# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _publ_requested_journal Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'John F. Hartwig' _publ_contact_author_email jhartwig@uiuc.edu _publ_section_title ;Pronounced Effects of Substituents on the Iridium-Catalyzed Borylation of Aryl C-H Bonds ; loop_ _publ_author_name 'John F. Hartwig' 'Carl W. Liskey' 'Carolyn S. Wei' 'Dale R. Pahls' # Attachment 'Irborylationcombined.cif' data_dtbpyIr(Bcat*)3(COE), _database_code_depnum_ccdc_archive 'CCDC 740059' #1b _audit_creation_method SHELXL-97 _audit_update_record ; 2007-08-27 text and data added, srw ; _chemical_formula_moiety 'C56 H74 B3 Ir N2 O6, C5 H12' _chemical_formula_sum 'C61 H86 B3 Ir N2 O6' _chemical_formula_weight 1167.95 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.849(4) _cell_length_b 14.181(4) _cell_length_c 15.889(4) _cell_angle_alpha 79.705(4) _cell_angle_beta 79.622(4) _cell_angle_gamma 74.051(4) _cell_volume 2923.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 919 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 20.03 _exptl_crystal_description tabular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1212 _exptl_crystal_id g08vas _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (1 1 1) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 2.333 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5881 _exptl_absorpt_correction_T_max 0.8819 _exptl_absorpt_process_details 'SHELXTL/XPREP (Bruker, 2001)' _exptl_special_details ; One distinct cell was identified using SMART (Bruker, 2001). Six frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2001) then corrected for absorption by integration using SHELXTL/XPREP (Bruker, 2001) before using SAINT/SADABS (Bruker, 2001) to sort, merge, and scale the combined data. A series of identical frames was collected twice during the experiment to monitor decay. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id g08vas _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_device 'Siemens Platform/CCD' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 57 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 493 _diffrn_standards_decay_% 14.0 _diffrn_reflns_number 30653 _diffrn_reflns_av_R_equivalents 0.0684 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.40 _reflns_number_total 10724 _reflns_number_gt 7935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2001)' _computing_data_reduction 'SAINT V7.23A(Bruker, 2001)' _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL V6.12 (Bruker, 2001)' _computing_publication_material 'XCIF (Bruker, 2001)' _refine_special_details ; Structure was phased by direct methods in P1 and transformed into P-1. Systematic conditions suggested the ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The highest peaks in the final difference Fourier map were in the vicinity of atom Ir1; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed depence on amplitude and resolution. For the data crystal, mean I/\s(I) was less than 1 for reflections beyond 1\%A resolution. Reflections between 1 and 0.8\%A resolution were used for least-squares refinement to improve the data-to-variable ratio at the expense of agreement factors. ; _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^)+(0.0417P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10724 _refine_ls_number_parameters 840 _refine_ls_number_restraints 932 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.0863 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.015 _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 B1 B 0.1304(4) 0.8989(4) 0.1895(3) 0.0245(14) Uani 1 1 d . B . B3 B 0.1555(4) 0.7413(4) 0.1089(4) 0.0289(15) Uani 1 1 d . B . B2 B 0.2324(4) 0.7258(4) 0.2624(4) 0.0246(14) Uani 1 1 d . B . C1 C 0.0277(4) 0.6272(3) 0.2390(3) 0.0308(13) Uani 1 1 d . A . H1A H 0.0329 0.6061 0.1812 0.037 Uiso 1 1 calc R . . C2 C 0.1202(4) 0.5959(3) 0.2715(3) 0.0313(13) Uani 1 1 d . A . H2A H 0.1757 0.5566 0.2326 0.038 Uiso 1 1 calc R . . C3 C 0.1283(5) 0.5620(4) 0.3658(3) 0.0422(15) Uani 1 1 d . A . H3A H 0.0701 0.6024 0.4004 0.051 Uiso 1 1 calc R . . H3B H 0.1910 0.5737 0.3788 0.051 Uiso 1 1 calc R . . C4 C 0.1302(4) 0.4514(4) 0.3931(4) 0.0466(14) Uani 1 1 d DU . . H4C H 0.2006 0.4126 0.3780 0.056 Uiso 0.175(8) 1 calc PR A 2 H4D H 0.1144 0.4407 0.4569 0.056 Uiso 0.175(8) 1 calc PR A 2 H4A H 0.1781 0.4128 0.3501 0.056 Uiso 0.825(8) 1 calc PR A 1 H4B H 0.1564 0.4293 0.4492 0.056 Uiso 0.825(8) 1 calc PR A 1 C5 C 0.0278(5) 0.4278(5) 0.4018(4) 0.0469(18) Uani 0.825(8) 1 d PDU A 1 H5A H -0.0224 0.4741 0.4377 0.056 Uiso 0.825(8) 1 calc PR A 1 H5B H 0.0332 0.3602 0.4333 0.056 Uiso 0.825(8) 1 calc PR A 1 C6 C -0.0132(5) 0.4336(4) 0.3178(4) 0.0419(17) Uani 0.825(8) 1 d PDU A 1 H6A H 0.0436 0.4314 0.2698 0.050 Uiso 0.825(8) 1 calc PR A 1 H6B H -0.0386 0.3742 0.3206 0.050 Uiso 0.825(8) 1 calc PR A 1 C7 C -0.0977(4) 0.5250(4) 0.2966(4) 0.0466(14) Uani 1 1 d DU . . H7A H -0.1576 0.5228 0.3408 0.056 Uiso 0.825(8) 1 calc PR A 1 H7B H -0.1169 0.5220 0.2403 0.056 Uiso 0.825(8) 1 calc PR A 1 H7C H -0.1721 0.5344 0.3049 0.056 Uiso 0.175(8) 1 calc PR A 2 H7D H -0.0688 0.4965 0.2423 0.056 Uiso 0.175(8) 1 calc PR A 2 C8 C -0.0715(4) 0.6252(4) 0.2923(4) 0.0379(14) Uani 1 1 d . A . H8A H -0.1252 0.6792 0.2674 0.045 Uiso 1 1 calc R . . H8B H -0.0697 0.6370 0.3514 0.045 Uiso 1 1 calc R . . C9 C 0.0380(4) 0.7962(3) 0.4298(3) 0.0272(12) Uani 1 1 d . . . H9A H 0.1070 0.7623 0.4329 0.033 Uiso 1 1 calc R . . C10 C -0.0201(4) 0.8303(4) 0.5024(3) 0.0305(13) Uani 1 1 d . B . H10A H 0.0097 0.8200 0.5537 0.037 Uiso 1 1 calc R . . C11 C -0.1219(4) 0.8797(3) 0.5032(3) 0.0294(12) Uani 1 1 d D . . C12 C -0.1589(4) 0.8919(4) 0.4246(3) 0.0309(12) Uani 1 1 d . B . H12A H -0.2277 0.9255 0.4204 0.037 Uiso 1 1 calc R . . C13 C -0.0963(4) 0.8554(3) 0.3521(3) 0.0257(12) Uani 1 1 d . . . C14 C -0.1339(4) 0.8705(3) 0.2684(3) 0.0242(12) Uani 1 1 d . B . C15 C -0.2353(4) 0.9069(3) 0.2585(3) 0.0291(12) Uani 1 1 d . . . H15A H -0.2833 0.9231 0.3079 0.035 Uiso 1 1 calc R B . C16 C -0.2694(4) 0.9206(4) 0.1795(3) 0.0310(13) Uani 1 1 d . B . C17 C -0.1923(4) 0.8999(4) 0.1092(3) 0.0341(13) Uani 1 1 d . . . H17A H -0.2094 0.9124 0.0523 0.041 Uiso 1 1 calc R B . C18 C -0.0930(4) 0.8621(3) 0.1221(3) 0.0295(12) Uani 1 1 d . B . H18A H -0.0435 0.8480 0.0732 0.035 Uiso 1 1 calc R . . C19 C -0.1879(4) 0.9190(4) 0.5840(3) 0.0427(15) Uani 0.800(5) 1 d PDU B 1 C20 C -0.2974(4) 0.9671(6) 0.5695(4) 0.064(2) Uani 0.800(5) 1 d PDU B 1 H20A H -0.2993 1.0219 0.5220 0.095 Uiso 0.800(5) 1 calc PR B 1 H20B H -0.3363 0.9925 0.6223 0.095 Uiso 0.800(5) 1 calc PR B 1 H20C H -0.3272 0.9179 0.5550 0.095 Uiso 0.800(5) 1 calc PR B 1 C21 C -0.1422(5) 0.9955(5) 0.6094(5) 0.0590(19) Uani 0.800(5) 1 d PDU B 1 H21A H -0.0719 0.9645 0.6192 0.088 Uiso 0.800(5) 1 calc PR B 1 H21B H -0.1819 1.0195 0.6625 0.088 Uiso 0.800(5) 1 calc PR B 1 H21C H -0.1439 1.0512 0.5628 0.088 Uiso 0.800(5) 1 calc PR B 1 C22 C -0.1867(6) 0.8334(4) 0.6588(4) 0.061(2) Uani 0.800(5) 1 d PDU B 1 H22A H -0.1168 0.8036 0.6705 0.091 Uiso 0.800(5) 1 calc PR B 1 H22B H -0.2140 0.7832 0.6429 0.091 Uiso 0.800(5) 1 calc PR B 1 H22C H -0.2283 0.8587 0.7106 0.091 Uiso 0.800(5) 1 calc PR B 1 C23 C -0.3803(4) 0.9544(4) 0.1686(3) 0.0382(14) Uani 1 1 d . . . C24 C -0.4504(4) 0.9793(5) 0.2519(4) 0.0626(19) Uani 1 1 d . B . H24A H -0.4343 1.0338 0.2722 0.094 Uiso 1 1 calc R . . H24B H -0.4408 0.9209 0.2961 0.094 Uiso 1 1 calc R . . H24C H -0.5210 0.9991 0.2408 0.094 Uiso 1 1 calc R . . C25 C -0.4093(4) 0.8708(5) 0.1371(4) 0.0611(19) Uani 1 1 d . B . H25A H -0.3640 0.8527 0.0843 0.092 Uiso 1 1 calc R . . H25B H -0.4795 0.8935 0.1249 0.092 Uiso 1 1 calc R . . H25C H -0.4028 0.8131 0.1819 0.092 Uiso 1 1 calc R . . C26 C -0.3963(4) 1.0467(5) 0.1013(4) 0.0588(18) Uani 1 1 d . B . H26A H -0.3733 1.0983 0.1197 0.088 Uiso 1 1 calc R . . H26B H -0.4686 1.0707 0.0953 0.088 Uiso 1 1 calc R . . H26C H -0.3575 1.0302 0.0456 0.088 Uiso 1 1 calc R . . C27 C 0.2191(4) 1.0131(3) 0.1421(3) 0.0266(12) Uani 1 1 d . B . C28 C 0.1184(4) 1.0592(4) 0.1407(3) 0.0261(12) Uani 1 1 d . B . C29 C 0.0858(4) 1.1594(4) 0.1139(3) 0.0316(13) Uani 1 1 d . B . H29A H 0.0158 1.1905 0.1130 0.038 Uiso 1 1 calc R . . C30 C 0.1599(4) 1.2145(3) 0.0878(3) 0.0301(12) Uani 1 1 d D . . C31 C 0.2603(4) 1.1655(4) 0.0907(3) 0.0336(13) Uani 1 1 d . C . H31A H 0.3097 1.2027 0.0730 0.040 Uiso 1 1 calc R . . C32 C 0.2934(4) 1.0639(4) 0.1183(3) 0.0305(12) Uani 1 1 d . . . H32A H 0.3630 1.0320 0.1204 0.037 Uiso 1 1 calc R C . C33 C 0.1305(5) 1.3272(4) 0.0610(5) 0.0389(17) Uani 0.736(14) 1 d PDU C 1 C34 C 0.0174(4) 1.3696(5) 0.0858(7) 0.047(2) Uani 0.736(14) 1 d PDU C 1 H34A H -0.0207 1.3392 0.0567 0.070 Uiso 0.736(14) 1 calc PR C 1 H34B H 0.0004 1.4414 0.0681 0.070 Uiso 0.736(14) 1 calc PR C 1 H34C H -0.0004 1.3554 0.1485 0.070 Uiso 0.736(14) 1 calc PR C 1 C35 C 0.1598(8) 1.3505(7) -0.0369(5) 0.045(2) Uani 0.736(14) 1 d PDU C 1 H35A H 0.2328 1.3237 -0.0522 0.067 Uiso 0.736(14) 1 calc PR C 1 H35B H 0.1425 1.4224 -0.0540 0.067 Uiso 0.736(14) 1 calc PR C 1 H35C H 0.1226 1.3204 -0.0671 0.067 Uiso 0.736(14) 1 calc PR C 1 C36 C 0.1891(7) 1.3755(6) 0.1072(6) 0.042(2) Uani 0.736(14) 1 d PDU C 1 H36A H 0.2621 1.3494 0.0909 0.064 Uiso 0.736(14) 1 calc PR C 1 H36B H 0.1718 1.3603 0.1698 0.064 Uiso 0.736(14) 1 calc PR C 1 H36C H 0.1709 1.4473 0.0902 0.064 Uiso 0.736(14) 1 calc PR C 1 C37 C 0.2218(4) 0.6617(4) -0.0083(3) 0.0279(12) Uani 1 1 d . B . C38 C 0.1879(3) 0.7616(4) -0.0371(3) 0.0249(12) Uani 1 1 d . B . C39 C 0.1928(4) 0.7973(4) -0.1239(3) 0.0296(12) Uani 1 1 d . . . H39A H 0.1709 0.8662 -0.1429 0.036 Uiso 1 1 calc R . . C40 C 0.2309(4) 0.7293(4) -0.1838(3) 0.0305(12) Uani 1 1 d . . . C41 C 0.2647(4) 0.6298(4) -0.1527(3) 0.0369(14) Uani 1 1 d . . . H41A H 0.2919 0.5839 -0.1929 0.044 Uiso 1 1 calc R . . C42 C 0.2604(4) 0.5946(4) -0.0650(3) 0.0371(14) Uani 1 1 d . . . H42A H 0.2837 0.5260 -0.0453 0.045 Uiso 1 1 calc R . . C43 C 0.2351(4) 0.7678(4) -0.2809(3) 0.0378(14) Uani 1 1 d . . . C44 C 0.2678(5) 0.6832(4) -0.3358(3) 0.0488(16) Uani 1 1 d . . . H44A H 0.3361 0.6439 -0.3261 0.073 Uiso 1 1 calc R . . H44B H 0.2681 0.7106 -0.3970 0.073 Uiso 1 1 calc R . . H44C H 0.2202 0.6410 -0.3196 0.073 Uiso 1 1 calc R . . C45 C 0.3109(4) 0.8322(4) -0.3061(3) 0.0455(15) Uani 1 1 d . . . H45A H 0.3786 0.7922 -0.2953 0.068 Uiso 1 1 calc R . . H45B H 0.2902 0.8871 -0.2717 0.068 Uiso 1 1 calc R . . H45C H 0.3126 0.8587 -0.3676 0.068 Uiso 1 1 calc R . . C46 C 0.1305(4) 0.8316(5) -0.3007(4) 0.0550(17) Uani 1 1 d . . . H46A H 0.1084 0.8859 -0.2656 0.083 Uiso 1 1 calc R . . H46B H 0.0816 0.7907 -0.2871 0.083 Uiso 1 1 calc R . . H46C H 0.1349 0.8589 -0.3621 0.083 Uiso 1 1 calc R . . C47 C 0.3575(4) 0.7110(4) 0.3416(3) 0.0316(13) Uani 1 1 d . B . C48 C 0.3988(4) 0.6609(4) 0.2715(4) 0.0391(14) Uani 1 1 d . B . C49 C 0.4991(4) 0.6128(5) 0.2598(4) 0.0568(19) Uani 1 1 d . . . H49A H 0.5283 0.5787 0.2114 0.068 Uiso 1 1 calc R . . C50 C 0.5569(4) 0.6159(4) 0.3222(4) 0.0502(17) Uani 1 1 d . D . H50A H 0.6268 0.5823 0.3155 0.060 Uiso 1 1 calc R . . C51 C 0.5177(4) 0.6657(4) 0.3939(3) 0.0385(14) Uani 1 1 d D . . C52 C 0.4152(4) 0.7139(4) 0.4033(3) 0.0361(13) Uani 1 1 d . B . H52A H 0.3851 0.7483 0.4514 0.043 Uiso 1 1 calc R . . C53 C 0.5845(7) 0.6686(8) 0.4604(5) 0.047(2) Uani 0.56(2) 1 d PDU D 1 C54 C 0.6802(8) 0.6992(12) 0.4132(9) 0.051(3) Uani 0.56(2) 1 d PDU D 1 H54A H 0.7173 0.6519 0.3734 0.076 Uiso 0.56(2) 1 calc PR D 1 H54B H 0.7235 0.6999 0.4554 0.076 Uiso 0.56(2) 1 calc PR D 1 H54C H 0.6610 0.7655 0.3806 0.076 Uiso 0.56(2) 1 calc PR D 1 C55 C 0.6153(12) 0.5651(9) 0.5117(10) 0.054(3) Uani 0.56(2) 1 d PDU D 1 H55A H 0.6511 0.5174 0.4718 0.081 Uiso 0.56(2) 1 calc PR D 1 H55B H 0.5544 0.5458 0.5432 0.081 Uiso 0.56(2) 1 calc PR D 1 H55C H 0.6599 0.5659 0.5528 0.081 Uiso 0.56(2) 1 calc PR D 1 C56 C 0.5310(9) 0.7430(13) 0.5235(8) 0.051(3) Uani 0.56(2) 1 d PDU D 1 H56A H 0.5769 0.7426 0.5639 0.077 Uiso 0.56(2) 1 calc PR D 1 H56B H 0.4701 0.7246 0.5557 0.077 Uiso 0.56(2) 1 calc PR D 1 H56C H 0.5118 0.8095 0.4912 0.077 Uiso 0.56(2) 1 calc PR D 1 Ir1 Ir 0.090615(16) 0.767225(15) 0.228819(13) 0.02443(7) Uani 1 1 d . . . N2 N 0.0025(3) 0.8083(3) 0.3541(2) 0.0229(9) Uani 1 1 d . B . N1 N -0.0615(3) 0.8435(3) 0.2008(2) 0.0243(10) Uani 1 1 d . B . O1 O 0.2294(2) 0.9141(2) 0.1730(2) 0.0293(8) Uani 1 1 d . . . O2 O 0.0613(2) 0.9918(2) 0.1695(2) 0.0284(8) Uani 1 1 d . . . O3 O 0.2038(2) 0.6470(2) 0.0810(2) 0.0308(8) Uani 1 1 d . . . O4 O 0.1496(2) 0.8124(2) 0.03224(19) 0.0286(8) Uani 1 1 d . . . O5 O 0.2563(2) 0.7519(2) 0.3385(2) 0.0326(8) Uani 1 1 d . . . O6 O 0.3232(3) 0.6695(3) 0.2223(2) 0.0421(10) Uani 1 1 d . . . C57 C 0.5988(8) 0.6119(8) 0.7617(5) 0.081(3) Uani 0.776(7) 1 d PDU E 1 H57A H 0.6317 0.5543 0.7316 0.122 Uiso 0.776(7) 1 calc PR E 1 H57B H 0.6465 0.6529 0.7577 0.122 Uiso 0.776(7) 1 calc PR E 1 H57C H 0.5391 0.6509 0.7350 0.122 Uiso 0.776(7) 1 calc PR E 1 C58 C 0.5661(7) 0.5770(5) 0.8565(5) 0.076(2) Uani 0.776(7) 1 d PDU E 1 H58A H 0.6257 0.5383 0.8848 0.092 Uiso 0.776(7) 1 calc PR E 1 H58B H 0.5182 0.5351 0.8618 0.092 Uiso 0.776(7) 1 calc PR E 1 C59 C 0.5145(7) 0.6719(5) 0.8978(4) 0.073(2) Uani 0.776(7) 1 d PDU E 1 H59A H 0.5551 0.7213 0.8775 0.087 Uiso 0.776(7) 1 calc PR E 1 H59B H 0.4464 0.7007 0.8798 0.087 Uiso 0.776(7) 1 calc PR E 1 C60 C 0.5047(7) 0.6492(5) 0.9941(5) 0.070(2) Uani 0.776(7) 1 d PDU E 1 H60A H 0.5728 0.6198 1.0118 0.084 Uiso 0.776(7) 1 calc PR E 1 H60B H 0.4638 0.6001 1.0142 0.084 Uiso 0.776(7) 1 calc PR E 1 C61 C 0.4542(7) 0.7431(6) 1.0363(5) 0.086(3) Uani 0.776(7) 1 d PDU E 1 H61A H 0.4504 0.7267 1.0992 0.129 Uiso 0.776(7) 1 calc PR E 1 H61B H 0.3856 0.7705 1.0209 0.129 Uiso 0.776(7) 1 calc PR E 1 H61C H 0.4941 0.7921 1.0158 0.129 Uiso 0.776(7) 1 calc PR E 1 C62 C 0.571(3) 0.599(3) 0.7409(16) 0.081(5) Uani 0.224(7) 1 d PDU E 2 H62A H 0.5977 0.6292 0.6840 0.121 Uiso 0.224(7) 1 calc PR E 2 H62B H 0.5048 0.5890 0.7389 0.121 Uiso 0.224(7) 1 calc PR E 2 H62C H 0.6182 0.5354 0.7572 0.121 Uiso 0.224(7) 1 calc PR E 2 C63 C 0.561(2) 0.6686(18) 0.8082(14) 0.079(3) Uani 0.224(7) 1 d PDU E 2 H63A H 0.5115 0.7322 0.7943 0.094 Uiso 0.224(7) 1 calc PR E 2 H63B H 0.6275 0.6824 0.8089 0.094 Uiso 0.224(7) 1 calc PR E 2 C64 C 0.525(3) 0.6145(17) 0.8967(14) 0.079(3) Uani 0.224(7) 1 d PDU E 2 H64A H 0.4546 0.6103 0.8981 0.094 Uiso 0.224(7) 1 calc PR E 2 H64B H 0.5687 0.5462 0.9051 0.094 Uiso 0.224(7) 1 calc PR E 2 C65 C 0.5298(19) 0.670(2) 0.9694(15) 0.073(3) Uani 0.224(7) 1 d PDU E 2 H65A H 0.5364 0.7375 0.9452 0.088 Uiso 0.224(7) 1 calc PR E 2 H65B H 0.5900 0.6350 0.9984 0.088 Uiso 0.224(7) 1 calc PR E 2 C66 C 0.433(2) 0.676(3) 1.0353(17) 0.084(4) Uani 0.224(7) 1 d PDU E 2 H66A H 0.4414 0.7016 1.0862 0.126 Uiso 0.224(7) 1 calc PR E 2 H66B H 0.4216 0.6095 1.0528 0.126 Uiso 0.224(7) 1 calc PR E 2 H66C H 0.3753 0.7198 1.0092 0.126 Uiso 0.224(7) 1 calc PR E 2 C67 C -0.1933(10) 0.9218(11) 0.5808(7) 0.054(3) Uani 0.200(5) 1 d PDU B 2 C68 C -0.1334(17) 0.9121(19) 0.6555(10) 0.059(3) Uani 0.200(5) 1 d PDU B 2 H68A H -0.0914 0.8442 0.6654 0.088 Uiso 0.200(5) 1 calc PR B 2 H68B H -0.1807 0.9275 0.7079 0.088 Uiso 0.200(5) 1 calc PR B 2 H68C H -0.0899 0.9584 0.6409 0.088 Uiso 0.200(5) 1 calc PR B 2 C69 C -0.2765(14) 0.8660(18) 0.6103(14) 0.058(3) Uani 0.200(5) 1 d PDU B 2 H69A H -0.2465 0.7981 0.6352 0.087 Uiso 0.200(5) 1 calc PR B 2 H69B H -0.3088 0.8647 0.5606 0.087 Uiso 0.200(5) 1 calc PR B 2 H69C H -0.3273 0.8996 0.6539 0.087 Uiso 0.200(5) 1 calc PR B 2 C70 C -0.2423(18) 1.0317(11) 0.5556(14) 0.055(3) Uani 0.200(5) 1 d PDU B 2 H70A H -0.2854 1.0590 0.6060 0.083 Uiso 0.200(5) 1 calc PR B 2 H70B H -0.2835 1.0392 0.5096 0.083 Uiso 0.200(5) 1 calc PR B 2 H70C H -0.1892 1.0673 0.5350 0.083 Uiso 0.200(5) 1 calc PR B 2 C71 C 0.1299(10) 1.3222(7) 0.0441(10) 0.042(3) Uani 0.264(14) 1 d PDU C 2 C72 C 0.148(2) 1.3920(11) 0.0995(17) 0.046(3) Uani 0.264(14) 1 d PDU C 2 H72A H 0.1083 1.3850 0.1567 0.069 Uiso 0.264(14) 1 calc PR C 2 H72B H 0.1280 1.4606 0.0716 0.069 Uiso 0.264(14) 1 calc PR C 2 H72C H 0.2205 1.3752 0.1056 0.069 Uiso 0.264(14) 1 calc PR C 2 C73 C 0.0180(11) 1.3530(13) 0.0307(18) 0.046(3) Uani 0.264(14) 1 d PDU C 2 H73A H -0.0246 1.3464 0.0867 0.070 Uiso 0.264(14) 1 calc PR C 2 H73B H 0.0063 1.3103 -0.0065 0.070 Uiso 0.264(14) 1 calc PR C 2 H73C H 0.0009 1.4220 0.0034 0.070 Uiso 0.264(14) 1 calc PR C 2 C74 C 0.1957(18) 1.3343(16) -0.0442(12) 0.042(4) Uani 0.264(14) 1 d PDU C 2 H74A H 0.2675 1.3136 -0.0364 0.063 Uiso 0.264(14) 1 calc PR C 2 H74B H 0.1788 1.4038 -0.0702 0.063 Uiso 0.264(14) 1 calc PR C 2 H74C H 0.1827 1.2931 -0.0822 0.063 Uiso 0.264(14) 1 calc PR C 2 C75 C 0.5907(8) 0.6554(9) 0.4590(6) 0.048(2) Uani 0.44(2) 1 d PDU D 2 C76 C 0.5335(11) 0.6948(19) 0.5424(8) 0.056(3) Uani 0.44(2) 1 d PDU D 2 H76A H 0.4994 0.7651 0.5294 0.084 Uiso 0.44(2) 1 calc PR D 2 H76B H 0.5814 0.6872 0.5831 0.084 Uiso 0.44(2) 1 calc PR D 2 H76C H 0.4829 0.6576 0.5682 0.084 Uiso 0.44(2) 1 calc PR D 2 C77 C 0.6692(11) 0.7147(14) 0.4197(11) 0.050(3) Uani 0.44(2) 1 d PDU D 2 H77A H 0.6345 0.7846 0.4057 0.074 Uiso 0.44(2) 1 calc PR D 2 H77B H 0.7078 0.6890 0.3670 0.074 Uiso 0.44(2) 1 calc PR D 2 H77C H 0.7156 0.7085 0.4614 0.074 Uiso 0.44(2) 1 calc PR D 2 C78 C 0.6458(14) 0.5463(9) 0.4817(13) 0.051(3) Uani 0.44(2) 1 d PDU D 2 H78A H 0.6920 0.5408 0.5233 0.077 Uiso 0.44(2) 1 calc PR D 2 H78B H 0.6845 0.5202 0.4292 0.077 Uiso 0.44(2) 1 calc PR D 2 H78C H 0.5959 0.5081 0.5071 0.077 Uiso 0.44(2) 1 calc PR D 2 C79 C 0.0607(12) 0.4069(13) 0.3568(19) 0.044(3) Uani 0.175(8) 1 d PDU A 2 H79A H 0.0716 0.3362 0.3818 0.053 Uiso 0.175(8) 1 calc PR A 2 H79B H 0.0817 0.4094 0.2937 0.053 Uiso 0.175(8) 1 calc PR A 2 C80 C -0.0525(11) 0.4556(18) 0.3727(12) 0.046(3) Uani 0.175(8) 1 d PDU A 2 H80A H -0.0652 0.4936 0.4219 0.055 Uiso 0.175(8) 1 calc PR A 2 H80B H -0.0891 0.4028 0.3903 0.055 Uiso 0.175(8) 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 B1 0.024(3) 0.034(4) 0.014(3) -0.004(3) 0.000(3) -0.006(3) B3 0.017(3) 0.034(4) 0.037(4) -0.005(3) -0.005(3) -0.008(3) B2 0.028(3) 0.018(3) 0.025(3) 0.001(3) 0.000(3) -0.006(3) C1 0.037(3) 0.021(3) 0.035(3) -0.008(2) 0.001(3) -0.011(2) C2 0.035(3) 0.019(3) 0.038(3) -0.001(2) -0.006(3) -0.005(2) C3 0.061(4) 0.029(3) 0.037(3) 0.007(3) -0.014(3) -0.014(3) C4 0.064(4) 0.027(3) 0.047(3) 0.007(3) -0.016(3) -0.012(3) C5 0.066(4) 0.028(3) 0.043(4) 0.002(3) 0.001(3) -0.016(3) C6 0.052(4) 0.030(3) 0.047(4) -0.007(3) 0.004(3) -0.020(3) C7 0.044(3) 0.037(3) 0.063(4) -0.005(3) -0.004(3) -0.020(3) C8 0.039(4) 0.028(3) 0.045(4) -0.003(3) -0.001(3) -0.010(3) C9 0.028(3) 0.027(3) 0.026(3) 0.001(2) -0.007(2) -0.007(2) C10 0.039(3) 0.033(3) 0.023(3) -0.002(2) -0.008(3) -0.014(3) C11 0.039(3) 0.023(3) 0.027(3) -0.007(2) 0.002(3) -0.012(3) C12 0.027(3) 0.034(3) 0.032(3) -0.004(3) -0.009(3) -0.006(2) C13 0.033(3) 0.020(3) 0.026(3) -0.001(2) -0.006(2) -0.009(2) C14 0.026(3) 0.021(3) 0.027(3) -0.006(2) 0.000(2) -0.008(2) C15 0.025(3) 0.031(3) 0.034(3) -0.010(2) 0.000(2) -0.010(2) C16 0.032(3) 0.024(3) 0.041(3) -0.010(2) -0.014(3) -0.003(2) C17 0.030(3) 0.043(3) 0.028(3) -0.007(3) -0.008(3) -0.006(3) C18 0.029(3) 0.033(3) 0.026(3) -0.007(2) -0.004(2) -0.004(2) C19 0.054(3) 0.047(3) 0.027(3) -0.017(3) 0.004(3) -0.012(3) C20 0.062(4) 0.078(4) 0.041(4) -0.023(3) 0.007(3) -0.001(4) C21 0.076(4) 0.054(4) 0.048(4) -0.026(3) 0.011(3) -0.018(3) C22 0.075(4) 0.058(4) 0.033(4) -0.004(3) 0.022(3) -0.010(3) C23 0.027(3) 0.044(4) 0.042(4) -0.010(3) -0.012(3) 0.000(3) C24 0.026(3) 0.102(6) 0.058(4) -0.028(4) -0.009(3) 0.000(4) C25 0.035(4) 0.074(5) 0.080(5) -0.031(4) -0.015(3) -0.006(3) C26 0.034(4) 0.068(5) 0.072(5) -0.007(4) -0.018(3) -0.002(3) C27 0.034(3) 0.021(3) 0.026(3) -0.001(2) -0.008(2) -0.008(2) C28 0.029(3) 0.028(3) 0.024(3) -0.005(2) -0.002(2) -0.012(3) C29 0.024(3) 0.028(3) 0.039(3) -0.006(2) -0.002(2) 0.000(2) C30 0.037(3) 0.024(3) 0.031(3) -0.001(2) -0.005(3) -0.012(3) C31 0.036(3) 0.028(3) 0.041(3) -0.002(3) -0.007(3) -0.016(3) C32 0.023(3) 0.041(3) 0.027(3) -0.003(3) -0.006(2) -0.008(3) C33 0.043(3) 0.024(3) 0.050(4) 0.000(3) -0.009(3) -0.010(3) C34 0.048(4) 0.022(4) 0.066(5) 0.001(4) -0.011(4) -0.005(3) C35 0.058(5) 0.020(4) 0.048(4) 0.003(3) -0.014(4) 0.002(4) C36 0.046(5) 0.024(4) 0.058(4) -0.011(3) -0.007(4) -0.006(4) C37 0.026(3) 0.032(3) 0.026(3) -0.006(2) -0.002(2) -0.009(2) C38 0.022(3) 0.027(3) 0.025(3) -0.007(2) -0.001(2) -0.005(2) C39 0.029(3) 0.030(3) 0.030(3) -0.004(2) -0.004(2) -0.008(2) C40 0.027(3) 0.041(3) 0.025(3) -0.009(3) 0.001(2) -0.012(3) C41 0.043(4) 0.035(3) 0.034(3) -0.012(3) -0.001(3) -0.010(3) C42 0.046(4) 0.024(3) 0.038(3) -0.005(3) 0.000(3) -0.008(3) C43 0.044(4) 0.044(3) 0.027(3) -0.012(3) 0.002(3) -0.014(3) C44 0.073(5) 0.056(4) 0.026(3) -0.013(3) 0.004(3) -0.032(3) C45 0.060(4) 0.048(4) 0.031(3) -0.005(3) 0.005(3) -0.025(3) C46 0.052(4) 0.085(5) 0.031(3) -0.007(3) -0.012(3) -0.018(4) C47 0.029(3) 0.029(3) 0.033(3) 0.003(2) -0.005(3) -0.005(3) C48 0.028(3) 0.047(4) 0.043(4) -0.011(3) -0.010(3) -0.004(3) C49 0.033(4) 0.078(5) 0.058(4) -0.040(4) -0.015(3) 0.013(3) C50 0.024(3) 0.057(4) 0.067(5) -0.017(4) -0.012(3) 0.003(3) C51 0.033(3) 0.048(4) 0.035(3) 0.000(3) -0.010(3) -0.013(3) C52 0.033(3) 0.049(4) 0.025(3) -0.005(3) -0.003(3) -0.009(3) C53 0.033(4) 0.068(4) 0.042(4) 0.004(3) -0.016(3) -0.016(4) C54 0.040(4) 0.060(5) 0.053(5) 0.002(4) -0.013(4) -0.017(4) C55 0.045(5) 0.073(5) 0.047(6) 0.013(4) -0.020(5) -0.024(4) C56 0.042(4) 0.075(6) 0.041(5) -0.003(4) -0.019(4) -0.017(5) Ir1 0.02733(12) 0.02305(11) 0.02323(11) -0.00168(8) -0.00581(8) -0.00628(8) N2 0.023(2) 0.024(2) 0.022(2) -0.0014(18) -0.0038(19) -0.0063(19) N1 0.028(2) 0.023(2) 0.024(2) -0.0038(19) -0.006(2) -0.0082(19) O1 0.026(2) 0.026(2) 0.033(2) 0.0023(16) -0.0063(16) -0.0057(16) O2 0.0232(19) 0.0237(19) 0.036(2) 0.0008(16) -0.0035(16) -0.0065(16) O3 0.037(2) 0.0233(19) 0.028(2) -0.0038(16) -0.0015(16) -0.0028(16) O4 0.037(2) 0.0261(19) 0.0203(19) -0.0052(15) -0.0013(16) -0.0056(16) O5 0.025(2) 0.041(2) 0.032(2) -0.0061(17) -0.0071(16) -0.0052(17) O6 0.032(2) 0.052(2) 0.045(2) -0.020(2) -0.0127(19) -0.0017(19) C57 0.068(6) 0.084(5) 0.086(5) -0.006(5) -0.034(5) 0.002(5) C58 0.061(5) 0.059(4) 0.110(5) -0.009(4) -0.020(4) -0.012(4) C59 0.053(4) 0.053(4) 0.118(5) -0.009(4) -0.017(4) -0.022(4) C60 0.045(4) 0.054(4) 0.110(5) 0.021(4) -0.019(4) -0.026(4) C61 0.081(5) 0.076(5) 0.099(6) 0.021(4) -0.015(5) -0.035(5) C62 0.059(9) 0.076(8) 0.106(7) 0.000(7) -0.028(8) -0.011(8) C63 0.057(6) 0.069(6) 0.104(6) -0.002(5) -0.026(6) -0.005(5) C64 0.055(5) 0.059(6) 0.116(6) 0.012(5) -0.017(5) -0.016(5) C65 0.054(6) 0.057(6) 0.105(6) 0.023(5) -0.017(5) -0.025(5) C66 0.065(7) 0.070(7) 0.112(7) 0.021(7) -0.019(6) -0.026(7) C67 0.064(4) 0.057(4) 0.036(4) -0.018(4) 0.010(4) -0.009(4) C68 0.070(5) 0.061(6) 0.038(5) -0.017(5) 0.010(5) -0.007(5) C69 0.064(5) 0.063(5) 0.037(5) -0.015(5) 0.014(5) -0.008(5) C70 0.065(6) 0.057(5) 0.038(5) -0.023(5) 0.012(5) -0.007(5) C71 0.048(5) 0.022(4) 0.053(5) 0.003(4) -0.010(4) -0.006(4) C72 0.051(6) 0.028(6) 0.052(6) 0.000(5) -0.004(6) -0.003(6) C73 0.051(5) 0.023(6) 0.058(6) 0.005(6) -0.008(5) -0.004(5) C74 0.052(7) 0.019(7) 0.047(6) 0.010(6) -0.014(6) 0.001(7) C75 0.036(4) 0.068(4) 0.043(4) 0.003(4) -0.016(4) -0.018(4) C76 0.042(5) 0.080(6) 0.044(5) 0.003(5) -0.015(4) -0.013(5) C77 0.039(5) 0.062(5) 0.049(5) 0.001(5) -0.013(4) -0.015(5) C78 0.042(7) 0.072(5) 0.039(7) 0.012(5) -0.015(6) -0.019(5) C79 0.060(5) 0.026(5) 0.046(6) 0.000(5) -0.002(5) -0.017(5) C80 0.058(5) 0.029(5) 0.052(6) -0.003(5) 0.001(5) -0.020(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 B1 O1 1.417(6) . ? B1 O2 1.421(6) . ? B1 Ir1 2.051(6) . ? B3 O3 1.431(7) . ? B3 O4 1.435(7) . ? B3 Ir1 2.006(6) . ? B2 O6 1.402(6) . ? B2 O5 1.441(6) . ? B2 Ir1 2.029(6) . ? C1 C2 1.396(7) . ? C1 C8 1.483(7) . ? C1 Ir1 2.348(5) . ? C1 H1A 1.0000 . ? C2 C3 1.504(7) . ? C2 Ir1 2.344(5) . ? C2 H2A 1.0000 . ? C3 C4 1.545(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.521(6) . ? C4 C79 1.524(9) . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.521(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C80 1.526(9) . ? C7 C8 1.547(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 H7C 0.9900 . ? C7 H7D 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.347(6) . ? C9 C10 1.365(6) . ? C9 H9A 0.9500 . ? C10 C11 1.390(7) . ? C10 H10A 0.9500 . ? C11 C12 1.399(6) . ? C11 C19 1.531(6) . ? C11 C67 1.533(8) . ? C12 C13 1.397(7) . ? C12 H12A 0.9500 . ? C13 N2 1.350(6) . ? C13 C14 1.475(7) . ? C14 N1 1.362(6) . ? C14 C15 1.383(6) . ? C15 C16 1.383(7) . ? C15 H15A 0.9500 . ? C16 C17 1.410(7) . ? C16 C23 1.510(7) . ? C17 C18 1.370(7) . ? C17 H17A 0.9500 . ? C18 N1 1.355(6) . ? C18 H18A 0.9500 . ? C19 C20 1.524(6) . ? C19 C21 1.538(6) . ? C19 C22 1.538(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.527(7) . ? C23 C26 1.527(8) . ? C23 C25 1.537(7) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.370(7) . ? C27 C32 1.376(7) . ? C27 O1 1.379(5) . ? C28 O2 1.371(5) . ? C28 C29 1.380(6) . ? C29 C30 1.416(6) . ? C29 H29A 0.9500 . ? C30 C31 1.377(7) . ? C30 C33 1.537(6) . ? C30 C71 1.538(8) . ? C31 C32 1.400(7) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C33 C34 1.521(6) . ? C33 C35 1.536(6) . ? C33 C36 1.538(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.363(7) . ? C37 O3 1.383(5) . ? C37 C38 1.385(6) . ? C38 O4 1.370(5) . ? C38 C39 1.377(6) . ? C39 C40 1.407(7) . ? C39 H39A 0.9500 . ? C40 C41 1.388(7) . ? C40 C43 1.539(7) . ? C41 C42 1.390(7) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.529(7) . ? C43 C45 1.531(7) . ? C43 C46 1.535(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 O5 1.368(6) . ? C47 C48 1.380(7) . ? C47 C52 1.383(7) . ? C48 C49 1.364(7) . ? C48 O6 1.383(6) . ? C49 C50 1.395(8) . ? C49 H49A 0.9500 . ? C50 C51 1.395(7) . ? C50 H50A 0.9500 . ? C51 C52 1.390(7) . ? C51 C75 1.534(7) . ? C51 C53 1.537(7) . ? C52 H52A 0.9500 . ? C53 C56 1.532(6) . ? C53 C54 1.533(6) . ? C53 C55 1.534(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? Ir1 N1 2.173(4) . ? Ir1 N2 2.222(4) . ? C57 C58 1.525(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.540(5) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.496(5) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.534(5) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.541(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.546(5) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.528(5) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.535(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C69 1.532(7) . ? C67 C70 1.532(7) . ? C67 C68 1.533(7) . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 C73 1.533(7) . ? C71 C72 1.533(7) . ? C71 C74 1.539(7) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C76 1.529(7) . ? C75 C77 1.533(7) . ? C75 C78 1.536(7) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.524(9) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 B1 O2 107.8(4) . . ? O1 B1 Ir1 127.4(4) . . ? O2 B1 Ir1 124.7(4) . . ? O3 B3 O4 106.3(4) . . ? O3 B3 Ir1 126.9(4) . . ? O4 B3 Ir1 126.2(4) . . ? O6 B2 O5 106.5(4) . . ? O6 B2 Ir1 130.6(4) . . ? O5 B2 Ir1 123.0(4) . . ? C2 C1 C8 123.9(5) . . ? C2 C1 Ir1 72.5(3) . . ? C8 C1 Ir1 118.7(3) . . ? C2 C1 H1A 112.0 . . ? C8 C1 H1A 112.0 . . ? Ir1 C1 H1A 112.0 . . ? C1 C2 C3 122.9(5) . . ? C1 C2 Ir1 72.8(3) . . ? C3 C2 Ir1 115.5(3) . . ? C1 C2 H2A 113.2 . . ? C3 C2 H2A 113.2 . . ? Ir1 C2 H2A 113.2 . . ? C2 C3 C4 113.2(4) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? C5 C4 C3 114.7(5) . . ? C79 C4 C3 119.5(9) . . ? C79 C4 H4C 107.4 . . ? C3 C4 H4C 107.4 . . ? C79 C4 H4D 107.4 . . ? C3 C4 H4D 107.4 . . ? H4C C4 H4D 107.0 . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? C4 C5 C6 116.2(5) . . ? C4 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? C4 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C7 C6 C5 115.4(5) . . ? C7 C6 H6A 108.4 . . ? C5 C6 H6A 108.4 . . ? C7 C6 H6B 108.4 . . ? C5 C6 H6B 108.4 . . ? H6A C6 H6B 107.5 . . ? C6 C7 C8 115.3(5) . . ? C80 C7 C8 107.7(11) . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C80 C7 H7C 110.2 . . ? C8 C7 H7C 110.2 . . ? C80 C7 H7D 110.2 . . ? C8 C7 H7D 110.2 . . ? H7C C7 H7D 108.5 . . ? C1 C8 C7 111.7(4) . . ? C1 C8 H8A 109.3 . . ? C7 C8 H8A 109.3 . . ? C1 C8 H8B 109.3 . . ? C7 C8 H8B 109.3 . . ? H8A C8 H8B 107.9 . . ? N2 C9 C10 123.3(5) . . ? N2 C9 H9A 118.4 . . ? C10 C9 H9A 118.4 . . ? C9 C10 C11 121.7(5) . . ? C9 C10 H10A 119.1 . . ? C11 C10 H10A 119.1 . . ? C10 C11 C12 114.9(4) . . ? C10 C11 C19 122.3(5) . . ? C12 C11 C19 122.8(5) . . ? C10 C11 C67 125.8(7) . . ? C12 C11 C67 119.3(7) . . ? C13 C12 C11 121.2(5) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? N2 C13 C12 121.9(4) . . ? N2 C13 C14 116.6(4) . . ? C12 C13 C14 121.4(5) . . ? N1 C14 C15 121.8(4) . . ? N1 C14 C13 115.0(4) . . ? C15 C14 C13 123.2(4) . . ? C16 C15 C14 122.5(5) . . ? C16 C15 H15A 118.8 . . ? C14 C15 H15A 118.8 . . ? C15 C16 C17 114.8(5) . . ? C15 C16 C23 123.0(5) . . ? C17 C16 C23 122.2(5) . . ? C18 C17 C16 120.7(5) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? N1 C18 C17 123.7(5) . . ? N1 C18 H18A 118.1 . . ? C17 C18 H18A 118.1 . . ? C20 C19 C11 112.3(5) . . ? C20 C19 C21 109.4(5) . . ? C11 C19 C21 108.3(4) . . ? C20 C19 C22 108.6(5) . . ? C11 C19 C22 109.6(4) . . ? C21 C19 C22 108.6(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C16 C23 C24 113.6(4) . . ? C16 C23 C26 108.8(5) . . ? C24 C23 C26 108.3(5) . . ? C16 C23 C25 108.3(4) . . ? C24 C23 C25 108.2(5) . . ? C26 C23 C25 109.6(5) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 122.1(5) . . ? C28 C27 O1 109.4(4) . . ? C32 C27 O1 128.4(5) . . ? C27 C28 O2 109.8(4) . . ? C27 C28 C29 121.8(5) . . ? O2 C28 C29 128.4(5) . . ? C28 C29 C30 118.0(5) . . ? C28 C29 H29A 121.0 . . ? C30 C29 H29A 121.0 . . ? C31 C30 C29 118.4(4) . . ? C31 C30 C33 119.8(5) . . ? C29 C30 C33 121.7(5) . . ? C31 C30 C71 120.9(6) . . ? C29 C30 C71 120.0(6) . . ? C30 C31 C32 123.6(5) . . ? C30 C31 H31A 118.2 . . ? C32 C31 H31A 118.2 . . ? C27 C32 C31 116.0(5) . . ? C27 C32 H32A 122.0 . . ? C31 C32 H32A 122.0 . . ? C34 C33 C35 110.0(5) . . ? C34 C33 C30 110.9(5) . . ? C35 C33 C30 109.3(5) . . ? C34 C33 C36 108.8(5) . . ? C35 C33 C36 108.7(5) . . ? C30 C33 C36 109.1(5) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 O3 129.9(5) . . ? C42 C37 C38 121.0(5) . . ? O3 C37 C38 109.0(4) . . ? O4 C38 C39 128.9(4) . . ? O4 C38 C37 109.5(4) . . ? C39 C38 C37 121.6(5) . . ? C38 C39 C40 118.5(5) . . ? C38 C39 H39A 120.8 . . ? C40 C39 H39A 120.8 . . ? C41 C40 C39 118.4(5) . . ? C41 C40 C43 122.4(5) . . ? C39 C40 C43 119.1(5) . . ? C40 C41 C42 122.6(5) . . ? C40 C41 H41A 118.7 . . ? C42 C41 H41A 118.7 . . ? C37 C42 C41 117.8(5) . . ? C37 C42 H42A 121.1 . . ? C41 C42 H42A 121.1 . . ? C44 C43 C45 108.9(4) . . ? C44 C43 C46 108.6(5) . . ? C45 C43 C46 108.4(5) . . ? C44 C43 C40 111.9(4) . . ? C45 C43 C40 108.9(4) . . ? C46 C43 C40 110.1(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O5 C47 C48 109.3(5) . . ? O5 C47 C52 128.9(5) . . ? C48 C47 C52 121.8(5) . . ? C49 C48 C47 121.0(5) . . ? C49 C48 O6 130.3(5) . . ? C47 C48 O6 108.7(5) . . ? C48 C49 C50 117.0(5) . . ? C48 C49 H49A 121.5 . . ? C50 C49 H49A 121.5 . . ? C49 C50 C51 123.6(5) . . ? C49 C50 H50A 118.2 . . ? C51 C50 H50A 118.2 . . ? C52 C51 C50 117.5(4) . . ? C52 C51 C75 125.9(6) . . ? C50 C51 C75 116.4(6) . . ? C52 C51 C53 120.6(6) . . ? C50 C51 C53 121.9(6) . . ? C47 C52 C51 119.1(5) . . ? C47 C52 H52A 120.4 . . ? C51 C52 H52A 120.4 . . ? C56 C53 C54 107.4(6) . . ? C56 C53 C55 109.1(6) . . ? C54 C53 C55 109.1(6) . . ? C56 C53 C51 112.7(6) . . ? C54 C53 C51 109.3(7) . . ? C55 C53 C51 109.1(6) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? B3 Ir1 B2 87.2(2) . . ? B3 Ir1 B1 82.7(2) . . ? B2 Ir1 B1 81.1(2) . . ? B3 Ir1 N1 98.57(19) . . ? B2 Ir1 N1 167.05(17) . . ? B1 Ir1 N1 88.16(18) . . ? B3 Ir1 N2 172.87(19) . . ? B2 Ir1 N2 99.32(19) . . ? B1 Ir1 N2 95.48(17) . . ? N1 Ir1 N2 74.44(14) . . ? B3 Ir1 C2 89.0(2) . . ? B2 Ir1 C2 75.5(2) . . ? B1 Ir1 C2 155.5(2) . . ? N1 Ir1 C2 115.99(16) . . ? N2 Ir1 C2 95.29(16) . . ? B3 Ir1 C1 87.2(2) . . ? B2 Ir1 C1 109.9(2) . . ? B1 Ir1 C1 164.80(19) . . ? N1 Ir1 C1 82.08(16) . . ? N2 Ir1 C1 93.10(16) . . ? C2 Ir1 C1 34.62(16) . . ? C9 N2 C13 117.0(4) . . ? C9 N2 Ir1 127.2(3) . . ? C13 N2 Ir1 115.8(3) . . ? C18 N1 C14 116.2(4) . . ? C18 N1 Ir1 125.9(3) . . ? C14 N1 Ir1 117.8(3) . . ? C27 O1 B1 106.5(4) . . ? C28 O2 B1 106.5(4) . . ? C37 O3 B3 107.4(4) . . ? C38 O4 B3 107.6(4) . . ? C47 O5 B2 107.3(4) . . ? C48 O6 B2 108.1(4) . . ? C58 C57 H57A 109.5 . . ? C58 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C58 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C57 C58 C59 105.6(5) . . ? C57 C58 H58A 110.6 . . ? C59 C58 H58A 110.6 . . ? C57 C58 H58B 110.6 . . ? C59 C58 H58B 110.6 . . ? H58A C58 H58B 108.7 . . ? C60 C59 C58 110.3(5) . . ? C60 C59 H59A 109.6 . . ? C58 C59 H59A 109.6 . . ? C60 C59 H59B 109.6 . . ? C58 C59 H59B 109.6 . . ? H59A C59 H59B 108.1 . . ? C59 C60 C61 111.0(5) . . ? C59 C60 H60A 109.4 . . ? C61 C60 H60A 109.4 . . ? C59 C60 H60B 109.4 . . ? C61 C60 H60B 109.4 . . ? H60A C60 H60B 108.0 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 H62A 109.5 . . ? C63 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C63 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C62 C63 C64 106.6(7) . . ? C62 C63 H63A 110.4 . . ? C64 C63 H63A 110.4 . . ? C62 C63 H63B 110.4 . . ? C64 C63 H63B 110.4 . . ? H63A C63 H63B 108.6 . . ? C65 C64 C63 110.3(7) . . ? C65 C64 H64A 109.6 . . ? C63 C64 H64A 109.6 . . ? C65 C64 H64B 109.6 . . ? C63 C64 H64B 109.6 . . ? H64A C64 H64B 108.1 . . ? C64 C65 C66 109.9(8) . . ? C64 C65 H65A 109.7 . . ? C66 C65 H65A 109.7 . . ? C64 C65 H65B 109.7 . . ? C66 C65 H65B 109.7 . . ? H65A C65 H65B 108.2 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C69 C67 C70 109.2(7) . . ? C69 C67 C68 109.5(7) . . ? C70 C67 C68 108.2(7) . . ? C69 C67 C11 110.1(8) . . ? C70 C67 C11 109.7(8) . . ? C68 C67 C11 110.0(8) . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C67 C70 H70A 109.5 . . ? C67 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C67 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C73 C71 C72 109.0(7) . . ? C73 C71 C30 111.3(8) . . ? C72 C71 C30 110.1(8) . . ? C73 C71 C74 108.8(7) . . ? C72 C71 C74 107.6(7) . . ? C30 C71 C74 109.9(8) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C76 C75 C77 108.7(7) . . ? C76 C75 C51 110.9(7) . . ? C77 C75 C51 109.4(8) . . ? C76 C75 C78 108.3(6) . . ? C77 C75 C78 109.1(7) . . ? C51 C75 C78 110.4(7) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C4 C79 C80 116.4(12) . . ? C4 C79 H79A 108.2 . . ? C80 C79 H79A 108.2 . . ? C4 C79 H79B 108.2 . . ? C80 C79 H79B 108.2 . . ? H79A C79 H79B 107.3 . . ? C79 C80 C7 116.0(12) . . ? C79 C80 H80A 108.3 . . ? C7 C80 H80A 108.3 . . ? C79 C80 H80B 108.3 . . ? C7 C80 H80B 108.3 . . ? H80A C80 H80B 107.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.40 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.477 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.114 #===END data_dippeIr(Bcat*)3 _database_code_depnum_ccdc_archive 'CCDC 740060' _audit_creation_method SHELXL-97 _audit_update_record ; 2008-03-08 text and data added, srw ; _chemical_formula_moiety 'C44 H68 B3 Ir O6 P2, C5 H12' _chemical_formula_sum 'C49 H80 B3 Ir O6 P2' _chemical_formula_weight 1051.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.5747(8) _cell_length_b 16.6713(7) _cell_length_c 30.6305(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10506.5(7) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5147 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 24.11 _exptl_crystal_description tabular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4352 _exptl_crystal_id ga39zas _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (1 -1 7) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 2.646 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6650 _exptl_absorpt_correction_T_max 0.8227 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; All crystals examined exhibited some non-merohedral twinning and were rapidly decomposing at room temperature under oil. For the data crystal one distinct cell was identified using APEX2 (Bruker, 2004)); however, some small crystallites could not be removed. Four frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2005) then corrected for absorption by integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using SAINT/SADABS (Bruker, 2005) to sort, merge, and scale the combined data. No decay correction was applied. ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id ga39zas _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_device 'Bruker Kappa/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 153721 _diffrn_reflns_av_R_equivalents 0.1203 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.30 _reflns_number_total 12930 _reflns_number_gt 8170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.0-1 (Bruker, 2004)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction ; SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 (Bruker, 2005 & 2007) ; _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2005)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2005)' _computing_molecular_graphics 'SHELXTL V6.12 (Bruker, 2005)' _computing_publication_material 'XCIF V6.12 (Bruker, 2005)' _refine_special_details ; Structure was phased by direct methods. Systematic conditions suggested the unambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The highest peaks in the final difference Fourier map were in the vicinity of atoms Ir1 and O6; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed no dependence on amplitude or resolution. ; _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^)+(0.0225P)^2^+18.4621P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12930 _refine_ls_number_parameters 820 _refine_ls_number_restraints 1347 _refine_ls_R_factor_all 0.0872 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1535(2) 0.1524(3) -0.10299(14) 0.0320(10) Uani 1 1 d . A . C2 C 0.1123(2) 0.1829(3) -0.07225(13) 0.0310(10) Uani 1 1 d . A . C3 C 0.0550(2) 0.2204(3) -0.08363(14) 0.0371(11) Uani 1 1 d . A . H3 H 0.0259 0.2394 -0.0619 0.045 Uiso 1 1 calc R . . C4 C 0.0408(2) 0.2297(3) -0.12769(14) 0.0377(10) Uani 1 1 d DU . . C5 C 0.0847(2) 0.2000(3) -0.15816(15) 0.0448(12) Uani 1 1 d . A . H5 H 0.0753 0.2070 -0.1883 0.054 Uiso 1 1 calc R . . C6 C 0.1418(2) 0.1605(3) -0.14679(15) 0.0443(12) Uani 1 1 d . . . H6 H 0.1709 0.1402 -0.1682 0.053 Uiso 1 1 calc R A . C7 C -0.0217(3) 0.2684(4) -0.1446(2) 0.0527(16) Uani 0.715(4) 1 d PDU A 1 C8 C -0.0622(4) 0.3058(6) -0.1077(3) 0.063(2) Uani 0.715(4) 1 d PDU A 1 H8A H -0.0357 0.3449 -0.0918 0.094 Uiso 0.715(4) 1 calc PR A 1 H8B H -0.0765 0.2635 -0.0876 0.094 Uiso 0.715(4) 1 calc PR A 1 H8C H -0.1003 0.3327 -0.1202 0.094 Uiso 0.715(4) 1 calc PR A 1 C9 C -0.0055(4) 0.3340(6) -0.1781(3) 0.068(2) Uani 0.715(4) 1 d PDU A 1 H9A H 0.0209 0.3757 -0.1641 0.101 Uiso 0.715(4) 1 calc PR A 1 H9B H -0.0459 0.3578 -0.1890 0.101 Uiso 0.715(4) 1 calc PR A 1 H9C H 0.0188 0.3105 -0.2024 0.101 Uiso 0.715(4) 1 calc PR A 1 C10 C -0.0633(4) 0.2039(5) -0.1675(4) 0.067(2) Uani 0.715(4) 1 d PDU A 1 H10A H -0.1044 0.2278 -0.1772 0.100 Uiso 0.715(4) 1 calc PR A 1 H10B H -0.0723 0.1601 -0.1470 0.100 Uiso 0.715(4) 1 calc PR A 1 H10C H -0.0396 0.1829 -0.1928 0.100 Uiso 0.715(4) 1 calc PR A 1 C11 C 0.2279(2) 0.2477(3) 0.11517(13) 0.0337(10) Uani 1 1 d . B . C12 C 0.1699(2) 0.2631(2) 0.09478(13) 0.0271(9) Uani 1 1 d . B . C13 C 0.1220(2) 0.3071(3) 0.11420(13) 0.0320(10) Uani 1 1 d . B . H13 H 0.0823 0.3172 0.0994 0.038 Uiso 1 1 calc R . . C14 C 0.1324(2) 0.3373(2) 0.15655(13) 0.0318(10) Uani 1 1 d DU . . C15 C 0.1917(2) 0.3211(3) 0.17621(14) 0.0407(11) Uani 1 1 d . B . H15 H 0.1994 0.3418 0.2046 0.049 Uiso 1 1 calc R . . C16 C 0.2401(2) 0.2764(3) 0.15645(14) 0.0452(12) Uani 1 1 d . . . H16 H 0.2801 0.2660 0.1708 0.054 Uiso 1 1 calc R B . C17 C 0.0817(3) 0.3879(4) 0.18069(19) 0.0416(16) Uani 0.715(7) 1 d PDU B 1 C18 C 0.0187(3) 0.3970(6) 0.1547(2) 0.058(2) Uani 0.715(7) 1 d PDU B 1 H18A H 0.0000 0.3438 0.1491 0.088 Uiso 0.715(7) 1 calc PR B 1 H18B H 0.0279 0.4236 0.1268 0.088 Uiso 0.715(7) 1 calc PR B 1 H18C H -0.0124 0.4293 0.1714 0.088 Uiso 0.715(7) 1 calc PR B 1 C19 C 0.1087(4) 0.4725(4) 0.1894(3) 0.063(2) Uani 0.715(7) 1 d PDU B 1 H19A H 0.1177 0.4992 0.1615 0.094 Uiso 0.715(7) 1 calc PR B 1 H19B H 0.1490 0.4684 0.2063 0.094 Uiso 0.715(7) 1 calc PR B 1 H19C H 0.0767 0.5038 0.2058 0.094 Uiso 0.715(7) 1 calc PR B 1 C20 C 0.0661(4) 0.3488(5) 0.2249(2) 0.072(3) Uani 0.715(7) 1 d PD B 1 H20A H 0.0504 0.2940 0.2201 0.108 Uiso 0.715(7) 1 calc PR B 1 H20B H 0.0324 0.3801 0.2398 0.108 Uiso 0.715(7) 1 calc PR B 1 H20C H 0.1054 0.3474 0.2429 0.108 Uiso 0.715(7) 1 calc PR B 1 C21 C 0.4067(2) 0.2434(3) -0.04970(15) 0.0367(11) Uani 1 1 d . C . C22 C 0.3540(2) 0.2655(3) -0.07468(15) 0.0369(11) Uani 1 1 d . C . C23 C 0.3588(3) 0.3133(3) -0.11103(16) 0.0473(13) Uani 1 1 d . C . H23 H 0.3215 0.3261 -0.1279 0.057 Uiso 1 1 calc R . . C24 C 0.4201(3) 0.3427(3) -0.12255(15) 0.0515(13) Uani 1 1 d DU . . C25 C 0.4727(3) 0.3209(3) -0.09638(19) 0.0537(14) Uani 1 1 d . C . H25 H 0.5145 0.3408 -0.1039 0.064 Uiso 1 1 calc R . . C26 C 0.4673(2) 0.2716(3) -0.05975(17) 0.0451(12) Uani 1 1 d . . . H26 H 0.5041 0.2583 -0.0425 0.054 Uiso 1 1 calc R C . C27 C 0.4301(5) 0.4028(6) -0.1599(3) 0.069(2) Uani 0.517(4) 1 d PDU C 1 C28 C 0.4628(8) 0.4803(6) -0.1435(5) 0.071(3) Uani 0.517(4) 1 d PDU C 1 H28A H 0.4357 0.5049 -0.1208 0.107 Uiso 0.517(4) 1 calc PR C 1 H28B H 0.4679 0.5178 -0.1679 0.107 Uiso 0.517(4) 1 calc PR C 1 H28C H 0.5056 0.4674 -0.1313 0.107 Uiso 0.517(4) 1 calc PR C 1 C29 C 0.4744(7) 0.3638(10) -0.1945(3) 0.081(3) Uani 0.517(4) 1 d PDU C 1 H29A H 0.4541 0.3146 -0.2053 0.122 Uiso 0.517(4) 1 calc PR C 1 H29B H 0.5166 0.3509 -0.1813 0.122 Uiso 0.517(4) 1 calc PR C 1 H29C H 0.4809 0.4012 -0.2188 0.122 Uiso 0.517(4) 1 calc PR C 1 C30 C 0.3649(5) 0.4256(9) -0.1808(4) 0.084(5) Uani 0.517(4) 1 d PD C 1 H30A H 0.3343 0.4423 -0.1580 0.127 Uiso 0.517(4) 1 calc PR C 1 H30B H 0.3471 0.3791 -0.1964 0.127 Uiso 0.517(4) 1 calc PR C 1 H30C H 0.3715 0.4698 -0.2014 0.127 Uiso 0.517(4) 1 calc PR C 1 C31 C 0.2325(2) -0.1043(3) 0.02773(16) 0.0452(11) Uani 1 1 d . . . H31A H 0.2643 -0.1173 0.0509 0.054 Uiso 1 1 calc R . . H31B H 0.1983 -0.1460 0.0282 0.054 Uiso 1 1 calc R . . C32 C 0.2669(2) -0.1066(3) -0.01659(15) 0.0415(11) Uani 1 1 d . D . H32A H 0.2343 -0.1168 -0.0397 0.050 Uiso 1 1 calc R . . H32B H 0.2982 -0.1517 -0.0168 0.050 Uiso 1 1 calc R . . C33 C 0.1860(3) -0.0107(3) 0.10001(15) 0.0498(13) Uani 1 1 d . . . H33A H 0.1677 -0.0645 0.1075 0.060 Uiso 1 1 calc R . . C34 C 0.1399(3) 0.0521(4) 0.11733(18) 0.0684(17) Uani 1 1 d . . . H34A H 0.1289 0.0398 0.1477 0.103 Uiso 1 1 calc R . . H34B H 0.1002 0.0523 0.0997 0.103 Uiso 1 1 calc R . . H34C H 0.1606 0.1049 0.1158 0.103 Uiso 1 1 calc R . . C35 C 0.2519(3) -0.0034(4) 0.12226(16) 0.0658(17) Uani 1 1 d . . . H35A H 0.2461 -0.0065 0.1540 0.099 Uiso 1 1 calc R . . H35B H 0.2717 0.0481 0.1146 0.099 Uiso 1 1 calc R . . H35C H 0.2801 -0.0473 0.1126 0.099 Uiso 1 1 calc R . . C36 C 0.1104(2) -0.0143(3) 0.01976(16) 0.0468(13) Uani 1 1 d . . . H36A H 0.0888 0.0387 0.0246 0.056 Uiso 1 1 calc R . . C37 C 0.1076(3) -0.0321(3) -0.02914(18) 0.0571(14) Uani 1 1 d . . . H37A H 0.0633 -0.0227 -0.0399 0.086 Uiso 1 1 calc R . . H37B H 0.1197 -0.0881 -0.0343 0.086 Uiso 1 1 calc R . . H37C H 0.1379 0.0033 -0.0446 0.086 Uiso 1 1 calc R . . C38 C 0.0689(3) -0.0785(4) 0.0428(2) 0.0760(19) Uani 1 1 d . . . H38A H 0.0256 -0.0802 0.0296 0.114 Uiso 1 1 calc R . . H38B H 0.0651 -0.0652 0.0739 0.114 Uiso 1 1 calc R . . H38C H 0.0898 -0.1310 0.0397 0.114 Uiso 1 1 calc R . . C39 C 0.3916(2) -0.0205(3) -0.00409(15) 0.0416(11) Uani 1 1 d . D . H39A H 0.4205 0.0167 -0.0208 0.050 Uiso 1 1 calc R . . C40 C 0.4246(3) -0.1022(3) -0.00465(19) 0.0625(15) Uani 1 1 d . . . H40A H 0.4670 -0.0984 0.0099 0.094 Uiso 1 1 calc R . . H40B H 0.4308 -0.1196 -0.0349 0.094 Uiso 1 1 calc R . . H40C H 0.3974 -0.1412 0.0108 0.094 Uiso 1 1 calc R . . C41 C 0.3883(3) 0.0121(3) 0.04243(16) 0.0545(14) Uani 1 1 d . . . H41A H 0.4325 0.0191 0.0538 0.082 Uiso 1 1 calc R . . H41B H 0.3646 -0.0259 0.0610 0.082 Uiso 1 1 calc R . . H41C H 0.3658 0.0638 0.0424 0.082 Uiso 1 1 calc R . . C42 C 0.3194(3) -0.0183(3) -0.08944(16) 0.0474(15) Uani 0.839(8) 1 d PDU D 1 H42A H 0.2746 -0.0093 -0.1012 0.057 Uiso 0.839(8) 1 calc PR D 1 C43 C 0.3592(4) 0.0510(4) -0.1067(2) 0.0542(19) Uani 0.839(8) 1 d PDU D 1 H43A H 0.3665 0.0438 -0.1381 0.081 Uiso 0.839(8) 1 calc PR D 1 H43B H 0.4012 0.0527 -0.0916 0.081 Uiso 0.839(8) 1 calc PR D 1 H43C H 0.3358 0.1013 -0.1017 0.081 Uiso 0.839(8) 1 calc PR D 1 C44 C 0.3395(4) -0.0994(4) -0.1069(2) 0.0674(19) Uani 0.839(8) 1 d PDU D 1 H44A H 0.3330 -0.1007 -0.1386 0.101 Uiso 0.839(8) 1 calc PR D 1 H44B H 0.3130 -0.1412 -0.0932 0.101 Uiso 0.839(8) 1 calc PR D 1 H44C H 0.3854 -0.1087 -0.1002 0.101 Uiso 0.839(8) 1 calc PR D 1 B1 B 0.1967(2) 0.1287(3) -0.03729(16) 0.0311(11) Uani 1 1 d . A . B2 B 0.2283(2) 0.1823(3) 0.05102(15) 0.0307(11) Uani 1 1 d . A . B3 B 0.3181(3) 0.1793(3) -0.02344(17) 0.0325(12) Uani 1 1 d . A . O1 O 0.20543(14) 0.11548(17) -0.08254(9) 0.0350(7) Uani 1 1 d . . . O2 O 0.13743(14) 0.16963(18) -0.03102(9) 0.0345(7) Uani 1 1 d . . . O3 O 0.26587(14) 0.19998(18) 0.08864(9) 0.0364(7) Uani 1 1 d . . . O4 O 0.16920(13) 0.22539(17) 0.05467(8) 0.0316(7) Uani 1 1 d . . . O5 O 0.38608(14) 0.19214(18) -0.01690(9) 0.0373(7) Uani 1 1 d . . . O6 O 0.29874(14) 0.23013(18) -0.05839(9) 0.0372(7) Uani 1 1 d . . . P2 P 0.19521(6) -0.00584(7) 0.03988(4) 0.0348(3) Uani 1 1 d . . . P1 P 0.31028(6) -0.01321(7) -0.02910(4) 0.0325(3) Uani 1 1 d DU . . Ir1 Ir 0.260262(7) 0.095230(9) 0.007630(5) 0.02728(5) Uani 1 1 d . A . C45 C 0.3263(14) 0.1277(14) 0.7738(7) 0.193(7) Uani 0.600(15) 1 d PDU E 1 H45A H 0.3115 0.1629 0.7502 0.290 Uiso 0.600(15) 1 calc PR E 1 H45B H 0.3599 0.1551 0.7908 0.290 Uiso 0.600(15) 1 calc PR E 1 H45C H 0.2895 0.1144 0.7927 0.290 Uiso 0.600(15) 1 calc PR E 1 C46 C 0.3547(10) 0.0499(14) 0.7541(7) 0.193(7) Uani 0.600(15) 1 d PDU E 1 H46A H 0.3625 0.0571 0.7225 0.231 Uiso 0.600(15) 1 calc PR E 1 H46B H 0.3966 0.0371 0.7683 0.231 Uiso 0.600(15) 1 calc PR E 1 C47 C 0.3070(9) -0.0179(13) 0.7614(8) 0.187(7) Uani 0.600(15) 1 d PDU E 1 H47A H 0.2673 -0.0092 0.7437 0.225 Uiso 0.600(15) 1 calc PR E 1 H47B H 0.2945 -0.0207 0.7925 0.225 Uiso 0.600(15) 1 calc PR E 1 C48 C 0.3409(10) -0.0963(14) 0.7474(7) 0.197(8) Uani 0.600(15) 1 d PDU E 1 H48A H 0.3425 -0.1002 0.7152 0.236 Uiso 0.600(15) 1 calc PR E 1 H48B H 0.3860 -0.0977 0.7587 0.236 Uiso 0.600(15) 1 calc PR E 1 C49 C 0.3023(11) -0.1645(15) 0.7660(6) 0.196(8) Uani 0.600(15) 1 d PDU E 1 H49A H 0.2967 -0.1566 0.7975 0.293 Uiso 0.600(15) 1 calc PR E 1 H49B H 0.3253 -0.2151 0.7608 0.293 Uiso 0.600(15) 1 calc PR E 1 H49C H 0.2596 -0.1665 0.7519 0.293 Uiso 0.600(15) 1 calc PR E 1 C50 C 0.0776(5) 0.3814(7) 0.1808(4) 0.044(3) Uani 0.285(7) 1 d PDU B 2 C51 C 0.0278(7) 0.3202(10) 0.1980(7) 0.062(6) Uani 0.285(7) 1 d PDU B 2 H51A H 0.0104 0.2890 0.1735 0.093 Uiso 0.285(7) 1 calc PR B 2 H51B H -0.0078 0.3486 0.2126 0.093 Uiso 0.285(7) 1 calc PR B 2 H51C H 0.0490 0.2840 0.2188 0.093 Uiso 0.285(7) 1 calc PR B 2 C52 C 0.1049(8) 0.4282(10) 0.2200(5) 0.054(3) Uani 0.285(7) 1 d PDU B 2 H52A H 0.1349 0.4697 0.2096 0.081 Uiso 0.285(7) 1 calc PR B 2 H52B H 0.1282 0.3912 0.2394 0.081 Uiso 0.285(7) 1 calc PR B 2 H52C H 0.0691 0.4533 0.2361 0.081 Uiso 0.285(7) 1 calc PR B 2 C53 C 0.0444(9) 0.4414(11) 0.1498(5) 0.056(3) Uani 0.285(7) 1 d PDU B 2 H53A H 0.0252 0.4124 0.1252 0.083 Uiso 0.285(7) 1 calc PR B 2 H53B H 0.0766 0.4798 0.1390 0.083 Uiso 0.285(7) 1 calc PR B 2 H53C H 0.0102 0.4702 0.1656 0.083 Uiso 0.285(7) 1 calc PR B 2 C54 C 0.4212(6) 0.3895(7) -0.1659(3) 0.071(3) Uani 0.301(7) 1 d PDU C 2 C55 C 0.4900(7) 0.4205(12) -0.1762(6) 0.076(3) Uani 0.301(7) 1 d PDU C 2 H55A H 0.5050 0.4551 -0.1524 0.114 Uiso 0.301(7) 1 calc PR C 2 H55B H 0.4891 0.4512 -0.2035 0.114 Uiso 0.301(7) 1 calc PR C 2 H55C H 0.5197 0.3749 -0.1794 0.114 Uiso 0.301(7) 1 calc PR C 2 C56 C 0.3999(10) 0.3378(10) -0.2052(4) 0.075(4) Uani 0.301(7) 1 d PDU C 2 H56A H 0.3556 0.3182 -0.2004 0.113 Uiso 0.301(7) 1 calc PR C 2 H56B H 0.4296 0.2921 -0.2083 0.113 Uiso 0.301(7) 1 calc PR C 2 H56C H 0.4012 0.3703 -0.2318 0.113 Uiso 0.301(7) 1 calc PR C 2 C57 C 0.3751(9) 0.4621(9) -0.1635(6) 0.068(4) Uani 0.301(7) 1 d PDU C 2 H57A H 0.3884 0.4972 -0.1395 0.102 Uiso 0.301(7) 1 calc PR C 2 H57B H 0.3306 0.4435 -0.1586 0.102 Uiso 0.301(7) 1 calc PR C 2 H57C H 0.3771 0.4920 -0.1911 0.102 Uiso 0.301(7) 1 calc PR C 2 C58 C 0.3082(18) 0.1807(19) 0.7864(11) 0.196(8) Uani 0.400(15) 1 d PDU E 2 H58A H 0.2707 0.2023 0.7705 0.294 Uiso 0.400(15) 1 calc PR E 2 H58B H 0.3399 0.2235 0.7914 0.294 Uiso 0.400(15) 1 calc PR E 2 H58C H 0.2937 0.1589 0.8145 0.294 Uiso 0.400(15) 1 calc PR E 2 C59 C 0.339(2) 0.1143(18) 0.7596(12) 0.193(7) Uani 0.400(15) 1 d PDU E 2 H59A H 0.3852 0.1061 0.7686 0.232 Uiso 0.400(15) 1 calc PR E 2 H59B H 0.3384 0.1275 0.7281 0.232 Uiso 0.400(15) 1 calc PR E 2 C60 C 0.2983(14) 0.0387(18) 0.7693(11) 0.187(8) Uani 0.400(15) 1 d PDU E 2 H60A H 0.2848 0.0374 0.8003 0.225 Uiso 0.400(15) 1 calc PR E 2 H60B H 0.2590 0.0373 0.7506 0.225 Uiso 0.400(15) 1 calc PR E 2 C61 C 0.3433(12) -0.0318(19) 0.7587(13) 0.190(8) Uani 0.400(15) 1 d PDU E 2 H61A H 0.3725 -0.0431 0.7837 0.228 Uiso 0.400(15) 1 calc PR E 2 H61B H 0.3703 -0.0195 0.7328 0.228 Uiso 0.400(15) 1 calc PR E 2 C62 C 0.2993(15) -0.104(2) 0.7496(11) 0.193(8) Uani 0.400(15) 1 d PDU E 2 H62A H 0.2710 -0.1138 0.7748 0.289 Uiso 0.400(15) 1 calc PR E 2 H62B H 0.3262 -0.1520 0.7444 0.289 Uiso 0.400(15) 1 calc PR E 2 H62C H 0.2726 -0.0937 0.7238 0.289 Uiso 0.400(15) 1 calc PR E 2 C63 C 0.3402(11) -0.0342(16) -0.0850(4) 0.056(3) Uiso 0.161(8) 1 d PDU D 2 H63A H 0.3709 -0.0804 -0.0816 0.067 Uiso 0.161(8) 1 calc PR D 2 C64 C 0.3808(15) 0.033(2) -0.1036(8) 0.054(4) Uani 0.161(8) 1 d PDU D 2 H64A H 0.3842 0.0262 -0.1353 0.081 Uiso 0.161(8) 1 calc PR D 2 H64B H 0.4244 0.0309 -0.0907 0.081 Uiso 0.161(8) 1 calc PR D 2 H64C H 0.3604 0.0843 -0.0969 0.081 Uiso 0.161(8) 1 calc PR D 2 C65 C 0.2868(14) -0.0651(18) -0.1143(6) 0.056(3) Uani 0.161(8) 1 d PDU D 2 H65A H 0.3012 -0.0629 -0.1447 0.084 Uiso 0.161(8) 1 calc PR D 2 H65B H 0.2480 -0.0318 -0.1106 0.084 Uiso 0.161(8) 1 calc PR D 2 H65C H 0.2766 -0.1207 -0.1065 0.084 Uiso 0.161(8) 1 calc PR D 2 C66 C -0.0239(6) 0.2686(12) -0.1408(7) 0.057(3) Uiso 0.138(8) 1 d PDU A 2 C67 C -0.0799(8) 0.208(2) -0.1356(15) 0.066(4) Uani 0.138(8) 1 d PDU A 2 H67A H -0.1036 0.2195 -0.1085 0.099 Uiso 0.138(8) 1 calc PR A 2 H67B H -0.0623 0.1536 -0.1345 0.099 Uiso 0.138(8) 1 calc PR A 2 H67C H -0.1096 0.2130 -0.1605 0.099 Uiso 0.138(8) 1 calc PR A 2 C68 C -0.0383(16) 0.3424(18) -0.1122(12) 0.062(3) Uani 0.138(8) 1 d PDU A 2 H68A H -0.0104 0.3412 -0.0862 0.093 Uiso 0.138(8) 1 calc PR A 2 H68B H -0.0840 0.3416 -0.1032 0.093 Uiso 0.138(8) 1 calc PR A 2 H68C H -0.0296 0.3914 -0.1289 0.093 Uiso 0.138(8) 1 calc PR A 2 C69 C -0.0224(16) 0.296(2) -0.1887(8) 0.061(3) Uani 0.138(8) 1 d PDU A 2 H69A H -0.0619 0.3269 -0.1952 0.091 Uiso 0.138(8) 1 calc PR A 2 H69B H -0.0201 0.2494 -0.2079 0.091 Uiso 0.138(8) 1 calc PR A 2 H69C H 0.0158 0.3304 -0.1935 0.091 Uiso 0.138(8) 1 calc PR A 2 C70 C 0.4377(10) 0.3918(13) -0.1632(5) 0.073(3) Uani 0.182(8) 1 d PDU C 3 C71 C 0.450(2) 0.4801(13) -0.1512(12) 0.071(4) Uani 0.182(8) 1 d PDU C 3 H71A H 0.4825 0.4830 -0.1279 0.107 Uiso 0.182(8) 1 calc PR C 3 H71B H 0.4094 0.5046 -0.1412 0.107 Uiso 0.182(8) 1 calc PR C 3 H71C H 0.4659 0.5090 -0.1770 0.107 Uiso 0.182(8) 1 calc PR C 3 C72 C 0.5001(13) 0.359(3) -0.1843(9) 0.077(4) Uani 0.182(8) 1 d PDU C 3 H72A H 0.4966 0.3002 -0.1872 0.116 Uiso 0.182(8) 1 calc PR C 3 H72B H 0.5376 0.3717 -0.1658 0.116 Uiso 0.182(8) 1 calc PR C 3 H72C H 0.5060 0.3826 -0.2132 0.116 Uiso 0.182(8) 1 calc PR C 3 C73 C 0.3824(14) 0.388(2) -0.1968(7) 0.075(4) Uani 0.182(8) 1 d PDU C 3 H73A H 0.3791 0.3331 -0.2084 0.112 Uiso 0.182(8) 1 calc PR C 3 H73B H 0.3915 0.4250 -0.2208 0.112 Uiso 0.182(8) 1 calc PR C 3 H73C H 0.3413 0.4027 -0.1828 0.112 Uiso 0.182(8) 1 calc PR C 3 C74 C -0.0209(6) 0.2763(11) -0.1399(7) 0.059(3) Uani 0.147(8) 1 d PDU A 3 C75 C -0.0703(11) 0.274(2) -0.1022(11) 0.062(4) Uani 0.147(8) 1 d PDU A 3 H75A H -0.0806 0.2186 -0.0949 0.094 Uiso 0.147(8) 1 calc PR A 3 H75B H -0.1101 0.3023 -0.1111 0.094 Uiso 0.147(8) 1 calc PR A 3 H75C H -0.0517 0.3011 -0.0766 0.094 Uiso 0.147(8) 1 calc PR A 3 C76 C -0.0036(14) 0.3641(11) -0.1500(14) 0.065(4) Uani 0.147(8) 1 d PDU A 3 H76A H 0.0141 0.3896 -0.1238 0.097 Uiso 0.147(8) 1 calc PR A 3 H76B H -0.0428 0.3927 -0.1593 0.097 Uiso 0.147(8) 1 calc PR A 3 H76C H 0.0289 0.3658 -0.1734 0.097 Uiso 0.147(8) 1 calc PR A 3 C77 C -0.0530(14) 0.239(2) -0.1804(10) 0.059(3) Uani 0.147(8) 1 d PDU A 3 H77A H -0.0574 0.1810 -0.1762 0.089 Uiso 0.147(8) 1 calc PR A 3 H77B H -0.0260 0.2496 -0.2061 0.089 Uiso 0.147(8) 1 calc PR A 3 H77C H -0.0961 0.2628 -0.1846 0.089 Uiso 0.147(8) 1 calc PR A 3 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 C1 0.032(3) 0.031(2) 0.033(2) 0.0007(19) -0.0018(19) 0.0015(19) C2 0.035(3) 0.028(2) 0.029(2) -0.0018(18) -0.0026(18) -0.0009(19) C3 0.041(3) 0.034(3) 0.036(3) -0.005(2) -0.002(2) 0.008(2) C4 0.041(3) 0.032(3) 0.040(3) 0.006(2) -0.007(2) -0.002(2) C5 0.048(3) 0.058(3) 0.028(2) 0.007(2) -0.005(2) 0.003(3) C6 0.044(3) 0.058(3) 0.030(3) 0.004(2) 0.006(2) 0.010(2) C7 0.046(3) 0.065(4) 0.047(3) 0.006(3) -0.010(3) 0.019(3) C8 0.050(4) 0.076(5) 0.063(4) 0.006(4) -0.005(3) 0.023(4) C9 0.065(5) 0.069(5) 0.068(5) 0.017(4) -0.008(4) 0.031(4) C10 0.043(4) 0.092(5) 0.065(5) -0.007(4) -0.020(4) 0.012(4) C11 0.036(3) 0.032(2) 0.034(2) -0.0037(18) 0.0001(18) 0.003(2) C12 0.031(2) 0.026(2) 0.025(2) -0.0005(17) -0.0024(17) 0.0001(18) C13 0.031(2) 0.033(3) 0.032(2) 0.0011(19) -0.0014(18) 0.0002(19) C14 0.036(3) 0.029(2) 0.030(2) -0.0004(18) 0.0024(18) -0.0024(19) C15 0.051(3) 0.047(3) 0.025(2) -0.007(2) -0.005(2) 0.000(2) C16 0.039(3) 0.059(3) 0.038(2) -0.009(2) -0.014(2) 0.007(3) C17 0.045(4) 0.045(4) 0.036(3) -0.006(3) 0.009(3) 0.004(3) C18 0.046(4) 0.076(5) 0.053(4) -0.009(4) 0.008(3) 0.016(4) C19 0.070(5) 0.048(4) 0.070(5) -0.015(4) 0.009(4) 0.011(4) C20 0.079(7) 0.092(8) 0.044(5) 0.015(5) 0.031(4) 0.019(6) C21 0.040(3) 0.028(2) 0.042(3) 0.001(2) 0.005(2) -0.002(2) C22 0.039(3) 0.028(3) 0.044(3) 0.000(2) 0.008(2) 0.000(2) C23 0.053(3) 0.044(3) 0.045(3) 0.010(2) 0.003(2) -0.007(3) C24 0.059(4) 0.041(3) 0.054(3) 0.005(2) 0.013(3) -0.010(3) C25 0.041(3) 0.043(3) 0.077(4) -0.004(3) 0.019(3) -0.007(3) C26 0.038(3) 0.037(3) 0.061(3) 0.000(2) 0.007(2) 0.005(2) C27 0.081(5) 0.066(5) 0.059(4) 0.021(4) 0.022(4) -0.019(4) C28 0.076(7) 0.062(5) 0.075(6) 0.029(4) 0.004(5) -0.012(5) C29 0.096(6) 0.085(6) 0.062(5) 0.019(4) 0.025(5) -0.005(6) C30 0.093(11) 0.112(14) 0.048(8) 0.041(8) -0.011(7) -0.035(9) C31 0.052(3) 0.024(2) 0.060(3) 0.005(2) 0.014(2) 0.005(2) C32 0.043(3) 0.027(2) 0.054(3) -0.005(2) 0.002(2) 0.000(2) C33 0.061(4) 0.047(3) 0.041(3) 0.012(2) 0.015(2) 0.011(3) C34 0.087(5) 0.067(4) 0.051(3) 0.001(3) 0.027(3) 0.008(3) C35 0.085(5) 0.078(4) 0.035(3) 0.012(3) 0.002(3) 0.020(3) C36 0.040(3) 0.040(3) 0.061(3) -0.003(2) 0.007(2) -0.001(2) C37 0.046(3) 0.047(3) 0.079(4) -0.003(3) -0.008(3) -0.009(3) C38 0.057(4) 0.075(5) 0.096(5) 0.001(4) 0.013(3) -0.020(3) C39 0.041(3) 0.041(3) 0.042(3) 0.005(2) -0.001(2) 0.004(2) C40 0.049(3) 0.059(4) 0.080(4) 0.003(3) -0.006(3) 0.020(3) C41 0.061(4) 0.052(3) 0.051(3) 0.000(3) -0.017(3) 0.009(3) C42 0.064(4) 0.043(3) 0.035(3) -0.005(2) 0.005(3) 0.019(3) C43 0.061(4) 0.062(4) 0.039(3) 0.000(3) 0.014(3) 0.006(3) C44 0.096(4) 0.058(3) 0.049(3) -0.011(3) 0.005(3) 0.025(3) B1 0.034(3) 0.023(2) 0.037(3) 0.003(2) 0.005(2) 0.000(2) B2 0.037(3) 0.024(2) 0.031(3) 0.0037(19) -0.002(2) 0.001(2) B3 0.036(3) 0.027(3) 0.035(3) -0.003(2) 0.002(2) 0.003(2) O1 0.0370(18) 0.0387(19) 0.0294(16) 0.0012(13) -0.0017(13) 0.0050(14) O2 0.0367(18) 0.0384(18) 0.0284(16) -0.0028(13) -0.0046(13) 0.0097(14) O3 0.0317(17) 0.0414(18) 0.0361(16) -0.0084(13) -0.0054(13) 0.0057(15) O4 0.0323(17) 0.0354(17) 0.0272(15) -0.0056(13) -0.0038(12) 0.0050(13) O5 0.0373(18) 0.0323(18) 0.0423(19) 0.0068(14) -0.0008(13) 0.0008(13) O6 0.0363(18) 0.0359(18) 0.0394(18) 0.0095(14) -0.0009(13) 0.0020(14) P2 0.0386(7) 0.0283(6) 0.0377(6) 0.0047(5) 0.0075(5) 0.0041(5) P1 0.0352(7) 0.0274(6) 0.0350(6) -0.0031(5) 0.0045(5) 0.0011(5) Ir1 0.03112(8) 0.02405(8) 0.02667(7) 0.00045(7) 0.00028(7) 0.00306(7) C45 0.196(12) 0.30(2) 0.083(12) 0.019(12) -0.011(9) 0.018(13) C46 0.181(10) 0.31(2) 0.087(7) 0.009(10) -0.003(7) 0.002(13) C47 0.174(10) 0.31(2) 0.078(7) 0.011(10) -0.005(8) 0.003(13) C48 0.185(11) 0.31(2) 0.090(8) -0.005(9) -0.006(8) -0.008(13) C49 0.195(12) 0.30(2) 0.087(9) -0.003(10) -0.010(9) 0.000(13) C50 0.041(6) 0.053(6) 0.040(6) -0.008(5) 0.008(5) 0.004(5) C51 0.046(12) 0.052(11) 0.086(16) -0.014(8) 0.039(10) 0.004(7) C52 0.058(6) 0.050(7) 0.055(6) -0.018(5) 0.012(5) 0.005(6) C53 0.054(7) 0.062(7) 0.052(6) -0.010(6) 0.011(5) 0.018(5) C54 0.084(6) 0.069(6) 0.058(5) 0.016(5) 0.023(5) -0.014(5) C55 0.089(6) 0.076(6) 0.064(5) 0.024(5) 0.017(5) -0.015(5) C56 0.102(11) 0.070(10) 0.053(7) 0.015(7) 0.009(8) -0.007(8) C57 0.092(8) 0.058(8) 0.054(9) 0.026(6) 0.010(8) -0.014(7) C58 0.195(13) 0.30(2) 0.092(12) 0.018(12) -0.012(10) 0.011(14) C59 0.189(11) 0.30(2) 0.087(11) 0.025(11) -0.001(9) 0.009(13) C60 0.171(11) 0.31(2) 0.083(9) 0.011(11) -0.015(9) -0.006(13) C61 0.180(11) 0.31(2) 0.080(8) 0.007(10) -0.004(8) -0.001(13) C62 0.184(11) 0.31(2) 0.085(8) 0.001(10) -0.001(9) -0.006(13) C64 0.056(7) 0.057(7) 0.049(7) 0.021(7) 0.029(6) 0.032(6) C65 0.072(6) 0.053(6) 0.043(5) 0.006(5) 0.017(6) 0.029(5) C67 0.042(6) 0.090(8) 0.066(8) 0.005(7) -0.010(7) 0.011(7) C68 0.052(6) 0.072(6) 0.061(6) 0.014(6) -0.005(6) 0.028(5) C69 0.054(6) 0.069(7) 0.060(6) 0.012(6) -0.009(6) 0.029(6) C70 0.086(6) 0.072(6) 0.060(5) 0.018(5) 0.023(5) -0.015(6) C71 0.081(8) 0.063(6) 0.069(8) 0.029(6) 0.010(7) -0.010(6) C72 0.090(8) 0.083(8) 0.059(8) 0.019(7) 0.023(6) -0.006(7) C73 0.095(8) 0.070(10) 0.059(7) 0.021(8) 0.014(7) -0.008(8) C74 0.052(5) 0.068(5) 0.057(5) 0.019(5) 0.005(5) 0.029(5) C75 0.046(6) 0.079(7) 0.062(6) 0.010(7) -0.004(6) 0.022(6) C76 0.058(8) 0.069(6) 0.068(8) 0.020(7) -0.005(7) 0.030(6) C77 0.048(5) 0.073(6) 0.057(5) 0.017(5) 0.001(5) 0.030(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 C1 C2 1.366(6) . ? C1 C6 1.370(6) . ? C1 O1 1.383(5) . ? C2 C3 1.379(6) . ? C2 O2 1.383(5) . ? C3 C4 1.390(6) . ? C3 H3 0.9500 . ? C4 C5 1.390(6) . ? C4 C7 1.529(6) . ? C4 C74 1.534(8) . ? C4 C66 1.534(8) . ? C5 C6 1.389(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C9 1.536(6) . ? C7 C8 1.536(6) . ? C7 C10 1.543(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.371(6) . ? C11 C16 1.375(6) . ? C11 O3 1.380(5) . ? C12 C13 1.365(6) . ? C12 O4 1.381(4) . ? C13 C14 1.407(5) . ? C13 H13 0.9500 . ? C14 C15 1.386(6) . ? C14 C17 1.533(6) . ? C14 C50 1.537(8) . ? C15 C16 1.383(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.529(6) . ? C17 C20 1.537(6) . ? C17 C19 1.539(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.367(6) . ? C21 C22 1.378(6) . ? C21 O5 1.386(5) . ? C22 C23 1.373(6) . ? C22 O6 1.374(5) . ? C23 C24 1.397(6) . ? C23 H23 0.9500 . ? C24 C25 1.395(7) . ? C24 C70 1.534(8) . ? C24 C27 1.535(7) . ? C24 C54 1.540(8) . ? C25 C26 1.395(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C30 1.534(7) . ? C27 C28 1.541(7) . ? C27 C29 1.541(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.531(6) . ? C31 P2 1.850(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 P1 1.835(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.509(7) . ? C33 C35 1.521(7) . ? C33 P2 1.853(5) . ? C33 H33A 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.528(7) . ? C36 C38 1.540(7) . ? C36 P2 1.856(5) . ? C36 H36A 1.0000 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.522(7) . ? C39 C41 1.526(6) . ? C39 P1 1.845(5) . ? C39 H39A 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.510(6) . ? C42 C43 1.512(6) . ? C42 P1 1.860(5) . ? C42 H42A 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? B1 O2 1.411(6) . ? B1 O1 1.415(5) . ? B1 Ir1 1.979(5) . ? B2 O4 1.417(5) . ? B2 O3 1.418(5) . ? B2 Ir1 2.075(5) . ? B3 O6 1.423(6) . ? B3 O5 1.430(6) . ? B3 Ir1 2.070(5) . ? P2 Ir1 2.3678(12) . ? P1 C63 1.853(10) . ? P1 Ir1 2.3651(11) . ? C45 C46 1.545(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 C47 1.512(9) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.542(9) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.500(9) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C53 1.538(7) . ? C50 C51 1.540(7) . ? C50 C52 1.540(7) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C57 1.539(7) . ? C54 C55 1.541(7) . ? C54 C56 1.544(7) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 C59 1.520(10) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.547(10) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.531(10) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.537(10) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.505(9) . ? C63 C65 1.508(9) . ? C63 H63A 1.0000 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C68 1.538(7) . ? C66 C69 1.538(7) . ? C66 C67 1.539(7) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C73 1.537(7) . ? C70 C71 1.538(7) . ? C70 C72 1.541(7) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 C76 1.537(7) . ? C74 C77 1.537(7) . ? C74 C75 1.538(7) . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 121.9(4) . . ? C2 C1 O1 109.5(4) . . ? C6 C1 O1 128.6(4) . . ? C1 C2 C3 121.7(4) . . ? C1 C2 O2 109.7(4) . . ? C3 C2 O2 128.6(4) . . ? C2 C3 C4 118.4(4) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 118.4(4) . . ? C3 C4 C7 123.5(4) . . ? C5 C4 C7 118.0(4) . . ? C3 C4 C74 117.8(8) . . ? C5 C4 C74 123.7(8) . . ? C3 C4 C66 118.9(8) . . ? C5 C4 C66 122.7(8) . . ? C6 C5 C4 123.3(4) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C1 C6 C5 116.2(4) . . ? C1 C6 H6 121.9 . . ? C5 C6 H6 121.9 . . ? C4 C7 C9 110.1(5) . . ? C4 C7 C8 112.3(5) . . ? C9 C7 C8 108.7(6) . . ? C4 C7 C10 109.1(5) . . ? C9 C7 C10 108.2(6) . . ? C8 C7 C10 108.4(6) . . ? C12 C11 C16 120.8(4) . . ? C12 C11 O3 109.4(4) . . ? C16 C11 O3 129.7(4) . . ? C13 C12 C11 122.0(4) . . ? C13 C12 O4 128.7(4) . . ? C11 C12 O4 109.2(3) . . ? C12 C13 C14 118.9(4) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C15 C14 C13 117.7(4) . . ? C15 C14 C17 119.8(4) . . ? C13 C14 C17 122.5(4) . . ? C15 C14 C50 121.9(6) . . ? C13 C14 C50 120.3(6) . . ? C16 C15 C14 123.2(4) . . ? C16 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C11 C16 C15 117.3(4) . . ? C11 C16 H16 121.3 . . ? C15 C16 H16 121.3 . . ? C18 C17 C14 112.4(5) . . ? C18 C17 C20 108.9(5) . . ? C14 C17 C20 109.5(5) . . ? C18 C17 C19 107.9(5) . . ? C14 C17 C19 110.0(5) . . ? C20 C17 C19 108.2(5) . . ? C26 C21 C22 120.1(4) . . ? C26 C21 O5 130.9(4) . . ? C22 C21 O5 109.0(4) . . ? C23 C22 O6 127.1(4) . . ? C23 C22 C21 123.2(4) . . ? O6 C22 C21 109.6(4) . . ? C22 C23 C24 118.3(5) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C25 C24 C23 117.6(4) . . ? C25 C24 C70 115.0(9) . . ? C23 C24 C70 127.3(9) . . ? C25 C24 C27 119.6(5) . . ? C23 C24 C27 122.5(5) . . ? C25 C24 C54 128.0(6) . . ? C23 C24 C54 114.1(6) . . ? C24 C25 C26 123.6(5) . . ? C24 C25 H25 118.2 . . ? C26 C25 H25 118.2 . . ? C21 C26 C25 117.1(5) . . ? C21 C26 H26 121.4 . . ? C25 C26 H26 121.4 . . ? C30 C27 C24 110.8(6) . . ? C30 C27 C28 108.1(7) . . ? C24 C27 C28 111.2(6) . . ? C30 C27 C29 109.6(7) . . ? C24 C27 C29 108.4(6) . . ? C28 C27 C29 108.6(7) . . ? C32 C31 P2 113.1(3) . . ? C32 C31 H31A 109.0 . . ? P2 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? P2 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 P1 112.9(3) . . ? C31 C32 H32A 109.0 . . ? P1 C32 H32A 109.0 . . ? C31 C32 H32B 109.0 . . ? P1 C32 H32B 109.0 . . ? H32A C32 H32B 107.8 . . ? C34 C33 C35 110.3(5) . . ? C34 C33 P2 112.5(4) . . ? C35 C33 P2 110.6(3) . . ? C34 C33 H33A 107.7 . . ? C35 C33 H33A 107.7 . . ? P2 C33 H33A 107.7 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C38 107.1(4) . . ? C37 C36 P2 112.1(3) . . ? C38 C36 P2 114.9(4) . . ? C37 C36 H36A 107.5 . . ? C38 C36 H36A 107.5 . . ? P2 C36 H36A 107.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C41 110.4(4) . . ? C40 C39 P1 117.3(4) . . ? C41 C39 P1 108.9(3) . . ? C40 C39 H39A 106.5 . . ? C41 C39 H39A 106.5 . . ? P1 C39 H39A 106.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 114.3(5) . . ? C44 C42 P1 114.8(4) . . ? C43 C42 P1 111.6(4) . . ? C44 C42 H42A 105.0 . . ? C43 C42 H42A 105.0 . . ? P1 C42 H42A 105.0 . . ? O2 B1 O1 108.6(4) . . ? O2 B1 Ir1 127.8(3) . . ? O1 B1 Ir1 123.6(3) . . ? O4 B2 O3 107.3(4) . . ? O4 B2 Ir1 132.6(3) . . ? O3 B2 Ir1 119.6(3) . . ? O6 B3 O5 106.8(4) . . ? O6 B3 Ir1 126.1(3) . . ? O5 B3 Ir1 126.9(3) . . ? C1 O1 B1 106.1(3) . . ? C2 O2 B1 106.1(3) . . ? C11 O3 B2 106.9(3) . . ? C12 O4 B2 107.0(3) . . ? C21 O5 B3 106.9(3) . . ? C22 O6 B3 107.3(3) . . ? C31 P2 C33 101.7(2) . . ? C31 P2 C36 104.8(2) . . ? C33 P2 C36 103.3(2) . . ? C31 P2 Ir1 108.24(15) . . ? C33 P2 Ir1 120.21(18) . . ? C36 P2 Ir1 116.56(16) . . ? C32 P1 C39 107.4(2) . . ? C32 P1 C63 101.2(8) . . ? C39 P1 C63 94.0(8) . . ? C32 P1 C42 102.6(2) . . ? C39 P1 C42 108.6(3) . . ? C32 P1 Ir1 109.73(15) . . ? C39 P1 Ir1 104.33(15) . . ? C63 P1 Ir1 136.8(9) . . ? C42 P1 Ir1 123.48(18) . . ? B1 Ir1 B3 82.5(2) . . ? B1 Ir1 B2 92.23(19) . . ? B3 Ir1 B2 90.18(19) . . ? B1 Ir1 P1 99.92(15) . . ? B3 Ir1 P1 92.79(14) . . ? B2 Ir1 P1 167.77(13) . . ? B1 Ir1 P2 96.72(15) . . ? B3 Ir1 P2 176.80(14) . . ? B2 Ir1 P2 92.95(14) . . ? P1 Ir1 P2 84.29(4) . . ? C47 C46 C45 109.0(12) . . ? C47 C46 H46A 109.9 . . ? C45 C46 H46A 109.9 . . ? C47 C46 H46B 109.9 . . ? C45 C46 H46B 109.9 . . ? H46A C46 H46B 108.3 . . ? C46 C47 C48 107.4(12) . . ? C46 C47 H47A 110.2 . . ? C48 C47 H47A 110.2 . . ? C46 C47 H47B 110.2 . . ? C48 C47 H47B 110.2 . . ? H47A C47 H47B 108.5 . . ? C49 C48 C47 107.3(12) . . ? C49 C48 H48A 110.2 . . ? C47 C48 H48A 110.3 . . ? C49 C48 H48B 110.2 . . ? C47 C48 H48B 110.2 . . ? H48A C48 H48B 108.5 . . ? C14 C50 C53 109.9(8) . . ? C14 C50 C51 109.7(7) . . ? C53 C50 C51 110.2(13) . . ? C14 C50 C52 110.6(8) . . ? C53 C50 C52 108.3(8) . . ? C51 C50 C52 108.1(8) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C53 H53A 109.5 . . ? C50 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C50 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C57 C54 C24 110.4(8) . . ? C57 C54 C55 108.2(8) . . ? C24 C54 C55 111.2(8) . . ? C57 C54 C56 107.5(8) . . ? C24 C54 C56 112.6(8) . . ? C55 C54 C56 106.7(8) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C59 C58 H58A 109.4 . . ? C59 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C59 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C58 C59 C60 105.0(13) . . ? C58 C59 H59A 110.7 . . ? C60 C59 H59A 110.7 . . ? C58 C59 H59B 110.8 . . ? C60 C59 H59B 110.8 . . ? H59A C59 H59B 108.8 . . ? C61 C60 C59 104.7(13) . . ? C61 C60 H60A 110.8 . . ? C59 C60 H60A 110.8 . . ? C61 C60 H60B 110.8 . . ? C59 C60 H60B 110.8 . . ? H60A C60 H60B 108.9 . . ? C60 C61 C62 106.6(12) . . ? C60 C61 H61A 110.4 . . ? C62 C61 H61A 110.4 . . ? C60 C61 H61B 110.4 . . ? C62 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? C61 C62 H62A 109.4 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C65 115.6(15) . . ? C64 C63 P1 113.2(11) . . ? C65 C63 P1 111.8(11) . . ? C64 C63 H63A 105.0 . . ? C65 C63 H63A 105.0 . . ? P1 C63 H63A 105.0 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C63 C65 H65A 109.5 . . ? C63 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C63 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C4 C66 C68 110.9(9) . . ? C4 C66 C69 111.0(9) . . ? C68 C66 C69 107.8(9) . . ? C4 C66 C67 110.3(9) . . ? C68 C66 C67 108.7(9) . . ? C69 C66 C67 108.0(9) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C66 C69 H69A 109.5 . . ? C66 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C66 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C24 C70 C73 110.2(9) . . ? C24 C70 C71 110.9(9) . . ? C73 C70 C71 108.9(9) . . ? C24 C70 C72 110.2(9) . . ? C73 C70 C72 108.7(9) . . ? C71 C70 C72 107.9(9) . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C4 C74 C76 109.9(9) . . ? C4 C74 C77 110.4(9) . . ? C76 C74 C77 108.7(9) . . ? C4 C74 C75 110.8(9) . . ? C76 C74 C75 108.9(9) . . ? C77 C74 C75 108.2(9) . . ? C74 C75 H75A 109.5 . . ? C74 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C74 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C74 C76 H76A 109.5 . . ? C74 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C74 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C74 C77 H77A 109.5 . . ? C74 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C74 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.468 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.104