# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Neutral and Zwitterionic Half-sandwich Ir, Rh Complexes Supported by P, S-Substituted o-Carboranyl Ligands: Synthesis, Characterization and Reactivity ; loop_ _publ_author_name 'Guo-Xin Jin.' 'Xian-Kuan Huo.' 'Ge Su.' # Attachment '1a.cif' data_f90319d _database_code_depnum_ccdc_archive 'CCDC 746417' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H35 B10 Cl Ir P S' _chemical_formula_weight 722.30 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.230(4) _cell_length_b 11.756(4) _cell_length_c 21.071(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.154(4) _cell_angle_gamma 90.00 _cell_volume 2998.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1000 _cell_measurement_theta_min 3.580 _cell_measurement_theta_max 26.124 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 4.680 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6036 _exptl_absorpt_correction_T_max 0.6519 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.32 _diffrn_reflns_number 13304 _diffrn_reflns_av_R_equivalents 0.0336 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5784 _reflns_number_gt 4536 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5784 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_restrained_S_all 0.870 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.785357(12) 0.210759(11) 0.537565(6) 0.03022(5) Uani 1 1 d . . . P1 P 0.78765(8) 0.33552(8) 0.62192(4) 0.0320(2) Uani 1 1 d . . . S1 S 0.97461(9) 0.17636(9) 0.56979(5) 0.0492(3) Uani 1 1 d . . . Cl1 Cl 0.74315(10) 0.04841(9) 0.60050(5) 0.0575(3) Uani 1 1 d . . . B3 B 0.9452(4) 0.1865(4) 0.7109(2) 0.0499(13) Uani 1 1 d . . . H3 H 0.8827 0.1186 0.7072 0.060 Uiso 1 1 calc R . . B4 B 0.9365(5) 0.3078(4) 0.7595(2) 0.0579(15) Uani 1 1 d . . . H4 H 0.8683 0.3178 0.7880 0.069 Uiso 1 1 calc R . . B5 B 0.9909(5) 0.4263(4) 0.7227(2) 0.0591(15) Uani 1 1 d . . . H5 H 0.9579 0.5126 0.7271 0.071 Uiso 1 1 calc R . . B6 B 1.0375(4) 0.3769(4) 0.6514(2) 0.0492(13) Uani 1 1 d . . . H6 H 1.0350 0.4312 0.6088 0.059 Uiso 1 1 calc R . . B7 B 1.1434(4) 0.2772(5) 0.6719(2) 0.0599(15) Uani 1 1 d . . . H7 H 1.2109 0.2671 0.6430 0.072 Uiso 1 1 calc R . . B8 B 1.0873(4) 0.1583(4) 0.7084(2) 0.0557(14) Uani 1 1 d . . . H8 H 1.1174 0.0711 0.7032 0.067 Uiso 1 1 calc R . . B9 B 1.0442(4) 0.2081(5) 0.7799(2) 0.0622(15) Uani 1 1 d . . . H9 H 1.0474 0.1531 0.8224 0.075 Uiso 1 1 calc R . . B10 B 1.0720(5) 0.3549(5) 0.7866(2) 0.0688(17) Uani 1 1 d . . . H10 H 1.0935 0.3960 0.8337 0.083 Uiso 1 1 calc R . . B11 B 1.1326(5) 0.3986(5) 0.7206(2) 0.0696(18) Uani 1 1 d . . . H11 H 1.1931 0.4683 0.7240 0.084 Uiso 1 1 calc R . . B12 B 1.1649(5) 0.2630(5) 0.7557(2) 0.0668(17) Uani 1 1 d . . . H12 H 1.2471 0.2437 0.7819 0.080 Uiso 1 1 calc R . . C1 C 0.9226(3) 0.3196(3) 0.67753(16) 0.0360(9) Uani 1 1 d . . . C2 C 1.0107(3) 0.2330(3) 0.64815(16) 0.0406(10) Uani 1 1 d . . . C3 C 0.6788(3) 0.3217(3) 0.67146(17) 0.0421(10) Uani 1 1 d . . . C4 C 0.6756(4) 0.3810(3) 0.72900(18) 0.0535(11) Uani 1 1 d . . . H4A H 0.7339 0.4285 0.7448 0.064 Uiso 1 1 calc R . . C5 C 0.5874(4) 0.3696(4) 0.7622(2) 0.0741(15) Uani 1 1 d . . . H5A H 0.5865 0.4088 0.8005 0.089 Uiso 1 1 calc R . . C6 C 0.5012(5) 0.3007(5) 0.7391(3) 0.100(2) Uani 1 1 d . . . H6A H 0.4422 0.2923 0.7622 0.120 Uiso 1 1 calc R . . C7 C 0.5005(5) 0.2446(5) 0.6829(3) 0.107(2) Uani 1 1 d . . . H7A H 0.4399 0.2003 0.6667 0.129 Uiso 1 1 calc R . . C8 C 0.5899(4) 0.2529(4) 0.6495(2) 0.0715(15) Uani 1 1 d . . . H8A H 0.5901 0.2117 0.6119 0.086 Uiso 1 1 calc R . . C9 C 0.7836(3) 0.4875(3) 0.60084(16) 0.0357(9) Uani 1 1 d . . . C10 C 0.8474(3) 0.5238(3) 0.55558(17) 0.0404(9) Uani 1 1 d . . . H10A H 0.8914 0.4716 0.5378 0.048 Uiso 1 1 calc R . . C11 C 0.8468(4) 0.6366(3) 0.53628(19) 0.0537(11) Uani 1 1 d . . . H11A H 0.8903 0.6601 0.5059 0.064 Uiso 1 1 calc R . . C12 C 0.7813(4) 0.7131(4) 0.5627(2) 0.0675(14) Uani 1 1 d . . . H12A H 0.7816 0.7893 0.5509 0.081 Uiso 1 1 calc R . . C13 C 0.7163(5) 0.6781(4) 0.6058(2) 0.0730(15) Uani 1 1 d . . . H13 H 0.6709 0.7303 0.6225 0.088 Uiso 1 1 calc R . . C14 C 0.7165(4) 0.5654(3) 0.62526(19) 0.0571(12) Uani 1 1 d . . . H14 H 0.6712 0.5424 0.6548 0.069 Uiso 1 1 calc R . . C15 C 0.7784(3) 0.2968(3) 0.44376(15) 0.0349(9) Uani 1 1 d . . . C16 C 0.8057(3) 0.1785(3) 0.43531(16) 0.0373(10) Uani 1 1 d . . . C17 C 0.7187(3) 0.1109(3) 0.45114(15) 0.0363(9) Uani 1 1 d . . . C18 C 0.6337(3) 0.1852(3) 0.46889(16) 0.0361(9) Uani 1 1 d . . . C19 C 0.6707(3) 0.2994(3) 0.46347(15) 0.0345(9) Uani 1 1 d . . . C20 C 0.8375(4) 0.3933(3) 0.41739(17) 0.0534(12) Uani 1 1 d . . . H20A H 0.9142 0.3913 0.4352 0.080 Uiso 1 1 calc R . . H20B H 0.8057 0.4640 0.4285 0.080 Uiso 1 1 calc R . . H20C H 0.8304 0.3867 0.3716 0.080 Uiso 1 1 calc R . . C21 C 0.9079(3) 0.1374(3) 0.41086(18) 0.0538(11) Uani 1 1 d . . . H21A H 0.9299 0.0657 0.4304 0.081 Uiso 1 1 calc R . . H21B H 0.9661 0.1919 0.4213 0.081 Uiso 1 1 calc R . . H21C H 0.8931 0.1283 0.3652 0.081 Uiso 1 1 calc R . . C22 C 0.7109(3) -0.0162(3) 0.44633(18) 0.0522(12) Uani 1 1 d . . . H22A H 0.6666 -0.0369 0.4067 0.078 Uiso 1 1 calc R . . H22B H 0.6776 -0.0454 0.4816 0.078 Uiso 1 1 calc R . . H22C H 0.7836 -0.0477 0.4476 0.078 Uiso 1 1 calc R . . C23 C 0.5226(3) 0.1489(3) 0.48296(19) 0.0539(11) Uani 1 1 d . . . H23A H 0.4835 0.2138 0.4959 0.081 Uiso 1 1 calc R . . H23B H 0.5312 0.0937 0.5169 0.081 Uiso 1 1 calc R . . H23C H 0.4816 0.1160 0.4452 0.081 Uiso 1 1 calc R . . C24 C 0.6020(3) 0.4043(3) 0.46922(18) 0.0491(11) Uani 1 1 d . . . H24A H 0.5551 0.4176 0.4294 0.074 Uiso 1 1 calc R . . H24B H 0.6498 0.4686 0.4792 0.074 Uiso 1 1 calc R . . H24C H 0.5574 0.3936 0.5027 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03314(8) 0.02955(8) 0.02716(8) 0.00186(7) 0.00145(5) -0.00229(7) P1 0.0347(6) 0.0350(5) 0.0266(5) 0.0013(4) 0.0055(4) -0.0038(4) S1 0.0403(6) 0.0660(7) 0.0391(6) -0.0054(5) -0.0023(5) 0.0127(5) Cl1 0.0749(8) 0.0486(6) 0.0456(6) 0.0144(5) -0.0035(5) -0.0203(6) B3 0.060(3) 0.052(3) 0.035(3) 0.020(2) 0.000(2) -0.010(3) B4 0.072(4) 0.079(4) 0.020(2) 0.007(2) 0.000(2) 0.000(3) B5 0.071(4) 0.054(3) 0.047(3) -0.009(2) -0.013(3) -0.014(3) B6 0.045(3) 0.050(3) 0.049(3) 0.017(2) -0.006(2) -0.015(2) B7 0.036(3) 0.085(4) 0.054(3) 0.024(3) -0.008(2) -0.009(3) B8 0.054(4) 0.054(3) 0.053(3) 0.016(3) -0.014(3) 0.005(3) B9 0.070(4) 0.079(4) 0.032(3) 0.017(3) -0.014(2) -0.008(3) B10 0.080(4) 0.079(4) 0.040(3) -0.001(3) -0.018(3) -0.014(3) B11 0.066(4) 0.069(4) 0.066(4) 0.019(3) -0.023(3) -0.028(3) B12 0.062(4) 0.079(4) 0.052(3) 0.017(3) -0.021(3) -0.012(3) C1 0.042(2) 0.038(2) 0.0262(19) 0.0023(16) -0.0016(16) -0.0061(17) C2 0.034(2) 0.052(3) 0.033(2) 0.0093(18) -0.0034(17) -0.0038(19) C3 0.041(2) 0.051(3) 0.037(2) -0.0064(18) 0.0146(18) -0.0056(19) C4 0.062(3) 0.053(3) 0.048(3) -0.004(2) 0.017(2) -0.008(2) C5 0.088(4) 0.082(4) 0.063(3) -0.013(3) 0.044(3) -0.009(3) C6 0.092(4) 0.115(5) 0.108(5) -0.042(4) 0.071(4) -0.045(4) C7 0.074(4) 0.144(6) 0.116(5) -0.064(4) 0.054(4) -0.061(4) C8 0.058(3) 0.096(4) 0.066(3) -0.029(3) 0.028(2) -0.024(3) C9 0.043(2) 0.035(2) 0.028(2) -0.0023(16) -0.0006(17) -0.0036(18) C10 0.044(3) 0.035(2) 0.041(2) 0.0029(18) 0.0039(19) -0.0029(19) C11 0.060(3) 0.047(3) 0.053(3) 0.012(2) 0.004(2) -0.005(2) C12 0.099(4) 0.033(2) 0.067(3) 0.014(2) -0.003(3) 0.004(3) C13 0.107(5) 0.051(3) 0.064(3) 0.004(2) 0.023(3) 0.033(3) C14 0.071(3) 0.054(3) 0.050(3) 0.007(2) 0.021(2) 0.014(2) C15 0.040(2) 0.041(2) 0.0232(18) 0.0027(17) 0.0009(15) -0.005(2) C16 0.048(3) 0.040(2) 0.0217(19) 0.0007(15) -0.0014(17) -0.0017(19) C17 0.045(2) 0.033(2) 0.027(2) -0.0010(16) -0.0059(17) -0.0041(19) C18 0.038(2) 0.037(2) 0.030(2) 0.0019(16) -0.0060(17) -0.0060(18) C19 0.039(2) 0.033(2) 0.0289(19) 0.0000(16) -0.0049(16) -0.0014(18) C20 0.070(3) 0.049(3) 0.042(2) 0.006(2) 0.011(2) -0.017(2) C21 0.059(3) 0.058(3) 0.046(2) -0.003(2) 0.014(2) 0.001(2) C22 0.073(3) 0.036(2) 0.044(3) -0.0013(18) -0.004(2) -0.003(2) C23 0.046(3) 0.053(3) 0.061(3) 0.001(2) 0.001(2) -0.007(2) C24 0.053(3) 0.039(2) 0.052(3) -0.0040(19) -0.005(2) 0.007(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 Ir1 C18 2.206(3) . ? Ir1 C19 2.206(3) . ? Ir1 C15 2.211(3) . ? Ir1 C17 2.222(3) . ? Ir1 C16 2.236(4) . ? Ir1 P1 2.3016(10) . ? Ir1 S1 2.3529(12) . ? Ir1 Cl1 2.4210(11) . ? P1 C3 1.812(4) . ? P1 C9 1.840(4) . ? P1 C1 1.893(4) . ? S1 C2 1.777(4) . ? B3 C1 1.723(5) . ? B3 C2 1.729(6) . ? B3 B4 1.767(7) . ? B3 B9 1.773(6) . ? B3 B8 1.777(7) . ? B4 C1 1.717(5) . ? B4 B10 1.764(7) . ? B4 B9 1.770(7) . ? B4 B5 1.770(7) . ? B5 C1 1.718(5) . ? B5 B10 1.767(7) . ? B5 B11 1.769(8) . ? B5 B6 1.779(7) . ? B6 C1 1.717(6) . ? B6 C2 1.723(6) . ? B6 B11 1.749(6) . ? B6 B7 1.754(7) . ? B7 C2 1.711(6) . ? B7 B12 1.755(7) . ? B7 B11 1.773(8) . ? B7 B8 1.780(7) . ? B8 C2 1.710(5) . ? B8 B9 1.764(7) . ? B8 B12 1.772(7) . ? B9 B12 1.753(8) . ? B9 B10 1.761(8) . ? B10 B11 1.745(8) . ? B10 B12 1.760(8) . ? B11 B12 1.778(7) . ? C1 C2 1.665(5) . ? C3 C8 1.380(5) . ? C3 C4 1.404(5) . ? C4 C5 1.373(6) . ? C5 C6 1.363(6) . ? C6 C7 1.355(7) . ? C7 C8 1.385(6) . ? C9 C14 1.377(5) . ? C9 C10 1.383(5) . ? C10 C11 1.387(5) . ? C11 C12 1.373(6) . ? C12 C13 1.353(6) . ? C13 C14 1.388(5) . ? C15 C19 1.437(5) . ? C15 C16 1.447(5) . ? C15 C20 1.494(5) . ? C16 C17 1.405(5) . ? C16 C21 1.497(5) . ? C17 C18 1.447(5) . ? C17 C22 1.500(5) . ? C18 C19 1.427(5) . ? C18 C23 1.493(5) . ? C19 C24 1.507(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 Ir1 C19 37.74(12) . . ? C18 Ir1 C15 63.51(13) . . ? C19 Ir1 C15 37.96(13) . . ? C18 Ir1 C17 38.14(13) . . ? C19 Ir1 C17 63.06(13) . . ? C15 Ir1 C17 62.98(13) . . ? C18 Ir1 C16 62.80(14) . . ? C19 Ir1 C16 62.91(13) . . ? C15 Ir1 C16 37.96(12) . . ? C17 Ir1 C16 36.75(13) . . ? C18 Ir1 P1 120.70(10) . . ? C19 Ir1 P1 100.52(9) . . ? C15 Ir1 P1 113.19(10) . . ? C17 Ir1 P1 158.81(10) . . ? C16 Ir1 P1 149.47(9) . . ? C18 Ir1 S1 150.16(10) . . ? C19 Ir1 S1 141.78(10) . . ? C15 Ir1 S1 104.35(10) . . ? C17 Ir1 S1 112.17(10) . . ? C16 Ir1 S1 90.55(10) . . ? P1 Ir1 S1 89.02(4) . . ? C18 Ir1 Cl1 91.54(9) . . ? C19 Ir1 Cl1 126.62(10) . . ? C15 Ir1 Cl1 150.00(9) . . ? C17 Ir1 Cl1 87.17(10) . . ? C16 Ir1 Cl1 117.10(10) . . ? P1 Ir1 Cl1 93.41(4) . . ? S1 Ir1 Cl1 89.08(4) . . ? C3 P1 C9 103.24(18) . . ? C3 P1 C1 106.39(17) . . ? C9 P1 C1 103.69(15) . . ? C3 P1 Ir1 117.27(13) . . ? C9 P1 Ir1 115.81(12) . . ? C1 P1 Ir1 109.23(12) . . ? C2 S1 Ir1 107.95(13) . . ? C1 B3 C2 57.7(2) . . ? C1 B3 B4 58.9(2) . . ? C2 B3 B4 105.1(3) . . ? C1 B3 B9 104.8(3) . . ? C2 B3 B9 104.2(3) . . ? B4 B3 B9 60.0(3) . . ? C1 B3 B8 104.9(3) . . ? C2 B3 B8 58.3(2) . . ? B4 B3 B8 107.9(4) . . ? B9 B3 B8 59.6(3) . . ? C1 B4 B10 104.8(4) . . ? C1 B4 B3 59.2(2) . . ? B10 B4 B3 108.1(4) . . ? C1 B4 B9 105.2(4) . . ? B10 B4 B9 59.8(3) . . ? B3 B4 B9 60.2(3) . . ? C1 B4 B5 59.0(2) . . ? B10 B4 B5 60.0(3) . . ? B3 B4 B5 108.9(3) . . ? B9 B4 B5 108.3(4) . . ? C1 B5 B10 104.6(3) . . ? C1 B5 B11 104.6(4) . . ? B10 B5 B11 59.1(3) . . ? C1 B5 B4 58.9(2) . . ? B10 B5 B4 59.8(3) . . ? B11 B5 B4 107.3(4) . . ? C1 B5 B6 58.8(2) . . ? B10 B5 B6 106.0(4) . . ? B11 B5 B6 59.1(3) . . ? B4 B5 B6 107.3(3) . . ? C1 B6 C2 57.9(2) . . ? C1 B6 B11 105.5(3) . . ? C2 B6 B11 106.1(3) . . ? C1 B6 B7 105.6(3) . . ? C2 B6 B7 58.9(3) . . ? B11 B6 B7 60.8(3) . . ? C1 B6 B5 58.9(3) . . ? C2 B6 B5 105.8(3) . . ? B11 B6 B5 60.2(3) . . ? B7 B6 B5 108.9(3) . . ? C2 B7 B6 59.6(2) . . ? C2 B7 B12 105.4(4) . . ? B6 B7 B12 108.1(4) . . ? C2 B7 B11 105.6(4) . . ? B6 B7 B11 59.4(3) . . ? B12 B7 B11 60.5(3) . . ? C2 B7 B8 58.6(2) . . ? B6 B7 B8 108.3(4) . . ? B12 B7 B8 60.2(3) . . ? B11 B7 B8 108.5(4) . . ? C2 B8 B9 105.4(4) . . ? C2 B8 B12 104.7(3) . . ? B9 B8 B12 59.4(3) . . ? C2 B8 B3 59.4(2) . . ? B9 B8 B3 60.1(3) . . ? B12 B8 B3 107.6(4) . . ? C2 B8 B7 58.7(2) . . ? B9 B8 B7 106.8(4) . . ? B12 B8 B7 59.2(3) . . ? B3 B8 B7 107.8(3) . . ? B12 B9 B10 60.1(3) . . ? B12 B9 B8 60.5(3) . . ? B10 B9 B8 108.4(4) . . ? B12 B9 B4 108.3(4) . . ? B10 B9 B4 59.9(3) . . ? B8 B9 B4 108.3(3) . . ? B12 B9 B3 108.6(3) . . ? B10 B9 B3 107.9(3) . . ? B8 B9 B3 60.3(3) . . ? B4 B9 B3 59.8(3) . . ? B11 B10 B12 61.0(3) . . ? B11 B10 B9 108.9(4) . . ? B12 B10 B9 59.7(3) . . ? B11 B10 B4 108.6(3) . . ? B12 B10 B4 108.3(4) . . ? B9 B10 B4 60.3(3) . . ? B11 B10 B5 60.5(3) . . ? B12 B10 B5 109.3(4) . . ? B9 B10 B5 108.9(3) . . ? B4 B10 B5 60.2(3) . . ? B10 B11 B6 108.3(4) . . ? B10 B11 B5 60.4(3) . . ? B6 B11 B5 60.7(3) . . ? B10 B11 B7 107.4(4) . . ? B6 B11 B7 59.7(3) . . ? B5 B11 B7 108.5(3) . . ? B10 B11 B12 59.9(3) . . ? B6 B11 B12 107.3(4) . . ? B5 B11 B12 108.4(4) . . ? B7 B11 B12 59.2(3) . . ? B9 B12 B7 108.4(3) . . ? B9 B12 B10 60.2(3) . . ? B7 B12 B10 107.6(4) . . ? B9 B12 B8 60.1(3) . . ? B7 B12 B8 60.6(3) . . ? B10 B12 B8 108.2(4) . . ? B9 B12 B11 107.7(4) . . ? B7 B12 B11 60.3(3) . . ? B10 B12 B11 59.1(3) . . ? B8 B12 B11 108.6(3) . . ? C2 C1 B4 110.3(3) . . ? C2 C1 B6 61.2(3) . . ? B4 C1 B6 112.7(3) . . ? C2 C1 B5 111.3(3) . . ? B4 C1 B5 62.0(3) . . ? B6 C1 B5 62.4(3) . . ? C2 C1 B3 61.4(2) . . ? B4 C1 B3 61.8(2) . . ? B6 C1 B3 113.3(3) . . ? B5 C1 B3 113.6(3) . . ? C2 C1 P1 112.6(2) . . ? B4 C1 P1 125.7(3) . . ? B6 C1 P1 116.4(2) . . ? B5 C1 P1 125.7(3) . . ? B3 C1 P1 114.7(2) . . ? C1 C2 B8 110.7(3) . . ? C1 C2 B7 110.0(3) . . ? B8 C2 B7 62.7(3) . . ? C1 C2 B6 60.9(2) . . ? B8 C2 B6 113.1(3) . . ? B7 C2 B6 61.5(3) . . ? C1 C2 B3 61.0(2) . . ? B8 C2 B3 62.2(3) . . ? B7 C2 B3 113.3(3) . . ? B6 C2 B3 112.7(3) . . ? C1 C2 S1 119.1(2) . . ? B8 C2 S1 122.4(3) . . ? B7 C2 S1 119.1(3) . . ? B6 C2 S1 115.2(2) . . ? B3 C2 S1 120.8(3) . . ? C8 C3 C4 117.6(4) . . ? C8 C3 P1 117.9(3) . . ? C4 C3 P1 124.4(3) . . ? C5 C4 C3 120.8(4) . . ? C6 C5 C4 120.0(5) . . ? C7 C6 C5 120.6(5) . . ? C6 C7 C8 120.1(5) . . ? C3 C8 C7 120.8(4) . . ? C14 C9 C10 118.5(4) . . ? C14 C9 P1 123.5(3) . . ? C10 C9 P1 117.9(3) . . ? C9 C10 C11 121.2(4) . . ? C12 C11 C10 119.1(4) . . ? C13 C12 C11 120.3(4) . . ? C12 C13 C14 120.8(5) . . ? C9 C14 C13 120.0(4) . . ? C19 C15 C16 107.0(3) . . ? C19 C15 C20 127.0(3) . . ? C16 C15 C20 123.5(3) . . ? C19 C15 Ir1 70.83(19) . . ? C16 C15 Ir1 72.0(2) . . ? C20 C15 Ir1 136.1(2) . . ? C17 C16 C15 108.6(3) . . ? C17 C16 C21 126.6(3) . . ? C15 C16 C21 124.8(3) . . ? C17 C16 Ir1 71.1(2) . . ? C15 C16 Ir1 70.08(19) . . ? C21 C16 Ir1 126.8(2) . . ? C16 C17 C18 108.5(3) . . ? C16 C17 C22 126.1(4) . . ? C18 C17 C22 125.3(4) . . ? C16 C17 Ir1 72.18(19) . . ? C18 C17 Ir1 70.32(19) . . ? C22 C17 Ir1 126.4(2) . . ? C19 C18 C17 107.4(3) . . ? C19 C18 C23 126.4(3) . . ? C17 C18 C23 125.9(3) . . ? C19 C18 Ir1 71.15(19) . . ? C17 C18 Ir1 71.53(19) . . ? C23 C18 Ir1 127.8(3) . . ? C18 C19 C15 108.5(3) . . ? C18 C19 C24 125.2(4) . . ? C15 C19 C24 125.8(3) . . ? C18 C19 Ir1 71.10(19) . . ? C15 C19 Ir1 71.21(19) . . ? C24 C19 Ir1 129.4(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.806 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.085 # Attachment '2a.cif' data_f90317a _database_code_depnum_ccdc_archive 'CCDC 746418' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 B9 Ir O P S' _chemical_formula_weight 706.07 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.231(3) _cell_length_b 16.911(5) _cell_length_c 17.352(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.047(4) _cell_angle_gamma 90.00 _cell_volume 2924.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 940 _cell_measurement_theta_min 3.213 _cell_measurement_theta_max 27.357 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 4.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4526 _exptl_absorpt_correction_T_max 0.7044 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.59 _diffrn_reflns_number 13726 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6225 _reflns_number_gt 4649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6225 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0267 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.630814(14) 0.237059(8) 0.068949(8) 0.03494(5) Uani 1 1 d . . . P1 P 0.49834(9) 0.26476(5) 0.15556(5) 0.02960(19) Uani 1 1 d . . . S1 S 0.54595(11) 0.11716(6) 0.05896(6) 0.0472(3) Uani 1 1 d . . . O1 O 0.6813(3) 0.12691(17) 0.24750(18) 0.0604(8) Uani 1 1 d . . . B1 B 0.4513(5) 0.0443(3) 0.2805(3) 0.0481(12) Uani 1 1 d . . . H1A H 0.4980 0.0123 0.3349 0.058 Uiso 1 1 calc R . . B2 B 0.4749(5) 0.0155(3) 0.1872(3) 0.0458(11) Uani 1 1 d . . . H2A H 0.5400 -0.0344 0.1798 0.055 Uiso 1 1 calc R . . B3 B 0.5479(4) 0.1042(3) 0.2311(3) 0.0402(10) Uani 1 1 d . . . B4 B 0.4289(5) 0.1475(3) 0.2796(3) 0.0446(11) Uani 1 1 d . . . H4A H 0.4634 0.1836 0.3330 0.053 Uiso 1 1 calc R . . B5 B 0.2878(5) 0.0869(3) 0.2660(3) 0.0542(13) Uani 1 1 d . . . H5A H 0.2287 0.0837 0.3116 0.065 Uiso 1 1 calc R . . B6 B 0.3177(5) 0.0034(3) 0.2086(3) 0.0501(12) Uani 1 1 d . . . H6A H 0.2796 -0.0563 0.2158 0.060 Uiso 1 1 calc R . . B9 B 0.2830(5) 0.1715(3) 0.2063(3) 0.0460(12) Uani 1 1 d . . . H9A H 0.226(4) 0.224(2) 0.211(2) 0.043(10) Uiso 1 1 d . . . B10 B 0.2034(5) 0.0780(3) 0.1668(4) 0.0560(14) Uani 1 1 d . . . H10A H 0.102(5) 0.062(3) 0.158(3) 0.093(16) Uiso 1 1 d . . . H10B H 0.222(5) 0.113(3) 0.125(3) 0.086(16) Uiso 1 1 d . . . B11 B 0.3262(5) 0.0394(3) 0.1149(3) 0.0473(12) Uani 1 1 d . . . H11A H 0.301(3) 0.004(2) 0.061(2) 0.055(11) Uiso 1 1 d . . . C1 C 0.1402(5) 0.3962(3) 0.0015(3) 0.0633(13) Uani 1 1 d . . . H1 H 0.0674 0.4214 -0.0311 0.076 Uiso 1 1 calc R . . C2 C 0.1649(4) 0.3176(3) -0.0098(3) 0.0616(13) Uani 1 1 d . . . H2 H 0.1102 0.2901 -0.0513 0.074 Uiso 1 1 calc R . . C3 C 0.7837(4) 0.0749(3) 0.2340(3) 0.0744(15) Uani 1 1 d . . . H3A H 0.8013 0.0352 0.2746 0.112 Uiso 1 1 calc R . . H3B H 0.8642 0.1045 0.2350 0.112 Uiso 1 1 calc R . . H3C H 0.7546 0.0499 0.1834 0.112 Uiso 1 1 calc R . . C4 C 0.3547(3) 0.3202(2) 0.1004(2) 0.0323(8) Uani 1 1 d . . . C5 C 0.3305(4) 0.3994(2) 0.1097(2) 0.0448(10) Uani 1 1 d . . . H5 H 0.3872 0.4280 0.1494 0.054 Uiso 1 1 calc R . . C6 C 0.2225(5) 0.4370(3) 0.0606(3) 0.0567(12) Uani 1 1 d . . . H6 H 0.2064 0.4902 0.0681 0.068 Uiso 1 1 calc R . . C7 C 0.4494(4) 0.1008(2) 0.1332(2) 0.0353(8) Uani 1 1 d . . . C8 C 0.4267(3) 0.1732(2) 0.1834(2) 0.0308(8) Uani 1 1 d . . . C9 C 0.2692(4) 0.2796(2) 0.0392(2) 0.0466(10) Uani 1 1 d . . . H9 H 0.2832 0.2260 0.0318 0.056 Uiso 1 1 calc R . . C10 C 0.5670(3) 0.3176(2) 0.2461(2) 0.0346(8) Uani 1 1 d . . . C11 C 0.4870(4) 0.3595(2) 0.2868(2) 0.0441(10) Uani 1 1 d . . . H11 H 0.3948 0.3623 0.2670 0.053 Uiso 1 1 calc R . . C12 C 0.5458(5) 0.3973(2) 0.3572(2) 0.0555(12) Uani 1 1 d . . . H12 H 0.4927 0.4271 0.3833 0.067 Uiso 1 1 calc R . . C13 C 0.6799(5) 0.3914(3) 0.3886(2) 0.0587(13) Uani 1 1 d . . . H13 H 0.7179 0.4172 0.4356 0.070 Uiso 1 1 calc R . . C14 C 0.7576(4) 0.3480(3) 0.3514(2) 0.0539(11) Uani 1 1 d . . . H14 H 0.8487 0.3428 0.3741 0.065 Uiso 1 1 calc R . . C15 C 0.7039(4) 0.3109(2) 0.2798(2) 0.0438(9) Uani 1 1 d . . . H15 H 0.7590 0.2817 0.2545 0.053 Uiso 1 1 calc R . . C16 C 0.6382(4) 0.3289(2) -0.0162(2) 0.0462(10) Uani 1 1 d . . . C17 C 0.7223(4) 0.3545(2) 0.0571(2) 0.0455(10) Uani 1 1 d . . . C18 C 0.8240(4) 0.2973(3) 0.0801(2) 0.0491(10) Uani 1 1 d . . . C19 C 0.8098(4) 0.2386(3) 0.0176(3) 0.0550(11) Uani 1 1 d . . . C20 C 0.6976(5) 0.2587(2) -0.0417(2) 0.0523(11) Uani 1 1 d . . . C21 C 0.5203(5) 0.3728(3) -0.0634(3) 0.0733(15) Uani 1 1 d . . . H21A H 0.4791 0.4029 -0.0284 0.110 Uiso 1 1 calc R . . H21B H 0.4565 0.3358 -0.0924 0.110 Uiso 1 1 calc R . . H21C H 0.5495 0.4078 -0.0997 0.110 Uiso 1 1 calc R . . C22 C 0.7053(5) 0.4284(3) 0.1015(3) 0.0619(12) Uani 1 1 d . . . H22A H 0.7482 0.4219 0.1563 0.093 Uiso 1 1 calc R . . H22B H 0.6114 0.4386 0.0966 0.093 Uiso 1 1 calc R . . H22C H 0.7453 0.4721 0.0800 0.093 Uiso 1 1 calc R . . C23 C 0.9401(4) 0.3016(3) 0.1507(3) 0.0753(15) Uani 1 1 d . . . H23A H 1.0162 0.3244 0.1352 0.113 Uiso 1 1 calc R . . H23B H 0.9622 0.2494 0.1711 0.113 Uiso 1 1 calc R . . H23C H 0.9159 0.3339 0.1908 0.113 Uiso 1 1 calc R . . C24 C 0.9000(5) 0.1686(3) 0.0184(4) 0.0895(18) Uani 1 1 d . . . H24A H 0.8536 0.1288 -0.0170 0.134 Uiso 1 1 calc R . . H24B H 0.9250 0.1474 0.0710 0.134 Uiso 1 1 calc R . . H24C H 0.9791 0.1847 0.0015 0.134 Uiso 1 1 calc R . . C25 C 0.6487(6) 0.2160(3) -0.1182(3) 0.0850(18) Uani 1 1 d . . . H25A H 0.7028 0.2305 -0.1546 0.127 Uiso 1 1 calc R . . H25B H 0.5570 0.2301 -0.1402 0.127 Uiso 1 1 calc R . . H25C H 0.6550 0.1600 -0.1091 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03835(8) 0.03572(9) 0.03500(8) -0.00095(7) 0.01723(6) -0.00211(7) P1 0.0306(5) 0.0309(5) 0.0279(4) -0.0007(4) 0.0080(4) 0.0003(4) S1 0.0642(7) 0.0387(6) 0.0478(6) -0.0092(5) 0.0318(5) -0.0085(5) O1 0.0455(18) 0.0529(19) 0.078(2) -0.0019(16) 0.0040(16) 0.0047(14) B1 0.058(3) 0.043(3) 0.045(3) 0.015(2) 0.015(2) 0.007(2) B2 0.049(3) 0.033(3) 0.058(3) 0.006(2) 0.018(2) 0.002(2) B3 0.039(3) 0.039(3) 0.041(3) 0.004(2) 0.007(2) 0.0043(19) B4 0.057(3) 0.049(3) 0.029(2) 0.006(2) 0.014(2) 0.003(2) B5 0.065(3) 0.053(3) 0.053(3) 0.015(2) 0.031(3) 0.002(3) B6 0.054(3) 0.042(3) 0.058(3) 0.008(2) 0.021(2) -0.007(2) B9 0.044(3) 0.045(3) 0.054(3) 0.013(2) 0.021(2) 0.007(2) B10 0.038(3) 0.058(3) 0.074(4) 0.016(3) 0.016(3) -0.010(2) B11 0.055(3) 0.044(3) 0.043(3) -0.004(2) 0.010(2) -0.013(2) C1 0.054(3) 0.073(4) 0.057(3) 0.021(3) 0.000(2) 0.015(2) C2 0.055(3) 0.070(3) 0.049(3) 0.005(2) -0.012(2) -0.002(2) C3 0.050(3) 0.071(4) 0.100(4) 0.011(3) 0.011(3) 0.015(2) C4 0.0328(19) 0.037(2) 0.0274(19) 0.0040(15) 0.0075(15) 0.0025(15) C5 0.054(3) 0.041(2) 0.039(2) 0.0010(18) 0.0093(19) 0.0049(19) C6 0.070(3) 0.045(3) 0.056(3) 0.008(2) 0.015(2) 0.020(2) C7 0.042(2) 0.033(2) 0.034(2) 0.0008(16) 0.0146(17) -0.0046(16) C8 0.0331(19) 0.031(2) 0.0295(19) 0.0046(15) 0.0091(15) 0.0013(15) C9 0.051(2) 0.044(3) 0.041(2) 0.0016(18) 0.0025(19) 0.0010(19) C10 0.039(2) 0.034(2) 0.0300(19) -0.0037(16) 0.0073(16) -0.0039(16) C11 0.051(3) 0.046(3) 0.036(2) -0.0005(18) 0.0109(19) 0.0057(19) C12 0.090(4) 0.044(3) 0.036(2) -0.0028(19) 0.022(2) 0.008(2) C13 0.090(4) 0.048(3) 0.030(2) -0.0060(19) -0.003(2) -0.016(2) C14 0.051(3) 0.067(3) 0.039(2) 0.000(2) 0.000(2) -0.013(2) C15 0.037(2) 0.049(3) 0.045(2) 0.0013(19) 0.0093(18) -0.0036(18) C16 0.053(2) 0.052(3) 0.038(2) 0.0099(19) 0.0183(19) -0.005(2) C17 0.052(3) 0.041(2) 0.048(2) 0.0025(19) 0.021(2) -0.0107(19) C18 0.038(2) 0.064(3) 0.050(3) 0.004(2) 0.0187(19) -0.011(2) C19 0.055(3) 0.058(3) 0.065(3) 0.000(2) 0.041(2) -0.006(2) C20 0.067(3) 0.055(3) 0.045(2) -0.002(2) 0.034(2) -0.014(2) C21 0.074(3) 0.083(4) 0.062(3) 0.031(3) 0.015(3) -0.003(3) C22 0.081(3) 0.046(3) 0.065(3) -0.007(2) 0.028(3) -0.019(2) C23 0.043(3) 0.112(4) 0.073(3) 0.012(3) 0.018(2) -0.009(3) C24 0.073(4) 0.084(4) 0.131(5) 0.002(4) 0.064(3) 0.019(3) C25 0.119(5) 0.099(4) 0.052(3) -0.021(3) 0.051(3) -0.043(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C16 2.158(4) . ? Ir1 C18 2.193(4) . ? Ir1 S1 2.1971(11) . ? Ir1 C20 2.210(4) . ? Ir1 C19 2.210(4) . ? Ir1 C17 2.224(4) . ? Ir1 P1 2.2880(10) . ? P1 C10 1.807(4) . ? P1 C4 1.822(3) . ? P1 C8 1.825(3) . ? S1 C7 1.812(3) . ? O1 B3 1.384(5) . ? O1 C3 1.427(5) . ? B1 B4 1.758(6) . ? B1 B2 1.760(7) . ? B1 B3 1.767(6) . ? B1 B6 1.771(7) . ? B1 B5 1.786(7) . ? B2 C7 1.707(6) . ? B2 B6 1.742(6) . ? B2 B3 1.770(6) . ? B2 B11 1.786(7) . ? B3 C8 1.765(5) . ? B3 C7 1.769(6) . ? B3 B4 1.786(6) . ? B4 C8 1.720(5) . ? B4 B5 1.743(7) . ? B4 B9 1.776(7) . ? B5 B10 1.750(8) . ? B5 B9 1.761(6) . ? B5 B6 1.793(7) . ? B6 B11 1.757(6) . ? B6 B10 1.761(7) . ? B9 C8 1.608(5) . ? B9 B10 1.840(7) . ? B10 B11 1.823(8) . ? B11 C7 1.608(6) . ? C1 C6 1.358(6) . ? C1 C2 1.376(6) . ? C2 C9 1.366(5) . ? C4 C5 1.378(5) . ? C4 C9 1.395(5) . ? C5 C6 1.387(5) . ? C7 C8 1.550(5) . ? C10 C11 1.389(5) . ? C10 C15 1.395(5) . ? C11 C12 1.389(5) . ? C12 C13 1.361(6) . ? C13 C14 1.348(6) . ? C14 C15 1.389(5) . ? C16 C17 1.433(5) . ? C16 C20 1.448(6) . ? C16 C21 1.493(6) . ? C17 C18 1.410(6) . ? C17 C22 1.499(6) . ? C18 C19 1.452(6) . ? C18 C23 1.503(6) . ? C19 C20 1.401(6) . ? C19 C24 1.499(6) . ? C20 C25 1.494(6) . ? 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 C16 Ir1 C18 63.62(15) . . ? C16 Ir1 S1 133.22(11) . . ? C18 Ir1 S1 140.16(12) . . ? C16 Ir1 C20 38.70(15) . . ? C18 Ir1 C20 63.27(16) . . ? S1 Ir1 C20 106.18(11) . . ? C16 Ir1 C19 63.58(16) . . ? C18 Ir1 C19 38.52(15) . . ? S1 Ir1 C19 109.13(11) . . ? C20 Ir1 C19 36.95(16) . . ? C16 Ir1 C17 38.13(14) . . ? C18 Ir1 C17 37.23(15) . . ? S1 Ir1 C17 169.60(11) . . ? C20 Ir1 C17 63.42(15) . . ? C19 Ir1 C17 63.13(15) . . ? C16 Ir1 P1 114.84(11) . . ? C18 Ir1 P1 120.19(12) . . ? S1 Ir1 P1 87.63(4) . . ? C20 Ir1 P1 151.91(12) . . ? C19 Ir1 P1 158.42(12) . . ? C17 Ir1 P1 101.65(11) . . ? C10 P1 C4 108.16(16) . . ? C10 P1 C8 106.85(16) . . ? C4 P1 C8 104.59(16) . . ? C10 P1 Ir1 120.07(12) . . ? C4 P1 Ir1 106.69(11) . . ? C8 P1 Ir1 109.45(11) . . ? C7 S1 Ir1 110.72(12) . . ? B3 O1 C3 121.4(4) . . ? B4 B1 B2 108.1(3) . . ? B4 B1 B3 60.9(3) . . ? B2 B1 B3 60.3(3) . . ? B4 B1 B6 107.6(3) . . ? B2 B1 B6 59.1(3) . . ? B3 B1 B6 108.0(3) . . ? B4 B1 B5 58.9(3) . . ? B2 B1 B5 107.5(3) . . ? B3 B1 B5 108.0(3) . . ? B6 B1 B5 60.5(3) . . ? C7 B2 B6 100.5(3) . . ? C7 B2 B1 103.6(3) . . ? B6 B2 B1 60.7(3) . . ? C7 B2 B3 61.1(2) . . ? B6 B2 B3 109.1(3) . . ? B1 B2 B3 60.1(3) . . ? C7 B2 B11 54.8(2) . . ? B6 B2 B11 59.7(3) . . ? B1 B2 B11 108.2(3) . . ? B3 B2 B11 108.7(3) . . ? O1 B3 C8 118.0(3) . . ? O1 B3 B1 133.8(4) . . ? C8 B3 B1 101.3(3) . . ? O1 B3 C7 121.9(3) . . ? C8 B3 C7 52.0(2) . . ? B1 B3 C7 100.8(3) . . ? O1 B3 B2 128.6(4) . . ? C8 B3 B2 100.1(3) . . ? B1 B3 B2 59.7(3) . . ? C7 B3 B2 57.7(2) . . ? O1 B3 B4 122.3(4) . . ? C8 B3 B4 57.9(2) . . ? B1 B3 B4 59.3(3) . . ? C7 B3 B4 99.5(3) . . ? B2 B3 B4 106.5(3) . . ? C8 B4 B5 100.9(3) . . ? C8 B4 B1 103.4(3) . . ? B5 B4 B1 61.3(3) . . ? C8 B4 B9 54.8(2) . . ? B5 B4 B9 60.0(3) . . ? B1 B4 B9 108.7(3) . . ? C8 B4 B3 60.4(2) . . ? B5 B4 B3 109.1(3) . . ? B1 B4 B3 59.8(3) . . ? B9 B4 B3 108.0(3) . . ? B4 B5 B10 113.2(3) . . ? B4 B5 B9 60.9(3) . . ? B10 B5 B9 63.2(3) . . ? B4 B5 B1 59.8(3) . . ? B10 B5 B1 110.1(4) . . ? B9 B5 B1 108.1(3) . . ? B4 B5 B6 107.3(3) . . ? B10 B5 B6 59.6(3) . . ? B9 B5 B6 107.4(3) . . ? B1 B5 B6 59.3(3) . . ? B2 B6 B11 61.4(3) . . ? B2 B6 B10 112.8(3) . . ? B11 B6 B10 62.4(3) . . ? B2 B6 B1 60.1(3) . . ? B11 B6 B1 109.0(3) . . ? B10 B6 B1 110.2(4) . . ? B2 B6 B5 107.9(3) . . ? B11 B6 B5 107.0(3) . . ? B10 B6 B5 59.0(3) . . ? B1 B6 B5 60.1(3) . . ? C8 B9 B5 104.7(3) . . ? C8 B9 B4 60.9(2) . . ? B5 B9 B4 59.0(3) . . ? C8 B9 B10 106.0(3) . . ? B5 B9 B10 58.1(3) . . ? B4 B9 B10 107.5(3) . . ? B5 B10 B6 61.4(3) . . ? B5 B10 B11 105.9(4) . . ? B6 B10 B11 58.7(3) . . ? B5 B10 B9 58.7(3) . . ? B6 B10 B9 105.3(3) . . ? B11 B10 B9 101.2(3) . . ? C7 B11 B6 104.0(3) . . ? C7 B11 B2 60.1(3) . . ? B6 B11 B2 58.9(3) . . ? C7 B11 B10 105.6(3) . . ? B6 B11 B10 58.9(3) . . ? B2 B11 B10 107.9(3) . . ? C6 C1 C2 119.7(4) . . ? C9 C2 C1 120.6(4) . . ? C5 C4 C9 118.0(3) . . ? C5 C4 P1 125.7(3) . . ? C9 C4 P1 116.1(3) . . ? C4 C5 C6 120.8(4) . . ? C1 C6 C5 120.2(4) . . ? C8 C7 B11 114.2(3) . . ? C8 C7 B2 112.5(3) . . ? B11 C7 B2 65.1(3) . . ? C8 C7 B3 63.8(2) . . ? B11 C7 B3 117.5(3) . . ? B2 C7 B3 61.2(2) . . ? C8 C7 S1 117.0(2) . . ? B11 C7 S1 119.2(3) . . ? B2 C7 S1 118.6(3) . . ? B3 C7 S1 113.2(2) . . ? C7 C8 B9 112.7(3) . . ? C7 C8 B4 112.1(3) . . ? B9 C8 B4 64.4(3) . . ? C7 C8 B3 64.1(2) . . ? B9 C8 B3 117.2(3) . . ? B4 C8 B3 61.6(2) . . ? C7 C8 P1 113.6(2) . . ? B9 C8 P1 121.6(3) . . ? B4 C8 P1 123.6(3) . . ? B3 C8 P1 113.8(2) . . ? C2 C9 C4 120.6(4) . . ? C11 C10 C15 118.6(3) . . ? C11 C10 P1 122.4(3) . . ? C15 C10 P1 118.7(3) . . ? C12 C11 C10 119.6(4) . . ? C13 C12 C11 121.0(4) . . ? C14 C13 C12 119.9(4) . . ? C13 C14 C15 121.1(4) . . ? C14 C15 C10 119.7(4) . . ? C17 C16 C20 108.0(4) . . ? C17 C16 C21 125.9(4) . . ? C20 C16 C21 125.7(4) . . ? C17 C16 Ir1 73.5(2) . . ? C20 C16 Ir1 72.6(2) . . ? C21 C16 Ir1 125.7(3) . . ? C18 C17 C16 107.5(4) . . ? C18 C17 C22 126.2(4) . . ? C16 C17 C22 126.3(4) . . ? C18 C17 Ir1 70.2(2) . . ? C16 C17 Ir1 68.4(2) . . ? C22 C17 Ir1 126.6(3) . . ? C17 C18 C19 108.3(4) . . ? C17 C18 C23 126.4(4) . . ? C19 C18 C23 124.7(4) . . ? C17 C18 Ir1 72.6(2) . . ? C19 C18 Ir1 71.4(2) . . ? C23 C18 Ir1 128.7(3) . . ? C20 C19 C18 108.1(4) . . ? C20 C19 C24 126.8(4) . . ? C18 C19 C24 125.1(5) . . ? C20 C19 Ir1 71.5(2) . . ? C18 C19 Ir1 70.1(2) . . ? C24 C19 Ir1 123.5(3) . . ? C19 C20 C16 107.8(4) . . ? C19 C20 C25 126.2(4) . . ? C16 C20 C25 126.0(4) . . ? C19 C20 Ir1 71.5(2) . . ? C16 C20 Ir1 68.7(2) . . ? C25 C20 Ir1 125.8(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.493 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.092 # Attachment '3b.cif' data_f90407c _database_code_depnum_ccdc_archive 'CCDC 746419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H39 B9 Cl2 O3 P Rh S' _chemical_formula_weight 733.70 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 '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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.934(12) _cell_length_b 11.386(9) _cell_length_c 22.427(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.797(13) _cell_angle_gamma 90.00 _cell_volume 3746(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 545 _cell_measurement_theta_min 2.346 _cell_measurement_theta_max 19.928 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8993 _exptl_absorpt_correction_T_max 0.9312 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 8.00 _diffrn_reflns_number 15207 _diffrn_reflns_av_R_equivalents 0.1377 _diffrn_reflns_av_sigmaI/netI 0.2319 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6590 _reflns_number_gt 2652 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0888P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6590 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1603 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2089 _refine_ls_wR_factor_gt 0.1843 _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_restrained_S_all 0.818 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.30400(6) 0.80814(7) 0.80708(4) 0.0433(3) Uani 1 1 d . . . S1 S 0.2929(2) 0.6559(2) 0.74081(12) 0.0498(7) Uani 1 1 d . . . P1 P 0.22008(18) 0.9062(2) 0.72557(12) 0.0416(7) Uani 1 1 d . . . O1 O 0.4135(4) 0.8635(6) 0.7568(3) 0.0504(18) Uani 1 1 d . . . O2 O 0.3661(5) 0.5736(6) 0.7592(3) 0.059(2) Uani 1 1 d . . . O3 O 0.2017(5) 0.6049(5) 0.7258(3) 0.0576(19) Uani 1 1 d . . . B1 B 0.4449(9) 0.8585(12) 0.6318(6) 0.062(4) Uani 1 1 d . . . H1 H 0.5147 0.8924 0.6354 0.074 Uiso 1 1 calc R . . B2 B 0.3546(8) 0.9509(11) 0.6405(5) 0.046(3) Uani 1 1 d . . . H2 H 0.3666 1.0446 0.6512 0.056 Uiso 1 1 calc R . . B3 B 0.3905(9) 0.8409(10) 0.6933(5) 0.051(3) Uani 1 1 d . . . B4 B 0.4212(9) 0.7144(11) 0.6567(6) 0.062(4) Uani 1 1 d . . . H4 H 0.4762 0.6556 0.6784 0.075 Uiso 1 1 calc R . . B5 B 0.3993(11) 0.7408(12) 0.5796(6) 0.074(5) Uani 1 1 d . . . H5 H 0.4410 0.6993 0.5499 0.089 Uiso 1 1 calc R . . B6 B 0.3535(10) 0.8924(13) 0.5692(6) 0.072(4) Uani 1 1 d . . . H6 H 0.3639 0.9505 0.5319 0.087 Uiso 1 1 calc R . . B9 B 0.3200(11) 0.6603(12) 0.6113(6) 0.066(4) Uani 1 1 d . . . H9 H 0.2836 0.5759 0.6051 0.079 Uiso 1 1 calc R . . B10 B 0.2785(11) 0.7651(14) 0.5515(6) 0.076(5) Uani 1 1 d . . . H10 H 0.2255 0.7337 0.5140 0.092 Uiso 1 1 calc R . . H10' H 0.234(11) 0.698(14) 0.588(7) 0.18(6) Uiso 1 1 d . . . B11 B 0.2500(10) 0.8956(12) 0.5949(6) 0.063(4) Uani 1 1 d . . . H11 H 0.1794 0.9264 0.5803 0.076 Uiso 1 1 calc R . . C1 C -0.0839(8) 0.8249(13) 0.6787(6) 0.082(4) Uani 1 1 d . . . H1A H -0.1460 0.8082 0.6708 0.099 Uiso 1 1 calc R . . C2 C -0.0266(8) 0.7616(11) 0.6517(6) 0.082(4) Uani 1 1 d . . . H2A H -0.0484 0.7004 0.6255 0.098 Uiso 1 1 calc R . . C3 C 0.5076(7) 0.8679(12) 0.7850(5) 0.080(4) Uani 1 1 d . . . H3A H 0.5327 0.7900 0.7874 0.120 Uiso 1 1 calc R . . H3B H 0.5133 0.9000 0.8251 0.120 Uiso 1 1 calc R . . H3C H 0.5402 0.9166 0.7613 0.120 Uiso 1 1 calc R . . C4 C 0.1017(6) 0.8795(8) 0.7040(4) 0.043(2) Uani 1 1 d . . . C5 C 0.0407(7) 0.9404(11) 0.7307(5) 0.064(3) Uani 1 1 d . . . H5A H 0.0613 1.0005 0.7579 0.077 Uiso 1 1 calc R . . C6 C -0.0511(8) 0.9134(11) 0.7177(5) 0.068(3) Uani 1 1 d . . . H6A H -0.0914 0.9566 0.7360 0.082 Uiso 1 1 calc R . . C7 C 0.2780(6) 0.8568(8) 0.6657(4) 0.038(2) Uani 1 1 d . . . C8 C 0.3149(7) 0.7294(8) 0.6737(4) 0.045(3) Uani 1 1 d . . . C9 C 0.0672(7) 0.7898(10) 0.6639(5) 0.068(3) Uani 1 1 d . . . H9A H 0.1069 0.7474 0.6447 0.082 Uiso 1 1 calc R . . C10 C 0.2282(7) 1.0628(9) 0.7262(5) 0.045(3) Uani 1 1 d . . . C11 C 0.2935(8) 1.1175(10) 0.7665(5) 0.062(3) Uani 1 1 d . . . H11A H 0.3323 1.0728 0.7951 0.074 Uiso 1 1 calc R . . C12 C 0.3044(10) 1.2408(11) 0.7665(7) 0.085(4) Uani 1 1 d . . . H12A H 0.3495 1.2770 0.7948 0.102 Uiso 1 1 calc R . . C13 C 0.2492(12) 1.3041(12) 0.7254(8) 0.094(5) Uani 1 1 d . . . H13 H 0.2556 1.3853 0.7258 0.112 Uiso 1 1 calc R . . C14 C 0.1837(11) 1.2539(12) 0.6828(8) 0.094(5) Uani 1 1 d . . . H14 H 0.1479 1.2991 0.6529 0.113 Uiso 1 1 calc R . . C15 C 0.1716(8) 1.1320(10) 0.6853(5) 0.067(3) Uani 1 1 d . . . H15 H 0.1240 1.0971 0.6585 0.080 Uiso 1 1 calc R . . C16 C 0.2894(8) 0.6866(10) 0.8843(4) 0.056(3) Uani 1 1 d . . . C17 C 0.3702(8) 0.7457(11) 0.8990(5) 0.058(3) Uani 1 1 d . . . C18 C 0.3506(8) 0.8741(10) 0.9019(4) 0.055(3) Uani 1 1 d . . . C19 C 0.2563(8) 0.8875(9) 0.8863(4) 0.054(3) Uani 1 1 d . . . C20 C 0.2168(7) 0.7734(9) 0.8700(4) 0.054(3) Uani 1 1 d . . . C21 C 0.2766(8) 0.5576(8) 0.8812(5) 0.073(4) Uani 1 1 d . . . H21A H 0.3279 0.5217 0.8683 0.109 Uiso 1 1 calc R . . H21B H 0.2219 0.5392 0.8528 0.109 Uiso 1 1 calc R . . H21C H 0.2717 0.5282 0.9206 0.109 Uiso 1 1 calc R . . C22 C 0.4617(8) 0.6882(11) 0.9154(5) 0.081(4) Uani 1 1 d . . . H22A H 0.4732 0.6679 0.9577 0.121 Uiso 1 1 calc R . . H22B H 0.5080 0.7415 0.9075 0.121 Uiso 1 1 calc R . . H22C H 0.4627 0.6184 0.8915 0.121 Uiso 1 1 calc R . . C23 C 0.4183(8) 0.9668(11) 0.9255(5) 0.086(4) Uani 1 1 d . . . H23A H 0.4052 1.0365 0.9014 0.129 Uiso 1 1 calc R . . H23B H 0.4785 0.9395 0.9234 0.129 Uiso 1 1 calc R . . H23C H 0.4148 0.9841 0.9669 0.129 Uiso 1 1 calc R . . C24 C 0.1998(9) 1.0007(10) 0.8892(5) 0.088(4) Uani 1 1 d . . . H24A H 0.2386 1.0681 0.8898 0.132 Uiso 1 1 calc R . . H24B H 0.1741 0.9997 0.9254 0.132 Uiso 1 1 calc R . . H24C H 0.1517 1.0045 0.8543 0.132 Uiso 1 1 calc R . . C25 C 0.1167(8) 0.7475(12) 0.8564(5) 0.089(4) Uani 1 1 d . . . H25A H 0.0964 0.7288 0.8935 0.134 Uiso 1 1 calc R . . H25B H 0.1054 0.6820 0.8291 0.134 Uiso 1 1 calc R . . H25C H 0.0843 0.8150 0.8380 0.134 Uiso 1 1 calc R . . C26 C 0.2475(19) 0.2000(15) 0.5025(14) 0.31(2) Uani 1 1 d . . . H26A H 0.2540 0.1280 0.5261 0.374 Uiso 1 1 calc R . . H26B H 0.1850 0.2092 0.4813 0.374 Uiso 1 1 calc R . . Cl1 Cl 0.2945(5) 0.3415(5) 0.5519(3) 0.198(3) Uani 1 1 d . . . Cl2 Cl 0.3244(7) 0.2106(6) 0.4554(3) 0.259(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0508(5) 0.0330(4) 0.0482(5) -0.0021(4) 0.0145(4) -0.0023(5) S1 0.068(2) 0.0315(14) 0.0544(16) -0.0018(12) 0.0214(15) -0.0006(13) P1 0.0465(17) 0.0312(14) 0.0484(16) -0.0015(12) 0.0124(13) 0.0000(12) O1 0.046(5) 0.048(4) 0.060(5) 0.003(3) 0.016(4) -0.004(3) O2 0.078(5) 0.042(4) 0.057(5) 0.008(4) 0.014(4) 0.021(4) O3 0.068(5) 0.031(4) 0.076(5) -0.001(4) 0.019(4) -0.005(4) B1 0.054(9) 0.079(10) 0.057(8) 0.008(7) 0.021(7) 0.011(7) B2 0.045(8) 0.040(7) 0.057(8) 0.011(6) 0.016(6) -0.001(6) B3 0.063(9) 0.049(8) 0.043(7) 0.003(6) 0.018(6) 0.000(6) B4 0.071(10) 0.048(8) 0.077(9) 0.012(7) 0.038(8) 0.022(7) B5 0.104(12) 0.062(9) 0.070(10) 0.007(7) 0.050(9) 0.025(9) B6 0.086(11) 0.075(10) 0.065(9) 0.010(8) 0.035(9) 0.011(9) B9 0.089(11) 0.052(9) 0.063(9) -0.017(7) 0.031(8) 0.002(8) B10 0.082(12) 0.091(12) 0.051(9) -0.018(8) 0.000(8) -0.015(9) B11 0.068(10) 0.060(9) 0.066(9) 0.002(7) 0.025(8) 0.009(7) C1 0.040(8) 0.099(11) 0.107(10) -0.015(9) 0.011(7) -0.015(8) C2 0.044(8) 0.079(9) 0.123(11) -0.015(8) 0.020(8) -0.011(7) C3 0.035(7) 0.122(11) 0.078(9) -0.031(8) -0.001(6) -0.022(7) C4 0.041(6) 0.039(6) 0.049(6) 0.002(5) 0.009(5) -0.007(5) C5 0.042(8) 0.079(9) 0.072(8) -0.002(7) 0.017(6) 0.002(6) C6 0.052(8) 0.074(9) 0.079(9) 0.010(7) 0.016(7) 0.013(7) C7 0.033(6) 0.031(5) 0.048(6) 0.002(4) 0.004(5) -0.005(4) C8 0.051(7) 0.041(6) 0.047(6) 0.001(5) 0.016(5) 0.007(5) C9 0.045(7) 0.072(9) 0.086(9) -0.015(7) 0.009(6) 0.013(6) C10 0.041(6) 0.036(6) 0.057(7) 0.008(5) 0.006(5) -0.002(5) C11 0.072(9) 0.049(7) 0.071(8) -0.004(6) 0.033(7) 0.004(7) C12 0.094(11) 0.042(7) 0.132(13) -0.024(8) 0.055(10) -0.024(8) C13 0.122(13) 0.027(7) 0.146(14) 0.014(9) 0.065(11) 0.019(9) C14 0.113(13) 0.043(8) 0.140(15) 0.018(9) 0.057(11) 0.014(9) C15 0.076(9) 0.042(7) 0.085(9) 0.005(6) 0.023(8) 0.006(6) C16 0.075(8) 0.053(7) 0.043(6) 0.005(6) 0.023(6) 0.001(7) C17 0.057(8) 0.069(8) 0.049(7) 0.002(6) 0.015(6) -0.002(7) C18 0.068(9) 0.053(7) 0.044(7) 0.010(5) 0.016(6) 0.009(6) C19 0.078(9) 0.043(7) 0.047(6) -0.009(5) 0.026(6) 0.001(6) C20 0.049(7) 0.060(8) 0.052(7) -0.001(5) 0.011(5) -0.002(6) C21 0.124(11) 0.034(6) 0.063(7) 0.023(6) 0.024(7) -0.001(7) C22 0.067(8) 0.094(10) 0.076(8) 0.033(8) 0.001(7) 0.010(8) C23 0.102(11) 0.090(10) 0.066(8) -0.010(7) 0.015(8) -0.030(8) C24 0.131(12) 0.062(8) 0.078(9) -0.006(7) 0.038(8) 0.009(8) C25 0.085(10) 0.106(11) 0.084(10) -0.016(8) 0.034(8) -0.020(8) C26 0.46(4) 0.044(10) 0.56(5) 0.066(19) 0.43(4) 0.023(17) Cl1 0.293(8) 0.121(5) 0.188(6) 0.002(4) 0.061(6) 0.043(5) Cl2 0.418(13) 0.117(5) 0.216(7) -0.011(5) -0.008(8) 0.009(7) _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 Rh1 C20 2.128(10) . ? Rh1 C19 2.225(10) . ? Rh1 C17 2.229(11) . ? Rh1 C18 2.239(11) . ? Rh1 O1 2.243(6) . ? Rh1 C16 2.259(10) . ? Rh1 S1 2.269(3) . ? Rh1 P1 2.302(3) . ? S1 O2 1.440(7) . ? S1 O3 1.460(7) . ? S1 C8 1.805(9) . ? P1 C4 1.769(10) . ? P1 C10 1.787(10) . ? P1 C7 1.818(9) . ? O1 B3 1.425(13) . ? O1 C3 1.430(11) . ? B1 B3 1.739(16) . ? B1 B2 1.751(17) . ? B1 B4 1.790(18) . ? B1 B6 1.806(19) . ? B1 B5 1.82(2) . ? B2 B6 1.730(17) . ? B2 C7 1.736(14) . ? B2 B3 1.737(16) . ? B2 B11 1.812(18) . ? B3 C7 1.688(15) . ? B3 C8 1.702(15) . ? B3 B4 1.760(17) . ? B4 C8 1.709(15) . ? B4 B5 1.725(18) . ? B4 B9 1.77(2) . ? B5 B9 1.750(19) . ? B5 B10 1.82(2) . ? B5 B6 1.86(2) . ? B6 B11 1.748(18) . ? B6 B10 1.83(2) . ? B9 C8 1.620(15) . ? B9 B10 1.82(2) . ? B10 B11 1.869(19) . ? B11 C7 1.625(15) . ? C1 C2 1.347(16) . ? C1 C6 1.364(16) . ? C2 C9 1.414(14) . ? C4 C5 1.368(13) . ? C4 C9 1.395(14) . ? C5 C6 1.382(14) . ? C7 C8 1.551(12) . ? C10 C11 1.352(13) . ? C10 C15 1.374(13) . ? C11 C12 1.413(15) . ? C12 C13 1.329(18) . ? C13 C14 1.358(19) . ? C14 C15 1.402(16) . ? C16 C17 1.368(14) . ? C16 C20 1.457(14) . ? C16 C21 1.482(14) . ? C17 C18 1.495(14) . ? C17 C22 1.497(14) . ? C18 C19 1.393(14) . ? C18 C23 1.489(15) . ? C19 C20 1.444(14) . ? C19 C24 1.549(15) . ? C20 C25 1.498(15) . ? C26 Cl2 1.705(18) . ? C26 Cl1 2.01(3) . ? 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 C20 Rh1 C19 38.7(4) . . ? C20 Rh1 C17 63.2(4) . . ? C19 Rh1 C17 62.9(4) . . ? C20 Rh1 C18 63.4(4) . . ? C19 Rh1 C18 36.4(4) . . ? C17 Rh1 C18 39.1(4) . . ? C20 Rh1 O1 168.3(3) . . ? C19 Rh1 O1 131.2(3) . . ? C17 Rh1 O1 108.4(3) . . ? C18 Rh1 O1 104.9(3) . . ? C20 Rh1 C16 38.7(4) . . ? C19 Rh1 C16 63.0(4) . . ? C17 Rh1 C16 35.5(4) . . ? C18 Rh1 C16 62.3(4) . . ? O1 Rh1 C16 137.9(3) . . ? C20 Rh1 S1 108.3(3) . . ? C19 Rh1 S1 146.9(3) . . ? C17 Rh1 S1 109.1(3) . . ? C18 Rh1 S1 148.2(3) . . ? O1 Rh1 S1 81.74(19) . . ? C16 Rh1 S1 91.6(3) . . ? C20 Rh1 P1 107.9(3) . . ? C19 Rh1 P1 103.2(3) . . ? C17 Rh1 P1 166.0(3) . . ? C18 Rh1 P1 128.1(3) . . ? O1 Rh1 P1 78.73(19) . . ? C16 Rh1 P1 142.1(3) . . ? S1 Rh1 P1 83.59(11) . . ? O2 S1 O3 115.7(4) . . ? O2 S1 C8 107.0(4) . . ? O3 S1 C8 107.4(5) . . ? O2 S1 Rh1 110.6(3) . . ? O3 S1 Rh1 113.9(3) . . ? C8 S1 Rh1 100.9(3) . . ? C4 P1 C10 103.7(5) . . ? C4 P1 C7 109.5(4) . . ? C10 P1 C7 105.9(4) . . ? C4 P1 Rh1 120.1(3) . . ? C10 P1 Rh1 116.8(4) . . ? C7 P1 Rh1 100.0(3) . . ? B3 O1 C3 118.8(8) . . ? B3 O1 Rh1 112.9(6) . . ? C3 O1 Rh1 122.5(6) . . ? B3 B1 B2 59.7(7) . . ? B3 B1 B4 59.8(7) . . ? B2 B1 B4 108.3(9) . . ? B3 B1 B6 104.1(9) . . ? B2 B1 B6 58.2(7) . . ? B4 B1 B6 105.9(10) . . ? B3 B1 B5 104.5(9) . . ? B2 B1 B5 108.1(10) . . ? B4 B1 B5 57.0(7) . . ? B6 B1 B5 61.5(8) . . ? B6 B2 C7 99.8(9) . . ? B6 B2 B3 107.5(9) . . ? C7 B2 B3 58.2(6) . . ? B6 B2 B1 62.5(7) . . ? C7 B2 B1 103.5(8) . . ? B3 B2 B1 59.8(7) . . ? B6 B2 B11 59.1(7) . . ? C7 B2 B11 54.5(6) . . ? B3 B2 B11 104.9(9) . . ? B1 B2 B11 109.2(9) . . ? O1 B3 C7 112.6(9) . . ? O1 B3 C8 114.6(8) . . ? C7 B3 C8 54.4(6) . . ? O1 B3 B2 122.5(9) . . ? C7 B3 B2 60.9(6) . . ? C8 B3 B2 104.9(9) . . ? O1 B3 B1 135.4(10) . . ? C7 B3 B1 106.1(8) . . ? C8 B3 B1 105.5(8) . . ? B2 B3 B1 60.5(7) . . ? O1 B3 B4 125.3(9) . . ? C7 B3 B4 104.1(9) . . ? C8 B3 B4 59.1(7) . . ? B2 B3 B4 110.3(8) . . ? B1 B3 B4 61.5(7) . . ? C8 B4 B5 101.4(10) . . ? C8 B4 B3 58.7(6) . . ? B5 B4 B3 107.9(9) . . ? C8 B4 B9 55.5(7) . . ? B5 B4 B9 60.2(8) . . ? B3 B4 B9 106.6(9) . . ? C8 B4 B1 103.0(8) . . ? B5 B4 B1 62.5(7) . . ? B3 B4 B1 58.7(7) . . ? B9 B4 B1 109.7(10) . . ? B4 B5 B9 61.1(8) . . ? B4 B5 B10 111.3(10) . . ? B9 B5 B10 61.2(9) . . ? B4 B5 B1 60.5(7) . . ? B9 B5 B1 108.9(9) . . ? B10 B5 B1 109.7(9) . . ? B4 B5 B6 106.5(9) . . ? B9 B5 B6 106.1(9) . . ? B10 B5 B6 59.7(8) . . ? B1 B5 B6 58.8(7) . . ? B2 B6 B11 62.8(7) . . ? B2 B6 B1 59.3(7) . . ? B11 B6 B1 109.6(9) . . ? B2 B6 B10 113.9(9) . . ? B11 B6 B10 62.9(8) . . ? B1 B6 B10 110.0(10) . . ? B2 B6 B5 107.6(9) . . ? B11 B6 B5 107.8(10) . . ? B1 B6 B5 59.7(8) . . ? B10 B6 B5 59.1(8) . . ? C8 B9 B5 104.0(10) . . ? C8 B9 B4 60.4(7) . . ? B5 B9 B4 58.7(8) . . ? C8 B9 B10 104.7(9) . . ? B5 B9 B10 61.3(8) . . ? B4 B9 B10 109.5(10) . . ? B9 B10 B5 57.6(8) . . ? B9 B10 B6 104.4(10) . . ? B5 B10 B6 61.2(8) . . ? B9 B10 B11 102.5(9) . . ? B5 B10 B11 104.4(9) . . ? B6 B10 B11 56.4(7) . . ? C7 B11 B6 103.6(10) . . ? C7 B11 B2 60.4(7) . . ? B6 B11 B2 58.1(7) . . ? C7 B11 B10 104.5(9) . . ? B6 B11 B10 60.7(8) . . ? B2 B11 B10 108.3(9) . . ? C2 C1 C6 120.1(12) . . ? C1 C2 C9 118.8(12) . . ? C5 C4 C9 117.2(10) . . ? C5 C4 P1 120.4(8) . . ? C9 C4 P1 122.1(8) . . ? C4 C5 C6 120.7(12) . . ? C1 C6 C5 121.5(12) . . ? C8 C7 B11 112.9(8) . . ? C8 C7 B3 63.2(6) . . ? B11 C7 B3 116.4(8) . . ? C8 C7 B2 112.0(8) . . ? B11 C7 B2 65.2(7) . . ? B3 C7 B2 61.0(6) . . ? C8 C7 P1 114.3(6) . . ? B11 C7 P1 124.5(7) . . ? B3 C7 P1 109.9(6) . . ? B2 C7 P1 118.9(6) . . ? C7 C8 B9 115.3(8) . . ? C7 C8 B3 62.3(6) . . ? B9 C8 B3 116.7(8) . . ? C7 C8 B4 113.1(8) . . ? B9 C8 B4 64.1(8) . . ? B3 C8 B4 62.1(7) . . ? C7 C8 S1 114.5(6) . . ? B9 C8 S1 122.7(7) . . ? B3 C8 S1 110.3(6) . . ? B4 C8 S1 117.5(7) . . ? C4 C9 C2 121.6(11) . . ? C11 C10 C15 117.3(10) . . ? C11 C10 P1 120.3(8) . . ? C15 C10 P1 122.3(9) . . ? C10 C11 C12 121.8(12) . . ? C13 C12 C11 118.8(14) . . ? C12 C13 C14 122.1(13) . . ? C13 C14 C15 118.0(14) . . ? C10 C15 C14 121.8(13) . . ? C17 C16 C20 107.8(10) . . ? C17 C16 C21 126.8(11) . . ? C20 C16 C21 125.4(11) . . ? C17 C16 Rh1 71.1(6) . . ? C20 C16 Rh1 65.8(6) . . ? C21 C16 Rh1 127.0(7) . . ? C16 C17 C18 108.6(10) . . ? C16 C17 C22 124.6(11) . . ? C18 C17 C22 126.5(11) . . ? C16 C17 Rh1 73.4(6) . . ? C18 C17 Rh1 70.8(6) . . ? C22 C17 Rh1 126.4(7) . . ? C19 C18 C23 126.8(11) . . ? C19 C18 C17 107.1(10) . . ? C23 C18 C17 125.6(11) . . ? C19 C18 Rh1 71.3(6) . . ? C23 C18 Rh1 130.2(8) . . ? C17 C18 Rh1 70.1(6) . . ? C18 C19 C20 108.1(10) . . ? C18 C19 C24 127.8(11) . . ? C20 C19 C24 124.0(11) . . ? C18 C19 Rh1 72.3(6) . . ? C20 C19 Rh1 67.0(5) . . ? C24 C19 Rh1 129.1(8) . . ? C19 C20 C16 107.6(10) . . ? C19 C20 C25 125.0(10) . . ? C16 C20 C25 125.7(11) . . ? C19 C20 Rh1 74.3(6) . . ? C16 C20 Rh1 75.5(6) . . ? C25 C20 Rh1 127.8(8) . . ? Cl2 C26 Cl1 94.5(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.813 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.128 # Attachment '4.cif' data_f90611d _database_code_depnum_ccdc_archive 'CCDC 746420' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H74 B18 Ir2 O3 P2 S2' _chemical_formula_weight 1440.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 24.198(7) _cell_length_b 12.368(4) _cell_length_c 22.609(6) _cell_angle_alpha 90.00 _cell_angle_beta 114.066(3) _cell_angle_gamma 90.00 _cell_volume 6178(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 960 _cell_measurement_theta_min 2.472 _cell_measurement_theta_max 24.217 _exptl_crystal_description prism _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2840 _exptl_absorpt_coefficient_mu 4.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6165 _exptl_absorpt_correction_T_max 0.6638 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.26 _diffrn_reflns_number 25157 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.01 _reflns_number_total 10908 _reflns_number_gt 7359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10908 _refine_ls_number_parameters 728 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1933 _refine_ls_wR_factor_gt 0.1782 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.37860(2) 0.17388(4) 0.96607(2) 0.04004(16) Uani 1 1 d . . . P1 P 0.33029(13) 0.2930(2) 0.88154(13) 0.0363(6) Uani 1 1 d . . . S1 S 0.46329(13) 0.2118(3) 0.94160(13) 0.0488(8) Uani 1 1 d . . . O1 O 0.3342(6) -0.0327(9) 0.8933(5) 0.088(3) Uani 1 1 d . . . O2 O 0.3687(5) 0.0873(7) 0.8095(4) 0.065(3) Uani 1 1 d . . . B3 B 0.3896(7) 0.1876(14) 0.7990(7) 0.057(4) Uani 1 1 d . . . B2 B 0.4609(7) 0.2206(17) 0.8053(7) 0.066(5) Uani 1 1 d . . . H2 H 0.4939 0.1552 0.8128 0.079 Uiso 1 1 calc R . . B11 B 0.4822(8) 0.3456(15) 0.8446(8) 0.062(4) Uani 1 1 d . . . H11 H 0.5193 0.3792 0.8875 0.074 Uiso 1 1 calc R . . B10 B 0.4356(7) 0.4437(16) 0.7875(8) 0.070(5) Uani 1 1 d . . . H10 H 0.4517 0.5274 0.7997 0.084 Uiso 1 1 calc R . . H11' H 0.455(6) 0.383(12) 0.866(7) 0.09(5) Uiso 1 1 d . . . B9 B 0.3602(7) 0.4156(13) 0.7841(7) 0.051(4) Uani 1 1 d . . . H9 H 0.3373 0.4822 0.7973 0.062 Uiso 1 1 calc R . . B4 B 0.3386(7) 0.2861(13) 0.7455(6) 0.049(4) Uani 1 1 d . . . H4 H 0.2917 0.2642 0.7140 0.059 Uiso 1 1 calc R . . B1 B 0.4033(9) 0.2354(16) 0.7323(8) 0.073(5) Uani 1 1 d . . . H1 H 0.3980 0.1829 0.6911 0.087 Uiso 1 1 calc R . . B6 B 0.4592(8) 0.3320(18) 0.7609(8) 0.080(6) Uani 1 1 d . . . H6 H 0.4916 0.3402 0.7383 0.096 Uiso 1 1 calc R . . B5 B 0.3831(8) 0.3853(16) 0.7221(7) 0.067(5) Uani 1 1 d . . . H5 H 0.3642 0.4296 0.6759 0.081 Uiso 1 1 calc R . . C7 C 0.4371(5) 0.2694(11) 0.8609(5) 0.044(3) Uani 1 1 d . . . C8 C 0.3696(5) 0.3064(10) 0.8294(5) 0.042(3) Uani 1 1 d . . . C3 C 0.3604(9) 0.0054(15) 0.7668(7) 0.112(7) Uani 1 1 d . . . H3A H 0.3429 0.0333 0.7235 0.168 Uiso 1 1 calc R . . H3B H 0.3339 -0.0476 0.7722 0.168 Uiso 1 1 calc R . . H3C H 0.3988 -0.0275 0.7747 0.168 Uiso 1 1 calc R . . C4 C 0.2514(5) 0.2684(9) 0.8348(6) 0.046(3) Uani 1 1 d . . . C5 C 0.2188(5) 0.3278(10) 0.7781(6) 0.049(3) Uani 1 1 d . . . H5A H 0.2380 0.3816 0.7648 0.058 Uiso 1 1 calc R . . C6 C 0.1580(6) 0.3064(12) 0.7421(6) 0.062(4) Uani 1 1 d . . . H6A H 0.1370 0.3461 0.7047 0.074 Uiso 1 1 calc R . . C1 C 0.1284(6) 0.2294(12) 0.7601(7) 0.062(4) Uani 1 1 d . . . H1A H 0.0873 0.2179 0.7361 0.074 Uiso 1 1 calc R . . C2 C 0.1595(6) 0.1679(11) 0.8142(6) 0.062(4) Uani 1 1 d . . . H2A H 0.1400 0.1126 0.8261 0.074 Uiso 1 1 calc R . . C9 C 0.2194(6) 0.1890(12) 0.8505(6) 0.062(4) Uani 1 1 d . . . H9A H 0.2396 0.1479 0.8875 0.074 Uiso 1 1 calc R . . C10 C 0.3334(5) 0.4301(9) 0.9109(5) 0.039(3) Uani 1 1 d . . . C11 C 0.3907(6) 0.4797(11) 0.9375(6) 0.057(3) Uani 1 1 d . . . H11A H 0.4246 0.4426 0.9388 0.069 Uiso 1 1 calc R . . C12 C 0.3965(8) 0.5841(13) 0.9617(7) 0.076(5) Uani 1 1 d . . . H12 H 0.4342 0.6172 0.9787 0.091 Uiso 1 1 calc R . . C13 C 0.3480(10) 0.6375(14) 0.9608(8) 0.089(5) Uani 1 1 d . . . H13 H 0.3530 0.7067 0.9784 0.106 Uiso 1 1 calc R . . C14 C 0.2902(7) 0.5926(12) 0.9343(6) 0.064(4) Uani 1 1 d . . . H14 H 0.2566 0.6311 0.9327 0.076 Uiso 1 1 calc R . . C15 C 0.2848(6) 0.4866(10) 0.9099(5) 0.051(3) Uani 1 1 d . . . H15 H 0.2468 0.4542 0.8926 0.062 Uiso 1 1 calc R . . C16 C 0.3533(6) 0.0506(13) 0.9145(6) 0.060(4) Uani 1 1 d . . . C17 C 0.3527(6) 0.2445(11) 1.0447(5) 0.053(3) Uani 1 1 d . . . C18 C 0.3396(6) 0.1350(12) 1.0371(5) 0.055(3) Uani 1 1 d . . . C19 C 0.3922(7) 0.0751(12) 1.0541(6) 0.061(4) Uani 1 1 d . . . C20 C 0.4382(6) 0.1411(14) 1.0682(6) 0.062(4) Uani 1 1 d . . . C21 C 0.4168(7) 0.2528(14) 1.0628(6) 0.072(5) Uani 1 1 d . . . C22 C 0.3094(9) 0.3289(16) 1.0402(8) 0.113(8) Uani 1 1 d . . . H22A H 0.2699 0.2975 1.0277 0.170 Uiso 1 1 calc R . . H22B H 0.3084 0.3811 1.0083 0.170 Uiso 1 1 calc R . . H22C H 0.3213 0.3637 1.0815 0.170 Uiso 1 1 calc R . . C23 C 0.2787(8) 0.087(2) 1.0262(8) 0.118(8) Uani 1 1 d . . . H23A H 0.2794 0.0618 1.0667 0.177 Uiso 1 1 calc R . . H23B H 0.2702 0.0272 0.9966 0.177 Uiso 1 1 calc R . . H23C H 0.2478 0.1408 1.0083 0.177 Uiso 1 1 calc R . . C24 C 0.3972(10) -0.0445(15) 1.0603(8) 0.113(7) Uani 1 1 d . . . H24A H 0.4356 -0.0671 1.0613 0.170 Uiso 1 1 calc R . . H24B H 0.3652 -0.0772 1.0239 0.170 Uiso 1 1 calc R . . H24C H 0.3941 -0.0664 1.0995 0.170 Uiso 1 1 calc R . . C25 C 0.5054(6) 0.114(2) 1.0944(8) 0.122(9) Uani 1 1 d . . . H25A H 0.5170 0.0747 1.1343 0.183 Uiso 1 1 calc R . . H25B H 0.5285 0.1795 1.1020 0.183 Uiso 1 1 calc R . . H25C H 0.5131 0.0703 1.0634 0.183 Uiso 1 1 calc R . . C26 C 0.4531(11) 0.3556(17) 1.0846(8) 0.137(10) Uani 1 1 d . . . H26A H 0.4261 0.4158 1.0776 0.206 Uiso 1 1 calc R . . H26B H 0.4772 0.3659 1.0603 0.206 Uiso 1 1 calc R . . H26C H 0.4790 0.3505 1.1299 0.206 Uiso 1 1 calc R . . Ir2 Ir 0.10150(2) 0.74592(4) 0.62908(2) 0.05035(18) Uani 1 1 d . . . P2 P 0.15893(14) 0.8088(2) 0.57771(14) 0.0402(7) Uani 1 1 d . . . S2 S 0.04064(14) 0.6746(3) 0.53695(15) 0.0518(8) Uani 1 1 d . . . O3 O 0.1677(5) 0.5574(7) 0.5545(5) 0.069(3) Uani 1 1 d . . . B8 B 0.0245(9) 0.6931(18) 0.4012(8) 0.080(6) Uani 1 1 d . . . H8 H -0.0220 0.7188 0.3912 0.096 Uiso 1 1 calc R . . B7 B 0.0697(8) 0.5763(16) 0.4312(8) 0.073(5) Uani 1 1 d . . . H7A H 0.0485 0.4974 0.4306 0.088 Uiso 1 1 calc R . . B12 B 0.1386(7) 0.6101(12) 0.4973(7) 0.053(4) Uani 1 1 d . . . B13 B 0.1785(7) 0.6996(12) 0.4642(7) 0.052(4) Uani 1 1 d . . . H13A H 0.2282 0.7016 0.4852 0.062 Uiso 1 1 calc R . . B14 B 0.1366(8) 0.8145(14) 0.4362(7) 0.062(4) Uani 1 1 d . . . H14A H 0.1452 0.9018 0.4441 0.074 Uiso 1 1 calc R . . B15 B 0.0644(9) 0.777(2) 0.3649(8) 0.079(6) Uani 1 1 d . . . H15A H 0.0368 0.8428 0.3341 0.095 Uiso 1 1 calc R . . H15' H 0.063(6) 0.818(10) 0.404(6) 0.06(4) Uiso 1 1 d . . . B16 B 0.0674(10) 0.638(2) 0.3617(8) 0.091(7) Uani 1 1 d . . . H16 H 0.0447 0.5976 0.3146 0.110 Uiso 1 1 calc R . . B17 B 0.1383(9) 0.5856(13) 0.4204(8) 0.069(5) Uani 1 1 d . . . H17 H 0.1613 0.5146 0.4117 0.083 Uiso 1 1 calc R . . B18 B 0.1354(12) 0.7202(18) 0.3816(9) 0.092(7) Uani 1 1 d . . . H18 H 0.1568 0.7372 0.3481 0.110 Uiso 1 1 calc R . . C27 C 0.0709(6) 0.6866(10) 0.4784(5) 0.047(3) Uani 1 1 d . . . C28 C 0.1310(5) 0.7513(9) 0.4973(5) 0.039(3) Uani 1 1 d . . . C29 C 0.1481(9) 0.4541(13) 0.5671(10) 0.108(6) Uani 1 1 d . . . H29A H 0.1047 0.4528 0.5501 0.161 Uiso 1 1 calc R . . H29B H 0.1645 0.4416 0.6130 0.161 Uiso 1 1 calc R . . H29C H 0.1618 0.3986 0.5466 0.161 Uiso 1 1 calc R . . C30 C 0.1435(6) 0.9549(10) 0.5653(6) 0.049(3) Uani 1 1 d . . . C31 C 0.0885(6) 0.9889(11) 0.5221(7) 0.059(3) Uani 1 1 d . . . H31 H 0.0616 0.9379 0.4954 0.071 Uiso 1 1 calc R . . C32 C 0.0711(7) 1.0932(13) 0.5164(8) 0.073(4) Uani 1 1 d . . . H32 H 0.0330 1.1135 0.4864 0.088 Uiso 1 1 calc R . . C33 C 0.1093(9) 1.1671(13) 0.5542(10) 0.090(5) Uani 1 1 d . . . H33 H 0.0976 1.2393 0.5495 0.108 Uiso 1 1 calc R . . C34 C 0.1650(9) 1.1394(13) 0.5995(9) 0.085(5) Uani 1 1 d . . . H34 H 0.1906 1.1920 0.6260 0.102 Uiso 1 1 calc R . . C35 C 0.1834(7) 1.0316(11) 0.6057(7) 0.063(4) Uani 1 1 d . . . H35 H 0.2213 1.0112 0.6362 0.075 Uiso 1 1 calc R . . C36 C 0.2391(3) 0.7926(7) 0.6161(4) 0.045(3) Uani 1 1 d GU . . C37 C 0.2751(4) 0.8565(7) 0.5965(4) 0.061(4) Uani 1 1 d G . . H37 H 0.2578 0.9107 0.5660 0.074 Uiso 1 1 calc R . . C38 C 0.3367(4) 0.8401(8) 0.6220(5) 0.074(4) Uani 1 1 d G . . H38 H 0.3611 0.8833 0.6088 0.089 Uiso 1 1 calc R . . C39 C 0.3624(4) 0.7598(9) 0.6672(5) 0.083(5) Uani 1 1 d G . . H39 H 0.4040 0.7488 0.6844 0.100 Uiso 1 1 calc R . . C40 C 0.3264(4) 0.6959(8) 0.6868(5) 0.090(5) Uani 1 1 d G . . H40 H 0.3437 0.6417 0.7173 0.108 Uiso 1 1 calc R . . C41 C 0.2647(4) 0.7123(7) 0.6612(4) 0.065(3) Uani 1 1 d GU . . H41 H 0.2404 0.6691 0.6745 0.078 Uiso 1 1 calc R . . C42 C 0.1456(6) 0.8236(11) 0.7256(5) 0.049(3) Uani 1 1 d . . . C43 C 0.0849(6) 0.8571(11) 0.6923(5) 0.050(3) Uani 1 1 d . . . C44 C 0.0449(7) 0.7661(13) 0.6828(6) 0.063(4) Uani 1 1 d . . . C45 C 0.0828(8) 0.6750(12) 0.7071(7) 0.066(4) Uani 1 1 d . . . C46 C 0.1430(7) 0.7092(12) 0.7312(6) 0.060(4) Uani 1 1 d . . . C47 C 0.2016(6) 0.8927(13) 0.7513(7) 0.077(5) Uani 1 1 d . . . H47A H 0.1937 0.9599 0.7281 0.115 Uiso 1 1 calc R . . H47B H 0.2340 0.8556 0.7458 0.115 Uiso 1 1 calc R . . H47C H 0.2127 0.9067 0.7965 0.115 Uiso 1 1 calc R . . C48 C 0.0620(8) 0.9735(13) 0.6748(8) 0.089(5) Uani 1 1 d . . . H48A H 0.0343 0.9904 0.6941 0.133 Uiso 1 1 calc R . . H48B H 0.0418 0.9803 0.6286 0.133 Uiso 1 1 calc R . . H48C H 0.0957 1.0225 0.6909 0.133 Uiso 1 1 calc R . . C49 C -0.0214(8) 0.772(2) 0.6578(8) 0.123(9) Uani 1 1 d . . . H49A H -0.0382 0.7013 0.6431 0.184 Uiso 1 1 calc R . . H49B H -0.0364 0.8217 0.6223 0.184 Uiso 1 1 calc R . . H49C H -0.0329 0.7953 0.6916 0.184 Uiso 1 1 calc R . . C50 C 0.0575(12) 0.5625(14) 0.7093(10) 0.137(10) Uani 1 1 d . . . H50A H 0.0145 0.5673 0.6967 0.206 Uiso 1 1 calc R . . H50B H 0.0763 0.5344 0.7526 0.206 Uiso 1 1 calc R . . H50C H 0.0656 0.5152 0.6802 0.206 Uiso 1 1 calc R . . C51 C 0.1976(9) 0.6383(17) 0.7687(9) 0.113(7) Uani 1 1 d . . . H51A H 0.1902 0.5978 0.8009 0.170 Uiso 1 1 calc R . . H51B H 0.2327 0.6830 0.7893 0.170 Uiso 1 1 calc R . . H51C H 0.2044 0.5893 0.7393 0.170 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0388(3) 0.0506(3) 0.0297(2) 0.00474(19) 0.01289(19) 0.0064(2) P1 0.0366(15) 0.0445(16) 0.0275(14) 0.0002(12) 0.0128(12) 0.0054(13) S1 0.0365(15) 0.078(2) 0.0308(14) 0.0082(14) 0.0123(13) 0.0116(15) O1 0.130(10) 0.055(7) 0.078(7) -0.013(6) 0.042(7) -0.018(7) O2 0.097(7) 0.051(6) 0.046(5) -0.011(4) 0.027(5) 0.000(5) B3 0.064(10) 0.070(11) 0.039(8) -0.011(7) 0.024(7) 0.018(8) B2 0.050(9) 0.110(14) 0.047(9) -0.016(9) 0.030(8) -0.003(9) B11 0.053(9) 0.085(12) 0.058(9) 0.001(8) 0.035(8) 0.008(8) B10 0.064(10) 0.085(13) 0.068(11) 0.008(9) 0.032(9) -0.015(9) B9 0.062(9) 0.053(9) 0.048(8) 0.002(7) 0.032(7) -0.001(7) B4 0.048(8) 0.081(10) 0.021(6) 0.003(6) 0.016(6) 0.000(8) B1 0.092(13) 0.096(14) 0.040(9) -0.002(8) 0.037(9) 0.011(11) B6 0.053(10) 0.139(19) 0.050(10) 0.006(10) 0.023(8) 0.007(11) B5 0.068(11) 0.099(14) 0.038(8) 0.011(8) 0.025(8) -0.004(10) C7 0.041(6) 0.078(9) 0.017(5) 0.002(5) 0.016(5) 0.007(6) C8 0.042(6) 0.057(7) 0.025(6) -0.004(5) 0.012(5) 0.004(6) C3 0.143(17) 0.095(14) 0.055(10) -0.039(9) -0.004(10) -0.004(13) C4 0.049(7) 0.042(7) 0.053(7) -0.005(6) 0.028(6) 0.003(6) C5 0.043(7) 0.050(7) 0.048(7) 0.012(6) 0.014(6) 0.008(6) C6 0.055(8) 0.072(10) 0.048(8) 0.008(7) 0.010(7) 0.018(7) C1 0.044(7) 0.066(9) 0.067(9) -0.003(7) 0.013(7) -0.003(7) C2 0.039(7) 0.071(10) 0.065(9) 0.020(7) 0.010(6) -0.010(6) C9 0.054(8) 0.082(10) 0.045(7) 0.015(7) 0.015(6) 0.014(7) C10 0.041(6) 0.052(7) 0.024(5) 0.007(5) 0.013(5) 0.009(5) C11 0.061(8) 0.071(9) 0.042(7) -0.005(6) 0.024(6) 0.006(7) C12 0.089(11) 0.069(10) 0.080(10) -0.031(8) 0.045(9) -0.048(9) C13 0.142(17) 0.058(10) 0.078(11) -0.021(8) 0.057(12) 0.009(11) C14 0.062(9) 0.074(10) 0.050(8) -0.006(7) 0.019(7) 0.014(8) C15 0.058(8) 0.056(8) 0.036(6) -0.001(6) 0.014(6) 0.022(6) C16 0.066(9) 0.071(10) 0.054(8) 0.012(7) 0.035(7) 0.012(8) C17 0.079(9) 0.061(9) 0.017(5) 0.009(5) 0.018(6) 0.026(7) C18 0.053(8) 0.084(10) 0.029(6) 0.009(6) 0.019(6) -0.009(7) C19 0.069(9) 0.072(10) 0.047(7) 0.018(7) 0.027(7) 0.012(8) C20 0.055(8) 0.093(12) 0.033(7) 0.005(7) 0.012(6) 0.019(8) C21 0.081(11) 0.114(14) 0.019(6) -0.013(7) 0.021(7) -0.052(10) C22 0.143(17) 0.159(19) 0.066(11) 0.032(11) 0.071(12) 0.084(15) C23 0.092(12) 0.20(2) 0.069(11) 0.011(13) 0.042(10) -0.049(15) C24 0.165(19) 0.102(15) 0.086(12) 0.050(11) 0.064(13) 0.056(14) C25 0.045(9) 0.24(3) 0.073(11) 0.060(14) 0.018(8) 0.030(13) C26 0.23(3) 0.134(18) 0.068(12) -0.041(12) 0.081(15) -0.100(19) Ir2 0.0593(3) 0.0609(4) 0.0362(3) -0.0071(2) 0.0249(2) -0.0131(3) P2 0.0451(17) 0.0424(18) 0.0339(15) -0.0027(13) 0.0170(13) -0.0030(14) S2 0.0481(17) 0.069(2) 0.0425(17) -0.0072(15) 0.0224(15) -0.0136(16) O3 0.088(7) 0.049(6) 0.076(6) 0.019(5) 0.040(6) 0.013(5) B8 0.081(13) 0.119(17) 0.040(9) -0.013(10) 0.024(9) -0.013(12) B7 0.090(12) 0.082(13) 0.053(9) -0.036(9) 0.035(9) -0.038(11) B12 0.068(10) 0.051(9) 0.044(8) -0.009(7) 0.027(7) -0.008(8) B13 0.059(9) 0.061(9) 0.045(8) -0.023(7) 0.030(7) -0.018(8) B14 0.070(10) 0.074(11) 0.045(8) 0.015(8) 0.027(8) -0.005(9) B15 0.075(12) 0.122(17) 0.042(9) 0.023(10) 0.025(9) 0.031(12) B16 0.103(15) 0.128(19) 0.033(9) -0.021(10) 0.018(9) -0.036(14) B17 0.107(14) 0.046(9) 0.067(11) -0.019(8) 0.048(11) -0.003(9) B18 0.15(2) 0.100(15) 0.054(11) -0.001(10) 0.077(13) -0.007(15) C27 0.054(7) 0.056(8) 0.032(6) -0.003(5) 0.019(6) -0.004(6) C28 0.038(6) 0.055(7) 0.019(5) 0.006(5) 0.007(5) -0.001(5) C29 0.148(17) 0.044(9) 0.154(18) 0.017(10) 0.086(15) -0.002(11) C30 0.067(8) 0.039(7) 0.046(7) -0.013(6) 0.026(6) -0.011(6) C31 0.060(8) 0.049(8) 0.066(9) 0.005(7) 0.022(7) 0.006(7) C32 0.060(9) 0.062(10) 0.098(12) 0.010(9) 0.032(9) 0.008(8) C33 0.090(13) 0.053(10) 0.139(17) 0.019(11) 0.059(13) 0.004(9) C34 0.095(13) 0.058(10) 0.091(12) -0.022(9) 0.026(11) -0.014(9) C35 0.071(9) 0.057(9) 0.066(9) -0.005(7) 0.034(8) -0.009(7) C36 0.019(4) 0.042(4) 0.053(4) -0.041(4) -0.006(3) 0.013(3) C37 0.047(8) 0.067(9) 0.063(9) -0.006(7) 0.016(7) -0.001(7) C38 0.062(9) 0.087(12) 0.076(10) 0.002(9) 0.032(9) 0.001(8) C39 0.038(8) 0.110(14) 0.089(12) -0.036(10) 0.013(8) 0.005(9) C40 0.062(10) 0.101(14) 0.098(13) 0.016(11) 0.023(10) 0.013(10) C41 0.076(5) 0.073(5) 0.064(5) -0.015(4) 0.047(4) -0.029(4) C42 0.059(8) 0.067(9) 0.023(5) -0.007(5) 0.018(5) 0.009(7) C43 0.062(8) 0.060(8) 0.039(7) 0.000(6) 0.032(6) 0.005(7) C44 0.084(10) 0.083(11) 0.041(7) -0.010(7) 0.046(8) -0.004(9) C45 0.094(12) 0.064(9) 0.062(9) -0.006(7) 0.054(9) -0.013(9) C46 0.075(10) 0.073(10) 0.036(7) 0.020(6) 0.028(7) 0.019(8) C47 0.064(9) 0.095(12) 0.062(9) -0.035(9) 0.016(7) -0.035(9) C48 0.109(13) 0.081(12) 0.084(11) 0.002(9) 0.049(11) 0.017(10) C49 0.074(12) 0.25(3) 0.057(10) -0.033(13) 0.041(9) -0.055(14) C50 0.27(3) 0.066(12) 0.138(17) -0.008(11) 0.15(2) -0.042(15) C51 0.126(17) 0.115(15) 0.092(13) 0.030(12) 0.036(13) 0.062(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C16 1.865(16) . ? Ir1 C20 2.206(12) . ? Ir1 C18 2.223(11) . ? Ir1 C21 2.224(12) . ? Ir1 C19 2.242(12) . ? Ir1 C17 2.286(11) . ? Ir1 P1 2.316(3) . ? Ir1 S1 2.377(3) . ? P1 C4 1.791(13) . ? P1 C8 1.799(11) . ? P1 C10 1.812(12) . ? S1 C7 1.815(10) . ? O1 C16 1.150(17) . ? O2 C3 1.355(16) . ? O2 B3 1.40(2) . ? B3 B2 1.72(2) . ? B3 C7 1.729(19) . ? B3 C8 1.771(18) . ? B3 B1 1.77(2) . ? B3 B4 1.80(2) . ? B2 B1 1.68(2) . ? B2 C7 1.694(17) . ? B2 B6 1.70(3) . ? B2 B11 1.75(3) . ? B11 C7 1.59(2) . ? B11 B6 1.75(2) . ? B11 B10 1.80(2) . ? B10 B5 1.67(2) . ? B10 B6 1.70(3) . ? B10 B9 1.83(2) . ? B9 C8 1.653(18) . ? B9 B5 1.75(2) . ? B9 B4 1.80(2) . ? B4 C8 1.751(15) . ? B4 B1 1.82(2) . ? B4 B5 1.85(2) . ? B1 B6 1.72(3) . ? B1 B5 1.91(3) . ? B6 B5 1.81(2) . ? C7 C8 1.559(15) . ? C4 C9 1.383(18) . ? C4 C5 1.408(16) . ? C5 C6 1.386(18) . ? C6 C1 1.350(19) . ? C1 C2 1.374(18) . ? C2 C9 1.368(18) . ? C10 C15 1.360(15) . ? C10 C11 1.407(17) . ? C11 C12 1.386(19) . ? C12 C13 1.34(2) . ? C13 C14 1.39(2) . ? C14 C15 1.407(19) . ? C17 C18 1.386(19) . ? C17 C21 1.44(2) . ? C17 C22 1.452(19) . ? C18 C19 1.387(18) . ? C18 C23 1.513(19) . ? C19 C20 1.31(2) . ? C19 C24 1.49(2) . ? C20 C21 1.46(2) . ? C20 C25 1.524(19) . ? C21 C26 1.51(2) . ? Ir2 C43 2.137(12) . ? Ir2 C46 2.157(12) . ? Ir2 C45 2.176(13) . ? Ir2 C44 2.184(12) . ? Ir2 S2 2.187(3) . ? Ir2 C42 2.219(11) . ? Ir2 P2 2.281(3) . ? P2 C36 1.784(7) . ? P2 C28 1.806(11) . ? P2 C30 1.843(13) . ? S2 C27 1.762(11) . ? O3 B12 1.359(17) . ? O3 C29 1.432(17) . ? B8 C27 1.65(2) . ? B8 B16 1.76(3) . ? B8 B7 1.77(3) . ? B8 B15 1.83(3) . ? B7 C27 1.72(2) . ? B7 B16 1.73(3) . ? B7 B12 1.78(2) . ? B7 B17 1.78(2) . ? B12 C28 1.757(19) . ? B12 B17 1.763(19) . ? B12 C27 1.79(2) . ? B12 B13 1.82(2) . ? B13 B14 1.71(2) . ? B13 C28 1.728(17) . ? B13 B18 1.75(3) . ? B13 B17 1.77(2) . ? B14 C28 1.641(17) . ? B14 B18 1.69(3) . ? B14 B15 1.89(3) . ? B15 B16 1.73(3) . ? B15 B18 1.75(3) . ? B16 B17 1.81(3) . ? B16 B18 1.83(3) . ? B17 B18 1.87(3) . ? C27 C28 1.560(16) . ? C30 C31 1.358(18) . ? C30 C35 1.394(17) . ? C31 C32 1.347(19) . ? C32 C33 1.33(2) . ? C33 C34 1.36(2) . ? C34 C35 1.39(2) . ? C36 C37 1.377(5) . ? C36 C41 1.377(5) . ? C37 C38 1.377(5) . ? C38 C39 1.377(5) . ? C39 C40 1.377(5) . ? C40 C41 1.377(5) . ? C42 C43 1.413(17) . ? C42 C46 1.425(19) . ? C42 C47 1.502(18) . ? C43 C44 1.442(19) . ? C43 C48 1.53(2) . ? C44 C45 1.41(2) . ? C44 C49 1.47(2) . ? C45 C46 1.40(2) . ? C45 C50 1.53(2) . ? C46 C51 1.52(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 Ir1 C20 114.4(6) . . ? C16 Ir1 C18 98.5(5) . . ? C20 Ir1 C18 59.5(5) . . ? C16 Ir1 C21 150.8(6) . . ? C20 Ir1 C21 38.6(6) . . ? C18 Ir1 C21 60.8(5) . . ? C16 Ir1 C19 90.1(6) . . ? C20 Ir1 C19 34.3(5) . . ? C18 Ir1 C19 36.2(5) . . ? C21 Ir1 C19 60.9(6) . . ? C16 Ir1 C17 132.4(5) . . ? C20 Ir1 C17 61.7(5) . . ? C18 Ir1 C17 35.8(5) . . ? C21 Ir1 C17 37.2(5) . . ? C19 Ir1 C17 60.4(5) . . ? C16 Ir1 P1 94.4(4) . . ? C20 Ir1 P1 151.1(5) . . ? C18 Ir1 P1 120.9(4) . . ? C21 Ir1 P1 113.6(5) . . ? C19 Ir1 P1 157.1(4) . . ? C17 Ir1 P1 101.1(3) . . ? C16 Ir1 S1 96.3(4) . . ? C20 Ir1 S1 91.3(4) . . ? C18 Ir1 S1 150.6(3) . . ? C21 Ir1 S1 95.2(4) . . ? C19 Ir1 S1 119.0(4) . . ? C17 Ir1 S1 129.9(4) . . ? P1 Ir1 S1 82.84(10) . . ? C4 P1 C8 110.5(5) . . ? C4 P1 C10 104.5(5) . . ? C8 P1 C10 101.5(5) . . ? C4 P1 Ir1 115.9(4) . . ? C8 P1 Ir1 112.0(4) . . ? C10 P1 Ir1 111.2(3) . . ? C7 S1 Ir1 109.3(4) . . ? C3 O2 B3 120.1(12) . . ? O2 B3 B2 128.0(13) . . ? O2 B3 C7 123.3(11) . . ? B2 B3 C7 58.8(8) . . ? O2 B3 C8 119.8(11) . . ? B2 B3 C8 101.2(12) . . ? C7 B3 C8 52.9(7) . . ? O2 B3 B1 130.3(12) . . ? B2 B3 B1 57.5(10) . . ? C7 B3 B1 101.6(12) . . ? C8 B3 B1 103.3(11) . . ? O2 B3 B4 121.2(13) . . ? B2 B3 B4 106.6(12) . . ? C7 B3 B4 101.3(11) . . ? C8 B3 B4 58.7(7) . . ? B1 B3 B4 61.3(9) . . ? B1 B2 C7 107.1(11) . . ? B1 B2 B6 61.3(11) . . ? C7 B2 B6 102.5(13) . . ? B1 B2 B3 62.8(10) . . ? C7 B2 B3 60.8(8) . . ? B6 B2 B3 111.2(13) . . ? B1 B2 B11 110.9(14) . . ? C7 B2 B11 55.1(8) . . ? B6 B2 B11 61.0(11) . . ? B3 B2 B11 109.1(11) . . ? C7 B11 B6 104.4(13) . . ? C7 B11 B2 60.6(9) . . ? B6 B11 B2 57.9(11) . . ? C7 B11 B10 106.1(11) . . ? B6 B11 B10 57.2(10) . . ? B2 B11 B10 105.2(13) . . ? B5 B10 B6 65.0(11) . . ? B5 B10 B11 111.8(14) . . ? B6 B10 B11 60.1(10) . . ? B5 B10 B9 59.7(9) . . ? B6 B10 B9 107.7(13) . . ? B11 B10 B9 103.0(11) . . ? C8 B9 B5 108.3(11) . . ? C8 B9 B4 60.8(7) . . ? B5 B9 B4 62.8(9) . . ? C8 B9 B10 104.2(11) . . ? B5 B9 B10 55.7(9) . . ? B4 B9 B10 106.1(11) . . ? C8 B4 B9 55.5(7) . . ? C8 B4 B3 59.7(7) . . ? B9 B4 B3 107.0(10) . . ? C8 B4 B1 102.1(10) . . ? B9 B4 B1 106.7(11) . . ? B3 B4 B1 58.5(8) . . ? C8 B4 B5 99.9(10) . . ? B9 B4 B5 57.2(9) . . ? B3 B4 B5 108.7(11) . . ? B1 B4 B5 62.6(10) . . ? B2 B1 B6 59.8(11) . . ? B2 B1 B3 59.7(9) . . ? B6 B1 B3 107.6(12) . . ? B2 B1 B4 107.5(10) . . ? B6 B1 B4 107.2(13) . . ? B3 B1 B4 60.2(8) . . ? B2 B1 B5 107.1(13) . . ? B6 B1 B5 59.6(10) . . ? B3 B1 B5 107.4(11) . . ? B4 B1 B5 59.4(9) . . ? B2 B6 B10 112.5(12) . . ? B2 B6 B1 58.9(11) . . ? B10 B6 B1 111.8(13) . . ? B2 B6 B11 61.1(10) . . ? B10 B6 B11 62.8(10) . . ? B1 B6 B11 109.1(13) . . ? B2 B6 B5 110.9(13) . . ? B10 B6 B5 56.8(10) . . ? B1 B6 B5 65.3(11) . . ? B11 B6 B5 107.5(12) . . ? B10 B5 B9 64.7(9) . . ? B10 B5 B6 58.2(10) . . ? B9 B5 B6 106.4(11) . . ? B10 B5 B4 110.8(10) . . ? B9 B5 B4 59.9(8) . . ? B6 B5 B4 102.5(12) . . ? B10 B5 B1 104.4(12) . . ? B9 B5 B1 105.1(11) . . ? B6 B5 B1 55.1(11) . . ? B4 B5 B1 58.0(9) . . ? C8 C7 B11 114.1(11) . . ? C8 C7 B2 112.0(9) . . ? B11 C7 B2 64.3(10) . . ? C8 C7 B3 64.9(8) . . ? B11 C7 B3 116.7(10) . . ? B2 C7 B3 60.3(8) . . ? C8 C7 S1 116.5(7) . . ? B11 C7 S1 118.2(9) . . ? B2 C7 S1 121.4(10) . . ? B3 C7 S1 115.4(9) . . ? C7 C8 B9 112.2(10) . . ? C7 C8 B4 111.1(8) . . ? B9 C8 B4 63.6(8) . . ? C7 C8 B3 62.2(8) . . ? B9 C8 B3 115.3(9) . . ? B4 C8 B3 61.6(8) . . ? C7 C8 P1 114.1(7) . . ? B9 C8 P1 120.3(8) . . ? B4 C8 P1 126.0(8) . . ? B3 C8 P1 118.6(9) . . ? C9 C4 C5 116.0(11) . . ? C9 C4 P1 122.9(10) . . ? C5 C4 P1 121.1(9) . . ? C6 C5 C4 120.2(12) . . ? C1 C6 C5 121.5(13) . . ? C6 C1 C2 119.6(13) . . ? C9 C2 C1 119.3(13) . . ? C2 C9 C4 123.3(12) . . ? C15 C10 C11 118.5(12) . . ? C15 C10 P1 124.6(9) . . ? C11 C10 P1 116.8(9) . . ? C12 C11 C10 119.8(13) . . ? C13 C12 C11 120.5(15) . . ? C12 C13 C14 121.9(14) . . ? C13 C14 C15 117.3(13) . . ? C10 C15 C14 122.0(13) . . ? O1 C16 Ir1 165.0(12) . . ? C18 C17 C21 105.7(12) . . ? C18 C17 C22 124.8(16) . . ? C21 C17 C22 129.2(16) . . ? C18 C17 Ir1 69.7(7) . . ? C21 C17 Ir1 69.1(7) . . ? C22 C17 Ir1 129.7(9) . . ? C17 C18 C19 110.5(12) . . ? C17 C18 C23 124.3(15) . . ? C19 C18 C23 124.0(16) . . ? C17 C18 Ir1 74.6(7) . . ? C19 C18 Ir1 72.7(7) . . ? C23 C18 Ir1 129.7(9) . . ? C20 C19 C18 109.2(13) . . ? C20 C19 C24 124.7(16) . . ? C18 C19 C24 126.0(16) . . ? C20 C19 Ir1 71.3(8) . . ? C18 C19 Ir1 71.2(7) . . ? C24 C19 Ir1 127.0(11) . . ? C19 C20 C21 109.3(13) . . ? C19 C20 C25 128.5(17) . . ? C21 C20 C25 121.8(17) . . ? C19 C20 Ir1 74.4(8) . . ? C21 C20 Ir1 71.4(7) . . ? C25 C20 Ir1 125.9(10) . . ? C17 C21 C20 105.1(12) . . ? C17 C21 C26 124.7(18) . . ? C20 C21 C26 129.0(18) . . ? C17 C21 Ir1 73.8(7) . . ? C20 C21 Ir1 70.0(7) . . ? C26 C21 Ir1 130.1(9) . . ? C43 Ir2 C46 63.4(5) . . ? C43 Ir2 C45 63.8(5) . . ? C46 Ir2 C45 37.6(6) . . ? C43 Ir2 C44 39.0(5) . . ? C46 Ir2 C44 63.4(5) . . ? C45 Ir2 C44 37.8(5) . . ? C43 Ir2 S2 131.2(4) . . ? C46 Ir2 S2 140.6(4) . . ? C45 Ir2 S2 109.1(4) . . ? C44 Ir2 S2 104.1(4) . . ? C43 Ir2 C42 37.8(5) . . ? C46 Ir2 C42 38.0(5) . . ? C45 Ir2 C42 63.5(5) . . ? C44 Ir2 C42 64.1(5) . . ? S2 Ir2 C42 168.0(3) . . ? C43 Ir2 P2 116.2(4) . . ? C46 Ir2 P2 120.2(4) . . ? C45 Ir2 P2 157.2(5) . . ? C44 Ir2 P2 153.5(4) . . ? S2 Ir2 P2 88.05(11) . . ? C42 Ir2 P2 101.8(3) . . ? C36 P2 C28 109.3(5) . . ? C36 P2 C30 107.3(5) . . ? C28 P2 C30 105.3(5) . . ? C36 P2 Ir2 118.8(3) . . ? C28 P2 Ir2 108.8(4) . . ? C30 P2 Ir2 106.5(4) . . ? C27 S2 Ir2 110.9(4) . . ? B12 O3 C29 122.1(13) . . ? C27 B8 B16 103.3(14) . . ? C27 B8 B7 60.4(9) . . ? B16 B8 B7 58.5(11) . . ? C27 B8 B15 104.3(13) . . ? B16 B8 B15 57.6(11) . . ? B7 B8 B15 106.2(14) . . ? C27 B7 B16 101.5(13) . . ? C27 B7 B8 56.2(9) . . ? B16 B7 B8 60.3(12) . . ? C27 B7 B12 61.3(8) . . ? B16 B7 B12 109.5(12) . . ? B8 B7 B12 110.6(12) . . ? C27 B7 B17 104.6(11) . . ? B16 B7 B17 62.1(11) . . ? B8 B7 B17 111.1(13) . . ? B12 B7 B17 59.5(9) . . ? O3 B12 C28 119.4(10) . . ? O3 B12 B17 130.4(13) . . ? C28 B12 B17 102.3(10) . . ? O3 B12 B7 129.2(13) . . ? C28 B12 B7 99.9(11) . . ? B17 B12 B7 60.3(9) . . ? O3 B12 C27 123.5(11) . . ? C28 B12 C27 52.2(7) . . ? B17 B12 C27 102.7(10) . . ? B7 B12 C27 57.9(9) . . ? O3 B12 B13 121.8(12) . . ? C28 B12 B13 57.8(7) . . ? B17 B12 B13 59.2(8) . . ? B7 B12 B13 105.6(10) . . ? C27 B12 B13 99.6(10) . . ? B14 B13 C28 57.0(8) . . ? B14 B13 B18 58.5(10) . . ? C28 B13 B18 101.4(12) . . ? B14 B13 B17 110.4(12) . . ? C28 B13 B17 103.2(10) . . ? B18 B13 B17 64.2(10) . . ? B14 B13 B12 109.0(11) . . ? C28 B13 B12 59.3(8) . . ? B18 B13 B12 110.1(12) . . ? B17 B13 B12 58.9(8) . . ? C28 B14 B18 107.7(12) . . ? C28 B14 B13 62.1(8) . . ? B18 B14 B13 61.8(11) . . ? C28 B14 B15 103.7(11) . . ? B18 B14 B15 58.2(12) . . ? B13 B14 B15 108.4(13) . . ? B16 B15 B18 63.5(13) . . ? B16 B15 B8 59.3(12) . . ? B18 B15 B8 109.0(15) . . ? B16 B15 B14 103.9(13) . . ? B18 B15 B14 55.2(10) . . ? B8 B15 B14 103.3(11) . . ? B7 B16 B15 113.0(13) . . ? B7 B16 B8 61.1(11) . . ? B15 B16 B8 63.2(12) . . ? B7 B16 B17 60.3(11) . . ? B15 B16 B17 111.7(13) . . ? B8 B16 B17 110.3(12) . . ? B7 B16 B18 109.3(12) . . ? B15 B16 B18 58.9(12) . . ? B8 B16 B18 108.5(14) . . ? B17 B16 B18 61.9(11) . . ? B12 B17 B13 62.0(8) . . ? B12 B17 B7 60.2(9) . . ? B13 B17 B7 107.8(10) . . ? B12 B17 B16 106.4(12) . . ? B13 B17 B16 105.4(12) . . ? B7 B17 B16 57.5(10) . . ? B12 B17 B18 107.1(11) . . ? B13 B17 B18 57.3(10) . . ? B7 B17 B18 105.3(14) . . ? B16 B17 B18 59.6(12) . . ? B14 B18 B13 59.7(10) . . ? B14 B18 B15 66.6(12) . . ? B13 B18 B15 113.3(12) . . ? B14 B18 B16 108.0(14) . . ? B13 B18 B16 105.5(12) . . ? B15 B18 B16 57.6(13) . . ? B14 B18 B17 106.7(10) . . ? B13 B18 B17 58.5(9) . . ? B15 B18 B17 107.8(15) . . ? B16 B18 B17 58.5(12) . . ? C28 C27 B8 115.0(10) . . ? C28 C27 B7 110.8(10) . . ? B8 C27 B7 63.4(11) . . ? C28 C27 S2 117.6(8) . . ? B8 C27 S2 119.2(10) . . ? B7 C27 S2 119.4(9) . . ? C28 C27 B12 62.9(8) . . ? B8 C27 B12 116.3(11) . . ? B7 C27 B12 60.8(9) . . ? S2 C27 B12 113.4(8) . . ? C27 C28 B14 113.6(9) . . ? C27 C28 B13 113.6(9) . . ? B14 C28 B13 60.9(9) . . ? C27 C28 B12 64.8(8) . . ? B14 C28 B12 115.4(10) . . ? B13 C28 B12 62.9(8) . . ? C27 C28 P2 113.8(7) . . ? B14 C28 P2 122.3(9) . . ? B13 C28 P2 122.7(8) . . ? B12 C28 P2 113.3(7) . . ? C31 C30 C35 118.3(12) . . ? C31 C30 P2 119.4(10) . . ? C35 C30 P2 121.6(10) . . ? C32 C31 C30 122.8(14) . . ? C33 C32 C31 119.2(15) . . ? C32 C33 C34 121.6(16) . . ? C33 C34 C35 119.6(16) . . ? C34 C35 C30 118.4(14) . . ? C37 C36 C41 120.0 . . ? C37 C36 P2 118.9(6) . . ? C41 C36 P2 120.9(6) . . ? C38 C37 C36 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C40 C41 C36 120.0 . . ? C43 C42 C46 105.2(12) . . ? C43 C42 C47 128.1(13) . . ? C46 C42 C47 126.6(13) . . ? C43 C42 Ir2 67.9(7) . . ? C46 C42 Ir2 68.6(7) . . ? C47 C42 Ir2 128.6(9) . . ? C42 C43 C44 109.8(12) . . ? C42 C43 C48 126.8(13) . . ? C44 C43 C48 123.0(13) . . ? C42 C43 Ir2 74.3(7) . . ? C44 C43 Ir2 72.3(7) . . ? C48 C43 Ir2 125.3(9) . . ? C45 C44 C43 106.0(13) . . ? C45 C44 C49 128.3(17) . . ? C43 C44 C49 125.6(16) . . ? C45 C44 Ir2 70.8(7) . . ? C43 C44 Ir2 68.8(7) . . ? C49 C44 Ir2 128.7(10) . . ? C46 C45 C44 108.5(13) . . ? C46 C45 C50 129.1(18) . . ? C44 C45 C50 122.2(17) . . ? C46 C45 Ir2 70.5(7) . . ? C44 C45 Ir2 71.4(7) . . ? C50 C45 Ir2 127.8(11) . . ? C45 C46 C42 110.1(12) . . ? C45 C46 C51 125.0(16) . . ? C42 C46 C51 124.1(15) . . ? C45 C46 Ir2 71.9(8) . . ? C42 C46 Ir2 73.4(6) . . ? C51 C46 Ir2 129.5(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 6.272 _refine_diff_density_min -3.910 _refine_diff_density_rms 0.191