# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_cutab _database_code_depnum_ccdc_archive 'CCDC 924358' #TrackingRef 'Combined-CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H47 B9 Cl2 Cu P3' _chemical_formula_weight 912.47 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 17.0593(14) _cell_length_b 20.6703(16) _cell_length_c 13.3203(11) _cell_angle_alpha 90.00 _cell_angle_beta 102.592(4) _cell_angle_gamma 90.00 _cell_volume 4584.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 6855 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 30.4 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.731 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7753 _exptl_absorpt_correction_T_max 0.9371 _exptl_absorpt_process_details XPREP loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 0.00 0.1240 0.00 1.00 0.00 0.1250 1.00 0.00 0.00 0.0510 -1.00 0.00 0.00 0.0400 0.00 1.00 -1.00 0.2010 0.00 -1.00 -1.00 0.2030 0.00 -1.00 2.00 0.1600 _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- & \f-scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88097 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetl/netI 0.0400 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 30.03 _reflns_number_total 13399 _reflns_number_gt 8772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SAMRT' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _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^)+(0.0532P)^2^] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13399 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.1029 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.277617(11) 0.501117(8) 0.829930(15) 0.01664(6) Uani 1 1 d . . . P1 P 0.33771(2) 0.421916(17) 0.75688(3) 0.01535(9) Uani 1 1 d . . . P2 P 0.34495(2) 0.576180(17) 0.75891(3) 0.01554(9) Uani 1 1 d . . . P3 P 0.17451(2) 0.504949(18) 0.90581(3) 0.01832(9) Uani 1 1 d . . . C1 C 0.43364(8) 0.45794(7) 0.74480(12) 0.0145(3) Uani 1 1 d . . . C2 C 0.43790(9) 0.53506(7) 0.74630(12) 0.0154(3) Uani 1 1 d . . . B3 B 0.50204(11) 0.56488(9) 0.68524(15) 0.0192(4) Uani 1 1 d . . . H3 H 0.4945(10) 0.6107(8) 0.6541(13) 0.022(5) Uiso 1 1 d . . . B4 B 0.54943(11) 0.49592(9) 0.63622(15) 0.0201(4) Uani 1 1 d . . . H4A H 0.5810(10) 0.4959(6) 0.5710(14) 0.018(4) Uiso 1 1 d . . . H4B H 0.4813(13) 0.4883(9) 0.6086(17) 0.043(6) Uiso 1 1 d . . . B5 B 0.49363(11) 0.42772(9) 0.67643(15) 0.0191(4) Uani 1 1 d . . . H5 H 0.4785(10) 0.3845(9) 0.6355(14) 0.029(5) Uiso 1 1 d . . . B6 B 0.47862(10) 0.49391(8) 0.85911(14) 0.0176(3) Uani 1 1 d . . . H6 H 0.4538 0.4939 0.9303 0.021 Uiso 1 1 calc R . . B7 B 0.52865(11) 0.56257(9) 0.82275(15) 0.0194(4) Uani 1 1 d . . . H7 H 0.5392 0.6071 0.8717 0.023 Uiso 1 1 calc R . . B8 B 0.59608(11) 0.53580(9) 0.75011(14) 0.0198(4) Uani 1 1 d . . . H8 H 0.6523 0.5639 0.7508 0.024 Uiso 1 1 calc R . . B9 B 0.59230(11) 0.44839(9) 0.74554(15) 0.0203(4) Uani 1 1 d . . . H9 H 0.6453 0.4170 0.7430 0.024 Uiso 1 1 calc R . . B10 B 0.52129(10) 0.42414(8) 0.81523(14) 0.0187(4) Uani 1 1 d . . . H10 H 0.5274 0.3776 0.8593 0.022 Uiso 1 1 calc R . . B11 B 0.58220(11) 0.49055(8) 0.86041(15) 0.0197(4) Uani 1 1 d . . . H11 H 0.6291 0.4878 0.9337 0.024 Uiso 1 1 calc R . . C11 C 0.35805(9) 0.34287(7) 0.81613(13) 0.0214(3) Uani 1 1 d . . . C12 C 0.34467(11) 0.33341(9) 0.91400(16) 0.0344(4) Uani 1 1 d . . . H12 H 0.3274 0.3683 0.9503 0.041 Uiso 1 1 calc R . . C13 C 0.35678(13) 0.27207(11) 0.95870(19) 0.0516(6) Uani 1 1 d . . . H13 H 0.3473 0.2652 1.0256 0.062 Uiso 1 1 calc R . . C14 C 0.38236(12) 0.22164(9) 0.9067(2) 0.0489(6) Uani 1 1 d . . . H14 H 0.3907 0.1802 0.9380 0.059 Uiso 1 1 calc R . . C15 C 0.39600(12) 0.23078(8) 0.80946(18) 0.0404(5) Uani 1 1 d . . . H15 H 0.4137 0.1958 0.7738 0.048 Uiso 1 1 calc R . . C16 C 0.38381(11) 0.29129(8) 0.76385(15) 0.0305(4) Uani 1 1 d . . . H16 H 0.3930 0.2977 0.6967 0.037 Uiso 1 1 calc R . . C21 C 0.28355(9) 0.40210(7) 0.62707(12) 0.0182(3) Uani 1 1 d . . . C22 C 0.21816(10) 0.35955(8) 0.61498(15) 0.0288(4) Uani 1 1 d . . . H22 H 0.2043 0.3408 0.6739 0.035 Uiso 1 1 calc R . . C23 C 0.17386(11) 0.34481(9) 0.51845(16) 0.0355(5) Uani 1 1 d . . . H23 H 0.1297 0.3159 0.5112 0.043 Uiso 1 1 calc R . . C24 C 0.19302(11) 0.37177(9) 0.43177(15) 0.0309(4) Uani 1 1 d . . . H24 H 0.1628 0.3608 0.3652 0.037 Uiso 1 1 calc R . . C25 C 0.25640(10) 0.41473(9) 0.44271(14) 0.0278(4) Uani 1 1 d . . . H25 H 0.2693 0.4340 0.3836 0.033 Uiso 1 1 calc R . . C26 C 0.30131(10) 0.42983(8) 0.53979(13) 0.0218(3) Uani 1 1 d . . . H26 H 0.3447 0.4595 0.5466 0.026 Uiso 1 1 calc R . . C31 C 0.28679(9) 0.59585(7) 0.63072(12) 0.0183(3) Uani 1 1 d . . . C32 C 0.31623(10) 0.59621(8) 0.54124(13) 0.0240(4) Uani 1 1 d . . . H32 H 0.3708 0.5852 0.5442 0.029 Uiso 1 1 calc R . . C33 C 0.26664(11) 0.61250(8) 0.44775(14) 0.0297(4) Uani 1 1 d . . . H33 H 0.2872 0.6123 0.3870 0.036 Uiso 1 1 calc R . . C34 C 0.18766(11) 0.62900(9) 0.44255(15) 0.0324(4) Uani 1 1 d . . . H34 H 0.1540 0.6407 0.3785 0.039 Uiso 1 1 calc R . . C35 C 0.15767(11) 0.62850(10) 0.53086(15) 0.0366(5) Uani 1 1 d . . . H35 H 0.1031 0.6396 0.5274 0.044 Uiso 1 1 calc R . . C36 C 0.20653(10) 0.61192(9) 0.62414(14) 0.0286(4) Uani 1 1 d . . . H36 H 0.1852 0.6115 0.6844 0.034 Uiso 1 1 calc R . . C41 C 0.37496(9) 0.65426(7) 0.81616(13) 0.0188(3) Uani 1 1 d . . . C42 C 0.37700(10) 0.70975(7) 0.75716(14) 0.0254(4) Uani 1 1 d . . . H42 H 0.3626 0.7074 0.6842 0.030 Uiso 1 1 calc R . . C43 C 0.40013(12) 0.76859(8) 0.80528(15) 0.0328(4) Uani 1 1 d . . . H43 H 0.4016 0.8063 0.7651 0.039 Uiso 1 1 calc R . . C44 C 0.42092(11) 0.77233(8) 0.91113(15) 0.0311(4) Uani 1 1 d . . . H44 H 0.4362 0.8127 0.9436 0.037 Uiso 1 1 calc R . . C45 C 0.41962(11) 0.71735(8) 0.97042(14) 0.0273(4) Uani 1 1 d . . . H45 H 0.4345 0.7200 1.0433 0.033 Uiso 1 1 calc R . . C46 C 0.39658(10) 0.65855(7) 0.92316(13) 0.0229(3) Uani 1 1 d . . . H46 H 0.3955 0.6210 0.9638 0.027 Uiso 1 1 calc R . . C51 C 0.17026(9) 0.57459(8) 0.98854(13) 0.0217(3) Uani 1 1 d . . . C52 C 0.21052(11) 0.63038(8) 0.97170(15) 0.0303(4) Uani 1 1 d . . . H52 H 0.2389 0.6314 0.9178 0.036 Uiso 1 1 calc R . . C53 C 0.20996(12) 0.68465(9) 1.03237(18) 0.0421(5) Uani 1 1 d . . . H53 H 0.2377 0.7226 1.0199 0.051 Uiso 1 1 calc R . . C54 C 0.16912(13) 0.68350(10) 1.11091(18) 0.0448(5) Uani 1 1 d . . . H54 H 0.1692 0.7205 1.1531 0.054 Uiso 1 1 calc R . . C55 C 0.12830(12) 0.62868(10) 1.12812(16) 0.0421(5) Uani 1 1 d . . . H55 H 0.0996 0.6282 1.1818 0.050 Uiso 1 1 calc R . . C56 C 0.12873(11) 0.57412(9) 1.06771(15) 0.0326(4) Uani 1 1 d . . . H56 H 0.1006 0.5364 1.0803 0.039 Uiso 1 1 calc R . . C61 C 0.08270(10) 0.50778(7) 0.80601(13) 0.0217(3) Uani 1 1 d . . . C62 C 0.01080(10) 0.53314(8) 0.82178(14) 0.0257(4) Uani 1 1 d . . . H62 H 0.0089 0.5528 0.8857 0.031 Uiso 1 1 calc R . . C63 C -0.05809(11) 0.52983(9) 0.74439(15) 0.0318(4) Uani 1 1 d . . . H63 H -0.1070 0.5473 0.7555 0.038 Uiso 1 1 calc R . . C64 C -0.05620(12) 0.50134(8) 0.65142(16) 0.0352(4) Uani 1 1 d . . . H64 H -0.1037 0.4991 0.5987 0.042 Uiso 1 1 calc R . . C65 C 0.01526(12) 0.47590(10) 0.63503(15) 0.0362(4) Uani 1 1 d . . . H65 H 0.0167 0.4561 0.5711 0.043 Uiso 1 1 calc R . . C66 C 0.08422(11) 0.47940(9) 0.71156(14) 0.0292(4) Uani 1 1 d . . . H66 H 0.1331 0.4623 0.6997 0.035 Uiso 1 1 calc R . . C71 C 0.15946(9) 0.43484(7) 0.98290(13) 0.0201(3) Uani 1 1 d . . . C72 C 0.21419(10) 0.42353(8) 1.07468(14) 0.0288(4) Uani 1 1 d . . . H72 H 0.2555 0.4542 1.0989 0.035 Uiso 1 1 calc R . . C73 C 0.20941(11) 0.36835(8) 1.13132(15) 0.0307(4) Uani 1 1 d . . . H73 H 0.2473 0.3611 1.1940 0.037 Uiso 1 1 calc R . . C74 C 0.14952(12) 0.32359(9) 1.09682(16) 0.0374(5) Uani 1 1 d . . . H74 H 0.1462 0.2854 1.1355 0.045 Uiso 1 1 calc R . . C75 C 0.09455(13) 0.33460(9) 1.00597(17) 0.0455(6) Uani 1 1 d . . . H75 H 0.0530 0.3040 0.9824 0.055 Uiso 1 1 calc R . . C76 C 0.09934(11) 0.38996(8) 0.94870(15) 0.0335(4) Uani 1 1 d . . . H76 H 0.0614 0.3971 0.8860 0.040 Uiso 1 1 calc R . . C99 C 0.03568(19) 0.72204(14) 0.8173(2) 0.0804(9) Uani 1 1 d . . . H99A H 0.0935 0.7262 0.8493 0.096 Uiso 1 1 calc R . . H99B H 0.0124 0.6901 0.8579 0.096 Uiso 1 1 calc R . . Cl1 Cl -0.01130(4) 0.79727(3) 0.82346(5) 0.05602(16) Uani 1 1 d . . . Cl2 Cl 0.02567(5) 0.69338(3) 0.69380(6) 0.0758(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu 0.01729(10) 0.01640(9) 0.01818(11) -0.00005(8) 0.00814(7) -0.00053(7) P1 0.01734(19) 0.01266(17) 0.0170(2) 0.00024(15) 0.00586(16) -0.00114(14) P2 0.01777(19) 0.01276(17) 0.0174(2) -0.00025(15) 0.00663(16) 0.00016(14) P3 0.01744(19) 0.02036(19) 0.0187(2) 0.00004(16) 0.00734(15) -0.00105(15) C1 0.0155(7) 0.0138(6) 0.0149(8) -0.0006(6) 0.0047(6) 0.0000(5) C2 0.0175(7) 0.0124(7) 0.0169(8) -0.0002(6) 0.0053(6) -0.0008(5) B3 0.0196(9) 0.0198(8) 0.0193(10) 0.0034(7) 0.0062(7) -0.0027(7) B4 0.0181(8) 0.0278(9) 0.0151(9) -0.0001(8) 0.0052(7) -0.0006(7) B5 0.0192(8) 0.0193(8) 0.0198(10) -0.0033(7) 0.0060(7) 0.0010(7) B6 0.0182(8) 0.0209(8) 0.0138(9) -0.0007(7) 0.0035(6) -0.0017(7) B7 0.0192(8) 0.0208(8) 0.0185(10) -0.0029(7) 0.0048(7) -0.0039(7) B8 0.0178(8) 0.0243(9) 0.0174(10) 0.0011(7) 0.0044(7) -0.0011(7) B9 0.0185(8) 0.0234(9) 0.0197(10) -0.0011(7) 0.0055(7) 0.0021(7) B10 0.0190(8) 0.0193(8) 0.0174(10) 0.0029(7) 0.0035(7) 0.0033(7) B11 0.0176(8) 0.0268(9) 0.0147(9) 0.0005(7) 0.0036(7) -0.0012(7) C11 0.0208(8) 0.0162(7) 0.0263(10) 0.0041(6) 0.0034(7) -0.0030(6) C12 0.0342(10) 0.0353(10) 0.0363(12) 0.0146(8) 0.0130(9) 0.0026(8) C13 0.0500(14) 0.0536(14) 0.0543(16) 0.0336(12) 0.0183(12) 0.0037(11) C14 0.0372(11) 0.0254(10) 0.0791(19) 0.0271(11) 0.0016(11) -0.0023(8) C15 0.0361(11) 0.0159(8) 0.0614(16) 0.0026(9) -0.0062(10) -0.0003(7) C16 0.0348(10) 0.0164(8) 0.0370(12) -0.0008(7) 0.0007(8) 0.0008(7) C21 0.0177(7) 0.0167(7) 0.0200(9) -0.0018(6) 0.0033(6) 0.0012(6) C22 0.0301(9) 0.0275(9) 0.0272(11) 0.0053(7) 0.0025(8) -0.0092(7) C23 0.0346(10) 0.0328(10) 0.0339(12) -0.0004(8) -0.0041(9) -0.0147(8) C24 0.0322(10) 0.0333(9) 0.0225(10) -0.0032(8) -0.0046(8) 0.0013(8) C25 0.0268(9) 0.0353(10) 0.0214(10) 0.0033(8) 0.0054(7) 0.0024(7) C26 0.0208(8) 0.0220(8) 0.0232(9) 0.0021(7) 0.0063(7) -0.0003(6) C31 0.0216(8) 0.0150(7) 0.0190(9) -0.0003(6) 0.0055(6) 0.0006(6) C32 0.0240(8) 0.0269(8) 0.0225(10) -0.0010(7) 0.0084(7) 0.0015(7) C33 0.0334(10) 0.0346(10) 0.0217(10) -0.0010(8) 0.0075(8) 0.0008(8) C34 0.0326(10) 0.0399(10) 0.0214(10) 0.0013(8) -0.0015(8) 0.0041(8) C35 0.0251(9) 0.0527(12) 0.0302(12) 0.0009(9) 0.0023(8) 0.0108(8) C36 0.0252(9) 0.0393(10) 0.0225(10) -0.0002(8) 0.0080(7) 0.0030(7) C41 0.0214(8) 0.0136(7) 0.0231(9) -0.0006(6) 0.0084(6) 0.0005(6) C42 0.0361(10) 0.0174(7) 0.0243(10) 0.0018(7) 0.0103(8) -0.0016(7) C43 0.0495(12) 0.0140(7) 0.0371(12) 0.0019(7) 0.0141(9) -0.0044(7) C44 0.0394(10) 0.0177(8) 0.0390(12) -0.0090(8) 0.0144(9) -0.0057(7) C45 0.0337(9) 0.0245(8) 0.0248(10) -0.0070(7) 0.0087(8) -0.0040(7) C46 0.0293(9) 0.0164(7) 0.0246(10) -0.0006(6) 0.0094(7) -0.0010(6) C51 0.0193(8) 0.0238(8) 0.0225(9) -0.0037(7) 0.0061(7) 0.0013(6) C52 0.0316(9) 0.0261(9) 0.0371(12) -0.0019(8) 0.0161(8) 0.0002(7) C53 0.0444(12) 0.0273(9) 0.0587(15) -0.0131(9) 0.0200(11) -0.0067(8) C54 0.0448(12) 0.0404(11) 0.0509(15) -0.0244(10) 0.0141(11) 0.0003(9) C55 0.0413(12) 0.0540(13) 0.0355(13) -0.0153(10) 0.0186(10) -0.0014(10) C56 0.0332(10) 0.0376(10) 0.0306(11) -0.0076(8) 0.0150(8) -0.0056(8) C61 0.0224(8) 0.0221(8) 0.0210(9) 0.0034(6) 0.0057(6) -0.0020(6) C62 0.0267(9) 0.0269(9) 0.0254(10) 0.0037(7) 0.0096(7) 0.0021(7) C63 0.0240(9) 0.0361(10) 0.0353(12) 0.0091(9) 0.0066(8) 0.0047(8) C64 0.0288(9) 0.0375(10) 0.0339(11) 0.0080(9) -0.0048(8) -0.0002(8) C65 0.0409(11) 0.0413(10) 0.0234(11) -0.0028(9) 0.0005(8) 0.0043(9) C66 0.0271(9) 0.0352(9) 0.0254(10) -0.0014(8) 0.0057(8) 0.0047(7) C71 0.0193(8) 0.0216(7) 0.0211(9) 0.0012(6) 0.0079(6) 0.0004(6) C72 0.0236(9) 0.0334(9) 0.0271(11) 0.0055(8) 0.0007(7) -0.0085(7) C73 0.0292(9) 0.0324(9) 0.0279(11) 0.0067(8) 0.0002(8) -0.0033(7) C74 0.0466(12) 0.0252(9) 0.0370(12) 0.0083(8) 0.0018(9) -0.0100(8) C75 0.0525(13) 0.0279(10) 0.0466(14) 0.0069(9) -0.0097(10) -0.0184(9) C76 0.0336(10) 0.0276(9) 0.0330(12) 0.0047(8) -0.0066(8) -0.0075(7) C99 0.089(2) 0.079(2) 0.072(2) 0.0132(16) 0.0155(17) 0.0390(17) Cl1 0.0468(3) 0.0493(3) 0.0753(5) -0.0070(3) 0.0205(3) -0.0059(3) Cl2 0.0967(6) 0.0550(4) 0.0863(6) -0.0041(4) 0.0434(5) 0.0009(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 Cu P3 2.2128(5) . Y Cu P2 2.2573(4) . Y Cu P1 2.2611(4) . Y P1 C11 1.8147(16) . Y P1 C21 1.8206(16) . Y P1 C1 1.8368(14) . Y P2 C41 1.8106(15) . Y P2 C31 1.8239(17) . Y P2 C2 1.8389(15) . Y P3 C61 1.8210(18) . Y P3 C51 1.8240(16) . Y P3 C71 1.8264(16) . Y C1 C2 1.596(2) . Y C1 B5 1.635(2) . Y C1 B6 1.718(2) . Y C1 B10 1.730(2) . Y C2 B3 1.621(2) . Y C2 B6 1.735(2) . Y C2 B7 1.752(2) . Y B3 B8 1.754(3) . Y B3 B7 1.789(3) . Y B3 B4 1.828(3) . Y B4 B8 1.757(3) . Y B4 B9 1.777(3) . Y B4 B5 1.845(3) . Y B5 B9 1.785(3) . Y B5 B10 1.807(3) . Y B6 B11 1.765(2) . Y B6 B10 1.771(2) . Y B6 B7 1.777(2) . Y B7 B8 1.747(2) . Y B7 B11 1.761(3) . Y B8 B11 1.800(3) . Y B8 B9 1.809(3) . Y B9 B10 1.752(2) . Y B9 B11 1.802(3) . Y B10 B11 1.747(3) . Y C11 C12 1.386(2) . ? C11 C16 1.396(2) . ? C12 C13 1.397(3) . ? C13 C14 1.375(3) . ? C14 C15 1.378(3) . ? C15 C16 1.386(2) . ? C21 C26 1.388(2) . ? C21 C22 1.402(2) . ? C22 C23 1.376(3) . ? C23 C24 1.384(3) . ? C24 C25 1.382(2) . ? C25 C26 1.387(2) . ? C31 C32 1.391(2) . ? C31 C36 1.393(2) . ? C32 C33 1.386(2) . ? C33 C34 1.377(2) . ? C34 C35 1.381(3) . ? C35 C36 1.380(2) . ? C41 C42 1.395(2) . ? C41 C46 1.395(2) . ? C42 C43 1.391(2) . ? C43 C44 1.379(3) . ? C44 C45 1.387(2) . ? C45 C46 1.386(2) . ? C51 C52 1.385(2) . ? C51 C56 1.393(2) . ? C52 C53 1.384(2) . ? C53 C54 1.378(3) . ? C54 C55 1.375(3) . ? C55 C56 1.386(3) . ? C61 C62 1.391(2) . ? C61 C66 1.393(2) . ? C62 C63 1.386(2) . ? C63 C64 1.378(3) . ? C64 C65 1.388(3) . ? C65 C66 1.380(3) . ? C71 C76 1.384(2) . ? C71 C72 1.387(2) . ? C72 C73 1.380(2) . ? C73 C74 1.381(2) . ? C74 C75 1.379(3) . ? C75 C76 1.387(3) . ? C99 Cl2 1.721(3) . ? C99 Cl1 1.760(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 P3 Cu P2 133.992(16) . . Y P3 Cu P1 134.632(16) . . Y P2 Cu P1 89.855(16) . . Y C11 P1 C21 102.70(7) . . Y C11 P1 C1 108.27(7) . . Y C21 P1 C1 106.59(7) . . Y C11 P1 Cu 121.76(6) . . Y C21 P1 Cu 112.82(5) . . Y C1 P1 Cu 103.91(5) . . Y C41 P2 C31 103.99(7) . . Y C41 P2 C2 106.28(7) . . Y C31 P2 C2 108.75(7) . . Y C41 P2 Cu 124.00(5) . . Y C31 P2 Cu 108.84(5) . . Y C2 P2 Cu 104.38(5) . . Y C61 P3 C51 105.94(7) . . Y C61 P3 C71 103.41(7) . . Y C51 P3 C71 104.93(8) . . Y C61 P3 Cu 108.09(6) . . Y C51 P3 Cu 116.39(5) . . Y C71 P3 Cu 116.85(5) . . Y C2 C1 B5 110.87(11) . . Y C2 C1 B6 63.01(9) . . Y B5 C1 B6 116.50(12) . . Y C2 C1 B10 111.41(11) . . Y B5 C1 B10 64.90(10) . . Y B6 C1 B10 61.83(10) . . Y C2 C1 P1 116.29(9) . . Y B5 C1 P1 124.87(11) . . Y B6 C1 P1 109.41(10) . . Y B10 C1 P1 118.04(10) . . Y C1 C2 B3 114.05(12) . . Y C1 C2 B6 61.94(9) . . Y B3 C2 B6 115.76(12) . . Y C1 C2 B7 111.32(11) . . Y B3 C2 B7 63.93(10) . . Y B6 C2 B7 61.28(10) . . Y C1 C2 P2 115.16(9) . . Y B3 C2 P2 124.06(11) . . Y B6 C2 P2 109.75(10) . . Y B7 C2 P2 117.85(10) . . Y C2 B3 B8 105.52(13) . . Y C2 B3 B7 61.60(10) . . Y B8 B3 B7 59.06(10) . . Y C2 B3 B4 106.39(12) . . Y B8 B3 B4 58.71(10) . . Y B7 B3 B4 108.16(13) . . Y B8 B4 B9 61.56(11) . . Y B8 B4 B3 58.54(10) . . Y B9 B4 B3 105.87(13) . . Y B8 B4 B5 105.85(13) . . Y B9 B4 B5 59.04(10) . . Y B3 B4 B5 101.29(11) . . Y C1 B5 B9 104.81(13) . . Y C1 B5 B10 60.09(10) . . Y B9 B5 B10 58.39(10) . . Y C1 B5 B4 107.16(12) . . Y B9 B5 B4 58.58(10) . . Y B10 B5 B4 106.99(12) . . Y C1 B6 C2 55.05(9) . . Y C1 B6 B11 104.15(12) . . Y C2 B6 B11 103.82(12) . . Y C1 B6 B10 59.42(9) . . Y C2 B6 B10 103.25(12) . . Y B11 B6 B10 59.24(10) . . Y C1 B6 B7 104.62(12) . . Y C2 B6 B7 59.85(9) . . Y B11 B6 B7 59.65(10) . . Y B10 B6 B7 107.70(12) . . Y B8 B7 C2 100.39(12) . . Y B8 B7 B11 61.75(10) . . Y C2 B7 B11 103.23(12) . . Y B8 B7 B6 108.15(12) . . Y C2 B7 B6 58.88(9) . . Y B11 B7 B6 59.83(10) . . Y B8 B7 B3 59.47(10) . . Y C2 B7 B3 54.46(9) . . Y B11 B7 B3 108.31(13) . . Y B6 B7 B3 105.70(12) . . Y B7 B8 B3 61.46(10) . . Y B7 B8 B4 113.44(13) . . Y B3 B8 B4 62.75(11) . . Y B7 B8 B11 59.53(10) . . Y B3 B8 B11 108.13(12) . . Y B4 B8 B11 110.21(13) . . Y B7 B8 B9 108.19(12) . . Y B3 B8 B9 107.68(12) . . Y B4 B8 B9 59.74(10) . . Y B11 B8 B9 59.89(10) . . Y B10 B9 B4 112.57(13) . . Y B10 B9 B5 61.43(10) . . Y B4 B9 B5 62.38(11) . . Y B10 B9 B11 58.88(10) . . Y B4 B9 B11 109.28(12) . . Y B5 B9 B11 107.44(12) . . Y B10 B9 B8 106.95(12) . . Y B4 B9 B8 58.69(10) . . Y B5 B9 B8 106.21(12) . . Y B11 B9 B8 59.83(10) . . Y C1 B10 B11 104.38(12) . . Y C1 B10 B9 102.28(12) . . Y B11 B10 B9 61.96(10) . . Y C1 B10 B6 58.75(9) . . Y B11 B10 B6 60.20(10) . . Y B9 B10 B6 108.86(12) . . Y C1 B10 B5 55.01(9) . . Y B11 B10 B5 108.85(13) . . Y B9 B10 B5 60.18(10) . . Y B6 B10 B5 105.65(12) . . Y B10 B11 B7 109.47(13) . . Y B10 B11 B6 60.57(10) . . Y B7 B11 B6 60.52(10) . . Y B10 B11 B8 107.53(13) . . Y B7 B11 B8 58.72(10) . . Y B6 B11 B8 106.32(12) . . Y B10 B11 B9 59.16(10) . . Y B7 B11 B9 107.86(13) . . Y B6 B11 B9 106.96(13) . . Y B8 B11 B9 60.28(10) . . Y C12 C11 C16 119.73(16) . . ? C12 C11 P1 118.77(13) . . ? C16 C11 P1 121.46(14) . . ? C11 C12 C13 119.33(19) . . ? C14 C13 C12 120.5(2) . . ? C13 C14 C15 120.47(18) . . ? C14 C15 C16 119.73(19) . . ? C15 C16 C11 120.26(19) . . ? C26 C21 C22 118.46(15) . . ? C26 C21 P1 122.99(12) . . ? C22 C21 P1 118.46(13) . . ? C23 C22 C21 120.49(17) . . ? C22 C23 C24 120.60(17) . . ? C25 C24 C23 119.50(17) . . ? C24 C25 C26 120.21(17) . . ? C25 C26 C21 120.73(15) . . ? C32 C31 C36 118.58(16) . . ? C32 C31 P2 125.40(12) . . ? C36 C31 P2 116.02(12) . . ? C33 C32 C31 120.52(15) . . ? C34 C33 C32 120.28(17) . . ? C33 C34 C35 119.69(18) . . ? C36 C35 C34 120.36(17) . . ? C35 C36 C31 120.56(17) . . ? C42 C41 C46 119.32(14) . . ? C42 C41 P2 122.36(13) . . ? C46 C41 P2 118.32(11) . . ? C43 C42 C41 119.91(17) . . ? C44 C43 C42 120.26(16) . . ? C43 C44 C45 120.25(16) . . ? C46 C45 C44 119.88(17) . . ? C45 C46 C41 120.37(15) . . ? C52 C51 C56 118.71(16) . . ? C52 C51 P3 118.22(13) . . ? C56 C51 P3 123.07(13) . . ? C53 C52 C51 120.90(18) . . ? C54 C53 C52 119.90(18) . . ? C55 C54 C53 119.94(18) . . ? C54 C55 C56 120.44(19) . . ? C55 C56 C51 120.11(17) . . ? C62 C61 C66 119.04(16) . . ? C62 C61 P3 123.23(14) . . ? C66 C61 P3 117.61(13) . . ? C63 C62 C61 120.11(17) . . ? C64 C63 C62 120.49(17) . . ? C63 C64 C65 119.78(18) . . ? C66 C65 C64 120.02(19) . . ? C65 C66 C61 120.55(17) . . ? C76 C71 C72 119.03(15) . . ? C76 C71 P3 122.12(13) . . ? C72 C71 P3 118.64(12) . . ? C73 C72 C71 120.84(16) . . ? C72 C73 C74 119.97(18) . . ? C75 C74 C73 119.60(17) . . ? C74 C75 C76 120.56(17) . . ? C71 C76 C75 120.00(18) . . ? Cl2 C99 Cl1 113.42(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.994 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.062 data_lol68as _database_code_depnum_ccdc_archive 'CCDC 924359' #TrackingRef 'Combined-CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H45 Au B9 O P3' _chemical_formula_weight 928.93 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' Au Au -2.0133 8.8022 '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' _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 11.9805(17) _cell_length_b 12.7651(18) _cell_length_c 14.375(2) _cell_angle_alpha 79.691(3) _cell_angle_beta 70.189(3) _cell_angle_gamma 76.404(3) _cell_volume 1998.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1806 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 19.9 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 3.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5790 _exptl_absorpt_correction_T_max 0.8026 _exptl_absorpt_process_details ; SADABS; Area-Detector Absorption Correction. Bruker-AXS within SAINT+ package, v. 6.02 (1999). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21974 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_unetl/netI 0.1045 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7830 _reflns_number_gt 6208 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.10 (Bruker, 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. Restrains correspond to ISOR for C2 and C63 and SAME AND FLAT for the phenyl rings ; _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^)+(0.0430P)^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 7830 _refine_ls_number_parameters 518 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.1002 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.999 _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 Au1 Au 0.94092(3) 0.73478(2) 0.70137(2) 0.01485(9) Uani 1 1 d . . . P1 P 0.74808(16) 0.82696(14) 0.68678(13) 0.0137(4) Uani 1 1 d . . . P2 P 0.91889(16) 0.88339(15) 0.79062(13) 0.0136(4) Uani 1 1 d . . . P3 P 1.06511(18) 0.57123(15) 0.68837(14) 0.0183(4) Uani 1 1 d . . . B3 B 0.7725(7) 1.1116(6) 0.7907(6) 0.0153(17) Uani 1 1 d . . . H3 H 0.786(6) 1.118(5) 0.861(5) 0.018 Uiso 1 1 d . . . B4 B 0.6332(8) 1.1702(7) 0.7604(6) 0.0193(19) Uani 1 1 d . . . H1 H 0.636(6) 1.085(6) 0.803(5) 0.023 Uiso 1 1 d . . . H4 H 0.566(6) 1.232(6) 0.799(5) 0.023 Uiso 1 1 d . . . B5 B 0.6224(7) 1.0645(7) 0.6947(6) 0.0163(18) Uani 1 1 d . . . H5 H 0.545(6) 1.053(5) 0.698(5) 0.020 Uiso 1 1 d . . . B6 B 0.8750(8) 1.0099(7) 0.6136(6) 0.0167(18) Uani 1 1 d . . . H6 H 0.949(6) 0.954(6) 0.575(5) 0.020 Uiso 1 1 d . . . B7 B 0.8932(8) 1.1088(7) 0.6772(6) 0.0185(19) Uani 1 1 d . . . H7 H 0.973(7) 1.113(6) 0.678(5) 0.022 Uiso 1 1 d . . . B8 B 0.7702(8) 1.2132(7) 0.6905(6) 0.0180(18) Uani 1 1 d . . . H8 H 0.777(6) 1.291(6) 0.690(5) 0.022 Uiso 1 1 d . . . B9 B 0.6734(8) 1.1830(7) 0.6298(6) 0.0183(18) Uani 1 1 d . . . H9 H 0.625(6) 1.245(6) 0.598(5) 0.022 Uiso 1 1 d . . . B10 B 0.7413(8) 1.0610(7) 0.5813(6) 0.0179(18) Uani 1 1 d . . . H10 H 0.728(6) 1.040(6) 0.525(5) 0.022 Uiso 1 1 d . . . B11 B 0.8339(8) 1.1489(7) 0.5788(6) 0.0168(18) Uani 1 1 d . . . H11 H 0.885(6) 1.190(5) 0.517(5) 0.020 Uiso 1 1 d . . . O1 O 1.0977(4) 0.5060(4) 0.5951(3) 0.0216(12) Uani 1 1 d . . . C1 C 0.7418(6) 0.9703(5) 0.6872(5) 0.0117(14) Uani 1 1 d . . . C2 C 0.8269(6) 0.9985(5) 0.7410(5) 0.0117(14) Uani 1 1 d U . . C11 C 0.6959(6) 0.8163(5) 0.5853(5) 0.0140(15) Uani 1 1 d . . . C12 C 0.5789(7) 0.8099(6) 0.5983(6) 0.0220(17) Uani 1 1 d . . . H12 H 0.5209 0.8123 0.6626 0.026 Uiso 1 1 calc R . . C13 C 0.5451(7) 0.7997(6) 0.5169(6) 0.0278(19) Uani 1 1 d . . . H13 H 0.4635 0.7973 0.5255 0.033 Uiso 1 1 calc R . . C14 C 0.6291(7) 0.7932(6) 0.4253(6) 0.028(2) Uani 1 1 d . . . H14 H 0.6057 0.7861 0.3701 0.034 Uiso 1 1 calc R . . C15 C 0.7462(7) 0.7968(6) 0.4120(6) 0.0253(18) Uani 1 1 d . . . H15 H 0.8039 0.7920 0.3477 0.030 Uiso 1 1 calc R . . C16 C 0.7824(7) 0.8075(5) 0.4917(5) 0.0184(16) Uani 1 1 d . . . H16 H 0.8644 0.8087 0.4826 0.022 Uiso 1 1 calc R . . C21 C 0.6362(7) 0.7824(6) 0.7996(5) 0.0190(16) Uani 1 1 d . . . C22 C 0.5287(7) 0.8456(6) 0.8473(5) 0.0205(17) Uani 1 1 d . . . H22 H 0.5082 0.9183 0.8202 0.025 Uiso 1 1 calc R . . C23 C 0.4498(7) 0.8052(7) 0.9339(6) 0.0263(18) Uani 1 1 d . . . H23 H 0.3766 0.8505 0.9665 0.032 Uiso 1 1 calc R . . C24 C 0.4774(7) 0.6999(7) 0.9726(6) 0.032(2) Uani 1 1 d . . . H24 H 0.4229 0.6713 1.0315 0.038 Uiso 1 1 calc R . . C25 C 0.5834(8) 0.6365(7) 0.9261(6) 0.038(2) Uani 1 1 d . . . H25 H 0.6032 0.5640 0.9541 0.045 Uiso 1 1 calc R . . C26 C 0.6620(7) 0.6745(6) 0.8404(6) 0.0235(17) Uani 1 1 d . . . H26 H 0.7343 0.6280 0.8082 0.028 Uiso 1 1 calc R . . C31 C 1.0527(6) 0.9274(5) 0.7891(5) 0.0152(15) Uani 1 1 d . . . C32 C 1.1530(6) 0.9147(6) 0.7061(5) 0.0168(16) Uani 1 1 d . . . H32 H 1.1517 0.8815 0.6525 0.020 Uiso 1 1 calc R . . C33 C 1.2549(6) 0.9503(6) 0.7011(5) 0.0207(17) Uani 1 1 d . . . H33 H 1.3234 0.9432 0.6432 0.025 Uiso 1 1 calc R . . C34 C 1.2579(7) 0.9960(6) 0.7798(5) 0.0239(18) Uani 1 1 d . . . H34 H 1.3291 1.0190 0.7769 0.029 Uiso 1 1 calc R . . C35 C 1.1589(7) 1.0083(7) 0.8618(6) 0.0283(19) Uani 1 1 d . . . H35 H 1.1612 1.0398 0.9160 0.034 Uiso 1 1 calc R . . C36 C 1.0557(7) 0.9756(7) 0.8664(5) 0.0235(18) Uani 1 1 d . . . H36 H 0.9862 0.9861 0.9232 0.028 Uiso 1 1 calc R . . C41 C 0.8344(6) 0.8535(6) 0.9196(5) 0.0151(15) Uani 1 1 d . . . C42 C 0.7144(6) 0.8965(6) 0.9599(5) 0.0159(15) Uani 1 1 d . . . H42 H 0.6748 0.9518 0.9218 0.019 Uiso 1 1 calc R . . C43 C 0.6510(6) 0.8604(6) 1.0543(5) 0.0202(17) Uani 1 1 d . . . H43 H 0.5682 0.8916 1.0813 0.024 Uiso 1 1 calc R . . C44 C 0.7058(7) 0.7791(6) 1.1110(6) 0.0260(18) Uani 1 1 d . . . H44 H 0.6610 0.7529 1.1759 0.031 Uiso 1 1 calc R . . C45 C 0.8264(7) 0.7369(6) 1.0718(6) 0.0268(19) Uani 1 1 d . . . H45 H 0.8656 0.6822 1.1105 0.032 Uiso 1 1 calc R . . C46 C 0.8914(7) 0.7730(6) 0.9765(5) 0.0217(17) Uani 1 1 d . . . H46 H 0.9747 0.7430 0.9500 0.026 Uiso 1 1 calc R . . C51 C 1.2092(7) 0.5598(6) 0.7070(5) 0.0218(17) Uani 1 1 d . . . C52 C 1.2290(7) 0.6365(7) 0.7536(6) 0.0276(19) Uani 1 1 d . . . H52 H 1.1669 0.6973 0.7735 0.033 Uiso 1 1 calc R . . C53 C 1.3363(7) 0.6265(7) 0.7716(6) 0.032(2) Uani 1 1 d . . . H53 H 1.3469 0.6790 0.8055 0.039 Uiso 1 1 calc R . . C54 C 1.4285(8) 0.5410(7) 0.7408(7) 0.040(2) Uani 1 1 d . . . H54 H 1.5040 0.5351 0.7514 0.048 Uiso 1 1 calc R . . C55 C 1.4107(8) 0.4641(8) 0.6945(7) 0.044(2) Uani 1 1 d . . . H55 H 1.4740 0.4043 0.6741 0.053 Uiso 1 1 calc R . . C56 C 1.3024(7) 0.4722(7) 0.6772(7) 0.035(2) Uani 1 1 d . . . H56 H 1.2913 0.4183 0.6452 0.042 Uiso 1 1 calc R . . C61 C 0.9879(6) 0.4783(6) 0.7865(5) 0.0203(17) Uani 1 1 d U . . C62 C 0.9385(7) 0.5099(6) 0.8814(5) 0.0260(18) Uani 1 1 d . . . H62 H 0.9490 0.5768 0.8941 0.031 Uiso 1 1 calc R . . C63 C 0.8737(7) 0.4441(7) 0.9578(6) 0.031(2) Uani 1 1 d . . . H63 H 0.8409 0.4663 1.0229 0.038 Uiso 1 1 calc R . . C64 C 0.8558(7) 0.3481(7) 0.9418(6) 0.034(2) Uani 1 1 d . . . H64 H 0.8108 0.3033 0.9944 0.040 Uiso 1 1 calc R . . C65 C 0.9054(8) 0.3182(7) 0.8462(7) 0.040(2) Uani 1 1 d . . . H65 H 0.8952 0.2515 0.8326 0.048 Uiso 1 1 calc R . . C66 C 0.9707(7) 0.3858(6) 0.7690(6) 0.0274(19) Uani 1 1 d . . . H66 H 1.0029 0.3649 0.7034 0.033 Uiso 1 1 calc R . . C71 C 1.1468(7) 0.5577(6) 0.4964(5) 0.0281(19) Uani 1 1 d . . . H71A H 1.2084 0.5978 0.4959 0.034 Uiso 1 1 calc R . . H71B H 1.0818 0.6101 0.4761 0.034 Uiso 1 1 calc R . . C72 C 1.2016(8) 0.4760(6) 0.4267(6) 0.033(2) Uani 1 1 d . . . H72A H 1.2708 0.4284 0.4433 0.050 Uiso 1 1 calc R . . H72B H 1.2287 0.5118 0.3589 0.050 Uiso 1 1 calc R . . H72C H 1.1419 0.4329 0.4310 0.050 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 Au1 0.01585(15) 0.01186(14) 0.01740(15) -0.00024(10) -0.00701(11) -0.00194(10) P1 0.0148(10) 0.0124(9) 0.0159(9) -0.0011(7) -0.0078(8) -0.0023(8) P2 0.0124(9) 0.0138(10) 0.0155(10) 0.0009(8) -0.0060(8) -0.0037(8) P3 0.0210(11) 0.0134(10) 0.0213(10) -0.0006(8) -0.0096(9) -0.0012(8) B3 0.017(4) 0.012(4) 0.019(4) -0.001(3) -0.005(4) -0.007(3) B4 0.022(5) 0.011(4) 0.019(5) -0.003(4) 0.002(4) -0.001(4) B5 0.006(4) 0.018(5) 0.025(5) -0.004(4) -0.004(3) -0.002(3) B6 0.021(5) 0.015(4) 0.011(4) 0.002(3) -0.003(3) -0.003(4) B7 0.019(5) 0.014(4) 0.025(5) 0.003(4) -0.006(4) -0.012(4) B8 0.020(5) 0.021(5) 0.015(4) -0.003(4) -0.004(4) -0.010(4) B9 0.015(4) 0.017(5) 0.023(5) -0.003(4) -0.009(4) 0.001(4) B10 0.025(5) 0.010(4) 0.022(5) -0.001(3) -0.017(4) 0.004(3) B11 0.018(5) 0.013(4) 0.016(4) 0.002(3) -0.007(4) 0.002(3) O1 0.029(3) 0.011(3) 0.021(3) 0.000(2) -0.005(2) -0.003(2) C1 0.015(4) 0.012(4) 0.013(3) 0.001(3) -0.012(3) -0.003(3) C2 0.011(3) 0.014(3) 0.014(3) 0.001(2) -0.006(2) -0.009(2) C11 0.016(4) 0.005(3) 0.024(4) -0.002(3) -0.011(3) 0.001(3) C12 0.028(5) 0.021(4) 0.021(4) -0.009(3) -0.014(3) 0.002(3) C13 0.020(4) 0.030(5) 0.042(5) -0.012(4) -0.019(4) 0.001(4) C14 0.037(5) 0.026(5) 0.028(5) -0.012(4) -0.023(4) 0.011(4) C15 0.039(5) 0.015(4) 0.022(4) -0.002(3) -0.012(4) -0.001(4) C16 0.028(4) 0.012(4) 0.019(4) 0.001(3) -0.011(3) -0.006(3) C21 0.024(4) 0.023(4) 0.017(4) 0.007(3) -0.013(3) -0.015(3) C22 0.025(4) 0.018(4) 0.019(4) -0.005(3) -0.009(3) -0.002(3) C23 0.019(4) 0.036(5) 0.025(4) -0.004(4) -0.006(3) -0.008(4) C24 0.026(5) 0.042(6) 0.025(5) 0.004(4) 0.000(4) -0.020(4) C25 0.031(5) 0.037(5) 0.037(5) 0.021(4) -0.010(4) -0.012(4) C26 0.018(4) 0.021(4) 0.031(5) 0.000(3) -0.007(3) -0.005(3) C31 0.014(4) 0.012(4) 0.020(4) -0.001(3) -0.006(3) -0.004(3) C32 0.017(4) 0.016(4) 0.021(4) -0.001(3) -0.009(3) -0.005(3) C33 0.014(4) 0.022(4) 0.022(4) -0.002(3) -0.001(3) -0.002(3) C34 0.016(4) 0.033(5) 0.028(4) -0.001(4) -0.010(3) -0.010(4) C35 0.020(4) 0.052(6) 0.022(4) -0.009(4) -0.008(3) -0.017(4) C36 0.021(4) 0.044(5) 0.007(4) -0.005(3) -0.004(3) -0.008(4) C41 0.022(4) 0.016(4) 0.014(4) 0.001(3) -0.011(3) -0.010(3) C42 0.018(4) 0.017(4) 0.018(4) 0.000(3) -0.010(3) -0.006(3) C43 0.012(4) 0.019(4) 0.027(4) -0.002(3) -0.005(3) -0.003(3) C44 0.022(4) 0.030(5) 0.027(4) -0.002(4) -0.005(4) -0.009(4) C45 0.032(5) 0.025(4) 0.027(4) 0.009(4) -0.018(4) -0.009(4) C46 0.019(4) 0.024(4) 0.021(4) 0.000(3) -0.003(3) -0.007(3) C51 0.018(4) 0.017(4) 0.026(4) 0.006(3) -0.008(3) -0.002(3) C52 0.027(5) 0.033(5) 0.020(4) -0.005(4) -0.002(4) -0.007(4) C53 0.030(5) 0.034(5) 0.040(5) 0.000(4) -0.018(4) -0.013(4) C54 0.021(5) 0.047(6) 0.057(6) 0.001(5) -0.022(4) -0.009(4) C55 0.027(5) 0.042(6) 0.063(7) -0.013(5) -0.017(5) 0.007(4) C56 0.032(5) 0.025(5) 0.054(6) -0.013(4) -0.019(4) 0.000(4) C61 0.017(3) 0.019(3) 0.022(3) 0.006(3) -0.009(3) 0.003(3) C62 0.033(5) 0.019(4) 0.024(4) 0.005(3) -0.011(4) -0.003(4) C63 0.025(5) 0.033(5) 0.028(5) 0.012(4) -0.010(4) 0.002(4) C64 0.033(5) 0.049(6) 0.029(5) 0.019(4) -0.023(4) -0.025(4) C65 0.057(6) 0.036(5) 0.047(6) 0.015(4) -0.035(5) -0.033(5) C66 0.039(5) 0.029(5) 0.025(4) -0.005(4) -0.022(4) -0.009(4) C71 0.034(5) 0.024(5) 0.020(4) 0.001(3) -0.002(4) -0.004(4) C72 0.047(6) 0.018(4) 0.031(5) -0.001(4) -0.008(4) -0.008(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 Au1 P3 2.2579(19) . ? Au1 P2 2.3917(19) . ? Au1 P1 2.3934(18) . ? P1 C11 1.808(7) . ? P1 C1 1.815(7) . ? P1 C21 1.818(7) . ? P2 C41 1.806(7) . ? P2 C31 1.811(7) . ? P2 C2 1.811(7) . ? P3 O1 1.593(5) . ? P3 C51 1.804(7) . ? P3 C61 1.813(7) . ? B3 C2 1.622(10) . ? B3 B8 1.761(11) . ? B3 B7 1.775(12) . ? B3 B4 1.823(12) . ? B4 B9 1.759(12) . ? B4 B8 1.765(12) . ? B4 B5 1.830(12) . ? B5 C1 1.623(10) . ? B5 B9 1.754(12) . ? B5 B10 1.764(12) . ? B6 C2 1.714(10) . ? B6 C1 1.722(11) . ? B6 B11 1.755(11) . ? B6 B10 1.763(11) . ? B6 B7 1.777(12) . ? B7 B8 1.721(12) . ? B7 B11 1.737(12) . ? B7 C2 1.738(10) . ? B8 B11 1.783(11) . ? B8 B9 1.808(12) . ? B9 B10 1.727(12) . ? B9 B11 1.786(12) . ? B10 C1 1.740(10) . ? B10 B11 1.743(12) . ? O1 C71 1.440(8) . ? C1 C2 1.605(8) . ? C11 C12 1.370(10) . ? C11 C16 1.397(10) . ? C12 C13 1.397(10) . ? C13 C14 1.363(11) . ? C14 C15 1.362(11) . ? C15 C16 1.393(10) . ? C21 C22 1.375(10) . ? C21 C26 1.404(10) . ? C22 C23 1.382(10) . ? C23 C24 1.369(11) . ? C24 C25 1.360(11) . ? C25 C26 1.362(10) . ? C31 C32 1.378(9) . ? C31 C36 1.378(10) . ? C32 C33 1.375(10) . ? C33 C34 1.378(10) . ? C34 C35 1.360(10) . ? C35 C36 1.373(10) . ? C41 C42 1.371(9) . ? C41 C46 1.393(9) . ? C42 C43 1.369(9) . ? C43 C44 1.383(10) . ? C44 C45 1.373(10) . ? C45 C46 1.384(10) . ? C51 C52 1.384(10) . ? C51 C56 1.392(10) . ? C52 C53 1.367(11) . ? C53 C54 1.373(12) . ? C54 C55 1.370(12) . ? C55 C56 1.380(11) . ? C61 C66 1.326(10) . ? C61 C62 1.382(10) . ? C62 C63 1.383(10) . ? C63 C64 1.364(11) . ? C64 C65 1.384(12) . ? C65 C66 1.405(11) . ? C71 C72 1.459(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 P3 Au1 P2 132.95(7) . . ? P3 Au1 P1 141.51(7) . . ? P2 Au1 P1 83.15(6) . . ? C11 P1 C1 106.3(3) . . ? C11 P1 C21 105.8(3) . . ? C1 P1 C21 107.8(3) . . ? C11 P1 Au1 123.3(2) . . ? C1 P1 Au1 106.7(2) . . ? C21 P1 Au1 106.2(2) . . ? C41 P2 C31 106.9(3) . . ? C41 P2 C2 106.5(3) . . ? C31 P2 C2 107.3(3) . . ? C41 P2 Au1 109.3(2) . . ? C31 P2 Au1 119.2(2) . . ? C2 P2 Au1 106.9(2) . . ? O1 P3 C51 103.5(3) . . ? O1 P3 C61 100.2(3) . . ? C51 P3 C61 105.0(3) . . ? O1 P3 Au1 122.2(2) . . ? C51 P3 Au1 117.1(3) . . ? C61 P3 Au1 106.5(2) . . ? C2 B3 B8 105.4(6) . . ? C2 B3 B7 61.4(4) . . ? B8 B3 B7 58.2(5) . . ? C2 B3 B4 106.7(6) . . ? B8 B3 B4 59.0(5) . . ? B7 B3 B4 107.4(6) . . ? B9 B4 B8 61.7(5) . . ? B9 B4 B3 106.0(6) . . ? B8 B4 B3 58.8(5) . . ? B9 B4 B5 58.5(5) . . ? B8 B4 B5 105.7(6) . . ? B3 B4 B5 101.3(5) . . ? C1 B5 B9 106.5(6) . . ? C1 B5 B10 61.7(4) . . ? B9 B5 B10 58.8(5) . . ? C1 B5 B4 107.6(6) . . ? B9 B5 B4 58.7(5) . . ? B10 B5 B4 107.7(6) . . ? C2 B6 C1 55.7(4) . . ? C2 B6 B11 103.9(6) . . ? C1 B6 B11 104.8(6) . . ? C2 B6 B10 104.0(6) . . ? C1 B6 B10 59.9(4) . . ? B11 B6 B10 59.4(5) . . ? C2 B6 B7 59.7(4) . . ? C1 B6 B7 104.7(6) . . ? B11 B6 B7 58.9(5) . . ? B10 B6 B7 107.1(6) . . ? B8 B7 B11 62.1(5) . . ? B8 B7 C2 102.2(6) . . ? B11 B7 C2 103.7(6) . . ? B8 B7 B3 60.5(5) . . ? B11 B7 B3 109.0(6) . . ? C2 B7 B3 55.0(4) . . ? B8 B7 B6 108.8(6) . . ? B11 B7 B6 59.9(5) . . ? C2 B7 B6 58.4(4) . . ? B3 B7 B6 105.5(6) . . ? B7 B8 B3 61.3(5) . . ? B7 B8 B4 112.6(6) . . ? B3 B8 B4 62.3(5) . . ? B7 B8 B11 59.4(5) . . ? B3 B8 B11 107.5(6) . . ? B4 B8 B11 109.2(6) . . ? B7 B8 B9 107.6(6) . . ? B3 B8 B9 106.6(6) . . ? B4 B8 B9 59.0(5) . . ? B11 B8 B9 59.6(5) . . ? B10 B9 B5 60.9(5) . . ? B10 B9 B4 112.7(6) . . ? B5 B9 B4 62.8(5) . . ? B10 B9 B11 59.4(5) . . ? B5 B9 B11 107.4(6) . . ? B4 B9 B11 109.3(6) . . ? B10 B9 B8 107.5(6) . . ? B5 B9 B8 107.1(6) . . ? B4 B9 B8 59.3(5) . . ? B11 B9 B8 59.5(5) . . ? B9 B10 C1 102.7(6) . . ? B9 B10 B11 62.0(5) . . ? C1 B10 B11 104.5(5) . . ? B9 B10 B6 108.9(6) . . ? C1 B10 B6 58.9(4) . . ? B11 B10 B6 60.1(5) . . ? B9 B10 B5 60.3(5) . . ? C1 B10 B5 55.2(4) . . ? B11 B10 B5 108.9(6) . . ? B6 B10 B5 105.7(6) . . ? B7 B11 B10 109.8(6) . . ? B7 B11 B6 61.2(5) . . ? B10 B11 B6 60.6(5) . . ? B7 B11 B8 58.5(5) . . ? B10 B11 B8 108.0(6) . . ? B6 B11 B8 107.0(6) . . ? B7 B11 B9 107.8(6) . . ? B10 B11 B9 58.6(5) . . ? B6 B11 B9 106.6(6) . . ? B8 B11 B9 60.9(5) . . ? C71 O1 P3 119.4(4) . . ? C2 C1 B5 111.1(5) . . ? C2 C1 B6 61.9(4) . . ? B5 C1 B6 114.4(5) . . ? C2 C1 B10 110.0(5) . . ? B5 C1 B10 63.1(5) . . ? B6 C1 B10 61.2(4) . . ? C2 C1 P1 115.5(4) . . ? B5 C1 P1 125.3(5) . . ? B6 C1 P1 111.8(5) . . ? B10 C1 P1 121.0(5) . . ? C1 C2 B3 113.1(5) . . ? C1 C2 B6 62.4(4) . . ? B3 C2 B6 115.9(5) . . ? C1 C2 B7 111.9(5) . . ? B3 C2 B7 63.7(5) . . ? B6 C2 B7 62.0(5) . . ? C1 C2 P2 115.8(4) . . ? B3 C2 P2 123.6(5) . . ? B6 C2 P2 110.6(5) . . ? B7 C2 P2 118.2(5) . . ? C12 C11 C16 120.0(7) . . ? C12 C11 P1 122.8(6) . . ? C16 C11 P1 117.0(5) . . ? C11 C12 C13 119.9(7) . . ? C14 C13 C12 120.0(7) . . ? C15 C14 C13 120.5(7) . . ? C14 C15 C16 120.7(7) . . ? C15 C16 C11 118.8(7) . . ? C22 C21 C26 117.7(7) . . ? C22 C21 P1 125.3(6) . . ? C26 C21 P1 117.0(6) . . ? C21 C22 C23 121.3(7) . . ? C24 C23 C22 119.9(8) . . ? C25 C24 C23 119.5(8) . . ? C24 C25 C26 121.5(8) . . ? C25 C26 C21 120.1(7) . . ? C32 C31 C36 119.5(7) . . ? C32 C31 P2 118.3(5) . . ? C36 C31 P2 122.2(5) . . ? C33 C32 C31 119.9(7) . . ? C32 C33 C34 120.1(7) . . ? C35 C34 C33 119.9(7) . . ? C34 C35 C36 120.4(7) . . ? C35 C36 C31 120.1(7) . . ? C42 C41 C46 119.0(6) . . ? C42 C41 P2 123.3(5) . . ? C46 C41 P2 117.2(6) . . ? C43 C42 C41 120.7(6) . . ? C42 C43 C44 121.0(7) . . ? C45 C44 C43 118.7(7) . . ? C44 C45 C46 120.8(7) . . ? C45 C46 C41 119.8(7) . . ? C52 C51 C56 118.2(7) . . ? C52 C51 P3 120.8(6) . . ? C56 C51 P3 120.9(6) . . ? C53 C52 C51 121.4(8) . . ? C52 C53 C54 120.2(8) . . ? C55 C54 C53 119.3(8) . . ? C54 C55 C56 121.1(8) . . ? C55 C56 C51 119.8(8) . . ? C66 C61 C62 119.6(7) . . ? C66 C61 P3 122.4(6) . . ? C62 C61 P3 117.9(6) . . ? C63 C62 C61 120.1(8) . . ? C64 C63 C62 121.4(8) . . ? C63 C64 C65 117.6(8) . . ? C64 C65 C66 120.5(8) . . ? C61 C66 C65 120.8(8) . . ? O1 C71 C72 109.7(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.615 _refine_diff_density_min -1.623 _refine_diff_density_rms 0.184 data_con96as _database_code_depnum_ccdc_archive 'CCDC 924360' #TrackingRef 'Combined-CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H89 Au2 B18 Cl9 P6' _chemical_formula_weight 2167.91 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' Au Au -2.0133 8.8022 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.2394(17) _cell_length_b 17.7117(19) _cell_length_c 17.7130(19) _cell_angle_alpha 72.326(2) _cell_angle_beta 69.982(2) _cell_angle_gamma 80.111(2) _cell_volume 4547.9(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9833 _cell_measurement_theta_min 4.31 _cell_measurement_theta_max 28.25 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 3.636 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.4084 _exptl_absorpt_correction_T_max 0.4885 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27310 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_unetl/netI 0.1003 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.50 _reflns_number_total 15890 _reflns_number_gt 11737 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v. 5.611 (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT+ v. 6.02 (Bruker AXS, 1999)' _computing_data_reduction 'SAINT+ v. 6.02 (Bruker AXS, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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. The two hydrogen atoms correspond to the briding hydrogen atoms of the two nido-carborane cages which could not be located. The crystallographic data used for the elucidation of the structure of this complex were taken time ago with HEMISPHERE strategy. ; _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^)+(0.0000P)^2^] 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 15890 _refine_ls_number_parameters 1054 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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 Au1 Au 1.047877(16) 0.565319(12) 0.196603(13) 0.01562(7) Uani 1 1 d . . . Au2 Au 0.651586(16) 0.886602(12) 0.189888(13) 0.01662(7) Uani 1 1 d . . . P1 P 1.18569(11) 0.48715(8) 0.19001(9) 0.0153(3) Uani 1 1 d . . . P2 P 1.13078(11) 0.63812(8) 0.05940(9) 0.0146(3) Uani 1 1 d . . . P3 P 0.90741(11) 0.56277(8) 0.28503(9) 0.0148(3) Uani 1 1 d . . . P4 P 0.77675(11) 0.84744(8) 0.09908(9) 0.0150(3) Uani 1 1 d . . . P5 P 0.57340(11) 0.81425(8) 0.32941(9) 0.0162(4) Uani 1 1 d . . . P6 P 0.54646(11) 0.99237(8) 0.21715(9) 0.0154(3) Uani 1 1 d . . . B1 B 1.3371(5) 0.4538(4) 0.0419(4) 0.0225(17) Uani 1 1 d . . . H1' H 1.3815 0.4516 0.0791 0.027 Uiso 1 1 calc R . . B2 B 1.3772(5) 0.5123(4) -0.0686(4) 0.0242(17) Uani 1 1 d . . . H2' H 1.4434 0.5359 -0.0898 0.029 Uiso 1 1 calc R . . B3 B 1.2836(5) 0.5852(4) -0.0762(4) 0.0215(17) Uani 1 1 d . . . H3' H 1.3014 0.6483 -0.0975 0.026 Uiso 1 1 calc R . . B4 B 1.3003(5) 0.5022(4) -0.1148(4) 0.0230(18) Uani 1 1 d . . . H4' H 1.3226 0.5080 -0.1834 0.028 Uiso 1 1 calc R . . B5 B 1.1942(5) 0.5352(4) -0.0656(4) 0.0215(17) Uani 1 1 d . . . H5' H 1.1453 0.5625 -0.0999 0.026 Uiso 1 1 calc R . . B6 B 1.1604(5) 0.4755(4) 0.0382(4) 0.0204(17) Uani 1 1 d . . . H6' H 1.0897 0.4649 0.0733 0.024 Uiso 1 1 calc R . . B7 B 1.2471(5) 0.4030(4) 0.0510(4) 0.0210(17) Uani 1 1 d . . . H7' H 1.2334 0.3423 0.0939 0.025 Uiso 1 1 calc R . . C7 C 1.2377(4) 0.4891(3) 0.0800(3) 0.0179(14) Uani 1 1 d . . . C8 C 1.2089(4) 0.5638(3) 0.0139(3) 0.0171(14) Uani 1 1 d . . . B9 B 1.2240(5) 0.4321(4) -0.0429(4) 0.0254(18) Uani 1 1 d . . . H9' H 1.1964 0.3908 -0.0633 0.030 Uiso 1 1 calc R . . B10 B 0.3628(5) 0.9958(4) 0.3421(4) 0.0234(17) Uani 1 1 d . . . H10' H 0.3780 1.0520 0.3494 0.028 Uiso 1 1 calc R . . B11 B 0.3099(5) 0.9264(4) 0.4414(4) 0.0215(17) Uani 1 1 d . . . H11' H 0.2938 0.9476 0.4987 0.026 Uiso 1 1 calc R . . B12 B 0.3834(5) 0.8373(4) 0.4371(4) 0.0196(17) Uani 1 1 d . . . H12' H 0.4095 0.8149 0.4914 0.024 Uiso 1 1 calc R . . B13 B 0.2725(5) 0.9472(4) 0.3541(4) 0.0201(16) Uani 1 1 d . . . H13' H 0.2072 0.9811 0.3564 0.024 Uiso 1 1 calc R . . B14 B 0.3575(5) 0.9585(4) 0.2599(4) 0.0203(16) Uani 1 1 d . . . H14' H 0.3499 0.9982 0.1996 0.024 Uiso 1 1 calc R . . B15 B 0.4250(5) 0.8699(4) 0.2621(4) 0.0208(17) Uani 1 1 d . . . H15' H 0.4643 0.8510 0.2043 0.025 Uiso 1 1 calc R . . B16 B 0.3776(5) 0.7998(4) 0.3570(4) 0.0190(16) Uani 1 1 d . . . H16' H 0.3838 0.7349 0.3608 0.023 Uiso 1 1 calc R . . B17 B 0.2848(5) 0.8466(4) 0.4148(4) 0.0186(16) Uani 1 1 d . . . H17' H 0.2280 0.8114 0.4586 0.022 Uiso 1 1 calc R . . B18 B 0.3095(5) 0.8684(4) 0.3048(4) 0.0233(17) Uani 1 1 d . . . H18' H 0.2684 0.8490 0.2756 0.028 Uiso 1 1 calc R . . C9 C 0.4593(4) 0.8572(3) 0.3488(3) 0.0158(13) Uani 1 1 d . . . C10 C 0.4484(4) 0.9462(3) 0.2915(3) 0.0143(13) Uani 1 1 d . . . C1 C 1.2585(4) 0.5295(3) 0.2208(4) 0.0162(13) Uani 1 1 d . . . C2 C 1.2351(4) 0.5271(3) 0.3055(4) 0.0237(15) Uani 1 1 d . . . H2 H 1.1857 0.5000 0.3445 0.028 Uiso 1 1 calc R . . C3 C 1.2843(5) 0.5643(4) 0.3317(4) 0.0343(18) Uani 1 1 d . . . H3 H 1.2696 0.5611 0.3893 0.041 Uiso 1 1 calc R . . C4 C 1.3537(5) 0.6057(4) 0.2758(5) 0.0362(19) Uani 1 1 d . . . H4 H 1.3859 0.6323 0.2945 0.043 Uiso 1 1 calc R . . C5 C 1.3769(5) 0.6089(4) 0.1936(4) 0.0358(18) Uani 1 1 d . . . H5 H 1.4259 0.6369 0.1551 0.043 Uiso 1 1 calc R . . C6 C 1.3289(4) 0.5713(3) 0.1659(4) 0.0259(16) Uani 1 1 d . . . H6 H 1.3449 0.5745 0.1082 0.031 Uiso 1 1 calc R . . C11 C 1.1865(4) 0.3830(3) 0.2458(3) 0.0156(13) Uani 1 1 d . . . C12 C 1.1109(4) 0.3446(3) 0.2713(3) 0.0185(14) Uani 1 1 d . . . H12 H 1.0586 0.3738 0.2626 0.022 Uiso 1 1 calc R . . C13 C 1.1105(4) 0.2632(3) 0.3098(3) 0.0221(14) Uani 1 1 d . . . H13 H 1.0582 0.2368 0.3271 0.027 Uiso 1 1 calc R . . C14 C 1.1864(5) 0.2216(3) 0.3223(4) 0.0246(16) Uani 1 1 d . . . H14 H 1.1869 0.1660 0.3475 0.030 Uiso 1 1 calc R . . C15 C 1.2613(4) 0.2597(3) 0.2988(4) 0.0253(16) Uani 1 1 d . . . H15 H 1.3128 0.2306 0.3097 0.030 Uiso 1 1 calc R . . C16 C 1.2630(4) 0.3401(3) 0.2595(3) 0.0211(14) Uani 1 1 d . . . H16 H 1.3157 0.3659 0.2419 0.025 Uiso 1 1 calc R . . C21 C 1.0823(4) 0.6930(3) -0.0218(3) 0.0134(13) Uani 1 1 d . . . C22 C 1.0095(4) 0.6645(3) -0.0242(4) 0.0200(14) Uani 1 1 d . . . H22 H 0.9856 0.6183 0.0168 0.024 Uiso 1 1 calc R . . C23 C 0.9710(4) 0.7029(4) -0.0859(4) 0.0255(15) Uani 1 1 d . . . H23 H 0.9211 0.6828 -0.0873 0.031 Uiso 1 1 calc R . . C24 C 1.0048(4) 0.7698(3) -0.1448(4) 0.0235(15) Uani 1 1 d . . . H24 H 0.9779 0.7963 -0.1868 0.028 Uiso 1 1 calc R . . C25 C 1.0774(4) 0.7987(3) -0.1434(4) 0.0238(15) Uani 1 1 d . . . H25 H 1.1010 0.8448 -0.1847 0.029 Uiso 1 1 calc R . . C26 C 1.1162(4) 0.7605(3) -0.0819(3) 0.0213(14) Uani 1 1 d . . . H26 H 1.1664 0.7806 -0.0810 0.026 Uiso 1 1 calc R . . C31 C 1.1952(4) 0.7074(3) 0.0685(4) 0.0163(14) Uani 1 1 d . . . C32 C 1.2745(4) 0.7322(3) 0.0110(4) 0.0251(16) Uani 1 1 d . . . H32 H 1.2985 0.7122 -0.0367 0.030 Uiso 1 1 calc R . . C33 C 1.3196(4) 0.7860(3) 0.0220(4) 0.0250(15) Uani 1 1 d . . . H33 H 1.3739 0.8027 -0.0180 0.030 Uiso 1 1 calc R . . C34 C 1.2846(5) 0.8150(4) 0.0915(4) 0.0303(17) Uani 1 1 d . . . H34 H 1.3148 0.8521 0.0993 0.036 Uiso 1 1 calc R . . C35 C 1.2068(5) 0.7903(4) 0.1489(4) 0.0335(18) Uani 1 1 d . . . H35 H 1.1832 0.8100 0.1969 0.040 Uiso 1 1 calc R . . C36 C 1.1617(4) 0.7364(3) 0.1379(4) 0.0220(14) Uani 1 1 d . . . H36 H 1.1076 0.7195 0.1784 0.026 Uiso 1 1 calc R . . C41 C 0.8626(4) 0.4663(3) 0.3264(3) 0.0162(13) Uani 1 1 d . . . C42 C 0.8662(4) 0.4252(3) 0.2693(4) 0.0268(16) Uani 1 1 d . . . H42 H 0.8968 0.4454 0.2120 0.032 Uiso 1 1 calc R . . C43 C 0.8254(5) 0.3551(4) 0.2958(4) 0.0329(18) Uani 1 1 d . . . H43 H 0.8273 0.3278 0.2566 0.039 Uiso 1 1 calc R . . C44 C 0.7820(5) 0.3251(4) 0.3790(4) 0.0379(19) Uani 1 1 d . . . H44 H 0.7532 0.2775 0.3972 0.045 Uiso 1 1 calc R . . C45 C 0.7804(5) 0.3640(4) 0.4358(4) 0.0371(18) Uani 1 1 d . . . H45 H 0.7518 0.3424 0.4934 0.045 Uiso 1 1 calc R . . C46 C 0.8204(5) 0.4348(4) 0.4093(4) 0.0309(17) Uani 1 1 d . . . H46 H 0.8186 0.4617 0.4489 0.037 Uiso 1 1 calc R . . C51 C 0.8904(4) 0.5975(3) 0.3760(4) 0.0187(14) Uani 1 1 d . . . C52 C 0.9593(5) 0.5887(4) 0.4077(4) 0.0295(16) Uani 1 1 d . . . H52 H 1.0156 0.5675 0.3801 0.035 Uiso 1 1 calc R . . C53 C 0.9463(5) 0.6105(4) 0.4793(4) 0.0380(19) Uani 1 1 d . . . H53 H 0.9936 0.6039 0.5012 0.046 Uiso 1 1 calc R . . C54 C 0.8647(5) 0.6423(4) 0.5198(4) 0.0350(19) Uani 1 1 d . . . H54 H 0.8559 0.6568 0.5696 0.042 Uiso 1 1 calc R . . C55 C 0.7973(5) 0.6524(4) 0.4876(4) 0.0369(19) Uani 1 1 d . . . H55 H 0.7417 0.6754 0.5142 0.044 Uiso 1 1 calc R . . C56 C 0.8095(5) 0.6295(3) 0.4163(4) 0.0293(17) Uani 1 1 d . . . H56 H 0.7618 0.6358 0.3948 0.035 Uiso 1 1 calc R . . C57 C 0.8253(4) 0.6186(3) 0.2361(3) 0.0158(13) Uani 1 1 d . . . H57A H 0.8291 0.5972 0.1893 0.019 Uiso 1 1 calc R . . H57B H 0.7663 0.6091 0.2772 0.019 Uiso 1 1 calc R . . C58 C 0.8333(4) 0.7076(3) 0.2031(3) 0.0196(15) Uani 1 1 d . . . H58A H 0.8950 0.7189 0.1900 0.024 Uiso 1 1 calc R . . H58B H 0.7961 0.7342 0.2465 0.024 Uiso 1 1 calc R . . C59 C 0.8048(4) 0.7406(3) 0.1248(3) 0.0155(13) Uani 1 1 d . . . H59A H 0.7531 0.7133 0.1323 0.019 Uiso 1 1 calc R . . H59B H 0.8529 0.7277 0.0771 0.019 Uiso 1 1 calc R . . C61 C 0.8712(4) 0.8895(3) 0.0983(4) 0.0174(14) Uani 1 1 d . . . C62 C 0.9556(4) 0.8685(3) 0.0521(4) 0.0241(15) Uani 1 1 d . . . H62 H 0.9641 0.8352 0.0165 0.029 Uiso 1 1 calc R . . C63 C 1.0258(5) 0.8955(4) 0.0580(4) 0.0309(17) Uani 1 1 d . . . H63 H 1.0834 0.8803 0.0268 0.037 Uiso 1 1 calc R . . C64 C 1.0146(5) 0.9448(4) 0.1086(4) 0.0376(19) Uani 1 1 d . . . H64 H 1.0645 0.9632 0.1121 0.045 Uiso 1 1 calc R . . C65 C 0.9314(5) 0.9673(4) 0.1540(4) 0.040(2) Uani 1 1 d . . . H65 H 0.9236 1.0014 0.1886 0.048 Uiso 1 1 calc R . . C66 C 0.8595(4) 0.9398(3) 0.1489(4) 0.0253(15) Uani 1 1 d . . . H66 H 0.8019 0.9552 0.1800 0.030 Uiso 1 1 calc R . . C71 C 0.7801(4) 0.8714(3) -0.0088(3) 0.0155(13) Uani 1 1 d . . . C72 C 0.7759(4) 0.8144(3) -0.0458(4) 0.0208(14) Uani 1 1 d . . . H72 H 0.7692 0.7608 -0.0136 0.025 Uiso 1 1 calc R . . C73 C 0.7814(4) 0.8341(3) -0.1283(4) 0.0244(15) Uani 1 1 d . . . H73 H 0.7777 0.7944 -0.1528 0.029 Uiso 1 1 calc R . . C74 C 0.7921(4) 0.9113(4) -0.1756(4) 0.0244(15) Uani 1 1 d . . . H74 H 0.7981 0.9248 -0.2333 0.029 Uiso 1 1 calc R . . C75 C 0.7940(4) 0.9694(4) -0.1386(4) 0.0289(16) Uani 1 1 d . . . H75 H 0.7997 1.0230 -0.1709 0.035 Uiso 1 1 calc R . . C76 C 0.7880(4) 0.9502(3) -0.0565(4) 0.0239(15) Uani 1 1 d . . . H76 H 0.7891 0.9905 -0.0316 0.029 Uiso 1 1 calc R . . C81 C 0.5711(4) 0.7082(3) 0.3531(4) 0.0200(14) Uani 1 1 d . . . C82 C 0.5727(4) 0.6762(4) 0.2900(4) 0.0282(16) Uani 1 1 d . . . H82 H 0.5715 0.7109 0.2376 0.034 Uiso 1 1 calc R . . C83 C 0.5760(4) 0.5955(4) 0.3015(5) 0.0361(18) Uani 1 1 d . . . H83 H 0.5763 0.5747 0.2579 0.043 Uiso 1 1 calc R . . C84 C 0.5789(5) 0.5451(4) 0.3779(5) 0.044(2) Uani 1 1 d . . . H84 H 0.5819 0.4892 0.3865 0.053 Uiso 1 1 calc R . . C85 C 0.5775(5) 0.5756(4) 0.4413(5) 0.044(2) Uani 1 1 d . . . H85 H 0.5791 0.5409 0.4936 0.053 Uiso 1 1 calc R . . C86 C 0.5737(4) 0.6568(3) 0.4286(4) 0.0274(16) Uani 1 1 d . . . H86 H 0.5729 0.6775 0.4724 0.033 Uiso 1 1 calc R . . C91 C 0.6191(4) 0.8304(3) 0.4031(4) 0.0162(14) Uani 1 1 d . . . C92 C 0.7077(4) 0.8414(3) 0.3747(4) 0.0247(15) Uani 1 1 d . . . H92 H 0.7409 0.8389 0.3196 0.030 Uiso 1 1 calc R . . C93 C 0.7489(5) 0.8559(4) 0.4242(4) 0.0313(17) Uani 1 1 d . . . H93 H 0.8102 0.8625 0.4038 0.038 Uiso 1 1 calc R . . C94 C 0.7011(5) 0.8609(3) 0.5039(4) 0.0275(17) Uani 1 1 d . . . H94 H 0.7291 0.8729 0.5375 0.033 Uiso 1 1 calc R . . C95 C 0.6129(5) 0.8486(3) 0.5348(4) 0.0266(16) Uani 1 1 d . . . H95 H 0.5803 0.8510 0.5901 0.032 Uiso 1 1 calc R . . C96 C 0.5719(4) 0.8328(3) 0.4849(4) 0.0231(15) Uani 1 1 d . . . H96 H 0.5112 0.8236 0.5064 0.028 Uiso 1 1 calc R . . C101 C 0.5122(4) 1.0692(3) 0.1364(4) 0.0176(14) Uani 1 1 d . . . C102 C 0.5306(4) 1.0568(3) 0.0591(4) 0.0208(14) Uani 1 1 d . . . H102 H 0.5637 1.0096 0.0475 0.025 Uiso 1 1 calc R . . C103 C 0.5012(4) 1.1128(4) -0.0022(4) 0.0305(17) Uani 1 1 d . . . H103 H 0.5125 1.1033 -0.0549 0.037 Uiso 1 1 calc R . . C104 C 0.4560(5) 1.1815(4) 0.0138(4) 0.0350(18) Uani 1 1 d . . . H104 H 0.4368 1.2203 -0.0285 0.042 Uiso 1 1 calc R . . C105 C 0.4377(4) 1.1955(3) 0.0912(4) 0.0274(16) Uani 1 1 d . . . H105 H 0.4062 1.2436 0.1018 0.033 Uiso 1 1 calc R . . C106 C 0.4654(4) 1.1392(3) 0.1524(4) 0.0230(14) Uani 1 1 d . . . H106 H 0.4526 1.1482 0.2056 0.028 Uiso 1 1 calc R . . C111 C 0.5852(4) 1.0455(3) 0.2699(3) 0.0157(13) Uani 1 1 d . . . C112 C 0.5648(4) 1.0255(3) 0.3550(4) 0.0191(14) Uani 1 1 d . . . H112 H 0.5223 0.9882 0.3885 0.023 Uiso 1 1 calc R . . C113 C 0.6052(4) 1.0589(3) 0.3923(4) 0.0258(16) Uani 1 1 d . . . H113 H 0.5910 1.0443 0.4512 0.031 Uiso 1 1 calc R . . C114 C 0.6656(4) 1.1128(3) 0.3452(4) 0.0250(15) Uani 1 1 d . . . H114 H 0.6937 1.1354 0.3713 0.030 Uiso 1 1 calc R . . C115 C 0.6857(4) 1.1345(4) 0.2608(4) 0.0273(16) Uani 1 1 d . . . H115 H 0.7262 1.1738 0.2283 0.033 Uiso 1 1 calc R . . C116 C 0.6476(4) 1.0997(3) 0.2222(4) 0.0227(15) Uani 1 1 d . . . H116 H 0.6641 1.1130 0.1631 0.027 Uiso 1 1 calc R . . C117 C 0.0760(5) 0.8021(4) 0.3842(4) 0.046(2) Uani 1 1 d . . . H117 H 0.1168 0.8449 0.3667 0.055 Uiso 1 1 calc R . . C118 C 0.5295(5) 0.3582(4) 0.2745(4) 0.0311(17) Uani 1 1 d . . . H118 H 0.5659 0.3982 0.2271 0.037 Uiso 1 1 calc R . . C119 C 0.9246(5) 0.0621(4) 0.4090(5) 0.051(2) Uani 1 1 d . . . H119 H 0.8966 0.0496 0.4708 0.061 Uiso 1 1 calc R . . Cl1 Cl 0.13962(14) 0.71300(11) 0.37481(12) 0.0482(5) Uani 1 1 d . . . Cl2 Cl 0.01222(17) 0.82735(16) 0.31724(14) 0.0827(9) Uani 1 1 d . . . Cl3 Cl 0.01045(17) 0.79731(15) 0.48519(13) 0.0764(8) Uani 1 1 d . . . Cl4 Cl 0.50920(13) 0.28792(10) 0.23378(12) 0.0424(5) Uani 1 1 d . . . Cl5 Cl 0.58835(14) 0.31665(11) 0.34482(12) 0.0501(5) Uani 1 1 d . . . Cl6 Cl 0.43286(15) 0.40818(13) 0.32084(15) 0.0621(7) Uani 1 1 d . . . Cl7 Cl 0.89638(14) 0.16103(12) 0.36658(13) 0.0534(5) Uani 1 1 d . . . Cl8 Cl 1.03767(15) 0.04454(14) 0.38845(15) 0.0704(7) Uani 1 1 d . . . Cl9 Cl 0.88110(19) 0.00379(16) 0.3703(2) 0.1019(10) Uani 1 1 d . . . B8 B 1.3342(5) 0.4179(4) -0.0407(4) 0.0254(18) Uani 1 1 d . . . H8 H 1.3796 0.3666 -0.0586 0.031 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 Au1 0.01505(16) 0.01901(12) 0.01306(12) -0.00600(9) -0.00333(11) -0.00084(10) Au2 0.01575(16) 0.01974(12) 0.01426(13) -0.00682(9) -0.00411(11) 0.00207(10) P1 0.0151(10) 0.0171(7) 0.0130(8) -0.0035(6) -0.0048(8) 0.0010(7) P2 0.0150(10) 0.0150(7) 0.0136(8) -0.0043(6) -0.0043(7) -0.0004(6) P3 0.0137(10) 0.0167(7) 0.0147(8) -0.0041(6) -0.0071(8) 0.0029(7) P4 0.0155(10) 0.0167(7) 0.0107(8) -0.0030(6) -0.0035(7) 0.0020(7) P5 0.0179(10) 0.0170(7) 0.0137(8) -0.0048(6) -0.0063(8) 0.0031(7) P6 0.0159(10) 0.0171(7) 0.0121(8) -0.0033(6) -0.0046(7) 0.0012(7) B1 0.016(5) 0.031(4) 0.021(4) -0.011(3) -0.005(4) 0.004(3) B2 0.018(5) 0.026(4) 0.022(4) -0.003(3) -0.001(4) -0.002(3) B3 0.021(5) 0.023(3) 0.017(4) -0.005(3) -0.003(4) 0.002(3) B4 0.032(5) 0.021(3) 0.013(4) -0.005(3) -0.007(4) 0.007(3) B5 0.032(5) 0.022(3) 0.012(4) -0.010(3) -0.007(4) 0.002(3) B6 0.023(5) 0.022(3) 0.023(4) -0.013(3) -0.010(4) -0.001(3) B7 0.030(5) 0.013(3) 0.018(4) -0.004(3) -0.006(4) -0.001(3) C7 0.024(4) 0.018(3) 0.015(3) -0.006(2) -0.007(3) -0.003(3) C8 0.020(4) 0.022(3) 0.009(3) -0.005(2) -0.003(3) -0.001(3) B9 0.031(5) 0.028(4) 0.019(4) -0.011(3) -0.008(4) 0.002(3) B10 0.023(5) 0.024(4) 0.021(4) -0.007(3) -0.008(4) 0.007(3) B11 0.022(5) 0.026(4) 0.016(4) -0.007(3) -0.005(4) 0.000(3) B12 0.021(5) 0.023(3) 0.020(4) -0.006(3) -0.013(4) 0.001(3) B13 0.011(5) 0.028(4) 0.016(4) -0.001(3) -0.006(3) 0.005(3) B14 0.013(5) 0.030(4) 0.016(4) -0.002(3) -0.006(4) -0.002(3) B15 0.024(5) 0.026(4) 0.017(4) -0.006(3) -0.009(4) -0.006(3) B16 0.017(5) 0.022(3) 0.020(4) -0.006(3) -0.007(4) -0.003(3) B17 0.014(5) 0.025(3) 0.013(4) 0.002(3) -0.005(3) -0.004(3) B18 0.018(5) 0.036(4) 0.017(4) -0.002(3) -0.010(4) -0.006(3) C9 0.018(4) 0.018(3) 0.013(3) -0.003(2) -0.009(3) 0.002(3) C10 0.011(4) 0.016(3) 0.015(3) -0.002(2) -0.006(3) 0.003(3) C1 0.014(4) 0.015(3) 0.022(3) -0.005(2) -0.010(3) 0.001(3) C2 0.020(4) 0.031(3) 0.022(3) -0.014(3) -0.006(3) 0.003(3) C3 0.037(5) 0.043(4) 0.033(4) -0.023(3) -0.019(4) 0.012(4) C4 0.029(5) 0.041(4) 0.056(5) -0.028(4) -0.026(4) 0.004(4) C5 0.032(5) 0.035(4) 0.044(5) -0.009(3) -0.015(4) -0.007(3) C6 0.028(5) 0.026(3) 0.024(4) -0.005(3) -0.010(3) 0.000(3) C11 0.021(4) 0.015(3) 0.010(3) -0.003(2) -0.004(3) -0.002(3) C12 0.016(4) 0.026(3) 0.012(3) -0.002(2) -0.005(3) 0.002(3) C13 0.020(4) 0.030(3) 0.014(3) -0.003(3) -0.001(3) -0.010(3) C14 0.039(5) 0.018(3) 0.019(3) -0.004(3) -0.012(3) -0.003(3) C15 0.033(5) 0.027(3) 0.019(3) -0.005(3) -0.017(3) 0.008(3) C16 0.024(4) 0.024(3) 0.017(3) -0.004(3) -0.009(3) 0.000(3) C21 0.011(4) 0.018(3) 0.008(3) -0.003(2) -0.001(3) 0.001(3) C22 0.017(4) 0.021(3) 0.020(3) -0.008(3) -0.007(3) 0.008(3) C23 0.014(4) 0.038(4) 0.026(4) -0.012(3) -0.008(3) 0.003(3) C24 0.021(4) 0.033(3) 0.011(3) -0.004(3) -0.004(3) 0.006(3) C25 0.025(4) 0.025(3) 0.016(3) -0.001(3) -0.006(3) 0.001(3) C26 0.018(4) 0.026(3) 0.019(3) -0.008(3) -0.006(3) 0.004(3) C31 0.020(4) 0.013(3) 0.018(3) -0.005(2) -0.009(3) 0.002(3) C32 0.025(5) 0.030(3) 0.025(4) -0.014(3) -0.011(4) 0.002(3) C33 0.020(4) 0.030(3) 0.023(4) -0.003(3) -0.004(3) -0.010(3) C34 0.034(5) 0.033(4) 0.029(4) -0.007(3) -0.011(4) -0.016(3) C35 0.038(5) 0.043(4) 0.028(4) -0.022(3) -0.009(4) -0.005(4) C36 0.020(4) 0.025(3) 0.021(3) -0.008(3) -0.004(3) -0.005(3) C41 0.008(4) 0.021(3) 0.016(3) -0.001(2) -0.005(3) 0.002(3) C42 0.032(5) 0.031(3) 0.015(3) 0.001(3) -0.007(3) -0.010(3) C43 0.043(5) 0.030(3) 0.034(4) -0.007(3) -0.021(4) -0.008(3) C44 0.051(6) 0.027(4) 0.036(4) 0.006(3) -0.021(4) -0.016(3) C45 0.045(6) 0.035(4) 0.027(4) 0.000(3) -0.008(4) -0.011(4) C46 0.036(5) 0.031(4) 0.028(4) -0.008(3) -0.014(4) -0.003(3) C51 0.020(4) 0.019(3) 0.016(3) -0.006(2) -0.005(3) 0.002(3) C52 0.025(5) 0.042(4) 0.030(4) -0.018(3) -0.012(4) -0.001(3) C53 0.041(6) 0.051(4) 0.031(4) -0.013(4) -0.017(4) -0.013(4) C54 0.054(6) 0.033(4) 0.019(4) -0.011(3) -0.008(4) -0.005(4) C55 0.050(6) 0.029(4) 0.023(4) -0.009(3) -0.004(4) 0.008(3) C56 0.033(5) 0.034(4) 0.018(3) -0.008(3) -0.009(3) 0.013(3) C57 0.014(4) 0.019(3) 0.013(3) -0.001(2) -0.005(3) -0.002(3) C58 0.025(4) 0.018(3) 0.017(3) -0.004(3) -0.013(3) 0.007(3) C59 0.017(4) 0.014(3) 0.016(3) -0.005(2) -0.009(3) 0.006(2) C61 0.019(4) 0.012(3) 0.021(3) 0.000(2) -0.012(3) 0.003(3) C62 0.020(4) 0.029(3) 0.028(4) -0.011(3) -0.015(3) 0.008(3) C63 0.023(5) 0.037(4) 0.026(4) 0.003(3) -0.010(4) -0.001(3) C64 0.036(6) 0.040(4) 0.044(5) 0.002(3) -0.026(4) -0.018(4) C65 0.053(6) 0.038(4) 0.041(5) -0.018(3) -0.023(5) -0.003(4) C66 0.026(5) 0.025(3) 0.027(4) -0.010(3) -0.006(3) -0.002(3) C71 0.008(4) 0.022(3) 0.013(3) -0.004(2) -0.002(3) 0.003(3) C72 0.018(4) 0.022(3) 0.020(3) -0.005(3) -0.009(3) 0.008(3) C73 0.026(4) 0.030(3) 0.019(3) -0.010(3) -0.010(3) 0.009(3) C74 0.018(4) 0.038(4) 0.013(3) -0.002(3) -0.006(3) 0.002(3) C75 0.031(5) 0.027(3) 0.022(4) 0.009(3) -0.013(3) -0.004(3) C76 0.026(4) 0.022(3) 0.025(4) -0.006(3) -0.013(3) 0.002(3) C81 0.015(4) 0.017(3) 0.025(4) -0.005(3) -0.004(3) 0.001(3) C82 0.023(4) 0.032(3) 0.034(4) -0.019(3) -0.007(4) 0.004(3) C83 0.023(5) 0.034(4) 0.054(5) -0.027(4) -0.002(4) 0.000(3) C84 0.030(5) 0.022(4) 0.079(6) -0.015(4) -0.014(5) 0.000(3) C85 0.046(6) 0.027(4) 0.053(5) 0.001(3) -0.018(5) -0.005(3) C86 0.026(5) 0.021(3) 0.030(4) -0.001(3) -0.008(3) -0.003(3) C91 0.015(4) 0.015(3) 0.020(3) -0.001(2) -0.010(3) 0.002(3) C92 0.022(5) 0.027(3) 0.026(4) -0.011(3) -0.010(3) 0.007(3) C93 0.020(5) 0.043(4) 0.037(4) -0.014(3) -0.013(4) -0.004(3) C94 0.034(5) 0.028(3) 0.028(4) -0.006(3) -0.020(4) -0.003(3) C95 0.029(5) 0.034(4) 0.019(4) -0.006(3) -0.012(4) -0.001(3) C96 0.016(4) 0.034(3) 0.017(3) -0.006(3) -0.003(3) 0.001(3) C101 0.015(4) 0.013(3) 0.020(3) 0.004(2) -0.005(3) -0.005(3) C102 0.025(4) 0.018(3) 0.021(3) -0.003(2) -0.007(3) -0.012(3) C103 0.040(5) 0.037(4) 0.018(3) 0.004(3) -0.015(4) -0.021(3) C104 0.032(5) 0.032(4) 0.041(4) 0.012(3) -0.025(4) -0.011(3) C105 0.022(4) 0.020(3) 0.035(4) 0.006(3) -0.011(4) -0.005(3) C106 0.015(4) 0.025(3) 0.022(4) -0.002(3) 0.001(3) -0.004(3) C111 0.015(4) 0.016(3) 0.016(3) -0.005(2) -0.007(3) 0.006(3) C112 0.015(4) 0.019(3) 0.020(3) -0.005(2) -0.004(3) 0.004(3) C113 0.038(5) 0.027(3) 0.017(3) -0.008(3) -0.017(3) 0.008(3) C114 0.022(4) 0.030(3) 0.027(4) -0.007(3) -0.015(3) 0.002(3) C115 0.024(5) 0.032(3) 0.025(4) -0.002(3) -0.007(3) -0.010(3) C116 0.018(4) 0.032(3) 0.018(3) -0.005(3) -0.006(3) -0.005(3) C117 0.040(6) 0.060(5) 0.034(4) -0.014(4) -0.005(4) -0.006(4) C118 0.034(5) 0.033(4) 0.024(4) 0.002(3) -0.012(4) -0.008(3) C119 0.022(5) 0.055(5) 0.068(6) -0.023(4) 0.002(5) -0.003(4) Cl1 0.0478(15) 0.0474(11) 0.0454(12) 0.0002(9) -0.0191(11) -0.0064(10) Cl2 0.070(2) 0.123(2) 0.0530(14) -0.0441(15) -0.0288(14) 0.0580(16) Cl3 0.087(2) 0.1084(19) 0.0393(13) -0.0383(13) 0.0073(13) -0.0438(15) Cl4 0.0394(13) 0.0445(10) 0.0526(12) -0.0232(9) -0.0176(11) -0.0016(9) Cl5 0.0496(15) 0.0597(12) 0.0500(12) -0.0175(10) -0.0346(12) 0.0183(10) Cl6 0.0544(16) 0.0722(14) 0.0884(17) -0.0538(13) -0.0492(14) 0.0369(12) Cl7 0.0511(16) 0.0565(12) 0.0471(13) -0.0064(10) -0.0143(12) -0.0051(10) Cl8 0.0391(16) 0.0742(15) 0.0726(17) 0.0020(13) -0.0098(14) 0.0068(12) Cl9 0.079(2) 0.0931(19) 0.149(3) -0.080(2) -0.009(2) -0.0124(16) B8 0.033(6) 0.022(4) 0.018(4) -0.006(3) -0.006(4) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P3 2.2815(17) . ? Au1 P1 2.4071(16) . ? Au1 P2 2.4155(16) . ? Au2 P4 2.2704(16) . ? Au2 P6 2.3546(15) . ? Au2 P5 2.4186(16) . ? P1 C1 1.803(5) . ? P1 C11 1.809(5) . ? P1 C7 1.831(6) . ? P2 C21 1.815(5) . ? P2 C31 1.816(6) . ? P2 C8 1.834(6) . ? P3 C41 1.813(6) . ? P3 C51 1.814(5) . ? P3 C57 1.824(5) . ? P4 C61 1.810(6) . ? P4 C71 1.811(5) . ? P4 C59 1.821(5) . ? P5 C81 1.800(5) . ? P5 C91 1.817(5) . ? P5 C9 1.836(6) . ? P6 C10 1.815(6) . ? P6 C111 1.815(5) . ? P6 C101 1.820(5) . ? B1 C7 1.617(9) . ? B1 B8 1.782(9) . ? B1 B7 1.782(10) . ? B1 B2 1.859(10) . ? B2 B4 1.768(10) . ? B2 B8 1.786(10) . ? B2 B3 1.832(10) . ? B3 C8 1.620(9) . ? B3 B4 1.747(9) . ? B3 B5 1.755(10) . ? B4 B5 1.733(11) . ? B4 B9 1.784(11) . ? B4 B8 1.810(9) . ? B5 C8 1.732(8) . ? B5 B9 1.764(9) . ? B5 B6 1.768(10) . ? B6 C7 1.740(8) . ? B6 C8 1.741(8) . ? B6 B9 1.761(9) . ? B6 B7 1.761(9) . ? B7 C7 1.719(8) . ? B7 B8 1.733(10) . ? B7 B9 1.735(9) . ? C7 C8 1.600(7) . ? B9 B8 1.775(11) . ? B10 C10 1.648(9) . ? B10 B13 1.745(10) . ? B10 B14 1.803(9) . ? B10 B11 1.833(10) . ? B11 B13 1.766(9) . ? B11 B17 1.766(9) . ? B11 B12 1.812(9) . ? B12 C9 1.607(9) . ? B12 B17 1.746(9) . ? B12 B16 1.775(8) . ? B13 B14 1.745(10) . ? B13 B18 1.778(9) . ? B13 B17 1.797(9) . ? B14 C10 1.709(8) . ? B14 B18 1.738(10) . ? B14 B15 1.751(9) . ? B15 C10 1.726(8) . ? B15 C9 1.747(8) . ? B15 B18 1.768(11) . ? B15 B16 1.770(10) . ? B16 B17 1.744(10) . ? B16 C9 1.747(8) . ? B16 B18 1.764(9) . ? B17 B18 1.781(9) . ? C9 C10 1.614(7) . ? C1 C6 1.376(8) . ? C1 C2 1.404(8) . ? C2 C3 1.382(8) . ? C3 C4 1.367(10) . ? C4 C5 1.360(9) . ? C5 C6 1.391(8) . ? C11 C12 1.375(8) . ? C11 C16 1.397(8) . ? C12 C13 1.396(7) . ? C13 C14 1.375(8) . ? C14 C15 1.369(9) . ? C15 C16 1.383(7) . ? C21 C22 1.381(8) . ? C21 C26 1.384(8) . ? C22 C23 1.385(7) . ? C23 C24 1.369(8) . ? C24 C25 1.373(8) . ? C25 C26 1.385(7) . ? C31 C36 1.380(7) . ? C31 C32 1.383(8) . ? C32 C33 1.389(8) . ? C33 C34 1.381(8) . ? C34 C35 1.366(9) . ? C35 C36 1.391(8) . ? C41 C46 1.371(8) . ? C41 C42 1.396(7) . ? C42 C43 1.384(8) . ? C43 C44 1.376(9) . ? C44 C45 1.371(9) . ? C45 C46 1.390(9) . ? C51 C56 1.379(8) . ? C51 C52 1.382(8) . ? C52 C53 1.373(8) . ? C53 C54 1.387(9) . ? C54 C55 1.361(9) . ? C55 C56 1.383(8) . ? C57 C58 1.518(7) . ? C58 C59 1.528(7) . ? C61 C62 1.389(8) . ? C61 C66 1.395(7) . ? C62 C63 1.355(8) . ? C63 C64 1.382(9) . ? C64 C65 1.378(10) . ? C65 C66 1.378(9) . ? C71 C72 1.381(7) . ? C71 C76 1.396(7) . ? C72 C73 1.371(7) . ? C73 C74 1.374(8) . ? C74 C75 1.386(8) . ? C75 C76 1.362(8) . ? C81 C86 1.380(8) . ? C81 C82 1.391(8) . ? C82 C83 1.374(8) . ? C83 C84 1.388(10) . ? C84 C85 1.380(10) . ? C85 C86 1.379(8) . ? C91 C92 1.379(8) . ? C91 C96 1.399(8) . ? C92 C93 1.371(8) . ? C93 C94 1.380(9) . ? C94 C95 1.377(8) . ? C95 C96 1.386(7) . ? C101 C102 1.377(7) . ? C101 C106 1.391(8) . ? C102 C103 1.388(8) . ? C103 C104 1.365(9) . ? C104 C105 1.390(9) . ? C105 C106 1.377(8) . ? C111 C112 1.372(7) . ? C111 C116 1.385(8) . ? C112 C113 1.372(7) . ? C113 C114 1.359(9) . ? C114 C115 1.360(8) . ? C115 C116 1.381(7) . ? C117 Cl3 1.725(7) . ? C117 Cl2 1.743(7) . ? C117 Cl1 1.752(7) . ? C118 Cl6 1.732(7) . ? C118 Cl5 1.739(6) . ? C118 Cl4 1.741(6) . ? C119 Cl7 1.734(8) . ? C119 Cl8 1.736(8) . ? C119 Cl9 1.746(8) . ? 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 P3 Au1 P1 137.77(5) . . ? P3 Au1 P2 139.42(5) . . ? P1 Au1 P2 82.62(5) . . ? P4 Au2 P6 145.96(5) . . ? P4 Au2 P5 128.78(5) . . ? P6 Au2 P5 85.05(5) . . ? C1 P1 C11 105.6(2) . . ? C1 P1 C7 107.5(3) . . ? C11 P1 C7 105.2(2) . . ? C1 P1 Au1 112.59(18) . . ? C11 P1 Au1 119.8(2) . . ? C7 P1 Au1 105.44(19) . . ? C21 P2 C31 105.8(2) . . ? C21 P2 C8 103.9(2) . . ? C31 P2 C8 106.9(3) . . ? C21 P2 Au1 124.0(2) . . ? C31 P2 Au1 109.65(19) . . ? C8 P2 Au1 105.38(18) . . ? C41 P3 C51 104.7(3) . . ? C41 P3 C57 99.3(2) . . ? C51 P3 C57 106.5(3) . . ? C41 P3 Au1 115.4(2) . . ? C51 P3 Au1 115.0(2) . . ? C57 P3 Au1 114.2(2) . . ? C61 P4 C71 105.8(3) . . ? C61 P4 C59 104.2(3) . . ? C71 P4 C59 103.4(2) . . ? C61 P4 Au2 111.2(2) . . ? C71 P4 Au2 117.03(19) . . ? C59 P4 Au2 114.0(2) . . ? C81 P5 C91 105.5(2) . . ? C81 P5 C9 107.5(3) . . ? C91 P5 C9 109.5(3) . . ? C81 P5 Au2 119.2(2) . . ? C91 P5 Au2 109.4(2) . . ? C9 P5 Au2 105.53(18) . . ? C10 P6 C111 107.1(3) . . ? C10 P6 C101 107.2(3) . . ? C111 P6 C101 105.0(2) . . ? C10 P6 Au2 105.55(17) . . ? C111 P6 Au2 107.62(18) . . ? C101 P6 Au2 123.5(2) . . ? C7 B1 B8 105.0(5) . . ? C7 B1 B7 60.5(4) . . ? B8 B1 B7 58.2(4) . . ? C7 B1 B2 106.8(5) . . ? B8 B1 B2 58.7(4) . . ? B7 B1 B2 106.8(5) . . ? B4 B2 B8 61.2(4) . . ? B4 B2 B3 58.0(4) . . ? B8 B2 B3 105.0(5) . . ? B4 B2 B1 105.3(5) . . ? B8 B2 B1 58.5(4) . . ? B3 B2 B1 101.2(5) . . ? C8 B3 B4 105.9(5) . . ? C8 B3 B5 61.6(4) . . ? B4 B3 B5 59.3(4) . . ? C8 B3 B2 106.4(5) . . ? B4 B3 B2 59.1(4) . . ? B5 B3 B2 108.6(5) . . ? B5 B4 B3 60.6(4) . . ? B5 B4 B2 112.6(5) . . ? B3 B4 B2 62.8(4) . . ? B5 B4 B9 60.2(4) . . ? B3 B4 B9 108.1(5) . . ? B2 B4 B9 109.9(5) . . ? B5 B4 B8 107.7(5) . . ? B3 B4 B8 107.6(4) . . ? B2 B4 B8 59.9(4) . . ? B9 B4 B8 59.2(4) . . ? C8 B5 B4 101.8(5) . . ? C8 B5 B3 55.4(3) . . ? B4 B5 B3 60.1(4) . . ? C8 B5 B9 103.8(4) . . ? B4 B5 B9 61.3(4) . . ? B3 B5 B9 108.7(5) . . ? C8 B5 B6 59.7(3) . . ? B4 B5 B6 108.8(5) . . ? B3 B5 B6 107.3(5) . . ? B9 B5 B6 59.8(4) . . ? C7 B6 C8 54.7(3) . . ? C7 B6 B9 103.4(5) . . ? C8 B6 B9 103.5(5) . . ? C7 B6 B7 58.8(3) . . ? C8 B6 B7 102.5(5) . . ? B9 B6 B7 59.0(4) . . ? C7 B6 B5 103.4(5) . . ? C8 B6 B5 59.1(3) . . ? B9 B6 B5 59.9(4) . . ? B7 B6 B5 107.2(5) . . ? C7 B7 B8 102.9(5) . . ? C7 B7 B9 105.4(4) . . ? B8 B7 B9 61.6(4) . . ? C7 B7 B6 60.0(3) . . ? B8 B7 B6 109.4(5) . . ? B9 B7 B6 60.5(4) . . ? C7 B7 B1 55.0(3) . . ? B8 B7 B1 60.9(4) . . ? B9 B7 B1 109.6(5) . . ? B6 B7 B1 107.1(4) . . ? C8 C7 B1 111.8(5) . . ? C8 C7 B7 110.7(4) . . ? B1 C7 B7 64.5(4) . . ? C8 C7 B6 62.7(3) . . ? B1 C7 B6 116.1(4) . . ? B7 C7 B6 61.2(4) . . ? C8 C7 P1 116.3(4) . . ? B1 C7 P1 124.2(4) . . ? B7 C7 P1 118.5(4) . . ? B6 C7 P1 110.0(4) . . ? C7 C8 B3 113.7(5) . . ? C7 C8 B5 111.4(4) . . ? B3 C8 B5 63.0(4) . . ? C7 C8 B6 62.6(3) . . ? B3 C8 B6 115.1(4) . . ? B5 C8 B6 61.2(4) . . ? C7 C8 P2 114.8(4) . . ? B3 C8 P2 123.7(4) . . ? B5 C8 P2 119.9(4) . . ? B6 C8 P2 111.4(4) . . ? B7 B9 B6 60.5(4) . . ? B7 B9 B5 108.5(4) . . ? B6 B9 B5 60.2(4) . . ? B7 B9 B8 59.1(4) . . ? B6 B9 B8 107.5(5) . . ? B5 B9 B8 107.9(5) . . ? B7 B9 B4 108.0(5) . . ? B6 B9 B4 106.8(5) . . ? B5 B9 B4 58.5(4) . . ? B8 B9 B4 61.1(4) . . ? C10 B10 B13 104.7(5) . . ? C10 B10 B14 59.2(4) . . ? B13 B10 B14 58.9(4) . . ? C10 B10 B11 107.2(5) . . ? B13 B10 B11 59.1(4) . . ? B14 B10 B11 107.5(5) . . ? B13 B11 B17 61.2(4) . . ? B13 B11 B12 105.0(4) . . ? B17 B11 B12 58.4(4) . . ? B13 B11 B10 58.0(4) . . ? B17 B11 B10 105.5(5) . . ? B12 B11 B10 101.9(5) . . ? C9 B12 B17 106.3(5) . . ? C9 B12 B16 62.0(4) . . ? B17 B12 B16 59.4(4) . . ? C9 B12 B11 106.8(5) . . ? B17 B12 B11 59.5(4) . . ? B16 B12 B11 109.1(4) . . ? B14 B13 B10 62.2(4) . . ? B14 B13 B11 113.3(5) . . ? B10 B13 B11 62.9(4) . . ? B14 B13 B18 59.1(4) . . ? B10 B13 B18 109.1(5) . . ? B11 B13 B18 110.1(5) . . ? B14 B13 B17 107.3(5) . . ? B10 B13 B17 107.9(5) . . ? B11 B13 B17 59.4(3) . . ? B18 B13 B17 59.7(4) . . ? C10 B14 B18 105.7(5) . . ? C10 B14 B13 102.1(4) . . ? B18 B14 B13 61.4(4) . . ? C10 B14 B15 59.9(3) . . ? B18 B14 B15 60.9(4) . . ? B13 B14 B15 108.9(5) . . ? C10 B14 B10 55.9(3) . . ? B18 B14 B10 108.3(5) . . ? B13 B14 B10 58.9(4) . . ? B15 B14 B10 107.0(4) . . ? C10 B15 C9 55.4(3) . . ? C10 B15 B14 58.9(3) . . ? C9 B15 B14 102.8(4) . . ? C10 B15 B18 103.7(5) . . ? C9 B15 B18 103.3(5) . . ? B14 B15 B18 59.2(4) . . ? C10 B15 B16 104.8(4) . . ? C9 B15 B16 59.6(3) . . ? B14 B15 B16 107.8(5) . . ? B18 B15 B16 59.8(4) . . ? B17 B16 C9 100.6(4) . . ? B17 B16 B18 61.0(4) . . ? C9 B16 B18 103.5(4) . . ? B17 B16 B15 108.2(5) . . ? C9 B16 B15 59.6(3) . . ? B18 B16 B15 60.0(4) . . ? B17 B16 B12 59.5(4) . . ? C9 B16 B12 54.3(3) . . ? B18 B16 B12 107.6(5) . . ? B15 B16 B12 106.0(4) . . ? B16 B17 B12 61.1(4) . . ? B16 B17 B11 112.7(5) . . ? B12 B17 B11 62.1(4) . . ? B16 B17 B18 60.1(4) . . ? B12 B17 B18 108.1(5) . . ? B11 B17 B18 110.0(5) . . ? B16 B17 B13 107.7(5) . . ? B12 B17 B13 106.5(5) . . ? B11 B17 B13 59.4(4) . . ? B18 B17 B13 59.6(4) . . ? B14 B18 B16 108.7(5) . . ? B14 B18 B15 59.9(4) . . ? B16 B18 B15 60.2(4) . . ? B14 B18 B13 59.5(4) . . ? B16 B18 B13 107.7(4) . . ? B15 B18 B13 106.6(5) . . ? B14 B18 B17 108.3(5) . . ? B16 B18 B17 58.9(4) . . ? B15 B18 B17 106.7(5) . . ? B13 B18 B17 60.7(4) . . ? B12 C9 C10 114.1(4) . . ? B12 C9 B15 115.1(5) . . ? C10 C9 B15 61.7(3) . . ? B12 C9 B16 63.7(4) . . ? C10 C9 B16 111.0(4) . . ? B15 C9 B16 60.9(4) . . ? B12 C9 P5 125.0(4) . . ? C10 C9 P5 114.0(4) . . ? B15 C9 P5 110.2(4) . . ? B16 C9 P5 119.2(4) . . ? C9 C10 B10 109.9(5) . . ? C9 C10 B14 110.7(4) . . ? B10 C10 B14 64.9(4) . . ? C9 C10 B15 63.0(3) . . ? B10 C10 B15 115.7(5) . . ? B14 C10 B15 61.3(4) . . ? C9 C10 P6 118.5(4) . . ? B10 C10 P6 123.4(4) . . ? B14 C10 P6 117.9(4) . . ? B15 C10 P6 111.5(4) . . ? C6 C1 C2 118.4(5) . . ? C6 C1 P1 124.2(4) . . ? C2 C1 P1 117.0(5) . . ? C3 C2 C1 119.7(6) . . ? C4 C3 C2 120.8(6) . . ? C5 C4 C3 120.3(6) . . ? C4 C5 C6 120.0(7) . . ? C1 C6 C5 120.9(6) . . ? C12 C11 C16 119.5(5) . . ? C12 C11 P1 118.9(4) . . ? C16 C11 P1 121.5(5) . . ? C11 C12 C13 120.6(5) . . ? C14 C13 C12 119.3(6) . . ? C15 C14 C13 120.5(5) . . ? C14 C15 C16 120.7(6) . . ? C15 C16 C11 119.3(6) . . ? C22 C21 C26 119.0(5) . . ? C22 C21 P2 117.9(4) . . ? C26 C21 P2 123.1(4) . . ? C21 C22 C23 120.4(6) . . ? C24 C23 C22 120.1(6) . . ? C23 C24 C25 120.2(5) . . ? C24 C25 C26 120.0(6) . . ? C21 C26 C25 120.3(6) . . ? C36 C31 C32 118.7(5) . . ? C36 C31 P2 116.8(5) . . ? C32 C31 P2 124.5(4) . . ? C31 C32 C33 121.1(6) . . ? C34 C33 C32 119.4(6) . . ? C35 C34 C33 119.9(6) . . ? C34 C35 C36 120.7(6) . . ? C31 C36 C35 120.2(6) . . ? C46 C41 C42 118.9(5) . . ? C46 C41 P3 123.6(4) . . ? C42 C41 P3 117.4(4) . . ? C43 C42 C41 120.4(6) . . ? C44 C43 C42 119.9(6) . . ? C45 C44 C43 120.0(6) . . ? C44 C45 C46 120.2(6) . . ? C41 C46 C45 120.6(6) . . ? C56 C51 C52 119.3(5) . . ? C56 C51 P3 121.6(4) . . ? C52 C51 P3 119.0(5) . . ? C53 C52 C51 119.8(6) . . ? C52 C53 C54 120.7(6) . . ? C55 C54 C53 119.4(6) . . ? C54 C55 C56 120.3(7) . . ? C51 C56 C55 120.4(6) . . ? C58 C57 P3 115.4(4) . . ? C57 C58 C59 110.8(4) . . ? C58 C59 P4 114.7(3) . . ? C62 C61 C66 119.4(5) . . ? C62 C61 P4 121.0(4) . . ? C66 C61 P4 119.5(5) . . ? C63 C62 C61 120.0(6) . . ? C62 C63 C64 120.9(7) . . ? C65 C64 C63 120.1(6) . . ? C64 C65 C66 119.5(6) . . ? C65 C66 C61 120.1(6) . . ? C72 C71 C76 118.9(5) . . ? C72 C71 P4 122.4(4) . . ? C76 C71 P4 118.8(4) . . ? C73 C72 C71 120.9(5) . . ? C72 C73 C74 120.0(5) . . ? C73 C74 C75 119.7(5) . . ? C76 C75 C74 120.6(6) . . ? C75 C76 C71 120.0(5) . . ? C86 C81 C82 118.3(5) . . ? C86 C81 P5 123.6(4) . . ? C82 C81 P5 117.9(5) . . ? C83 C82 C81 121.6(6) . . ? C82 C83 C84 118.9(6) . . ? C85 C84 C83 120.4(6) . . ? C86 C85 C84 119.8(7) . . ? C85 C86 C81 121.0(6) . . ? C92 C91 C96 118.3(5) . . ? C92 C91 P5 116.3(4) . . ? C96 C91 P5 125.3(5) . . ? C93 C92 C91 121.4(6) . . ? C92 C93 C94 119.8(7) . . ? C95 C94 C93 120.2(6) . . ? C94 C95 C96 119.7(6) . . ? C95 C96 C91 120.4(6) . . ? C102 C101 C106 119.6(5) . . ? C102 C101 P6 119.3(4) . . ? C106 C101 P6 121.0(4) . . ? C101 C102 C103 120.4(6) . . ? C104 C103 C102 119.7(6) . . ? C103 C104 C105 120.7(6) . . ? C106 C105 C104 119.5(6) . . ? C105 C106 C101 120.1(6) . . ? C112 C111 C116 118.9(5) . . ? C112 C111 P6 122.1(4) . . ? C116 C111 P6 118.3(4) . . ? C111 C112 C113 120.5(6) . . ? C114 C113 C112 120.3(6) . . ? C113 C114 C115 120.1(6) . . ? C114 C115 C116 120.3(6) . . ? C115 C116 C111 119.7(6) . . ? Cl3 C117 Cl2 110.5(4) . . ? Cl3 C117 Cl1 112.4(4) . . ? Cl2 C117 Cl1 109.8(4) . . ? Cl6 C118 Cl5 110.1(4) . . ? Cl6 C118 Cl4 111.4(4) . . ? Cl5 C118 Cl4 112.2(3) . . ? Cl7 C119 Cl8 110.9(4) . . ? Cl7 C119 Cl9 108.1(5) . . ? Cl8 C119 Cl9 112.9(4) . . ? B7 B8 B9 59.3(4) . . ? B7 B8 B1 60.9(4) . . ? B9 B8 B1 107.8(5) . . ? B7 B8 B2 112.3(5) . . ? B9 B8 B2 109.5(5) . . ? B1 B8 B2 62.8(4) . . ? B7 B8 B4 106.9(5) . . ? B9 B8 B4 59.7(4) . . ? B1 B8 B4 106.8(4) . . ? B2 B8 B4 58.9(4) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 2.357 _refine_diff_density_min -2.326 _refine_diff_density_rms 0.163