0278(9) 0.115(10) Uiso 1 1 d . . . O3 O -0.0903(11) 0.9379(14) 0.1756(7) 0.094(8) Uiso 1 1 d . . . O4 O -0.1118(13) 0.8662(15) 0.0453(9) 0.108(9) Uiso 1 1 d . . . O5 O -0.0490(12) 0.5206(15) 0.0951(8) 0.102(9) Uiso 1 1 d . . . O6 O 0.0292(10) 0.6026(12) 0.2143(7) 0.074(7) Uiso 1 1 d . . . O7 O 0.1712(11) 0.7324(12) 0.2231(7) 0.077(7) Uiso 1 1 d . . . O8 O -0.0246(10) 0.7903(11) 0.2441(6) 0.068(6) Uiso 1 1 d . . . C1 C 0.1658(18) 0.820(2) 0.1337(11) 0.084(12) Uiso 1 1 d . . . C2 C 0.0819(16) 0.7939(18) 0.0613(11) 0.071(10) Uiso 1 1 d . . . C3 C -0.0706(17) 0.893(2) 0.1562(11) 0.083(12) Uiso 1 1 d . . . C4 C -0.084(2) 0.852(2) 0.0756(13) 0.100(14) Uiso 1 1 d . . . C5 C -0.0309(15) 0.5808(18) 0.1106(9) 0.064(9) Uiso 1 1 d . . . C6 C 0.0225(16) 0.6298(19) 0.1850(11) 0.076(11) Uiso 1 1 d . . . C7 C 0.1251(14) 0.7564(16) 0.2072(9) 0.056(9) Uiso 1 1 d . . . C8 C 0.0011(14) 0.7931(17) 0.2194(10) 0.060(9) Uiso 1 1 d . . . C9 C 0.0716(14) 0.9516(17) 0.1630(9) 0.060(9) Uiso 1 1 d . . . C10 C 0.0796(14) 0.9051(16) 0.1956(9) 0.057(9) Uiso 1 1 d . . . C11 C 0.0411(10) 0.9768(10) 0.0828(5) 0.046(8) Uiso 1 1 d G . . C12 C -0.0104(8) 1.0230(12) 0.0742(6) 0.067(10) Uiso 1 1 d G . . H12 H -0.0432 1.0159 0.0868 0.080 Uiso 1 1 calc R . . C13 C -0.0127(10) 1.0796(11) 0.0469(7) 0.112(15) Uiso 1 1 d G . . H13 H -0.0471 1.1105 0.0411 0.135 Uiso 1 1 calc R . . C14 C 0.0364(12) 1.0901(11) 0.0280(6) 0.098(13) Uiso 1 1 d G . . H14 H 0.0349 1.1280 0.0097 0.117 Uiso 1 1 calc R . . C15 C 0.0878(10) 1.0439(13) 0.0366(6) 0.096(13) Uiso 1 1 d G . . H15 H 0.1207 1.0509 0.0240 0.115 Uiso 1 1 calc R . . C16 C 0.0901(8) 0.9873(12) 0.0639(7) 0.082(11) Uiso 1 1 d G . . H16 H 0.1245 0.9564 0.0696 0.098 Uiso 1 1 calc R . . C17 C 0.0914(9) 1.0332(9) 0.1675(6) 0.048(8) Uiso 1 1 d G . . C18 C 0.1478(8) 1.0556(10) 0.1594(6) 0.068(10) Uiso 1 1 d G . . H18 H 0.1752 1.0192 0.1537 0.082 Uiso 1 1 calc R . . C19 C 0.1632(8) 1.1323(12) 0.1599(6) 0.071(10) Uiso 1 1 d G . . H19 H 0.2009 1.1473 0.1545 0.085 Uiso 1 1 calc R . . C20 C 0.1222(11) 1.1867(8) 0.1685(7) 0.078(11) Uiso 1 1 d G . . H20 H 0.1325 1.2381 0.1688 0.093 Uiso 1 1 calc R . . C21 C 0.0658(10) 1.1644(11) 0.1765(7) 0.106(14) Uiso 1 1 d G . . H21 H 0.0384 1.2008 0.1822 0.127 Uiso 1 1 calc R . . C22 C 0.0504(8) 1.0876(12) 0.1760(6) 0.073(10) Uiso 1 1 d G . . H22 H 0.0126 1.0727 0.1814 0.087 Uiso 1 1 calc R . . C23 C 0.1012(10) 0.9249(11) 0.2337(5) 0.053(8) Uiso 1 1 d G . . C24 C 0.1633(9) 0.9199(12) 0.2484(7) 0.082(11) Uiso 1 1 d G . . H24 H 0.1906 0.9047 0.2328 0.098 Uiso 1 1 calc R . . C25 C 0.1846(8) 0.9374(13) 0.2863(7) 0.127(17) Uiso 1 1 d G . . H25 H 0.2262 0.9340 0.2961 0.153 Uiso 1 1 calc R . . C26 C 0.1438(11) 0.9600(12) 0.3095(5) 0.085(12) Uiso 1 1 d G . . H26 H 0.1580 0.9718 0.3349 0.102 Uiso 1 1 calc R . . C27 C 0.0817(10) 0.9651(11) 0.2948(6) 0.076(11) Uiso 1 1 d G . . H27 H 0.0544 0.9802 0.3104 0.091 Uiso 1 1 calc R . . C28 C 0.0604(7) 0.9475(11) 0.2569(6) 0.064(9) Uiso 1 1 d G . . H28 H 0.0189 0.9509 0.2471 0.077 Uiso 1 1 calc R . . C29 C -0.1314(9) 0.7223(12) 0.1734(6) 0.061(9) Uiso 1 1 d G . . C30 C -0.1714(10) 0.7815(10) 0.1772(6) 0.069(10) Uiso 1 1 d G . . H30 H -0.1758 0.8219 0.1601 0.083 Uiso 1 1 calc R . . C31 C -0.2050(9) 0.7803(11) 0.2066(7) 0.083(11) Uiso 1 1 d G . . H31 H -0.2318 0.8199 0.2092 0.100 Uiso 1 1 calc R . . C32 C -0.1985(10) 0.7200(14) 0.2322(6) 0.087(12) Uiso 1 1 d G . . H32 H -0.2209 0.7192 0.2518 0.104 Uiso 1 1 calc R . . C33 C -0.1585(11) 0.6608(11) 0.2283(6) 0.098(13) Uiso 1 1 d G . . H33 H -0.1541 0.6204 0.2454 0.117 Uiso 1 1 calc R . . C34 C -0.1249(9) 0.6620(10) 0.1989(7) 0.074(10) Uiso 1 1 d G . . H34 H -0.0981 0.6224 0.1964 0.089 Uiso 1 1 calc R . . C35 C -0.1498(11) 0.6861(11) 0.0948(6) 0.053(8) Uiso 1 1 d G . . C36 C -0.2075(13) 0.6663(14) 0.1016(7) 0.117(15) Uiso 1 1 d G . . H36 H -0.2165 0.6701 0.1260 0.141 Uiso 1 1 calc R . . C37 C -0.2519(9) 0.6408(16) 0.0719(10) 0.19(3) Uiso 1 1 d G . . H37 H -0.2905 0.6275 0.0764 0.234 Uiso 1 1 calc R . . C38 C -0.2385(12) 0.6351(15) 0.0354(8) 0.15(2) Uiso 1 1 d G . . H38 H -0.2682 0.6181 0.0156 0.181 Uiso 1 1 calc R . . C39 C -0.1807(14) 0.6550(14) 0.0287(5) 0.106(14) Uiso 1 1 d G . . H39 H -0.1718 0.6512 0.0043 0.128 Uiso 1 1 calc R . . C40 C -0.1364(9) 0.6804(12) 0.0584(7) 0.070(10) Uiso 1 1 d G . . H40 H -0.0977 0.6937 0.0539 0.084 Uiso 1 1 calc R . . C41 C 0.2805(8) 0.6193(12) 0.1641(6) 0.057(9) Uiso 1 1 d G . . C42 C 0.3246(12) 0.6751(9) 0.1746(7) 0.086(12) Uiso 1 1 d G . . H42 H 0.3140 0.7263 0.1720 0.104 Uiso 1 1 calc R . . C43 C 0.3846(10) 0.6543(14) 0.1889(7) 0.128(17) Uiso 1 1 d G . . H43 H 0.4142 0.6916 0.1959 0.153 Uiso 1 1 calc R . . C44 C 0.4005(8) 0.5778(16) 0.1928(7) 0.115(15) Uiso 1 1 d G . . H44 H 0.4406 0.5639 0.2024 0.138 Uiso 1 1 calc R . . C45 C 0.3563(11) 0.5220(11) 0.1824(7) 0.098(13) Uiso 1 1 d G . . H45 H 0.3669 0.4708 0.1850 0.117 Uiso 1 1 calc R . . C46 C 0.2963(10) 0.5428(11) 0.1680(6) 0.069(10) Uiso 1 1 d G . . H46 H 0.2668 0.5055 0.1610 0.083 Uiso 1 1 calc R . . C47 C 0.0943(12) 0.6066(12) 0.0728(6) 0.063(9) Uiso 1 1 d G . . C48 C 0.0458(10) 0.6178(13) 0.0429(8) 0.108(14) Uiso 1 1 d G . . H48 H 0.0132 0.6488 0.0462 0.129 Uiso 1 1 calc R . . C49 C 0.0461(11) 0.5826(15) 0.0081(6) 0.108(14) Uiso 1 1 d G . . H49 H 0.0137 0.5900 -0.0119 0.129 Uiso 1 1 calc R . . C50 C 0.0949(14) 0.5363(14) 0.0032(6) 0.128(17) Uiso 1 1 d G . . H50 H 0.0951 0.5127 -0.0201 0.154 Uiso 1 1 calc R . . C51 C 0.1433(11) 0.5251(13) 0.0330(9) 0.139(18) Uiso 1 1 d G . . H51 H 0.1760 0.4941 0.0297 0.167 Uiso 1 1 calc R . . C52 C 0.1430(10) 0.5603(14) 0.0678(7) 0.093(12) Uiso 1 1 d G . . H52 H 0.1754 0.5529 0.0878 0.112 Uiso 1 1 calc R . . C53 C 0.1513(10) 0.5470(10) 0.1722(6) 0.051(8) Uiso 1 1 d G . . C54 C 0.1125(9) 0.4889(13) 0.1564(5) 0.080(11) Uiso 1 1 d G . . H54 H 0.0937 0.4916 0.1311 0.096 Uiso 1 1 calc R . . C55 C 0.1020(9) 0.4267(11) 0.1785(7) 0.094(13) Uiso 1 1 d G . . H55 H 0.0760 0.3878 0.1679 0.113 Uiso 1 1 calc R . . C56 C 0.1302(11) 0.4227(11) 0.2163(7) 0.100(13) Uiso 1 1 d G . . H56 H 0.1231 0.3811 0.2311 0.120 Uiso 1 1 calc R . . C57 C 0.1689(10) 0.4808(13) 0.2321(5) 0.083(11) Uiso 1 1 d G . . H57 H 0.1878 0.4781 0.2575 0.100 Uiso 1 1 calc R . . C58 C 0.1795(9) 0.5429(10) 0.2101(6) 0.069(10) Uiso 1 1 d G . . H58 H 0.2054 0.5818 0.2207 0.082 Uiso 1 1 calc R . . C59 C 0.1607(13) 0.6126(15) 0.1484(8) 0.046(8) Uiso 1 1 d . . . C60 C 0.2157(14) 0.6457(17) 0.1469(9) 0.063(9) Uiso 1 1 d . . . H60 H 0.2136 0.6912 0.1334 0.076 Uiso 1 1 calc R . . Ir1B Ir 0.40469(6) 0.48906(7) 0.38124(4) 0.0520(4) Uani 1 1 d . . . Ir2B Ir 0.53157(6) 0.44459(7) 0.37404(4) 0.0546(4) Uani 1 1 d . . . Ir3B Ir 0.49404(6) 0.61449(6) 0.35813(4) 0.0515(4) Uani 1 1 d . . . Ir4B Ir 0.44554(6) 0.48825(6) 0.31340(4) 0.0486(4) Uani 1 1 d . . . P1B P 0.3981(4) 0.6219(4) 0.3751(2) 0.051(2) Uani 1 1 d . . . P2B P 0.5886(4) 0.5546(4) 0.3652(3) 0.051(2) Uani 1 1 d . . . P3B P 0.4458(4) 0.3698(4) 0.3744(2) 0.051(2) Uani 1 1 d . . . O1B O 0.2785(13) 0.4374(15) 0.3447(8) 0.104(9) Uiso 1 1 d . . . O2B O 0.4099(15) 0.4810(17) 0.4666(10) 0.131(11) Uiso 1 1 d . . . O3B O 0.5856(12) 0.3368(15) 0.3244(8) 0.101(9) Uiso 1 1 d . . . O4B O 0.5908(15) 0.4128(17) 0.4532(10) 0.138(12) Uiso 1 1 d . . . O5B O 0.5455(13) 0.7529(16) 0.4012(8) 0.119(10) Uiso 1 1 d . . . O6B O 0.4690(9) 0.6731(11) 0.2776(6) 0.068(6) Uiso 1 1 d . . . O7B O 0.3264(11) 0.5429(13) 0.2684(7) 0.085(7) Uiso 1 1 d . . . O8B O 0.5261(10) 0.4837(12) 0.2531(7) 0.072(7) Uiso 1 1 d . . . C1B C 0.3293(16) 0.4612(18) 0.3617(10) 0.068(10) Uiso 1 1 d . . . C2B C 0.4060(19) 0.488(2) 0.4339(13) 0.101(14) Uiso 1 1 d . . . C3B C 0.5648(15) 0.3787(19) 0.3441(10) 0.068(10) Uiso 1 1 d . . . C4B C 0.566(2) 0.420(3) 0.4197(16) 0.136(18) Uiso 1 1 d . . . C5B C 0.5242(15) 0.6968(19) 0.3864(10) 0.067(10) Uiso 1 1 d . . . C6B C 0.4781(14) 0.6471(16) 0.3098(9) 0.056(9) Uiso 1 1 d . . . C7B C 0.3751(16) 0.5251(18) 0.2869(10) 0.072(10) Uiso 1 1 d . . . C8B C 0.4962(15) 0.4874(17) 0.2752(10) 0.062(9) Uiso 1 1 d . . . C9B C 0.4214(13) 0.3269(16) 0.3296(8) 0.049(8) Uiso 1 1 d . . . C10B C 0.4165(14) 0.3748(16) 0.2999(9) 0.057(9) Uiso 1 1 d . . . C11B C 0.4429(11) 0.2988(11) 0.4090(6) 0.047(8) Uiso 1 1 d G . . C12B C 0.4866(10) 0.2414(14) 0.4121(7) 0.105(14) Uiso 1 1 d G . . H12B H 0.5172 0.2431 0.3973 0.126 Uiso 1 1 calc R . . C13B C 0.4845(12) 0.1814(12) 0.4372(8) 0.122(16) Uiso 1 1 d G . . H13B H 0.5138 0.1430 0.4392 0.146 Uiso 1 1 calc R . . C14B C 0.4388(15) 0.1787(13) 0.4592(7) 0.131(17) Uiso 1 1 d G . . H14B H 0.4374 0.1386 0.4760 0.157 Uiso 1 1 calc R . . C15B C 0.3951(12) 0.2361(17) 0.4561(7) 0.15(2) Uiso 1 1 d G . . H15B H 0.3645 0.2344 0.4708 0.177 Uiso 1 1 calc R . . C16B C 0.3971(10) 0.2961(13) 0.4310(8) 0.098(13) Uiso 1 1 d G . . H16B H 0.3679 0.3345 0.4289 0.118 Uiso 1 1 calc R . . C17B C 0.4029(9) 0.2445(8) 0.3260(6) 0.045(8) Uiso 1 1 d G . . C18B C 0.3503(9) 0.2187(11) 0.3381(6) 0.072(10) Uiso 1 1 d G . . H18B H 0.3238 0.2532 0.3463 0.087 Uiso 1 1 calc R . . C19B C 0.3375(8) 0.1412(12) 0.3379(6) 0.079(11) Uiso 1 1 d G . . H19B H 0.3023 0.1239 0.3460 0.095 Uiso 1 1 calc R . . C20B C 0.3772(10) 0.0895(8) 0.3255(6) 0.069(10) Uiso 1 1 d G . . H20B H 0.3687 0.0377 0.3254 0.083 Uiso 1 1 calc R . . C21B C 0.4298(9) 0.1153(11) 0.3134(6) 0.087(12) Uiso 1 1 d G . . H21B H 0.4564 0.0808 0.3052 0.104 Uiso 1 1 calc R . . C22B C 0.4426(8) 0.1928(12) 0.3136(6) 0.074(10) Uiso 1 1 d G . . H22B H 0.4778 0.2101 0.3055 0.088 Uiso 1 1 calc R . . C23B C 0.3956(10) 0.3563(11) 0.2603(5) 0.050(8) Uiso 1 1 d G . . C24B C 0.3333(9) 0.3576(12) 0.2457(6) 0.079(11) Uiso 1 1 d G . . H24B H 0.3057 0.3729 0.2610 0.095 Uiso 1 1 calc R . . C25B C 0.3123(8) 0.3360(12) 0.2083(7) 0.093(12) Uiso 1 1 d G . . H25B H 0.2707 0.3369 0.1985 0.111 Uiso 1 1 calc R . . C26B C 0.3536(11) 0.3131(11) 0.1854(5) 0.077(11) Uiso 1 1 d G . . H26B H 0.3396 0.2986 0.1604 0.093 Uiso 1 1 calc R . . C27B C 0.4159(10) 0.3118(11) 0.2000(6) 0.094(13) Uiso 1 1 d G . . H27B H 0.4435 0.2964 0.1847 0.113 Uiso 1 1 calc R . . C28B C 0.4369(7) 0.3334(11) 0.2374(6) 0.061(9) Uiso 1 1 d G . . H28B H 0.4786 0.3325 0.2472 0.074 Uiso 1 1 calc R . . C29B C 0.6315(9) 0.5506(13) 0.3269(6) 0.060(9) Uiso 1 1 d G . . C30B C 0.6708(10) 0.4902(10) 0.3238(6) 0.079(11) Uiso 1 1 d G . . H30B H 0.6728 0.4492 0.3405 0.095 Uiso 1 1 calc R . . C31B C 0.7072(9) 0.4910(11) 0.2959(7) 0.074(10) Uiso 1 1 d G . . H31B H 0.7335 0.4506 0.2938 0.089 Uiso 1 1 calc R . . C32B C 0.7043(10) 0.5522(14) 0.2710(6) 0.095(13) Uiso 1 1 d G . . H32B H 0.7286 0.5528 0.2523 0.114 Uiso 1 1 calc R . . C33B C 0.6650(11) 0.6126(11) 0.2740(6) 0.093(12) Uiso 1 1 d G . . H33B H 0.6630 0.6536 0.2574 0.111 Uiso 1 1 calc R . . C34B C 0.6286(9) 0.6118(10) 0.3020(7) 0.078(11) Uiso 1 1 d G . . H34B H 0.6023 0.6522 0.3040 0.094 Uiso 1 1 calc R . . C35B C 0.6435(11) 0.5868(12) 0.4049(6) 0.058(9) Uiso 1 1 d G . . C36B C 0.7022(13) 0.6070(14) 0.4002(7) 0.125(16) Uiso 1 1 d G . . H36B H 0.7136 0.6027 0.3765 0.150 Uiso 1 1 calc R . . C37B C 0.7439(9) 0.6337(15) 0.4310(10) 0.138(18) Uiso 1 1 d G . . H37B H 0.7832 0.6472 0.4279 0.166 Uiso 1 1 calc R . . C38B C 0.7269(12) 0.6402(15) 0.4665(8) 0.146(19) Uiso 1 1 d G . . H38B H 0.7548 0.6581 0.4871 0.175 Uiso 1 1 calc R . . C39B C 0.6681(14) 0.6200(14) 0.4712(5) 0.106(14) Uiso 1 1 d G . . H39B H 0.6567 0.6244 0.4949 0.127 Uiso 1 1 calc R . . C40B C 0.6264(9) 0.5933(12) 0.4404(7) 0.075(11) Uiso 1 1 d G . . H40B H 0.5871 0.5798 0.4435 0.090 Uiso 1 1 calc R . . C41B C 0.2166(8) 0.6593(12) 0.3294(6) 0.051(8) Uiso 1 1 d G . . C42B C 0.1751(10) 0.6006(9) 0.3188(6) 0.089(12) Uiso 1 1 d G . . H42B H 0.1881 0.5502 0.3213 0.107 Uiso 1 1 calc R . . C43B C 0.1143(9) 0.6172(11) 0.3043(7) 0.085(11) Uiso 1 1 d G . . H43B H 0.0866 0.5779 0.2972 0.101 Uiso 1 1 calc R . . C44B C 0.0950(8) 0.6925(13) 0.3004(6) 0.083(11) Uiso 1 1 d G . . H44B H 0.0543 0.7036 0.2907 0.099 Uiso 1 1 calc R . . C45B C 0.1364(10) 0.7512(9) 0.3110(7) 0.072(10) Uiso 1 1 d G . . H45B H 0.1235 0.8016 0.3085 0.087 Uiso 1 1 calc R . . C46B C 0.1972(9) 0.7346(10) 0.3255(6) 0.093(13) Uiso 1 1 d G . . H46B H 0.2250 0.7739 0.3326 0.112 Uiso 1 1 calc R . . C47B C 0.3989(10) 0.6758(11) 0.4210(5) 0.045(8) Uiso 1 1 d G . . C48B C 0.4467(8) 0.6635(10) 0.4512(6) 0.059(9) Uiso 1 1 d G . . H48B H 0.4782 0.6304 0.4483 0.071 Uiso 1 1 calc R . . C49B C 0.4472(10) 0.7008(13) 0.4855(5) 0.096(13) Uiso 1 1 d G . . H49B H 0.4791 0.6926 0.5057 0.115 Uiso 1 1 calc R . . C50B C 0.4000(12) 0.7503(13) 0.4897(6) 0.117(16) Uiso 1 1 d G . . H50B H 0.4003 0.7752 0.5127 0.141 Uiso 1 1 calc R . . C51B C 0.3523(10) 0.7626(11) 0.4595(8) 0.093(13) Uiso 1 1 d G . . H51B H 0.3207 0.7957 0.4624 0.112 Uiso 1 1 calc R . . C52B C 0.3517(8) 0.7253(12) 0.4252(6) 0.093(12) Uiso 1 1 d G . . H52B H 0.3198 0.7335 0.4050 0.112 Uiso 1 1 calc R . . C53B C 0.3459(10) 0.7323(10) 0.3213(6) 0.058(9) Uiso 1 1 d G . . C54B C 0.3856(9) 0.7896(12) 0.3370(5) 0.069(10) Uiso 1 1 d G . . H54B H 0.4040 0.7873 0.3624 0.083 Uiso 1 1 calc R . . C55B C 0.3979(9) 0.8505(10) 0.3146(7) 0.073(10) Uiso 1 1 d G . . H55B H 0.4245 0.8888 0.3251 0.088 Uiso 1 1 calc R . . C56B C 0.3705(11) 0.8540(11) 0.2766(6) 0.095(13) Uiso 1 1 d G . . H56B H 0.3787 0.8947 0.2616 0.114 Uiso 1 1 calc R . . C57B C 0.3308(11) 0.7966(14) 0.2609(5) 0.108(14) Uiso 1 1 d G . . H57B H 0.3124 0.7990 0.2355 0.129 Uiso 1 1 calc R . . C58B C 0.3185(9) 0.7358(11) 0.2833(6) 0.070(10) Uiso 1 1 d G . . H58B H 0.2920 0.6974 0.2728 0.084 Uiso 1 1 calc R . . C59B C 0.3327(13) 0.6649(15) 0.3433(8) 0.049(8) Uiso 1 1 d . . . C60B C 0.2769(14) 0.6333(17) 0.3451(9) 0.060(9) Uiso 1 1 d . . . H60B H 0.2783 0.5879 0.3585 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0536(8) 0.0425(7) 0.0518(8) 0.0021(6) 0.0109(7) 0.0024(6) Ir2 0.0510(8) 0.0475(8) 0.0550(9) 0.0070(7) 0.0077(7) 0.0025(6) Ir3 0.0463(8) 0.0405(7) 0.0581(9) -0.0025(6) 0.0103(7) 0.0000(6) Ir4 0.0511(8) 0.0371(7) 0.0509(8) 0.0036(6) 0.0092(7) 0.0002(6) P1 0.041(5) 0.037(4) 0.064(6) -0.003(4) 0.012(4) 0.005(4) P2 0.034(4) 0.049(5) 0.057(6) 0.004(4) 0.010(4) 0.005(4) P3 0.052(5) 0.045(5) 0.063(6) 0.007(4) 0.017(5) 0.010(4) Ir1B 0.0568(8) 0.0442(7) 0.0568(9) 0.0005(6) 0.0152(7) -0.0021(6) Ir2B 0.0518(8) 0.0473(8) 0.0638(10) 0.0055(7) 0.0074(7) -0.0044(6) Ir3B 0.0479(8) 0.0413(7) 0.0665(10) -0.0010(7) 0.0139(7) -0.0015(6) Ir4B 0.0519(8) 0.0399(7) 0.0546(9) 0.0022(6) 0.0113(7) -0.0007(6) P1B 0.048(5) 0.042(5) 0.060(6) 0.006(4) 0.006(5) -0.003(4) P2B 0.044(5) 0.043(5) 0.067(6) -0.004(4) 0.011(5) -0.006(4) P3B 0.057(5) 0.040(5) 0.052(6) 0.012(4) 0.000(5) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C2 1.84(4) . ? Ir1 C1 1.85(4) . ? Ir1 P3 2.310(8) . ? Ir1 P1 2.356(7) . ? Ir1 Ir4 2.7314(19) . ? Ir1 Ir2 3.0023(19) . ? Ir1 Ir3 3.1523(17) . ? Ir2 C3 1.82(4) . ? Ir2 C4 1.83(5) . ? Ir2 P3 2.307(8) . ? Ir2 P2 2.353(8) . ? Ir2 Ir4 2.7381(19) . ? Ir2 Ir3 3.1371(17) . ? Ir3 C6 1.77(4) . ? Ir3 C5 1.80(3) . ? Ir3 P1 2.306(8) . ? Ir3 P2 2.327(7) . ? Ir3 Ir4 2.8394(17) . ? Ir4 C7 1.85(3) . ? Ir4 C8 1.86(3) . ? Ir4 C10 2.17(3) . ? P1 C59 1.81(3) . ? P1 C47 1.83(2) . ? P2 C29 1.763(18) . ? P2 C35 1.82(2) . ? P3 C9 1.74(3) . ? P3 C11 1.803(18) . ? O1 C1 1.15(4) . ? O2 C2 1.21(4) . ? O3 C3 1.19(4) . ? O4 C4 1.18(4) . ? O5 C5 1.23(3) . ? O6 C6 1.14(4) . ? O7 C7 1.16(3) . ? O8 C8 1.13(3) . ? C9 C10 1.41(4) . ? C9 C17 1.50(3) . ? C10 C23 1.41(3) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C17 C18 1.3900 . ? C17 C22 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C23 C24 1.3900 . ? C23 C28 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C29 C30 1.3900 . ? C29 C34 1.3900 . ? C30 C31 1.3900 . ? C31 C32 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C35 C36 1.3900 . ? C35 C40 1.3900 . ? C36 C37 1.3900 . ? C37 C38 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C60 1.53(3) . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C47 C48 1.3900 . ? C47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C53 C59 1.47(3) . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C59 C60 1.36(4) . ? Ir1B C1B 1.77(3) . ? Ir1B C2B 1.88(5) . ? Ir1B P3B 2.315(8) . ? Ir1B P1B 2.346(8) . ? Ir1B Ir4B 2.7340(19) . ? Ir1B Ir2B 2.9780(19) . ? Ir1B Ir3B 3.1696(18) . ? Ir2B C4B 1.73(6) . ? Ir2B C3B 1.82(4) . ? Ir2B P3B 2.316(8) . ? Ir2B P2B 2.362(8) . ? Ir2B Ir4B 2.7361(19) . ? Ir2B Ir3B 3.1235(18) . ? Ir3B C6B 1.79(3) . ? Ir3B C5B 1.82(3) . ? Ir3B P1B 2.319(8) . ? Ir3B P2B 2.323(8) . ? Ir3B Ir4B 2.8336(18) . ? Ir4B C7B 1.80(4) . ? Ir4B C8B 1.92(4) . ? Ir4B C10B 2.12(3) . ? P1B C59B 1.84(3) . ? P1B C47B 1.890(18) . ? P2B C35B 1.79(2) . ? P2B C29B 1.802(18) . ? P3B C11B 1.765(19) . ? P3B C9B 1.77(3) . ? O1B C1B 1.26(4) . ? O2B C2B 1.16(5) . ? O3B C3B 1.17(4) . ? O4B C4B 1.23(5) . ? O5B C5B 1.18(4) . ? O6B C6B 1.22(3) . ? O7B C7B 1.21(4) . ? O8B C8B 1.12(3) . ? C9B C10B 1.34(4) . ? C9B C17B 1.50(3) . ? C10B C23B 1.45(3) . ? C11B C12B 1.3900 . ? C11B C16B 1.3900 . ? C12B C13B 1.3900 . ? C13B C14B 1.3900 . ? C14B C15B 1.3900 . ? C15B C16B 1.3900 . ? C17B C18B 1.3900 . ? C17B C22B 1.3900 . ? C18B C19B 1.3900 . ? C19B C20B 1.3900 . ? C20B C21B 1.3900 . ? C21B C22B 1.3900 . ? C23B C24B 1.3900 . ? C23B C28B 1.3900 . ? C24B C25B 1.3900 . ? C25B C26B 1.3900 . ? C26B C27B 1.3900 . ? C27B C28B 1.3900 . ? C29B C30B 1.3900 . ? C29B C34B 1.3900 . ? C30B C31B 1.3900 . ? C31B C32B 1.3900 . ? C32B C33B 1.3900 . ? C33B C34B 1.3900 . ? C35B C36B 1.3900 . ? C35B C40B 1.3900 . ? C36B C37B 1.3900 . ? C37B C38B 1.3900 . ? C38B C39B 1.3900 . ? C39B C40B 1.3900 . ? C41B C42B 1.3900 . ? C41B C46B 1.3900 . ? C41B C60B 1.43(3) . ? C42B C43B 1.3900 . ? C43B C44B 1.3900 . ? C44B C45B 1.3900 . ? C45B C46B 1.3900 . ? C47B C48B 1.3900 . ? C47B C52B 1.3900 . ? C48B C49B 1.3900 . ? C49B C50B 1.3900 . ? C50B C51B 1.3900 . ? C51B C52B 1.3900 . ? C53B C54B 1.3900 . ? C53B C58B 1.3900 . ? C53B C59B 1.48(3) . ? C54B C55B 1.3900 . ? C55B C56B 1.3900 . ? C56B C57B 1.3900 . ? C57B C58B 1.3900 . ? C59B C60B 1.37(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 C2 Ir1 C1 106.0(16) . . ? C2 Ir1 P3 96.4(10) . . ? C1 Ir1 P3 94.5(11) . . ? C2 Ir1 P1 96.2(10) . . ? C1 Ir1 P1 102.0(11) . . ? P3 Ir1 P1 155.7(3) . . ? C2 Ir1 Ir4 158.5(11) . . ? C1 Ir1 Ir4 93.7(12) . . ? P3 Ir1 Ir4 73.1(2) . . ? P1 Ir1 Ir4 87.9(2) . . ? C2 Ir1 Ir2 102.0(11) . . ? C1 Ir1 Ir2 136.5(11) . . ? P3 Ir1 Ir2 49.4(2) . . ? P1 Ir1 Ir2 107.4(2) . . ? Ir4 Ir1 Ir2 56.81(5) . . ? C2 Ir1 Ir3 111.7(10) . . ? C1 Ir1 Ir3 132.3(11) . . ? P3 Ir1 Ir3 109.0(2) . . ? P1 Ir1 Ir3 46.8(2) . . ? Ir4 Ir1 Ir3 57.17(4) . . ? Ir2 Ir1 Ir3 61.23(4) . . ? C3 Ir2 C4 106.7(17) . . ? C3 Ir2 P3 94.9(12) . . ? C4 Ir2 P3 98.2(13) . . ? C3 Ir2 P2 97.1(12) . . ? C4 Ir2 P2 97.4(13) . . ? P3 Ir2 P2 156.7(3) . . ? C3 Ir2 Ir4 87.6(12) . . ? C4 Ir2 Ir4 164.0(13) . . ? P3 Ir2 Ir4 73.0(2) . . ? P2 Ir2 Ir4 87.6(2) . . ? C3 Ir2 Ir1 133.3(12) . . ? C4 Ir2 Ir1 107.5(13) . . ? P3 Ir2 Ir1 49.48(19) . . ? P2 Ir2 Ir1 108.94(19) . . ? Ir4 Ir2 Ir1 56.60(5) . . ? C3 Ir2 Ir3 125.9(11) . . ? C4 Ir2 Ir3 116.0(12) . . ? P3 Ir2 Ir3 109.55(19) . . ? P2 Ir2 Ir3 47.56(18) . . ? Ir4 Ir2 Ir3 57.32(4) . . ? Ir1 Ir2 Ir3 61.74(4) . . ? C6 Ir3 C5 105.9(15) . . ? C6 Ir3 P1 100.2(12) . . ? C5 Ir3 P1 96.2(10) . . ? C6 Ir3 P2 105.3(12) . . ? C5 Ir3 P2 92.5(10) . . ? P1 Ir3 P2 149.6(3) . . ? C6 Ir3 Ir4 72.6(11) . . ? C5 Ir3 Ir4 177.3(10) . . ? P1 Ir3 Ir4 86.3(2) . . ? P2 Ir3 Ir4 85.7(2) . . ? C6 Ir3 Ir2 118.5(11) . . ? C5 Ir3 Ir2 125.7(10) . . ? P1 Ir3 Ir2 104.57(19) . . ? P2 Ir3 Ir2 48.25(19) . . ? Ir4 Ir3 Ir2 54.26(4) . . ? C6 Ir3 Ir1 114.8(11) . . ? C5 Ir3 Ir1 128.6(10) . . ? P1 Ir3 Ir1 48.13(18) . . ? P2 Ir3 Ir1 104.9(2) . . ? Ir4 Ir3 Ir1 53.93(4) . . ? Ir2 Ir3 Ir1 57.03(4) . . ? C7 Ir4 C8 104.5(14) . . ? C7 Ir4 C10 87.9(12) . . ? C8 Ir4 C10 89.8(12) . . ? C7 Ir4 Ir1 92.4(10) . . ? C8 Ir4 Ir1 162.8(10) . . ? C10 Ir4 Ir1 93.9(8) . . ? C7 Ir4 Ir2 159.0(10) . . ? C8 Ir4 Ir2 96.4(10) . . ? C10 Ir4 Ir2 94.1(8) . . ? Ir1 Ir4 Ir2 66.59(5) . . ? C7 Ir4 Ir3 104.3(9) . . ? C8 Ir4 Ir3 103.3(9) . . ? C10 Ir4 Ir3 159.0(8) . . ? Ir1 Ir4 Ir3 68.89(5) . . ? Ir2 Ir4 Ir3 68.42(5) . . ? C59 P1 C47 102.6(13) . . ? C59 P1 Ir3 120.6(10) . . ? C47 P1 Ir3 114.1(9) . . ? C59 P1 Ir1 120.3(9) . . ? C47 P1 Ir1 114.5(8) . . ? Ir3 P1 Ir1 85.1(2) . . ? C29 P2 C35 104.9(11) . . ? C29 P2 Ir3 122.1(8) . . ? C35 P2 Ir3 113.1(8) . . ? C29 P2 Ir2 116.3(8) . . ? C35 P2 Ir2 116.0(8) . . ? Ir3 P2 Ir2 84.2(3) . . ? C9 P3 C11 107.9(13) . . ? C9 P3 Ir2 112.6(11) . . ? C11 P3 Ir2 120.0(8) . . ? C9 P3 Ir1 113.9(11) . . ? C11 P3 Ir1 119.5(8) . . ? Ir2 P3 Ir1 81.1(3) . . ? O1 C1 Ir1 174(3) . . ? O2 C2 Ir1 174(3) . . ? O3 C3 Ir2 174(3) . . ? O4 C4 Ir2 180(4) . . ? O5 C5 Ir3 173(3) . . ? O6 C6 Ir3 171(3) . . ? O7 C7 Ir4 177(3) . . ? O8 C8 Ir4 173(3) . . ? C10 C9 C17 118(3) . . ? C10 C9 P3 116(2) . . ? C17 C9 P3 125(2) . . ? C23 C10 C9 129(3) . . ? C23 C10 Ir4 119(2) . . ? C9 C10 Ir4 112(2) . . ? C12 C11 C16 120.0 . . ? C12 C11 P3 118.7(13) . . ? C16 C11 P3 121.2(14) . . ? C13 C12 C11 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C18 C17 C22 120.0 . . ? C18 C17 C9 120.3(18) . . ? C22 C17 C9 119.4(18) . . ? C17 C18 C19 120.0 . . ? C20 C19 C18 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C17 120.0 . . ? C24 C23 C28 120.0 . . ? C24 C23 C10 120(2) . . ? C28 C23 C10 120(2) . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C27 C28 C23 120.0 . . ? C30 C29 C34 120.0 . . ? C30 C29 P2 120.1(14) . . ? C34 C29 P2 119.7(14) . . ? C29 C30 C31 120.0 . . ? C32 C31 C30 120.0 . . ? C31 C32 C33 120.0 . . ? C32 C33 C34 120.0 . . ? C33 C34 C29 120.0 . . ? C36 C35 C40 120.0 . . ? C36 C35 P2 118.9(17) . . ? C40 C35 P2 121.1(17) . . ? C37 C36 C35 120.0 . . ? C36 C37 C38 120.0 . . ? C39 C38 C37 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C35 120.0 . . ? C42 C41 C46 120.0 . . ? C42 C41 C60 117.6(19) . . ? C46 C41 C60 122.4(19) . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C48 C47 C52 120.0 . . ? C48 C47 P1 120.3(17) . . ? C52 C47 P1 119.7(17) . . ? C49 C48 C47 120.0 . . ? C50 C49 C48 120.0 . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C47 120.0 . . ? C54 C53 C58 120.0 . . ? C54 C53 C59 118.7(18) . . ? C58 C53 C59 121.3(19) . . ? C53 C54 C55 120.0 . . ? C54 C55 C56 120.0 . . ? C57 C56 C55 120.0 . . ? C58 C57 C56 120.0 . . ? C57 C58 C53 120.0 . . ? C60 C59 C53 125(3) . . ? C60 C59 P1 115(2) . . ? C53 C59 P1 119.7(19) . . ? C59 C60 C41 130(3) . . ? C1B Ir1B C2B 104.0(17) . . ? C1B Ir1B P3B 94.1(10) . . ? C2B Ir1B P3B 99.3(12) . . ? C1B Ir1B P1B 101.5(10) . . ? C2B Ir1B P1B 95.2(12) . . ? P3B Ir1B P1B 155.4(3) . . ? C1B Ir1B Ir4B 94.9(11) . . ? C2B Ir1B Ir4B 160.0(13) . . ? P3B Ir1B Ir4B 72.7(2) . . ? P1B Ir1B Ir4B 87.0(2) . . ? C1B Ir1B Ir2B 137.6(11) . . ? C2B Ir1B Ir2B 103.6(13) . . ? P3B Ir1B Ir2B 50.0(2) . . ? P1B Ir1B Ir2B 107.3(2) . . ? Ir4B Ir1B Ir2B 57.05(5) . . ? C1B Ir1B Ir3B 133.0(11) . . ? C2B Ir1B Ir3B 111.5(13) . . ? P3B Ir1B Ir3B 109.0(2) . . ? P1B Ir1B Ir3B 46.8(2) . . ? Ir4B Ir1B Ir3B 56.79(4) . . ? Ir2B Ir1B Ir3B 60.98(4) . . ? C4B Ir2B C3B 103.8(19) . . ? C4B Ir2B P3B 94.6(17) . . ? C3B Ir2B P3B 93.5(11) . . ? C4B Ir2B P2B 100.0(16) . . ? C3B Ir2B P2B 99.2(11) . . ? P3B Ir2B P2B 157.8(3) . . ? C4B Ir2B Ir4B 161.5(17) . . ? C3B Ir2B Ir4B 90.6(11) . . ? P3B Ir2B Ir4B 72.7(2) . . ? P2B Ir2B Ir4B 88.9(2) . . ? C4B Ir2B Ir1B 104.6(17) . . ? C3B Ir2B Ir1B 134.9(10) . . ? P3B Ir2B Ir1B 50.0(2) . . ? P2B Ir2B Ir1B 109.6(2) . . ? Ir4B Ir2B Ir1B 56.98(5) . . ? C4B Ir2B Ir3B 118.1(16) . . ? C3B Ir2B Ir3B 128.6(10) . . ? P3B Ir2B Ir3B 110.5(2) . . ? P2B Ir2B Ir3B 47.7(2) . . ? Ir4B Ir2B Ir3B 57.38(4) . . ? Ir1B Ir2B Ir3B 62.54(4) . . ? C6B Ir3B C5B 105.8(14) . . ? C6B Ir3B P1B 101.4(10) . . ? C5B Ir3B P1B 94.3(11) . . ? C6B Ir3B P2B 105.8(10) . . ? C5B Ir3B P2B 93.5(10) . . ? P1B Ir3B P2B 148.4(3) . . ? C6B Ir3B Ir4B 73.5(9) . . ? C5B Ir3B Ir4B 179.0(11) . . ? P1B Ir3B Ir4B 85.2(2) . . ? P2B Ir3B Ir4B 87.4(2) . . ? C6B Ir3B Ir2B 118.8(9) . . ? C5B Ir3B Ir2B 126.6(10) . . ? P1B Ir3B Ir2B 103.54(19) . . ? P2B Ir3B Ir2B 48.73(19) . . ? Ir4B Ir3B Ir2B 54.42(4) . . ? C6B Ir3B Ir1B 116.5(10) . . ? C5B Ir3B Ir1B 126.3(11) . . ? P1B Ir3B Ir1B 47.56(19) . . ? P2B Ir3B Ir1B 104.6(2) . . ? Ir4B Ir3B Ir1B 53.83(4) . . ? Ir2B Ir3B Ir1B 56.48(4) . . ? C7B Ir4B C8B 101.1(15) . . ? C7B Ir4B C10B 90.9(13) . . ? C8B Ir4B C10B 91.3(12) . . ? C7B Ir4B Ir1B 94.2(11) . . ? C8B Ir4B Ir1B 163.7(10) . . ? C10B Ir4B Ir1B 94.1(9) . . ? C7B Ir4B Ir2B 159.9(11) . . ? C8B Ir4B Ir2B 98.4(10) . . ? C10B Ir4B Ir2B 93.4(8) . . ? Ir1B Ir4B Ir2B 65.97(5) . . ? C7B Ir4B Ir3B 103.0(10) . . ? C8B Ir4B Ir3B 101.3(9) . . ? C10B Ir4B Ir3B 158.9(9) . . ? Ir1B Ir4B Ir3B 69.38(5) . . ? Ir2B Ir4B Ir3B 68.20(5) . . ? C59B P1B C47B 102.5(12) . . ? C59B P1B Ir3B 121.5(10) . . ? C47B P1B Ir3B 112.7(7) . . ? C59B P1B Ir1B 119.7(9) . . ? C47B P1B Ir1B 115.2(7) . . ? Ir3B P1B Ir1B 85.6(3) . . ? C35B P2B C29B 103.8(12) . . ? C35B P2B Ir3B 114.8(9) . . ? C29B P2B Ir3B 121.6(8) . . ? C35B P2B Ir2B 117.3(9) . . ? C29B P2B Ir2B 115.9(8) . . ? Ir3B P2B Ir2B 83.6(3) . . ? C11B P3B C9B 106.9(12) . . ? C11B P3B Ir1B 120.1(9) . . ? C9B P3B Ir1B 114.7(10) . . ? C11B P3B Ir2B 122.4(8) . . ? C9B P3B Ir2B 111.0(10) . . ? Ir1B P3B Ir2B 80.0(2) . . ? O1B C1B Ir1B 173(3) . . ? O2B C2B Ir1B 173(4) . . ? O3B C3B Ir2B 179(3) . . ? O4B C4B Ir2B 171(4) . . ? O5B C5B Ir3B 173(3) . . ? O6B C6B Ir3B 176(3) . . ? O7B C7B Ir4B 174(3) . . ? O8B C8B Ir4B 177(3) . . ? C10B C9B C17B 123(3) . . ? C10B C9B P3B 115(2) . . ? C17B C9B P3B 122(2) . . ? C9B C10B C23B 127(3) . . ? C9B C10B Ir4B 115(2) . . ? C23B C10B Ir4B 117.8(19) . . ? C12B C11B C16B 120.0 . . ? C12B C11B P3B 117.2(16) . . ? C16B C11B P3B 122.7(16) . . ? C13B C12B C11B 120.0 . . ? C12B C13B C14B 120.0 . . ? C15B C14B C13B 120.0 . . ? C16B C15B C14B 120.0 . . ? C15B C16B C11B 120.0 . . ? C18B C17B C22B 120.0 . . ? C18B C17B C9B 121.2(18) . . ? C22B C17B C9B 118.5(18) . . ? C17B C18B C19B 120.0 . . ? C20B C19B C18B 120.0 . . ? C19B C20B C21B 120.0 . . ? C22B C21B C20B 120.0 . . ? C21B C22B C17B 120.0 . . ? C24B C23B C28B 120.0 . . ? C24B C23B C10B 119.4(19) . . ? C28B C23B C10B 120.5(19) . . ? C25B C24B C23B 120.0 . . ? C24B C25B C26B 120.0 . . ? C27B C26B C25B 120.0 . . ? C26B C27B C28B 120.0 . . ? C27B C28B C23B 120.0 . . ? C30B C29B C34B 120.0 . . ? C30B C29B P2B 120.8(14) . . ? C34B C29B P2B 119.0(14) . . ? C29B C30B C31B 120.0 . . ? C32B C31B C30B 120.0 . . ? C33B C32B C31B 120.0 . . ? C34B C33B C32B 120.0 . . ? C33B C34B C29B 120.0 . . ? C36B C35B C40B 120.0 . . ? C36B C35B P2B 120.5(17) . . ? C40B C35B P2B 119.5(17) . . ? C35B C36B C37B 120.0 . . ? C36B C37B C38B 120.0 . . ? C39B C38B C37B 120.0 . . ? C38B C39B C40B 120.0 . . ? C39B C40B C35B 120.0 . . ? C42B C41B C46B 120.0 . . ? C42B C41B C60B 113.6(19) . . ? C46B C41B C60B 126.4(19) . . ? C41B C42B C43B 120.0 . . ? C42B C43B C44B 120.0 . . ? C45B C44B C43B 120.0 . . ? C44B C45B C46B 120.0 . . ? C45B C46B C41B 120.0 . . ? C48B C47B C52B 120.0 . . ? C48B C47B P1B 119.1(13) . . ? C52B C47B P1B 120.9(13) . . ? C49B C48B C47B 120.0 . . ? C48B C49B C50B 120.0 . . ? C51B C50B C49B 120.0 . . ? C52B C51B C50B 120.0 . . ? C51B C52B C47B 120.0 . . ? C54B C53B C58B 120.0 . . ? C54B C53B C59B 122.4(19) . . ? C58B C53B C59B 117.5(19) . . ? C53B C54B C55B 120.0 . . ? C54B C55B C56B 120.0 . . ? C57B C56B C55B 120.0 . . ? C56B C57B C58B 120.0 . . ? C57B C58B C53B 120.0 . . ? C60B C59B C53B 128(3) . . ? C60B C59B P1B 115(2) . . ? C53B C59B P1B 116.6(19) . . ? C59B C60B C41B 130(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.518 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.246 #===END data_jul1799 _audit_creation_date 1999-08-13T10:01:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common IR10PP1 _chemical_formula_moiety 'C41 H26 Ir4 O9 P2' _chemical_formula_structural 'C41 H26 Ir4 O9 P2' _chemical_formula_sum 'C41 H26 Ir4 O9 P2' _chemical_formula_weight 1493.36 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 12.2575(3) _cell_length_b 18.6562(4) _cell_length_c 19.2753(6) _cell_angle_alpha 90 _cell_angle_beta 107.346(2) _cell_angle_gamma 90 _cell_volume 4207.38(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22183 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION USING SORTAV #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 12.74 _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.65 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 22183 _diffrn_reflns_av_R_equivalents 0.079 _diffrn_reflns_av_sigmaI/netI 0.049 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 7386 _reflns_number_gt 5889 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0263P)^2^+6.6695P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7386 _refine_ls_number_parameters 475 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.051 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.979 _refine_diff_density_min -1.148 _refine_diff_density_rms 0.162 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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 0.13489(2) 0.791080(13) 0.092941(14) 0.03638(6) Uani 1 1 d . A . Ir2 Ir -0.02505(2) 0.685512(13) 0.048375(15) 0.03822(7) Uani 1 1 d . A . Ir3 Ir -0.01457(2) 0.856713(14) -0.035319(16) 0.04619(7) Uani 1 1 d . A . Ir4 Ir 0.09844(2) 0.727925(13) -0.043230(14) 0.03775(7) Uani 1 1 d . A . P1 P 0.16809(14) 0.66910(9) 0.09307(9) 0.0370(4) Uani 1 1 d . . . P2 P -0.14851(14) 0.77540(10) -0.01479(10) 0.0436(4) Uani 1 1 d . . . O1 O 0.3535(5) 0.8759(3) 0.1115(4) 0.087(2) Uani 1 1 d . A . O2 O 0.1196(5) 0.7897(3) 0.2471(3) 0.0821(18) Uani 1 1 d . A . O3 O -0.0983(5) 0.6664(3) 0.1853(3) 0.0846(19) Uani 1 1 d . A . O4 O -0.1354(5) 0.5550(3) -0.0363(4) 0.085(2) Uani 1 1 d . A . O5 O 0.1722(6) 0.9431(3) -0.0730(5) 0.109(2) Uani 1 1 d . A . O6 O -0.2064(5) 0.9587(3) -0.1001(4) 0.089(2) Uani 1 1 d . A . O7 O 0.0128(5) 0.9358(3) 0.1036(3) 0.0715(17) Uani 1 1 d . A . O8 O 0.2721(5) 0.7963(3) -0.1058(4) 0.0858(18) Uani 1 1 d . A . O9 O -0.0723(5) 0.6907(4) -0.1870(3) 0.088(2) Uani 1 1 d . A . C1 C 0.2727(6) 0.8436(4) 0.1044(4) 0.0514(19) Uani 1 1 d . . . C2 C 0.1262(6) 0.7927(4) 0.1893(4) 0.0501(19) Uani 1 1 d . . . C3 C -0.0711(6) 0.6746(4) 0.1341(5) 0.058(2) Uani 1 1 d . . . C4 C -0.0947(6) 0.6055(4) -0.0041(4) 0.054(2) Uani 1 1 d . . . C5 C 0.1045(7) 0.9104(4) -0.0593(5) 0.066(2) Uani 1 1 d . . . C6 C -0.1303(7) 0.9201(4) -0.0763(5) 0.062(2) Uani 1 1 d . . . C7 C 0.0320(6) 0.8887(4) 0.0687(4) 0.0501(19) Uani 1 1 d . . . C8 C 0.2053(6) 0.7713(4) -0.0826(4) 0.0518(19) Uani 1 1 d . . . C9 C -0.0134(6) 0.7076(4) -0.1320(4) 0.057(2) Uani 1 1 d . . . C10 C 0.2272(5) 0.6433(3) 0.0219(4) 0.0388(16) Uani 1 1 d . A . C11 C 0.1568(6) 0.6092(3) -0.0404(3) 0.0394(16) Uani 1 1 d . . . H11 H 0.0812 0.6025 -0.0412 0.047 Uiso 1 1 calc R A . C18 C 0.3551(5) 0.6413(3) 0.0407(3) 0.0408(16) Uani 1 1 d . . . C19 C 0.4266(6) 0.7010(4) 0.0525(4) 0.0509(19) Uani 1 1 d . A . H19 H 0.3952 0.7467 0.0453 0.061 Uiso 1 1 calc R . . C20 C 0.5446(7) 0.6925(5) 0.0748(5) 0.068(2) Uani 1 1 d . . . H20 H 0.5917 0.7327 0.0825 0.082 Uiso 1 1 calc R A . C21 C 0.5915(7) 0.6261(5) 0.0855(5) 0.075(3) Uani 1 1 d . A . H21 H 0.6705 0.6209 0.0997 0.09 Uiso 1 1 calc R . . C22 C 0.5235(8) 0.5672(5) 0.0757(5) 0.080(3) Uani 1 1 d . . . H22 H 0.5563 0.5218 0.0844 0.096 Uiso 1 1 calc R A . C23 C 0.4057(7) 0.5741(4) 0.0526(5) 0.062(2) Uani 1 1 d . A . H23 H 0.3601 0.5333 0.045 0.075 Uiso 1 1 calc R . . C24 C 0.1859(6) 0.5827(4) -0.1040(4) 0.0476(18) Uani 1 1 d . A . C25 C 0.2799(6) 0.6048(4) -0.1260(4) 0.060(2) Uani 1 1 d . . . H25 H 0.3312 0.6378 -0.098 0.072 Uiso 1 1 calc R A . C26 C 0.2972(8) 0.5781(5) -0.1890(5) 0.075(3) Uani 1 1 d . A . H26 H 0.3594 0.5941 -0.2029 0.09 Uiso 1 1 calc R . . C27 C 0.2252(9) 0.5290(5) -0.2308(5) 0.084(3) Uani 1 1 d . . . H27 H 0.2391 0.5107 -0.2723 0.101 Uiso 1 1 calc R A . C28 C 0.1326(11) 0.5067(5) -0.2115(5) 0.099(4) Uani 1 1 d . A . H28 H 0.083 0.4731 -0.2401 0.118 Uiso 1 1 calc R . . C29 C 0.1117(8) 0.5337(4) -0.1494(5) 0.075(3) Uani 1 1 d . . . H29 H 0.0468 0.5188 -0.1378 0.09 Uiso 1 1 calc R A . C30 C -0.2405(5) 0.8200(4) 0.0312(4) 0.0467(18) Uani 1 1 d . A . C31 C -0.2039(6) 0.8298(4) 0.1077(4) 0.055(2) Uani 1 1 d . . . H31 H -0.1336 0.8115 0.1349 0.067 Uiso 1 1 calc R A . C32 C -0.2700(7) 0.8655(5) 0.1418(6) 0.080(3) Uani 1 1 d . A . H32 H -0.244 0.8715 0.1919 0.096 Uiso 1 1 calc R . . C33 C -0.3731(7) 0.8925(5) 0.1038(5) 0.074(3) Uani 1 1 d . . . H33 H -0.4172 0.9165 0.1281 0.089 Uiso 1 1 calc R A . C34 C -0.4126(7) 0.8848(5) 0.0306(6) 0.076(3) Uani 1 1 d . A . H34 H -0.4834 0.9036 0.0048 0.092 Uiso 1 1 calc R . . C35 C -0.3462(6) 0.8482(4) -0.0060(5) 0.063(2) Uani 1 1 d . . . H35 H -0.3736 0.8429 -0.0562 0.075 Uiso 1 1 calc R A . C36 C -0.2577(6) 0.7441(4) -0.0963(4) 0.053(2) Uani 1 1 d . A . C37 C -0.2730(7) 0.7721(5) -0.1643(5) 0.075(3) Uani 1 1 d . . . H37 H -0.2278 0.8096 -0.1717 0.089 Uiso 1 1 calc R A . C38 C -0.3584(9) 0.7426(7) -0.2221(5) 0.101(4) Uani 1 1 d . A . H38 H -0.3697 0.7615 -0.2684 0.121 Uiso 1 1 calc R . . C39 C -0.4235(9) 0.6894(7) -0.2144(6) 0.107(4) Uani 1 1 d . . . H39 H -0.4796 0.6715 -0.2545 0.128 Uiso 1 1 calc R A . C40 C -0.4088(9) 0.6600(7) -0.1470(6) 0.105(4) Uani 1 1 d . A . H40 H -0.454 0.6219 -0.141 0.126 Uiso 1 1 calc R . . C41 C -0.3270(7) 0.6874(5) -0.0891(5) 0.074(3) Uani 1 1 d . . . H41 H -0.3172 0.6677 -0.0433 0.089 Uiso 1 1 calc R A . C12 C 0.2582(8) 0.6292(5) 0.1777(5) 0.053(5) Uiso 0.5 1 d PG A 1 C13 C 0.3407(9) 0.6682(5) 0.2289(6) 0.053(4) Uiso 0.5 1 d PG A 1 H13 H 0.3442 0.7178 0.2247 0.063 Uiso 0.5 1 calc PR A 1 C14 C 0.4181(9) 0.6332(8) 0.2865(6) 0.114(10) Uiso 0.5 1 d PG A 1 H14 H 0.4734 0.6593 0.3208 0.137 Uiso 0.5 1 calc PR A 1 C15 C 0.4130(11) 0.5591(8) 0.2929(7) 0.095(6) Uiso 0.5 1 d PG A 1 H15 H 0.4647 0.5357 0.3315 0.114 Uiso 0.5 1 calc PR A 1 C16 C 0.3304(12) 0.5201(5) 0.2417(8) 0.107(7) Uiso 0.5 1 d PG A 1 H16 H 0.3269 0.4706 0.246 0.128 Uiso 0.5 1 calc PR A 1 C17 C 0.2530(10) 0.5552(5) 0.1841(6) 0.080(5) Uiso 0.5 1 d PG A 1 H17 H 0.1977 0.5291 0.1499 0.096 Uiso 0.5 1 calc PR A 1 C12B C 0.2455(8) 0.6255(5) 0.1759(5) 0.049(5) Uiso 0.5 1 d PG A 2 C13B C 0.3526(8) 0.6510(5) 0.2154(5) 0.052(4) Uiso 0.5 1 d PG A 2 H13B H 0.3868 0.6876 0.1966 0.062 Uiso 0.5 1 calc PR A 2 C14B C 0.4086(8) 0.6216(6) 0.2829(5) 0.073(6) Uiso 0.5 1 d PG A 2 H14B H 0.4802 0.6387 0.3093 0.087 Uiso 0.5 1 calc PR A 2 C15B C 0.3574(10) 0.5668(6) 0.3110(5) 0.072(5) Uiso 0.5 1 d PG A 2 H15B H 0.3949 0.5472 0.3561 0.087 Uiso 0.5 1 calc PR A 2 C16B C 0.2504(10) 0.5414(5) 0.2715(6) 0.083(5) Uiso 0.5 1 d PG A 2 H16B H 0.2162 0.5047 0.2902 0.099 Uiso 0.5 1 calc PR A 2 C17B C 0.1944(8) 0.5707(5) 0.2039(6) 0.056(4) Uiso 0.5 1 d PG A 2 H17B H 0.1227 0.5537 0.1775 0.067 Uiso 0.5 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03500(12) 0.03591(12) 0.03660(14) 0.00048(10) 0.00816(10) -0.00158(10) Ir2 0.03598(12) 0.04105(13) 0.03598(14) 0.00211(11) 0.00821(11) -0.00555(11) Ir3 0.04504(14) 0.04465(15) 0.05084(17) 0.01414(12) 0.01730(12) 0.00789(12) Ir4 0.03852(13) 0.04128(13) 0.03273(14) 0.00304(11) 0.00951(11) 0.00062(11) P1 0.0395(8) 0.0385(8) 0.0303(9) 0.0016(7) 0.0062(7) -0.0011(7) P2 0.0378(8) 0.0550(10) 0.0371(10) 0.0019(8) 0.0097(7) 0.0012(8) O1 0.056(3) 0.076(4) 0.133(6) -0.012(4) 0.034(3) -0.019(3) O2 0.101(4) 0.103(4) 0.052(4) -0.014(3) 0.038(3) -0.025(4) O3 0.112(4) 0.094(4) 0.062(4) 0.010(3) 0.049(3) -0.019(4) O4 0.097(4) 0.066(3) 0.087(5) -0.020(3) 0.020(4) -0.029(3) O5 0.110(4) 0.070(4) 0.180(7) 0.030(4) 0.092(4) 0.002(4) O6 0.078(4) 0.090(4) 0.101(5) 0.044(4) 0.028(4) 0.031(3) O7 0.078(3) 0.055(3) 0.080(4) -0.007(3) 0.020(3) 0.014(3) O8 0.086(3) 0.089(4) 0.107(4) 0.019(3) 0.065(3) -0.006(3) O9 0.060(3) 0.149(6) 0.045(4) -0.028(4) 0.001(3) 0.004(4) C1 0.048(4) 0.045(4) 0.061(5) -0.003(3) 0.017(4) -0.003(3) C2 0.046(4) 0.046(4) 0.058(5) -0.008(3) 0.016(3) -0.011(3) C3 0.059(4) 0.058(4) 0.063(5) 0.004(4) 0.024(4) -0.016(4) C4 0.047(4) 0.051(4) 0.060(5) -0.004(4) 0.008(4) -0.018(3) C5 0.061(4) 0.048(4) 0.097(6) 0.017(4) 0.036(4) 0.009(4) C6 0.066(4) 0.058(4) 0.067(5) 0.029(4) 0.028(4) 0.018(4) C7 0.043(4) 0.039(4) 0.065(5) 0.010(3) 0.011(3) -0.003(3) C8 0.065(4) 0.047(4) 0.047(4) 0.001(3) 0.022(4) -0.002(4) C9 0.050(4) 0.077(5) 0.039(4) 0.004(4) 0.009(4) 0.010(4) C10 0.043(3) 0.034(3) 0.036(4) 0.000(3) 0.006(3) 0.004(3) C11 0.042(3) 0.038(3) 0.034(4) -0.001(3) 0.004(3) 0.003(3) C18 0.044(3) 0.050(4) 0.027(3) -0.005(3) 0.008(3) 0.009(3) C19 0.043(4) 0.053(4) 0.052(5) -0.016(3) 0.007(3) 0.006(3) C20 0.057(5) 0.080(6) 0.067(6) -0.015(4) 0.017(4) -0.002(4) C21 0.035(4) 0.112(7) 0.069(6) 0.001(5) 0.005(4) 0.007(5) C22 0.068(5) 0.079(6) 0.084(7) 0.008(5) 0.007(5) 0.030(5) C23 0.059(4) 0.049(4) 0.072(6) -0.006(4) 0.009(4) 0.008(4) C24 0.052(4) 0.044(4) 0.043(4) -0.003(3) 0.008(3) 0.005(3) C25 0.044(4) 0.077(5) 0.050(5) -0.006(4) 0.000(4) 0.018(4) C26 0.079(5) 0.094(6) 0.059(5) -0.008(5) 0.031(4) 0.031(5) C27 0.111(7) 0.089(6) 0.045(5) -0.021(5) 0.012(5) 0.013(6) C28 0.155(10) 0.072(6) 0.056(6) -0.016(5) 0.013(7) -0.006(7) C29 0.093(6) 0.066(5) 0.056(6) -0.007(4) 0.008(5) -0.017(5) C30 0.037(3) 0.060(4) 0.047(4) 0.001(3) 0.019(3) 0.003(3) C31 0.045(4) 0.060(4) 0.061(5) -0.001(4) 0.014(4) 0.000(4) C32 0.065(5) 0.089(6) 0.085(7) -0.032(5) 0.023(5) 0.008(5) C33 0.069(5) 0.084(6) 0.076(6) -0.022(5) 0.031(5) 0.016(5) C34 0.061(5) 0.078(6) 0.093(7) 0.006(5) 0.027(5) 0.023(5) C35 0.055(4) 0.072(5) 0.057(5) -0.002(4) 0.010(4) 0.015(4) C36 0.039(4) 0.077(5) 0.040(4) -0.003(4) 0.006(3) 0.000(4) C37 0.063(5) 0.107(7) 0.048(5) -0.001(5) 0.008(4) 0.024(5) C38 0.082(6) 0.165(10) 0.044(6) 0.001(6) 0.002(5) 0.036(7) C39 0.065(6) 0.171(11) 0.064(7) -0.031(7) -0.013(6) 0.001(7) C40 0.068(6) 0.140(9) 0.085(8) -0.022(7) -0.008(6) -0.039(6) C41 0.047(4) 0.108(7) 0.056(6) -0.012(5) -0.001(4) -0.020(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 1.892(8) . ? Ir1 C1 1.908(7) . ? Ir1 C7 2.186(7) . ? Ir1 P1 2.3117(17) . ? Ir1 Ir2 2.7305(3) . ? Ir1 Ir4 2.7889(4) . ? Ir1 Ir3 2.8752(4) . ? Ir2 C4 1.862(7) . ? Ir2 C3 1.909(9) . ? Ir2 P1 2.2856(17) . ? Ir2 P2 2.3423(18) . ? Ir2 Ir4 2.7620(4) . ? Ir3 C6 1.834(7) . ? Ir3 C5 1.937(8) . ? Ir3 C7 2.005(8) . ? Ir3 P2 2.3539(18) . ? Ir3 Ir4 2.8002(4) . ? Ir4 C8 1.882(8) . ? Ir4 C9 1.885(8) . ? Ir4 C10 2.319(6) . ? Ir4 C11 2.324(6) . ? Ir4 P1 2.7382(17) . ? P1 C12B 1.791(8) . ? P1 C10 1.798(7) . ? P1 C12 1.833(9) . ? P2 C30 1.829(7) . ? P2 C36 1.829(7) . ? O1 C1 1.131(8) . ? O2 C2 1.142(9) . ? O3 C3 1.143(10) . ? O4 C4 1.156(8) . ? O5 C5 1.122(9) . ? O6 C6 1.159(9) . ? O7 C7 1.172(9) . ? O8 C8 1.142(9) . ? O9 C9 1.134(9) . ? C10 C11 1.405(9) . ? C10 C18 1.500(9) . ? C11 C24 1.462(10) . ? C18 C23 1.386(10) . ? C18 C19 1.394(9) . ? C19 C20 1.389(10) . ? C20 C21 1.355(12) . ? C21 C22 1.358(13) . ? C22 C23 1.385(11) . ? C24 C29 1.398(10) . ? C24 C25 1.403(11) . ? C25 C26 1.386(11) . ? C26 C27 1.357(12) . ? C27 C28 1.360(15) . ? C28 C29 1.392(13) . ? C30 C35 1.384(10) . ? C30 C31 1.418(10) . ? C31 C32 1.360(11) . ? C32 C33 1.355(12) . ? C33 C34 1.356(13) . ? C34 C35 1.403(12) . ? C36 C37 1.371(11) . ? C36 C41 1.389(11) . ? C37 C38 1.395(13) . ? C38 C39 1.309(16) . ? C39 C40 1.372(16) . ? C40 C41 1.358(12) . ? C12 C13 1.39 . ? C12 C17 1.39 . ? C13 C14 1.39 . ? C14 C15 1.39 . ? C15 C16 1.39 . ? C16 C17 1.39 . ? C12B C13B 1.39 . ? C12B C17B 1.39 . ? C13B C14B 1.39 . ? C14B C15B 1.39 . ? C15B C16B 1.39 . ? C16B C17B 1.39 . ? 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 C2 Ir1 C1 100.7(3) . . ? C2 Ir1 C7 90.0(3) . . ? C1 Ir1 C7 91.8(3) . . ? C2 Ir1 P1 94.3(2) . . ? C1 Ir1 P1 110.9(2) . . ? C7 Ir1 P1 155.64(18) . . ? C2 Ir1 Ir2 94.3(2) . . ? C1 Ir1 Ir2 159.2(2) . . ? C7 Ir1 Ir2 102.68(18) . . ? P1 Ir1 Ir2 53.12(4) . . ? C2 Ir1 Ir4 152.9(2) . . ? C1 Ir1 Ir4 102.4(2) . . ? C7 Ir1 Ir4 103.3(2) . . ? P1 Ir1 Ir4 64.14(4) . . ? Ir2 Ir1 Ir4 60.043(9) . . ? C2 Ir1 Ir3 129.0(2) . . ? C1 Ir1 Ir3 101.3(2) . . ? C7 Ir1 Ir3 44.1(2) . . ? P1 Ir1 Ir3 119.14(4) . . ? Ir2 Ir1 Ir3 79.807(10) . . ? Ir4 Ir1 Ir3 59.233(9) . . ? C4 Ir2 C3 100.3(3) . . ? C4 Ir2 P1 110.7(2) . . ? C3 Ir2 P1 101.5(2) . . ? C4 Ir2 P2 99.9(2) . . ? C3 Ir2 P2 102.4(2) . . ? P1 Ir2 P2 136.71(6) . . ? C4 Ir2 Ir1 156.8(2) . . ? C3 Ir2 Ir1 100.1(2) . . ? P1 Ir2 Ir1 54.00(4) . . ? P2 Ir2 Ir1 86.51(4) . . ? C4 Ir2 Ir4 97.6(2) . . ? C3 Ir2 Ir4 160.7(2) . . ? P1 Ir2 Ir4 64.91(4) . . ? P2 Ir2 Ir4 81.66(5) . . ? Ir1 Ir2 Ir4 61.026(10) . . ? C6 Ir3 C5 96.0(3) . . ? C6 Ir3 C7 101.0(3) . . ? C5 Ir3 C7 94.3(3) . . ? C6 Ir3 P2 90.0(2) . . ? C5 Ir3 P2 170.6(2) . . ? C7 Ir3 P2 91.7(2) . . ? C6 Ir3 Ir4 149.4(3) . . ? C5 Ir3 Ir4 90.6(2) . . ? C7 Ir3 Ir4 108.2(2) . . ? P2 Ir3 Ir4 80.64(5) . . ? C6 Ir3 Ir1 149.0(3) . . ? C5 Ir3 Ir1 95.4(2) . . ? C7 Ir3 Ir1 49.4(2) . . ? P2 Ir3 Ir1 83.02(4) . . ? Ir4 Ir3 Ir1 58.848(9) . . ? C8 Ir4 C9 97.2(3) . . ? C8 Ir4 C10 93.9(3) . . ? C9 Ir4 C10 123.2(3) . . ? C8 Ir4 C11 100.0(3) . . ? C9 Ir4 C11 88.0(3) . . ? C10 Ir4 C11 35.2(2) . . ? C8 Ir4 P1 120.3(2) . . ? C9 Ir4 P1 136.4(3) . . ? C10 Ir4 P1 40.59(17) . . ? C11 Ir4 P1 65.76(16) . . ? C8 Ir4 Ir2 164.0(2) . . ? C9 Ir4 Ir2 97.7(2) . . ? C10 Ir4 Ir2 82.71(17) . . ? C11 Ir4 Ir2 86.29(17) . . ? P1 Ir4 Ir2 49.11(4) . . ? C8 Ir4 Ir1 105.2(2) . . ? C9 Ir4 Ir1 144.0(2) . . ? C10 Ir4 Ir1 83.45(16) . . ? C11 Ir4 Ir1 114.75(16) . . ? P1 Ir4 Ir1 49.44(4) . . ? Ir2 Ir4 Ir1 58.930(9) . . ? C8 Ir4 Ir3 93.9(2) . . ? C9 Ir4 Ir3 89.1(2) . . ? C10 Ir4 Ir3 145.34(16) . . ? C11 Ir4 Ir3 166.07(17) . . ? P1 Ir4 Ir3 108.03(4) . . ? Ir2 Ir4 Ir3 80.603(11) . . ? Ir1 Ir4 Ir3 61.919(10) . . ? C12B P1 C10 109.4(4) . . ? C12B P1 C12 5.0(5) . . ? C10 P1 C12 107.3(4) . . ? C12B P1 Ir2 127.6(3) . . ? C10 P1 Ir2 110.9(2) . . ? C12 P1 Ir2 132.2(3) . . ? C12B P1 Ir1 119.6(3) . . ? C10 P1 Ir1 111.9(2) . . ? C12 P1 Ir1 117.4(3) . . ? Ir2 P1 Ir1 72.87(5) . . ? C12B P1 Ir4 165.5(3) . . ? C10 P1 Ir4 57.1(2) . . ? C12 P1 Ir4 161.7(3) . . ? Ir2 P1 Ir4 65.99(4) . . ? Ir1 P1 Ir4 66.42(4) . . ? C30 P2 C36 99.4(3) . . ? C30 P2 Ir2 118.0(2) . . ? C36 P2 Ir2 114.3(3) . . ? C30 P2 Ir3 110.5(2) . . ? C36 P2 Ir3 115.4(3) . . ? Ir2 P2 Ir3 100.01(6) . . ? O1 C1 Ir1 178.7(7) . . ? O2 C2 Ir1 176.3(6) . . ? O3 C3 Ir2 178.5(7) . . ? O4 C4 Ir2 178.3(7) . . ? O5 C5 Ir3 178.3(7) . . ? O6 C6 Ir3 176.6(7) . . ? O7 C7 Ir3 138.8(6) . . ? O7 C7 Ir1 134.6(6) . . ? Ir3 C7 Ir1 86.5(3) . . ? O8 C8 Ir4 178.3(7) . . ? O9 C9 Ir4 172.7(7) . . ? C11 C10 C18 121.7(6) . . ? C11 C10 P1 119.3(5) . . ? C18 C10 P1 116.9(5) . . ? C11 C10 Ir4 72.6(3) . . ? C18 C10 Ir4 129.9(4) . . ? P1 C10 Ir4 82.3(2) . . ? C10 C11 C24 129.0(6) . . ? C10 C11 Ir4 72.2(3) . . ? C24 C11 Ir4 116.9(4) . . ? C23 C18 C19 117.8(6) . . ? C23 C18 C10 116.6(6) . . ? C19 C18 C10 125.5(6) . . ? C20 C19 C18 120.4(7) . . ? C21 C20 C19 120.4(8) . . ? C20 C21 C22 120.3(8) . . ? C21 C22 C23 120.4(8) . . ? C22 C23 C18 120.7(8) . . ? C29 C24 C25 116.3(8) . . ? C29 C24 C11 118.1(7) . . ? C25 C24 C11 125.6(6) . . ? C26 C25 C24 120.8(8) . . ? C27 C26 C25 121.4(9) . . ? C26 C27 C28 119.4(9) . . ? C27 C28 C29 120.5(10) . . ? C28 C29 C24 121.5(9) . . ? C35 C30 C31 116.5(7) . . ? C35 C30 P2 122.6(6) . . ? C31 C30 P2 120.9(5) . . ? C32 C31 C30 121.1(7) . . ? C33 C32 C31 121.0(9) . . ? C32 C33 C34 120.6(8) . . ? C33 C34 C35 119.6(8) . . ? C30 C35 C34 121.2(8) . . ? C37 C36 C41 118.1(8) . . ? C37 C36 P2 123.8(6) . . ? C41 C36 P2 118.0(6) . . ? C36 C37 C38 118.1(10) . . ? C39 C38 C37 123.1(11) . . ? C38 C39 C40 119.9(10) . . ? C41 C40 C39 118.9(11) . . ? C40 C41 C36 121.9(10) . . ? C13 C12 C17 120 . . ? C13 C12 P1 122.5(6) . . ? C17 C12 P1 116.8(6) . . ? C14 C13 C12 120 . . ? C13 C14 C15 120 . . ? C16 C15 C14 120 . . ? C15 C16 C17 120 . . ? C16 C17 C12 120 . . ? C13B C12B C17B 120 . . ? C13B C12B P1 119.7(5) . . ? C17B C12B P1 120.0(5) . . ? C12B C13B C14B 120 . . ? C15B C14B C13B 120 . . ? C14B C15B C16B 120 . . ? C17B C16B C15B 120 . . ? C16B C17B C12B 120 . . ? #===END