# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_c294 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H64 Au Cl2 F3 N2 O3 P2 S' _chemical_formula_weight 1280.00 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3839(2) _cell_length_b 12.7921(2) _cell_length_c 20.0475(3) _cell_angle_alpha 81.878(2) _cell_angle_beta 76.444(2) _cell_angle_gamma 89.880(2) _cell_volume 2808.14(8) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 33414 _cell_measurement_theta_min 4.1311 _cell_measurement_theta_max 28.1373 _exptl_crystal_description prism _exptl_crystal_colour pale-green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 2.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7626 _exptl_absorpt_correction_T_max 0.8032 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0655 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52544 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _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 4.14 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10415 _reflns_number_gt 9710 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0256P)^2^+2.7856P] 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 10415 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0548 _refine_ls_wR_factor_gt 0.0535 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.145165(9) 0.195026(7) 0.226799(5) 0.01444(4) Uani 1 1 d . . . P1 P 0.08671(6) 0.12198(5) 0.34120(3) 0.01386(14) Uani 1 1 d . . . P2 P 0.23312(7) 0.34108(5) 0.33407(4) 0.02046(15) Uani 1 1 d . . . N1 N 0.2401(2) 0.15902(16) 0.07827(11) 0.0168(5) Uani 1 1 d . . . N2 N 0.1770(2) 0.31665(17) 0.07893(11) 0.0173(5) Uani 1 1 d . . . C1 C 0.1931(2) 0.2291(2) 0.12150(14) 0.0164(5) Uani 1 1 d . . . C2 C 0.2523(3) 0.2030(2) 0.00954(14) 0.0211(6) Uani 1 1 d . . . H2 H 0.2831 0.1699 -0.0303 0.025 Uiso 1 1 calc R . . C3 C 0.2118(3) 0.3015(2) 0.01058(14) 0.0203(6) Uani 1 1 d . . . H3 H 0.2078 0.3515 -0.0286 0.024 Uiso 1 1 calc R . . C4 C 0.2731(2) 0.0538(2) 0.10271(14) 0.0186(6) Uani 1 1 d . . . C5 C 0.1842(3) -0.0277(2) 0.11782(14) 0.0206(6) Uani 1 1 d . . . C6 C 0.2163(3) -0.1261(2) 0.14679(15) 0.0261(7) Uani 1 1 d . . . H6 H 0.1583 -0.1831 0.1593 0.031 Uiso 1 1 calc R . . C7 C 0.3303(3) -0.1422(2) 0.15763(15) 0.0272(7) Uani 1 1 d . . . H7 H 0.3495 -0.2099 0.1778 0.033 Uiso 1 1 calc R . . C8 C 0.4173(3) -0.0616(2) 0.13975(15) 0.0250(6) Uani 1 1 d . . . H8 H 0.4962 -0.0750 0.1463 0.030 Uiso 1 1 calc R . . C9 C 0.3903(3) 0.0393(2) 0.11211(14) 0.0207(6) Uani 1 1 d . . . C10 C 0.0594(3) -0.0135(2) 0.10429(15) 0.0253(6) Uani 1 1 d . . . H10 H 0.0590 0.0572 0.0758 0.030 Uiso 1 1 calc R . . C11 C -0.0372(3) -0.0151(3) 0.17195(17) 0.0380(8) Uani 1 1 d . . . H11A H -0.1167 -0.0053 0.1615 0.057 Uiso 1 1 calc R . . H11B H -0.0195 0.0421 0.1963 0.057 Uiso 1 1 calc R . . H11C H -0.0372 -0.0831 0.2014 0.057 Uiso 1 1 calc R . . C12 C 0.0290(3) -0.0975(3) 0.06310(18) 0.0374(8) Uani 1 1 d . . . H12A H -0.0520 -0.0861 0.0549 0.056 Uiso 1 1 calc R . . H12B H 0.0309 -0.1678 0.0895 0.056 Uiso 1 1 calc R . . H12C H 0.0884 -0.0924 0.0185 0.056 Uiso 1 1 calc R . . C13 C 0.4852(3) 0.1287(2) 0.09525(15) 0.0238(6) Uani 1 1 d . . . H13 H 0.4537 0.1905 0.0689 0.029 Uiso 1 1 calc R . . C14 C 0.5048(3) 0.1624(3) 0.16188(17) 0.0376(8) Uani 1 1 d . . . H14A H 0.5658 0.2202 0.1504 0.056 Uiso 1 1 calc R . . H14B H 0.5326 0.1023 0.1896 0.056 Uiso 1 1 calc R . . H14C H 0.4286 0.1865 0.1885 0.056 Uiso 1 1 calc R . . C15 C 0.6045(3) 0.0989(3) 0.04986(18) 0.0364(8) Uani 1 1 d . . . H15A H 0.6628 0.1586 0.0400 0.055 Uiso 1 1 calc R . . H15B H 0.5907 0.0814 0.0062 0.055 Uiso 1 1 calc R . . H15C H 0.6364 0.0376 0.0742 0.055 Uiso 1 1 calc R . . C16 C 0.1229(2) 0.4113(2) 0.10271(13) 0.0181(6) Uani 1 1 d . . . C17 C 0.1987(3) 0.4949(2) 0.10623(14) 0.0204(6) Uani 1 1 d . . . C18 C 0.1427(3) 0.5835(2) 0.13098(15) 0.0254(6) Uani 1 1 d . . . H18 H 0.1911 0.6422 0.1343 0.030 Uiso 1 1 calc R . . C19 C 0.0181(3) 0.5876(2) 0.15080(15) 0.0284(7) Uani 1 1 d . . . H19 H -0.0181 0.6484 0.1681 0.034 Uiso 1 1 calc R . . C20 C -0.0540(3) 0.5039(2) 0.14563(15) 0.0267(7) Uani 1 1 d . . . H20 H -0.1394 0.5082 0.1591 0.032 Uiso 1 1 calc R . . C21 C -0.0036(3) 0.4133(2) 0.12094(14) 0.0222(6) Uani 1 1 d . . . C22 C 0.3350(3) 0.4900(2) 0.08543(15) 0.0243(6) Uani 1 1 d . . . H22 H 0.3550 0.4386 0.0515 0.029 Uiso 1 1 calc R . . C23 C 0.3971(3) 0.5961(2) 0.04952(16) 0.0311(7) Uani 1 1 d . . . H23A H 0.4849 0.5879 0.0371 0.047 Uiso 1 1 calc R . . H23B H 0.3776 0.6490 0.0810 0.047 Uiso 1 1 calc R . . H23C H 0.3687 0.6191 0.0074 0.047 Uiso 1 1 calc R . . C24 C 0.3861(3) 0.4482(3) 0.14771(18) 0.0358(8) Uani 1 1 d . . . H24A H 0.4743 0.4455 0.1328 0.054 Uiso 1 1 calc R . . H24B H 0.3521 0.3771 0.1672 0.054 Uiso 1 1 calc R . . H24C H 0.3647 0.4952 0.1830 0.054 Uiso 1 1 calc R . . C25 C -0.0831(3) 0.3239(2) 0.11231(16) 0.0273(7) Uani 1 1 d . . . H25 H -0.0296 0.2658 0.0964 0.033 Uiso 1 1 calc R . . C26 C -0.1708(3) 0.2797(3) 0.18060(19) 0.0453(9) Uani 1 1 d . . . H26A H -0.2202 0.2219 0.1731 0.068 Uiso 1 1 calc R . . H26B H -0.2233 0.3358 0.1977 0.068 Uiso 1 1 calc R . . H26C H -0.1250 0.2532 0.2149 0.068 Uiso 1 1 calc R . . C27 C -0.1517(4) 0.3605(3) 0.0568(2) 0.0516(10) Uani 1 1 d . . . H27A H -0.2023 0.3018 0.0515 0.077 Uiso 1 1 calc R . . H27B H -0.0940 0.3841 0.0126 0.077 Uiso 1 1 calc R . . H27C H -0.2029 0.4191 0.0707 0.077 Uiso 1 1 calc R . . C28 C 0.0342(2) 0.2084(2) 0.40632(13) 0.0151(5) Uani 1 1 d . . . C29 C -0.0713(2) 0.1810(2) 0.45778(13) 0.0172(5) Uani 1 1 d . . . H29 H -0.1145 0.1171 0.4588 0.021 Uiso 1 1 calc R . . C30 C -0.1137(3) 0.2459(2) 0.50736(14) 0.0212(6) Uani 1 1 d . . . H30 H -0.1867 0.2275 0.5414 0.025 Uiso 1 1 calc R . . C31 C -0.0490(3) 0.3378(2) 0.50701(14) 0.0223(6) Uani 1 1 d . . . H31 H -0.0770 0.3819 0.5414 0.027 Uiso 1 1 calc R . . C32 C 0.0562(3) 0.3651(2) 0.45667(14) 0.0213(6) Uani 1 1 d . . . H32 H 0.1002 0.4280 0.4571 0.026 Uiso 1 1 calc R . . C39 C 0.2903(2) 0.0016(2) 0.31717(15) 0.0208(6) Uani 1 1 d . . . H39 H 0.2764 0.0035 0.2721 0.025 Uiso 1 1 calc R . . C33 C 0.0992(2) 0.3021(2) 0.40506(14) 0.0181(6) Uani 1 1 d . . . C34 C 0.2125(2) 0.0525(2) 0.36627(14) 0.0165(5) Uani 1 1 d . . . C35 C 0.2339(2) 0.0503(2) 0.43220(14) 0.0194(6) Uani 1 1 d . . . H35 H 0.1813 0.0849 0.4658 0.023 Uiso 1 1 calc R . . C36 C 0.3322(3) -0.0027(2) 0.44848(16) 0.0256(6) Uani 1 1 d . . . H36 H 0.3473 -0.0040 0.4932 0.031 Uiso 1 1 calc R . . C37 C 0.4083(3) -0.0537(2) 0.39966(17) 0.0269(7) Uani 1 1 d . . . H37 H 0.4751 -0.0904 0.4113 0.032 Uiso 1 1 calc R . . C38 C 0.3885(3) -0.0520(2) 0.33420(16) 0.0254(6) Uani 1 1 d . . . H38 H 0.4413 -0.0871 0.3010 0.030 Uiso 1 1 calc R . . C40 C -0.0347(2) 0.0239(2) 0.35468(13) 0.0160(5) Uani 1 1 d . . . C41 C -0.1429(3) 0.0556(2) 0.33766(15) 0.0239(6) Uani 1 1 d . . . H41 H -0.1531 0.1279 0.3221 0.029 Uiso 1 1 calc R . . C42 C -0.2351(3) -0.0179(3) 0.34342(16) 0.0303(7) Uani 1 1 d . . . H42 H -0.3085 0.0041 0.3319 0.036 Uiso 1 1 calc R . . C43 C -0.2206(3) -0.1234(2) 0.36593(15) 0.0292(7) Uani 1 1 d . . . H43 H -0.2834 -0.1740 0.3691 0.035 Uiso 1 1 calc R . . C44 C -0.1152(3) -0.1549(2) 0.38366(16) 0.0285(7) Uani 1 1 d . . . H44 H -0.1060 -0.2271 0.3999 0.034 Uiso 1 1 calc R . . C45 C -0.0216(3) -0.0818(2) 0.37802(14) 0.0211(6) Uani 1 1 d . . . H45 H 0.0512 -0.1043 0.3902 0.025 Uiso 1 1 calc R . . C46 C 0.2322(3) 0.4847(2) 0.33057(14) 0.0226(6) Uani 1 1 d . . . C47 C 0.3210(3) 0.5449(2) 0.34654(15) 0.0265(7) Uani 1 1 d . . . H47 H 0.3858 0.5108 0.3623 0.032 Uiso 1 1 calc R . . C48 C 0.3155(3) 0.6543(2) 0.33967(16) 0.0305(7) Uani 1 1 d . . . H48 H 0.3770 0.6948 0.3501 0.037 Uiso 1 1 calc R . . C49 C 0.2208(3) 0.7043(2) 0.31767(15) 0.0299(7) Uani 1 1 d . . . H49 H 0.2162 0.7789 0.3141 0.036 Uiso 1 1 calc R . . C50 C 0.1328(3) 0.6460(2) 0.30078(15) 0.0307(7) Uani 1 1 d . . . H50 H 0.0679 0.6805 0.2854 0.037 Uiso 1 1 calc R . . C51 C 0.1395(3) 0.5371(2) 0.30638(15) 0.0287(7) Uani 1 1 d . . . H51 H 0.0800 0.4975 0.2935 0.034 Uiso 1 1 calc R . . C52 C 0.3593(3) 0.3009(2) 0.37305(15) 0.0237(6) Uani 1 1 d . . . C53 C 0.3561(3) 0.2931(2) 0.44343(16) 0.0278(7) Uani 1 1 d . . . H53 H 0.2847 0.3103 0.4748 0.033 Uiso 1 1 calc R . . C54 C 0.4563(3) 0.2603(3) 0.46809(18) 0.0338(7) Uani 1 1 d . . . H54 H 0.4531 0.2551 0.5162 0.041 Uiso 1 1 calc R . . C55 C 0.5606(3) 0.2350(3) 0.42298(19) 0.0368(8) Uani 1 1 d . . . H55 H 0.6292 0.2129 0.4400 0.044 Uiso 1 1 calc R . . C56 C 0.5646(3) 0.2421(3) 0.35345(19) 0.0392(8) Uani 1 1 d . . . H56 H 0.6362 0.2247 0.3223 0.047 Uiso 1 1 calc R . . C57 C 0.4653(3) 0.2744(2) 0.32862(17) 0.0318(7) Uani 1 1 d . . . H57 H 0.4691 0.2786 0.2805 0.038 Uiso 1 1 calc R . . S1 S 0.68311(7) 0.76067(6) 0.21884(4) 0.03061(18) Uani 1 1 d . . . F1 F 0.60253(18) 0.56299(15) 0.25024(10) 0.0426(5) Uani 1 1 d . . . F2 F 0.50215(17) 0.66304(16) 0.19081(11) 0.0450(5) Uani 1 1 d . . . F3 F 0.67597(18) 0.61047(17) 0.14257(10) 0.0454(5) Uani 1 1 d . . . O1 O 0.79811(18) 0.72377(17) 0.22881(12) 0.0333(5) Uani 1 1 d . . . O2 O 0.6003(2) 0.7828(2) 0.28055(14) 0.0498(7) Uani 1 1 d . . . O3 O 0.6885(2) 0.83551(19) 0.15703(15) 0.0519(7) Uani 1 1 d . . . C58 C 0.6130(3) 0.6454(3) 0.19999(16) 0.0297(7) Uani 1 1 d . . . Cl1 Cl 0.84574(8) 0.39201(8) 0.33836(5) 0.0455(2) Uani 1 1 d . . . Cl2 Cl 0.67021(10) 0.46325(8) 0.48613(6) 0.0553(3) Uani 1 1 d . . . C59 C 0.7946(4) 0.5231(3) 0.3546(2) 0.0591(12) Uani 1 1 d . . . H59A H 0.8507 0.5560 0.3772 0.071 Uiso 1 1 calc R . . H59B H 0.7960 0.5679 0.3100 0.071 Uiso 1 1 calc R . . C60 C 0.6716(4) 0.5183(3) 0.3993(2) 0.0581(11) Uani 1 1 d . . . H60A H 0.6182 0.4748 0.3809 0.070 Uiso 1 1 calc R . . H60B H 0.6396 0.5904 0.3986 0.070 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 0.01724(6) 0.01291(5) 0.01201(6) -0.00014(4) -0.00215(4) 0.00168(4) P1 0.0158(3) 0.0125(3) 0.0125(3) -0.0002(3) -0.0027(3) 0.0012(3) P2 0.0235(4) 0.0166(3) 0.0183(4) -0.0033(3) 0.0015(3) -0.0037(3) N1 0.0226(12) 0.0135(11) 0.0137(11) -0.0013(9) -0.0040(9) 0.0002(9) N2 0.0220(12) 0.0145(11) 0.0143(11) 0.0006(9) -0.0038(9) 0.0015(9) C1 0.0175(13) 0.0150(13) 0.0172(13) -0.0023(11) -0.0051(11) 0.0010(10) C2 0.0312(16) 0.0190(14) 0.0119(13) -0.0019(11) -0.0032(12) -0.0009(12) C3 0.0293(15) 0.0193(14) 0.0108(13) 0.0018(11) -0.0038(11) -0.0017(12) C4 0.0277(15) 0.0131(13) 0.0149(13) -0.0028(11) -0.0045(11) 0.0040(11) C5 0.0309(16) 0.0167(13) 0.0141(13) -0.0043(11) -0.0037(12) 0.0006(12) C6 0.0388(18) 0.0154(14) 0.0217(15) -0.0018(12) -0.0028(13) -0.0001(12) C7 0.0418(18) 0.0157(14) 0.0216(15) -0.0002(12) -0.0037(14) 0.0087(13) C8 0.0286(16) 0.0273(15) 0.0206(15) -0.0068(12) -0.0067(12) 0.0111(13) C9 0.0259(15) 0.0210(14) 0.0155(14) -0.0079(11) -0.0023(12) 0.0032(12) C10 0.0306(16) 0.0202(14) 0.0249(16) 0.0000(12) -0.0079(13) -0.0061(12) C11 0.0270(17) 0.053(2) 0.0326(18) -0.0065(16) -0.0044(14) -0.0070(15) C12 0.056(2) 0.0281(17) 0.0351(19) -0.0040(15) -0.0237(17) -0.0035(15) C13 0.0242(15) 0.0231(15) 0.0247(15) -0.0049(12) -0.0060(12) 0.0003(12) C14 0.0319(18) 0.049(2) 0.0321(18) -0.0173(16) -0.0013(15) -0.0070(15) C15 0.0321(18) 0.0379(18) 0.0349(19) -0.0120(15) 0.0047(15) -0.0046(15) C16 0.0260(15) 0.0144(13) 0.0122(13) 0.0009(10) -0.0029(11) 0.0039(11) C17 0.0259(15) 0.0191(14) 0.0149(13) -0.0001(11) -0.0038(11) 0.0027(11) C18 0.0338(17) 0.0178(14) 0.0231(15) -0.0045(12) -0.0029(13) 0.0013(12) C19 0.0354(17) 0.0217(15) 0.0247(16) -0.0019(12) -0.0010(13) 0.0099(13) C20 0.0239(15) 0.0277(16) 0.0250(16) 0.0032(13) -0.0027(13) 0.0080(13) C21 0.0245(15) 0.0220(14) 0.0184(14) 0.0040(12) -0.0060(12) 0.0022(12) C22 0.0261(15) 0.0208(14) 0.0239(15) -0.0079(12) 0.0007(12) -0.0005(12) C23 0.0312(17) 0.0299(16) 0.0268(17) -0.0007(13) 0.0017(14) -0.0046(13) C24 0.0268(17) 0.0341(18) 0.043(2) 0.0093(15) -0.0091(15) -0.0028(14) C25 0.0228(15) 0.0267(16) 0.0318(17) 0.0014(13) -0.0086(13) 0.0009(12) C26 0.039(2) 0.051(2) 0.040(2) 0.0089(17) -0.0082(17) -0.0147(17) C27 0.063(3) 0.048(2) 0.049(2) 0.0075(19) -0.033(2) -0.014(2) C28 0.0171(13) 0.0137(12) 0.0141(13) -0.0003(10) -0.0040(11) 0.0032(10) C29 0.0194(14) 0.0152(13) 0.0159(13) 0.0011(11) -0.0039(11) 0.0004(11) C30 0.0218(14) 0.0224(14) 0.0150(14) 0.0013(11) 0.0018(11) 0.0055(11) C31 0.0294(16) 0.0204(14) 0.0152(14) -0.0045(11) -0.0005(12) 0.0082(12) C32 0.0278(15) 0.0156(13) 0.0192(14) -0.0011(11) -0.0036(12) 0.0010(11) C39 0.0205(14) 0.0189(14) 0.0213(15) -0.0036(11) -0.0016(12) 0.0014(11) C33 0.0223(14) 0.0157(13) 0.0148(13) -0.0005(11) -0.0024(11) 0.0016(11) C34 0.0150(13) 0.0119(12) 0.0210(14) 0.0004(11) -0.0030(11) -0.0007(10) C35 0.0207(14) 0.0167(13) 0.0200(14) -0.0010(11) -0.0041(11) 0.0000(11) C36 0.0249(15) 0.0255(15) 0.0269(16) 0.0055(13) -0.0124(13) -0.0023(12) C37 0.0178(14) 0.0214(15) 0.0400(18) 0.0066(13) -0.0101(13) 0.0024(12) C38 0.0192(15) 0.0201(14) 0.0338(17) -0.0023(13) -0.0008(13) 0.0045(11) C40 0.0185(13) 0.0174(13) 0.0112(12) -0.0018(10) -0.0018(11) -0.0018(11) C41 0.0219(15) 0.0244(15) 0.0240(15) 0.0039(12) -0.0069(12) 0.0004(12) C42 0.0225(16) 0.0421(19) 0.0261(16) 0.0013(14) -0.0090(13) -0.0048(14) C43 0.0277(16) 0.0333(17) 0.0250(16) -0.0030(13) -0.0034(13) -0.0138(13) C44 0.0341(17) 0.0191(14) 0.0305(17) -0.0012(13) -0.0056(14) -0.0066(13) C45 0.0246(15) 0.0187(14) 0.0198(14) -0.0024(11) -0.0052(12) 0.0020(11) C46 0.0274(15) 0.0194(14) 0.0154(14) -0.0018(11) 0.0057(12) -0.0057(12) C47 0.0245(15) 0.0245(15) 0.0251(16) -0.0030(13) 0.0042(13) -0.0032(12) C48 0.0342(18) 0.0243(15) 0.0278(17) -0.0067(13) 0.0051(14) -0.0098(13) C49 0.0445(19) 0.0172(14) 0.0196(15) -0.0002(12) 0.0077(14) -0.0041(13) C50 0.0426(19) 0.0253(16) 0.0199(15) 0.0026(13) -0.0025(14) 0.0027(14) C51 0.0391(18) 0.0230(15) 0.0227(16) -0.0009(12) -0.0062(14) -0.0050(13) C52 0.0231(15) 0.0148(13) 0.0304(16) -0.0043(12) -0.0001(13) -0.0047(11) C53 0.0268(16) 0.0257(15) 0.0282(17) -0.0029(13) -0.0015(13) -0.0007(13) C54 0.0339(18) 0.0337(18) 0.0322(18) 0.0022(14) -0.0089(15) -0.0008(14) C55 0.0275(17) 0.0322(18) 0.050(2) -0.0024(16) -0.0102(16) 0.0013(14) C56 0.0248(17) 0.042(2) 0.048(2) -0.0118(17) -0.0001(15) 0.0053(15) C57 0.0287(17) 0.0350(17) 0.0290(17) -0.0092(14) 0.0012(14) 0.0015(14) S1 0.0220(4) 0.0311(4) 0.0404(5) -0.0072(4) -0.0095(3) 0.0079(3) F1 0.0500(12) 0.0414(11) 0.0346(11) 0.0006(9) -0.0101(9) -0.0068(9) F2 0.0308(10) 0.0544(13) 0.0599(14) -0.0235(11) -0.0221(10) 0.0116(9) F3 0.0458(12) 0.0597(13) 0.0289(10) -0.0157(10) 0.0002(9) 0.0114(10) O1 0.0212(11) 0.0372(12) 0.0402(13) -0.0007(10) -0.0072(10) 0.0084(9) O2 0.0239(12) 0.0661(17) 0.0673(18) -0.0424(15) -0.0075(12) 0.0058(12) O3 0.0565(17) 0.0369(14) 0.0648(18) 0.0125(13) -0.0313(14) 0.0023(12) C58 0.0238(16) 0.0417(18) 0.0233(16) -0.0067(14) -0.0039(13) 0.0134(14) Cl1 0.0420(5) 0.0551(6) 0.0386(5) -0.0011(4) -0.0111(4) -0.0051(4) Cl2 0.0601(6) 0.0616(6) 0.0570(6) -0.0271(5) -0.0286(5) 0.0209(5) C59 0.057(3) 0.041(2) 0.080(3) 0.019(2) -0.034(2) -0.0016(19) C60 0.059(3) 0.044(2) 0.078(3) 0.001(2) -0.036(2) 0.014(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.036(3) . ? Au1 P1 2.2929(7) . ? P1 C40 1.815(3) . ? P1 C34 1.817(3) . ? P1 C28 1.823(3) . ? P2 C46 1.828(3) . ? P2 C52 1.830(3) . ? P2 C33 1.840(3) . ? N1 C1 1.357(3) . ? N1 C2 1.388(3) . ? N1 C4 1.446(3) . ? N2 C1 1.349(3) . ? N2 C3 1.376(3) . ? N2 C16 1.448(3) . ? C2 C3 1.342(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C9 1.399(4) . ? C4 C5 1.405(4) . ? C5 C6 1.395(4) . ? C5 C10 1.513(4) . ? C6 C7 1.376(4) . ? C6 H6 0.9500 . ? C7 C8 1.380(4) . ? C7 H7 0.9500 . ? C8 C9 1.394(4) . ? C8 H8 0.9500 . ? C9 C13 1.522(4) . ? C10 C11 1.531(4) . ? C10 C12 1.531(4) . ? C10 H10 1.0000 . ? 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 C14 1.524(4) . ? C13 C15 1.528(4) . ? C13 H13 1.0000 . ? 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 C17 1.395(4) . ? C16 C21 1.402(4) . ? C17 C18 1.395(4) . ? C17 C22 1.512(4) . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.380(4) . ? C19 H19 0.9500 . ? C20 C21 1.394(4) . ? C20 H20 0.9500 . ? C21 C25 1.513(4) . ? C22 C24 1.528(4) . ? C22 C23 1.532(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.525(5) . ? C25 C26 1.527(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.395(4) . ? C28 C33 1.404(4) . ? C29 C30 1.384(4) . ? C29 H29 0.9500 . ? C30 C31 1.387(4) . ? C30 H30 0.9500 . ? C31 C32 1.382(4) . ? C31 H31 0.9500 . ? C32 C33 1.399(4) . ? C32 H32 0.9500 . ? C39 C38 1.395(4) . ? C39 C34 1.395(4) . ? C39 H39 0.9500 . ? C34 C35 1.395(4) . ? C35 C36 1.388(4) . ? C35 H35 0.9500 . ? C36 C37 1.384(4) . ? C36 H36 0.9500 . ? C37 C38 1.380(4) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C40 C45 1.387(4) . ? C40 C41 1.397(4) . ? C41 C42 1.385(4) . ? C41 H41 0.9500 . ? C42 C43 1.384(4) . ? C42 H42 0.9500 . ? C43 C44 1.373(4) . ? C43 H43 0.9500 . ? C44 C45 1.392(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.394(4) . ? C46 C51 1.394(4) . ? C47 C48 1.390(4) . ? C47 H47 0.9500 . ? C48 C49 1.380(5) . ? C48 H48 0.9500 . ? C49 C50 1.381(5) . ? C49 H49 0.9500 . ? C50 C51 1.385(4) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C53 1.392(4) . ? C52 C57 1.394(4) . ? C53 C54 1.388(4) . ? C53 H53 0.9500 . ? C54 C55 1.382(5) . ? C54 H54 0.9500 . ? C55 C56 1.374(5) . ? C55 H55 0.9500 . ? C56 C57 1.379(5) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? S1 O2 1.432(2) . ? S1 O1 1.439(2) . ? S1 O3 1.444(3) . ? S1 C58 1.805(3) . ? F1 C58 1.336(4) . ? F2 C58 1.332(3) . ? F3 C58 1.340(3) . ? Cl1 C59 1.821(4) . ? Cl2 C60 1.781(4) . ? C59 C60 1.471(6) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 168.27(7) . . ? C40 P1 C34 106.32(12) . . ? C40 P1 C28 105.04(12) . . ? C34 P1 C28 105.69(12) . . ? C40 P1 Au1 110.97(9) . . ? C34 P1 Au1 109.14(9) . . ? C28 P1 Au1 118.90(9) . . ? C46 P2 C52 104.28(13) . . ? C46 P2 C33 100.45(12) . . ? C52 P2 C33 103.40(13) . . ? C1 N1 C2 110.8(2) . . ? C1 N1 C4 123.0(2) . . ? C2 N1 C4 126.2(2) . . ? C1 N2 C3 111.1(2) . . ? C1 N2 C16 124.0(2) . . ? C3 N2 C16 124.8(2) . . ? N2 C1 N1 104.5(2) . . ? N2 C1 Au1 130.56(19) . . ? N1 C1 Au1 124.62(19) . . ? C3 C2 N1 106.3(2) . . ? C3 C2 H2 126.9 . . ? N1 C2 H2 126.9 . . ? C2 C3 N2 107.3(2) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C9 C4 C5 123.6(2) . . ? C9 C4 N1 118.4(2) . . ? C5 C4 N1 118.0(2) . . ? C6 C5 C4 116.4(3) . . ? C6 C5 C10 120.0(3) . . ? C4 C5 C10 123.7(2) . . ? C7 C6 C5 121.2(3) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 121.1(3) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 120.6(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 117.1(3) . . ? C8 C9 C13 120.2(3) . . ? C4 C9 C13 122.7(2) . . ? C5 C10 C11 111.4(2) . . ? C5 C10 C12 111.3(2) . . ? C11 C10 C12 110.3(3) . . ? C5 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 110.2(2) . . ? C9 C13 C15 112.1(2) . . ? C14 C13 C15 110.8(3) . . ? C9 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? 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 . . ? C17 C16 C21 123.8(2) . . ? C17 C16 N2 118.7(2) . . ? C21 C16 N2 117.5(2) . . ? C18 C17 C16 116.7(3) . . ? C18 C17 C22 121.1(3) . . ? C16 C17 C22 122.1(2) . . ? C19 C18 C17 121.2(3) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 120.5(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 121.1(3) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C16 116.7(3) . . ? C20 C21 C25 120.9(3) . . ? C16 C21 C25 122.4(2) . . ? C17 C22 C24 111.1(2) . . ? C17 C22 C23 113.2(2) . . ? C24 C22 C23 110.2(3) . . ? C17 C22 H22 107.3 . . ? C24 C22 H22 107.3 . . ? C23 C22 H22 107.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 110.3(3) . . ? C21 C25 C26 111.8(3) . . ? C27 C25 C26 110.6(3) . . ? C21 C25 H25 108.0 . . ? C27 C25 H25 108.0 . . ? C26 C25 H25 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 119.9(2) . . ? C29 C28 P1 119.70(19) . . ? C33 C28 P1 120.44(19) . . ? C30 C29 C28 120.8(2) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.6(3) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C32 C31 C30 120.0(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 121.3(3) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C38 C39 C34 120.0(3) . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? C32 C33 C28 118.4(2) . . ? C32 C33 P2 122.2(2) . . ? C28 C33 P2 119.40(19) . . ? C35 C34 C39 119.8(2) . . ? C35 C34 P1 122.0(2) . . ? C39 C34 P1 118.2(2) . . ? C36 C35 C34 119.7(3) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.1(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.8(3) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 119.5(3) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C45 C40 C41 119.1(2) . . ? C45 C40 P1 122.3(2) . . ? C41 C40 P1 118.6(2) . . ? C42 C41 C40 120.3(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 120.1(3) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 119.9(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.6(3) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C40 C45 C44 120.0(3) . . ? C40 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 C51 118.3(3) . . ? C47 C46 P2 124.5(2) . . ? C51 C46 P2 117.1(2) . . ? C48 C47 C46 120.6(3) . . ? C48 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? C49 C48 C47 120.1(3) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 120.2(3) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C51 119.7(3) . . ? C49 C50 H50 120.1 . . ? C51 C50 H50 120.1 . . ? C50 C51 C46 121.1(3) . . ? C50 C51 H51 119.5 . . ? C46 C51 H51 119.5 . . ? C53 C52 C57 118.2(3) . . ? C53 C52 P2 124.9(2) . . ? C57 C52 P2 117.0(2) . . ? C54 C53 C52 120.5(3) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C55 C54 C53 120.3(3) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C56 C55 C54 119.7(3) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C55 C56 C57 120.3(3) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C56 C57 C52 121.1(3) . . ? C56 C57 H57 119.5 . . ? C52 C57 H57 119.5 . . ? O2 S1 O1 114.61(15) . . ? O2 S1 O3 116.19(17) . . ? O1 S1 O3 115.19(15) . . ? O2 S1 C58 102.31(14) . . ? O1 S1 C58 103.28(14) . . ? O3 S1 C58 102.43(15) . . ? F2 C58 F1 106.4(3) . . ? F2 C58 F3 106.5(2) . . ? F1 C58 F3 105.1(2) . . ? F2 C58 S1 112.5(2) . . ? F1 C58 S1 112.9(2) . . ? F3 C58 S1 112.8(2) . . ? C60 C59 Cl1 111.5(3) . . ? C60 C59 H59A 109.3 . . ? Cl1 C59 H59A 109.3 . . ? C60 C59 H59B 109.3 . . ? Cl1 C59 H59B 109.3 . . ? H59A C59 H59B 108.0 . . ? C59 C60 Cl2 111.2(3) . . ? C59 C60 H60A 109.4 . . ? Cl2 C60 H60A 109.4 . . ? C59 C60 H60B 109.4 . . ? Cl2 C60 H60B 109.4 . . ? H60A C60 H60B 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 C1 Au1 P1 C40 -40.8(4) . . . . ? C1 Au1 P1 C34 76.0(4) . . . . ? C1 Au1 P1 C28 -162.8(4) . . . . ? C3 N2 C1 N1 0.7(3) . . . . ? C16 N2 C1 N1 177.0(2) . . . . ? C3 N2 C1 Au1 -173.4(2) . . . . ? C16 N2 C1 Au1 2.9(4) . . . . ? C2 N1 C1 N2 -0.3(3) . . . . ? C4 N1 C1 N2 179.0(2) . . . . ? C2 N1 C1 Au1 174.20(19) . . . . ? C4 N1 C1 Au1 -6.5(4) . . . . ? P1 Au1 C1 N2 147.8(3) . . . . ? P1 Au1 C1 N1 -25.2(5) . . . . ? C1 N1 C2 C3 -0.2(3) . . . . ? C4 N1 C2 C3 -179.5(2) . . . . ? N1 C2 C3 N2 0.6(3) . . . . ? C1 N2 C3 C2 -0.9(3) . . . . ? C16 N2 C3 C2 -177.1(2) . . . . ? C1 N1 C4 C9 -89.0(3) . . . . ? C2 N1 C4 C9 90.3(3) . . . . ? C1 N1 C4 C5 89.1(3) . . . . ? C2 N1 C4 C5 -91.7(3) . . . . ? C9 C4 C5 C6 3.2(4) . . . . ? N1 C4 C5 C6 -174.8(2) . . . . ? C9 C4 C5 C10 -176.8(2) . . . . ? N1 C4 C5 C10 5.3(4) . . . . ? C4 C5 C6 C7 -2.0(4) . . . . ? C10 C5 C6 C7 177.9(3) . . . . ? C5 C6 C7 C8 -0.4(4) . . . . ? C6 C7 C8 C9 2.0(4) . . . . ? C7 C8 C9 C4 -0.9(4) . . . . ? C7 C8 C9 C13 177.5(3) . . . . ? C5 C4 C9 C8 -1.8(4) . . . . ? N1 C4 C9 C8 176.2(2) . . . . ? C5 C4 C9 C13 179.9(2) . . . . ? N1 C4 C9 C13 -2.2(4) . . . . ? C6 C5 C10 C11 72.2(3) . . . . ? C4 C5 C10 C11 -107.9(3) . . . . ? C6 C5 C10 C12 -51.4(4) . . . . ? C4 C5 C10 C12 128.5(3) . . . . ? C8 C9 C13 C14 -71.9(3) . . . . ? C4 C9 C13 C14 106.5(3) . . . . ? C8 C9 C13 C15 52.0(4) . . . . ? C4 C9 C13 C15 -129.7(3) . . . . ? C1 N2 C16 C17 97.7(3) . . . . ? C3 N2 C16 C17 -86.5(3) . . . . ? C1 N2 C16 C21 -82.3(3) . . . . ? C3 N2 C16 C21 93.5(3) . . . . ? C21 C16 C17 C18 1.5(4) . . . . ? N2 C16 C17 C18 -178.5(2) . . . . ? C21 C16 C17 C22 -179.4(3) . . . . ? N2 C16 C17 C22 0.6(4) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C22 C17 C18 C19 -179.2(3) . . . . ? C17 C18 C19 C20 -0.8(5) . . . . ? C18 C19 C20 C21 0.5(5) . . . . ? C19 C20 C21 C16 0.8(4) . . . . ? C19 C20 C21 C25 -177.2(3) . . . . ? C17 C16 C21 C20 -1.8(4) . . . . ? N2 C16 C21 C20 178.2(2) . . . . ? C17 C16 C21 C25 176.1(3) . . . . ? N2 C16 C21 C25 -3.9(4) . . . . ? C18 C17 C22 C24 87.2(3) . . . . ? C16 C17 C22 C24 -91.9(3) . . . . ? C18 C17 C22 C23 -37.5(4) . . . . ? C16 C17 C22 C23 143.5(3) . . . . ? C20 C21 C25 C27 64.9(4) . . . . ? C16 C21 C25 C27 -113.0(3) . . . . ? C20 C21 C25 C26 -58.6(4) . . . . ? C16 C21 C25 C26 123.5(3) . . . . ? C40 P1 C28 C29 8.6(2) . . . . ? C34 P1 C28 C29 -103.6(2) . . . . ? Au1 P1 C28 C29 133.44(19) . . . . ? C40 P1 C28 C33 -171.5(2) . . . . ? C34 P1 C28 C33 76.3(2) . . . . ? Au1 P1 C28 C33 -46.6(2) . . . . ? C33 C28 C29 C30 0.8(4) . . . . ? P1 C28 C29 C30 -179.3(2) . . . . ? C28 C29 C30 C31 -1.7(4) . . . . ? C29 C30 C31 C32 1.1(4) . . . . ? C30 C31 C32 C33 0.5(4) . . . . ? C31 C32 C33 C28 -1.4(4) . . . . ? C31 C32 C33 P2 175.8(2) . . . . ? C29 C28 C33 C32 0.8(4) . . . . ? P1 C28 C33 C32 -179.2(2) . . . . ? C29 C28 C33 P2 -176.5(2) . . . . ? P1 C28 C33 P2 3.6(3) . . . . ? C46 P2 C33 C32 -25.3(3) . . . . ? C52 P2 C33 C32 82.3(2) . . . . ? C46 P2 C33 C28 151.9(2) . . . . ? C52 P2 C33 C28 -100.6(2) . . . . ? C38 C39 C34 C35 0.5(4) . . . . ? C38 C39 C34 P1 179.6(2) . . . . ? C40 P1 C34 C35 -96.0(2) . . . . ? C28 P1 C34 C35 15.3(3) . . . . ? Au1 P1 C34 C35 144.3(2) . . . . ? C40 P1 C34 C39 85.0(2) . . . . ? C28 P1 C34 C39 -163.7(2) . . . . ? Au1 P1 C34 C39 -34.8(2) . . . . ? C39 C34 C35 C36 -0.1(4) . . . . ? P1 C34 C35 C36 -179.1(2) . . . . ? C34 C35 C36 C37 -0.4(4) . . . . ? C35 C36 C37 C38 0.6(4) . . . . ? C36 C37 C38 C39 -0.2(4) . . . . ? C34 C39 C38 C37 -0.4(4) . . . . ? C34 P1 C40 C45 -1.6(3) . . . . ? C28 P1 C40 C45 -113.3(2) . . . . ? Au1 P1 C40 C45 117.0(2) . . . . ? C34 P1 C40 C41 -178.4(2) . . . . ? C28 P1 C40 C41 69.9(2) . . . . ? Au1 P1 C40 C41 -59.8(2) . . . . ? C45 C40 C41 C42 -0.6(4) . . . . ? P1 C40 C41 C42 176.3(2) . . . . ? C40 C41 C42 C43 -0.2(4) . . . . ? C41 C42 C43 C44 1.1(5) . . . . ? C42 C43 C44 C45 -1.2(5) . . . . ? C41 C40 C45 C44 0.5(4) . . . . ? P1 C40 C45 C44 -176.3(2) . . . . ? C43 C44 C45 C40 0.4(4) . . . . ? C52 P2 C46 C47 7.4(3) . . . . ? C33 P2 C46 C47 114.3(2) . . . . ? C52 P2 C46 C51 -176.4(2) . . . . ? C33 P2 C46 C51 -69.5(2) . . . . ? C51 C46 C47 C48 1.2(4) . . . . ? P2 C46 C47 C48 177.3(2) . . . . ? C46 C47 C48 C49 0.8(4) . . . . ? C47 C48 C49 C50 -1.6(4) . . . . ? C48 C49 C50 C51 0.4(4) . . . . ? C49 C50 C51 C46 1.7(4) . . . . ? C47 C46 C51 C50 -2.4(4) . . . . ? P2 C46 C51 C50 -178.9(2) . . . . ? C46 P2 C52 C53 77.5(3) . . . . ? C33 P2 C52 C53 -27.2(3) . . . . ? C46 P2 C52 C57 -103.9(2) . . . . ? C33 P2 C52 C57 151.4(2) . . . . ? C57 C52 C53 C54 0.4(4) . . . . ? P2 C52 C53 C54 179.0(2) . . . . ? C52 C53 C54 C55 0.0(5) . . . . ? C53 C54 C55 C56 -0.3(5) . . . . ? C54 C55 C56 C57 0.1(5) . . . . ? C55 C56 C57 C52 0.3(5) . . . . ? C53 C52 C57 C56 -0.6(4) . . . . ? P2 C52 C57 C56 -179.3(3) . . . . ? O2 S1 C58 F2 59.0(3) . . . . ? O1 S1 C58 F2 178.3(2) . . . . ? O3 S1 C58 F2 -61.7(3) . . . . ? O2 S1 C58 F1 -61.5(2) . . . . ? O1 S1 C58 F1 57.8(2) . . . . ? O3 S1 C58 F1 177.8(2) . . . . ? O2 S1 C58 F3 179.5(2) . . . . ? O1 S1 C58 F3 -61.2(2) . . . . ? O3 S1 C58 F3 58.8(2) . . . . ? Cl1 C59 C60 Cl2 71.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.049 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.076 _iucr_refine_instructions_details ; TITL c294 in P1 New: P-1 CELL 0.71073 11.3839 12.7921 20.0475 81.878 76.444 89.880 ZERR 2.00 0.0002 0.0002 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H AU CL F N O P S UNIT 120 128 2 4 6 4 6 4 2 MERG 2 OMIT -2.00 51.00 OMIT -1 7 2 OMIT -3 2 1 OMIT 2 -2 4 FMAP 2 PLAN 20 SIZE 0.08 0.08 0.10 ACTA LIST 4 BOND $H CONF L.S. 15 TEMP -143.00 WGHT 0.025600 2.785600 FVAR 1.74097 AU1 3 0.145165 0.195026 0.226799 11.00000 0.01724 0.01291 = 0.01201 -0.00014 -0.00215 0.00168 P1 8 0.086709 0.121978 0.341201 11.00000 0.01577 0.01252 = 0.01248 -0.00021 -0.00267 0.00124 P2 8 0.233123 0.341085 0.334071 11.00000 0.02350 0.01660 = 0.01828 -0.00332 0.00154 -0.00373 N1 6 0.240069 0.159025 0.078270 11.00000 0.02263 0.01355 = 0.01370 -0.00130 -0.00396 0.00022 N2 6 0.177003 0.316653 0.078934 11.00000 0.02198 0.01450 = 0.01434 0.00056 -0.00383 0.00148 C1 1 0.193059 0.229062 0.121500 11.00000 0.01746 0.01503 = 0.01717 -0.00233 -0.00508 0.00098 C2 1 0.252263 0.202967 0.009545 11.00000 0.03115 0.01902 = 0.01193 -0.00187 -0.00315 -0.00086 AFIX 43 H2 2 0.283108 0.169930 -0.030277 11.00000 -1.20000 AFIX 0 C3 1 0.211765 0.301482 0.010576 11.00000 0.02926 0.01929 = 0.01079 0.00180 -0.00384 -0.00166 AFIX 43 H3 2 0.207835 0.351456 -0.028618 11.00000 -1.20000 AFIX 0 C4 1 0.273101 0.053832 0.102712 11.00000 0.02766 0.01314 = 0.01486 -0.00285 -0.00448 0.00401 C5 1 0.184225 -0.027711 0.117824 11.00000 0.03093 0.01673 = 0.01409 -0.00426 -0.00373 0.00064 C6 1 0.216274 -0.126116 0.146790 11.00000 0.03881 0.01536 = 0.02171 -0.00184 -0.00278 -0.00008 AFIX 43 H6 2 0.158291 -0.183088 0.159267 11.00000 -1.20000 AFIX 0 C7 1 0.330330 -0.142204 0.157627 11.00000 0.04183 0.01566 = 0.02156 -0.00019 -0.00374 0.00869 AFIX 43 H7 2 0.349526 -0.209913 0.177750 11.00000 -1.20000 AFIX 0 C8 1 0.417288 -0.061618 0.139752 11.00000 0.02860 0.02729 = 0.02063 -0.00683 -0.00670 0.01114 AFIX 43 H8 2 0.496204 -0.075017 0.146341 11.00000 -1.20000 AFIX 0 C9 1 0.390303 0.039280 0.112106 11.00000 0.02587 0.02104 = 0.01554 -0.00789 -0.00229 0.00316 C10 1 0.059439 -0.013459 0.104286 11.00000 0.03064 0.02018 = 0.02492 0.00002 -0.00789 -0.00609 AFIX 13 H10 2 0.059039 0.057244 0.075767 11.00000 -1.20000 AFIX 0 C11 1 -0.037186 -0.015079 0.171954 11.00000 0.02704 0.05321 = 0.03257 -0.00655 -0.00436 -0.00705 AFIX 33 H11A 2 -0.116733 -0.005290 0.161519 11.00000 -1.50000 H11B 2 -0.019515 0.042108 0.196262 11.00000 -1.50000 H11C 2 -0.037168 -0.083092 0.201402 11.00000 -1.50000 AFIX 0 C12 1 0.028964 -0.097485 0.063102 11.00000 0.05554 0.02809 = 0.03505 -0.00396 -0.02371 -0.00351 AFIX 33 H12A 2 -0.051953 -0.086091 0.054905 11.00000 -1.50000 H12B 2 0.030922 -0.167799 0.089492 11.00000 -1.50000 H12C 2 0.088417 -0.092351 0.018548 11.00000 -1.50000 AFIX 0 C13 1 0.485204 0.128747 0.095250 11.00000 0.02424 0.02306 = 0.02469 -0.00491 -0.00596 0.00029 AFIX 13 H13 2 0.453736 0.190454 0.068909 11.00000 -1.20000 AFIX 0 C14 1 0.504815 0.162441 0.161879 11.00000 0.03188 0.04907 = 0.03215 -0.01735 -0.00128 -0.00697 AFIX 33 H14A 2 0.565846 0.220182 0.150398 11.00000 -1.50000 H14B 2 0.532616 0.102339 0.189580 11.00000 -1.50000 H14C 2 0.428593 0.186469 0.188503 11.00000 -1.50000 AFIX 0 C15 1 0.604458 0.098917 0.049860 11.00000 0.03208 0.03791 = 0.03490 -0.01202 0.00468 -0.00456 AFIX 33 H15A 2 0.662770 0.158585 0.040037 11.00000 -1.50000 H15B 2 0.590670 0.081440 0.006204 11.00000 -1.50000 H15C 2 0.636440 0.037589 0.074219 11.00000 -1.50000 AFIX 0 C16 1 0.122931 0.411327 0.102712 11.00000 0.02598 0.01444 = 0.01219 0.00088 -0.00290 0.00391 C17 1 0.198704 0.494916 0.106229 11.00000 0.02594 0.01913 = 0.01485 -0.00013 -0.00375 0.00269 C18 1 0.142746 0.583542 0.130984 11.00000 0.03378 0.01776 = 0.02314 -0.00449 -0.00295 0.00134 AFIX 43 H18 2 0.191051 0.642184 0.134302 11.00000 -1.20000 AFIX 0 C19 1 0.018134 0.587568 0.150795 11.00000 0.03536 0.02167 = 0.02466 -0.00190 -0.00100 0.00990 AFIX 43 H19 2 -0.018056 0.648365 0.168078 11.00000 -1.20000 AFIX 0 C20 1 -0.053975 0.503922 0.145635 11.00000 0.02386 0.02773 = 0.02501 0.00316 -0.00273 0.00804 AFIX 43 H20 2 -0.139403 0.508154 0.159141 11.00000 -1.20000 AFIX 0 C21 1 -0.003604 0.413299 0.120937 11.00000 0.02447 0.02199 = 0.01842 0.00404 -0.00600 0.00215 C22 1 0.334961 0.490018 0.085431 11.00000 0.02612 0.02077 = 0.02392 -0.00792 0.00074 -0.00052 AFIX 13 H22 2 0.354959 0.438573 0.051531 11.00000 -1.20000 AFIX 0 C23 1 0.397150 0.596051 0.049516 11.00000 0.03122 0.02993 = 0.02676 -0.00075 0.00167 -0.00461 AFIX 33 H23A 2 0.484875 0.587920 0.037134 11.00000 -1.50000 H23B 2 0.377605 0.648952 0.081013 11.00000 -1.50000 H23C 2 0.368739 0.619088 0.007435 11.00000 -1.50000 AFIX 0 C24 1 0.386102 0.448178 0.147712 11.00000 0.02681 0.03408 = 0.04270 0.00926 -0.00913 -0.00281 AFIX 33 H24A 2 0.474292 0.445494 0.132845 11.00000 -1.50000 H24B 2 0.352117 0.377051 0.167209 11.00000 -1.50000 H24C 2 0.364694 0.495154 0.183025 11.00000 -1.50000 AFIX 0 C25 1 -0.083096 0.323903 0.112308 11.00000 0.02281 0.02665 = 0.03183 0.00143 -0.00862 0.00090 AFIX 13 H25 2 -0.029611 0.265758 0.096380 11.00000 -1.20000 AFIX 0 C26 1 -0.170753 0.279730 0.180601 11.00000 0.03944 0.05146 = 0.03982 0.00885 -0.00818 -0.01472 AFIX 33 H26A 2 -0.220197 0.221880 0.173069 11.00000 -1.50000 H26B 2 -0.223324 0.335762 0.197662 11.00000 -1.50000 H26C 2 -0.124984 0.253205 0.214890 11.00000 -1.50000 AFIX 0 C27 1 -0.151715 0.360475 0.056833 11.00000 0.06343 0.04822 = 0.04873 0.00747 -0.03306 -0.01408 AFIX 33 H27A 2 -0.202343 0.301765 0.051545 11.00000 -1.50000 H27B 2 -0.093970 0.384064 0.012638 11.00000 -1.50000 H27C 2 -0.202936 0.419102 0.070657 11.00000 -1.50000 AFIX 0 C28 1 0.034184 0.208378 0.406320 11.00000 0.01713 0.01372 = 0.01412 -0.00028 -0.00399 0.00324 C29 1 -0.071267 0.181024 0.457782 11.00000 0.01937 0.01525 = 0.01587 0.00112 -0.00388 0.00043 AFIX 43 H29 2 -0.114462 0.117132 0.458799 11.00000 -1.20000 AFIX 0 C30 1 -0.113672 0.245867 0.507356 11.00000 0.02179 0.02242 = 0.01504 0.00132 0.00176 0.00550 AFIX 43 H30 2 -0.186710 0.227525 0.541443 11.00000 -1.20000 AFIX 0 C31 1 -0.048977 0.337772 0.507011 11.00000 0.02941 0.02036 = 0.01524 -0.00454 -0.00049 0.00824 AFIX 43 H31 2 -0.076980 0.381947 0.541398 11.00000 -1.20000 AFIX 0 C32 1 0.056211 0.365131 0.456669 11.00000 0.02781 0.01565 = 0.01916 -0.00110 -0.00357 0.00096 AFIX 43 H32 2 0.100172 0.427966 0.457123 11.00000 -1.20000 AFIX 0 C39 1 0.290306 0.001628 0.317174 11.00000 0.02053 0.01889 = 0.02135 -0.00357 -0.00161 0.00140 AFIX 43 H39 2 0.276378 0.003491 0.272121 11.00000 -1.20000 AFIX 0 C33 1 0.099194 0.302093 0.405063 11.00000 0.02226 0.01570 = 0.01482 -0.00045 -0.00239 0.00162 C34 1 0.212537 0.052522 0.366275 11.00000 0.01496 0.01194 = 0.02105 0.00041 -0.00300 -0.00068 C35 1 0.233865 0.050259 0.432204 11.00000 0.02074 0.01668 = 0.01996 -0.00096 -0.00406 0.00001 AFIX 43 H35 2 0.181270 0.084861 0.465815 11.00000 -1.20000 AFIX 0 C36 1 0.332225 -0.002747 0.448481 11.00000 0.02491 0.02550 = 0.02692 0.00549 -0.01243 -0.00227 AFIX 43 H36 2 0.347334 -0.004040 0.493222 11.00000 -1.20000 AFIX 0 C37 1 0.408323 -0.053714 0.399656 11.00000 0.01780 0.02137 = 0.03995 0.00663 -0.01006 0.00243 AFIX 43 H37 2 0.475052 -0.090354 0.411340 11.00000 -1.20000 AFIX 0 C38 1 0.388502 -0.051992 0.334199 11.00000 0.01917 0.02008 = 0.03378 -0.00227 -0.00085 0.00449 AFIX 43 H38 2 0.441345 -0.087067 0.300968 11.00000 -1.20000 AFIX 0 C40 1 -0.034726 0.023921 0.354683 11.00000 0.01850 0.01737 = 0.01122 -0.00176 -0.00181 -0.00179 C41 1 -0.142853 0.055581 0.337662 11.00000 0.02193 0.02435 = 0.02398 0.00388 -0.00688 0.00042 AFIX 43 H41 2 -0.153135 0.127909 0.322061 11.00000 -1.20000 AFIX 0 C42 1 -0.235127 -0.017923 0.343416 11.00000 0.02253 0.04208 = 0.02612 0.00127 -0.00900 -0.00480 AFIX 43 H42 2 -0.308540 0.004119 0.331887 11.00000 -1.20000 AFIX 0 C43 1 -0.220568 -0.123432 0.365931 11.00000 0.02768 0.03332 = 0.02499 -0.00298 -0.00345 -0.01380 AFIX 43 H43 2 -0.283360 -0.174008 0.369117 11.00000 -1.20000 AFIX 0 C44 1 -0.115151 -0.154861 0.383659 11.00000 0.03412 0.01910 = 0.03052 -0.00117 -0.00562 -0.00657 AFIX 43 H44 2 -0.105959 -0.227138 0.399921 11.00000 -1.20000 AFIX 0 C45 1 -0.021618 -0.081784 0.378020 11.00000 0.02463 0.01871 = 0.01985 -0.00243 -0.00517 0.00198 AFIX 43 H45 2 0.051161 -0.104333 0.390157 11.00000 -1.20000 AFIX 0 C46 1 0.232209 0.484657 0.330566 11.00000 0.02740 0.01942 = 0.01536 -0.00183 0.00574 -0.00570 C47 1 0.321006 0.544887 0.346538 11.00000 0.02454 0.02453 = 0.02509 -0.00300 0.00422 -0.00322 AFIX 43 H47 2 0.385837 0.510848 0.362257 11.00000 -1.20000 AFIX 0 C48 1 0.315513 0.654324 0.339666 11.00000 0.03424 0.02428 = 0.02777 -0.00667 0.00508 -0.00981 AFIX 43 H48 2 0.376991 0.694783 0.350118 11.00000 -1.20000 AFIX 0 C49 1 0.220823 0.704270 0.317668 11.00000 0.04453 0.01715 = 0.01963 -0.00021 0.00771 -0.00409 AFIX 43 H49 2 0.216191 0.778936 0.314132 11.00000 -1.20000 AFIX 0 C50 1 0.132785 0.646033 0.300782 11.00000 0.04257 0.02534 = 0.01990 0.00256 -0.00254 0.00266 AFIX 43 H50 2 0.067895 0.680522 0.285395 11.00000 -1.20000 AFIX 0 C51 1 0.139500 0.537124 0.306377 11.00000 0.03905 0.02299 = 0.02271 -0.00086 -0.00624 -0.00499 AFIX 43 H51 2 0.079967 0.497525 0.293523 11.00000 -1.20000 AFIX 0 C52 1 0.359318 0.300948 0.373051 11.00000 0.02313 0.01476 = 0.03036 -0.00434 -0.00009 -0.00471 C53 1 0.356073 0.293094 0.443433 11.00000 0.02685 0.02568 = 0.02821 -0.00290 -0.00148 -0.00074 AFIX 43 H53 2 0.284746 0.310323 0.474808 11.00000 -1.20000 AFIX 0 C54 1 0.456285 0.260277 0.468093 11.00000 0.03387 0.03372 = 0.03223 0.00222 -0.00887 -0.00076 AFIX 43 H54 2 0.453150 0.255137 0.516222 11.00000 -1.20000 AFIX 0 C55 1 0.560644 0.235031 0.422983 11.00000 0.02745 0.03221 = 0.05027 -0.00243 -0.01017 0.00132 AFIX 43 H55 2 0.629245 0.212889 0.439966 11.00000 -1.20000 AFIX 0 C56 1 0.564640 0.242129 0.353449 11.00000 0.02477 0.04173 = 0.04842 -0.01175 -0.00012 0.00535 AFIX 43 H56 2 0.636194 0.224717 0.322335 11.00000 -1.20000 AFIX 0 C57 1 0.465299 0.274399 0.328616 11.00000 0.02871 0.03499 = 0.02895 -0.00924 0.00122 0.00148 AFIX 43 H57 2 0.469118 0.278614 0.280459 11.00000 -1.20000 AFIX 0 S1 9 0.683114 0.760670 0.218838 11.00000 0.02197 0.03107 = 0.04041 -0.00724 -0.00946 0.00787 F1 5 0.602532 0.562991 0.250244 11.00000 0.05000 0.04141 = 0.03457 0.00055 -0.01009 -0.00681 F2 5 0.502148 0.663041 0.190805 11.00000 0.03084 0.05439 = 0.05990 -0.02353 -0.02212 0.01157 F3 5 0.675974 0.610474 0.142572 11.00000 0.04577 0.05965 = 0.02885 -0.01568 0.00017 0.01143 O1 7 0.798111 0.723766 0.228807 11.00000 0.02118 0.03715 = 0.04017 -0.00074 -0.00723 0.00844 O2 7 0.600302 0.782779 0.280547 11.00000 0.02393 0.06608 = 0.06734 -0.04241 -0.00745 0.00584 O3 7 0.688509 0.835506 0.157031 11.00000 0.05654 0.03689 = 0.06479 0.01249 -0.03131 0.00229 C58 1 0.613029 0.645353 0.199987 11.00000 0.02378 0.04169 = 0.02328 -0.00674 -0.00390 0.01335 CL1 4 0.845736 0.392011 0.338363 11.00000 0.04203 0.05513 = 0.03862 -0.00107 -0.01114 -0.00509 CL2 4 0.670211 0.463253 0.486133 11.00000 0.06012 0.06162 = 0.05703 -0.02712 -0.02861 0.02091 C59 1 0.794626 0.523080 0.354642 11.00000 0.05686 0.04059 = 0.08034 0.01928 -0.03376 -0.00163 AFIX 23 H59A 2 0.850728 0.555971 0.377214 11.00000 -1.20000 H59B 2 0.795997 0.567909 0.309951 11.00000 -1.20000 AFIX 0 C60 1 0.671561 0.518341 0.399263 11.00000 0.05892 0.04364 = 0.07847 0.00126 -0.03579 0.01414 AFIX 23 H60A 2 0.618163 0.474774 0.380893 11.00000 -1.20000 H60B 2 0.639645 0.590434 0.398641 11.00000 -1.20000 HKLF 4 REM c294 in P1 New: P-1 REM R1 = 0.0228 for 9710 Fo > 4sig(Fo) and 0.0261 for all 10415 data REM 667 parameters refined using 0 restraints END WGHT 0.0256 2.6640 REM Highest difference peak 1.049, deepest hole -0.730, 1-sigma level 0.076 Q1 1 0.7995 0.5628 0.4182 11.00000 0.05 1.05 Q2 1 0.1824 0.2583 0.2286 11.00000 0.05 0.97 Q3 1 0.6739 0.7666 0.2607 11.00000 0.05 0.80 Q4 1 0.6631 0.8586 0.2058 11.00000 0.05 0.69 Q5 1 0.1153 0.1169 0.2429 11.00000 0.05 0.64 Q6 1 0.1059 0.2360 0.2620 11.00000 0.05 0.58 Q7 1 0.5953 0.7259 0.3178 11.00000 0.05 0.56 Q8 1 0.2406 0.1888 0.2254 11.00000 0.05 0.55 Q9 1 0.6479 0.7020 0.2131 11.00000 0.05 0.54 Q10 1 0.0486 0.2157 0.2304 11.00000 0.05 0.51 Q11 1 0.1871 0.1549 0.1964 11.00000 0.05 0.50 Q12 1 0.5685 0.4189 0.3214 11.00000 0.05 0.48 Q13 1 0.1145 0.1836 0.3036 11.00000 0.05 0.47 Q14 1 0.1362 0.2014 0.2967 11.00000 0.05 0.41 Q15 1 0.0942 0.1559 0.1962 11.00000 0.05 0.41 Q16 1 0.6966 0.6787 0.1349 11.00000 0.05 0.40 Q17 1 0.0392 0.1596 0.2709 11.00000 0.05 0.40 Q18 1 0.2394 0.2390 0.1737 11.00000 0.05 0.40 Q19 1 0.0674 0.2717 0.2234 11.00000 0.05 0.39 Q20 1 0.7570 0.4767 0.3144 11.00000 0.05 0.39 ; _database_code_depnum_ccdc_archive 'CCDC 948445' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_con212-renso _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H64 Au Cl2 F3 N2 O3 P2 S' _chemical_formula_weight 1267.99 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4745(10) _cell_length_b 12.6486(11) _cell_length_c 19.5252(16) _cell_angle_alpha 85.6100(10) _cell_angle_beta 79.8940(10) _cell_angle_gamma 89.4190(10) _cell_volume 2781.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9891 _cell_measurement_theta_min 4.495 _cell_measurement_theta_max 56.297 _exptl_crystal_description tablet _exptl_crystal_colour pale-green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 2.892 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.3909 _exptl_absorpt_correction_T_max 0.6548 _exptl_absorpt_process_details SADABS _exptl_special_details ; There is a residual peak of electron density about 7 \%A near the gold atom, which has the same distance to the carbon of the NHC ligand and opposite bond distances to the phosphorus atoms. This peak may correspond with a slight disorder of the gold centre with an approximately 95: 5 ratio. The triflate anion is also disordered. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker p4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28157 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10289 _reflns_number_gt 9512 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0104P)^2^+53.7368P] 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 10289 _refine_ls_number_parameters 642 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 1.174 _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 0.70860(3) 0.76271(3) 0.728076(18) 0.02497(11) Uani 1 1 d . . . P1 P 0.7361(2) 0.84198(17) 0.82814(11) 0.0210(5) Uani 1 1 d . . . P2 P 0.5855(2) 0.62735(17) 0.83333(11) 0.0211(5) Uani 1 1 d . . . N1 N 0.7091(6) 0.8341(5) 0.5781(4) 0.0200(15) Uani 1 1 d . . . N2 N 0.7645(6) 0.6693(5) 0.5849(3) 0.0177(14) Uani 1 1 d . . . C1 C 0.7274(7) 0.7516(6) 0.6222(4) 0.0180(17) Uani 1 1 d . . . C2 C 0.7180(8) 0.8037(7) 0.5052(4) 0.0234(19) Uani 1 1 d . . . H2A H 0.7652 0.8560 0.4715 0.028 Uiso 1 1 calc R . . H2B H 0.6387 0.7964 0.4925 0.028 Uiso 1 1 calc R . . C3 C 0.7809(8) 0.6970(7) 0.5086(4) 0.0236(19) Uani 1 1 d . . . H3A H 0.7434 0.6437 0.4847 0.028 Uiso 1 1 calc R . . H3B H 0.8658 0.7036 0.4876 0.028 Uiso 1 1 calc R . . C4 C 0.6493(7) 0.9304(6) 0.5991(4) 0.0189(17) Uani 1 1 d . . . C5 C 0.7162(8) 1.0234(7) 0.5935(5) 0.0233(19) Uani 1 1 d . . . C6 C 0.6576(9) 1.1157(7) 0.6114(5) 0.030(2) Uani 1 1 d . . . H6 H 0.7011 1.1801 0.6074 0.036 Uiso 1 1 calc R . . C7 C 0.5366(9) 1.1163(7) 0.6349(5) 0.030(2) Uani 1 1 d . . . H7 H 0.4980 1.1806 0.6474 0.036 Uiso 1 1 calc R . . C8 C 0.4724(8) 1.0243(7) 0.6403(5) 0.030(2) Uani 1 1 d . . . H8 H 0.3896 1.0257 0.6572 0.035 Uiso 1 1 calc R . . C9 C 0.5259(8) 0.9285(7) 0.6216(5) 0.0253(19) Uani 1 1 d . . . C10 C 0.8500(8) 1.0225(7) 0.5688(5) 0.027(2) Uani 1 1 d . . . H10 H 0.8674 0.9678 0.5341 0.032 Uiso 1 1 calc R . . C11 C 0.8972(9) 1.1291(7) 0.5318(5) 0.034(2) Uani 1 1 d . . . H11A H 0.9830 1.1243 0.5162 0.050 Uiso 1 1 calc R . . H11B H 0.8803 1.1849 0.5643 0.050 Uiso 1 1 calc R . . H11C H 0.8586 1.1461 0.4914 0.050 Uiso 1 1 calc R . . C12 C 0.9138(9) 0.9893(8) 0.6291(6) 0.038(2) Uani 1 1 d . . . H12A H 0.9993 0.9881 0.6121 0.057 Uiso 1 1 calc R . . H12B H 0.8869 0.9184 0.6491 0.057 Uiso 1 1 calc R . . H12C H 0.8961 1.0400 0.6650 0.057 Uiso 1 1 calc R . . C13 C 0.4515(8) 0.8308(7) 0.6251(5) 0.029(2) Uani 1 1 d . . . H13 H 0.5061 0.7706 0.6120 0.035 Uiso 1 1 calc R . . C14 C 0.3664(11) 0.8423(11) 0.5730(7) 0.053(3) Uani 1 1 d . . . H14A H 0.3198 0.7770 0.5760 0.079 Uiso 1 1 calc R . . H14B H 0.4117 0.8551 0.5256 0.079 Uiso 1 1 calc R . . H14C H 0.3131 0.9021 0.5838 0.079 Uiso 1 1 calc R . . C15 C 0.3846(10) 0.8027(9) 0.6989(6) 0.040(3) Uani 1 1 d . . . H15A H 0.3377 0.7382 0.6995 0.061 Uiso 1 1 calc R . . H15B H 0.3318 0.8612 0.7138 0.061 Uiso 1 1 calc R . . H15C H 0.4412 0.7908 0.7309 0.061 Uiso 1 1 calc R . . C16 C 0.7945(8) 0.5656(6) 0.6118(4) 0.0182(17) Uani 1 1 d . . . C17 C 0.7080(8) 0.4869(6) 0.6243(4) 0.0205(18) Uani 1 1 d . . . C18 C 0.7357(8) 0.3879(7) 0.6539(4) 0.0219(18) Uani 1 1 d . . . H18 H 0.6765 0.3346 0.6665 0.026 Uiso 1 1 calc R . . C19 C 0.8508(8) 0.3679(7) 0.6650(4) 0.0227(19) Uani 1 1 d . . . H19 H 0.8694 0.3001 0.6846 0.027 Uiso 1 1 calc R . . C20 C 0.9375(8) 0.4434(6) 0.6484(4) 0.0205(18) Uani 1 1 d . . . H20 H 1.0161 0.4262 0.6544 0.025 Uiso 1 1 calc R . . C21 C 0.9119(7) 0.5462(6) 0.6226(4) 0.0192(17) Uani 1 1 d . . . C22 C 0.5849(8) 0.5036(7) 0.6060(4) 0.0214(18) Uani 1 1 d . . . H22 H 0.5856 0.5730 0.5777 0.026 Uiso 1 1 calc R . . C23 C 0.4892(9) 0.5091(9) 0.6699(5) 0.036(2) Uani 1 1 d . . . H23A H 0.4123 0.5204 0.6553 0.054 Uiso 1 1 calc R . . H23B H 0.5061 0.5679 0.6965 0.054 Uiso 1 1 calc R . . H23C H 0.4873 0.4424 0.6991 0.054 Uiso 1 1 calc R . . C24 C 0.5575(8) 0.4166(7) 0.5604(5) 0.029(2) Uani 1 1 d . . . H24A H 0.4786 0.4283 0.5486 0.044 Uiso 1 1 calc R . . H24B H 0.5598 0.3472 0.5861 0.044 Uiso 1 1 calc R . . H24C H 0.6166 0.4189 0.5175 0.044 Uiso 1 1 calc R . . C25 C 1.0079(8) 0.6287(7) 0.6061(5) 0.0233(18) Uani 1 1 d . . . H25 H 0.9733 0.6949 0.5866 0.028 Uiso 1 1 calc R . . C26 C 1.0539(10) 0.6548(9) 0.6722(6) 0.042(3) Uani 1 1 d . . . H26A H 1.1158 0.7092 0.6600 0.063 Uiso 1 1 calc R . . H26B H 1.0867 0.5906 0.6929 0.063 Uiso 1 1 calc R . . H26C H 0.9886 0.6812 0.7058 0.063 Uiso 1 1 calc R . . C27 C 1.1113(9) 0.5946(7) 0.5511(5) 0.032(2) Uani 1 1 d . . . H27A H 1.1715 0.6507 0.5414 0.047 Uiso 1 1 calc R . . H27B H 1.0822 0.5823 0.5081 0.047 Uiso 1 1 calc R . . H27C H 1.1460 0.5292 0.5687 0.047 Uiso 1 1 calc R . . C28 C 0.6179(7) 0.8076(7) 0.9014(4) 0.0208(18) Uani 1 1 d . . . C29 C 0.5954(9) 0.8744(7) 0.9576(5) 0.028(2) Uani 1 1 d . . . H29 H 0.6448 0.9342 0.9579 0.034 Uiso 1 1 calc R . . C39 C 0.8783(10) 0.7633(9) 0.9241(6) 0.045(3) Uani 1 1 d . . . H39 H 0.8065 0.7536 0.9566 0.054 Uiso 1 1 calc R . . C30 C 0.5016(9) 0.8524(7) 1.0119(5) 0.030(2) Uani 1 1 d . . . H30 H 0.4871 0.8966 1.0497 0.036 Uiso 1 1 calc R . . C31 C 0.4298(9) 0.7669(7) 1.0111(5) 0.030(2) Uani 1 1 d . . . H31 H 0.3636 0.7539 1.0474 0.036 Uiso 1 1 calc R . . C32 C 0.4526(8) 0.6992(7) 0.9578(5) 0.0261(19) Uani 1 1 d . . . H32 H 0.4029 0.6394 0.9586 0.031 Uiso 1 1 calc R . . C33 C 0.5481(8) 0.7179(7) 0.9029(4) 0.0216(18) Uani 1 1 d . . . C34 C 0.8735(9) 0.8052(7) 0.8578(5) 0.029(2) Uani 1 1 d . . . C35 C 0.9796(8) 0.8274(10) 0.8117(5) 0.042(3) Uani 1 1 d . . . H35 H 0.9797 0.8638 0.7673 0.051 Uiso 1 1 calc R . . C36 C 1.0856(10) 0.7947(11) 0.8327(6) 0.051(3) Uani 1 1 d . . . H36 H 1.1573 0.8013 0.7998 0.061 Uiso 1 1 calc R . . C37 C 1.0891(11) 0.7533(9) 0.8993(7) 0.050(3) Uani 1 1 d . . . H37 H 1.1627 0.7376 0.9136 0.060 Uiso 1 1 calc R . . C38 C 0.9837(11) 0.7346(10) 0.9454(7) 0.055(3) Uani 1 1 d . . . H38 H 0.9839 0.7025 0.9910 0.066 Uiso 1 1 calc R . . C40 C 0.7325(9) 0.9865(7) 0.8212(5) 0.029(2) Uani 1 1 d . . . C41 C 0.6409(12) 1.0354(8) 0.7941(5) 0.044(3) Uani 1 1 d . . . H41 H 0.5853 0.9945 0.7767 0.052 Uiso 1 1 calc R . . C42 C 0.6308(14) 1.1447(9) 0.7926(6) 0.057(4) Uani 1 1 d . . . H42 H 0.5654 1.1784 0.7764 0.069 Uiso 1 1 calc R . . C43 C 0.7144(14) 1.2051(8) 0.8144(6) 0.060(4) Uani 1 1 d . . . H43 H 0.7086 1.2803 0.8111 0.072 Uiso 1 1 calc R . . C44 C 0.8057(13) 1.1566(10) 0.8409(8) 0.064(4) Uani 1 1 d . . . H44 H 0.8627 1.1981 0.8566 0.077 Uiso 1 1 calc R . . C45 C 0.8153(11) 1.0479(8) 0.8447(6) 0.045(3) Uani 1 1 d . . . H45 H 0.8786 1.0146 0.8635 0.055 Uiso 1 1 calc R . . C46 C 0.7065(8) 0.5513(6) 0.8628(4) 0.0193(17) Uani 1 1 d . . . C47 C 0.7128(8) 0.5294(7) 0.9334(5) 0.027(2) Uani 1 1 d . . . H47 H 0.6512 0.5522 0.9683 0.032 Uiso 1 1 calc R . . C48 C 0.8087(9) 0.4746(8) 0.9525(5) 0.033(2) Uani 1 1 d . . . H48 H 0.8124 0.4594 1.0005 0.039 Uiso 1 1 calc R . . C49 C 0.8999(9) 0.4417(8) 0.9015(5) 0.034(2) Uani 1 1 d . . . H49 H 0.9666 0.4058 0.9147 0.041 Uiso 1 1 calc R . . C50 C 0.8927(9) 0.4615(8) 0.8314(5) 0.034(2) Uani 1 1 d . . . H50 H 0.9532 0.4373 0.7965 0.041 Uiso 1 1 calc R . . C51 C 0.7967(8) 0.5169(7) 0.8125(4) 0.0245(19) Uani 1 1 d . . . H51 H 0.7928 0.5314 0.7645 0.029 Uiso 1 1 calc R . . C52 C 0.4592(8) 0.5354(7) 0.8506(4) 0.0241(19) Uani 1 1 d . . . C53 C 0.4686(9) 0.4286(7) 0.8727(5) 0.029(2) Uani 1 1 d . . . H53 H 0.5421 0.4017 0.8824 0.035 Uiso 1 1 calc R . . C54 C 0.3715(9) 0.3611(8) 0.8808(6) 0.037(2) Uani 1 1 d . . . H54 H 0.3790 0.2885 0.8957 0.045 Uiso 1 1 calc R . . C55 C 0.2642(9) 0.3995(8) 0.8670(5) 0.033(2) Uani 1 1 d . . . H55 H 0.1978 0.3535 0.8723 0.040 Uiso 1 1 calc R . . C56 C 0.2540(9) 0.5066(8) 0.8453(5) 0.033(2) Uani 1 1 d . . . H56 H 0.1801 0.5337 0.8365 0.040 Uiso 1 1 calc R . . C57 C 0.3508(8) 0.5730(8) 0.8366(5) 0.031(2) Uani 1 1 d . . . H57 H 0.3435 0.6453 0.8209 0.037 Uiso 1 1 calc R . . C58 C 0.1325(6) 0.1800(6) 0.7010(4) 0.0113(14) Uiso 1 1 d . . . F1A F 0.1850(9) 0.0821(8) 0.6696(6) 0.047(2) Uiso 0.70 1 d P A 1 F2A F 0.0655(7) 0.2044(6) 0.6466(4) 0.0447(18) Uiso 0.90 1 d P A 1 F3A F 0.0625(10) 0.1460(9) 0.7526(6) 0.076(3) Uiso 0.80 1 d P A 1 F1B F 0.183(2) 0.0813(18) 0.7048(14) 0.047(6) Uiso 0.30 1 d P A 2 F2B F 0.038(6) 0.193(5) 0.681(4) 0.040(15) Uiso 0.10 1 d P A 2 F3B F 0.071(3) 0.207(3) 0.7742(19) 0.053(9) Uiso 0.20 1 d P A 2 S1 S 0.2370(3) 0.2750(2) 0.70129(16) 0.0451(7) Uiso 1 1 d . A . O1A O 0.3119(13) 0.2816(12) 0.6308(7) 0.031(4) Uiso 0.60 1 d P A 1 O2A O 0.1579(11) 0.3561(9) 0.7314(6) 0.030(3) Uiso 0.60 1 d P A 1 O3A O 0.3058(10) 0.2203(10) 0.7494(6) 0.024(3) Uiso 0.60 1 d P A 1 O1B O 0.288(2) 0.3072(18) 0.6319(11) 0.035(6) Uiso 0.40 1 d P A 2 O2B O 0.2038(18) 0.3817(15) 0.7053(11) 0.040(4) Uiso 0.40 1 d P A 2 O3B O 0.3276(16) 0.2546(15) 0.7401(9) 0.024(4) Uiso 0.40 1 d P A 2 Cl2 Cl 0.3344(4) -0.0461(4) 0.8838(3) 0.0904(14) Uani 1 1 d . . . Cl1 Cl 0.1300(6) 0.0807(6) 0.9339(3) 0.128(2) Uani 1 1 d . . . C59 C 0.2225(14) 0.0383(11) 0.8634(7) 0.064(4) Uani 1 1 d . . . H59A H 0.2592 0.1010 0.8345 0.077 Uiso 1 1 calc R . . H59B H 0.1750 0.0011 0.8349 0.077 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 0.0306(2) 0.02740(19) 0.01882(17) -0.00730(13) -0.00801(13) 0.01583(14) P1 0.0257(12) 0.0167(10) 0.0193(11) -0.0023(8) -0.0002(9) 0.0026(9) P2 0.0271(12) 0.0178(11) 0.0159(10) 0.0010(8) 0.0016(9) 0.0067(9) N1 0.024(4) 0.011(3) 0.026(4) -0.003(3) -0.007(3) 0.003(3) N2 0.028(4) 0.009(3) 0.016(3) -0.002(3) -0.003(3) 0.003(3) C1 0.022(4) 0.015(4) 0.016(4) 0.001(3) -0.001(3) 0.003(3) C2 0.036(5) 0.019(4) 0.016(4) -0.004(3) -0.006(4) 0.005(4) C3 0.036(5) 0.017(4) 0.016(4) 0.000(3) -0.001(4) 0.002(4) C4 0.023(4) 0.013(4) 0.020(4) 0.001(3) -0.005(3) 0.005(3) C5 0.031(5) 0.016(4) 0.023(4) -0.003(3) -0.005(4) 0.007(4) C6 0.038(6) 0.018(4) 0.030(5) -0.003(4) 0.001(4) 0.006(4) C7 0.035(5) 0.022(5) 0.030(5) -0.001(4) 0.004(4) 0.012(4) C8 0.024(5) 0.028(5) 0.034(5) 0.002(4) -0.001(4) 0.009(4) C9 0.031(5) 0.025(5) 0.021(4) 0.000(4) -0.009(4) 0.009(4) C10 0.028(5) 0.019(4) 0.033(5) -0.004(4) -0.002(4) 0.001(4) C11 0.036(6) 0.026(5) 0.037(6) 0.000(4) -0.003(4) 0.003(4) C12 0.034(6) 0.029(5) 0.052(7) 0.001(5) -0.014(5) 0.000(4) C13 0.024(5) 0.027(5) 0.037(5) 0.000(4) -0.009(4) 0.003(4) C14 0.044(7) 0.064(8) 0.053(7) 0.006(6) -0.023(6) -0.012(6) C15 0.037(6) 0.040(6) 0.040(6) 0.007(5) 0.002(5) -0.005(5) C16 0.028(5) 0.011(4) 0.016(4) -0.003(3) -0.003(3) 0.005(3) C17 0.029(5) 0.016(4) 0.018(4) -0.006(3) -0.007(4) 0.005(3) C18 0.026(5) 0.016(4) 0.021(4) 0.001(3) 0.001(4) -0.002(3) C19 0.035(5) 0.014(4) 0.019(4) -0.001(3) -0.009(4) 0.008(4) C20 0.022(4) 0.020(4) 0.019(4) -0.002(3) -0.004(3) 0.008(3) C21 0.021(4) 0.019(4) 0.017(4) -0.006(3) 0.000(3) 0.005(3) C22 0.024(5) 0.016(4) 0.024(4) 0.004(3) -0.008(4) -0.002(3) C23 0.026(5) 0.049(6) 0.034(6) -0.004(5) -0.006(4) 0.000(5) C24 0.031(5) 0.024(5) 0.036(5) -0.002(4) -0.016(4) -0.003(4) C25 0.025(5) 0.017(4) 0.028(5) -0.004(3) -0.003(4) 0.002(3) C26 0.043(6) 0.050(7) 0.036(6) -0.014(5) -0.006(5) -0.014(5) C27 0.034(5) 0.021(5) 0.035(5) -0.002(4) 0.007(4) -0.006(4) C28 0.022(4) 0.019(4) 0.018(4) 0.006(3) 0.003(3) 0.007(3) C29 0.036(5) 0.019(4) 0.027(5) -0.002(4) -0.001(4) 0.003(4) C39 0.036(6) 0.047(7) 0.053(7) 0.004(5) -0.011(5) 0.013(5) C30 0.046(6) 0.021(4) 0.019(4) 0.000(3) 0.001(4) 0.014(4) C31 0.041(6) 0.027(5) 0.018(4) 0.004(4) 0.008(4) 0.010(4) C32 0.030(5) 0.021(4) 0.025(5) 0.001(4) 0.000(4) 0.006(4) C33 0.028(5) 0.020(4) 0.016(4) 0.002(3) -0.002(3) 0.010(4) C34 0.034(5) 0.026(5) 0.028(5) -0.007(4) -0.008(4) 0.003(4) C35 0.018(5) 0.091(9) 0.018(5) -0.008(5) -0.001(4) 0.007(5) C36 0.032(6) 0.074(9) 0.048(7) -0.027(6) 0.002(5) 0.001(6) C37 0.038(6) 0.047(7) 0.068(9) -0.015(6) -0.014(6) 0.012(5) C38 0.046(7) 0.057(8) 0.061(8) 0.020(6) -0.018(6) 0.000(6) C40 0.043(6) 0.015(4) 0.021(5) -0.001(3) 0.013(4) 0.001(4) C41 0.076(8) 0.026(5) 0.028(5) 0.001(4) -0.007(5) 0.012(5) C42 0.101(11) 0.035(6) 0.035(6) -0.004(5) -0.009(7) 0.034(7) C43 0.107(12) 0.017(5) 0.037(6) -0.002(5) 0.040(7) 0.001(7) C44 0.071(9) 0.034(7) 0.073(9) -0.027(6) 0.036(8) -0.016(7) C45 0.047(7) 0.026(5) 0.056(7) -0.021(5) 0.016(6) -0.002(5) C46 0.024(4) 0.010(4) 0.022(4) 0.001(3) -0.002(3) 0.001(3) C47 0.029(5) 0.033(5) 0.018(4) -0.003(4) -0.002(4) 0.011(4) C48 0.044(6) 0.034(5) 0.019(5) 0.003(4) -0.005(4) 0.004(4) C49 0.032(5) 0.039(6) 0.029(5) 0.001(4) -0.002(4) 0.014(4) C50 0.030(5) 0.039(6) 0.031(5) -0.002(4) 0.000(4) 0.008(4) C51 0.036(5) 0.020(4) 0.015(4) 0.001(3) -0.001(4) 0.002(4) C52 0.031(5) 0.026(5) 0.015(4) -0.004(3) -0.001(4) 0.000(4) C53 0.036(5) 0.025(5) 0.027(5) -0.005(4) -0.010(4) 0.002(4) C54 0.042(6) 0.026(5) 0.045(6) -0.006(4) -0.011(5) -0.004(4) C55 0.033(5) 0.037(6) 0.032(5) -0.013(4) -0.006(4) -0.005(4) C56 0.032(5) 0.046(6) 0.021(5) -0.014(4) -0.001(4) 0.010(5) C57 0.027(5) 0.042(6) 0.026(5) -0.010(4) -0.004(4) 0.012(4) Cl2 0.081(3) 0.084(3) 0.120(4) 0.008(3) -0.061(3) -0.002(2) Cl1 0.131(5) 0.172(6) 0.079(3) -0.020(4) -0.012(3) 0.039(4) C59 0.084(10) 0.052(8) 0.058(8) 0.003(6) -0.024(8) -0.009(7) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.055(8) . ? Au1 P1 2.333(2) . ? Au1 P2 2.764(2) . ? P1 C34 1.816(10) . ? P1 C28 1.820(8) . ? P1 C40 1.823(9) . ? P2 C46 1.830(8) . ? P2 C33 1.834(9) . ? P2 C52 1.836(10) . ? N1 C1 1.340(10) . ? N1 C4 1.443(10) . ? N1 C2 1.489(10) . ? N2 C1 1.341(10) . ? N2 C16 1.437(10) . ? N2 C3 1.484(10) . ? C2 C3 1.527(11) . ? C4 C5 1.398(12) . ? C4 C9 1.406(12) . ? C5 C6 1.379(12) . ? C5 C10 1.527(13) . ? C6 C7 1.384(14) . ? C7 C8 1.371(14) . ? C8 C9 1.397(12) . ? C9 C13 1.500(13) . ? C10 C12 1.522(14) . ? C10 C11 1.537(13) . ? C13 C15 1.527(14) . ? C13 C14 1.528(14) . ? C16 C17 1.390(12) . ? C16 C21 1.415(12) . ? C17 C18 1.396(11) . ? C17 C22 1.525(12) . ? C18 C19 1.392(12) . ? C19 C20 1.366(13) . ? C20 C21 1.405(11) . ? C21 C25 1.502(12) . ? C22 C23 1.516(13) . ? C22 C24 1.534(12) . ? C25 C27 1.535(12) . ? C25 C26 1.537(13) . ? C28 C33 1.390(13) . ? C28 C29 1.422(12) . ? C29 C30 1.387(13) . ? C39 C34 1.372(15) . ? C39 C38 1.384(16) . ? C30 C31 1.369(14) . ? C31 C32 1.386(13) . ? C32 C33 1.401(12) . ? C34 C35 1.398(14) . ? C35 C36 1.399(15) . ? C36 C37 1.372(18) . ? C37 C38 1.386(17) . ? C40 C41 1.377(15) . ? C40 C45 1.393(15) . ? C41 C42 1.386(15) . ? C42 C43 1.37(2) . ? C43 C44 1.37(2) . ? C44 C45 1.375(16) . ? C46 C51 1.387(12) . ? C46 C47 1.400(12) . ? C47 C48 1.386(13) . ? C48 C49 1.396(13) . ? C49 C50 1.389(14) . ? C50 C51 1.388(13) . ? C52 C57 1.391(13) . ? C52 C53 1.395(13) . ? C53 C54 1.389(14) . ? C54 C55 1.381(14) . ? C55 C56 1.398(15) . ? C56 C57 1.378(14) . ? C58 F3A 1.225(13) . ? C58 F2B 1.23(6) . ? C58 F1B 1.37(2) . ? C58 F2A 1.430(10) . ? C58 F1A 1.498(12) . ? C58 F3B 1.54(4) . ? C58 S1 1.707(8) . ? S1 O3B 1.401(17) . ? S1 O2B 1.403(19) . ? S1 O1B 1.41(2) . ? S1 O2A 1.452(11) . ? S1 O3A 1.460(12) . ? S1 O1A 1.486(14) . ? Cl2 C59 1.741(15) . ? Cl1 C59 1.702(16) . ? 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 154.5(2) . . ? C1 Au1 P2 127.7(2) . . ? P1 Au1 P2 77.79(7) . . ? C34 P1 C28 106.2(4) . . ? C34 P1 C40 106.1(5) . . ? C28 P1 C40 102.7(4) . . ? C34 P1 Au1 114.0(3) . . ? C28 P1 Au1 111.8(3) . . ? C40 P1 Au1 115.0(3) . . ? C46 P2 C33 101.3(4) . . ? C46 P2 C52 104.5(4) . . ? C33 P2 C52 102.5(4) . . ? C46 P2 Au1 101.3(3) . . ? C33 P2 Au1 100.7(3) . . ? C52 P2 Au1 140.9(3) . . ? C1 N1 C4 124.4(7) . . ? C1 N1 C2 112.3(6) . . ? C4 N1 C2 120.2(7) . . ? C1 N2 C16 126.5(7) . . ? C1 N2 C3 112.6(6) . . ? C16 N2 C3 120.7(6) . . ? N1 C1 N2 108.4(7) . . ? N1 C1 Au1 122.5(6) . . ? N2 C1 Au1 129.0(6) . . ? N1 C2 C3 101.7(6) . . ? N2 C3 C2 101.8(6) . . ? C5 C4 C9 122.4(8) . . ? C5 C4 N1 118.3(7) . . ? C9 C4 N1 119.2(7) . . ? C6 C5 C4 117.9(8) . . ? C6 C5 C10 121.1(8) . . ? C4 C5 C10 121.0(7) . . ? C5 C6 C7 121.2(9) . . ? C8 C7 C6 120.1(8) . . ? C7 C8 C9 121.5(9) . . ? C8 C9 C4 116.8(9) . . ? C8 C9 C13 119.8(8) . . ? C4 C9 C13 123.4(8) . . ? C12 C10 C5 110.8(8) . . ? C12 C10 C11 111.3(8) . . ? C5 C10 C11 112.4(7) . . ? C9 C13 C15 111.6(8) . . ? C9 C13 C14 111.3(8) . . ? C15 C13 C14 110.9(9) . . ? C17 C16 C21 122.4(7) . . ? C17 C16 N2 118.7(7) . . ? C21 C16 N2 118.9(7) . . ? C16 C17 C18 118.4(8) . . ? C16 C17 C22 122.9(7) . . ? C18 C17 C22 118.7(8) . . ? C19 C18 C17 119.6(8) . . ? C20 C19 C18 121.6(8) . . ? C19 C20 C21 120.8(8) . . ? C20 C21 C16 117.0(8) . . ? C20 C21 C25 119.9(8) . . ? C16 C21 C25 123.1(7) . . ? C23 C22 C17 112.8(7) . . ? C23 C22 C24 111.1(8) . . ? C17 C22 C24 110.0(7) . . ? C21 C25 C27 112.0(7) . . ? C21 C25 C26 111.2(8) . . ? C27 C25 C26 109.8(8) . . ? C33 C28 C29 119.5(8) . . ? C33 C28 P1 121.1(6) . . ? C29 C28 P1 119.4(7) . . ? C30 C29 C28 120.0(9) . . ? C34 C39 C38 122.5(11) . . ? C31 C30 C29 120.0(8) . . ? C30 C31 C32 120.7(9) . . ? C31 C32 C33 120.8(9) . . ? C28 C33 C32 118.9(8) . . ? C28 C33 P2 118.8(6) . . ? C32 C33 P2 122.2(7) . . ? C39 C34 C35 118.7(9) . . ? C39 C34 P1 123.3(8) . . ? C35 C34 P1 117.9(7) . . ? C34 C35 C36 118.3(10) . . ? C37 C36 C35 121.9(11) . . ? C36 C37 C38 119.1(11) . . ? C39 C38 C37 119.0(12) . . ? C41 C40 C45 119.5(9) . . ? C41 C40 P1 117.9(8) . . ? C45 C40 P1 122.5(8) . . ? C40 C41 C42 119.4(12) . . ? C43 C42 C41 120.8(13) . . ? C44 C43 C42 119.7(11) . . ? C43 C44 C45 120.3(13) . . ? C44 C45 C40 120.2(13) . . ? C51 C46 C47 119.2(8) . . ? C51 C46 P2 118.1(6) . . ? C47 C46 P2 122.7(6) . . ? C48 C47 C46 120.1(8) . . ? C47 C48 C49 120.2(9) . . ? C50 C49 C48 119.8(9) . . ? C51 C50 C49 119.7(9) . . ? C46 C51 C50 120.9(8) . . ? C57 C52 C53 118.7(9) . . ? C57 C52 P2 117.9(7) . . ? C53 C52 P2 123.2(7) . . ? C54 C53 C52 120.7(9) . . ? C55 C54 C53 120.1(10) . . ? C54 C55 C56 119.5(10) . . ? C57 C56 C55 120.2(9) . . ? C56 C57 C52 120.8(10) . . ? F3A C58 F2B 79(3) . . ? F3A C58 F1B 85.0(12) . . ? F2B C58 F1B 121(3) . . ? F3A C58 F2A 107.0(8) . . ? F2B C58 F2A 29(3) . . ? F1B C58 F2A 117.6(12) . . ? F3A C58 F1A 104.0(8) . . ? F2B C58 F1A 106(3) . . ? F1B C58 F1A 27.1(10) . . ? F2A C58 F1A 93.3(7) . . ? F3A C58 F3B 36.5(13) . . ? F2B C58 F3B 89(4) . . ? F1B C58 F3B 109.7(18) . . ? F2A C58 F3B 114.9(14) . . ? F1A C58 F3B 135.1(15) . . ? F3A C58 S1 124.6(8) . . ? F2B C58 S1 126(3) . . ? F1B C58 S1 109.8(11) . . ? F2A C58 S1 111.2(6) . . ? F1A C58 S1 112.1(6) . . ? F3B C58 S1 90.3(14) . . ? O3B S1 O2B 108.7(11) . . ? O3B S1 O1B 108.7(12) . . ? O2B S1 O1B 84.6(13) . . ? O3B S1 O2A 110.6(8) . . ? O2B S1 O2A 29.4(8) . . ? O1B S1 O2A 110.7(11) . . ? O3B S1 O3A 20.3(8) . . ? O2B S1 O3A 122.7(9) . . ? O1B S1 O3A 121.6(11) . . ? O2A S1 O3A 114.7(7) . . ? O3B S1 O1A 97.6(9) . . ? O2B S1 O1A 99.7(11) . . ? O1B S1 O1A 16.4(10) . . ? O2A S1 O1A 126.8(8) . . ? O3A S1 O1A 107.3(8) . . ? O3B S1 C58 119.5(9) . . ? O2B S1 C58 120.1(9) . . ? O1B S1 C58 109.2(10) . . ? O2A S1 C58 97.6(6) . . ? O3A S1 C58 99.3(6) . . ? O1A S1 C58 106.5(6) . . ? Cl1 C59 Cl2 114.5(8) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 7.308 _refine_diff_density_min -3.195 _refine_diff_density_rms 0.181 _database_code_depnum_ccdc_archive 'CCDC 960723'