# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'C Russell' 'Michael Green' 'Thomas N. Hooper' 'John McGrady' 'Jaynika R Patel' _publ_contact_author_name 'C Russell' _publ_contact_author_email CHRIS.RUSSELL@BRIS.AC.UK _publ_section_title ; Synthesis and Structural Characterisation of Stable Cationic Gold(I) Alkene Complexes ; # Attachment 'merged_gold_alkene_cifs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 729111' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C19 H37 Au P, F6 Sb' _chemical_formula_sum 'C19 H37 Au F6 P Sb' _chemical_formula_weight 729.17 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.1323(3) _cell_length_b 16.5890(4) _cell_length_c 22.2175(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4840.12(19) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9972 _cell_measurement_theta_min 3.668 _cell_measurement_theta_max 27.471 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.001 _exptl_crystal_density_method none _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 7.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.471 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 30521 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5541 _reflns_number_gt 4754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0209P)^2^+5.3056P] 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 5541 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0531 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Au1 Au 0.856646(9) 0.050482(8) 0.348324(5) 0.01667(5) Uani 1 1 d . . . C1 C 0.8976(3) -0.0230(2) 0.26397(15) 0.0205(8) Uani 1 1 d . . . H1 H 0.8431 0.0041 0.2466 0.025 Uiso 1 1 calc R . . C2 C 0.9850(3) 0.0111(2) 0.28565(14) 0.0194(7) Uani 1 1 d . . . H2 H 1.0013 0.0656 0.2855 0.023 Uiso 1 1 calc R . . C3 C 1.0499(3) -0.0565(2) 0.30997(16) 0.0220(8) Uani 1 1 d . . . H3 H 1.1024 -0.0414 0.3392 0.026 Uiso 1 1 calc R . . C4 C 0.9700(3) -0.1169(2) 0.33131(16) 0.0234(8) Uani 1 1 d . . . H4A H 0.9330 -0.0984 0.3665 0.028 Uiso 1 1 calc R . . H4B H 0.9981 -0.1701 0.3385 0.028 Uiso 1 1 calc R . . C5 C 0.9063(3) -0.1127(2) 0.27349(16) 0.0241(8) Uani 1 1 d . . . H5 H 0.8426 -0.1434 0.2731 0.029 Uiso 1 1 calc R . . C6 C 0.9894(3) -0.1379(3) 0.22618(17) 0.0299(9) Uani 1 1 d . . . H6A H 0.9957 -0.1961 0.2237 0.036 Uiso 1 1 calc R . . H6B H 0.9735 -0.1167 0.1866 0.036 Uiso 1 1 calc R . . C7 C 1.0876(3) -0.0995(3) 0.25148(16) 0.0267(9) Uani 1 1 d . . . H7A H 1.1163 -0.0611 0.2233 0.032 Uiso 1 1 calc R . . H7B H 1.1382 -0.1403 0.2606 0.032 Uiso 1 1 calc R . . P1 P 0.77554(6) 0.12033(6) 0.42370(4) 0.01451(18) Uani 1 1 d . . . C8 C 0.8283(3) 0.2265(2) 0.42177(15) 0.0204(7) Uani 1 1 d . . . C9 C 0.7852(3) 0.2721(3) 0.36729(17) 0.0290(9) Uani 1 1 d . . . H9A H 0.7133 0.2797 0.3724 0.043 Uiso 1 1 calc R . . H9B H 0.7976 0.2416 0.3313 0.043 Uiso 1 1 calc R . . H9C H 0.8180 0.3237 0.3641 0.043 Uiso 1 1 calc R . . C10 C 0.8061(3) 0.2747(2) 0.47894(16) 0.0266(8) Uani 1 1 d . . . H10A H 0.8329 0.3283 0.4748 0.040 Uiso 1 1 calc R . . H10B H 0.8375 0.2488 0.5128 0.040 Uiso 1 1 calc R . . H10C H 0.7338 0.2775 0.4852 0.040 Uiso 1 1 calc R . . C11 C 0.9444(3) 0.2226(3) 0.41097(17) 0.0280(9) Uani 1 1 d . . . H11A H 0.9707 0.2762 0.4061 0.042 Uiso 1 1 calc R . . H11B H 0.9580 0.1918 0.3753 0.042 Uiso 1 1 calc R . . H11C H 0.9768 0.1974 0.4448 0.042 Uiso 1 1 calc R . . C12 C 0.8033(3) 0.0705(2) 0.49863(15) 0.0205(7) Uani 1 1 d . . . C13 C 0.7316(3) 0.0965(3) 0.54989(15) 0.0262(8) Uani 1 1 d . . . H13A H 0.6634 0.0794 0.5409 0.039 Uiso 1 1 calc R . . H13B H 0.7332 0.1541 0.5539 0.039 Uiso 1 1 calc R . . H13C H 0.7534 0.0722 0.5869 0.039 Uiso 1 1 calc R . . C14 C 0.9143(3) 0.0891(3) 0.51758(16) 0.0259(8) Uani 1 1 d . . . H14A H 0.9325 0.0561 0.5514 0.039 Uiso 1 1 calc R . . H14B H 0.9200 0.1449 0.5284 0.039 Uiso 1 1 calc R . . H14C H 0.9594 0.0778 0.4846 0.039 Uiso 1 1 calc R . . C15 C 0.7980(3) -0.0215(2) 0.49100(17) 0.0303(9) Uani 1 1 d . . . H15A H 0.8165 -0.0471 0.5282 0.045 Uiso 1 1 calc R . . H15B H 0.8442 -0.0380 0.4599 0.045 Uiso 1 1 calc R . . H15C H 0.7299 -0.0369 0.4802 0.045 Uiso 1 1 calc R . . C16 C 0.6340(2) 0.1191(3) 0.40797(16) 0.0239(8) Uani 1 1 d . . . C17 C 0.6161(3) 0.1334(3) 0.34002(16) 0.0332(10) Uani 1 1 d . . . H17A H 0.6535 0.0941 0.3172 0.050 Uiso 1 1 calc R . . H17B H 0.6387 0.1865 0.3294 0.050 Uiso 1 1 calc R . . H17C H 0.5448 0.1283 0.3312 0.050 Uiso 1 1 calc R . . C18 C 0.5747(3) 0.1834(3) 0.44378(16) 0.0316(10) Uani 1 1 d . . . H18A H 0.5031 0.1779 0.4358 0.047 Uiso 1 1 calc R . . H18B H 0.5969 0.2361 0.4318 0.047 Uiso 1 1 calc R . . H18C H 0.5870 0.1762 0.4860 0.047 Uiso 1 1 calc R . . C19 C 0.5906(3) 0.0358(3) 0.42165(18) 0.0333(10) Uani 1 1 d . . . H19A H 0.5970 0.0248 0.4639 0.050 Uiso 1 1 calc R . . H19B H 0.6274 -0.0042 0.3992 0.050 Uiso 1 1 calc R . . H19C H 0.5200 0.0342 0.4105 0.050 Uiso 1 1 calc R . . Sb1 Sb 0.772305(17) 0.169927(16) 0.164161(10) 0.01949(6) Uani 1 1 d . . . F1 F 0.86914(17) 0.16591(16) 0.22641(10) 0.0362(6) Uani 1 1 d . . . F2 F 0.70437(19) 0.08391(18) 0.20056(12) 0.0495(7) Uani 1 1 d . . . F3 F 0.6985(2) 0.2427(2) 0.20877(12) 0.0615(9) Uani 1 1 d . . . F4 F 0.67703(17) 0.17356(17) 0.10210(10) 0.0403(6) Uani 1 1 d . . . F5 F 0.8470(2) 0.25299(17) 0.12827(11) 0.0471(7) Uani 1 1 d . . . F6 F 0.84913(17) 0.09538(18) 0.12014(12) 0.0467(7) 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 Au1 0.01900(7) 0.01689(8) 0.01410(7) -0.00228(5) 0.00224(5) 0.00207(6) C1 0.0220(16) 0.024(2) 0.0157(16) -0.0039(15) 0.0021(13) 0.0076(16) C2 0.0237(16) 0.0171(19) 0.0173(16) -0.0018(14) 0.0063(13) 0.0016(16) C3 0.0204(16) 0.024(2) 0.0216(17) 0.0022(15) -0.0007(13) -0.0012(16) C4 0.0237(16) 0.021(2) 0.0252(18) 0.0027(16) 0.0036(14) 0.0059(16) C5 0.0251(17) 0.021(2) 0.0256(18) -0.0075(16) 0.0051(14) -0.0038(17) C6 0.035(2) 0.026(2) 0.0286(19) -0.0109(18) 0.0082(16) -0.0017(19) C7 0.0257(18) 0.028(2) 0.0265(19) 0.0001(17) 0.0088(15) 0.0054(17) P1 0.0149(4) 0.0164(5) 0.0122(4) -0.0016(3) -0.0007(3) 0.0019(4) C8 0.0267(17) 0.0166(19) 0.0180(16) 0.0000(15) -0.0026(14) 0.0003(15) C9 0.042(2) 0.022(2) 0.0230(18) 0.0048(16) -0.0004(16) 0.0058(19) C10 0.038(2) 0.017(2) 0.0251(18) -0.0063(16) -0.0036(16) 0.0016(18) C11 0.0304(19) 0.024(2) 0.0293(19) 0.0010(17) 0.0008(15) -0.0076(18) C12 0.0272(17) 0.020(2) 0.0145(16) 0.0037(14) -0.0026(13) 0.0013(16) C13 0.0328(18) 0.031(2) 0.0152(16) 0.0026(15) -0.0005(14) 0.0004(18) C14 0.0269(18) 0.031(2) 0.0199(17) 0.0039(16) -0.0063(14) 0.0052(17) C15 0.044(2) 0.021(2) 0.0258(19) 0.0060(17) 0.0055(17) 0.0019(19) C16 0.0158(15) 0.036(2) 0.0198(17) -0.0070(16) -0.0030(13) 0.0006(16) C17 0.0234(17) 0.053(3) 0.0229(19) -0.0070(19) -0.0070(14) 0.006(2) C18 0.0208(17) 0.052(3) 0.0222(18) -0.0062(19) -0.0005(14) 0.0148(19) C19 0.0237(18) 0.044(3) 0.032(2) -0.0088(19) -0.0017(16) -0.0083(19) Sb1 0.02257(11) 0.02051(14) 0.01538(11) -0.00217(9) 0.00106(8) -0.00085(10) F1 0.0438(13) 0.0383(16) 0.0266(12) 0.0053(11) -0.0130(10) -0.0064(12) F2 0.0475(15) 0.0505(19) 0.0506(16) 0.0124(14) 0.0027(12) -0.0253(14) F3 0.0655(18) 0.068(2) 0.0513(16) -0.0314(16) -0.0017(14) 0.0337(17) F4 0.0298(11) 0.0590(19) 0.0321(12) -0.0054(13) -0.0130(10) 0.0048(12) F5 0.0674(17) 0.0405(17) 0.0334(13) 0.0171(12) -0.0113(12) -0.0256(14) F6 0.0346(13) 0.0512(19) 0.0543(17) -0.0277(14) 0.0034(11) 0.0098(13) _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 C2 2.281(3) . ? Au1 C1 2.299(3) . ? Au1 P1 2.2981(8) . ? C1 C2 1.366(5) . ? C1 C5 1.508(5) . ? C1 H1 0.9300 . ? C2 C3 1.509(5) . ? C2 H2 0.9300 . ? C3 C4 1.526(5) . ? C3 C7 1.563(5) . ? C3 H3 0.9800 . ? C4 C5 1.534(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.572(5) . ? C5 H5 0.9800 . ? C6 C7 1.543(5) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? P1 C16 1.892(3) . ? P1 C8 1.894(4) . ? P1 C12 1.894(3) . ? C8 C10 1.529(5) . ? C8 C9 1.536(5) . ? C8 C11 1.545(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C15 1.537(5) . ? C12 C13 1.540(5) . ? C12 C14 1.548(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C19 1.527(6) . ? C16 C18 1.542(5) . ? C16 C17 1.546(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Sb1 F3 1.838(3) . ? Sb1 F4 1.863(2) . ? Sb1 F2 1.867(3) . ? Sb1 F5 1.870(2) . ? Sb1 F6 1.872(2) . ? Sb1 F1 1.880(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 C2 Au1 C1 34.70(12) . . ? C2 Au1 P1 158.66(10) . . ? C1 Au1 P1 165.85(9) . . ? C2 C1 C5 107.2(3) . . ? C2 C1 Au1 71.9(2) . . ? C5 C1 Au1 115.2(2) . . ? C2 C1 H1 126.4 . . ? C5 C1 H1 126.4 . . ? Au1 C1 H1 84.4 . . ? C1 C2 C3 107.1(3) . . ? C1 C2 Au1 73.37(19) . . ? C3 C2 Au1 114.3(2) . . ? C1 C2 H2 126.5 . . ? C3 C2 H2 126.5 . . ? Au1 C2 H2 83.9 . . ? C2 C3 C4 102.2(3) . . ? C2 C3 C7 102.7(3) . . ? C4 C3 C7 100.2(3) . . ? C2 C3 H3 116.4 . . ? C4 C3 H3 116.4 . . ? C7 C3 H3 116.4 . . ? C3 C4 C5 94.9(3) . . ? C3 C4 H4A 112.8 . . ? C5 C4 H4A 112.8 . . ? C3 C4 H4B 112.8 . . ? C5 C4 H4B 112.8 . . ? H4A C4 H4B 110.2 . . ? C1 C5 C4 101.8(3) . . ? C1 C5 C6 102.8(3) . . ? C4 C5 C6 99.7(3) . . ? C1 C5 H5 116.7 . . ? C4 C5 H5 116.7 . . ? C6 C5 H5 116.7 . . ? C7 C6 C5 103.1(3) . . ? C7 C6 H6A 111.1 . . ? C5 C6 H6A 111.1 . . ? C7 C6 H6B 111.1 . . ? C5 C6 H6B 111.1 . . ? H6A C6 H6B 109.1 . . ? C6 C7 C3 103.1(3) . . ? C6 C7 H7A 111.1 . . ? C3 C7 H7A 111.1 . . ? C6 C7 H7B 111.1 . . ? C3 C7 H7B 111.1 . . ? H7A C7 H7B 109.1 . . ? C16 P1 C8 111.42(18) . . ? C16 P1 C12 110.31(16) . . ? C8 P1 C12 110.81(16) . . ? C16 P1 Au1 108.40(12) . . ? C8 P1 Au1 106.43(11) . . ? C12 P1 Au1 109.34(12) . . ? C10 C8 C9 109.0(3) . . ? C10 C8 C11 109.8(3) . . ? C9 C8 C11 105.2(3) . . ? C10 C8 P1 113.4(3) . . ? C9 C8 P1 110.0(3) . . ? C11 C8 P1 109.0(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 109.4(3) . . ? C15 C12 C14 105.7(3) . . ? C13 C12 C14 108.6(3) . . ? C15 C12 P1 109.1(2) . . ? C13 C12 P1 114.2(2) . . ? C14 C12 P1 109.5(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C18 109.6(3) . . ? C19 C16 C17 106.0(3) . . ? C18 C16 C17 108.8(3) . . ? C19 C16 P1 109.9(3) . . ? C18 C16 P1 113.2(3) . . ? C17 C16 P1 109.2(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F3 Sb1 F4 91.36(12) . . ? F3 Sb1 F2 90.94(15) . . ? F4 Sb1 F2 91.40(12) . . ? F3 Sb1 F5 91.30(15) . . ? F4 Sb1 F5 90.75(11) . . ? F2 Sb1 F5 176.87(13) . . ? F3 Sb1 F6 178.80(13) . . ? F4 Sb1 F6 89.81(11) . . ? F2 Sb1 F6 88.80(13) . . ? F5 Sb1 F6 88.92(13) . . ? F3 Sb1 F1 89.04(12) . . ? F4 Sb1 F1 179.58(11) . . ? F2 Sb1 F1 88.71(11) . . ? F5 Sb1 F1 89.13(11) . . ? F6 Sb1 F1 89.79(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 C1 C2 164.6(3) . . . . ? C2 Au1 C1 C5 100.9(3) . . . . ? P1 Au1 C1 C5 -94.4(4) . . . . ? C5 C1 C2 C3 -0.6(4) . . . . ? Au1 C1 C2 C3 111.0(2) . . . . ? C5 C1 C2 Au1 -111.6(2) . . . . ? P1 Au1 C2 C1 -169.8(2) . . . . ? C1 Au1 C2 C3 -101.6(4) . . . . ? P1 Au1 C2 C3 88.7(4) . . . . ? C1 C2 C3 C4 -31.0(3) . . . . ? Au1 C2 C3 C4 48.0(3) . . . . ? C1 C2 C3 C7 72.5(3) . . . . ? Au1 C2 C3 C7 151.5(2) . . . . ? C2 C3 C4 C5 47.4(3) . . . . ? C7 C3 C4 C5 -58.1(3) . . . . ? C2 C1 C5 C4 31.9(3) . . . . ? Au1 C1 C5 C4 -45.8(3) . . . . ? C2 C1 C5 C6 -71.1(3) . . . . ? Au1 C1 C5 C6 -148.8(2) . . . . ? C3 C4 C5 C1 -47.7(3) . . . . ? C3 C4 C5 C6 57.7(3) . . . . ? C1 C5 C6 C7 68.8(4) . . . . ? C4 C5 C6 C7 -35.7(4) . . . . ? C5 C6 C7 C3 -0.2(4) . . . . ? C2 C3 C7 C6 -68.7(4) . . . . ? C4 C3 C7 C6 36.4(4) . . . . ? C2 Au1 P1 C16 156.3(3) . . . . ? C1 Au1 P1 C16 0.7(4) . . . . ? C2 Au1 P1 C8 36.3(3) . . . . ? C1 Au1 P1 C8 -119.2(4) . . . . ? C2 Au1 P1 C12 -83.4(3) . . . . ? C1 Au1 P1 C12 121.0(4) . . . . ? C16 P1 C8 C10 78.2(3) . . . . ? C12 P1 C8 C10 -45.0(3) . . . . ? Au1 P1 C8 C10 -163.8(2) . . . . ? C16 P1 C8 C9 -44.2(3) . . . . ? C12 P1 C8 C9 -167.4(2) . . . . ? Au1 P1 C8 C9 73.8(2) . . . . ? C16 P1 C8 C11 -159.0(2) . . . . ? C12 P1 C8 C11 77.7(3) . . . . ? Au1 P1 C8 C11 -41.0(2) . . . . ? C16 P1 C12 C15 77.7(3) . . . . ? C8 P1 C12 C15 -158.5(2) . . . . ? Au1 P1 C12 C15 -41.4(3) . . . . ? C16 P1 C12 C13 -45.1(3) . . . . ? C8 P1 C12 C13 78.8(3) . . . . ? Au1 P1 C12 C13 -164.2(2) . . . . ? C16 P1 C12 C14 -167.1(3) . . . . ? C8 P1 C12 C14 -43.2(3) . . . . ? Au1 P1 C12 C14 73.8(3) . . . . ? C8 P1 C16 C19 -169.2(2) . . . . ? C12 P1 C16 C19 -45.7(3) . . . . ? Au1 P1 C16 C19 74.0(3) . . . . ? C8 P1 C16 C18 -46.3(3) . . . . ? C12 P1 C16 C18 77.2(3) . . . . ? Au1 P1 C16 C18 -163.1(3) . . . . ? C8 P1 C16 C17 75.0(3) . . . . ? C12 P1 C16 C17 -161.5(3) . . . . ? Au1 P1 C16 C17 -41.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.228 _refine_diff_density_min -1.345 _refine_diff_density_rms 0.123 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 729112' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C20 H41 Au P, F6 Sb' _chemical_formula_sum 'C20 H41 Au F6 P Sb' _chemical_formula_weight 745.21 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 16.1038(5) _cell_length_b 17.5224(6) _cell_length_c 9.1760(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2589.26(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7528 _cell_measurement_theta_min 2.505 _cell_measurement_theta_max 29.626 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 6.812 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.219 _exptl_absorpt_correction_T_max 0.360 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 19702 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 29.67 _reflns_number_total 5963 _reflns_number_gt 5400 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The occupancy of the disordered carbon atoms in the trans-cyclooctene ring were allowed to freely refine and found to be approximately 60:40. Similarly the 4 disordered fluorine atoms in the SbF6 anion were found to be approximately 57:43. The disordered atom pairs, C3A and C3B, C4A and C4B, C7A and C7B and C8A and C8B were described using the EXYZ and EADP commands. The atoms C1A and C2A and C1B and C2B were described using the DELU command. The fluorine atom F3B was described using the EADP command using F5B. 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^)+(0.0114P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.089(5) _refine_ls_number_reflns 5963 _refine_ls_number_parameters 340 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0423 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.993 _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 0.924445(7) 0.180126(6) 0.68778(3) 0.01998(4) Uani 1 1 d . . . P1 P 0.96274(5) 0.30654(4) 0.68640(15) 0.01653(15) Uani 1 1 d . A . C1A C 0.9107(5) 0.0590(4) 0.7553(10) 0.0202(17) Uani 0.603(11) 1 d PDU A 1 H1A H 0.8703 0.0538 0.8375 0.024 Uiso 0.603(11) 1 calc PRD A 1 C2A C 0.8711(5) 0.0669(4) 0.6262(11) 0.0199(17) Uani 0.603(11) 1 d PU A 1 H2A H 0.9038 0.0430 0.5456 0.024 Uiso 0.603(11) 1 calc PR A 1 C3A C 0.7840(3) 0.0574(3) 0.6027(7) 0.0518(15) Uani 0.603(11) 1 d P A 1 H3A1 H 0.7683 0.0806 0.5083 0.062 Uiso 0.603(11) 1 calc PR A 1 H3A2 H 0.7527 0.0837 0.6808 0.062 Uiso 0.603(11) 1 calc PR A 1 C4A C 0.7617(3) -0.0276(3) 0.6021(6) 0.0444(13) Uani 0.603(11) 1 d P A 1 H4A1 H 0.7011 -0.0322 0.6179 0.053 Uiso 0.603(11) 1 calc PR A 1 H4A2 H 0.7737 -0.0481 0.5038 0.053 Uiso 0.603(11) 1 calc PR A 1 C5A C 0.8049(7) -0.0775(5) 0.7124(10) 0.041(3) Uani 0.603(11) 1 d P A 1 H5A1 H 0.7730 -0.1257 0.7187 0.049 Uiso 0.603(11) 1 calc PR A 1 H5A2 H 0.7997 -0.0520 0.8082 0.049 Uiso 0.603(11) 1 calc PR A 1 C6A C 0.8969(5) -0.0993(3) 0.6935(11) 0.035(2) Uani 0.603(11) 1 d P A 1 H6A1 H 0.9005 -0.1557 0.6944 0.042 Uiso 0.603(11) 1 calc PR A 1 H6A2 H 0.9146 -0.0822 0.5956 0.042 Uiso 0.603(11) 1 calc PR A 1 C7A C 0.9591(3) -0.0694(3) 0.8022(6) 0.0424(12) Uani 0.603(11) 1 d P A 1 H7A1 H 1.0091 -0.1022 0.7980 0.051 Uiso 0.603(11) 1 calc PR A 1 H7A2 H 0.9351 -0.0748 0.9010 0.051 Uiso 0.603(11) 1 calc PR A 1 C8A C 0.9866(3) 0.0137(3) 0.7825(7) 0.0511(15) Uani 0.603(11) 1 d P A 1 H8A1 H 1.0152 0.0322 0.8713 0.061 Uiso 0.603(11) 1 calc PR A 1 H8A2 H 1.0253 0.0181 0.6991 0.061 Uiso 0.603(11) 1 calc PR A 1 C1B C 0.9328(7) 0.0499(5) 0.687(2) 0.025(2) Uani 0.397(11) 1 d PU A 2 H1B H 0.9454 0.0324 0.5861 0.030 Uiso 0.397(11) 1 calc PR A 2 C2B C 0.8499(8) 0.0696(5) 0.6948(16) 0.020(2) Uani 0.397(11) 1 d PDU A 2 H2B H 0.8304 0.0614 0.7971 0.024 Uiso 0.397(11) 1 calc PRD A 2 C3B C 0.7840(3) 0.0574(3) 0.6027(7) 0.0518(15) Uani 0.397(11) 1 d P A 2 H3B1 H 0.7988 0.0739 0.5029 0.062 Uiso 0.397(11) 1 calc PR A 2 H3B2 H 0.7356 0.0877 0.6354 0.062 Uiso 0.397(11) 1 calc PR A 2 C4B C 0.7617(3) -0.0276(3) 0.6021(6) 0.0444(13) Uani 0.397(11) 1 d P A 2 H4B1 H 0.7165 -0.0347 0.6740 0.053 Uiso 0.397(11) 1 calc PR A 2 H4B2 H 0.7377 -0.0390 0.5052 0.053 Uiso 0.397(11) 1 calc PR A 2 C5B C 0.8266(10) -0.0890(7) 0.633(2) 0.041(4) Uani 0.397(11) 1 d P A 2 H5B1 H 0.8725 -0.0827 0.5623 0.050 Uiso 0.397(11) 1 calc PR A 2 H5B2 H 0.8010 -0.1394 0.6147 0.050 Uiso 0.397(11) 1 calc PR A 2 C6B C 0.8658(9) -0.0895(7) 0.7954(15) 0.038(4) Uani 0.397(11) 1 d P A 2 H6B1 H 0.8347 -0.0527 0.8564 0.045 Uiso 0.397(11) 1 calc PR A 2 H6B2 H 0.8577 -0.1409 0.8382 0.045 Uiso 0.397(11) 1 calc PR A 2 C7B C 0.9591(3) -0.0694(3) 0.8022(6) 0.0424(12) Uani 0.397(11) 1 d P A 2 H7B1 H 0.9803 -0.0869 0.8979 0.051 Uiso 0.397(11) 1 calc PR A 2 H7B2 H 0.9877 -0.1001 0.7268 0.051 Uiso 0.397(11) 1 calc PR A 2 C8B C 0.9866(3) 0.0137(3) 0.7825(7) 0.0511(15) Uani 0.397(11) 1 d P A 2 H8B1 H 0.9863 0.0402 0.8778 0.061 Uiso 0.397(11) 1 calc PR A 2 H8B2 H 1.0438 0.0154 0.7431 0.061 Uiso 0.397(11) 1 calc PR A 2 C9 C 1.0365(3) 0.3202(2) 0.5267(5) 0.0238(11) Uani 1 1 d . . . C10 C 1.0528(3) 0.4039(3) 0.4879(5) 0.0332(11) Uani 1 1 d . A . H10A H 1.0017 0.4270 0.4504 0.050 Uiso 1 1 calc R . . H10B H 1.0962 0.4068 0.4133 0.050 Uiso 1 1 calc R . . H10C H 1.0709 0.4315 0.5752 0.050 Uiso 1 1 calc R . . C11 C 1.1198(3) 0.2805(2) 0.5624(5) 0.0299(9) Uani 1 1 d . A . H11A H 1.1446 0.3043 0.6487 0.045 Uiso 1 1 calc R . . H11B H 1.1577 0.2858 0.4795 0.045 Uiso 1 1 calc R . . H11C H 1.1098 0.2263 0.5817 0.045 Uiso 1 1 calc R . . C12 C 1.0014(3) 0.2781(2) 0.3927(4) 0.0333(10) Uani 1 1 d . A . H12A H 1.0419 0.2800 0.3132 0.050 Uiso 1 1 calc R . . H12B H 0.9498 0.3028 0.3615 0.050 Uiso 1 1 calc R . . H12C H 0.9900 0.2248 0.4183 0.050 Uiso 1 1 calc R . . C13 C 1.0165(3) 0.3291(3) 0.8634(5) 0.0244(10) Uani 1 1 d . . . C14 C 0.9536(3) 0.3395(3) 0.9888(5) 0.0362(11) Uani 1 1 d . A . H14A H 0.9835 0.3463 1.0808 0.054 Uiso 1 1 calc R . . H14B H 0.9180 0.2943 0.9954 0.054 Uiso 1 1 calc R . . H14C H 0.9192 0.3846 0.9698 0.054 Uiso 1 1 calc R . . C15 C 1.0705(3) 0.4014(3) 0.8583(6) 0.0349(12) Uani 1 1 d . A . H15A H 1.1160 0.3939 0.7887 0.052 Uiso 1 1 calc R . . H15B H 1.0935 0.4113 0.9553 0.052 Uiso 1 1 calc R . . H15C H 1.0365 0.4449 0.8276 0.052 Uiso 1 1 calc R . . C16 C 1.0709(3) 0.2599(3) 0.9095(5) 0.0320(10) Uani 1 1 d . A . H16A H 1.1002 0.2721 1.0002 0.048 Uiso 1 1 calc R . . H16B H 1.1115 0.2489 0.8327 0.048 Uiso 1 1 calc R . . H16C H 1.0354 0.2152 0.9247 0.048 Uiso 1 1 calc R . . C17 C 0.8665(2) 0.36685(19) 0.6642(4) 0.0242(8) Uani 1 1 d . . . C18 C 0.8787(2) 0.45109(19) 0.7013(6) 0.0301(9) Uani 1 1 d . A . H18A H 0.8924 0.4562 0.8049 0.045 Uiso 1 1 calc R . . H18B H 0.8275 0.4792 0.6804 0.045 Uiso 1 1 calc R . . H18C H 0.9241 0.4719 0.6424 0.045 Uiso 1 1 calc R . . C19 C 0.7978(3) 0.3334(3) 0.7607(6) 0.0358(11) Uani 1 1 d . A . H19A H 0.7475 0.3645 0.7515 0.054 Uiso 1 1 calc R . . H19B H 0.8162 0.3332 0.8625 0.054 Uiso 1 1 calc R . . H19C H 0.7858 0.2810 0.7298 0.054 Uiso 1 1 calc R . . C20 C 0.8346(3) 0.3617(3) 0.5074(5) 0.0412(12) Uani 1 1 d . A . H20A H 0.8724 0.3895 0.4426 0.062 Uiso 1 1 calc R . . H20B H 0.7790 0.3843 0.5017 0.062 Uiso 1 1 calc R . . H20C H 0.8321 0.3081 0.4776 0.062 Uiso 1 1 calc R . . Sb1 Sb 0.703559(17) 0.646006(16) 0.64376(3) 0.02826(6) Uani 1 1 d . . . F1 F 0.59528(17) 0.6524(2) 0.5691(3) 0.0510(8) Uani 1 1 d . B . F2 F 0.81202(15) 0.63843(15) 0.7161(3) 0.0434(7) Uani 1 1 d . B . F3A F 0.6650(5) 0.6846(6) 0.8185(9) 0.063(3) Uani 0.570(17) 1 d P B 3 F4A F 0.7277(6) 0.7420(7) 0.5866(18) 0.112(6) Uani 0.570(17) 1 d P B 3 F5A F 0.7453(4) 0.6015(14) 0.4783(13) 0.169(9) Uani 0.570(17) 1 d P B 3 F6A F 0.6826(6) 0.5467(5) 0.722(2) 0.101(5) Uani 0.570(17) 1 d P B 3 F3B F 0.6609(6) 0.6365(12) 0.8291(9) 0.072(4) Uani 0.430(17) 1 d P B 4 F4B F 0.7007(8) 0.7513(7) 0.679(2) 0.095(6) Uani 0.430(17) 1 d P B 4 F5B F 0.7357(7) 0.6631(8) 0.4523(10) 0.072(4) Uani 0.430(17) 1 d P B 4 F6B F 0.6933(8) 0.5480(6) 0.611(2) 0.077(5) Uani 0.430(17) 1 d P B 4 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 0.02094(6) 0.01226(5) 0.02673(6) 0.00100(8) 0.00077(8) 0.00039(5) P1 0.0202(4) 0.0122(3) 0.0172(3) 0.0008(5) 0.0000(6) 0.0013(3) C1A 0.024(5) 0.005(3) 0.031(4) 0.000(3) 0.006(3) -0.006(3) C2A 0.012(4) 0.012(3) 0.036(5) -0.007(3) 0.002(3) -0.003(3) C3A 0.041(3) 0.037(3) 0.078(4) 0.008(3) -0.022(3) -0.006(2) C4A 0.032(3) 0.037(3) 0.064(3) -0.008(2) -0.013(2) -0.009(2) C5A 0.067(7) 0.025(4) 0.030(5) -0.004(3) 0.009(4) -0.027(4) C6A 0.059(5) 0.015(3) 0.030(4) 0.005(4) 0.001(5) -0.004(3) C7A 0.052(3) 0.020(2) 0.055(3) 0.005(2) -0.009(3) 0.009(2) C8A 0.044(3) 0.015(2) 0.094(4) 0.010(2) -0.026(3) 0.001(2) C1B 0.027(5) 0.008(4) 0.039(6) 0.005(7) 0.017(7) -0.005(3) C2B 0.027(6) 0.013(4) 0.020(6) 0.007(5) 0.007(6) -0.003(4) C3B 0.041(3) 0.037(3) 0.078(4) 0.008(3) -0.022(3) -0.006(2) C4B 0.032(3) 0.037(3) 0.064(3) -0.008(2) -0.013(2) -0.009(2) C5B 0.061(10) 0.014(6) 0.049(10) -0.009(6) -0.013(8) -0.005(6) C6B 0.049(9) 0.026(6) 0.039(8) 0.012(5) -0.005(6) 0.001(6) C7B 0.052(3) 0.020(2) 0.055(3) 0.005(2) -0.009(3) 0.009(2) C8B 0.044(3) 0.015(2) 0.094(4) 0.010(2) -0.026(3) 0.001(2) C9 0.034(3) 0.013(2) 0.024(2) 0.0031(15) 0.0105(19) 0.0033(18) C10 0.049(3) 0.016(2) 0.035(2) 0.0078(17) 0.015(2) 0.001(2) C11 0.035(3) 0.019(2) 0.035(2) 0.0069(17) 0.0161(19) 0.0026(18) C12 0.052(3) 0.027(2) 0.0209(18) -0.0020(16) 0.0044(19) 0.008(2) C13 0.025(3) 0.031(3) 0.0179(19) -0.0014(16) -0.0043(17) -0.0005(19) C14 0.040(3) 0.046(3) 0.022(2) -0.0010(18) 0.0001(19) 0.004(2) C15 0.029(3) 0.031(3) 0.045(3) -0.014(2) -0.006(2) -0.003(2) C16 0.032(3) 0.038(3) 0.026(2) 0.0037(18) -0.0110(18) 0.005(2) C17 0.0218(17) 0.0191(16) 0.032(2) -0.0008(16) -0.0033(17) 0.0101(13) C18 0.028(2) 0.0217(17) 0.041(3) -0.002(2) 0.008(2) 0.0080(14) C19 0.021(2) 0.032(2) 0.054(3) -0.004(2) 0.003(2) 0.0040(18) C20 0.044(3) 0.042(3) 0.037(2) -0.002(2) -0.018(2) 0.022(2) Sb1 0.02306(13) 0.03831(15) 0.02342(11) -0.00472(11) -0.00363(11) 0.00133(11) F1 0.0252(15) 0.077(2) 0.0506(18) 0.0077(16) -0.0139(13) -0.0017(15) F2 0.0262(13) 0.0465(15) 0.0576(19) -0.0049(14) -0.0173(13) 0.0033(11) F3A 0.074(5) 0.064(6) 0.053(4) -0.017(4) 0.012(3) 0.031(4) F4A 0.040(5) 0.091(8) 0.205(15) 0.109(9) -0.040(6) -0.021(5) F5A 0.021(4) 0.41(2) 0.071(7) -0.151(11) -0.017(4) 0.031(8) F6A 0.041(4) 0.037(4) 0.226(16) 0.042(8) -0.049(8) -0.006(3) F3B 0.035(4) 0.153(11) 0.027(3) 0.031(4) 0.004(2) 0.006(4) F4B 0.068(8) 0.053(6) 0.163(14) -0.079(9) -0.051(9) 0.016(5) F5B 0.035(4) 0.153(11) 0.027(3) 0.031(4) 0.004(2) 0.006(4) F6B 0.061(8) 0.020(5) 0.151(13) 0.012(7) -0.070(9) 0.009(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 C1A 2.223(6) . ? Au1 C2A 2.235(6) . ? Au1 C2B 2.279(10) . ? Au1 C1B 2.286(9) . ? Au1 P1 2.2994(7) . ? P1 C13 1.882(5) . ? P1 C17 1.887(3) . ? P1 C9 1.901(5) . ? C1A C2A 1.353(12) . ? C1A C8A 1.478(9) . ? C1A H1A 1.0000 . ? C2A C3A 1.428(9) . ? C2A H2A 1.0000 . ? C3A C4A 1.532(7) . ? C3A H3A1 0.9900 . ? C3A H3A2 0.9900 . ? C4A C5A 1.508(10) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.539(14) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A C7A 1.508(10) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.533(6) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C1B C2B 1.380(18) . ? C1B H1B 1.0000 . ? C2B H2B 1.0000 . ? C5B C6B 1.62(2) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9900 . ? C6B H6B2 0.9900 . ? C9 C10 1.532(6) . ? C9 C12 1.541(6) . ? C9 C11 1.546(7) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.537(7) . ? C13 C14 1.545(6) . ? C13 C16 1.554(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.528(5) . ? C17 C20 1.530(6) . ? C17 C19 1.534(6) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Sb1 F6B 1.751(11) . ? Sb1 F4A 1.805(8) . ? Sb1 F5A 1.835(7) . ? Sb1 F3B 1.842(8) . ? Sb1 F3A 1.848(6) . ? Sb1 F5B 1.856(9) . ? Sb1 F2 1.873(2) . ? Sb1 F4B 1.874(10) . ? Sb1 F1 1.877(3) . ? Sb1 F6A 1.913(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 C1A Au1 C2A 35.3(3) . . ? C1A Au1 C2B 29.3(3) . . ? C2A Au1 C2B 18.2(3) . . ? C1A Au1 C1B 18.7(4) . . ? C2A Au1 C1B 30.2(4) . . ? C2B Au1 C1B 35.2(4) . . ? C1A Au1 P1 161.5(2) . . ? C2A Au1 P1 163.1(2) . . ? C2B Au1 P1 163.7(3) . . ? C1B Au1 P1 161.1(3) . . ? C13 P1 C17 110.7(2) . . ? C13 P1 C9 110.6(2) . . ? C17 P1 C9 111.1(2) . . ? C13 P1 Au1 108.70(15) . . ? C17 P1 Au1 108.66(11) . . ? C9 P1 Au1 107.04(13) . . ? C2A C1A C8A 126.4(9) . . ? C2A C1A Au1 72.8(4) . . ? C8A C1A Au1 118.5(5) . . ? C2A C1A H1A 111.2 . . ? C8A C1A H1A 111.2 . . ? Au1 C1A H1A 111.2 . . ? C1A C2A C3A 125.7(9) . . ? C1A C2A Au1 71.8(4) . . ? C3A C2A Au1 121.3(5) . . ? C1A C2A H2A 110.9 . . ? C3A C2A H2A 110.9 . . ? Au1 C2A H2A 110.9 . . ? C2A C3A C4A 110.2(5) . . ? C2A C3A H3A1 109.6 . . ? C4A C3A H3A1 109.6 . . ? C2A C3A H3A2 109.6 . . ? C4A C3A H3A2 109.6 . . ? H3A1 C3A H3A2 108.1 . . ? C5A C4A C3A 116.9(5) . . ? C5A C4A H4A1 108.1 . . ? C3A C4A H4A1 108.1 . . ? C5A C4A H4A2 108.1 . . ? C3A C4A H4A2 108.1 . . ? H4A1 C4A H4A2 107.3 . . ? C4A C5A C6A 120.9(7) . . ? C4A C5A H5A1 107.1 . . ? C6A C5A H5A1 107.1 . . ? C4A C5A H5A2 107.1 . . ? C6A C5A H5A2 107.1 . . ? H5A1 C5A H5A2 106.8 . . ? C7A C6A C5A 118.6(7) . . ? C7A C6A H6A1 107.7 . . ? C5A C6A H6A1 107.7 . . ? C7A C6A H6A2 107.7 . . ? C5A C6A H6A2 107.7 . . ? H6A1 C6A H6A2 107.1 . . ? C6A C7A C8A 116.4(4) . . ? C6A C7A H7A1 108.2 . . ? C8A C7A H7A1 108.2 . . ? C6A C7A H7A2 108.2 . . ? C8A C7A H7A2 108.2 . . ? H7A1 C7A H7A2 107.3 . . ? C1A C8A C7A 106.9(4) . . ? C1A C8A H8A1 110.3 . . ? C7A C8A H8A1 110.3 . . ? C1A C8A H8A2 110.3 . . ? C7A C8A H8A2 110.3 . . ? H8A1 C8A H8A2 108.6 . . ? C2B C1B Au1 72.1(6) . . ? C2B C1B H1B 108.6 . . ? Au1 C1B H1B 108.6 . . ? C1B C2B Au1 72.7(6) . . ? C1B C2B H2B 108.3 . . ? Au1 C2B H2B 108.3 . . ? C6B C5B H5B1 108.2 . . ? C6B C5B H5B2 108.2 . . ? H5B1 C5B H5B2 107.4 . . ? C5B C6B H6B1 108.6 . . ? C5B C6B H6B2 108.6 . . ? H6B1 C6B H6B2 107.6 . . ? C10 C9 C12 109.6(4) . . ? C10 C9 C11 109.3(4) . . ? C12 C9 C11 105.8(3) . . ? C10 C9 P1 114.0(3) . . ? C12 C9 P1 109.0(3) . . ? C11 C9 P1 108.8(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 107.2(4) . . ? C15 C13 C16 109.3(4) . . ? C14 C13 C16 105.1(4) . . ? C15 C13 P1 114.0(3) . . ? C14 C13 P1 111.5(3) . . ? C16 C13 P1 109.3(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C20 108.0(4) . . ? C18 C17 C19 109.5(3) . . ? C20 C17 C19 106.2(4) . . ? C18 C17 P1 114.3(3) . . ? C20 C17 P1 110.1(3) . . ? C19 C17 P1 108.4(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F6B Sb1 F4A 152.2(7) . . ? F6B Sb1 F5A 58.4(7) . . ? F4A Sb1 F5A 94.4(7) . . ? F6B Sb1 F3B 92.0(7) . . ? F4A Sb1 F3B 115.6(6) . . ? F5A Sb1 F3B 149.6(7) . . ? F6B Sb1 F3A 118.5(6) . . ? F4A Sb1 F3A 89.0(5) . . ? F5A Sb1 F3A 175.6(6) . . ? F3B Sb1 F3A 26.7(4) . . ? F6B Sb1 F5B 91.2(7) . . ? F4A Sb1 F5B 61.0(6) . . ? F5A Sb1 F5B 35.2(6) . . ? F3B Sb1 F5B 173.1(4) . . ? F3A Sb1 F5B 148.9(5) . . ? F6B Sb1 F2 94.5(4) . . ? F4A Sb1 F2 88.2(3) . . ? F5A Sb1 F2 85.5(3) . . ? F3B Sb1 F2 90.8(3) . . ? F3A Sb1 F2 91.8(3) . . ? F5B Sb1 F2 95.0(3) . . ? F6B Sb1 F4B 173.2(6) . . ? F4A Sb1 F4B 30.4(5) . . ? F5A Sb1 F4B 124.8(8) . . ? F3B Sb1 F4B 85.4(7) . . ? F3A Sb1 F4B 58.7(6) . . ? F5B Sb1 F4B 90.7(7) . . ? F2 Sb1 F4B 91.8(3) . . ? F6B Sb1 F1 84.7(4) . . ? F4A Sb1 F1 92.2(3) . . ? F5A Sb1 F1 93.7(3) . . ? F3B Sb1 F1 89.8(3) . . ? F3A Sb1 F1 89.0(3) . . ? F5B Sb1 F1 84.5(3) . . ? F2 Sb1 F1 179.10(14) . . ? F4B Sb1 F1 88.9(4) . . ? F6B Sb1 F6A 32.3(5) . . ? F4A Sb1 F6A 174.5(5) . . ? F5A Sb1 F6A 89.3(7) . . ? F3B Sb1 F6A 60.4(6) . . ? F3A Sb1 F6A 87.1(5) . . ? F5B Sb1 F6A 123.4(6) . . ? F2 Sb1 F6A 88.1(3) . . ? F4B Sb1 F6A 145.8(7) . . ? F1 Sb1 F6A 91.6(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1A Au1 P1 C13 -6.3(8) . . . . ? C2A Au1 P1 C13 176.9(8) . . . . ? C2B Au1 P1 C13 109.4(13) . . . . ? C1B Au1 P1 C13 -67.1(16) . . . . ? C1A Au1 P1 C17 -126.8(8) . . . . ? C2A Au1 P1 C17 56.4(8) . . . . ? C2B Au1 P1 C17 -11.1(14) . . . . ? C1B Au1 P1 C17 172.4(16) . . . . ? C1A Au1 P1 C9 113.2(8) . . . . ? C2A Au1 P1 C9 -63.6(8) . . . . ? C2B Au1 P1 C9 -131.1(13) . . . . ? C1B Au1 P1 C9 52.4(16) . . . . ? C2B Au1 C1A C2A 32.6(7) . . . . ? C1B Au1 C1A C2A -60.5(14) . . . . ? P1 Au1 C1A C2A -178.4(5) . . . . ? C2A Au1 C1A C8A 122.6(10) . . . . ? C2B Au1 C1A C8A 155.2(14) . . . . ? C1B Au1 C1A C8A 62.1(14) . . . . ? P1 Au1 C1A C8A -55.8(12) . . . . ? C8A C1A C2A C3A 130.9(8) . . . . ? Au1 C1A C2A C3A -115.9(7) . . . . ? C8A C1A C2A Au1 -113.1(7) . . . . ? C2B Au1 C2A C1A -57.6(14) . . . . ? C1B Au1 C2A C1A 33.6(8) . . . . ? P1 Au1 C2A C1A 178.2(6) . . . . ? C1A Au1 C2A C3A 121.3(11) . . . . ? C2B Au1 C2A C3A 63.7(12) . . . . ? C1B Au1 C2A C3A 154.9(16) . . . . ? P1 Au1 C2A C3A -60.4(13) . . . . ? C1A C2A C3A C4A -75.8(9) . . . . ? Au1 C2A C3A C4A -165.1(5) . . . . ? C2A C3A C4A C5A 39.8(10) . . . . ? C3A C4A C5A C6A -73.6(9) . . . . ? C4A C5A C6A C7A 113.7(8) . . . . ? C5A C6A C7A C8A -78.4(8) . . . . ? C2A C1A C8A C7A -81.9(9) . . . . ? Au1 C1A C8A C7A -171.0(4) . . . . ? C6A C7A C8A C1A 45.2(8) . . . . ? C1A Au1 C1B C2B 58.1(12) . . . . ? C2A Au1 C1B C2B -32.9(6) . . . . ? P1 Au1 C1B C2B 178.3(9) . . . . ? C1A Au1 C2B C1B -33.7(9) . . . . ? C2A Au1 C2B C1B 60.8(15) . . . . ? P1 Au1 C2B C1B -178.0(11) . . . . ? C13 P1 C9 C10 -75.0(4) . . . . ? C17 P1 C9 C10 48.3(4) . . . . ? Au1 P1 C9 C10 166.8(3) . . . . ? C13 P1 C9 C12 162.2(3) . . . . ? C17 P1 C9 C12 -74.5(3) . . . . ? Au1 P1 C9 C12 44.0(3) . . . . ? C13 P1 C9 C11 47.3(3) . . . . ? C17 P1 C9 C11 170.6(3) . . . . ? Au1 P1 C9 C11 -70.9(3) . . . . ? C17 P1 C13 C15 -80.3(4) . . . . ? C9 P1 C13 C15 43.2(4) . . . . ? Au1 P1 C13 C15 160.4(3) . . . . ? C17 P1 C13 C14 41.2(4) . . . . ? C9 P1 C13 C14 164.8(3) . . . . ? Au1 P1 C13 C14 -78.0(3) . . . . ? C17 P1 C13 C16 157.0(3) . . . . ? C9 P1 C13 C16 -79.5(3) . . . . ? Au1 P1 C13 C16 37.7(3) . . . . ? C13 P1 C17 C18 45.3(4) . . . . ? C9 P1 C17 C18 -77.9(4) . . . . ? Au1 P1 C17 C18 164.6(3) . . . . ? C13 P1 C17 C20 167.1(3) . . . . ? C9 P1 C17 C20 43.9(4) . . . . ? Au1 P1 C17 C20 -73.6(3) . . . . ? C13 P1 C17 C19 -77.1(3) . . . . ? C9 P1 C17 C19 159.7(3) . . . . ? Au1 P1 C17 C19 42.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.67 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.071 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.106 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 729113' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C19 H35 Au P, F6 Sb, C H2 Cl2' _chemical_formula_sum 'C20 H37 Au Cl2 F6 P Sb' _chemical_formula_weight 812.08 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 11.7603(7) _cell_length_b 13.7090(8) _cell_length_c 16.9906(10) _cell_angle_alpha 90.00 _cell_angle_beta 100.338(3) _cell_angle_gamma 90.00 _cell_volume 2694.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9502 _cell_measurement_theta_min 2.750 _cell_measurement_theta_max 29.531 _exptl_crystal_description shard _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.002 _exptl_crystal_density_method none _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 6.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_T_max 0.509 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 37200 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 29.58 _reflns_number_total 7510 _reflns_number_gt 6529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+2.3421P] 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 7510 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.1237 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.416 _refine_ls_restrained_S_all 1.416 _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 0.225320(16) 0.348294(14) 0.115625(12) 0.01517(8) Uani 1 1 d . . . C1 C 0.1412(4) 0.4068(4) 0.2165(3) 0.0171(10) Uani 1 1 d . . . H1 H 0.2152 0.4000 0.2464 0.020 Uiso 1 1 calc R . . C2 C 0.1089(5) 0.4680(4) 0.1526(4) 0.0253(13) Uani 1 1 d . . . H2 H 0.1561 0.5108 0.1308 0.030 Uiso 1 1 calc R . . C3 C -0.0211(5) 0.4516(5) 0.1244(4) 0.0323(15) Uani 1 1 d . . . H3 H -0.0547 0.4741 0.0705 0.039 Uiso 1 1 calc R . . C4 C -0.0309(5) 0.3412(5) 0.1424(5) 0.0326(16) Uani 1 1 d . . . H4A H -0.1102 0.3194 0.1384 0.039 Uiso 1 1 calc R . . H4B H 0.0099 0.3002 0.1100 0.039 Uiso 1 1 calc R . . C5 C 0.0329(5) 0.3515(4) 0.2293(4) 0.0202(12) Uani 1 1 d . . . H5 H 0.0444 0.2920 0.2618 0.024 Uiso 1 1 calc R . . C6 C -0.0446(5) 0.4309(4) 0.2551(4) 0.0221(12) Uani 1 1 d . . . H6 H -0.0658 0.4364 0.3051 0.027 Uiso 1 1 calc R . . C7 C -0.0757(5) 0.4897(5) 0.1942(4) 0.0308(14) Uani 1 1 d . . . H7 H -0.1224 0.5446 0.1934 0.037 Uiso 1 1 calc R . . P1 P 0.34388(11) 0.25419(9) 0.05324(8) 0.0120(2) Uani 1 1 d . . . C8 C 0.4941(4) 0.2617(4) 0.1171(3) 0.0167(10) Uani 1 1 d . . . C9 C 0.4850(5) 0.2574(5) 0.2067(4) 0.0226(12) Uani 1 1 d . . . H9A H 0.4585 0.1940 0.2191 0.034 Uiso 1 1 calc R . . H9B H 0.4312 0.3059 0.2179 0.034 Uiso 1 1 calc R . . H9C H 0.5596 0.2697 0.2387 0.034 Uiso 1 1 calc R . . C10 C 0.5479(5) 0.3623(4) 0.1059(4) 0.0216(12) Uani 1 1 d . . . H10A H 0.6203 0.3682 0.1422 0.032 Uiso 1 1 calc R . . H10B H 0.4963 0.4128 0.1167 0.032 Uiso 1 1 calc R . . H10C H 0.5607 0.3683 0.0519 0.032 Uiso 1 1 calc R . . C11 C 0.5781(5) 0.1821(4) 0.0986(4) 0.0217(11) Uani 1 1 d . . . H11A H 0.5828 0.1842 0.0428 0.033 Uiso 1 1 calc R . . H11B H 0.5505 0.1193 0.1114 0.033 Uiso 1 1 calc R . . H11C H 0.6533 0.1934 0.1300 0.033 Uiso 1 1 calc R . . C12 C 0.3438(4) 0.3047(4) -0.0505(3) 0.0153(10) Uani 1 1 d . . . C13 C 0.3416(5) 0.4174(4) -0.0464(4) 0.0207(11) Uani 1 1 d . . . H13A H 0.3440 0.4440 -0.0983 0.031 Uiso 1 1 calc R . . H13B H 0.4074 0.4400 -0.0090 0.031 Uiso 1 1 calc R . . H13C H 0.2720 0.4383 -0.0293 0.031 Uiso 1 1 calc R . . C14 C 0.4472(5) 0.2724(4) -0.0874(4) 0.0210(11) Uani 1 1 d . . . H14A H 0.4505 0.2025 -0.0884 0.031 Uiso 1 1 calc R . . H14B H 0.5172 0.2975 -0.0561 0.031 Uiso 1 1 calc R . . H14C H 0.4388 0.2971 -0.1411 0.031 Uiso 1 1 calc R . . C15 C 0.2325(5) 0.2747(4) -0.1078(4) 0.0198(11) Uani 1 1 d . . . H15A H 0.2310 0.3048 -0.1590 0.030 Uiso 1 1 calc R . . H15B H 0.1664 0.2956 -0.0863 0.030 Uiso 1 1 calc R . . H15C H 0.2307 0.2051 -0.1139 0.030 Uiso 1 1 calc R . . C16 C 0.2879(4) 0.1239(4) 0.0482(3) 0.0162(10) Uani 1 1 d . . . C17 C 0.3108(5) 0.0806(4) 0.1329(4) 0.0210(11) Uani 1 1 d . . . H17A H 0.2738 0.0181 0.1323 0.031 Uiso 1 1 calc R . . H17B H 0.2804 0.1235 0.1687 0.031 Uiso 1 1 calc R . . H17C H 0.3926 0.0730 0.1507 0.031 Uiso 1 1 calc R . . C18 C 0.1553(5) 0.1235(4) 0.0217(4) 0.0207(11) Uani 1 1 d . . . H18A H 0.1278 0.0574 0.0179 0.031 Uiso 1 1 calc R . . H18B H 0.1353 0.1545 -0.0296 0.031 Uiso 1 1 calc R . . H18C H 0.1203 0.1583 0.0602 0.031 Uiso 1 1 calc R . . C19 C 0.3417(5) 0.0584(4) -0.0080(4) 0.0208(11) Uani 1 1 d . . . H19A H 0.4244 0.0615 0.0060 0.031 Uiso 1 1 calc R . . H19B H 0.3177 0.0802 -0.0621 0.031 Uiso 1 1 calc R . . H19C H 0.3166 -0.0076 -0.0031 0.031 Uiso 1 1 calc R . . Sb1 Sb 0.17928(3) 0.76210(3) 0.07685(2) 0.01447(9) Uani 1 1 d . . . F1 F 0.2486(3) 0.6658(3) 0.0238(3) 0.0324(9) Uani 1 1 d . . . F2 F 0.2255(3) 0.6969(3) 0.1739(2) 0.0322(9) Uani 1 1 d . . . F3 F 0.3171(3) 0.8333(2) 0.0950(2) 0.0230(7) Uani 1 1 d . . . F4 F 0.1103(3) 0.8598(3) 0.1305(3) 0.0293(9) Uani 1 1 d . . . F5 F 0.1336(3) 0.8302(3) -0.0190(2) 0.0299(8) Uani 1 1 d . . . F6 F 0.0408(3) 0.6913(3) 0.0591(2) 0.0281(8) Uani 1 1 d . . . Cl1 Cl 0.67763(13) 0.51535(14) 0.28611(10) 0.0327(4) Uani 1 1 d . . . Cl2 Cl 0.43400(13) 0.57033(12) 0.25166(11) 0.0309(3) Uani 1 1 d . . . C20 C 0.5494(5) 0.5281(5) 0.3250(4) 0.0263(13) Uani 1 1 d . . . H20A H 0.5623 0.5737 0.3694 0.032 Uiso 1 1 calc R . . H20B H 0.5288 0.4656 0.3453 0.032 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 0.01566(11) 0.01617(12) 0.01540(13) -0.00165(7) 0.00744(8) 0.00228(7) C1 0.015(2) 0.022(3) 0.014(3) -0.006(2) 0.0052(19) 0.0033(19) C2 0.033(3) 0.019(3) 0.030(3) -0.001(2) 0.020(3) 0.008(2) C3 0.026(3) 0.053(4) 0.018(3) 0.005(3) 0.006(2) 0.022(3) C4 0.016(3) 0.047(4) 0.036(4) -0.022(3) 0.007(3) -0.004(3) C5 0.023(3) 0.020(3) 0.020(3) -0.001(2) 0.010(2) 0.002(2) C6 0.019(2) 0.029(3) 0.021(3) -0.008(2) 0.009(2) -0.001(2) C7 0.025(3) 0.039(4) 0.030(4) -0.001(3) 0.010(3) 0.016(3) P1 0.0124(5) 0.0138(6) 0.0108(6) 0.0006(5) 0.0047(5) 0.0021(4) C8 0.015(2) 0.021(3) 0.014(3) -0.001(2) -0.0004(19) -0.0004(19) C9 0.023(3) 0.030(3) 0.014(3) 0.001(2) 0.001(2) 0.001(2) C10 0.018(2) 0.023(3) 0.024(3) -0.002(2) 0.003(2) -0.004(2) C11 0.015(2) 0.025(3) 0.026(3) 0.000(2) 0.003(2) 0.004(2) C12 0.017(2) 0.019(3) 0.010(2) 0.000(2) 0.0042(18) 0.0009(19) C13 0.023(3) 0.018(3) 0.021(3) 0.007(2) 0.005(2) 0.000(2) C14 0.022(3) 0.028(3) 0.015(3) 0.000(2) 0.010(2) 0.002(2) C15 0.018(2) 0.025(3) 0.017(3) 0.003(2) 0.004(2) 0.001(2) C16 0.016(2) 0.014(2) 0.020(3) -0.002(2) 0.007(2) 0.0006(19) C17 0.025(3) 0.020(3) 0.020(3) 0.004(2) 0.008(2) 0.000(2) C18 0.016(2) 0.023(3) 0.024(3) 0.001(2) 0.005(2) -0.001(2) C19 0.023(2) 0.018(3) 0.024(3) -0.003(2) 0.009(2) 0.003(2) Sb1 0.01321(16) 0.01639(17) 0.01442(19) 0.00049(13) 0.00416(12) 0.00129(12) F1 0.0265(18) 0.0263(19) 0.047(3) -0.0151(17) 0.0130(18) 0.0013(15) F2 0.036(2) 0.035(2) 0.023(2) 0.0165(17) 0.0001(16) 0.0053(17) F3 0.0168(15) 0.0251(17) 0.027(2) -0.0037(14) 0.0039(14) -0.0042(13) F4 0.0300(19) 0.0270(19) 0.034(2) -0.0068(16) 0.0143(17) 0.0070(15) F5 0.0336(19) 0.037(2) 0.0169(19) 0.0077(16) -0.0014(15) -0.0033(16) F6 0.0181(15) 0.0290(19) 0.038(2) 0.0022(16) 0.0066(15) -0.0054(14) Cl1 0.0197(6) 0.0556(10) 0.0231(8) 0.0001(7) 0.0048(5) 0.0004(6) Cl2 0.0235(6) 0.0351(8) 0.0357(9) 0.0094(7) 0.0099(6) 0.0056(6) C20 0.024(3) 0.035(3) 0.022(3) 0.000(3) 0.009(2) -0.005(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 Au1 C1 2.273(5) . ? Au1 P1 2.2939(12) . ? Au1 C2 2.296(5) . ? C1 C2 1.370(9) . ? C1 C5 1.531(8) . ? C1 H1 0.9300 . ? C2 C3 1.534(9) . ? C2 H2 0.9300 . ? C3 C7 1.538(9) . ? C3 C4 1.553(10) . ? C3 H3 0.9800 . ? C4 C5 1.539(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.533(8) . ? C5 H5 0.9800 . ? C6 C7 1.311(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? P1 C12 1.893(6) . ? P1 C16 1.900(5) . ? P1 C8 1.903(5) . ? C8 C11 1.542(7) . ? C8 C10 1.543(8) . ? C8 C9 1.546(8) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.531(7) . ? C12 C15 1.542(8) . ? C12 C13 1.547(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C19 1.528(7) . ? C16 C17 1.535(8) . ? C16 C18 1.544(7) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? Sb1 F1 1.866(4) . ? Sb1 F2 1.868(4) . ? Sb1 F3 1.869(3) . ? Sb1 F5 1.870(4) . ? Sb1 F6 1.874(3) . ? Sb1 F4 1.884(3) . ? Cl1 C20 1.761(6) . ? Cl2 C20 1.768(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 158.37(15) . . ? C1 Au1 C2 34.9(2) . . ? P1 Au1 C2 166.00(16) . . ? C2 C1 C5 107.2(5) . . ? C2 C1 Au1 73.5(3) . . ? C5 C1 Au1 114.8(4) . . ? C2 C1 H1 126.4 . . ? C5 C1 H1 126.4 . . ? Au1 C1 H1 83.5 . . ? C1 C2 C3 106.1(5) . . ? C1 C2 Au1 71.6(3) . . ? C3 C2 Au1 114.8(4) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? Au1 C2 H2 85.0 . . ? C2 C3 C7 103.9(5) . . ? C2 C3 C4 100.7(5) . . ? C7 C3 C4 97.1(5) . . ? C2 C3 H3 117.3 . . ? C7 C3 H3 117.3 . . ? C4 C3 H3 117.3 . . ? C5 C4 C3 93.4(5) . . ? C5 C4 H4A 113.0 . . ? C3 C4 H4A 113.0 . . ? C5 C4 H4B 113.0 . . ? C3 C4 H4B 113.0 . . ? H4A C4 H4B 110.4 . . ? C1 C5 C6 104.0(4) . . ? C1 C5 C4 100.5(5) . . ? C6 C5 C4 97.3(5) . . ? C1 C5 H5 117.3 . . ? C6 C5 H5 117.3 . . ? C4 C5 H5 117.3 . . ? C7 C6 C5 107.9(5) . . ? C7 C6 H6 126.1 . . ? C5 C6 H6 126.1 . . ? C6 C7 C3 107.7(5) . . ? C6 C7 H7 126.1 . . ? C3 C7 H7 126.1 . . ? C12 P1 C16 111.1(3) . . ? C12 P1 C8 110.9(2) . . ? C16 P1 C8 110.8(2) . . ? C12 P1 Au1 109.00(17) . . ? C16 P1 Au1 108.37(16) . . ? C8 P1 Au1 106.57(17) . . ? C11 C8 C10 108.3(4) . . ? C11 C8 C9 109.5(5) . . ? C10 C8 C9 104.9(5) . . ? C11 C8 P1 114.1(4) . . ? C10 C8 P1 109.7(4) . . ? C9 C8 P1 109.8(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C15 108.1(5) . . ? C14 C12 C13 109.2(4) . . ? C15 C12 C13 106.0(4) . . ? C14 C12 P1 114.1(4) . . ? C15 C12 P1 110.5(4) . . ? C13 C12 P1 108.7(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C17 109.6(5) . . ? C19 C16 C18 108.9(5) . . ? C17 C16 C18 105.7(4) . . ? C19 C16 P1 113.7(4) . . ? C17 C16 P1 108.7(4) . . ? C18 C16 P1 109.9(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F1 Sb1 F2 90.3(2) . . ? F1 Sb1 F3 90.46(16) . . ? F2 Sb1 F3 89.87(17) . . ? F1 Sb1 F5 90.87(19) . . ? F2 Sb1 F5 178.61(18) . . ? F3 Sb1 F5 89.31(17) . . ? F1 Sb1 F6 89.90(17) . . ? F2 Sb1 F6 90.03(17) . . ? F3 Sb1 F6 179.63(17) . . ? F5 Sb1 F6 90.78(17) . . ? F1 Sb1 F4 179.61(18) . . ? F2 Sb1 F4 89.71(19) . . ? F3 Sb1 F4 89.15(17) . . ? F5 Sb1 F4 89.15(19) . . ? F6 Sb1 F4 90.49(17) . . ? Cl1 C20 Cl2 111.6(3) . . ? Cl1 C20 H20A 109.3 . . ? Cl2 C20 H20A 109.3 . . ? Cl1 C20 H20B 109.3 . . ? Cl2 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 C1 C2 170.2(3) . . . . ? P1 Au1 C1 C5 -88.0(5) . . . . ? C2 Au1 C1 C5 101.7(5) . . . . ? C5 C1 C2 C3 -0.1(6) . . . . ? Au1 C1 C2 C3 111.4(4) . . . . ? C5 C1 C2 Au1 -111.4(4) . . . . ? P1 Au1 C2 C1 -165.0(5) . . . . ? C1 Au1 C2 C3 -99.7(6) . . . . ? P1 Au1 C2 C3 95.3(8) . . . . ? C1 C2 C3 C7 66.4(6) . . . . ? Au1 C2 C3 C7 143.2(5) . . . . ? C1 C2 C3 C4 -33.8(6) . . . . ? Au1 C2 C3 C4 43.0(6) . . . . ? C2 C3 C4 C5 51.4(5) . . . . ? C7 C3 C4 C5 -54.2(5) . . . . ? C2 C1 C5 C6 -66.1(6) . . . . ? Au1 C1 C5 C6 -145.5(4) . . . . ? C2 C1 C5 C4 34.2(6) . . . . ? Au1 C1 C5 C4 -45.1(5) . . . . ? C3 C4 C5 C1 -51.2(5) . . . . ? C3 C4 C5 C6 54.5(5) . . . . ? C1 C5 C6 C7 66.4(6) . . . . ? C4 C5 C6 C7 -36.4(6) . . . . ? C5 C6 C7 C3 0.5(7) . . . . ? C2 C3 C7 C6 -67.7(7) . . . . ? C4 C3 C7 C6 35.2(7) . . . . ? C1 Au1 P1 C12 -169.3(4) . . . . ? C2 Au1 P1 C12 -13.0(8) . . . . ? C1 Au1 P1 C16 69.7(4) . . . . ? C2 Au1 P1 C16 -134.0(7) . . . . ? C1 Au1 P1 C8 -49.6(4) . . . . ? C2 Au1 P1 C8 106.7(7) . . . . ? C12 P1 C8 C11 -77.6(4) . . . . ? C16 P1 C8 C11 46.3(5) . . . . ? Au1 P1 C8 C11 164.0(4) . . . . ? C12 P1 C8 C10 44.2(4) . . . . ? C16 P1 C8 C10 168.0(4) . . . . ? Au1 P1 C8 C10 -74.3(4) . . . . ? C12 P1 C8 C9 159.0(4) . . . . ? C16 P1 C8 C9 -77.1(4) . . . . ? Au1 P1 C8 C9 40.6(4) . . . . ? C16 P1 C12 C14 -80.3(4) . . . . ? C8 P1 C12 C14 43.3(5) . . . . ? Au1 P1 C12 C14 160.3(4) . . . . ? C16 P1 C12 C15 41.7(4) . . . . ? C8 P1 C12 C15 165.3(4) . . . . ? Au1 P1 C12 C15 -77.7(4) . . . . ? C16 P1 C12 C13 157.6(3) . . . . ? C8 P1 C12 C13 -78.8(4) . . . . ? Au1 P1 C12 C13 38.2(4) . . . . ? C12 P1 C16 C19 47.2(5) . . . . ? C8 P1 C16 C19 -76.5(5) . . . . ? Au1 P1 C16 C19 166.9(4) . . . . ? C12 P1 C16 C17 169.6(3) . . . . ? C8 P1 C16 C17 45.9(4) . . . . ? Au1 P1 C16 C17 -70.7(4) . . . . ? C12 P1 C16 C18 -75.2(4) . . . . ? C8 P1 C16 C18 161.1(4) . . . . ? Au1 P1 C16 C18 44.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.58 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 4.603 _refine_diff_density_min -4.150 _refine_diff_density_rms 0.433 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 729114' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C31 H62 Au2 P2, 2(F6 Sb)' _chemical_formula_sum 'C31 H62 Au2 F12 P2 Sb2' _chemical_formula_weight 1362.18 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 20.3711(4) _cell_length_b 12.6067(3) _cell_length_c 17.0445(4) _cell_angle_alpha 90.00 _cell_angle_beta 104.6320(10) _cell_angle_gamma 90.00 _cell_volume 4235.28(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9937 _cell_measurement_theta_min 2.792 _cell_measurement_theta_max 28.458 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 8.318 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.134 _exptl_absorpt_correction_T_max 0.189 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 60578 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 29.71 _reflns_number_total 11999 _reflns_number_gt 9602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The occupancy of each set of carbon atoms on the one disordered P(t)Bu3 unit was allowed to freely refine and found to be about 41:59. Disordered atom pairs, C30A and C31B, C28A and C27B, C27A and C28B, C24A and C23B were described using the EXYZ and EADP commands. 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^)+(0.0347P)^2^+3.4554P] 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 11999 _refine_ls_number_parameters 524 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 C1 C 0.1286(2) -0.0250(3) 0.1802(2) 0.0195(9) Uani 1 1 d . . . H1 H 0.0979 -0.0785 0.1878 0.023 Uiso 1 1 calc R . . C2 C 0.1208(2) 0.0396(4) 0.1147(3) 0.0219(9) Uani 1 1 d . . . H2 H 0.0840 0.0398 0.0675 0.026 Uiso 1 1 calc R . . C3 C 0.1841(2) 0.1131(4) 0.1325(3) 0.0225(9) Uani 1 1 d . . . H3 H 0.1942 0.1513 0.0854 0.027 Uiso 1 1 calc R . . C4 C 0.2380(2) 0.0356(3) 0.1794(3) 0.0199(9) Uani 1 1 d . . . H4A H 0.2814 0.0709 0.2058 0.024 Uiso 1 1 calc R . . H4B H 0.2461 -0.0247 0.1458 0.024 Uiso 1 1 calc R . . C5 C 0.1961(2) 0.0044(3) 0.2399(2) 0.0192(8) Uani 1 1 d . . . H5 H 0.2165 -0.0486 0.2828 0.023 Uiso 1 1 calc R . . C6 C 0.1806(2) 0.1148(4) 0.2679(3) 0.0213(9) Uani 1 1 d . . . H6 H 0.1765 0.1334 0.3205 0.026 Uiso 1 1 calc R . . C7 C 0.1739(2) 0.1813(4) 0.2036(3) 0.0227(9) Uani 1 1 d . . . H7 H 0.1646 0.2552 0.2026 0.027 Uiso 1 1 calc R . . Au1 Au 0.140636(9) -0.133342(14) 0.079622(10) 0.02168(5) Uani 1 1 d . . . P1 P 0.15342(7) -0.29603(11) 0.02486(7) 0.0283(3) Uani 1 1 d . . . C9 C 0.2446(3) -0.3162(6) 0.0235(4) 0.0511(18) Uani 1 1 d . . . C10 C 0.2883(4) -0.3407(7) 0.1097(4) 0.074(3) Uani 1 1 d . . . H10A H 0.3363 -0.3425 0.1093 0.111 Uiso 1 1 calc R . . H10B H 0.2752 -0.4097 0.1274 0.111 Uiso 1 1 calc R . . H10C H 0.2812 -0.2855 0.1472 0.111 Uiso 1 1 calc R . . C11 C 0.2728(3) -0.2133(6) -0.0032(4) 0.059(2) Uani 1 1 d . . . H11A H 0.2684 -0.1557 0.0337 0.089 Uiso 1 1 calc R . . H11B H 0.2473 -0.1953 -0.0584 0.089 Uiso 1 1 calc R . . H11C H 0.3208 -0.2232 -0.0021 0.089 Uiso 1 1 calc R . . C12 C 0.2553(3) -0.4097(6) -0.0313(4) 0.062(2) Uani 1 1 d . . . H12A H 0.2341 -0.3925 -0.0882 0.093 Uiso 1 1 calc R . . H12B H 0.2345 -0.4741 -0.0161 0.093 Uiso 1 1 calc R . . H12C H 0.3040 -0.4215 -0.0244 0.093 Uiso 1 1 calc R . . C13 C 0.0959(3) -0.3011(4) -0.0813(3) 0.0305(11) Uani 1 1 d . . . C14 C 0.0286(3) -0.2453(5) -0.0827(3) 0.0357(12) Uani 1 1 d . . . H14A H 0.0377 -0.1721 -0.0637 0.054 Uiso 1 1 calc R . . H14B H 0.0055 -0.2831 -0.0472 0.054 Uiso 1 1 calc R . . H14C H -0.0003 -0.2450 -0.1382 0.054 Uiso 1 1 calc R . . C15 C 0.1274(3) -0.2378(5) -0.1390(3) 0.0371(13) Uani 1 1 d . . . H15A H 0.1680 -0.2744 -0.1458 0.056 Uiso 1 1 calc R . . H15B H 0.1398 -0.1669 -0.1165 0.056 Uiso 1 1 calc R . . H15C H 0.0945 -0.2314 -0.1918 0.056 Uiso 1 1 calc R . . C16 C 0.0817(3) -0.4137(5) -0.1146(3) 0.0418(14) Uani 1 1 d . . . H16A H 0.0495 -0.4111 -0.1681 0.063 Uiso 1 1 calc R . . H16B H 0.0623 -0.4558 -0.0777 0.063 Uiso 1 1 calc R . . H16C H 0.1241 -0.4464 -0.1195 0.063 Uiso 1 1 calc R . . C17 C 0.1261(3) -0.3967(4) 0.0933(3) 0.0403(14) Uani 1 1 d . . . C18 C 0.1572(4) -0.3654(5) 0.1834(3) 0.0501(17) Uani 1 1 d . . . H18A H 0.1406 -0.4140 0.2190 0.075 Uiso 1 1 calc R . . H18B H 0.1438 -0.2927 0.1926 0.075 Uiso 1 1 calc R . . H18C H 0.2068 -0.3698 0.1954 0.075 Uiso 1 1 calc R . . C19 C 0.0491(4) -0.3886(5) 0.0812(4) 0.0500(17) Uani 1 1 d . . . H19A H 0.0261 -0.4147 0.0271 0.075 Uiso 1 1 calc R . . H19B H 0.0366 -0.3144 0.0865 0.075 Uiso 1 1 calc R . . H19C H 0.0354 -0.4315 0.1224 0.075 Uiso 1 1 calc R . . C20 C 0.1460(5) -0.5112(5) 0.0813(4) 0.069(2) Uani 1 1 d . . . H20A H 0.1282 -0.5580 0.1169 0.104 Uiso 1 1 calc R . . H20B H 0.1956 -0.5170 0.0946 0.104 Uiso 1 1 calc R . . H20C H 0.1272 -0.5320 0.0247 0.104 Uiso 1 1 calc R . . Au2 Au 0.272419(9) 0.221442(13) 0.305056(10) 0.02123(5) Uani 1 1 d . A . P2 P 0.36761(6) 0.30350(9) 0.38337(8) 0.0245(3) Uani 1 1 d . . . C21A C 0.4323(7) 0.3144(12) 0.3336(9) 0.039(4) Uani 0.412(7) 1 d P A 1 C22A C 0.5030(12) 0.3421(16) 0.3884(16) 0.042(6) Uani 0.412(7) 1 d P A 1 H22A H 0.5162 0.2887 0.4313 0.063 Uiso 0.412(7) 1 calc PR A 1 H22B H 0.5013 0.4121 0.4128 0.063 Uiso 0.412(7) 1 calc PR A 1 H22C H 0.5363 0.3431 0.3558 0.063 Uiso 0.412(7) 1 calc PR A 1 C23A C 0.4106(9) 0.3991(17) 0.2650(11) 0.045(5) Uani 0.412(7) 1 d P A 1 H23A H 0.3656 0.3813 0.2308 0.068 Uiso 0.412(7) 1 calc PR A 1 H23B H 0.4435 0.3999 0.2318 0.068 Uiso 0.412(7) 1 calc PR A 1 H23C H 0.4091 0.4692 0.2893 0.068 Uiso 0.412(7) 1 calc PR A 1 C24A C 0.4366(3) 0.2001(6) 0.2834(4) 0.0558(18) Uani 0.412(7) 1 d P A 1 H24A H 0.3916 0.1825 0.2492 0.084 Uiso 0.412(7) 1 calc PR A 1 H24B H 0.4523 0.1429 0.3225 0.084 Uiso 0.412(7) 1 calc PR A 1 H24C H 0.4685 0.2087 0.2493 0.084 Uiso 0.412(7) 1 calc PR A 1 C25A C 0.3937(6) 0.2269(9) 0.4877(6) 0.023(3) Uani 0.412(7) 1 d P A 1 C26A C 0.4337(8) 0.1295(10) 0.4759(9) 0.044(4) Uani 0.412(7) 1 d P A 1 H26A H 0.4746 0.1513 0.4599 0.066 Uiso 0.412(7) 1 calc PR A 1 H26B H 0.4056 0.0846 0.4335 0.066 Uiso 0.412(7) 1 calc PR A 1 H26C H 0.4466 0.0895 0.5268 0.066 Uiso 0.412(7) 1 calc PR A 1 C27A C 0.3394(4) 0.1847(5) 0.5095(4) 0.0498(16) Uani 0.412(7) 1 d P A 1 H27A H 0.3100 0.2420 0.5194 0.075 Uiso 0.412(7) 1 calc PR A 1 H27B H 0.3552 0.1426 0.5590 0.075 Uiso 0.412(7) 1 calc PR A 1 H27C H 0.3138 0.1392 0.4657 0.075 Uiso 0.412(7) 1 calc PR A 1 C28A C 0.4357(3) 0.3121(6) 0.5524(3) 0.0521(17) Uani 0.412(7) 1 d P A 1 H28A H 0.4741 0.3390 0.5333 0.078 Uiso 0.412(7) 1 calc PR A 1 H28B H 0.4526 0.2777 0.6052 0.078 Uiso 0.412(7) 1 calc PR A 1 H28C H 0.4059 0.3712 0.5577 0.078 Uiso 0.412(7) 1 calc PR A 1 C29A C 0.3345(5) 0.4434(8) 0.4131(6) 0.017(2) Uani 0.412(7) 1 d P A 1 C30A C 0.2915(3) 0.4881(4) 0.3303(4) 0.0467(16) Uani 0.412(7) 1 d P A 1 H30A H 0.3203 0.4948 0.2924 0.070 Uiso 0.412(7) 1 calc PR A 1 H30B H 0.2734 0.5579 0.3390 0.070 Uiso 0.412(7) 1 calc PR A 1 H30C H 0.2539 0.4396 0.3077 0.070 Uiso 0.412(7) 1 calc PR A 1 C31A C 0.3935(7) 0.5206(10) 0.4481(9) 0.029(3) Uani 0.412(7) 1 d P A 1 H31A H 0.4220 0.5275 0.4099 0.043 Uiso 0.412(7) 1 calc PR A 1 H31B H 0.4208 0.4930 0.4998 0.043 Uiso 0.412(7) 1 calc PR A 1 H31C H 0.3751 0.5902 0.4568 0.043 Uiso 0.412(7) 1 calc PR A 1 C32A C 0.2905(7) 0.4334(10) 0.4718(7) 0.027(3) Uani 0.412(7) 1 d P A 1 H32A H 0.2527 0.3851 0.4494 0.041 Uiso 0.412(7) 1 calc PR A 1 H32B H 0.2727 0.5033 0.4807 0.041 Uiso 0.412(7) 1 calc PR A 1 H32C H 0.3175 0.4052 0.5235 0.041 Uiso 0.412(7) 1 calc PR A 1 C21B C 0.4491(4) 0.2324(7) 0.3668(5) 0.031(2) Uani 0.588(7) 1 d P A 2 C22B C 0.4629(5) 0.1307(7) 0.4183(7) 0.044(3) Uani 0.588(7) 1 d P A 2 H22D H 0.4715 0.1492 0.4758 0.066 Uiso 0.588(7) 1 calc PR A 2 H22E H 0.5026 0.0944 0.4086 0.066 Uiso 0.588(7) 1 calc PR A 2 H22F H 0.4233 0.0838 0.4032 0.066 Uiso 0.588(7) 1 calc PR A 2 C23B C 0.4366(3) 0.2001(6) 0.2834(4) 0.0558(18) Uani 0.588(7) 1 d P A 2 H23D H 0.4277 0.2629 0.2484 0.084 Uiso 0.588(7) 1 calc PR A 2 H23E H 0.3971 0.1529 0.2699 0.084 Uiso 0.588(7) 1 calc PR A 2 H23F H 0.4764 0.1626 0.2751 0.084 Uiso 0.588(7) 1 calc PR A 2 C24B C 0.5132(7) 0.2999(10) 0.3887(10) 0.035(3) Uani 0.588(7) 1 d P A 2 H24D H 0.5221 0.3222 0.4455 0.052 Uiso 0.588(7) 1 calc PR A 2 H24E H 0.5071 0.3627 0.3537 0.052 Uiso 0.588(7) 1 calc PR A 2 H24F H 0.5517 0.2583 0.3809 0.052 Uiso 0.588(7) 1 calc PR A 2 C25B C 0.3659(4) 0.2973(7) 0.4885(5) 0.029(2) Uani 0.588(7) 1 d P A 2 C26B C 0.3104(5) 0.3739(10) 0.5021(6) 0.047(3) Uani 0.588(7) 1 d P A 2 H26D H 0.2681 0.3614 0.4606 0.070 Uiso 0.588(7) 1 calc PR A 2 H26E H 0.3251 0.4473 0.4985 0.070 Uiso 0.588(7) 1 calc PR A 2 H26F H 0.3029 0.3614 0.5559 0.070 Uiso 0.588(7) 1 calc PR A 2 C27B C 0.4357(3) 0.3121(6) 0.5524(3) 0.0521(17) Uani 0.588(7) 1 d P A 2 H27D H 0.4687 0.2613 0.5412 0.078 Uiso 0.588(7) 1 calc PR A 2 H27E H 0.4299 0.2998 0.6070 0.078 Uiso 0.588(7) 1 calc PR A 2 H27F H 0.4523 0.3845 0.5488 0.078 Uiso 0.588(7) 1 calc PR A 2 C28B C 0.3394(4) 0.1847(5) 0.5095(4) 0.0498(16) Uani 0.588(7) 1 d P A 2 H28D H 0.3709 0.1294 0.5017 0.075 Uiso 0.588(7) 1 calc PR A 2 H28E H 0.2944 0.1711 0.4737 0.075 Uiso 0.588(7) 1 calc PR A 2 H28F H 0.3365 0.1843 0.5660 0.075 Uiso 0.588(7) 1 calc PR A 2 C29B C 0.3668(5) 0.4436(7) 0.3401(6) 0.039(3) Uani 0.588(7) 1 d P A 2 C30B C 0.4140(6) 0.5178(8) 0.4011(8) 0.053(4) Uani 0.588(7) 1 d P A 2 H30D H 0.4016 0.5156 0.4530 0.080 Uiso 0.588(7) 1 calc PR A 2 H30E H 0.4092 0.5905 0.3800 0.080 Uiso 0.588(7) 1 calc PR A 2 H30F H 0.4611 0.4945 0.4090 0.080 Uiso 0.588(7) 1 calc PR A 2 C31B C 0.2915(3) 0.4881(4) 0.3303(4) 0.0467(16) Uani 0.588(7) 1 d P A 2 H31D H 0.2592 0.4438 0.2917 0.070 Uiso 0.588(7) 1 calc PR A 2 H31E H 0.2888 0.5613 0.3103 0.070 Uiso 0.588(7) 1 calc PR A 2 H31F H 0.2804 0.4865 0.3830 0.070 Uiso 0.588(7) 1 calc PR A 2 C32B C 0.3849(7) 0.4432(12) 0.2572(8) 0.058(5) Uani 0.588(7) 1 d P A 2 H32D H 0.3544 0.3948 0.2201 0.086 Uiso 0.588(7) 1 calc PR A 2 H32E H 0.4319 0.4196 0.2647 0.086 Uiso 0.588(7) 1 calc PR A 2 H32F H 0.3799 0.5150 0.2345 0.086 Uiso 0.588(7) 1 calc PR A 2 Sb1 Sb 0.381865(17) 0.84028(3) 0.30908(2) 0.03736(9) Uani 1 1 d . . . F1 F 0.29487(15) 0.7813(3) 0.2921(2) 0.0435(8) Uani 1 1 d . . . F2 F 0.36151(19) 0.8847(3) 0.2006(2) 0.0621(11) Uani 1 1 d . . . F3 F 0.41430(19) 0.7113(3) 0.2793(3) 0.0650(12) Uani 1 1 d . . . F4 F 0.46814(17) 0.8997(3) 0.3259(3) 0.0658(11) Uani 1 1 d . . . F5 F 0.40221(16) 0.7971(3) 0.4175(2) 0.0441(8) Uani 1 1 d . . . F6 F 0.34636(14) 0.9679(2) 0.33691(18) 0.0343(7) Uani 1 1 d . . . Sb2 Sb 0.078931(17) 0.11853(3) 0.864843(19) 0.03003(8) Uani 1 1 d . . . F7 F 0.02472(19) 0.1105(4) 0.9384(2) 0.0636(12) Uani 1 1 d . . . F8 F 0.03114(19) 0.0033(3) 0.8083(2) 0.0527(9) Uani 1 1 d . . . F9 F 0.14125(16) 0.0272(3) 0.93104(19) 0.0445(8) Uani 1 1 d . . . F10 F 0.13129(19) 0.1221(3) 0.7892(2) 0.0507(9) Uani 1 1 d . . . F11 F 0.1268(2) 0.2327(3) 0.9190(3) 0.0698(12) Uani 1 1 d . . . F12 F 0.0155(2) 0.2098(3) 0.80011(19) 0.0566(11) 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 C1 0.021(2) 0.021(2) 0.017(2) -0.0070(16) 0.0062(17) -0.0048(17) C2 0.019(2) 0.029(2) 0.015(2) -0.0047(17) -0.0016(16) -0.0012(18) C3 0.020(2) 0.029(2) 0.016(2) 0.0025(17) 0.0015(17) -0.0062(18) C4 0.018(2) 0.023(2) 0.019(2) -0.0016(17) 0.0057(16) -0.0037(17) C5 0.018(2) 0.024(2) 0.0151(19) -0.0003(16) 0.0019(16) -0.0056(17) C6 0.015(2) 0.028(2) 0.020(2) -0.0063(17) 0.0028(16) -0.0071(17) C7 0.017(2) 0.021(2) 0.027(2) -0.0038(18) -0.0016(17) -0.0068(17) Au1 0.01870(9) 0.02975(10) 0.01655(8) -0.00790(7) 0.00437(6) -0.00540(7) P1 0.0302(7) 0.0367(7) 0.0175(6) -0.0124(5) 0.0050(5) -0.0012(5) C9 0.032(3) 0.082(5) 0.037(3) -0.041(3) 0.004(2) 0.007(3) C10 0.049(4) 0.121(7) 0.040(4) -0.036(4) -0.010(3) 0.036(4) C11 0.025(3) 0.098(6) 0.056(4) -0.046(4) 0.014(3) -0.011(3) C12 0.047(4) 0.093(5) 0.043(4) -0.039(4) 0.009(3) 0.027(4) C13 0.032(3) 0.041(3) 0.019(2) -0.008(2) 0.006(2) -0.004(2) C14 0.033(3) 0.055(3) 0.019(2) -0.008(2) 0.004(2) -0.006(2) C15 0.036(3) 0.054(3) 0.023(2) -0.007(2) 0.010(2) -0.010(3) C16 0.044(3) 0.059(4) 0.022(3) -0.017(2) 0.009(2) -0.021(3) C17 0.070(4) 0.030(3) 0.019(2) -0.006(2) 0.007(3) 0.001(3) C18 0.087(5) 0.039(3) 0.022(3) -0.007(2) 0.009(3) 0.012(3) C19 0.074(5) 0.051(4) 0.033(3) -0.012(3) 0.029(3) -0.026(3) C20 0.141(8) 0.028(3) 0.039(4) -0.008(3) 0.021(4) 0.009(4) Au2 0.01656(8) 0.02221(9) 0.02116(9) -0.00256(6) -0.00221(6) -0.00565(6) P2 0.0183(6) 0.0205(6) 0.0279(6) -0.0010(5) -0.0069(5) -0.0051(5) C21A 0.023(7) 0.052(9) 0.045(8) -0.025(7) 0.014(6) -0.018(6) C22A 0.029(10) 0.045(13) 0.060(11) -0.032(12) 0.026(8) -0.009(9) C23A 0.032(10) 0.079(15) 0.029(9) -0.004(9) 0.015(8) -0.029(9) C24A 0.026(3) 0.082(5) 0.062(4) -0.025(4) 0.016(3) -0.009(3) C25A 0.026(6) 0.016(5) 0.019(5) -0.005(4) -0.007(4) 0.000(5) C26A 0.040(8) 0.036(7) 0.041(8) -0.012(6) -0.016(6) 0.017(6) C27A 0.061(4) 0.045(3) 0.035(3) 0.008(3) -0.004(3) -0.013(3) C28A 0.030(3) 0.089(5) 0.029(3) -0.018(3) -0.007(2) -0.011(3) C29A 0.004(4) 0.017(5) 0.031(6) -0.002(4) 0.004(4) -0.001(3) C30A 0.038(3) 0.024(3) 0.058(4) 0.005(2) -0.026(3) -0.002(2) C31A 0.024(6) 0.020(6) 0.035(7) -0.008(5) -0.006(5) -0.004(5) C32A 0.027(7) 0.028(6) 0.024(6) -0.009(5) 0.001(5) -0.002(5) C21B 0.020(4) 0.038(5) 0.032(5) -0.008(4) 0.002(3) -0.002(4) C22B 0.032(5) 0.027(5) 0.059(7) -0.007(4) -0.013(5) 0.002(4) C23B 0.026(3) 0.082(5) 0.062(4) -0.025(4) 0.016(3) -0.009(3) C24B 0.016(6) 0.043(9) 0.042(7) -0.004(7) 0.001(5) -0.011(6) C25B 0.026(4) 0.035(5) 0.022(4) 0.002(3) -0.002(3) -0.003(4) C26B 0.034(6) 0.071(8) 0.033(5) -0.024(5) 0.004(4) 0.008(5) C27B 0.030(3) 0.089(5) 0.029(3) -0.018(3) -0.007(2) -0.011(3) C28B 0.061(4) 0.045(3) 0.035(3) 0.008(3) -0.004(3) -0.013(3) C29B 0.035(5) 0.024(4) 0.045(5) 0.015(4) -0.016(4) -0.013(4) C30B 0.050(7) 0.019(5) 0.064(8) 0.009(5) -0.035(6) -0.016(4) C31B 0.038(3) 0.024(3) 0.058(4) 0.005(2) -0.026(3) -0.002(2) C32B 0.048(9) 0.073(10) 0.039(6) 0.041(7) -0.014(6) -0.024(7) Sb1 0.01619(16) 0.0484(2) 0.0449(2) -0.01297(17) 0.00294(14) 0.00740(15) F1 0.0220(16) 0.048(2) 0.055(2) -0.0223(16) -0.0014(14) 0.0019(14) F2 0.044(2) 0.096(3) 0.049(2) -0.009(2) 0.0177(18) 0.022(2) F3 0.044(2) 0.069(3) 0.081(3) -0.029(2) 0.012(2) 0.0286(19) F4 0.0156(17) 0.084(3) 0.095(3) 0.004(2) 0.0085(18) -0.0005(18) F5 0.0279(17) 0.052(2) 0.0465(19) -0.0030(16) -0.0022(14) 0.0091(15) F6 0.0233(15) 0.0355(16) 0.0411(17) -0.0084(13) 0.0025(13) 0.0012(12) Sb2 0.02618(17) 0.0429(2) 0.01998(15) 0.00793(13) 0.00396(13) 0.01113(14) F7 0.041(2) 0.124(4) 0.0308(18) 0.017(2) 0.0173(16) 0.030(2) F8 0.049(2) 0.057(2) 0.046(2) -0.0005(17) -0.0005(16) -0.0030(17) F9 0.0360(19) 0.059(2) 0.0356(17) 0.0170(15) 0.0041(14) 0.0196(16) F10 0.051(2) 0.063(2) 0.047(2) 0.0214(17) 0.0292(18) 0.0103(18) F11 0.073(3) 0.055(2) 0.066(3) -0.008(2) -0.012(2) 0.011(2) F12 0.069(3) 0.063(2) 0.0307(17) 0.0081(16) 0.0000(17) 0.043(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 C1 C2 1.359(6) . ? C1 C5 1.536(6) . ? C1 Au1 2.254(4) . ? C1 H1 0.9500 . ? C2 C3 1.555(6) . ? C2 Au1 2.323(4) . ? C2 H2 0.9500 . ? C3 C4 1.536(6) . ? C3 C7 1.543(6) . ? C3 H3 1.0000 . ? C4 C5 1.548(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.530(6) . ? C5 H5 1.0000 . ? C6 C7 1.359(6) . ? C6 Au2 2.260(4) . ? C6 H6 0.9500 . ? C7 Au2 2.350(4) . ? C7 H7 0.9500 . ? Au1 P1 2.2953(13) . ? P1 C9 1.881(6) . ? P1 C13 1.893(5) . ? P1 C17 1.899(6) . ? C9 C11 1.533(10) . ? C9 C10 1.544(9) . ? C9 C12 1.554(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.529(7) . ? C13 C15 1.528(7) . ? C13 C14 1.536(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.528(8) . ? C17 C19 1.532(9) . ? C17 C18 1.558(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Au2 P2 2.3032(12) . ? P2 C21A 1.743(13) . ? P2 C25B 1.803(8) . ? P2 C29B 1.913(8) . ? P2 C21B 1.969(9) . ? P2 C25A 1.975(11) . ? P2 C29A 1.999(10) . ? C21A C22A 1.55(3) . ? C21A C23A 1.56(3) . ? C21A C24A 1.689(15) . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C25A C27A 1.361(13) . ? C25A C26A 1.515(17) . ? C25A C28A 1.620(12) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29A C32A 1.509(15) . ? C29A C31A 1.544(15) . ? C29A C30A 1.566(11) . ? C30A H30A 0.9800 . ? C30A H30B 0.9800 . ? C30A H30C 0.9800 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C21B C24B 1.524(17) . ? C21B C22B 1.538(14) . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25B C26B 1.548(14) . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C29B C30B 1.541(12) . ? C29B C32B 1.547(18) . ? C30B H30D 0.9800 . ? C30B H30E 0.9800 . ? C30B H30F 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? Sb1 F4 1.865(4) . ? Sb1 F5 1.871(3) . ? Sb1 F6 1.874(3) . ? Sb1 F2 1.876(4) . ? Sb1 F3 1.873(3) . ? Sb1 F1 1.876(3) . ? Sb2 F11 1.849(4) . ? Sb2 F9 1.867(3) . ? Sb2 F12 1.868(3) . ? Sb2 F10 1.871(3) . ? Sb2 F7 1.871(3) . ? Sb2 F8 1.874(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.4(4) . . ? C2 C1 Au1 75.5(2) . . ? C5 C1 Au1 113.5(3) . . ? C2 C1 H1 126.3 . . ? C5 C1 H1 126.3 . . ? Au1 C1 H1 82.8 . . ? C1 C2 C3 106.1(4) . . ? C1 C2 Au1 70.0(2) . . ? C3 C2 Au1 114.8(3) . . ? C1 C2 H2 126.9 . . ? C3 C2 H2 126.9 . . ? Au1 C2 H2 86.3 . . ? C4 C3 C7 99.6(3) . . ? C4 C3 C2 99.9(3) . . ? C7 C3 C2 102.4(3) . . ? C4 C3 H3 117.3 . . ? C7 C3 H3 117.3 . . ? C2 C3 H3 117.3 . . ? C3 C4 C5 93.8(3) . . ? C3 C4 H4A 113.0 . . ? C5 C4 H4A 113.0 . . ? C3 C4 H4B 113.0 . . ? C5 C4 H4B 113.0 . . ? H4A C4 H4B 110.4 . . ? C6 C5 C1 101.8(3) . . ? C6 C5 C4 99.7(3) . . ? C1 C5 C4 99.9(3) . . ? C6 C5 H5 117.4 . . ? C1 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? C7 C6 C5 107.3(4) . . ? C7 C6 Au2 76.5(3) . . ? C5 C6 Au2 114.1(3) . . ? C7 C6 H6 126.4 . . ? C5 C6 H6 126.4 . . ? Au2 C6 H6 81.5 . . ? C6 C7 C3 106.5(4) . . ? C6 C7 Au2 69.2(2) . . ? C3 C7 Au2 116.0(3) . . ? C6 C7 H7 126.7 . . ? C3 C7 H7 126.7 . . ? Au2 C7 H7 86.0 . . ? C1 Au1 P1 153.67(12) . . ? C1 Au1 C2 34.51(15) . . ? P1 Au1 C2 171.22(11) . . ? C9 P1 C13 111.0(2) . . ? C9 P1 C17 111.2(3) . . ? C13 P1 C17 111.0(2) . . ? C9 P1 Au1 109.8(2) . . ? C13 P1 Au1 108.23(17) . . ? C17 P1 Au1 105.44(17) . . ? C11 C9 C10 106.5(6) . . ? C11 C9 C12 110.0(5) . . ? C10 C9 C12 106.6(6) . . ? C11 C9 P1 109.6(5) . . ? C10 C9 P1 110.5(5) . . ? C12 C9 P1 113.5(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 108.5(4) . . ? C16 C13 C14 109.6(4) . . ? C15 C13 C14 105.6(4) . . ? C16 C13 P1 113.6(4) . . ? C15 C13 P1 109.8(4) . . ? C14 C13 P1 109.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 110.1(6) . . ? C20 C17 C18 108.4(5) . . ? C19 C17 C18 105.3(5) . . ? C20 C17 P1 114.8(4) . . ? C19 C17 P1 108.8(4) . . ? C18 C17 P1 109.1(4) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C6 Au2 P2 161.00(12) . . ? C6 Au2 C7 34.22(16) . . ? P2 Au2 C7 163.93(12) . . ? C21A P2 C25B 134.0(6) . . ? C21A P2 C29B 71.0(6) . . ? C25B P2 C29B 115.0(4) . . ? C21A P2 C21B 36.7(6) . . ? C25B P2 C21B 110.6(4) . . ? C29B P2 C21B 106.9(4) . . ? C21A P2 C25A 114.4(7) . . ? C25B P2 C25A 32.0(4) . . ? C29B P2 C25A 140.6(4) . . ? C21B P2 C25A 82.0(4) . . ? C21A P2 C29A 113.5(6) . . ? C25B P2 C29A 72.1(4) . . ? C29B P2 C29A 46.5(4) . . ? C21B P2 C29A 142.1(4) . . ? C25A P2 C29A 103.5(4) . . ? C21A P2 Au2 112.5(4) . . ? C25B P2 Au2 109.4(3) . . ? C29B P2 Au2 105.5(3) . . ? C21B P2 Au2 109.2(2) . . ? C25A P2 Au2 107.3(3) . . ? C29A P2 Au2 104.8(3) . . ? C22A C21A C23A 110.0(14) . . ? C22A C21A C24A 109.8(11) . . ? C23A C21A C24A 104.2(11) . . ? C22A C21A P2 115.3(12) . . ? C23A C21A P2 108.2(11) . . ? C24A C21A P2 108.8(8) . . ? C21A C22A H22A 109.5 . . ? C21A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C21A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? C21A C23A H23A 109.5 . . ? C21A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? C21A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C21A C24A H24A 109.5 . . ? C21A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C21A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C27A C25A C26A 102.8(10) . . ? C27A C25A C28A 113.6(8) . . ? C26A C25A C28A 114.7(9) . . ? C27A C25A P2 112.6(7) . . ? C26A C25A P2 107.9(9) . . ? C28A C25A P2 105.3(6) . . ? C25A C26A H26A 109.5 . . ? C25A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C25A C27A H27A 109.5 . . ? C25A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C25A C28A H28A 109.5 . . ? C25A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C25A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C32A C29A C31A 109.3(10) . . ? C32A C29A C30A 109.7(8) . . ? C31A C29A C30A 108.9(8) . . ? C32A C29A P2 112.9(8) . . ? C31A C29A P2 112.0(7) . . ? C30A C29A P2 103.7(6) . . ? C29A C30A H30A 109.5 . . ? C29A C30A H30B 109.5 . . ? H30A C30A H30B 109.5 . . ? C29A C30A H30C 109.5 . . ? H30A C30A H30C 109.5 . . ? H30B C30A H30C 109.5 . . ? C29A C31A H31A 109.5 . . ? C29A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C29A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C29A C32A H32A 109.5 . . ? C29A C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C29A C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C24B C21B C22B 107.7(8) . . ? C24B C21B P2 114.3(7) . . ? C22B C21B P2 109.7(7) . . ? C21B C22B H22D 109.5 . . ? C21B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C21B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? C21B C24B H24D 109.5 . . ? C21B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C21B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C26B C25B P2 108.7(6) . . ? C25B C26B H26D 109.5 . . ? C25B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C30B C29B C32B 111.4(10) . . ? C30B C29B P2 110.9(6) . . ? C32B C29B P2 111.6(8) . . ? C29B C30B H30D 109.5 . . ? C29B C30B H30E 109.5 . . ? H30D C30B H30E 109.5 . . ? C29B C30B H30F 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C29B C32B H32D 109.5 . . ? C29B C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C29B C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? F4 Sb1 F5 90.02(17) . . ? F4 Sb1 F6 91.43(16) . . ? F5 Sb1 F6 90.18(14) . . ? F4 Sb1 F2 89.79(19) . . ? F5 Sb1 F2 179.54(16) . . ? F6 Sb1 F2 89.40(15) . . ? F4 Sb1 F3 90.42(18) . . ? F5 Sb1 F3 90.57(17) . . ? F6 Sb1 F3 178.01(15) . . ? F2 Sb1 F3 89.85(18) . . ? F4 Sb1 F1 179.66(16) . . ? F5 Sb1 F1 90.09(15) . . ? F6 Sb1 F1 88.25(13) . . ? F2 Sb1 F1 90.09(17) . . ? F3 Sb1 F1 89.91(16) . . ? F11 Sb2 F9 89.19(17) . . ? F11 Sb2 F12 90.85(17) . . ? F9 Sb2 F12 178.83(16) . . ? F11 Sb2 F10 90.3(2) . . ? F9 Sb2 F10 90.71(15) . . ? F12 Sb2 F10 90.46(16) . . ? F11 Sb2 F7 92.0(2) . . ? F9 Sb2 F7 89.31(15) . . ? F12 Sb2 F7 89.51(16) . . ? F10 Sb2 F7 177.76(19) . . ? F11 Sb2 F8 178.89(19) . . ? F9 Sb2 F8 91.06(16) . . ? F12 Sb2 F8 88.92(16) . . ? F10 Sb2 F8 88.64(17) . . ? F7 Sb2 F8 89.12(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.6(5) . . . . ? Au1 C1 C2 C3 -111.1(3) . . . . ? C5 C1 C2 Au1 110.5(3) . . . . ? C1 C2 C3 C4 34.8(4) . . . . ? Au1 C2 C3 C4 -40.1(4) . . . . ? C1 C2 C3 C7 -67.4(4) . . . . ? Au1 C2 C3 C7 -142.3(3) . . . . ? C7 C3 C4 C5 52.4(4) . . . . ? C2 C3 C4 C5 -52.1(4) . . . . ? C2 C1 C5 C6 68.6(4) . . . . ? Au1 C1 C5 C6 150.0(3) . . . . ? C2 C1 C5 C4 -33.6(4) . . . . ? Au1 C1 C5 C4 47.8(4) . . . . ? C3 C4 C5 C6 -52.1(4) . . . . ? C3 C4 C5 C1 51.9(4) . . . . ? C1 C5 C6 C7 -68.8(4) . . . . ? C4 C5 C6 C7 33.6(4) . . . . ? C1 C5 C6 Au2 -151.4(3) . . . . ? C4 C5 C6 Au2 -49.0(4) . . . . ? C5 C6 C7 C3 0.7(5) . . . . ? Au2 C6 C7 C3 112.1(3) . . . . ? C5 C6 C7 Au2 -111.4(3) . . . . ? C4 C3 C7 C6 -35.1(4) . . . . ? C2 C3 C7 C6 67.3(4) . . . . ? C4 C3 C7 Au2 39.4(4) . . . . ? C2 C3 C7 Au2 141.8(3) . . . . ? C2 C1 Au1 P1 -173.6(2) . . . . ? C5 C1 Au1 P1 83.4(4) . . . . ? C5 C1 Au1 C2 -103.0(4) . . . . ? C3 C2 Au1 C1 99.0(4) . . . . ? C1 Au1 P1 C9 -101.7(3) . . . . ? C1 Au1 P1 C13 136.9(3) . . . . ? C1 Au1 P1 C17 18.1(3) . . . . ? C13 P1 C9 C11 77.7(4) . . . . ? C17 P1 C9 C11 -158.3(4) . . . . ? Au1 P1 C9 C11 -42.0(4) . . . . ? C13 P1 C9 C10 -165.4(5) . . . . ? C17 P1 C9 C10 -41.4(6) . . . . ? Au1 P1 C9 C10 74.9(5) . . . . ? C13 P1 C9 C12 -45.8(6) . . . . ? C17 P1 C9 C12 78.3(6) . . . . ? Au1 P1 C9 C12 -165.4(5) . . . . ? C9 P1 C13 C16 78.0(5) . . . . ? C17 P1 C13 C16 -46.2(4) . . . . ? Au1 P1 C13 C16 -161.4(3) . . . . ? C9 P1 C13 C15 -43.7(5) . . . . ? C17 P1 C13 C15 -167.9(4) . . . . ? Au1 P1 C13 C15 76.9(4) . . . . ? C9 P1 C13 C14 -159.2(4) . . . . ? C17 P1 C13 C14 76.7(4) . . . . ? Au1 P1 C13 C14 -38.6(4) . . . . ? C9 P1 C17 C20 -46.9(6) . . . . ? C13 P1 C17 C20 77.1(5) . . . . ? Au1 P1 C17 C20 -165.9(5) . . . . ? C9 P1 C17 C19 -170.8(3) . . . . ? C13 P1 C17 C19 -46.7(4) . . . . ? Au1 P1 C17 C19 70.3(4) . . . . ? C9 P1 C17 C18 74.9(5) . . . . ? C13 P1 C17 C18 -161.0(4) . . . . ? Au1 P1 C17 C18 -44.1(5) . . . . ? C7 C6 Au2 P2 168.0(3) . . . . ? C5 C6 Au2 P2 -88.9(4) . . . . ? C5 C6 Au2 C7 103.1(4) . . . . ? C3 C7 Au2 C6 -98.8(4) . . . . ? C6 C7 Au2 P2 -165.8(3) . . . . ? C3 C7 Au2 P2 95.4(5) . . . . ? C6 Au2 P2 C21A 137.7(7) . . . . ? C7 Au2 P2 C21A -67.4(8) . . . . ? C6 Au2 P2 C25B -22.7(5) . . . . ? C7 Au2 P2 C25B 132.3(5) . . . . ? C6 Au2 P2 C29B -146.9(5) . . . . ? C7 Au2 P2 C29B 8.1(6) . . . . ? C6 Au2 P2 C21B 98.5(5) . . . . ? C7 Au2 P2 C21B -106.6(5) . . . . ? C6 Au2 P2 C25A 11.0(5) . . . . ? C7 Au2 P2 C25A 166.0(6) . . . . ? C6 Au2 P2 C29A -98.6(5) . . . . ? C7 Au2 P2 C29A 56.4(5) . . . . ? C25B P2 C21A C22A -11.4(17) . . . . ? C29B P2 C21A C22A 95.3(13) . . . . ? C21B P2 C21A C22A -72.9(14) . . . . ? C25A P2 C21A C22A -42.5(14) . . . . ? C29A P2 C21A C22A 76.0(14) . . . . ? Au2 P2 C21A C22A -165.3(11) . . . . ? C25B P2 C21A C23A -135.0(10) . . . . ? C29B P2 C21A C23A -28.2(10) . . . . ? C21B P2 C21A C23A 163.6(15) . . . . ? C25A P2 C21A C23A -166.1(10) . . . . ? C29A P2 C21A C23A -47.5(11) . . . . ? Au2 P2 C21A C23A 71.2(11) . . . . ? C25B P2 C21A C24A 112.4(8) . . . . ? C29B P2 C21A C24A -140.9(10) . . . . ? C21B P2 C21A C24A 50.9(8) . . . . ? C25A P2 C21A C24A 81.3(9) . . . . ? C29A P2 C21A C24A -160.2(7) . . . . ? Au2 P2 C21A C24A -41.5(10) . . . . ? C21A P2 C25A C27A -156.5(8) . . . . ? C25B P2 C25A C27A 68.0(10) . . . . ? C29B P2 C25A C27A 114.2(8) . . . . ? C21B P2 C25A C27A -138.7(8) . . . . ? C29A P2 C25A C27A 79.5(8) . . . . ? Au2 P2 C25A C27A -31.0(8) . . . . ? C21A P2 C25A C26A -43.8(10) . . . . ? C25B P2 C25A C26A -179.3(14) . . . . ? C29B P2 C25A C26A -133.1(9) . . . . ? C21B P2 C25A C26A -26.0(9) . . . . ? C29A P2 C25A C26A -167.8(8) . . . . ? Au2 P2 C25A C26A 81.7(9) . . . . ? C21A P2 C25A C28A 79.2(8) . . . . ? C25B P2 C25A C28A -56.3(7) . . . . ? C29B P2 C25A C28A -10.1(11) . . . . ? C21B P2 C25A C28A 97.0(7) . . . . ? C29A P2 C25A C28A -44.8(7) . . . . ? Au2 P2 C25A C28A -155.3(5) . . . . ? C21A P2 C29A C32A -167.1(8) . . . . ? C25B P2 C29A C32A -36.1(8) . . . . ? C29B P2 C29A C32A 167.4(10) . . . . ? C21B P2 C29A C32A -136.9(8) . . . . ? C25A P2 C29A C32A -42.5(9) . . . . ? Au2 P2 C29A C32A 69.9(8) . . . . ? C21A P2 C29A C31A -43.1(10) . . . . ? C25B P2 C29A C31A 87.9(9) . . . . ? C29B P2 C29A C31A -68.6(8) . . . . ? C21B P2 C29A C31A -13.0(12) . . . . ? C25A P2 C29A C31A 81.5(9) . . . . ? Au2 P2 C29A C31A -166.2(8) . . . . ? C21A P2 C29A C30A 74.2(7) . . . . ? C25B P2 C29A C30A -154.8(6) . . . . ? C29B P2 C29A C30A 48.7(5) . . . . ? C21B P2 C29A C30A 104.4(7) . . . . ? C25A P2 C29A C30A -161.2(6) . . . . ? Au2 P2 C29A C30A -48.8(5) . . . . ? C21A P2 C21B C24B 56.5(11) . . . . ? C25B P2 C21B C24B -81.1(9) . . . . ? C29B P2 C21B C24B 44.8(9) . . . . ? C25A P2 C21B C24B -95.8(9) . . . . ? C29A P2 C21B C24B 6.0(12) . . . . ? Au2 P2 C21B C24B 158.5(8) . . . . ? C21A P2 C21B C22B 177.6(11) . . . . ? C25B P2 C21B C22B 40.1(7) . . . . ? C29B P2 C21B C22B 166.0(6) . . . . ? C25A P2 C21B C22B 25.3(6) . . . . ? C29A P2 C21B C22B 127.2(7) . . . . ? Au2 P2 C21B C22B -80.3(6) . . . . ? C21A P2 C25B C26B 133.8(9) . . . . ? C29B P2 C25B C26B 46.6(8) . . . . ? C21B P2 C25B C26B 167.9(6) . . . . ? C25A P2 C25B C26B -163.7(12) . . . . ? C29A P2 C25B C26B 28.0(7) . . . . ? Au2 P2 C25B C26B -71.8(7) . . . . ? C21A P2 C29B C30B -88.5(10) . . . . ? C25B P2 C29B C30B 42.0(10) . . . . ? C21B P2 C29B C30B -81.2(9) . . . . ? C25A P2 C29B C30B 17.0(13) . . . . ? C29A P2 C29B C30B 66.7(9) . . . . ? Au2 P2 C29B C30B 162.6(8) . . . . ? C21A P2 C29B C32B 36.3(8) . . . . ? C25B P2 C29B C32B 166.9(7) . . . . ? C21B P2 C29B C32B 43.7(8) . . . . ? C25A P2 C29B C32B 141.9(8) . . . . ? C29A P2 C29B C32B -168.4(10) . . . . ? Au2 P2 C29B C32B -72.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.71 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.257 _refine_diff_density_min -2.520 _refine_diff_density_rms 0.187 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 729115' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C16 H35 Au P, F6 Sb' _chemical_formula_sum 'C16 H35 Au F6 P Sb' _chemical_formula_weight 691.13 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_space_group_name_Hall 'C -2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.5097(9) _cell_length_b 10.7868(7) _cell_length_c 16.7912(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.666(4) _cell_angle_gamma 90.00 _cell_volume 2289.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6942 _cell_measurement_theta_min 2.482 _cell_measurement_theta_max 30.730 _exptl_crystal_description shard _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 7.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.310 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details SADABS-2007/4 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.366 _diffrn_detector_type 'Bruker-AXS SMART APEX' _diffrn_measurement_details 'frames, 0.3\% width' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker-AXS Kappa' _diffrn_measurement_method '\w & \f scans' _diffrn_measurement_specimen_support ; glass fibre ; _diffrn_radiation_collimation '0.5 mm double pinhole' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71074 _diffrn_source 'sealed X-ray tube' _diffrn_source_current 40 _diffrn_source_power 2 _diffrn_source_size '0.4 x 8 mm fine focus' _diffrn_source_target Mo _diffrn_source_type 'Bruker-AXS KFF Mo 2K 90\% Ceramic' _diffrn_source_voltage 50 _diffrn_reflns_number 16090 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.80 _diffrn_reflns_theta_max 34.74 _reflns_number_total 6777 _reflns_number_gt 5923 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.029(7) _refine_ls_number_reflns 6777 _refine_ls_number_parameters 243 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 0.94241(3) 0.65405(2) 0.67727(2) 0.02009(8) Uani 1 1 d . . . C1 C 0.9807(9) 0.8420(8) 0.6420(7) 0.0293(19) Uani 1 1 d D . . H1B H 0.995(9) 0.887(11) 0.696(4) 0.035 Uiso 1 1 d D . . H1A H 1.038(7) 0.814(11) 0.623(7) 0.035 Uiso 1 1 d D . . C2 C 0.8789(8) 0.8289(7) 0.5908(6) 0.0232(17) Uani 1 1 d . . . C3 C 0.7891(8) 0.8809(10) 0.6151(7) 0.032(2) Uani 1 1 d . . . H3A H 0.7622 0.9569 0.5827 0.047 Uiso 1 1 calc R . . H3B H 0.8151 0.8998 0.6762 0.047 Uiso 1 1 calc R . . H3C H 0.7320 0.8197 0.6023 0.047 Uiso 1 1 calc R . . C4 C 0.8488(8) 0.7817(9) 0.5011(6) 0.0268(18) Uani 1 1 d . . . H4A H 0.9069 0.7320 0.4959 0.040 Uiso 1 1 calc R . . H4B H 0.8347 0.8520 0.4617 0.040 Uiso 1 1 calc R . . H4C H 0.7851 0.7303 0.4873 0.040 Uiso 1 1 calc R . . P1 P 0.93482(16) 0.45687(18) 0.72576(13) 0.0169(4) Uani 1 1 d . . . C5 C 1.0641(7) 0.4225(8) 0.8144(6) 0.0254(17) Uani 1 1 d . . . C6 C 1.0590(8) 0.3096(9) 0.8699(6) 0.033(2) Uani 1 1 d . . . H6A H 1.1266 0.3013 0.9173 0.050 Uiso 1 1 calc R . . H6B H 1.0453 0.2342 0.8352 0.050 Uiso 1 1 calc R . . H6C H 1.0020 0.3219 0.8925 0.050 Uiso 1 1 calc R . . C7 C 1.1519(8) 0.4044(10) 0.7780(8) 0.037(2) Uani 1 1 d . . . H7A H 1.1362 0.3314 0.7408 0.055 Uiso 1 1 calc R . . H7B H 1.2195 0.3921 0.8247 0.055 Uiso 1 1 calc R . . H7C H 1.1565 0.4779 0.7452 0.055 Uiso 1 1 calc R . . C8 C 1.0976(8) 0.5392(10) 0.8725(7) 0.036(2) Uani 1 1 d . . . H8A H 1.0987 0.6117 0.8376 0.054 Uiso 1 1 calc R . . H8B H 1.1683 0.5261 0.9150 0.054 Uiso 1 1 calc R . . H8C H 1.0469 0.5531 0.9013 0.054 Uiso 1 1 calc R . . C9 C 0.8194(7) 0.4500(7) 0.7641(5) 0.0197(15) Uani 1 1 d . . . C10 C 0.7810(7) 0.3184(7) 0.7730(6) 0.0231(16) Uani 1 1 d . . . H10A H 0.7233 0.3229 0.7955 0.035 Uiso 1 1 calc R . . H10B H 0.8396 0.2702 0.8120 0.035 Uiso 1 1 calc R . . H10C H 0.7555 0.2781 0.7171 0.035 Uiso 1 1 calc R . . C11 C 0.8491(8) 0.5143(9) 0.8525(6) 0.0293(19) Uani 1 1 d . . . H11A H 0.9042 0.4661 0.8951 0.044 Uiso 1 1 calc R . . H11B H 0.7864 0.5191 0.8689 0.044 Uiso 1 1 calc R . . H11C H 0.8753 0.5981 0.8492 0.044 Uiso 1 1 calc R . . C12 C 0.7267(7) 0.5264(8) 0.7036(6) 0.0269(18) Uani 1 1 d . . . H12A H 0.6666 0.5230 0.7234 0.040 Uiso 1 1 calc R . . H12B H 0.7056 0.4919 0.6460 0.040 Uiso 1 1 calc R . . H12C H 0.7489 0.6127 0.7029 0.040 Uiso 1 1 calc R . . C13 C 0.9142(8) 0.3480(8) 0.6337(5) 0.0249(18) Uani 1 1 d . . . C14 C 0.9346(10) 0.2082(9) 0.6602(7) 0.035(2) Uani 1 1 d . . . H14A H 0.9038 0.1556 0.6099 0.053 Uiso 1 1 calc R . . H14B H 0.9017 0.1886 0.7022 0.053 Uiso 1 1 calc R . . H14C H 1.0109 0.1931 0.6851 0.053 Uiso 1 1 calc R . . C15 C 0.9848(9) 0.3864(10) 0.5836(7) 0.034(2) Uani 1 1 d . . . H15A H 0.9619 0.4673 0.5570 0.052 Uiso 1 1 calc R . . H15B H 0.9791 0.3245 0.5395 0.052 Uiso 1 1 calc R . . H15C H 1.0584 0.3918 0.6224 0.052 Uiso 1 1 calc R . . C16 C 0.7991(9) 0.3590(10) 0.5702(6) 0.034(2) Uani 1 1 d . . . H16A H 0.7501 0.3321 0.5981 0.051 Uiso 1 1 calc R . . H16B H 0.7902 0.3064 0.5206 0.051 Uiso 1 1 calc R . . H16C H 0.7843 0.4454 0.5519 0.051 Uiso 1 1 calc R . . Sb1 Sb 0.99866(4) 0.06137(5) 0.41103(3) 0.01951(11) Uani 1 1 d . . . F1 F 0.9028(5) -0.0443(5) 0.3327(4) 0.0349(13) Uani 1 1 d . . . F2 F 1.0539(5) -0.0738(5) 0.4830(4) 0.0321(13) Uani 1 1 d . . . F3 F 0.9001(5) 0.0873(6) 0.4650(4) 0.0361(14) Uani 1 1 d . . . F4 F 0.9398(6) 0.1937(6) 0.3373(4) 0.0438(16) Uani 1 1 d . . . F5 F 1.0942(6) 0.1670(6) 0.4889(5) 0.0478(18) Uani 1 1 d . . . F6 F 1.0940(5) 0.0346(7) 0.3548(5) 0.0452(16) 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 Au1 0.02533(13) 0.01538(12) 0.02252(12) 0.00346(13) 0.01212(10) 0.00123(14) C1 0.043(5) 0.019(4) 0.033(5) 0.007(3) 0.022(4) -0.004(3) C2 0.036(5) 0.012(3) 0.026(4) 0.004(3) 0.016(4) 0.000(3) C3 0.031(5) 0.032(5) 0.034(5) 0.005(4) 0.015(4) 0.009(4) C4 0.032(4) 0.026(4) 0.025(4) 0.003(3) 0.013(4) 0.002(3) P1 0.0196(9) 0.0145(8) 0.0186(9) 0.0008(7) 0.0092(7) 0.0015(7) C5 0.024(4) 0.021(4) 0.031(4) 0.007(3) 0.010(3) 0.000(3) C6 0.036(5) 0.025(4) 0.030(5) 0.014(4) 0.000(4) 0.004(4) C7 0.024(5) 0.036(5) 0.053(6) 0.008(5) 0.018(4) 0.001(4) C8 0.033(5) 0.032(5) 0.033(5) -0.002(4) 0.001(4) -0.009(4) C9 0.024(4) 0.014(3) 0.025(4) 0.003(3) 0.014(3) 0.004(3) C10 0.028(4) 0.014(3) 0.029(4) 0.003(3) 0.013(3) -0.003(3) C11 0.039(5) 0.021(4) 0.036(5) -0.007(3) 0.022(4) -0.007(3) C12 0.021(4) 0.022(4) 0.039(5) 0.009(4) 0.012(4) 0.005(3) C13 0.034(5) 0.025(4) 0.016(4) -0.003(3) 0.009(3) 0.007(3) C14 0.047(6) 0.024(4) 0.039(6) 0.000(4) 0.021(6) 0.009(5) C15 0.050(6) 0.031(5) 0.034(5) 0.002(4) 0.029(5) 0.007(4) C16 0.041(5) 0.036(5) 0.023(4) -0.006(4) 0.008(4) -0.003(4) Sb1 0.0247(2) 0.0150(2) 0.0222(2) -0.0018(2) 0.0124(2) -0.00019(19) F1 0.044(3) 0.026(3) 0.029(3) -0.011(2) 0.007(3) 0.004(2) F2 0.036(3) 0.030(3) 0.031(3) 0.011(2) 0.013(3) 0.007(2) F3 0.032(3) 0.043(3) 0.039(3) -0.007(3) 0.020(3) 0.004(3) F4 0.064(4) 0.019(3) 0.050(4) 0.010(3) 0.022(3) 0.005(3) F5 0.040(4) 0.037(4) 0.057(4) -0.017(3) 0.005(3) -0.008(3) F6 0.046(4) 0.047(4) 0.059(4) 0.007(3) 0.039(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.224(9) . ? Au1 P1 2.293(2) . ? Au1 C2 2.350(8) . ? C1 C2 1.349(14) . ? C1 H1B 0.99(2) . ? C1 H1A 0.98(2) . ? C2 C4 1.502(13) . ? C2 C3 1.518(14) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? P1 C13 1.882(9) . ? P1 C9 1.887(9) . ? P1 C5 1.889(9) . ? C5 C7 1.527(14) . ? C5 C6 1.550(13) . ? C5 C8 1.558(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.537(11) . ? C9 C12 1.544(11) . ? C9 C11 1.557(12) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.533(15) . ? C13 C16 1.548(14) . ? C13 C14 1.570(13) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Sb1 F5 1.867(6) . ? Sb1 F6 1.868(7) . ? Sb1 F1 1.872(5) . ? Sb1 F4 1.873(6) . ? Sb1 F2 1.873(5) . ? Sb1 F3 1.877(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 C1 Au1 P1 169.8(3) . . ? C1 Au1 C2 34.1(4) . . ? P1 Au1 C2 155.7(2) . . ? C2 C1 Au1 78.1(5) . . ? C2 C1 H1B 118(7) . . ? Au1 C1 H1B 101(8) . . ? C2 C1 H1A 120(7) . . ? Au1 C1 H1A 95(8) . . ? H1B C1 H1A 122(10) . . ? C1 C2 C4 121.9(9) . . ? C1 C2 C3 121.5(9) . . ? C4 C2 C3 115.9(8) . . ? C1 C2 Au1 67.8(5) . . ? C4 C2 Au1 104.9(5) . . ? C3 C2 Au1 106.4(6) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C13 P1 C9 110.8(4) . . ? C13 P1 C5 110.7(4) . . ? C9 P1 C5 111.6(4) . . ? C13 P1 Au1 107.4(3) . . ? C9 P1 Au1 107.7(2) . . ? C5 P1 Au1 108.5(3) . . ? C7 C5 C6 110.2(8) . . ? C7 C5 C8 105.0(8) . . ? C6 C5 C8 108.9(8) . . ? C7 C5 P1 110.0(7) . . ? C6 C5 P1 113.8(6) . . ? C8 C5 P1 108.6(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 C12 109.5(7) . . ? C10 C9 C11 107.5(7) . . ? C12 C9 C11 105.4(7) . . ? C10 C9 P1 114.7(6) . . ? C12 C9 P1 109.3(6) . . ? C11 C9 P1 110.0(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C16 105.7(8) . . ? C15 C13 C14 109.5(8) . . ? C16 C13 C14 107.5(8) . . ? C15 C13 P1 110.0(7) . . ? C16 C13 P1 109.8(6) . . ? C14 C13 P1 113.9(6) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? F5 Sb1 F6 91.1(4) . . ? F5 Sb1 F1 179.9(4) . . ? F6 Sb1 F1 88.9(3) . . ? F5 Sb1 F4 91.5(3) . . ? F6 Sb1 F4 89.6(3) . . ? F1 Sb1 F4 88.4(3) . . ? F5 Sb1 F2 90.2(3) . . ? F6 Sb1 F2 90.9(3) . . ? F1 Sb1 F2 89.9(3) . . ? F4 Sb1 F2 178.3(3) . . ? F5 Sb1 F3 90.2(3) . . ? F6 Sb1 F3 178.6(3) . . ? F1 Sb1 F3 89.8(3) . . ? F4 Sb1 F3 89.8(3) . . ? F2 Sb1 F3 89.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 C1 C2 167.2(13) . . . . ? Au1 C1 C2 C4 -94.2(7) . . . . ? Au1 C1 C2 C3 96.2(8) . . . . ? P1 Au1 C2 C1 -174.5(6) . . . . ? C1 Au1 C2 C4 118.8(9) . . . . ? P1 Au1 C2 C4 -55.7(10) . . . . ? C1 Au1 C2 C3 -117.9(9) . . . . ? P1 Au1 C2 C3 67.6(9) . . . . ? C1 Au1 P1 C13 -102.3(16) . . . . ? C2 Au1 P1 C13 60.1(7) . . . . ? C1 Au1 P1 C9 138.2(16) . . . . ? C2 Au1 P1 C9 -59.3(6) . . . . ? C1 Au1 P1 C5 17.3(16) . . . . ? C2 Au1 P1 C5 179.7(7) . . . . ? C13 P1 C5 C7 45.2(8) . . . . ? C9 P1 C5 C7 169.2(6) . . . . ? Au1 P1 C5 C7 -72.4(7) . . . . ? C13 P1 C5 C6 -79.0(9) . . . . ? C9 P1 C5 C6 45.0(9) . . . . ? Au1 P1 C5 C6 163.5(7) . . . . ? C13 P1 C5 C8 159.6(7) . . . . ? C9 P1 C5 C8 -76.5(7) . . . . ? Au1 P1 C5 C8 42.0(7) . . . . ? C13 P1 C9 C10 44.9(7) . . . . ? C5 P1 C9 C10 -79.0(7) . . . . ? Au1 P1 C9 C10 162.0(5) . . . . ? C13 P1 C9 C12 -78.5(6) . . . . ? C5 P1 C9 C12 157.7(6) . . . . ? Au1 P1 C9 C12 38.7(6) . . . . ? C13 P1 C9 C11 166.2(6) . . . . ? C5 P1 C9 C11 42.3(7) . . . . ? Au1 P1 C9 C11 -76.6(6) . . . . ? C9 P1 C13 C15 159.8(6) . . . . ? C5 P1 C13 C15 -75.8(7) . . . . ? Au1 P1 C13 C15 42.5(7) . . . . ? C9 P1 C13 C16 43.9(8) . . . . ? C5 P1 C13 C16 168.3(7) . . . . ? Au1 P1 C13 C16 -73.4(7) . . . . ? C9 P1 C13 C14 -76.7(9) . . . . ? C5 P1 C13 C14 47.6(9) . . . . ? Au1 P1 C13 C14 165.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.796 _diffrn_reflns_theta_full 34.74 _diffrn_measured_fraction_theta_full 0.796 _refine_diff_density_max 5.257 _refine_diff_density_min -3.787 _refine_diff_density_rms 0.282