Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'John D. Kennedy' _publ_contact_author_email J.D.KENNEDY@LEEDS.AC.UK _publ_section_title ; Macropolyhedral boron-containing cluster chemistry. Cluster opening and B-frame rearrangement in the reaction of B16H20 with [{(IrCl2(?5-C5Me5)}2]. Synchrotron X-ray structures of [(eta-5-C5Me5)2Ir2B16H17Cl] and [(eta-5-C5Me5)2Ir2B16H15Cl]. ; loop_ _publ_author_name 'Michael J. Carr' 'Sarath D. Perera' 'Toma Jelinek' 'Colin A. Kilner' 'William Clegg' 'Bohumil Stibr' ; J.D.Kennedy ; # Attachment 'B611734A CCDC 286252.CIF' data_leeds61 _database_code_depnum_ccdc_archive 'CCDC 286252' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H49 B16 Cl Ir2' _chemical_formula_sum 'C20 H49 B16 Cl Ir2' _chemical_formula_weight 882.40 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6181(18) _cell_length_b 12.059(2) _cell_length_c 16.523(3) _cell_angle_alpha 73.335(3) _cell_angle_beta 73.499(3) _cell_angle_gamma 72.360(2) _cell_volume 1885.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 7.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7169 _exptl_absorpt_correction_T_max 0.8705 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68400 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12868 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0650 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6845 _reflns_number_gt 5605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material ; 'enCIFer (CCDC, 2002)' ; _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. One disordered chloroform solvent molecule was not modelled and the disordered density was taken into account using SQUEEZE/PLATON (Spek, 2003) ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.6422P] 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 6845 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 Ir7' Ir 1.20584(3) 1.19833(2) 0.803472(17) 0.03644(11) Uani 1 1 d . A . Ir9 Ir 1.48636(3) 0.73962(2) 0.78029(2) 0.04378(11) Uani 1 1 d . . . Cl2' Cl 1.3678(3) 1.0397(2) 0.63794(14) 0.0541(6) Uani 0.91 1 d P A 1 C11 C 1.6087(13) 0.6366(13) 0.6822(9) 0.088(4) Uani 1 1 d . . . C12 C 1.6642(12) 0.7320(11) 0.6718(7) 0.092(4) Uani 1 1 d . . . C13 C 1.7069(10) 0.7148(10) 0.7545(9) 0.073(3) Uani 1 1 d . . . C14 C 1.6692(9) 0.6066(8) 0.8078(6) 0.058(2) Uani 1 1 d . . . C15 C 1.6138(11) 0.5645(8) 0.7601(10) 0.080(3) Uani 1 1 d . . . C16 C 1.555(2) 0.620(3) 0.6128(14) 0.242(17) Uani 1 1 d . . . H16A H 1.4571 0.6538 0.6222 0.363 Uiso 1 1 calc R . . H16B H 1.5739 0.5343 0.6147 0.363 Uiso 1 1 calc R . . H16C H 1.5992 0.6598 0.5561 0.363 Uiso 1 1 calc R . . C17 C 1.683(2) 0.826(2) 0.5935(12) 0.236(17) Uani 1 1 d . . . H17A H 1.7690 0.7991 0.5548 0.354 Uiso 1 1 calc R . . H17B H 1.6824 0.8982 0.6092 0.354 Uiso 1 1 calc R . . H17C H 1.6084 0.8426 0.5641 0.354 Uiso 1 1 calc R . . C18 C 1.7759(12) 0.7878(16) 0.7807(15) 0.154(9) Uani 1 1 d . . . H18A H 1.7084 0.8391 0.8173 0.231 Uiso 1 1 calc R . . H18B H 1.8202 0.8374 0.7289 0.231 Uiso 1 1 calc R . . H18C H 1.8438 0.7343 0.8131 0.231 Uiso 1 1 calc R . . C19 C 1.6988(14) 0.5514(14) 0.8951(8) 0.110(5) Uani 1 1 d . . . H19A H 1.6328 0.5046 0.9295 0.166 Uiso 1 1 calc R . . H19B H 1.6928 0.6140 0.9239 0.166 Uiso 1 1 calc R . . H19C H 1.7901 0.4990 0.8897 0.166 Uiso 1 1 calc R . . C20 C 1.5608(15) 0.4478(11) 0.7967(16) 0.152(8) Uani 1 1 d . . . H20A H 1.6342 0.3793 0.7826 0.228 Uiso 1 1 calc R . . H20B H 1.4857 0.4551 0.7707 0.228 Uiso 1 1 calc R . . H20C H 1.5295 0.4361 0.8596 0.228 Uiso 1 1 calc R . . C21 C 1.3423(9) 1.3207(7) 0.7247(5) 0.051(2) Uani 1 1 d . . . C22 C 1.2264(9) 1.3840(7) 0.7789(5) 0.0481(18) Uani 1 1 d . . . C23 C 1.2274(9) 1.3305(7) 0.8652(5) 0.0453(17) Uani 1 1 d . . . C24 C 1.3471(9) 1.2307(7) 0.8679(5) 0.0500(19) Uani 1 1 d . . . C25 C 1.4162(9) 1.2271(8) 0.7810(6) 0.052(2) Uani 1 1 d . . . C26 C 1.3840(13) 1.3536(10) 0.6284(6) 0.075(3) Uani 1 1 d . . . H26A H 1.4579 1.3940 0.6121 0.112 Uiso 1 1 calc R . . H26B H 1.3068 1.4072 0.6046 0.112 Uiso 1 1 calc R . . H26C H 1.4148 1.2813 0.6053 0.112 Uiso 1 1 calc R . . C27 C 1.1290(12) 1.4987(8) 0.7451(7) 0.070(3) Uani 1 1 d . . . H27A H 1.0395 1.5037 0.7841 0.106 Uiso 1 1 calc R . . H27B H 1.1221 1.4991 0.6871 0.106 Uiso 1 1 calc R . . H27C H 1.1625 1.5672 0.7424 0.106 Uiso 1 1 calc R . . C28 C 1.1313(10) 1.3746(9) 0.9430(6) 0.061(2) Uani 1 1 d . . . H28A H 1.1719 1.4230 0.9621 0.092 Uiso 1 1 calc R . . H28B H 1.1141 1.3062 0.9901 0.092 Uiso 1 1 calc R . . H28C H 1.0458 1.4232 0.9272 0.092 Uiso 1 1 calc R . . C29 C 1.3944(11) 1.1536(9) 0.9483(6) 0.068(3) Uani 1 1 d . . . H29A H 1.4609 1.0813 0.9345 0.101 Uiso 1 1 calc R . . H29B H 1.3170 1.1315 0.9925 0.101 Uiso 1 1 calc R . . H29C H 1.4363 1.1978 0.9703 0.101 Uiso 1 1 calc R . . C30 C 1.5523(9) 1.1473(9) 0.7520(7) 0.068(3) Uani 1 1 d . . . H30A H 1.5524 1.1225 0.7005 0.102 Uiso 1 1 calc R . . H30B H 1.5702 1.0768 0.7985 0.102 Uiso 1 1 calc R . . H30C H 1.6227 1.1909 0.7382 0.102 Uiso 1 1 calc R . . B1 B 1.1906(11) 0.7693(8) 0.9311(9) 0.064(3) Uani 1 1 d . A . H1 H 1.1411 0.7129 0.9911 0.077 Uiso 1 1 calc R . . B1' B 1.0668(12) 1.0783(9) 0.7009(8) 0.060(3) Uani 1 1 d . A . H1' H 1.0758 1.0482 0.6409 0.071 Uiso 1 1 calc R . . B2 B 1.0995(10) 0.9174(8) 0.9004(7) 0.053(2) Uani 1 1 d . A . H2 H 1.0010 0.9531 0.9428 0.064 Uiso 1 1 calc R . . B2' B 1.2229(10) 1.0710(8) 0.7269(6) 0.045(2) Uani 1 1 d . . . H2' H 1.3223 1.0492 0.6806 0.054 Uiso 0.09 1 calc PR A 2 B3 B 1.2596(10) 0.8912(8) 0.9279(7) 0.051(2) Uani 1 1 d . . . H3 H 1.2612 0.9240 0.9844 0.061 Uiso 1 1 calc R A . B3' B 1.1072(10) 1.2127(8) 0.7004(6) 0.048(2) Uani 1 1 d . A . H3' H 1.1425 1.2779 0.6408 0.058 Uiso 1 1 calc R . . B4 B 1.3700(11) 0.7480(8) 0.9130(6) 0.052(2) Uani 1 1 d . A . H4 H 1.4289 0.6878 0.9622 0.062 Uiso 1 1 calc R . . B4' B 0.9331(10) 1.2009(9) 0.7254(8) 0.057(3) Uani 1 1 d . . . H4' H 0.8651 1.2552 0.6799 0.068 Uiso 1 1 calc R A . B5 B 1.1189(10) 0.8096(8) 0.8422(8) 0.054(2) Uani 1 1 d . . . H5 H 1.0597 0.7773 0.8112 0.064 Uiso 1 1 calc R A . B6 B 1.1162(10) 0.9666(8) 0.7881(7) 0.049(2) Uani 1 1 d . A . B7 B 1.2201(9) 1.0062(7) 0.8388(6) 0.044(2) Uani 1 1 d . A . B8 B 1.4068(9) 0.8879(7) 0.8493(6) 0.0409(19) Uani 1 1 d . A . H8 H 1.4920 0.9337 0.8254 0.049 Uiso 0.91 1 calc PR B 1 B8' B 0.9859(10) 1.2637(8) 0.7930(6) 0.046(2) Uani 1 1 d . A . H8' H 0.9505 1.3400 0.8263 0.056 Uiso 1 1 calc R . . B9' B 0.8615(11) 1.1774(9) 0.8336(9) 0.062(3) Uani 1 1 d . A . B10 B 1.2913(10) 0.6937(8) 0.8541(8) 0.057(3) Uani 1 1 d . A . H10 H 1.2998 0.6107 0.8332 0.068 Uiso 1 1 calc R . . B10' B 0.9302(12) 1.0551(11) 0.7812(10) 0.070(3) Uani 1 1 d . A . H10' H 0.8600 0.9939 0.8047 0.084 Uiso 1 1 calc R . . Cl8 Cl 1.550(2) 0.955(2) 0.8551(14) 0.050(5) Uani 0.09 1 d P A 2 H89' H 0.929(9) 1.207(8) 0.862(5) 0.05(2) Uiso 1 1 d . . . H89 H 1.422(10) 0.886(9) 0.779(6) 0.07(3) Uiso 1 1 d . . . H91' H 0.894(12) 1.070(10) 0.857(7) 0.08(3) Uiso 1 1 d . . . H58 H 1.162(10) 0.836(9) 0.786(6) 0.06(3) Uiso 1 1 d . . . H67' H 1.148(9) 1.118(7) 0.868(5) 0.05(2) Uiso 1 1 d . . . H91 H 1.335(15) 0.735(13) 0.775(9) 0.13(5) Uiso 1 1 d . . . H9' H 0.755(8) 1.200(6) 0.866(4) 0.033(18) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir7' 0.03526(17) 0.02862(16) 0.04473(17) -0.00813(11) -0.01470(12) -0.00094(11) Ir9 0.04276(19) 0.02997(16) 0.0600(2) -0.01313(13) -0.02162(14) 0.00216(12) Cl2' 0.0596(14) 0.0463(12) 0.0497(11) -0.0135(9) -0.0206(10) 0.0077(10) C11 0.074(8) 0.092(9) 0.099(9) -0.053(8) -0.029(7) 0.016(7) C12 0.069(7) 0.078(8) 0.070(6) 0.013(6) 0.009(6) 0.020(6) C13 0.040(5) 0.065(6) 0.127(9) -0.054(6) -0.015(5) -0.002(4) C14 0.040(5) 0.046(5) 0.070(5) -0.012(4) -0.014(4) 0.014(4) C15 0.062(7) 0.035(5) 0.150(11) -0.042(6) -0.033(7) 0.009(4) C16 0.150(18) 0.39(4) 0.23(2) -0.27(3) -0.109(17) 0.12(2) C17 0.124(15) 0.21(2) 0.141(14) 0.096(15) 0.063(12) 0.077(15) C18 0.035(6) 0.140(13) 0.34(3) -0.151(16) -0.014(10) -0.020(7) C19 0.079(9) 0.122(11) 0.098(9) -0.013(8) -0.038(7) 0.028(8) C20 0.071(9) 0.056(7) 0.35(3) -0.088(12) -0.050(13) 0.008(6) C21 0.055(5) 0.043(4) 0.056(4) -0.017(4) 0.000(4) -0.021(4) C22 0.048(5) 0.040(4) 0.061(5) -0.016(4) -0.013(4) -0.011(4) C23 0.049(5) 0.044(4) 0.052(4) -0.020(3) -0.011(3) -0.016(4) C24 0.050(5) 0.047(5) 0.064(5) -0.017(4) -0.022(4) -0.013(4) C25 0.046(5) 0.051(5) 0.066(5) -0.017(4) -0.019(4) -0.012(4) C26 0.102(9) 0.072(7) 0.053(5) -0.007(5) -0.009(5) -0.037(6) C27 0.092(8) 0.032(4) 0.091(7) -0.005(4) -0.043(6) -0.007(5) C28 0.063(6) 0.058(5) 0.064(5) -0.030(4) -0.008(4) -0.007(4) C29 0.073(7) 0.073(6) 0.058(5) -0.012(4) -0.031(5) -0.004(5) C30 0.042(5) 0.065(6) 0.099(7) -0.036(5) 0.002(5) -0.013(4) B1 0.050(6) 0.027(4) 0.105(8) 0.002(5) -0.023(6) -0.001(4) B1' 0.061(6) 0.039(5) 0.084(7) -0.019(5) -0.041(6) 0.009(4) B2 0.040(5) 0.035(5) 0.083(7) -0.008(4) -0.021(5) -0.003(4) B2' 0.052(5) 0.032(4) 0.059(5) -0.018(4) -0.028(4) 0.002(4) B3 0.046(5) 0.034(4) 0.067(6) 0.001(4) -0.019(4) -0.007(4) B3' 0.048(5) 0.035(4) 0.060(5) -0.008(4) -0.029(4) 0.008(4) B4 0.056(6) 0.029(4) 0.062(5) -0.005(4) -0.015(4) -0.001(4) B4' 0.045(5) 0.040(5) 0.093(7) -0.016(5) -0.038(5) 0.003(4) B5 0.040(5) 0.028(4) 0.093(8) -0.007(5) -0.024(5) -0.006(4) B6 0.043(5) 0.031(4) 0.080(6) -0.015(4) -0.027(5) -0.001(4) B7 0.038(4) 0.033(4) 0.054(5) -0.012(4) -0.015(4) 0.007(4) B8 0.041(5) 0.029(4) 0.049(4) -0.010(3) -0.013(4) 0.002(3) B8' 0.043(5) 0.035(4) 0.060(5) -0.010(4) -0.023(4) 0.003(4) B9' 0.034(5) 0.043(5) 0.109(9) -0.014(5) -0.025(5) 0.001(4) B10 0.037(5) 0.028(4) 0.104(8) -0.006(5) -0.024(5) -0.007(4) B10' 0.050(6) 0.052(6) 0.117(10) -0.020(6) -0.041(7) -0.003(5) Cl8 0.034(11) 0.071(15) 0.050(11) -0.030(11) -0.022(9) 0.006(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir7' B3' 2.183(9) . ? Ir7' B7 2.189(9) . ? Ir7' B2' 2.193(8) . ? Ir7' C23 2.218(7) . ? Ir7' C22 2.225(8) . ? Ir7' C24 2.244(8) . ? Ir7' C21 2.257(8) . ? Ir7' B8' 2.268(9) . ? Ir7' C25 2.275(9) . ? Ir7' H67' 1.36(8) . ? Ir9 C14 2.178(8) . ? Ir9 C15 2.195(8) . ? Ir9 C13 2.199(10) . ? Ir9 C11 2.199(11) . ? Ir9 C12 2.204(10) . ? Ir9 B4 2.204(10) . ? Ir9 B8 2.218(8) . ? Ir9 B10 2.226(10) . ? Ir9 H89 1.69(10) . ? Ir9 H91 1.65(15) . ? Cl2' B2' 1.830(10) . ? C11 C15 1.337(18) . ? C11 C12 1.393(19) . ? C11 C16 1.503(19) . ? C12 C17 1.462(17) . ? C12 C13 1.500(18) . ? C13 C14 1.447(15) . ? C13 C18 1.514(16) . ? C14 C15 1.378(15) . ? C14 C19 1.484(14) . ? C15 C20 1.569(18) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.426(12) . ? C21 C22 1.448(11) . ? C21 C26 1.493(12) . ? C22 C23 1.389(11) . ? C22 C27 1.520(12) . ? C23 C24 1.462(12) . ? C23 C28 1.515(11) . ? C24 C25 1.422(12) . ? C24 C29 1.507(12) . ? C25 C30 1.507(12) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 . ? B1 B10 1.702(17) . ? B1 B5 1.724(17) . ? B1 B2 1.759(12) . ? B1 B4 1.791(15) . ? B1 B3 1.814(15) . ? B1 H1 1.1200 . ? B1' B10' 1.698(19) . ? B1' B6 1.747(14) . ? B1' B4' 1.764(14) . ? B1' B3' 1.795(15) . ? B1' B2' 1.798(14) . ? B1' H1' 1.1200 . ? B2 B6 1.753(15) . ? B2 B5 1.759(15) . ? B2 B3 1.797(14) . ? B2 B7 1.814(14) . ? B2 H2 1.1200 . ? B2' B7 1.786(13) . ? B2' B3' 1.796(12) . ? B2' B6 1.837(14) . ? B2' H2' 1.1200 . ? B3 B8 1.722(13) . ? B3 B7 1.759(12) . ? B3 B4 1.808(13) . ? B3 H3 1.1200 . ? B3' B4' 1.816(15) . ? B3' B8' 1.822(14) . ? B3' H3' 1.1200 . ? B4 B10 1.799(15) . ? B4 B8 1.804(13) . ? B4 H4 1.1200 . ? B4' B9' 1.709(18) . ? B4' B10' 1.740(16) . ? B4' B8' 1.798(14) . ? B4' H4' 1.1200 . ? B5 B6 1.842(13) . ? B5 B10 1.960(13) . ? B5 H5 1.1200 . ? B5 H58 0.92(9) . ? B6 B7 1.796(14) . ? B6 B10' 1.958(15) . ? B6 H58 1.51(10) . ? B7 B8 2.082(12) . ? B7 H67' 1.48(8) . ? B8 Cl8 1.96(3) . ? B8 H8 1.1200 . ? B8 H89 1.14(9) . ? B8' B9' 1.791(15) . ? B8' H8' 1.1200 . ? B8' H89' 1.24(8) . ? B9' B10' 1.783(17) . ? B9' H89' 1.14(9) . ? B9' H91' 1.21(11) . ? B9' H9' 1.09(7) . ? B10 H10 1.1200 . ? B10 H91 1.26(13) . ? B10' H10' 1.1200 . ? B10' H91' 1.26(10) . ? 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 B3' Ir7' B7 88.8(3) . . ? B3' Ir7' B2' 48.5(3) . . ? B7 Ir7' B2' 48.1(3) . . ? B3' Ir7' C23 133.6(3) . . ? B7 Ir7' C23 135.7(3) . . ? B2' Ir7' C23 168.9(4) . . ? B3' Ir7' C22 101.2(3) . . ? B7 Ir7' C22 168.8(3) . . ? B2' Ir7' C22 137.5(3) . . ? C23 Ir7' C22 36.4(3) . . ? B3' Ir7' C24 158.1(4) . . ? B7 Ir7' C24 107.0(3) . . ? B2' Ir7' C24 134.5(3) . . ? C23 Ir7' C24 38.2(3) . . ? C22 Ir7' C24 62.0(3) . . ? B3' Ir7' C21 96.2(4) . . ? B7 Ir7' C21 137.0(3) . . ? B2' Ir7' C21 107.6(3) . . ? C23 Ir7' C21 62.3(3) . . ? C22 Ir7' C21 37.7(3) . . ? C24 Ir7' C21 61.8(3) . . ? B3' Ir7' B8' 48.3(4) . . ? B7 Ir7' B8' 98.7(3) . . ? B2' Ir7' B8' 86.1(4) . . ? C23 Ir7' B8' 102.2(3) . . ? C22 Ir7' B8' 91.7(3) . . ? C24 Ir7' B8' 139.3(3) . . ? C21 Ir7' B8' 116.3(3) . . ? B3' Ir7' C25 124.3(4) . . ? B7 Ir7' C25 108.4(3) . . ? B2' Ir7' C25 107.0(4) . . ? C23 Ir7' C25 62.3(3) . . ? C22 Ir7' C25 61.8(3) . . ? C24 Ir7' C25 36.7(3) . . ? C21 Ir7' C25 36.7(3) . . ? B8' Ir7' C25 152.1(3) . . ? B3' Ir7' H67' 101(4) . . ? B7 Ir7' H67' 41(3) . . ? B2' Ir7' H67' 82(3) . . ? C23 Ir7' H67' 107(3) . . ? C22 Ir7' H67' 139(3) . . ? C24 Ir7' H67' 101(4) . . ? C21 Ir7' H67' 163(4) . . ? B8' Ir7' H67' 78(4) . . ? C25 Ir7' H67' 128(4) . . ? C14 Ir9 C15 36.7(4) . . ? C14 Ir9 C13 38.6(4) . . ? C15 Ir9 C13 62.6(4) . . ? C14 Ir9 C11 61.7(4) . . ? C15 Ir9 C11 35.4(5) . . ? C13 Ir9 C11 63.5(5) . . ? C14 Ir9 C12 64.1(4) . . ? C15 Ir9 C12 61.2(5) . . ? C13 Ir9 C12 39.8(5) . . ? C11 Ir9 C12 36.9(5) . . ? C14 Ir9 B4 100.2(3) . . ? C15 Ir9 B4 116.5(5) . . ? C13 Ir9 B4 117.9(4) . . ? C11 Ir9 B4 150.8(5) . . ? C12 Ir9 B4 157.5(5) . . ? C14 Ir9 B8 118.4(4) . . ? C15 Ir9 B8 153.8(4) . . ? C13 Ir9 B8 103.1(4) . . ? C11 Ir9 B8 159.6(5) . . ? C12 Ir9 B8 123.0(5) . . ? B4 Ir9 B8 48.1(3) . . ? C14 Ir9 B10 116.0(4) . . ? C15 Ir9 B10 101.3(4) . . ? C13 Ir9 B10 153.6(4) . . ? C11 Ir9 B10 116.6(5) . . ? C12 Ir9 B10 152.3(6) . . ? B4 Ir9 B10 47.9(4) . . ? B8 Ir9 B10 82.4(4) . . ? C14 Ir9 H89 136(4) . . ? C15 Ir9 H89 166(3) . . ? C13 Ir9 H89 105(4) . . ? C11 Ir9 H89 134(3) . . ? C12 Ir9 H89 105(3) . . ? B4 Ir9 H89 75(3) . . ? B8 Ir9 H89 30(3) . . ? B10 Ir9 H89 93(3) . . ? C14 Ir9 H91 135(5) . . ? C15 Ir9 H91 104(5) . . ? C13 Ir9 H91 162(5) . . ? C11 Ir9 H91 99(5) . . ? C12 Ir9 H91 125(5) . . ? B4 Ir9 H91 78(5) . . ? B8 Ir9 H91 94(5) . . ? B10 Ir9 H91 34(5) . . ? H89 Ir9 H91 87(6) . . ? C15 C11 C12 110.3(11) . . ? C15 C11 C16 126.7(19) . . ? C12 C11 C16 123.0(18) . . ? C15 C11 Ir9 72.1(6) . . ? C12 C11 Ir9 71.7(6) . . ? C16 C11 Ir9 124.0(9) . . ? C11 C12 C17 126.1(19) . . ? C11 C12 C13 106.1(9) . . ? C17 C12 C13 127.7(19) . . ? C11 C12 Ir9 71.4(7) . . ? C17 C12 Ir9 125.8(9) . . ? C13 C12 Ir9 69.9(5) . . ? C14 C13 C12 104.3(9) . . ? C14 C13 C18 125.2(14) . . ? C12 C13 C18 130.6(15) . . ? C14 C13 Ir9 69.9(5) . . ? C12 C13 Ir9 70.2(6) . . ? C18 C13 Ir9 124.4(7) . . ? C15 C14 C13 107.7(9) . . ? C15 C14 C19 128.8(12) . . ? C13 C14 C19 123.3(11) . . ? C15 C14 Ir9 72.3(5) . . ? C13 C14 Ir9 71.5(5) . . ? C19 C14 Ir9 125.5(7) . . ? C11 C15 C14 111.5(11) . . ? C11 C15 C20 125.9(14) . . ? C14 C15 C20 122.5(13) . . ? C11 C15 Ir9 72.5(6) . . ? C14 C15 Ir9 71.0(5) . . ? C20 C15 Ir9 122.4(8) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 107.0(7) . . ? C25 C21 C26 126.1(9) . . ? C22 C21 C26 126.7(9) . . ? C25 C21 Ir7' 72.3(5) . . ? C22 C21 Ir7' 69.9(4) . . ? C26 C21 Ir7' 127.1(7) . . ? C23 C22 C21 109.3(7) . . ? C23 C22 C27 126.1(8) . . ? C21 C22 C27 124.3(8) . . ? C23 C22 Ir7' 71.5(4) . . ? C21 C22 Ir7' 72.4(4) . . ? C27 C22 Ir7' 127.4(7) . . ? C22 C23 C24 107.7(7) . . ? C22 C23 C28 126.5(8) . . ? C24 C23 C28 125.5(8) . . ? C22 C23 Ir7' 72.1(4) . . ? C24 C23 Ir7' 71.9(4) . . ? C28 C23 Ir7' 126.5(6) . . ? C25 C24 C23 107.4(7) . . ? C25 C24 C29 126.5(8) . . ? C23 C24 C29 125.9(8) . . ? C25 C24 Ir7' 72.8(5) . . ? C23 C24 Ir7' 69.9(4) . . ? C29 C24 Ir7' 126.8(7) . . ? C24 C25 C21 108.6(7) . . ? C24 C25 C30 126.4(8) . . ? C21 C25 C30 124.8(8) . . ? C24 C25 Ir7' 70.5(5) . . ? C21 C25 Ir7' 71.0(5) . . ? C30 C25 Ir7' 129.3(6) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? B10 B1 B5 69.8(7) . . ? B10 B1 B2 119.9(9) . . ? B5 B1 B2 60.7(6) . . ? B10 B1 B4 61.9(6) . . ? B5 B1 B4 118.2(9) . . ? B2 B1 B4 115.4(7) . . ? B10 B1 B3 109.3(8) . . ? B5 B1 B3 107.0(7) . . ? B2 B1 B3 60.4(5) . . ? B4 B1 B3 60.2(6) . . ? B10 B1 H1 114.8 . . ? B5 B1 H1 117.0 . . ? B2 B1 H1 116.6 . . ? B4 B1 H1 116.9 . . ? B3 B1 H1 125.5 . . ? B10' B1' B6 69.2(7) . . ? B10' B1' B4' 60.3(7) . . ? B6 B1' B4' 117.1(8) . . ? B10' B1' B3' 110.2(8) . . ? B6 B1' B3' 109.4(7) . . ? B4' B1' B3' 61.4(6) . . ? B10' B1' B2' 120.1(8) . . ? B6 B1' B2' 62.4(6) . . ? B4' B1' B2' 115.0(7) . . ? B3' B1' B2' 60.0(5) . . ? B10' B1' H1' 115.4 . . ? B6 B1' H1' 116.1 . . ? B4' B1' H1' 118.0 . . ? B3' B1' H1' 123.8 . . ? B2' B1' H1' 116.4 . . ? B6 B2 B1 112.9(8) . . ? B6 B2 B5 63.3(6) . . ? B1 B2 B5 58.7(6) . . ? B6 B2 B3 109.8(7) . . ? B1 B2 B3 61.3(6) . . ? B5 B2 B3 106.2(7) . . ? B6 B2 B7 60.4(5) . . ? B1 B2 B7 108.0(7) . . ? B5 B2 B7 106.6(7) . . ? B3 B2 B7 58.3(5) . . ? B6 B2 H2 117.9 . . ? B1 B2 H2 120.1 . . ? B5 B2 H2 122.7 . . ? B3 B2 H2 122.3 . . ? B7 B2 H2 123.3 . . ? B7 B2' B3' 117.3(6) . . ? B7 B2' B1' 110.9(8) . . ? B3' B2' B1' 59.9(5) . . ? B7 B2' Cl2' 125.1(6) . . ? B3' B2' Cl2' 113.4(6) . . ? B1' B2' Cl2' 111.6(6) . . ? B7 B2' B6 59.4(5) . . ? B3' B2' B6 105.4(7) . . ? B1' B2' B6 57.4(6) . . ? Cl2' B2' B6 123.9(6) . . ? B7 B2' Ir7' 65.8(4) . . ? B3' B2' Ir7' 65.5(4) . . ? B1' B2' Ir7' 114.2(5) . . ? Cl2' B2' Ir7' 122.1(5) . . ? B6 B2' Ir7' 110.0(5) . . ? B7 B2' H2' 116.6 . . ? B3' B2' H2' 118.9 . . ? B1' B2' H2' 121.1 . . ? Cl2' B2' H2' 9.7 . . ? B6 B2' H2' 125.7 . . ? Ir7' B2' H2' 115.8 . . ? B8 B3 B7 73.5(6) . . ? B8 B3 B2 121.1(8) . . ? B7 B3 B2 61.3(5) . . ? B8 B3 B4 61.4(5) . . ? B7 B3 B4 121.1(7) . . ? B2 B3 B4 112.7(7) . . ? B8 B3 B1 108.7(7) . . ? B7 B3 B1 108.1(7) . . ? B2 B3 B1 58.3(5) . . ? B4 B3 B1 59.3(6) . . ? B8 B3 H3 113.4 . . ? B7 B3 H3 113.7 . . ? B2 B3 H3 118.2 . . ? B4 B3 H3 117.7 . . ? B1 B3 H3 127.0 . . ? B1' B3' B2' 60.1(5) . . ? B1' B3' B4' 58.5(6) . . ? B2' B3' B4' 112.5(7) . . ? B1' B3' B8' 103.8(7) . . ? B2' B3' B8' 114.7(6) . . ? B4' B3' B8' 59.2(6) . . ? B1' B3' Ir7' 114.8(5) . . ? B2' B3' Ir7' 66.1(4) . . ? B4' B3' Ir7' 120.6(6) . . ? B8' B3' Ir7' 68.3(4) . . ? B1' B3' H3' 124.9 . . ? B2' B3' H3' 117.6 . . ? B4' B3' H3' 118.7 . . ? B8' B3' H3' 120.9 . . ? Ir7' B3' H3' 110.8 . . ? B1 B4 B10 56.6(6) . . ? B1 B4 B8 106.2(6) . . ? B10 B4 B8 108.8(7) . . ? B1 B4 B3 60.5(6) . . ? B10 B4 B3 105.3(7) . . ? B8 B4 B3 57.0(5) . . ? B1 B4 Ir9 116.5(7) . . ? B10 B4 Ir9 66.7(5) . . ? B8 B4 Ir9 66.3(4) . . ? B3 B4 Ir9 116.1(6) . . ? B1 B4 H4 121.8 . . ? B10 B4 H4 122.9 . . ? B8 B4 H4 122.5 . . ? B3 B4 H4 122.2 . . ? Ir9 B4 H4 111.3 . . ? B9' B4' B10' 62.2(7) . . ? B9' B4' B1' 111.1(8) . . ? B10' B4' B1' 58.0(7) . . ? B9' B4' B8' 61.4(6) . . ? B10' B4' B8' 105.8(8) . . ? B1' B4' B8' 106.1(7) . . ? B9' B4' B3' 113.6(7) . . ? B10' B4' B3' 107.3(7) . . ? B1' B4' B3' 60.2(6) . . ? B8' B4' B3' 60.5(5) . . ? B9' B4' H4' 117.2 . . ? B10' B4' H4' 123.4 . . ? B1' B4' H4' 122.5 . . ? B8' B4' H4' 123.3 . . ? B3' B4' H4' 119.9 . . ? B1 B5 B2 60.7(6) . . ? B1 B5 B6 110.3(7) . . ? B2 B5 B6 58.2(5) . . ? B1 B5 B10 54.6(6) . . ? B2 B5 B10 107.3(7) . . ? B6 B5 B10 120.2(7) . . ? B1 B5 H5 141.1 . . ? B2 B5 H5 141.0 . . ? B6 B5 H5 107.8 . . ? B10 B5 H5 110.6 . . ? B1 B5 H58 125(6) . . ? B2 B5 H58 108(6) . . ? B6 B5 H58 55(6) . . ? B10 B5 H58 86(6) . . ? H5 B5 H58 84.0 . . ? B1' B6 B2 148.1(7) . . ? B1' B6 B7 112.9(7) . . ? B2 B6 B7 61.5(6) . . ? B1' B6 B2' 60.2(6) . . ? B2 B6 B2' 119.9(7) . . ? B7 B6 B2' 58.9(5) . . ? B1' B6 B5 142.6(8) . . ? B2 B6 B5 58.5(6) . . ? B7 B6 B5 103.9(6) . . ? B2' B6 B5 144.1(7) . . ? B1' B6 B10' 54.2(6) . . ? B2 B6 B10' 100.8(7) . . ? B7 B6 B10' 123.9(7) . . ? B2' B6 B10' 105.9(6) . . ? B5 B6 B10' 109.5(7) . . ? B1' B6 H58 123(4) . . ? B2 B6 H58 85(4) . . ? B7 B6 H58 111(4) . . ? B2' B6 H58 122(4) . . ? B5 B6 H58 30(4) . . ? B10' B6 H58 120(4) . . ? B3 B7 B2' 155.1(7) . . ? B3 B7 B6 109.6(7) . . ? B2' B7 B6 61.7(6) . . ? B3 B7 B2 60.4(5) . . ? B2' B7 B2 119.4(7) . . ? B6 B7 B2 58.1(6) . . ? B3 B7 B8 52.5(5) . . ? B2' B7 B8 108.2(6) . . ? B6 B7 B8 116.5(6) . . ? B2 B7 B8 103.5(5) . . ? B3 B7 Ir7' 134.6(6) . . ? B2' B7 Ir7' 66.1(4) . . ? B6 B7 Ir7' 111.8(5) . . ? B2 B7 Ir7' 133.0(5) . . ? B8 B7 Ir7' 119.3(5) . . ? B3 B7 H67' 110(3) . . ? B2' B7 H67' 95(3) . . ? B6 B7 H67' 110(3) . . ? B2 B7 H67' 99(3) . . ? B8 B7 H67' 134(3) . . ? Ir7' B7 H67' 37(3) . . ? B3 B8 B4 61.6(5) . . ? B3 B8 Cl8 121.6(8) . . ? B4 B8 Cl8 126.1(9) . . ? B3 B8 B7 54.1(5) . . ? B4 B8 B7 105.9(6) . . ? Cl8 B8 B7 116.9(8) . . ? B3 B8 Ir9 119.4(6) . . ? B4 B8 Ir9 65.5(4) . . ? Cl8 B8 Ir9 112.4(7) . . ? B7 B8 Ir9 120.8(5) . . ? B3 B8 H8 138.5 . . ? B4 B8 H8 140.4 . . ? Cl8 B8 H8 21.9 . . ? B7 B8 H8 112.4 . . ? Ir9 B8 H8 101.3 . . ? B3 B8 H89 128(5) . . ? B4 B8 H89 107(5) . . ? Cl8 B8 H89 106(5) . . ? B7 B8 H89 87(5) . . ? Ir9 B8 H89 48(5) . . ? H8 B8 H89 84.8 . . ? B9' B8' B4' 56.9(7) . . ? B9' B8' B3' 109.5(7) . . ? B4' B8' B3' 60.2(6) . . ? B9' B8' Ir7' 126.1(6) . . ? B4' B8' Ir7' 117.1(6) . . ? B3' B8' Ir7' 63.4(4) . . ? B9' B8' H8' 107.7 . . ? B4' B8' H8' 140.5 . . ? B3' B8' H8' 141.6 . . ? Ir7' B8' H8' 101.3 . . ? B9' B8' H89' 39(4) . . ? B4' B8' H89' 94(4) . . ? B3' B8' H89' 131(4) . . ? Ir7' B8' H89' 102(4) . . ? H8' B8' H89' 85.5 . . ? B4' B9' B10' 59.7(7) . . ? B4' B9' B8' 61.8(6) . . ? B10' B9' B8' 104.3(8) . . ? B4' B9' H89' 103(4) . . ? B10' B9' H89' 120(4) . . ? B8' B9' H89' 43(4) . . ? B4' B9' H91' 103(5) . . ? B10' B9' H91' 45(5) . . ? B8' B9' H91' 121(6) . . ? H89' B9' H91' 102(7) . . ? B4' B9' H9' 129(4) . . ? B10' B9' H9' 122(4) . . ? B8' B9' H9' 131(4) . . ? H89' B9' H9' 113(6) . . ? H91' B9' H9' 103(7) . . ? B1 B10 B4 61.5(6) . . ? B1 B10 B5 55.7(6) . . ? B4 B10 B5 106.7(7) . . ? B1 B10 Ir9 119.5(6) . . ? B4 B10 Ir9 65.4(4) . . ? B5 B10 Ir9 120.4(6) . . ? B1 B10 H10 138.0 . . ? B4 B10 H10 140.4 . . ? B5 B10 H10 111.7 . . ? Ir9 B10 H10 101.5 . . ? B1 B10 H91 128(6) . . ? B4 B10 H91 106(7) . . ? B5 B10 H91 87(7) . . ? Ir9 B10 H91 47(7) . . ? H10 B10 H91 85.7 . . ? B1' B10' B4' 61.7(7) . . ? B1' B10' B9' 110.7(9) . . ? B4' B10' B9' 58.0(7) . . ? B1' B10' B6 56.6(6) . . ? B4' B10' B6 108.0(8) . . ? B9' B10' B6 116.4(8) . . ? B1' B10' H10' 139.1 . . ? B4' B10' H10' 140.0 . . ? B9' B10' H10' 109.3 . . ? B6 B10' H10' 111.1 . . ? B1' B10' H91' 132(5) . . ? B4' B10' H91' 99(5) . . ? B9' B10' H91' 43(5) . . ? B6 B10' H91' 96(5) . . ? H10' B10' H91' 84.6 . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 2.988 _refine_diff_density_min -1.381 _refine_diff_density_rms 0.189 # Attachment 'B611734A CCDC 286253.CIF' data_mc1di _database_code_depnum_ccdc_archive 'CCDC 286253' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H45 B16 Cl Ir2' _chemical_formula_sum 'C20 H45 B16 Cl Ir2' _chemical_formula_weight 878.37 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.5170(5) _cell_length_b 31.2197(13) _cell_length_c 9.6161(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.3370(10) _cell_angle_gamma 90.00 _cell_volume 3174.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description fragment _exptl_crystal_colour violet _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 8.472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6304 _exptl_absorpt_correction_T_max 0.8488 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69320 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29321 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 29.48 _reflns_number_total 8826 _reflns_number_gt 7769 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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 'w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+10.6007P] 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 8826 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir6 Ir 0.844493(19) 0.607147(6) 0.83759(2) 0.02470(6) Uani 1 1 d . . . Ir7' Ir 0.458418(19) 0.645079(6) 0.63759(2) 0.02628(7) Uani 1 1 d . . . Cl10 Cl 0.99909(19) 0.60923(6) 1.22888(19) 0.0512(4) Uani 1 1 d . . . C61 C 0.9153(6) 0.6526(2) 0.7082(8) 0.0376(14) Uani 1 1 d . . . C62 C 0.8840(6) 0.6129(2) 0.6279(7) 0.0381(13) Uani 1 1 d . . . C63 C 0.9645(6) 0.58026(19) 0.7252(7) 0.0346(12) Uani 1 1 d . . . C64 C 1.0459(5) 0.60012(19) 0.8617(7) 0.0321(11) Uani 1 1 d . . . C65 C 1.0156(6) 0.64504(18) 0.8559(7) 0.0330(12) Uani 1 1 d . . . C66 C 0.8614(8) 0.6953(3) 0.6463(11) 0.061(2) Uani 1 1 d . . . H66A H 0.8987 0.7054 0.5766 0.092 Uiso 1 1 calc R . . H66B H 0.8807 0.7158 0.7298 0.092 Uiso 1 1 calc R . . H66C H 0.7695 0.6929 0.5920 0.092 Uiso 1 1 calc R . . C67 C 0.7905(8) 0.6068(3) 0.4702(8) 0.063(2) Uani 1 1 d . . . H67A H 0.7217 0.6276 0.4481 0.094 Uiso 1 1 calc R . . H67B H 0.7561 0.5777 0.4585 0.094 Uiso 1 1 calc R . . H67C H 0.8320 0.6111 0.3998 0.094 Uiso 1 1 calc R . . C68 C 0.9677(7) 0.5342(2) 0.6859(10) 0.0507(18) Uani 1 1 d . . . H68A H 1.0313 0.5300 0.6432 0.076 Uiso 1 1 calc R . . H68B H 0.8845 0.5257 0.6113 0.076 Uiso 1 1 calc R . . H68C H 0.9895 0.5167 0.7774 0.076 Uiso 1 1 calc R . . C69 C 1.1507(6) 0.5782(2) 0.9896(9) 0.0466(16) Uani 1 1 d . . . H69A H 1.1258 0.5487 0.9989 0.070 Uiso 1 1 calc R . . H69B H 1.1673 0.5936 1.0843 0.070 Uiso 1 1 calc R . . H69C H 1.2275 0.5780 0.9688 0.070 Uiso 1 1 calc R . . C70 C 1.0834(7) 0.6781(2) 0.9714(10) 0.0547(19) Uani 1 1 d . . . H70A H 1.1099 0.6656 1.0729 0.082 Uiso 1 1 calc R . . H70B H 1.0269 0.7024 0.9618 0.082 Uiso 1 1 calc R . . H70C H 1.1581 0.6879 0.9555 0.082 Uiso 1 1 calc R . . C71 C 0.3044(5) 0.6722(2) 0.4330(7) 0.0356(12) Uani 1 1 d . . . C72 C 0.2500(6) 0.6506(2) 0.5230(8) 0.0423(15) Uani 1 1 d . . . C73 C 0.2774(6) 0.6059(2) 0.5213(8) 0.0409(14) Uani 1 1 d . . . C74 C 0.3544(6) 0.60053(19) 0.4382(7) 0.0367(13) Uani 1 1 d . . . C75 C 0.3728(5) 0.64214(18) 0.3873(7) 0.0308(11) Uani 1 1 d . . . C76 C 0.2798(7) 0.7186(2) 0.3826(9) 0.0523(19) Uani 1 1 d . . . H76A H 0.3496 0.7293 0.3583 0.078 Uiso 1 1 calc R . . H76B H 0.2734 0.7359 0.4643 0.078 Uiso 1 1 calc R . . H76C H 0.2005 0.7207 0.2926 0.078 Uiso 1 1 calc R . . C77 C 0.1620(7) 0.6700(4) 0.5862(11) 0.068(3) Uani 1 1 d . . . H77A H 0.1541 0.6507 0.6624 0.101 Uiso 1 1 calc R . . H77B H 0.0787 0.6743 0.5043 0.101 Uiso 1 1 calc R . . H77C H 0.1958 0.6976 0.6330 0.101 Uiso 1 1 calc R . . C78 C 0.2240(8) 0.5711(3) 0.5857(10) 0.069(3) Uani 1 1 d . . . H78A H 0.1371 0.5648 0.5153 0.103 Uiso 1 1 calc R . . H78B H 0.2240 0.5805 0.6830 0.103 Uiso 1 1 calc R . . H78C H 0.2758 0.5453 0.6010 0.103 Uiso 1 1 calc R . . C79 C 0.3985(9) 0.5589(2) 0.3979(9) 0.056(2) Uani 1 1 d . . . H79A H 0.4215 0.5391 0.4840 0.084 Uiso 1 1 calc R . . H79B H 0.4723 0.5640 0.3736 0.084 Uiso 1 1 calc R . . H79C H 0.3303 0.5463 0.3099 0.084 Uiso 1 1 calc R . . C80 C 0.4374(7) 0.6516(3) 0.2812(8) 0.0481(17) Uani 1 1 d . . . H80A H 0.3747 0.6513 0.1764 0.072 Uiso 1 1 calc R . . H80B H 0.5018 0.6297 0.2937 0.072 Uiso 1 1 calc R . . H80C H 0.4775 0.6798 0.3047 0.072 Uiso 1 1 calc R . . B1 B 0.6964(6) 0.5572(2) 0.7696(7) 0.0303(12) Uani 1 1 d . . . B1' B 0.6273(8) 0.6620(2) 1.0131(8) 0.0379(15) Uani 1 1 d . . . B2 B 0.6442(7) 0.6114(2) 0.7639(7) 0.0312(13) Uani 1 1 d . . . B3 B 0.5577(7) 0.5668(2) 0.7984(8) 0.0358(14) Uani 1 1 d . . . B3' B 0.4761(7) 0.6684(2) 0.8605(8) 0.0366(14) Uani 1 1 d . . . B4 B 0.6649(7) 0.5292(2) 0.9170(9) 0.0375(15) Uani 1 1 d . . . B4' B 0.5817(8) 0.7139(3) 0.9372(8) 0.0433(17) Uani 1 1 d . . . B5 B 0.8205(7) 0.5493(2) 0.9569(8) 0.0343(13) Uani 1 1 d . . . B7 B 0.5677(6) 0.6202(2) 0.8810(7) 0.0301(12) Uani 1 1 d . . . B8 B 0.5797(8) 0.5651(3) 0.9839(10) 0.0422(16) Uani 1 1 d . . . B8' B 0.5004(7) 0.7097(2) 0.7371(8) 0.0366(14) Uani 1 1 d . . . B9 B 0.7504(8) 0.5527(2) 1.0919(9) 0.0408(16) Uani 1 1 d . . . B9' B 0.6564(8) 0.7319(2) 0.8285(9) 0.0436(17) Uani 1 1 d . . . B10 B 0.8549(7) 0.5969(2) 1.0639(7) 0.0333(13) Uani 1 1 d . . . B10' B 0.7403(8) 0.6959(2) 0.9801(8) 0.0399(16) Uani 1 1 d . . . B11 B 0.7341(6) 0.6379(2) 0.9440(7) 0.0282(12) Uani 1 1 d . . . H1 H 0.693(7) 0.536(2) 0.680(8) 0.04(2) Uiso 1 1 d . . . H1' H 0.648(7) 0.655(2) 1.142(9) 0.04(2) Uiso 1 1 d . . . H3 H 0.468(7) 0.552(2) 0.723(8) 0.038(18) Uiso 1 1 d . . . H3' H 0.378(6) 0.6698(19) 0.897(7) 0.025(15) Uiso 1 1 d . . . H4 H 0.642(8) 0.495(3) 0.914(9) 0.06(2) Uiso 1 1 d . . . H4' H 0.573(6) 0.738(2) 1.010(8) 0.038(18) Uiso 1 1 d . . . H5 H 0.902(6) 0.525(2) 0.979(7) 0.028(16) Uiso 1 1 d . . . H8 H 0.505(7) 0.557(2) 1.042(9) 0.05(2) Uiso 1 1 d . . . H8' H 0.431(8) 0.734(3) 0.691(10) 0.06(2) Uiso 1 1 d . . . H9 H 0.792(6) 0.537(2) 1.210(8) 0.034(17) Uiso 1 1 d . . . H9' H 0.677(8) 0.771(3) 0.811(10) 0.06(2) Uiso 1 1 d . . . H19 H 0.842(7) 0.705(2) 1.088(8) 0.041(19) Uiso 1 1 d . . . H89 H 0.647(7) 0.575(2) 1.084(8) 0.036(18) Uiso 1 1 d . . . H910 H 0.739(7) 0.708(2) 0.857(9) 0.05(2) Uiso 1 1 d . . . H89' H 0.592(9) 0.714(3) 0.693(11) 0.07(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir6 0.02883(11) 0.02170(10) 0.02448(10) 0.00170(6) 0.01152(8) 0.00027(7) Ir7' 0.02701(11) 0.02606(11) 0.02729(11) -0.00343(7) 0.01236(8) -0.00247(7) Cl10 0.0506(10) 0.0632(11) 0.0308(7) 0.0022(7) 0.0066(7) 0.0039(8) C61 0.031(3) 0.039(3) 0.049(4) 0.019(3) 0.023(3) 0.005(2) C62 0.029(3) 0.056(4) 0.034(3) 0.006(3) 0.018(2) -0.001(3) C63 0.034(3) 0.033(3) 0.044(3) -0.002(2) 0.023(3) -0.002(2) C64 0.027(3) 0.034(3) 0.036(3) 0.008(2) 0.013(2) 0.004(2) C65 0.032(3) 0.029(3) 0.039(3) 0.004(2) 0.015(2) -0.003(2) C66 0.061(5) 0.057(5) 0.081(6) 0.042(4) 0.045(5) 0.022(4) C67 0.046(4) 0.118(8) 0.023(3) 0.002(4) 0.013(3) 0.004(4) C68 0.055(4) 0.042(4) 0.072(5) -0.019(3) 0.042(4) -0.008(3) C69 0.029(3) 0.050(4) 0.053(4) 0.010(3) 0.008(3) 0.010(3) C70 0.051(4) 0.036(3) 0.077(5) -0.012(3) 0.025(4) -0.017(3) C71 0.026(3) 0.041(3) 0.034(3) -0.006(2) 0.006(2) -0.005(2) C72 0.025(3) 0.056(4) 0.040(3) -0.004(3) 0.007(3) -0.002(3) C73 0.035(3) 0.043(3) 0.039(3) -0.002(3) 0.010(3) -0.016(3) C74 0.047(3) 0.031(3) 0.026(3) -0.004(2) 0.008(2) -0.003(2) C75 0.022(2) 0.034(3) 0.034(3) -0.001(2) 0.009(2) -0.003(2) C76 0.047(4) 0.037(3) 0.051(4) 0.002(3) -0.003(3) 0.007(3) C77 0.034(4) 0.110(8) 0.062(5) -0.016(5) 0.023(4) 0.005(4) C78 0.051(4) 0.086(6) 0.060(5) 0.015(4) 0.011(4) -0.038(4) C79 0.076(6) 0.038(4) 0.043(4) -0.014(3) 0.012(4) 0.001(3) C80 0.044(4) 0.073(5) 0.029(3) 0.001(3) 0.017(3) 0.000(3) B1 0.037(3) 0.025(3) 0.031(3) -0.002(2) 0.016(3) -0.001(2) B1' 0.047(4) 0.041(4) 0.029(3) -0.001(3) 0.020(3) 0.007(3) B2 0.040(3) 0.026(3) 0.029(3) -0.001(2) 0.015(3) -0.004(2) B3 0.037(3) 0.033(3) 0.039(4) -0.001(3) 0.017(3) -0.005(3) B3' 0.043(4) 0.045(4) 0.028(3) -0.005(3) 0.021(3) 0.008(3) B4 0.046(4) 0.023(3) 0.052(4) 0.006(3) 0.029(3) -0.002(3) B4' 0.051(4) 0.041(4) 0.033(3) -0.008(3) 0.011(3) 0.005(3) B5 0.042(4) 0.031(3) 0.032(3) 0.006(2) 0.017(3) 0.003(3) B7 0.035(3) 0.028(3) 0.030(3) 0.006(2) 0.015(3) 0.006(2) B8 0.043(4) 0.039(4) 0.051(4) 0.010(3) 0.026(4) 0.002(3) B8' 0.042(4) 0.032(3) 0.031(3) -0.003(2) 0.009(3) 0.003(3) B9 0.054(4) 0.035(3) 0.043(4) 0.011(3) 0.029(4) 0.007(3) B9' 0.055(4) 0.028(3) 0.037(4) -0.007(3) 0.005(3) 0.002(3) B10 0.038(3) 0.034(3) 0.028(3) 0.002(2) 0.013(3) 0.005(3) B10' 0.051(4) 0.029(3) 0.035(3) -0.007(3) 0.012(3) 0.003(3) B11 0.034(3) 0.026(3) 0.022(3) -0.002(2) 0.009(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir6 B2 2.132(7) . ? Ir6 B11 2.149(6) . ? Ir6 B10 2.156(7) . ? Ir6 B1 2.211(6) . ? Ir6 B5 2.215(7) . ? Ir6 C63 2.229(6) . ? Ir6 C61 2.242(6) . ? Ir6 C62 2.243(6) . ? Ir6 C65 2.245(6) . ? Ir6 C64 2.248(6) . ? Ir7' B3' 2.196(6) . ? Ir7' B8' 2.204(7) . ? Ir7' C75 2.212(6) . ? Ir7' C72 2.216(6) . ? Ir7' C71 2.230(6) . ? Ir7' B2 2.259(7) . ? Ir7' C74 2.286(6) . ? Ir7' C73 2.291(6) . ? Ir7' B7 2.309(6) . ? Cl10 B10 1.826(7) . ? C61 C62 1.428(10) . ? C61 C65 1.452(9) . ? C61 C66 1.494(9) . ? C62 C63 1.444(9) . ? C62 C67 1.484(10) . ? C63 C64 1.418(9) . ? C63 C68 1.490(9) . ? C64 C65 1.441(8) . ? C64 C69 1.504(8) . ? C65 C70 1.490(9) . ? C71 C75 1.404(9) . ? C71 C72 1.424(10) . ? C71 C76 1.519(9) . ? C72 C73 1.432(10) . ? C72 C77 1.500(10) . ? C73 C74 1.419(10) . ? C73 C78 1.497(10) . ? C74 C75 1.433(8) . ? C74 C79 1.501(9) . ? C75 C80 1.511(9) . ? B1 B3 1.751(10) . ? B1 B2 1.789(9) . ? B1 B4 1.818(9) . ? B1 B5 1.819(10) . ? B1' B7 1.759(10) . ? B1' B4' 1.770(11) . ? B1' B11 1.779(10) . ? B1' B3' 1.789(11) . ? B1' B10' 1.800(12) . ? B2 B7 1.705(9) . ? B2 B3 1.815(10) . ? B2 B11 1.827(9) . ? B3 B8 1.700(11) . ? B3 B4 1.757(10) . ? B3 B7 1.830(10) . ? B3' B7 1.803(9) . ? B3' B4' 1.824(11) . ? B3' B8' 1.848(11) . ? B4 B9 1.739(12) . ? B4 B8 1.770(11) . ? B4 B5 1.791(10) . ? B4' B9' 1.692(13) . ? B4' B8' 1.780(10) . ? B4' B10' 1.796(12) . ? B5 B10 1.760(10) . ? B5 B9 1.783(10) . ? B7 B11 1.851(10) . ? B7 B8 1.961(10) . ? B8 B9 1.864(12) . ? B8' B9' 1.797(11) . ? B9 B10 1.918(11) . ? B9' B10' 1.792(11) . ? B10 B11 1.907(9) . ? B10' B11 1.838(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B2 Ir6 B11 50.5(2) . . ? B2 Ir6 B10 88.0(3) . . ? B11 Ir6 B10 52.6(2) . . ? B2 Ir6 B1 48.6(2) . . ? B11 Ir6 B1 85.6(2) . . ? B10 Ir6 B1 85.5(3) . . ? B2 Ir6 B5 83.2(3) . . ? B11 Ir6 B5 84.2(2) . . ? B10 Ir6 B5 47.5(3) . . ? B1 Ir6 B5 48.5(3) . . ? B2 Ir6 C63 131.3(2) . . ? B11 Ir6 C63 175.5(2) . . ? B10 Ir6 C63 129.5(2) . . ? B1 Ir6 C63 98.3(2) . . ? B5 Ir6 C63 100.0(2) . . ? B2 Ir6 C61 111.1(2) . . ? B11 Ir6 C61 113.3(2) . . ? B10 Ir6 C61 140.1(3) . . ? B1 Ir6 C61 133.6(3) . . ? B5 Ir6 C61 161.9(2) . . ? C63 Ir6 C61 62.4(2) . . ? B2 Ir6 C62 105.9(2) . . ? B11 Ir6 C62 139.6(2) . . ? B10 Ir6 C62 165.8(3) . . ? B1 Ir6 C62 101.4(2) . . ? B5 Ir6 C62 130.0(3) . . ? C63 Ir6 C62 37.7(2) . . ? C61 Ir6 C62 37.1(3) . . ? B2 Ir6 C65 142.6(2) . . ? B11 Ir6 C65 113.2(2) . . ? B10 Ir6 C65 107.6(3) . . ? B1 Ir6 C65 161.0(2) . . ? B5 Ir6 C65 132.4(2) . . ? C63 Ir6 C65 62.8(2) . . ? C61 Ir6 C65 37.8(2) . . ? C62 Ir6 C65 62.9(2) . . ? B2 Ir6 C64 167.5(2) . . ? B11 Ir6 C64 140.8(2) . . ? B10 Ir6 C64 103.8(2) . . ? B1 Ir6 C64 127.3(2) . . ? B5 Ir6 C64 101.7(2) . . ? C63 Ir6 C64 36.9(2) . . ? C61 Ir6 C64 62.1(2) . . ? C62 Ir6 C64 62.1(2) . . ? C65 Ir6 C64 37.4(2) . . ? B3' Ir7' B8' 49.7(3) . . ? B3' Ir7' C75 154.8(2) . . ? B8' Ir7' C75 115.9(2) . . ? B3' Ir7' C72 97.1(3) . . ? B8' Ir7' C72 98.8(3) . . ? C75 Ir7' C72 62.2(2) . . ? B3' Ir7' C71 118.0(3) . . ? B8' Ir7' C71 89.8(2) . . ? C75 Ir7' C71 36.9(2) . . ? C72 Ir7' C71 37.4(2) . . ? B3' Ir7' B2 85.9(3) . . ? B8' Ir7' B2 101.3(3) . . ? C75 Ir7' B2 119.0(2) . . ? C72 Ir7' B2 155.8(3) . . ? C71 Ir7' B2 154.8(2) . . ? B3' Ir7' C74 146.7(3) . . ? B8' Ir7' C74 150.8(2) . . ? C75 Ir7' C74 37.1(2) . . ? C72 Ir7' C74 61.7(3) . . ? C71 Ir7' C74 61.4(2) . . ? B2 Ir7' C74 103.7(2) . . ? B3' Ir7' C73 111.6(3) . . ? B8' Ir7' C73 134.6(3) . . ? C75 Ir7' C73 61.3(2) . . ? C72 Ir7' C73 37.0(3) . . ? C71 Ir7' C73 61.3(2) . . ? B2 Ir7' C73 119.9(2) . . ? C74 Ir7' C73 36.1(3) . . ? B3' Ir7' B7 47.1(2) . . ? B8' Ir7' B7 86.0(2) . . ? C75 Ir7' B7 156.6(2) . . ? C72 Ir7' B7 125.3(3) . . ? C71 Ir7' B7 161.1(2) . . ? B2 Ir7' B7 43.8(2) . . ? C74 Ir7' B7 122.7(2) . . ? C73 Ir7' B7 109.9(2) . . ? C62 C61 C65 108.8(5) . . ? C62 C61 C66 125.8(7) . . ? C65 C61 C66 125.3(7) . . ? C62 C61 Ir6 71.5(3) . . ? C65 C61 Ir6 71.2(3) . . ? C66 C61 Ir6 127.0(5) . . ? C61 C62 C63 107.6(5) . . ? C61 C62 C67 126.1(7) . . ? C63 C62 C67 126.2(7) . . ? C61 C62 Ir6 71.4(3) . . ? C63 C62 Ir6 70.6(3) . . ? C67 C62 Ir6 125.8(5) . . ? C64 C63 C62 108.1(5) . . ? C64 C63 C68 125.7(6) . . ? C62 C63 C68 126.2(6) . . ? C64 C63 Ir6 72.3(3) . . ? C62 C63 Ir6 71.7(3) . . ? C68 C63 Ir6 124.6(4) . . ? C63 C64 C65 109.2(5) . . ? C63 C64 C69 125.4(6) . . ? C65 C64 C69 125.4(6) . . ? C63 C64 Ir6 70.8(3) . . ? C65 C64 Ir6 71.2(3) . . ? C69 C64 Ir6 126.2(4) . . ? C64 C65 C61 106.4(5) . . ? C64 C65 C70 126.7(6) . . ? C61 C65 C70 126.7(6) . . ? C64 C65 Ir6 71.4(3) . . ? C61 C65 Ir6 71.0(3) . . ? C70 C65 Ir6 127.4(5) . . ? C75 C71 C72 108.0(6) . . ? C75 C71 C76 126.5(6) . . ? C72 C71 C76 125.2(6) . . ? C75 C71 Ir7' 70.9(3) . . ? C72 C71 Ir7' 70.8(4) . . ? C76 C71 Ir7' 128.8(4) . . ? C71 C72 C73 107.7(6) . . ? C71 C72 C77 125.7(7) . . ? C73 C72 C77 125.9(7) . . ? C71 C72 Ir7' 71.8(4) . . ? C73 C72 Ir7' 74.3(4) . . ? C77 C72 Ir7' 127.0(5) . . ? C74 C73 C72 108.1(6) . . ? C74 C73 C78 126.8(7) . . ? C72 C73 C78 124.9(8) . . ? C74 C73 Ir7' 71.8(3) . . ? C72 C73 Ir7' 68.7(3) . . ? C78 C73 Ir7' 129.0(5) . . ? C73 C74 C75 107.2(5) . . ? C73 C74 C79 126.7(6) . . ? C75 C74 C79 125.9(6) . . ? C73 C74 Ir7' 72.1(3) . . ? C75 C74 Ir7' 68.6(3) . . ? C79 C74 Ir7' 128.7(5) . . ? C71 C75 C74 108.8(5) . . ? C71 C75 C80 124.7(6) . . ? C74 C75 C80 125.9(6) . . ? C71 C75 Ir7' 72.3(4) . . ? C74 C75 Ir7' 74.3(3) . . ? C80 C75 Ir7' 126.9(4) . . ? B3 B1 B2 61.7(4) . . ? B3 B1 B4 58.9(4) . . ? B2 B1 B4 108.0(5) . . ? B3 B1 B5 106.0(5) . . ? B2 B1 B5 106.3(4) . . ? B4 B1 B5 59.0(4) . . ? B3 B1 Ir6 118.5(4) . . ? B2 B1 Ir6 63.4(3) . . ? B4 B1 Ir6 118.5(4) . . ? B5 B1 Ir6 65.8(3) . . ? B7 B1' B4' 114.5(5) . . ? B7 B1' B11 63.1(4) . . ? B4' B1' B11 111.6(5) . . ? B7 B1' B3' 61.1(4) . . ? B4' B1' B3' 61.7(4) . . ? B11 B1' B3' 109.5(5) . . ? B7 B1' B10' 114.3(5) . . ? B4' B1' B10' 60.4(5) . . ? B11 B1' B10' 61.8(4) . . ? B3' B1' B10' 109.0(5) . . ? B7 B2 B1 112.8(5) . . ? B7 B2 B3 62.5(4) . . ? B1 B2 B3 58.2(4) . . ? B7 B2 B11 63.1(4) . . ? B1 B2 B11 110.1(5) . . ? B3 B2 B11 108.7(5) . . ? B7 B2 Ir6 124.4(4) . . ? B1 B2 Ir6 68.0(3) . . ? B3 B2 Ir6 119.5(4) . . ? B11 B2 Ir6 65.2(3) . . ? B7 B2 Ir7' 69.6(3) . . ? B1 B2 Ir7' 133.8(4) . . ? B3 B2 Ir7' 89.0(4) . . ? B11 B2 Ir7' 111.0(4) . . ? Ir6 B2 Ir7' 151.3(3) . . ? B8 B3 B1 113.2(5) . . ? B8 B3 B4 61.6(4) . . ? B1 B3 B4 62.4(4) . . ? B8 B3 B2 110.6(5) . . ? B1 B3 B2 60.2(4) . . ? B4 B3 B2 109.5(5) . . ? B8 B3 B7 67.4(4) . . ? B1 B3 B7 108.7(5) . . ? B4 B3 B7 114.8(5) . . ? B2 B3 B7 55.8(4) . . ? B1' B3' B7 58.6(4) . . ? B1' B3' B4' 58.7(4) . . ? B7 B3' B4' 109.8(5) . . ? B1' B3' B8' 105.0(5) . . ? B7 B3' B8' 114.9(5) . . ? B4' B3' B8' 58.0(4) . . ? B1' B3' Ir7' 116.5(4) . . ? B7 B3' Ir7' 69.7(3) . . ? B4' B3' Ir7' 116.2(4) . . ? B8' B3' Ir7' 65.4(3) . . ? B9 B4 B3 109.2(5) . . ? B9 B4 B8 64.2(5) . . ? B3 B4 B8 57.6(4) . . ? B9 B4 B5 60.7(4) . . ? B3 B4 B5 107.0(5) . . ? B8 B4 B5 110.6(5) . . ? B9 B4 B1 109.9(5) . . ? B3 B4 B1 58.6(4) . . ? B8 B4 B1 106.9(5) . . ? B5 B4 B1 60.5(4) . . ? B9' B4' B1' 114.8(6) . . ? B9' B4' B8' 62.3(5) . . ? B1' B4' B8' 108.8(5) . . ? B9' B4' B10' 61.8(5) . . ? B1' B4' B10' 60.6(4) . . ? B8' B4' B10' 106.1(5) . . ? B9' B4' B3' 115.5(5) . . ? B1' B4' B3' 59.7(4) . . ? B8' B4' B3' 61.7(4) . . ? B10' B4' B3' 107.7(5) . . ? B10 B5 B9 65.5(4) . . ? B10 B5 B4 113.3(5) . . ? B9 B5 B4 58.2(4) . . ? B10 B5 B1 111.8(5) . . ? B9 B5 B1 107.9(5) . . ? B4 B5 B1 60.5(4) . . ? B10 B5 Ir6 64.5(3) . . ? B9 B5 Ir6 120.9(4) . . ? B4 B5 Ir6 119.6(4) . . ? B1 B5 Ir6 65.6(3) . . ? B2 B7 B1' 116.2(5) . . ? B2 B7 B3' 119.8(5) . . ? B1' B7 B3' 60.3(4) . . ? B2 B7 B3 61.7(4) . . ? B1' B7 B3 158.1(5) . . ? B3' B7 B3 141.2(5) . . ? B2 B7 B11 61.7(4) . . ? B1' B7 B11 59.0(4) . . ? B3' B7 B11 105.7(5) . . ? B3 B7 B11 107.1(4) . . ? B2 B7 B8 103.8(4) . . ? B1' B7 B8 110.9(5) . . ? B3' B7 B8 135.1(5) . . ? B3 B7 B8 53.2(4) . . ? B11 B7 B8 103.9(4) . . ? B2 B7 Ir7' 66.5(3) . . ? B1' B7 Ir7' 112.5(4) . . ? B3' B7 Ir7' 63.2(3) . . ? B3 B7 Ir7' 87.2(3) . . ? B11 B7 Ir7' 108.0(3) . . ? B8 B7 Ir7' 135.0(4) . . ? B3 B8 B4 60.8(4) . . ? B3 B8 B9 106.1(5) . . ? B4 B8 B9 57.1(4) . . ? B3 B8 B7 59.4(4) . . ? B4 B8 B7 108.1(5) . . ? B9 B8 B7 108.1(5) . . ? B4' B8' B9' 56.4(5) . . ? B4' B8' B3' 60.3(4) . . ? B9' B8' B3' 109.3(5) . . ? B4' B8' Ir7' 117.8(4) . . ? B9' B8' Ir7' 124.8(5) . . ? B3' B8' Ir7' 64.9(3) . . ? B4 B9 B5 61.1(4) . . ? B4 B9 B8 58.7(5) . . ? B5 B9 B8 106.8(5) . . ? B4 B9 B10 108.3(5) . . ? B5 B9 B10 56.7(4) . . ? B8 B9 B10 110.7(5) . . ? B4' B9' B10' 62.0(5) . . ? B4' B9' B8' 61.3(5) . . ? B10' B9' B8' 105.5(5) . . ? B5 B10 Cl10 127.0(5) . . ? B5 B10 B11 105.8(4) . . ? Cl10 B10 B11 125.3(4) . . ? B5 B10 B9 57.8(4) . . ? Cl10 B10 B9 115.8(4) . . ? B11 B10 B9 102.7(5) . . ? B5 B10 Ir6 68.0(3) . . ? Cl10 B10 Ir6 120.9(4) . . ? B11 B10 Ir6 63.5(3) . . ? B9 B10 Ir6 117.5(4) . . ? B9' B10' B4' 56.3(5) . . ? B9' B10' B1' 108.6(6) . . ? B4' B10' B1' 59.0(5) . . ? B9' B10' B11 119.8(5) . . ? B4' B10' B11 107.8(5) . . ? B1' B10' B11 58.5(4) . . ? B1' B11 B2 109.2(5) . . ? B1' B11 B10' 59.7(4) . . ? B2 B11 B10' 126.3(5) . . ? B1' B11 B7 57.9(4) . . ? B2 B11 B7 55.2(4) . . ? B10' B11 B7 108.3(5) . . ? B1' B11 B10 120.3(5) . . ? B2 B11 B10 105.8(4) . . ? B10' B11 B10 125.6(5) . . ? B7 B11 B10 114.2(4) . . ? B1' B11 Ir6 173.4(4) . . ? B2 B11 Ir6 64.2(3) . . ? B10' B11 Ir6 123.0(4) . . ? B7 B11 Ir6 116.2(4) . . ? B10 B11 Ir6 63.9(3) . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 29.48 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 3.962 _refine_diff_density_min -1.557 _refine_diff_density_rms 0.215