# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # 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_Vo3MB58b _database_code_depnum_ccdc_archive 'CCDC 915632' #TrackingRef 'web_deposit_cif_file_0_EddyViseux_1355414187.V03MB58b.cif' _audit_creation_date 2012-02-10T11:14:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H25 Au F6 N O7 P S2' _chemical_formula_sum 'C30 H25 Au F6 N O7 P S2' _chemical_formula_weight 917.57 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.69020(10) _cell_length_b 34.9283(3) _cell_length_c 11.4932(2) _cell_angle_alpha 90 _cell_angle_beta 103.15 _cell_angle_gamma 90 _cell_volume 3397.14(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7718 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Block _exptl_crystal_colour Clear _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.794 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.579 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4429 _exptl_absorpt_correction_T_max 0.5095 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.728314E-1 _diffrn_orient_matrix_ub_12 -0.171236E-1 _diffrn_orient_matrix_ub_13 0.570963E-1 _diffrn_orient_matrix_ub_21 0.75533E-1 _diffrn_orient_matrix_ub_22 0 _diffrn_orient_matrix_ub_23 -0.539233E-1 _diffrn_orient_matrix_ub_31 0.543537E-1 _diffrn_orient_matrix_ub_32 0.229448E-1 _diffrn_orient_matrix_ub_33 0.426107E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_unetI/netI 0.0519 _diffrn_reflns_number 32544 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 27.11 _diffrn_reflns_theta_full 27.11 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 13530 _reflns_number_gt 11779 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0355P)^2^+3.2236P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 13530 _refine_ls_number_parameters 865 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.050(4) _refine_diff_density_max 0.67 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.006 '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' 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 0.7842(8) 0.7092(2) 0.9324(6) 0.0423(15) Uani 1 1 d . . . C2 C 0.6798(9) 0.7291(2) 0.9831(7) 0.0532(18) Uani 1 1 d . . . H2 H 0.6415 0.7179 1.0445 0.064 Uiso 1 1 calc R . . C3 C 0.6300(11) 0.7662(3) 0.9428(9) 0.075(3) Uani 1 1 d . . . H3 H 0.5578 0.7796 0.9758 0.09 Uiso 1 1 calc R . . C4 C 0.6914(10) 0.7822(3) 0.8530(8) 0.068(2) Uani 1 1 d . . . H4 H 0.661 0.8068 0.8266 0.081 Uiso 1 1 calc R . . C5 C 0.7951(11) 0.7628(2) 0.8025(7) 0.065(2) Uani 1 1 d . . . H5 H 0.8334 0.774 0.7413 0.078 Uiso 1 1 calc R . . C6 C 0.8439(9) 0.7263(2) 0.8422(7) 0.0526(18) Uani 1 1 d . . . H6 H 0.9164 0.7132 0.8087 0.063 Uiso 1 1 calc R . . C7 C 0.7424(7) 0.62664(19) 0.8903(6) 0.0393(14) Uani 1 1 d . . . C8 C 0.7489(9) 0.5893(2) 0.9290(7) 0.0506(18) Uani 1 1 d . . . H8 H 0.8082 0.5834 1.0049 0.061 Uiso 1 1 calc R . . C9 C 0.6697(11) 0.5602(3) 0.8581(9) 0.068(2) Uani 1 1 d . . . H9 H 0.6783 0.5349 0.8845 0.082 Uiso 1 1 calc R . . C10 C 0.5777(11) 0.5695(3) 0.7477(8) 0.072(2) Uani 1 1 d . . . H10 H 0.52 0.5505 0.7005 0.086 Uiso 1 1 calc R . . C11 C 0.5699(11) 0.6063(3) 0.7063(7) 0.070(2) Uani 1 1 d . . . H11 H 0.5091 0.612 0.6307 0.084 Uiso 1 1 calc R . . C12 C 0.6525(9) 0.6348(2) 0.7768(6) 0.0523(18) Uani 1 1 d . . . H12 H 0.6478 0.6598 0.7481 0.063 Uiso 1 1 calc R . . C13 C 1.0527(7) 0.6572(2) 0.9790(5) 0.0416(14) Uani 1 1 d . . . C14 C 1.0953(9) 0.6408(2) 0.8824(7) 0.057(2) Uani 1 1 d . . . H14 H 1.017 0.6317 0.8192 0.068 Uiso 1 1 calc R . . C15 C 1.2512(11) 0.6374(3) 0.8772(9) 0.073(3) Uani 1 1 d . . . H15 H 1.2784 0.6266 0.8107 0.087 Uiso 1 1 calc R . . C16 C 1.3643(9) 0.6500(4) 0.9704(9) 0.082(3) Uani 1 1 d . . . H16 H 1.4701 0.6471 0.9687 0.098 Uiso 1 1 calc R . . C17 C 1.3259(9) 0.6670(4) 1.0664(8) 0.085(3) Uani 1 1 d . . . H17 H 1.4048 0.6765 1.1284 0.102 Uiso 1 1 calc R . . C18 C 1.1687(8) 0.6700(3) 1.0715(7) 0.062(2) Uani 1 1 d . . . H18 H 1.1421 0.6808 1.1383 0.074 Uiso 1 1 calc R . . C19 C 0.8653(8) 0.6152(2) 1.4238(6) 0.0451(16) Uani 1 1 d . . . H19 H 0.8269 0.6146 1.4976 0.054 Uiso 1 1 calc R . . C20 C 1.0448(9) 0.6200(3) 1.4579(7) 0.059(2) Uani 1 1 d . . . C21 C 1.2674(9) 0.6478(3) 1.4100(9) 0.082(3) Uani 1 1 d . . . H21A H 1.2933 0.6637 1.3491 0.123 Uiso 1 1 calc R . . H21B H 1.3222 0.6238 1.4127 0.123 Uiso 1 1 calc R . . H21C H 1.2988 0.6603 1.486 0.123 Uiso 1 1 calc R . . C26 C 0.8251(10) 0.5770(2) 1.3604(8) 0.063(2) Uani 1 1 d . . . H26A H 0.8631 0.5772 1.2873 0.076 Uiso 1 1 calc R . . H26B H 0.8808 0.5568 1.411 0.076 Uiso 1 1 calc R . . C27 C 0.6499(10) 0.5677(2) 1.3297(7) 0.0554(19) Uani 1 1 d . . . C28 C 0.5727(11) 0.5557(2) 1.4158(7) 0.061(2) Uani 1 1 d . . . H28 H 0.6297 0.5535 1.4945 0.073 Uiso 1 1 calc R . . C29 C 0.4117(10) 0.5466(3) 1.3886(8) 0.068(2) Uani 1 1 d . . . H29 H 0.3619 0.5381 1.4474 0.082 Uiso 1 1 calc R . . C30 C 0.3321(10) 0.5506(2) 1.2755(8) 0.061(2) Uani 1 1 d . . . C31 C 0.4021(12) 0.5636(3) 1.1863(9) 0.084(3) Uani 1 1 d . . . H31 H 0.3429 0.5669 1.1087 0.1 Uiso 1 1 calc R . . C32 C 0.5605(12) 0.5716(3) 1.2146(8) 0.081(3) Uani 1 1 d . . . H32 H 0.609 0.5799 1.1548 0.097 Uiso 1 1 calc R . . C33 C 0.0627(10) 0.4760(3) 1.2860(7) 0.065(2) Uani 1 1 d . . . C34 C 0.8509(12) 0.7125(3) 1.4760(9) 0.075(3) Uani 1 1 d . . . C51 C 0.2720(8) 0.8822(2) 0.6816(6) 0.0441(16) Uani 1 1 d . . . C52 C 0.2222(10) 0.9039(3) 0.5805(8) 0.066(2) Uani 1 1 d . . . H52 H 0.1327 0.8969 0.5233 0.079 Uiso 1 1 calc R . . C53 C 0.3076(13) 0.9367(3) 0.5641(11) 0.090(4) Uani 1 1 d . . . H53 H 0.2762 0.9516 0.4958 0.107 Uiso 1 1 calc R . . C54 C 0.4392(13) 0.9466(3) 0.6514(13) 0.091(4) Uani 1 1 d . . . H54 H 0.4927 0.9692 0.6433 0.109 Uiso 1 1 calc R . . C55 C 0.4907(13) 0.9247(3) 0.7460(9) 0.081(3) Uani 1 1 d . . . H55 H 0.583 0.9313 0.8011 0.098 Uiso 1 1 calc R . . C56 C 0.4088(10) 0.8922(3) 0.7638(7) 0.062(2) Uani 1 1 d . . . H56 H 0.4455 0.877 0.8308 0.074 Uiso 1 1 calc R . . C57 C 0.2583(8) 0.7985(2) 0.6796(6) 0.0447(16) Uani 1 1 d . . . C58 C 0.3381(9) 0.7988(3) 0.5860(7) 0.057(2) Uani 1 1 d . . . H58 H 0.3436 0.8213 0.5436 0.068 Uiso 1 1 calc R . . C59 C 0.4090(11) 0.7655(3) 0.5569(8) 0.077(3) Uani 1 1 d . . . H59 H 0.4614 0.7656 0.4948 0.093 Uiso 1 1 calc R . . C60 C 0.4012(12) 0.7328(3) 0.6200(10) 0.078(3) Uani 1 1 d . . . H60 H 0.4494 0.7106 0.6014 0.094 Uiso 1 1 calc R . . C61 C 0.3230(11) 0.7325(3) 0.7100(10) 0.079(3) Uani 1 1 d . . . H61 H 0.3174 0.7098 0.7513 0.095 Uiso 1 1 calc R . . C62 C 0.2512(9) 0.7653(3) 0.7420(8) 0.061(2) Uani 1 1 d . . . H62 H 0.1994 0.7647 0.8045 0.073 Uiso 1 1 calc R . . C63 C -0.0306(8) 0.8426(2) 0.6155(6) 0.0451(14) Uani 1 1 d . . . C64 C -0.1565(8) 0.8590(2) 0.6541(7) 0.0524(18) Uani 1 1 d . . . H64 H -0.1431 0.8683 0.7316 0.063 Uiso 1 1 calc R . . C65 C -0.3017(9) 0.8611(3) 0.5746(9) 0.075(3) Uani 1 1 d . . . H65 H -0.3854 0.8731 0.5979 0.09 Uiso 1 1 calc R . . C66 C -0.3250(9) 0.8458(3) 0.4620(8) 0.073(2) Uani 1 1 d . . . H66 H -0.4243 0.8468 0.4103 0.087 Uiso 1 1 calc R . . C67 C -0.2015(10) 0.8293(3) 0.4266(8) 0.078(3) Uani 1 1 d . . . H67 H -0.2166 0.8192 0.3499 0.094 Uiso 1 1 calc R . . C68 C -0.0568(10) 0.8273(3) 0.5015(7) 0.068(2) Uani 1 1 d . . . H68 H 0.0258 0.8155 0.4761 0.081 Uiso 1 1 calc R . . C69 C 0.0653(9) 0.8860(2) 1.1229(6) 0.0546(18) Uani 1 1 d . . . H69 H 0.0823 0.887 1.2101 0.066 Uiso 1 1 calc R . . C70 C 0.1195(11) 0.9241(3) 1.0782(8) 0.065(2) Uani 1 1 d . . . H70A H 0.0969 0.9233 0.9916 0.078 Uiso 1 1 calc R . . H70B H 0.0564 0.9445 1.1006 0.078 Uiso 1 1 calc R . . C71 C 0.2905(11) 0.9342(2) 1.1230(8) 0.061(2) Uani 1 1 d . . . C72 C 0.3708(12) 0.9296(3) 1.2373(9) 0.081(3) Uani 1 1 d . . . H72 H 0.3178 0.9196 1.2923 0.097 Uiso 1 1 calc R . . C73 C 0.5285(14) 0.9392(3) 1.2759(9) 0.090(3) Uani 1 1 d . . . H73 H 0.5818 0.9353 1.3549 0.108 Uiso 1 1 calc R . . C74 C 0.6047(12) 0.9547(3) 1.1932(10) 0.076(3) Uani 1 1 d . . . C75 C 0.5256(12) 0.9595(3) 1.0771(9) 0.078(3) Uani 1 1 d . . . H75 H 0.5789 0.9695 1.0223 0.094 Uiso 1 1 calc R . . C76 C 0.3696(12) 0.9499(3) 1.0396(8) 0.071(2) Uani 1 1 d . . . H76 H 0.3166 0.9536 0.9605 0.085 Uiso 1 1 calc R . . C77 C -0.1066(10) 0.8794(3) 1.0700(7) 0.062(2) Uani 1 1 d . . . C78 C 0.1116(11) 0.7840(3) 1.1831(9) 0.068(2) Uani 1 1 d . . . C84 C 0.8876(18) 1.0291(4) 1.2186(12) 0.103(4) Uani 1 1 d . . . C89 C -0.3492(10) 0.8610(3) 1.1082(9) 0.082(3) Uani 1 1 d . . . H89A H -0.395 0.8558 1.175 0.124 Uiso 1 1 calc R . . H89B H -0.356 0.8386 1.059 0.124 Uiso 1 1 calc R . . H89C H -0.4053 0.8817 1.0621 0.124 Uiso 1 1 calc R . . Au2 Au 0.81663(3) 0.654719(8) 1.17602(2) 0.04115(7) Uani 1 1 d . . . Au51 Au 0.15616(3) 0.845221(8) 0.91082(2) 0.04558(8) Uani 1 1 d . . . F1 F 0.9225(8) 0.72727(19) 1.3976(7) 0.117(3) Uani 1 1 d . . . F2 F 0.7878(9) 0.74087(19) 1.5234(7) 0.113(2) Uani 1 1 d . . . F3 F 0.9552(7) 0.6953(2) 1.5600(6) 0.115(2) Uani 1 1 d . . . F4 F -0.0280(8) 0.49094(19) 1.3503(6) 0.108(2) Uani 1 1 d . . . F5 F 0.1941(7) 0.4662(2) 1.3578(6) 0.1009(18) Uani 1 1 d . . . F6 F -0.0075(9) 0.44470(17) 1.2366(6) 0.105(2) Uani 1 1 d . . . F51 F -0.0186(8) 0.7955(2) 1.2105(8) 0.124(3) Uani 1 1 d . . . F52 F 0.1763(8) 0.75775(18) 1.2607(6) 0.101(2) Uani 1 1 d . . . F53 F 0.0767(9) 0.76778(19) 1.0766(6) 0.106(2) Uani 1 1 d . . . F54 F 0.7515(13) 1.0402(3) 1.1548(9) 0.159(4) Uani 1 1 d . . . F55 F 0.9743(11) 1.0153(3) 1.1491(7) 0.149(3) Uani 1 1 d . . . F56 F 0.9700(13) 1.0558(3) 1.2806(9) 0.171(4) Uani 1 1 d . . . N1 N 0.7830(6) 0.64696(18) 1.3482(4) 0.0368(14) Uani 1 1 d . . . N51 N 0.1561(7) 0.85362(18) 1.0898(4) 0.0467(16) Uani 1 1 d . . . O1 O 0.6401(7) 0.66463(17) 1.5026(5) 0.0672(16) Uani 1 1 d . . . O2 O 0.5973(7) 0.70038(19) 1.3125(5) 0.0727(17) Uani 1 1 d . . . O4 O 0.1655(7) 0.54396(17) 1.2472(7) 0.0761(18) Uani 1 1 d . . . O5 O -0.0591(8) 0.5190(2) 1.1078(6) 0.090(2) Uani 1 1 d . . . O6 O 0.2025(7) 0.49007(19) 1.1150(6) 0.0746(17) Uani 1 1 d . . . O7 O 1.0994(6) 0.64098(19) 1.3832(5) 0.0738(18) Uani 1 1 d . . . O8 O 1.1252(9) 0.6060(3) 1.5440(8) 0.141(4) Uani 1 1 d . . . O51 O 0.3722(7) 0.8076(2) 1.1450(7) 0.088(2) Uani 1 1 d . . . O52 O 0.2685(8) 0.8393(2) 1.3038(5) 0.088(2) Uani 1 1 d . . . O53 O 0.7747(8) 0.9605(2) 1.2245(7) 0.092(2) Uani 1 1 d . . . O54 O 1.0033(11) 0.9774(3) 1.3718(9) 0.143(4) Uani 1 1 d . . . O55 O 0.7496(10) 1.0059(3) 1.3838(7) 0.103(3) Uani 1 1 d . . . O57 O -0.1862(6) 0.8716(2) 1.1507(5) 0.0699(16) Uani 1 1 d . . . O58 O -0.1673(8) 0.8804(3) 0.9654(6) 0.118(3) Uani 1 1 d . . . P1 P 0.84836(19) 0.66238(6) 0.98968(15) 0.0377(4) Uani 1 1 d . . . P51 P 0.1618(2) 0.84099(7) 0.71744(15) 0.0402(4) Uani 1 1 d . . . S1 S 0.6971(2) 0.67841(6) 1.40343(15) 0.0461(4) Uani 1 1 d . . . S51 S 0.2465(2) 0.82462(6) 1.18411(16) 0.0550(5) Uani 1 1 d . . . S52 S 0.8535(3) 0.99069(9) 1.3192(2) 0.0794(7) Uani 1 1 d . . . S100 S 0.0928(3) 0.50823(6) 1.1710(2) 0.0597(5) 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 0.042(4) 0.042(4) 0.041(4) -0.005(3) 0.005(3) -0.002(3) C2 0.055(4) 0.048(5) 0.058(5) -0.002(3) 0.015(3) -0.004(4) C3 0.064(5) 0.072(6) 0.089(7) -0.020(5) 0.017(5) 0.008(5) C4 0.073(6) 0.047(5) 0.074(6) 0.001(4) -0.001(4) 0.006(4) C5 0.080(6) 0.053(5) 0.055(5) 0.007(4) 0.003(4) -0.002(4) C6 0.062(5) 0.043(4) 0.056(4) 0.003(3) 0.017(4) 0.002(3) C7 0.035(3) 0.045(4) 0.041(3) -0.002(3) 0.013(3) -0.007(3) C8 0.061(5) 0.046(4) 0.044(4) 0.004(3) 0.010(3) -0.007(4) C9 0.088(7) 0.050(5) 0.068(6) -0.001(4) 0.019(5) -0.010(4) C10 0.073(6) 0.079(7) 0.063(5) -0.022(5) 0.013(4) -0.025(5) C11 0.083(6) 0.081(7) 0.039(4) 0.002(4) -0.001(4) -0.009(5) C12 0.057(4) 0.058(5) 0.040(4) 0.005(3) 0.006(3) 0.003(4) C13 0.034(3) 0.046(4) 0.045(3) -0.003(3) 0.010(2) -0.002(3) C14 0.046(4) 0.068(6) 0.062(4) -0.010(4) 0.025(3) -0.005(4) C15 0.068(6) 0.069(6) 0.099(7) -0.009(5) 0.054(5) 0.001(4) C16 0.033(4) 0.115(8) 0.099(7) 0.016(7) 0.019(4) 0.000(5) C17 0.043(4) 0.136(10) 0.067(6) -0.005(6) -0.005(4) -0.015(5) C18 0.042(4) 0.098(7) 0.044(4) 0.001(4) 0.007(3) -0.007(4) C19 0.056(4) 0.044(4) 0.037(3) 0.004(3) 0.015(3) 0.000(3) C20 0.050(4) 0.071(6) 0.053(5) 0.005(4) 0.004(4) -0.004(4) C21 0.044(4) 0.096(8) 0.100(7) -0.001(6) 0.008(4) -0.001(5) C26 0.075(6) 0.050(5) 0.074(6) -0.009(4) 0.034(4) -0.009(4) C27 0.077(5) 0.033(4) 0.064(5) -0.006(3) 0.031(4) -0.009(4) C28 0.086(6) 0.051(5) 0.050(4) -0.007(3) 0.025(4) -0.014(4) C29 0.074(6) 0.069(6) 0.073(6) -0.006(4) 0.039(5) -0.011(5) C30 0.061(5) 0.043(4) 0.083(6) -0.015(4) 0.025(4) -0.015(4) C31 0.091(7) 0.092(8) 0.067(6) 0.021(5) 0.016(5) -0.033(6) C32 0.094(7) 0.098(8) 0.056(5) 0.007(5) 0.026(5) -0.044(6) C33 0.066(5) 0.070(6) 0.055(5) 0.003(4) 0.009(4) 0.001(4) C34 0.084(7) 0.070(6) 0.079(6) -0.029(5) 0.036(6) -0.021(5) C51 0.050(4) 0.045(4) 0.040(4) -0.005(3) 0.017(3) -0.002(3) C52 0.054(5) 0.077(6) 0.072(5) 0.019(4) 0.022(4) -0.003(4) C53 0.079(7) 0.087(8) 0.115(9) 0.051(7) 0.047(6) 0.011(6) C54 0.073(7) 0.055(6) 0.156(11) 0.021(6) 0.049(7) -0.011(5) C55 0.092(7) 0.082(7) 0.075(6) -0.017(5) 0.030(5) -0.035(6) C56 0.063(5) 0.065(5) 0.060(5) -0.004(4) 0.019(4) -0.017(4) C57 0.043(4) 0.044(4) 0.049(4) 0.000(3) 0.012(3) 0.007(3) C58 0.052(5) 0.066(5) 0.054(5) -0.004(4) 0.015(4) 0.003(4) C59 0.077(6) 0.094(8) 0.061(5) -0.021(5) 0.017(4) 0.024(5) C60 0.075(6) 0.056(6) 0.099(7) -0.024(5) 0.011(5) 0.013(5) C61 0.079(6) 0.043(5) 0.106(8) 0.009(5) 0.002(6) -0.001(4) C62 0.060(5) 0.059(5) 0.063(5) 0.014(4) 0.011(4) 0.007(4) C63 0.047(4) 0.045(4) 0.047(3) 0.004(3) 0.017(3) 0.000(3) C64 0.049(4) 0.060(5) 0.051(4) -0.005(3) 0.018(3) 0.002(3) C65 0.040(4) 0.089(7) 0.097(7) -0.001(5) 0.019(4) 0.017(4) C66 0.044(4) 0.095(7) 0.072(5) 0.009(6) -0.002(4) 0.005(5) C67 0.059(5) 0.117(9) 0.053(5) -0.016(5) -0.001(4) 0.005(5) C68 0.059(5) 0.093(7) 0.051(4) -0.008(4) 0.012(4) 0.011(4) C69 0.059(5) 0.067(5) 0.040(4) -0.005(3) 0.017(3) 0.007(4) C70 0.074(6) 0.053(5) 0.069(5) -0.005(4) 0.018(4) 0.007(4) C71 0.074(5) 0.054(5) 0.058(5) -0.012(4) 0.020(4) 0.004(4) C72 0.086(7) 0.090(8) 0.065(6) 0.003(5) 0.015(5) -0.029(6) C73 0.109(8) 0.094(8) 0.062(6) -0.005(5) 0.010(6) -0.033(6) C74 0.077(6) 0.056(6) 0.101(8) -0.003(5) 0.033(6) -0.010(5) C75 0.084(7) 0.087(7) 0.070(6) -0.008(5) 0.032(5) -0.011(6) C76 0.091(7) 0.068(6) 0.057(5) 0.002(4) 0.022(5) -0.002(5) C77 0.058(5) 0.074(6) 0.053(5) -0.008(4) 0.012(4) 0.002(4) C78 0.075(6) 0.060(6) 0.072(6) 0.007(5) 0.025(5) -0.007(5) C84 0.121(10) 0.089(9) 0.102(9) -0.020(7) 0.032(8) -0.008(8) C89 0.062(6) 0.099(8) 0.091(7) -0.013(6) 0.027(5) -0.007(5) Au2 0.03911(13) 0.05340(17) 0.03191(12) -0.00176(12) 0.01010(9) -0.00079(14) Au51 0.05109(16) 0.05297(18) 0.03545(14) 0.00213(12) 0.01562(11) -0.00059(14) F1 0.138(6) 0.094(5) 0.147(6) -0.039(4) 0.089(5) -0.058(4) F2 0.138(5) 0.080(4) 0.136(6) -0.057(4) 0.062(5) -0.022(4) F3 0.083(4) 0.140(6) 0.101(5) -0.050(4) -0.021(3) -0.012(4) F4 0.134(5) 0.087(4) 0.126(5) 0.005(4) 0.080(4) 0.007(4) F5 0.094(4) 0.107(5) 0.091(4) 0.022(4) -0.002(3) 0.006(4) F6 0.146(6) 0.072(4) 0.098(4) -0.004(3) 0.031(4) -0.046(4) F51 0.097(4) 0.103(5) 0.198(8) 0.019(5) 0.087(5) -0.014(4) F52 0.132(5) 0.075(4) 0.093(4) 0.031(3) 0.017(4) -0.011(4) F53 0.143(6) 0.078(4) 0.087(4) -0.014(3) 0.005(4) -0.031(4) F54 0.190(9) 0.130(8) 0.154(8) 0.047(6) 0.033(7) 0.012(7) F55 0.197(8) 0.148(7) 0.138(7) -0.059(5) 0.114(6) -0.054(6) F56 0.241(10) 0.120(7) 0.173(9) -0.068(6) 0.089(8) -0.080(7) N1 0.040(3) 0.051(4) 0.022(2) 0.002(2) 0.0113(19) -0.005(2) N51 0.059(3) 0.058(5) 0.023(2) 0.000(2) 0.010(2) -0.002(3) O1 0.074(4) 0.081(5) 0.058(3) -0.010(3) 0.040(3) -0.014(3) O2 0.070(4) 0.083(4) 0.063(4) 0.003(3) 0.013(3) 0.030(3) O4 0.062(4) 0.054(4) 0.118(6) -0.020(4) 0.031(3) -0.006(3) O5 0.070(4) 0.095(5) 0.095(5) 0.023(4) -0.003(3) 0.010(4) O6 0.072(4) 0.081(5) 0.078(4) -0.012(3) 0.034(3) 0.000(3) O7 0.041(3) 0.104(5) 0.071(4) 0.018(3) 0.002(3) -0.014(3) O8 0.084(5) 0.188(10) 0.128(7) 0.098(7) -0.026(5) -0.017(5) O51 0.053(3) 0.100(5) 0.116(5) 0.041(4) 0.029(3) 0.012(3) O52 0.113(5) 0.097(5) 0.043(3) 0.008(3) -0.006(3) -0.014(4) O53 0.083(5) 0.080(5) 0.116(6) -0.032(4) 0.030(4) -0.012(4) O54 0.098(6) 0.183(11) 0.129(7) 0.022(7) -0.015(5) 0.035(6) O55 0.107(6) 0.134(7) 0.076(5) -0.027(5) 0.041(4) -0.025(5) O57 0.059(4) 0.090(5) 0.067(4) -0.002(3) 0.028(3) -0.004(3) O58 0.076(5) 0.217(11) 0.059(4) 0.008(5) 0.011(3) -0.016(5) P1 0.0339(8) 0.0455(13) 0.0349(8) 0.0000(7) 0.0108(6) 0.0014(7) P51 0.0427(9) 0.0457(11) 0.0339(8) -0.0004(8) 0.0120(7) 0.0012(9) S1 0.0432(9) 0.0569(11) 0.0418(9) -0.0049(8) 0.0174(7) -0.0019(8) S51 0.0491(11) 0.0671(13) 0.0445(10) 0.0093(9) 0.0014(8) -0.0106(9) S52 0.0760(16) 0.094(2) 0.0640(14) -0.0009(13) 0.0080(12) 0.0015(14) S100 0.0600(13) 0.0517(12) 0.0673(13) 0.0013(10) 0.0143(10) -0.0044(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.372(10) . ? C1 C6 1.394(10) . ? C1 P1 1.805(7) . ? C2 C3 1.413(12) . ? C2 H2 0.93 . ? C3 C4 1.382(14) . ? C3 H3 0.93 . ? C4 C5 1.359(13) . ? C4 H4 0.93 . ? C5 C6 1.388(11) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.376(10) . ? C7 C12 1.389(9) . ? C7 P1 1.798(7) . ? C8 C9 1.384(12) . ? C8 H8 0.93 . ? C9 C10 1.376(13) . ? C9 H9 0.93 . ? C10 C11 1.366(13) . ? C10 H10 0.93 . ? C11 C12 1.379(11) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.363(9) . ? C13 C14 1.374(9) . ? C13 P1 1.817(6) . ? C14 C15 1.374(11) . ? C14 H14 0.93 . ? C15 C16 1.353(13) . ? C15 H15 0.93 . ? C16 C17 1.360(14) . ? C16 H16 0.93 . ? C17 C18 1.385(11) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 N1 1.488(9) . ? C19 C26 1.523(11) . ? C19 C20 1.528(11) . ? C19 H19 0.98 . ? C20 O8 1.180(10) . ? C20 O7 1.297(9) . ? C21 O7 1.442(9) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C26 C27 1.518(12) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 C32 1.380(12) . ? C27 C28 1.381(11) . ? C28 C29 1.398(12) . ? C28 H28 0.93 . ? C29 C30 1.334(12) . ? C29 H29 0.93 . ? C30 C31 1.382(12) . ? C30 O4 1.429(10) . ? C31 C32 1.369(13) . ? C31 H31 0.93 . ? C32 H32 0.93 . ? C33 F5 1.294(10) . ? C33 F4 1.307(10) . ? C33 F6 1.315(10) . ? C33 S100 1.800(9) . ? C34 F3 1.311(13) . ? C34 F2 1.310(11) . ? C34 F1 1.313(11) . ? C34 S1 1.842(9) . ? C51 C52 1.372(11) . ? C51 C56 1.384(10) . ? C51 P51 1.828(7) . ? C52 C53 1.402(14) . ? C52 H52 0.93 . ? C53 C54 1.383(17) . ? C53 H53 0.93 . ? C54 C55 1.323(15) . ? C54 H54 0.93 . ? C55 C56 1.380(12) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C57 C62 1.373(11) . ? C57 C58 1.407(10) . ? C57 P51 1.805(7) . ? C58 C59 1.393(12) . ? C58 H58 0.93 . ? C59 C60 1.363(15) . ? C59 H59 0.93 . ? C60 C61 1.361(14) . ? C60 H60 0.93 . ? C61 C62 1.394(13) . ? C61 H61 0.93 . ? C62 H62 0.93 . ? C63 C68 1.385(10) . ? C63 C64 1.394(10) . ? C63 P51 1.811(7) . ? C64 C65 1.381(11) . ? C64 H64 0.93 . ? C65 C66 1.372(13) . ? C65 H65 0.93 . ? C66 C67 1.360(12) . ? C66 H66 0.93 . ? C67 C68 1.355(11) . ? C67 H67 0.93 . ? C68 H68 0.93 . ? C69 N51 1.478(10) . ? C69 C77 1.497(11) . ? C69 C70 1.536(12) . ? C69 H69 0.98 . ? C70 C71 1.499(13) . ? C70 H70A 0.97 . ? C70 H70B 0.97 . ? C71 C72 1.349(13) . ? C71 C76 1.411(13) . ? C72 C73 1.382(15) . ? C72 H72 0.93 . ? C73 C74 1.387(13) . ? C73 H73 0.93 . ? C74 C75 1.366(13) . ? C74 O53 1.453(12) . ? C75 C76 1.368(13) . ? C75 H75 0.93 . ? C76 H76 0.93 . ? C77 O58 1.198(10) . ? C77 O57 1.307(10) . ? C78 F51 1.306(11) . ? C78 F52 1.312(11) . ? C78 F53 1.320(11) . ? C78 S51 1.839(9) . ? C84 F56 1.289(14) . ? C84 F54 1.302(16) . ? C84 F55 1.308(14) . ? C84 S52 1.837(14) . ? C89 O57 1.437(10) . ? C89 H89A 0.96 . ? C89 H89B 0.96 . ? C89 H89C 0.96 . ? Au2 N1 2.083(4) . ? Au2 P1 2.2367(17) . ? Au51 N51 2.077(5) . ? Au51 P51 2.2390(17) . ? N1 S1 1.544(6) . ? N51 S51 1.559(6) . ? O1 S1 1.426(5) . ? O2 S1 1.422(6) . ? O4 S100 1.572(6) . ? O5 S100 1.405(7) . ? O6 S100 1.416(6) . ? O51 S51 1.405(7) . ? O52 S51 1.439(6) . ? O53 S52 1.557(7) . ? O54 S52 1.384(8) . ? O55 S52 1.399(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.7(7) . . ? C2 C1 P1 118.8(6) . . ? C6 C1 P1 121.4(6) . . ? C1 C2 C3 120.5(8) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 118.2(8) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 121.7(8) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 120.0(8) . . ? C4 C5 H5 120 . . ? C6 C5 H5 120 . . ? C5 C6 C1 119.9(8) . . ? C5 C6 H6 120 . . ? C1 C6 H6 120 . . ? C8 C7 C12 118.1(6) . . ? C8 C7 P1 118.4(5) . . ? C12 C7 P1 123.5(5) . . ? C7 C8 C9 121.9(7) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C8 C9 C10 118.4(8) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C11 C10 C9 121.1(8) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C10 C11 C12 119.8(8) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C7 120.7(7) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C18 C13 C14 118.7(6) . . ? C18 C13 P1 118.4(5) . . ? C14 C13 P1 122.9(5) . . ? C13 C14 C15 121.3(8) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 118.9(8) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C15 C16 C17 121.1(7) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.6(8) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 120.2(8) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? N1 C19 C26 110.3(6) . . ? N1 C19 C20 113.3(6) . . ? C26 C19 C20 109.2(6) . . ? N1 C19 H19 108 . . ? C26 C19 H19 108 . . ? C20 C19 H19 108 . . ? O8 C20 O7 123.6(8) . . ? O8 C20 C19 123.0(8) . . ? O7 C20 C19 113.4(6) . . ? O7 C21 H21A 109.5 . . ? O7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C26 C19 114.1(7) . . ? C27 C26 H26A 108.7 . . ? C19 C26 H26A 108.7 . . ? C27 C26 H26B 108.7 . . ? C19 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C32 C27 C28 117.3(8) . . ? C32 C27 C26 121.2(7) . . ? C28 C27 C26 121.6(8) . . ? C27 C28 C29 122.2(8) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C30 C29 C28 117.7(8) . . ? C30 C29 H29 121.2 . . ? C28 C29 H29 121.2 . . ? C29 C30 C31 122.6(8) . . ? C29 C30 O4 118.6(8) . . ? C31 C30 O4 118.6(9) . . ? C32 C31 C30 118.7(9) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C27 121.6(8) . . ? C31 C32 H32 119.2 . . ? C27 C32 H32 119.2 . . ? F5 C33 F4 107.7(8) . . ? F5 C33 F6 108.1(8) . . ? F4 C33 F6 107.2(8) . . ? F5 C33 S100 112.3(6) . . ? F4 C33 S100 111.9(7) . . ? F6 C33 S100 109.5(6) . . ? F3 C34 F2 109.0(8) . . ? F3 C34 F1 109.3(9) . . ? F2 C34 F1 107.3(9) . . ? F3 C34 S1 110.3(7) . . ? F2 C34 S1 110.4(7) . . ? F1 C34 S1 110.6(7) . . ? C52 C51 C56 119.7(7) . . ? C52 C51 P51 123.0(6) . . ? C56 C51 P51 117.2(6) . . ? C51 C52 C53 119.4(9) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C54 C53 C52 118.9(10) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C55 C54 C53 121.4(10) . . ? C55 C54 H54 119.3 . . ? C53 C54 H54 119.3 . . ? C54 C55 C56 120.6(10) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C55 C56 C51 119.9(9) . . ? C55 C56 H56 120.1 . . ? C51 C56 H56 120.1 . . ? C62 C57 C58 119.7(7) . . ? C62 C57 P51 119.3(6) . . ? C58 C57 P51 121.0(6) . . ? C59 C58 C57 119.9(9) . . ? C59 C58 H58 120 . . ? C57 C58 H58 120 . . ? C60 C59 C58 119.7(9) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C61 C60 C59 120.3(8) . . ? C61 C60 H60 119.9 . . ? C59 C60 H60 119.9 . . ? C60 C61 C62 121.7(9) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C57 C62 C61 118.7(8) . . ? C57 C62 H62 120.6 . . ? C61 C62 H62 120.6 . . ? C68 C63 C64 119.2(7) . . ? C68 C63 P51 121.9(6) . . ? C64 C63 P51 118.9(5) . . ? C65 C64 C63 118.5(7) . . ? C65 C64 H64 120.7 . . ? C63 C64 H64 120.7 . . ? C66 C65 C64 121.3(8) . . ? C66 C65 H65 119.3 . . ? C64 C65 H65 119.3 . . ? C67 C66 C65 119.3(7) . . ? C67 C66 H66 120.3 . . ? C65 C66 H66 120.3 . . ? C68 C67 C66 120.9(8) . . ? C68 C67 H67 119.5 . . ? C66 C67 H67 119.5 . . ? C67 C68 C63 120.7(8) . . ? C67 C68 H68 119.7 . . ? C63 C68 H68 119.7 . . ? N51 C69 C77 108.6(6) . . ? N51 C69 C70 110.7(6) . . ? C77 C69 C70 110.5(7) . . ? N51 C69 H69 109 . . ? C77 C69 H69 109 . . ? C70 C69 H69 109 . . ? C71 C70 C69 116.3(7) . . ? C71 C70 H70A 108.2 . . ? C69 C70 H70A 108.2 . . ? C71 C70 H70B 108.2 . . ? C69 C70 H70B 108.2 . . ? H70A C70 H70B 107.4 . . ? C72 C71 C76 118.9(9) . . ? C72 C71 C70 124.0(9) . . ? C76 C71 C70 117.1(8) . . ? C71 C72 C73 122.7(10) . . ? C71 C72 H72 118.7 . . ? C73 C72 H72 118.7 . . ? C72 C73 C74 117.9(10) . . ? C72 C73 H73 121.1 . . ? C74 C73 H73 121.1 . . ? C75 C74 C73 120.3(9) . . ? C75 C74 O53 118.8(9) . . ? C73 C74 O53 120.2(10) . . ? C76 C75 C74 121.3(9) . . ? C76 C75 H75 119.3 . . ? C74 C75 H75 119.3 . . ? C75 C76 C71 118.9(9) . . ? C75 C76 H76 120.6 . . ? C71 C76 H76 120.6 . . ? O58 C77 O57 122.3(8) . . ? O58 C77 C69 125.0(8) . . ? O57 C77 C69 112.6(7) . . ? F51 C78 F52 108.2(8) . . ? F51 C78 F53 109.1(9) . . ? F52 C78 F53 107.7(9) . . ? F51 C78 S51 110.2(7) . . ? F52 C78 S51 111.1(7) . . ? F53 C78 S51 110.4(6) . . ? F56 C84 F54 114.4(13) . . ? F56 C84 F55 106.2(12) . . ? F54 C84 F55 110.0(13) . . ? F56 C84 S52 109.3(10) . . ? F54 C84 S52 108.5(10) . . ? F55 C84 S52 108.3(10) . . ? O57 C89 H89A 109.5 . . ? O57 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? O57 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N1 Au2 P1 178.86(16) . . ? N51 Au51 P51 175.51(19) . . ? C19 N1 S1 120.2(4) . . ? C19 N1 Au2 119.9(4) . . ? S1 N1 Au2 118.9(3) . . ? C69 N51 S51 122.2(4) . . ? C69 N51 Au51 118.9(4) . . ? S51 N51 Au51 118.9(3) . . ? C30 O4 S100 120.9(5) . . ? C20 O7 C21 117.2(7) . . ? C74 O53 S52 122.0(6) . . ? C77 O57 C89 116.9(7) . . ? C7 P1 C1 109.1(3) . . ? C7 P1 C13 104.8(3) . . ? C1 P1 C13 106.9(3) . . ? C7 P1 Au2 111.6(2) . . ? C1 P1 Au2 111.2(2) . . ? C13 P1 Au2 112.8(2) . . ? C57 P51 C63 106.3(4) . . ? C57 P51 C51 107.3(3) . . ? C63 P51 C51 106.5(3) . . ? C57 P51 Au51 114.2(2) . . ? C63 P51 Au51 114.5(2) . . ? C51 P51 Au51 107.6(2) . . ? O2 S1 O1 120.4(4) . . ? O2 S1 N1 110.7(3) . . ? O1 S1 N1 112.1(3) . . ? O2 S1 C34 104.0(5) . . ? O1 S1 C34 101.8(4) . . ? N1 S1 C34 106.1(4) . . ? O51 S51 O52 120.8(5) . . ? O51 S51 N51 110.9(4) . . ? O52 S51 N51 111.7(4) . . ? O51 S51 C78 102.3(5) . . ? O52 S51 C78 103.1(4) . . ? N51 S51 C78 106.1(4) . . ? O54 S52 O55 123.5(6) . . ? O54 S52 O53 107.4(6) . . ? O55 S52 O53 113.2(4) . . ? O54 S52 C84 104.4(7) . . ? O55 S52 C84 105.9(6) . . ? O53 S52 C84 99.3(5) . . ? O5 S100 O6 122.4(5) . . ? O5 S100 O4 106.6(4) . . ? O6 S100 O4 112.5(4) . . ? O5 S100 C33 105.7(4) . . ? O6 S100 C33 106.2(4) . . ? O4 S100 C33 101.2(4) . . ? data_V03MB57 _database_code_depnum_ccdc_archive 'CCDC 915633' #TrackingRef 'web_deposit_cif_file_1_EddyViseux_1355414187.V03MB57.cif' _audit_creation_date 2011-12-14T10:08:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H27 Au F3 N2 O4 P S, C6 H6' _chemical_formula_sum 'C37 H33 Au F3 N2 O4 P S' _chemical_formula_weight 886.65 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.5810(2) _cell_length_b 13.0950(3) _cell_length_c 13.0305(3) _cell_angle_alpha 90 _cell_angle_beta 114.4260(10) _cell_angle_gamma 90 _cell_volume 1799.25(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1404 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Rod _exptl_crystal_colour Clear _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.637 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.248 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.3962 _exptl_absorpt_correction_T_max 0.4847 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.184611E-1 _diffrn_orient_matrix_ub_12 -0.747856E-1 _diffrn_orient_matrix_ub_13 0.25509E-2 _diffrn_orient_matrix_ub_21 -0.258596E-1 _diffrn_orient_matrix_ub_22 0 _diffrn_orient_matrix_ub_23 -0.833389E-1 _diffrn_orient_matrix_ub_31 0.893559E-1 _diffrn_orient_matrix_ub_32 0.154509E-1 _diffrn_orient_matrix_ub_33 0.12347E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_number 22995 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 27.26 _diffrn_reflns_theta_full 27.26 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 7832 _reflns_number_gt 7040 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0876P)^2^+0.5059P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7832 _refine_ls_number_parameters 443 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.046 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.124(9) _refine_diff_density_max 2.021 _refine_diff_density_min -2.166 _refine_diff_density_rms 0.139 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.006 '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' 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 0.0903(6) 0.2412(6) 0.8357(5) 0.0476(13) Uani 1 1 d . . . C2 C -0.0015(7) 0.2873(8) 0.7392(7) 0.076(3) Uani 1 1 d . . . H2 H 0.019 0.3423 0.7047 0.091 Uiso 1 1 calc R . . C3 C -0.1254(6) 0.2477(13) 0.6963(7) 0.081(2) Uani 1 1 d . . . H3 H -0.1884 0.2778 0.6333 0.097 Uiso 1 1 calc R . . C4 C -0.1543(8) 0.1659(9) 0.7459(9) 0.083(3) Uani 1 1 d . . . H4 H -0.236 0.1393 0.7149 0.099 Uiso 1 1 calc R . . C5 C -0.0630(10) 0.1218(7) 0.8425(11) 0.081(3) Uani 1 1 d . . . H5 H -0.0834 0.0667 0.877 0.097 Uiso 1 1 calc R . . C6 C 0.0587(8) 0.1613(6) 0.8863(7) 0.0639(18) Uani 1 1 d . . . H6 H 0.12 0.1329 0.9515 0.077 Uiso 1 1 calc R . . C7 C 0.3314(5) 0.2424(6) 0.8144(5) 0.0485(13) Uani 1 1 d . . . C8 C 0.4562(7) 0.2686(7) 0.8478(8) 0.071(2) Uani 1 1 d . . . H8 H 0.4964 0.3095 0.911 0.085 Uiso 1 1 calc R . . C9 C 0.5230(9) 0.2336(7) 0.7865(10) 0.082(3) Uani 1 1 d . . . H9 H 0.6078 0.2511 0.8093 0.098 Uiso 1 1 calc R . . C10 C 0.4637(11) 0.1736(10) 0.6927(11) 0.092(3) Uani 1 1 d . . . H10 H 0.5074 0.1521 0.6507 0.11 Uiso 1 1 calc R . . C11 C 0.3383(10) 0.1453(12) 0.6613(11) 0.111(5) Uani 1 1 d . . . H11 H 0.2987 0.1023 0.5998 0.134 Uiso 1 1 calc R . . C12 C 0.2727(9) 0.1805(10) 0.7206(10) 0.095(4) Uani 1 1 d . . . H12 H 0.1879 0.1628 0.6977 0.114 Uiso 1 1 calc R . . C13 C 0.2369(6) 0.4288(5) 0.8707(6) 0.0519(15) Uani 1 1 d . . . C14 C 0.2251(7) 0.4701(6) 0.7697(7) 0.0609(17) Uani 1 1 d . . . H14 H 0.2214 0.4267 0.7119 0.073 Uiso 1 1 calc R . . C15 C 0.2187(9) 0.5756(7) 0.7521(9) 0.077(2) Uani 1 1 d . . . H15 H 0.2145 0.6024 0.6845 0.093 Uiso 1 1 calc R . . C16 C 0.2187(11) 0.6394(7) 0.8365(12) 0.092(3) Uani 1 1 d . . . H16 H 0.2138 0.7098 0.8258 0.111 Uiso 1 1 calc R . . C17 C 0.2259(12) 0.5996(8) 0.9349(14) 0.094(4) Uani 1 1 d . . . H17 H 0.2246 0.6431 0.9908 0.113 Uiso 1 1 calc R . . C18 C 0.2353(9) 0.4943(7) 0.9539(8) 0.069(2) Uani 1 1 d . . . H18 H 0.2405 0.4681 1.0221 0.083 Uiso 1 1 calc R . . C19 C 0.4190(7) 0.1265(7) 1.2929(7) 0.0621(18) Uani 1 1 d . . . H19 H 0.4656 0.1295 1.3751 0.075 Uiso 1 1 calc R . . C20 C 0.4547(8) 0.0266(8) 1.2529(8) 0.071(2) Uani 1 1 d . . . H20A H 0.5461 0.0253 1.2784 0.085 Uiso 1 1 calc R . . H20B H 0.432 -0.0293 1.2897 0.085 Uiso 1 1 calc R . . C21 C 0.3962(7) 0.0068(6) 1.1287(7) 0.0587(17) Uani 1 1 d . . . C22 C 0.2778(7) -0.0444(5) 1.0628(6) 0.0553(15) Uani 1 1 d . . . C23 C 0.2682(9) -0.0488(7) 0.9502(7) 0.0602(18) Uani 1 1 d . . . C24 C 0.4500(8) 0.0278(7) 1.0560(9) 0.073(2) Uani 1 1 d . . . H24 H 0.5278 0.06 1.0758 0.088 Uiso 1 1 calc R . . C25 C 0.1826(9) -0.0853(6) 1.0869(8) 0.070(2) Uani 1 1 d . . . H25 H 0.1877 -0.0836 1.16 0.084 Uiso 1 1 calc R . . C26 C 0.0790(11) -0.1291(8) 1.0006(12) 0.086(3) Uani 1 1 d . . . H26 H 0.0147 -0.1575 1.0166 0.103 Uiso 1 1 calc R . . C27 C 0.0689(11) -0.1315(8) 0.8898(10) 0.088(3) Uani 1 1 d . . . H27 H -0.0024 -0.1606 0.8334 0.106 Uiso 1 1 calc R . . C28 C 0.1605(11) -0.0923(7) 0.8638(9) 0.083(3) Uani 1 1 d . . . H28 H 0.153 -0.0938 0.7899 0.099 Uiso 1 1 calc R . . C29 C 0.4950(15) 0.3708(12) 1.3902(12) 0.106(4) Uani 1 1 d . . . C30 C 0.2795(9) 0.1338(7) 1.2665(8) 0.0681(19) Uani 1 1 d . . . C31 C 0.1129(13) 0.0664(12) 1.3018(14) 0.116(5) Uani 1 1 d . . . H31A H 0.0965 0.0197 1.3509 0.174 Uiso 1 1 calc R . . H31B H 0.068 0.0445 1.2251 0.174 Uiso 1 1 calc R . . H31C H 0.0848 0.1335 1.3105 0.174 Uiso 1 1 calc R . . C101 C -0.063(4) 1.0122(15) 0.5477(18) 0.175(12) Uani 1 1 d . . . H101 H -0.0705 1.0828 0.5497 0.21 Uiso 1 1 calc R . . C102 C -0.160(2) 0.949(2) 0.5463(19) 0.152(8) Uani 1 1 d . . . H102 H -0.2327 0.9759 0.5486 0.183 Uiso 1 1 calc R . . C103 C -0.145(2) 0.847(2) 0.541(2) 0.160(9) Uani 1 1 d . . . H103 H -0.2094 0.8038 0.5391 0.192 Uiso 1 1 calc R . . C104 C -0.044(3) 0.8081(17) 0.5397(17) 0.156(8) Uani 1 1 d . . . H104 H -0.0372 0.7377 0.5349 0.187 Uiso 1 1 calc R . . C105 C 0.0549(16) 0.871(3) 0.5451(14) 0.187(15) Uani 1 1 d . . . H105 H 0.131 0.8458 0.5477 0.224 Uiso 1 1 calc R . . C106 C 0.032(3) 0.973(3) 0.5462(18) 0.174(12) Uani 1 1 d . . . H106 H 0.0953 1.0165 0.5459 0.209 Uiso 1 1 calc R . . Au1 Au 0.354724(19) 0.25309(4) 1.077064(16) 0.05575(10) Uani 1 1 d . . . F1 F 0.4389(12) 0.3224(7) 1.4457(9) 0.150(4) Uani 1 1 d . . . F2 F 0.5766(12) 0.4367(8) 1.4603(8) 0.156(4) Uani 1 1 d . . . F3 F 0.4029(12) 0.4275(8) 1.3141(12) 0.151(4) Uani 1 1 d . . . N1 N 0.4555(6) 0.2151(5) 1.2462(4) 0.0617(15) Uani 1 1 d . . . N2 N 0.3735(8) -0.0052(6) 0.9493(7) 0.0725(19) Uani 1 1 d . . . H2A H 0.39 0.0009 0.891 0.087 Uiso 1 1 calc R . . O1 O 0.6550(5) 0.2309(8) 1.4176(5) 0.092(3) Uani 1 1 d . . . O2 O 0.6057(7) 0.3525(7) 1.2596(6) 0.094(2) Uani 1 1 d . . . O3 O 0.2492(8) 0.0687(7) 1.3303(8) 0.095(2) Uani 1 1 d . . . O4 O 0.2029(7) 0.1858(8) 1.1976(7) 0.101(2) Uani 1 1 d . . . P1 P 0.25001(15) 0.29309(13) 0.89634(14) 0.0473(3) Uani 1 1 d . . . S5 S 0.56359(18) 0.28651(18) 1.32392(16) 0.0674(5) 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 0.050(3) 0.043(4) 0.046(3) -0.003(3) 0.017(2) 0.000(3) C2 0.047(3) 0.102(7) 0.058(4) 0.019(4) 0.002(3) -0.007(4) C3 0.044(3) 0.116(7) 0.066(4) -0.007(8) 0.006(3) -0.015(7) C4 0.050(4) 0.112(7) 0.081(6) -0.033(6) 0.022(4) -0.010(4) C5 0.075(5) 0.064(5) 0.114(8) -0.012(5) 0.050(6) -0.008(4) C6 0.063(4) 0.053(4) 0.067(5) 0.006(3) 0.018(4) 0.002(3) C7 0.049(3) 0.039(3) 0.051(3) -0.003(3) 0.014(2) 0.003(3) C8 0.061(4) 0.060(6) 0.089(5) -0.018(4) 0.029(4) -0.009(4) C9 0.065(4) 0.068(7) 0.120(7) -0.024(5) 0.046(5) -0.013(4) C10 0.084(7) 0.102(7) 0.094(8) -0.019(6) 0.042(6) 0.006(6) C11 0.070(6) 0.152(12) 0.105(9) -0.065(9) 0.028(6) -0.006(6) C12 0.051(4) 0.127(9) 0.090(7) -0.054(6) 0.012(4) -0.005(5) C13 0.043(3) 0.044(3) 0.065(4) -0.001(3) 0.018(3) 0.001(2) C14 0.056(4) 0.059(4) 0.062(4) 0.011(3) 0.018(3) 0.010(3) C15 0.067(5) 0.062(5) 0.097(7) 0.025(5) 0.029(5) 0.012(4) C16 0.100(7) 0.045(4) 0.134(10) 0.005(5) 0.050(7) 0.017(4) C17 0.096(8) 0.060(5) 0.146(12) -0.026(7) 0.070(8) 0.005(5) C18 0.071(5) 0.066(5) 0.073(5) -0.007(4) 0.031(4) 0.008(4) C19 0.057(4) 0.076(5) 0.045(4) 0.012(3) 0.012(3) 0.003(3) C20 0.060(4) 0.076(5) 0.061(5) 0.012(4) 0.009(3) 0.018(4) C21 0.061(4) 0.053(3) 0.056(4) 0.017(3) 0.019(3) 0.014(3) C22 0.065(4) 0.049(3) 0.052(4) 0.013(3) 0.025(3) 0.016(3) C23 0.077(5) 0.050(4) 0.055(4) 0.008(3) 0.029(4) 0.017(4) C24 0.063(4) 0.069(5) 0.093(7) 0.020(4) 0.039(5) 0.019(4) C25 0.075(5) 0.062(4) 0.074(5) 0.009(4) 0.034(4) 0.002(4) C26 0.087(6) 0.066(5) 0.116(9) -0.012(5) 0.053(6) -0.018(5) C27 0.081(6) 0.073(6) 0.097(8) -0.029(5) 0.024(6) -0.008(5) C28 0.102(8) 0.063(5) 0.070(6) -0.016(4) 0.023(5) 0.014(5) C29 0.125(10) 0.112(9) 0.089(8) -0.017(7) 0.051(8) -0.028(8) C30 0.074(5) 0.068(4) 0.064(5) -0.009(4) 0.030(4) -0.006(4) C31 0.098(9) 0.119(10) 0.155(14) -0.020(10) 0.077(10) -0.026(8) C101 0.33(4) 0.098(11) 0.116(14) -0.025(10) 0.11(2) -0.017(18) C102 0.18(2) 0.17(2) 0.111(12) -0.001(15) 0.063(12) 0.048(17) C103 0.18(2) 0.140(17) 0.21(2) -0.047(16) 0.131(19) -0.047(15) C104 0.22(3) 0.130(13) 0.118(13) 0.015(11) 0.067(16) 0.063(16) C105 0.077(9) 0.38(5) 0.068(8) -0.043(16) -0.002(7) 0.055(16) C106 0.21(3) 0.22(3) 0.130(16) -0.075(19) 0.111(19) -0.11(2) Au1 0.05261(13) 0.06131(14) 0.03844(12) 0.00324(15) 0.00390(9) -0.00256(16) F1 0.228(12) 0.120(6) 0.176(9) -0.019(6) 0.158(10) -0.019(7) F2 0.223(11) 0.131(7) 0.108(6) -0.062(6) 0.062(7) -0.064(7) F3 0.152(9) 0.111(7) 0.182(11) -0.012(7) 0.060(8) 0.019(6) N1 0.059(3) 0.076(4) 0.026(2) 0.004(2) -0.006(2) -0.016(3) N2 0.090(5) 0.074(4) 0.064(4) 0.010(3) 0.043(4) 0.018(4) O1 0.068(3) 0.105(10) 0.061(4) 0.004(3) -0.015(3) -0.005(3) O2 0.083(4) 0.129(6) 0.065(4) -0.005(4) 0.024(3) -0.046(4) O3 0.091(5) 0.104(5) 0.101(5) 0.015(4) 0.050(4) -0.007(4) O4 0.060(4) 0.138(7) 0.096(5) 0.025(5) 0.024(3) 0.014(4) P1 0.0471(8) 0.0466(7) 0.0374(7) 0.0029(6) 0.0066(6) 0.0005(6) S5 0.0516(8) 0.0922(15) 0.0465(8) -0.0092(8) 0.0086(7) -0.0147(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C6 1.365(11) . ? C1 C2 1.404(10) . ? C1 P1 1.816(7) . ? C2 C3 1.406(11) . ? C2 H2 0.93 . ? C3 C4 1.362(18) . ? C3 H3 0.93 . ? C4 C5 1.391(16) . ? C4 H4 0.93 . ? C5 C6 1.383(13) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C8 1.370(10) . ? C7 C12 1.388(11) . ? C7 P1 1.817(6) . ? C8 C9 1.399(12) . ? C8 H8 0.93 . ? C9 C10 1.374(16) . ? C9 H9 0.93 . ? C10 C11 1.387(16) . ? C10 H10 0.93 . ? C11 C12 1.368(15) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C14 1.376(11) . ? C13 C18 1.388(11) . ? C13 P1 1.803(7) . ? C14 C15 1.397(12) . ? C14 H14 0.93 . ? C15 C16 1.382(16) . ? C15 H15 0.93 . ? C16 C17 1.354(19) . ? C16 H16 0.93 . ? C17 C18 1.398(15) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 N1 1.452(11) . ? C19 C30 1.509(13) . ? C19 C20 1.528(14) . ? C19 H19 0.98 . ? C20 C21 1.496(12) . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C21 C24 1.360(12) . ? C21 C22 1.447(12) . ? C22 C25 1.374(11) . ? C22 C23 1.425(11) . ? C23 N2 1.351(13) . ? C23 C28 1.410(15) . ? C24 N2 1.374(13) . ? C24 H24 0.93 . ? C25 C26 1.385(15) . ? C25 H25 0.93 . ? C26 C27 1.399(17) . ? C26 H26 0.93 . ? C27 C28 1.342(17) . ? C27 H27 0.93 . ? C28 H28 0.93 . ? C29 F1 1.317(15) . ? C29 F2 1.327(16) . ? C29 F3 1.341(19) . ? C29 S5 1.778(15) . ? C30 O4 1.183(12) . ? C30 O3 1.334(12) . ? C31 O3 1.465(16) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C101 C106 1.23(4) . ? C101 C102 1.38(4) . ? C101 H101 0.93 . ? C102 C103 1.35(4) . ? C102 H102 0.93 . ? C103 C104 1.28(3) . ? C103 H103 0.93 . ? C104 C105 1.39(4) . ? C104 H104 0.93 . ? C105 C106 1.35(4) . ? C105 H105 0.93 . ? C106 H106 0.93 . ? Au1 N1 2.084(5) . ? Au1 P1 2.2201(16) . ? N1 S5 1.555(6) . ? N2 H2A 0.86 . ? O1 S5 1.440(7) . ? O2 S5 1.423(7) . ? 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 C6 C1 C2 120.5(7) . . ? C6 C1 P1 120.3(5) . . ? C2 C1 P1 119.1(6) . . ? C1 C2 C3 117.9(9) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 120.8(9) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.8(8) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 118.8(10) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? C1 C6 C5 121.2(8) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C12 119.6(7) . . ? C8 C7 P1 117.2(6) . . ? C12 C7 P1 123.2(6) . . ? C7 C8 C9 119.7(8) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C10 C9 C8 120.3(9) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 119.5(10) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 120.1(10) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C7 120.7(9) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C14 C13 C18 118.5(7) . . ? C14 C13 P1 122.1(6) . . ? C18 C13 P1 119.4(6) . . ? C13 C14 C15 121.5(9) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 119.0(9) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 120.0(9) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C16 C17 C18 121.2(10) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 C17 119.7(10) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? N1 C19 C30 108.9(7) . . ? N1 C19 C20 111.9(7) . . ? C30 C19 C20 113.1(7) . . ? N1 C19 H19 107.6 . . ? C30 C19 H19 107.6 . . ? C20 C19 H19 107.6 . . ? C21 C20 C19 116.9(6) . . ? C21 C20 H20A 108.1 . . ? C19 C20 H20A 108.1 . . ? C21 C20 H20B 108.1 . . ? C19 C20 H20B 108.1 . . ? H20A C20 H20B 107.3 . . ? C24 C21 C22 105.9(8) . . ? C24 C21 C20 125.8(8) . . ? C22 C21 C20 128.1(7) . . ? C25 C22 C23 119.4(8) . . ? C25 C22 C21 134.2(8) . . ? C23 C22 C21 106.4(7) . . ? N2 C23 C28 131.9(9) . . ? N2 C23 C22 107.8(8) . . ? C28 C23 C22 120.3(9) . . ? C21 C24 N2 110.6(8) . . ? C21 C24 H24 124.7 . . ? N2 C24 H24 124.7 . . ? C22 C25 C26 118.8(9) . . ? C22 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C25 C26 C27 121.5(9) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 121.0(10) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C23 118.9(10) . . ? C27 C28 H28 120.6 . . ? C23 C28 H28 120.6 . . ? F1 C29 F2 107.9(12) . . ? F1 C29 F3 104.6(14) . . ? F2 C29 F3 105.7(14) . . ? F1 C29 S5 112.9(11) . . ? F2 C29 S5 113.8(11) . . ? F3 C29 S5 111.3(10) . . ? O4 C30 O3 122.2(9) . . ? O4 C30 C19 127.2(9) . . ? O3 C30 C19 110.5(8) . . ? O3 C31 H31A 109.5 . . ? O3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C106 C101 C102 118(2) . . ? C106 C101 H101 120.9 . . ? C102 C101 H101 120.9 . . ? C103 C102 C101 118(2) . . ? C103 C102 H102 120.9 . . ? C101 C102 H102 120.9 . . ? C104 C103 C102 122(2) . . ? C104 C103 H103 119 . . ? C102 C103 H103 119 . . ? C103 C104 C105 120(2) . . ? C103 C104 H104 120 . . ? C105 C104 H104 120 . . ? C106 C105 C104 115.1(18) . . ? C106 C105 H105 122.4 . . ? C104 C105 H105 122.4 . . ? C101 C106 C105 126(2) . . ? C101 C106 H106 116.8 . . ? C105 C106 H106 116.8 . . ? N1 Au1 P1 179.1(2) . . ? C19 N1 S5 120.2(5) . . ? C19 N1 Au1 120.1(5) . . ? S5 N1 Au1 119.5(4) . . ? C23 N2 C24 109.3(7) . . ? C23 N2 H2A 125.4 . . ? C24 N2 H2A 125.4 . . ? C30 O3 C31 112.9(10) . . ? C13 P1 C1 107.2(3) . . ? C13 P1 C7 106.0(4) . . ? C1 P1 C7 106.8(3) . . ? C13 P1 Au1 113.3(3) . . ? C1 P1 Au1 112.6(2) . . ? C7 P1 Au1 110.4(2) . . ? O2 S5 O1 119.7(5) . . ? O2 S5 N1 111.2(4) . . ? O1 S5 N1 111.1(5) . . ? O2 S5 C29 103.9(6) . . ? O1 S5 C29 102.8(6) . . ? N1 S5 C29 106.7(6) . . ? data_V05MB60d _database_code_depnum_ccdc_archive 'CCDC 915634' #TrackingRef 'web_deposit_cif_file_2_EddyViseux_1355414187.V05MB60d.cif' _audit_creation_date 2012-03-12T13:39:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H42 Au2 F6 N4 O6 P2 S2, 5(C6H6)' _chemical_formula_sum 'C72 H72 Au2 F6 N4 O6 P2 S2' _chemical_formula_weight 1723.33 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' _symmetry_space_group_name_Hall 'P 1' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.5355(3) _cell_length_b 11.8539(4) _cell_length_c 15.7927(5) _cell_angle_alpha 94.235(2) _cell_angle_beta 100.1060(10) _cell_angle_gamma 112.490(2) _cell_volume 1772.35(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 26016 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description Plate _exptl_crystal_colour Clear _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 854 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4158 _exptl_absorpt_correction_T_max 0.6283 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.856296E-1 _diffrn_orient_matrix_ub_12 0.90589E-2 _diffrn_orient_matrix_ub_13 -0.227607E-1 _diffrn_orient_matrix_ub_21 -0.556272E-1 _diffrn_orient_matrix_ub_22 -0.78691E-1 _diffrn_orient_matrix_ub_23 -0.415127E-1 _diffrn_orient_matrix_ub_31 -0.25865E-1 _diffrn_orient_matrix_ub_32 0.476162E-1 _diffrn_orient_matrix_ub_33 -0.44691E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_unetI/netI 0.0469 _diffrn_reflns_number 25196 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 14989 _reflns_number_gt 13710 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0258P)^2^+2.1148P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 14989 _refine_ls_number_parameters 847 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(5) _refine_diff_density_max 0.988 _refine_diff_density_min -1.94 _refine_diff_density_rms 0.178 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.006 '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' 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 0.0506(8) 0.6234(7) 0.7779(5) 0.0237(16) Uani 1 1 d . . . C2 C -0.0800(9) 0.5319(8) 0.7358(6) 0.0310(19) Uani 1 1 d . . . H2 H -0.1643 0.5413 0.7404 0.037 Uiso 1 1 calc R . . C3 C -0.0859(8) 0.4284(7) 0.6878(6) 0.0364(19) Uani 1 1 d . . . H3 H -0.175 0.3651 0.6602 0.044 Uiso 1 1 calc R . . C4 C 0.0358(10) 0.4145(8) 0.6788(6) 0.040(2) Uani 1 1 d . . . H4 H 0.0307 0.3437 0.6435 0.048 Uiso 1 1 calc R . . C5 C 0.1637(9) 0.5038(8) 0.7213(6) 0.044(2) Uani 1 1 d . . . H5 H 0.2471 0.4929 0.7165 0.053 Uiso 1 1 calc R . . C6 C 0.1742(8) 0.6088(7) 0.7707(5) 0.0317(16) Uani 1 1 d . . . H6 H 0.2638 0.6704 0.7994 0.038 Uiso 1 1 calc R . . C7 C 0.1198(10) 0.7495(8) 0.9546(6) 0.0257(18) Uani 1 1 d . . . C8 C 0.0243(10) 0.6860(10) 1.0004(7) 0.045(2) Uani 1 1 d . . . H8 H -0.0733 0.653 0.974 0.054 Uiso 1 1 calc R . . C9 C 0.0676(10) 0.6685(10) 1.0857(7) 0.045(2) Uani 1 1 d . . . H9 H 0.0009 0.6195 1.1158 0.054 Uiso 1 1 calc R . . C10 C 0.2072(10) 0.7230(9) 1.1247(6) 0.039(2) Uani 1 1 d . . . H10 H 0.2376 0.7149 1.1834 0.046 Uiso 1 1 calc R . . C11 C 0.3038(10) 0.7891(8) 1.0805(6) 0.0358(19) Uani 1 1 d . . . H11 H 0.4005 0.8276 1.109 0.043 Uiso 1 1 calc R . . C12 C 0.2628(10) 0.8010(8) 0.9946(6) 0.0330(19) Uani 1 1 d . . . H12 H 0.3311 0.8436 0.9632 0.04 Uiso 1 1 calc R . . C13 C 0.1904(7) 0.8942(6) 0.8117(4) 0.0236(14) Uani 1 1 d . . . C14 C 0.1548(6) 1.0093(5) 0.8277(4) 0.0270(12) Uani 1 1 d . . . H14 H 0.0877 0.9925 0.8675 0.032 Uiso 1 1 calc R . . C15 C 0.0859(9) 1.0381(7) 0.7413(5) 0.0428(19) Uani 1 1 d . . . H15A H 0.1255 1.0186 0.6926 0.051 Uiso 1 1 calc R . . H15B H -0.0174 0.9899 0.7268 0.051 Uiso 1 1 calc R . . C16 C 0.1213(8) 1.1754(7) 0.7589(5) 0.0479(17) Uani 1 1 d . . . H16A H 0.1701 1.2184 0.715 0.057 Uiso 1 1 calc R . . H16B H 0.0347 1.1904 0.7572 0.057 Uiso 1 1 calc R . . C17 C 0.2165(7) 1.2200(6) 0.8486(4) 0.0410(15) Uani 1 1 d . . . H17A H 0.2929 1.3021 0.8511 0.049 Uiso 1 1 calc R . . H17B H 0.1626 1.2258 0.893 0.049 Uiso 1 1 calc R . . C18 C 0.3484(6) 1.1373(6) 0.9521(4) 0.0309(13) Uani 1 1 d . . . H18A H 0.4291 1.2188 0.9671 0.037 Uiso 1 1 calc R . . H18B H 0.3873 1.0734 0.9541 0.037 Uiso 1 1 calc R . . C19 C 0.2628(9) 1.1246(9) 1.0231(6) 0.0346(19) Uani 1 1 d . . . H19A H 0.2218 1.1871 1.0222 0.042 Uiso 1 1 calc R . . H19B H 0.1846 1.0416 1.0117 0.042 Uiso 1 1 calc R . . C20 C 0.3576(10) 1.1429(8) 1.1109(6) 0.0286(19) Uani 1 1 d . . . C21 C -0.0438(8) 1.3899(7) 1.2164(5) 0.0239(16) Uani 1 1 d . . . C22 C -0.1609(8) 1.4168(7) 1.2224(5) 0.0324(17) Uani 1 1 d . . . H22 H -0.2529 1.3603 1.193 0.039 Uiso 1 1 calc R . . C23 C -0.1413(10) 1.5268(8) 1.2717(6) 0.042(2) Uani 1 1 d . . . H23 H -0.2197 1.5461 1.2765 0.05 Uiso 1 1 calc R . . C24 C -0.0065(10) 1.6077(8) 1.3138(6) 0.045(2) Uani 1 1 d . . . H24 H 0.0067 1.683 1.3471 0.054 Uiso 1 1 calc R . . C25 C 0.1078(8) 1.5822(7) 1.3087(5) 0.0354(18) Uani 1 1 d . . . H25 H 0.1995 1.6387 1.3385 0.042 Uiso 1 1 calc R . . C26 C 0.0878(9) 1.4709(8) 1.2586(6) 0.0319(19) Uani 1 1 d . . . H26 H 0.1667 1.4522 1.2543 0.038 Uiso 1 1 calc R . . C27 C -0.1330(9) 1.2520(8) 1.0443(6) 0.0237(18) Uani 1 1 d . . . C28 C -0.2721(9) 1.2131(8) 1.0017(6) 0.0315(19) Uani 1 1 d . . . H28 H -0.3444 1.1734 1.0313 0.038 Uiso 1 1 calc R . . C29 C -0.3083(10) 1.2309(8) 0.9165(6) 0.038(2) Uani 1 1 d . . . H29 H -0.4046 1.2029 0.888 0.046 Uiso 1 1 calc R . . C30 C -0.2041(10) 1.2895(8) 0.8732(6) 0.035(2) Uani 1 1 d . . . H30 H -0.229 1.3021 0.815 0.042 Uiso 1 1 calc R . . C31 C -0.0630(10) 1.3301(9) 0.9143(7) 0.039(2) Uani 1 1 d . . . H31 H 0.0085 1.3698 0.8842 0.047 Uiso 1 1 calc R . . C32 C -0.0276(9) 1.3125(8) 0.9989(6) 0.0296(18) Uani 1 1 d . . . H32 H 0.0689 1.3413 1.0272 0.035 Uiso 1 1 calc R . . C33 C -0.2205(7) 1.1321(6) 1.1971(5) 0.0296(16) Uani 1 1 d . . . C34 C -0.2204(6) 1.0028(5) 1.1996(3) 0.0243(11) Uani 1 1 d . . . H34 H -0.3153 0.9451 1.2059 0.029 Uiso 1 1 calc R . . C35 C -0.1087(7) 0.9966(6) 1.2739(4) 0.0314(15) Uani 1 1 d . . . H35A H -0.0209 1.0726 1.2851 0.038 Uiso 1 1 calc R . . H35B H -0.1438 0.9853 1.3282 0.038 Uiso 1 1 calc R . . C36 C -0.0840(9) 0.8838(9) 1.2402(5) 0.0537(19) Uani 1 1 d . . . H36A H 0.0177 0.9013 1.2546 0.064 Uiso 1 1 calc R . . H36B H -0.1349 0.8117 1.267 0.064 Uiso 1 1 calc R . . C37 C -0.1377(8) 0.8589(7) 1.1451(4) 0.0486(17) Uani 1 1 d . . . H37A H -0.0616 0.8619 1.1152 0.058 Uiso 1 1 calc R . . H37B H -0.215 0.7755 1.1278 0.058 Uiso 1 1 calc R . . C38 C -0.3087(6) 0.9082(6) 1.0458(4) 0.0285(12) Uani 1 1 d . . . H38A H -0.3519 0.969 1.041 0.034 Uiso 1 1 calc R . . H38B H -0.3807 0.8291 1.054 0.034 Uiso 1 1 calc R . . C39 C -0.2594(9) 0.8894(8) 0.9630(5) 0.0330(18) Uani 1 1 d . . . H39A H -0.178 0.9658 0.9603 0.04 Uiso 1 1 calc R . . H39B H -0.226 0.822 0.9663 0.04 Uiso 1 1 calc R . . C40 C -0.3701(9) 0.8583(8) 0.8796(6) 0.0273(18) Uani 1 1 d . . . C41 C 0.4065(10) 1.0506(9) 1.3036(7) 0.041(2) Uani 1 1 d . . . C42 C -0.3969(11) 0.9618(10) 0.6960(7) 0.044(2) Uani 1 1 d . . . C101 C 0.4100(11) 0.4954(10) 0.0585(8) 0.061(3) Uani 1 1 d . . . H101 H 0.3469 0.4819 0.0966 0.073 Uiso 1 1 calc R . . C102 C 0.3838(11) 0.5405(9) -0.0189(7) 0.059(3) Uani 1 1 d . . . H102 H 0.3029 0.5585 -0.0341 0.07 Uiso 1 1 calc R . . C103 C 0.4787(10) 0.5590(8) -0.0737(7) 0.054(2) Uani 1 1 d . . . H103 H 0.4636 0.5906 -0.1264 0.064 Uiso 1 1 calc R . . C104 C 0.5910(11) 0.5317(9) -0.0512(7) 0.054(3) Uani 1 1 d . . . H104 H 0.6535 0.543 -0.0895 0.064 Uiso 1 1 calc R . . C105 C 0.6195(10) 0.4886(8) 0.0238(7) 0.051(2) Uani 1 1 d . . . H105 H 0.7011 0.4715 0.0379 0.061 Uiso 1 1 calc R . . C106 C 0.5294(10) 0.4701(8) 0.0792(6) 0.052(2) Uani 1 1 d . . . H106 H 0.5485 0.44 0.1319 0.062 Uiso 1 1 calc R . . C111 C 0.5361(11) 0.4439(11) 0.6895(8) 0.058(3) Uani 1 1 d . . . H111 H 0.5569 0.5184 0.7267 0.07 Uiso 1 1 calc R . . C112 C 0.5566(13) 0.4502(13) 0.6075(9) 0.065(3) Uani 1 1 d . . . H112 H 0.5978 0.5271 0.5878 0.077 Uiso 1 1 calc R . . C113 C 0.5136(15) 0.3369(14) 0.5529(9) 0.074(4) Uani 1 1 d . . . H113 H 0.5139 0.3357 0.4927 0.088 Uiso 1 1 calc R . . C114 C 0.4714(14) 0.2285(12) 0.5860(10) 0.075(4) Uani 1 1 d . . . H114 H 0.4548 0.1532 0.5513 0.09 Uiso 1 1 calc R . . C115 C 0.4537(13) 0.2295(12) 0.6681(11) 0.079(4) Uani 1 1 d . . . H115 H 0.4168 0.1535 0.6896 0.094 Uiso 1 1 calc R . . C116 C 0.4875(10) 0.3363(11) 0.7205(8) 0.058(3) Uani 1 1 d . . . H116 H 0.4769 0.3357 0.779 0.069 Uiso 1 1 calc R . . C121 C 0.4584(14) 0.6459(13) 0.4485(9) 0.064(3) Uani 1 1 d . . . H121 H 0.4246 0.6334 0.5005 0.076 Uiso 1 1 calc R . . C122 C 0.5191(14) 0.7624(12) 0.4266(8) 0.065(3) Uani 1 1 d . . . H122 H 0.5378 0.8323 0.4679 0.078 Uiso 1 1 calc R . . C123 C 0.5534(11) 0.7812(10) 0.3475(8) 0.056(3) Uani 1 1 d . . . H123 H 0.5889 0.8622 0.3329 0.067 Uiso 1 1 calc R . . C124 C 0.5355(10) 0.6801(10) 0.2889(7) 0.061(3) Uani 1 1 d . . . H124 H 0.5601 0.6919 0.2342 0.073 Uiso 1 1 calc R . . C125 C 0.4821(11) 0.5624(11) 0.3101(8) 0.058(3) Uani 1 1 d . . . H125 H 0.468 0.4929 0.2698 0.069 Uiso 1 1 calc R . . C126 C 0.4496(13) 0.5474(10) 0.3898(8) 0.056(3) Uani 1 1 d . . . H126 H 0.4201 0.4672 0.4059 0.067 Uiso 1 1 calc R . . C131 C 0.8284(14) 0.2493(16) 0.4550(8) 0.079(4) Uani 1 1 d . . . H131 H 0.7496 0.2693 0.4373 0.095 Uiso 1 1 calc R . . C132 C 0.8138(17) 0.1512(11) 0.4961(7) 0.086(5) Uani 1 1 d . . . H132 H 0.7243 0.1015 0.5061 0.104 Uiso 1 1 calc R . . C133 C 0.922(2) 0.1237(12) 0.5223(8) 0.088(6) Uani 1 1 d . . . H133 H 0.911 0.0554 0.5526 0.105 Uiso 1 1 calc R . . C134 C 1.0523(17) 0.1930(16) 0.5063(10) 0.086(5) Uani 1 1 d . . . H134 H 1.1297 0.1709 0.5235 0.103 Uiso 1 1 calc R . . C135 C 1.0680(18) 0.2922(19) 0.4660(11) 0.112(7) Uani 1 1 d . . . H135 H 1.157 0.3435 0.4561 0.134 Uiso 1 1 calc R . . C136 C 0.9499(15) 0.3172(13) 0.4395(7) 0.069(3) Uani 1 1 d . . . H136 H 0.9578 0.3853 0.4094 0.083 Uiso 1 1 calc R . . C141 C 0.997(3) 0.6738(19) 0.5485(12) 0.138(10) Uani 1 1 d . . . H141 H 0.9626 0.5989 0.5717 0.165 Uiso 1 1 calc R . . C142 C 1.138(3) 0.733(2) 0.5479(9) 0.122(9) Uani 1 1 d . . . H142 H 1.2036 0.6999 0.5712 0.146 Uiso 1 1 calc R . . C143 C 1.1812(13) 0.8368(19) 0.5144(10) 0.112(7) Uani 1 1 d . . . H143 H 1.2785 0.8767 0.5145 0.134 Uiso 1 1 calc R . . C144 C 1.0944(17) 0.8895(12) 0.4801(9) 0.078(4) Uani 1 1 d . . . H144 H 1.1288 0.9637 0.4561 0.093 Uiso 1 1 calc R . . C145 C 0.9595(14) 0.8331(11) 0.4814(8) 0.062(3) Uani 1 1 d . . . H145 H 0.8963 0.8684 0.4581 0.074 Uiso 1 1 calc R . . C146 C 0.9083(19) 0.7262(14) 0.5148(11) 0.096(5) Uani 1 1 d . . . H146 H 0.8109 0.6881 0.5147 0.115 Uiso 1 1 calc R . . Au1 Au -0.147812(14) 0.780705(13) 0.820544(11) 0.02574(8) Uani 1 1 d . . . Au52 Au 0.123293(13) 1.205179(13) 1.172847(10) 0.02486(8) Uani 1 1 d . . . F1 F 0.2821(7) 0.9598(6) 1.2774(6) 0.088(2) Uani 1 1 d . . . F2 F 0.4918(9) 1.0195(7) 1.2681(5) 0.085(2) Uani 1 1 d . . . F3 F 0.4455(8) 1.0588(6) 1.3885(4) 0.0663(18) Uani 1 1 d . . . F4 F -0.4392(8) 0.9659(6) 0.6132(4) 0.0651(17) Uani 1 1 d . . . F5 F -0.2629(8) 1.0424(7) 0.7202(7) 0.102(3) Uani 1 1 d . . . F6 F -0.4698(11) 0.9999(8) 0.7393(5) 0.103(3) Uani 1 1 d . . . N1 N -0.3276(8) 0.8194(8) 0.8082(5) 0.0296(18) Uani 1 1 d . . . N2 N 0.2741(5) 1.1265(4) 0.8629(3) 0.0280(9) Uani 1 1 d . . . N3 N 0.3045(8) 1.1696(8) 1.1816(5) 0.0271(17) Uani 1 1 d U . . N4 N -0.1894(5) 0.9525(4) 1.1202(3) 0.0257(10) Uani 1 1 d . . . O1 O -0.5614(7) 0.7334(7) 0.6974(5) 0.0494(18) Uani 1 1 d . . . O2 O -0.3349(8) 0.7779(7) 0.6533(5) 0.0443(17) Uani 1 1 d . . . O3 O -0.4792(7) 0.8670(7) 0.8773(4) 0.0385(16) Uani 1 1 d . . . O4 O 0.3237(8) 1.2240(7) 1.3373(4) 0.0476(18) Uani 1 1 d . . . O5 O 0.5430(7) 1.2796(7) 1.2883(5) 0.0486(17) Uani 1 1 d . . . O6 O 0.4683(7) 1.1289(7) 1.1201(5) 0.0452(18) Uani 1 1 d . . . P1 P 0.0572(3) 0.7601(2) 0.84086(16) 0.0242(5) Uani 1 1 d . . . P52 P -0.0729(2) 1.2411(2) 1.15691(15) 0.0212(5) Uani 1 1 d . . . S1 S -0.4145(3) 0.8043(2) 0.71104(17) 0.0327(5) Uani 1 1 d . . . S51 S 0.4001(3) 1.1981(2) 1.27975(17) 0.0318(5) 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 0.024(3) 0.023(3) 0.022(3) 0.007(2) 0.006(2) 0.006(3) C2 0.031(4) 0.028(4) 0.035(4) 0.002(3) 0.009(3) 0.013(3) C3 0.033(4) 0.027(4) 0.037(4) 0.003(3) -0.005(3) 0.005(3) C4 0.066(6) 0.035(4) 0.028(4) 0.000(3) 0.008(4) 0.032(4) C5 0.051(5) 0.052(5) 0.041(4) 0.002(4) 0.008(4) 0.035(4) C6 0.030(4) 0.028(4) 0.041(4) -0.001(3) 0.011(3) 0.016(3) C7 0.039(4) 0.018(3) 0.024(4) 0.007(3) 0.007(3) 0.014(3) C8 0.028(4) 0.050(5) 0.046(5) 0.004(4) 0.002(4) 0.008(4) C9 0.034(5) 0.063(6) 0.033(4) 0.021(4) 0.009(3) 0.010(4) C10 0.043(5) 0.050(5) 0.023(4) 0.002(3) 0.003(3) 0.021(4) C11 0.030(4) 0.040(4) 0.032(4) 0.007(3) 0.006(3) 0.008(3) C12 0.028(4) 0.037(4) 0.032(4) 0.010(3) 0.006(3) 0.011(3) C13 0.021(3) 0.025(3) 0.026(3) 0.009(3) 0.005(2) 0.009(2) C14 0.023(3) 0.019(3) 0.038(4) 0.005(3) 0.006(3) 0.007(2) C15 0.048(4) 0.037(4) 0.038(4) 0.008(3) -0.006(3) 0.017(4) C16 0.053(5) 0.038(4) 0.053(4) 0.013(3) 0.003(3) 0.021(3) C17 0.053(4) 0.028(3) 0.046(4) 0.008(3) 0.020(3) 0.017(3) C18 0.023(3) 0.039(4) 0.027(3) -0.003(3) 0.006(2) 0.010(3) C19 0.026(4) 0.050(5) 0.032(4) 0.010(3) 0.007(3) 0.018(3) C20 0.032(4) 0.031(4) 0.030(4) 0.009(3) 0.016(3) 0.014(3) C21 0.028(4) 0.023(3) 0.025(3) 0.007(3) 0.009(3) 0.012(3) C22 0.029(4) 0.031(4) 0.037(4) 0.010(3) 0.007(3) 0.012(3) C23 0.053(5) 0.044(5) 0.040(4) 0.003(4) 0.009(4) 0.032(4) C24 0.072(6) 0.038(5) 0.027(4) 0.006(3) 0.005(4) 0.027(4) C25 0.035(4) 0.027(4) 0.031(3) -0.004(3) -0.004(3) 0.005(3) C26 0.032(4) 0.030(4) 0.029(4) 0.006(3) 0.006(3) 0.008(3) C27 0.017(3) 0.033(4) 0.026(4) 0.001(3) 0.008(3) 0.015(3) C28 0.024(4) 0.043(4) 0.032(4) 0.012(3) 0.011(3) 0.015(3) C29 0.033(4) 0.052(5) 0.029(4) 0.009(3) 0.002(3) 0.019(4) C30 0.038(4) 0.041(4) 0.032(4) 0.021(3) 0.016(3) 0.016(3) C31 0.028(4) 0.049(5) 0.043(5) 0.018(4) 0.015(3) 0.015(3) C32 0.018(3) 0.042(4) 0.030(4) 0.019(3) 0.013(3) 0.009(3) C33 0.029(3) 0.024(3) 0.042(4) 0.008(3) 0.017(3) 0.013(3) C34 0.024(3) 0.028(3) 0.020(3) 0.002(2) 0.009(2) 0.008(2) C35 0.034(3) 0.032(4) 0.029(3) 0.009(3) 0.009(3) 0.013(3) C36 0.061(5) 0.063(5) 0.051(4) 0.008(4) 0.005(4) 0.044(5) C37 0.068(5) 0.046(4) 0.041(4) 0.001(3) 0.001(3) 0.039(4) C38 0.024(3) 0.032(3) 0.029(3) -0.001(2) 0.006(2) 0.011(2) C39 0.033(4) 0.043(4) 0.024(3) -0.005(3) 0.011(3) 0.017(3) C40 0.019(4) 0.032(4) 0.031(4) 0.004(3) 0.005(3) 0.010(3) C41 0.041(5) 0.042(5) 0.037(4) 0.007(3) 0.007(3) 0.015(4) C42 0.046(5) 0.050(5) 0.033(4) 0.008(4) -0.001(4) 0.023(5) C101 0.056(6) 0.067(7) 0.059(6) -0.008(5) 0.003(4) 0.031(5) C102 0.053(5) 0.045(6) 0.067(6) -0.006(5) -0.011(4) 0.022(5) C103 0.053(6) 0.034(5) 0.058(5) 0.016(4) 0.000(4) 0.005(4) C104 0.050(5) 0.050(5) 0.048(5) 0.005(4) 0.016(4) 0.005(4) C105 0.043(5) 0.044(5) 0.064(6) 0.001(4) 0.003(4) 0.020(4) C106 0.044(5) 0.049(5) 0.046(4) 0.006(4) -0.002(4) 0.006(4) C111 0.049(6) 0.061(6) 0.068(6) 0.001(5) 0.010(5) 0.029(5) C112 0.054(6) 0.083(8) 0.067(7) 0.036(6) 0.017(5) 0.033(6) C113 0.085(10) 0.096(11) 0.033(6) -0.005(6) 0.001(6) 0.038(8) C114 0.065(7) 0.049(6) 0.106(11) -0.001(7) 0.009(7) 0.025(5) C115 0.064(7) 0.063(8) 0.121(12) 0.048(8) 0.025(7) 0.030(6) C116 0.051(6) 0.075(7) 0.066(6) 0.020(5) 0.024(5) 0.039(5) C121 0.078(9) 0.075(8) 0.048(7) 0.030(6) 0.019(6) 0.037(7) C122 0.073(7) 0.065(7) 0.046(5) -0.014(5) -0.002(5) 0.028(6) C123 0.048(5) 0.043(5) 0.077(7) 0.020(5) 0.019(5) 0.015(4) C124 0.056(6) 0.064(6) 0.056(6) 0.014(5) 0.020(5) 0.014(5) C125 0.060(6) 0.054(6) 0.064(6) 0.006(5) 0.021(5) 0.026(5) C126 0.068(7) 0.035(5) 0.054(6) 0.009(4) -0.001(5) 0.016(4) C131 0.068(8) 0.121(12) 0.050(7) -0.005(7) -0.001(6) 0.047(8) C132 0.131(12) 0.059(6) 0.038(5) 0.011(5) 0.012(6) 0.006(7) C133 0.161(16) 0.053(7) 0.041(6) 0.003(5) -0.013(8) 0.050(10) C134 0.078(9) 0.102(12) 0.080(10) -0.036(8) -0.011(7) 0.061(10) C135 0.077(10) 0.132(15) 0.080(10) -0.024(10) 0.043(8) -0.011(9) C136 0.084(8) 0.074(8) 0.036(5) 0.013(5) 0.006(5) 0.020(6) C141 0.26(3) 0.100(13) 0.095(13) 0.058(10) 0.106(17) 0.084(18) C142 0.22(2) 0.168(19) 0.039(7) 0.021(9) -0.006(10) 0.160(19) C143 0.041(6) 0.178(17) 0.095(11) -0.056(11) -0.016(6) 0.048(8) C144 0.103(10) 0.048(6) 0.071(8) -0.011(5) 0.020(7) 0.021(6) C145 0.075(8) 0.055(6) 0.063(6) -0.001(5) 0.015(6) 0.036(6) C146 0.127(12) 0.074(9) 0.109(12) 0.012(7) 0.084(10) 0.040(8) Au1 0.02326(18) 0.02851(18) 0.0275(2) 0.00356(15) 0.00668(15) 0.01231(14) Au52 0.01998(16) 0.03028(18) 0.0278(2) 0.00534(15) 0.00690(14) 0.01297(14) F1 0.055(4) 0.040(3) 0.135(6) 0.018(3) -0.026(4) 0.000(3) F2 0.120(5) 0.114(5) 0.102(5) 0.071(4) 0.079(4) 0.101(5) F3 0.094(4) 0.073(4) 0.041(3) 0.018(3) 0.006(3) 0.046(4) F4 0.100(5) 0.065(4) 0.038(3) 0.019(2) 0.014(3) 0.041(3) F5 0.077(5) 0.054(4) 0.140(7) 0.026(4) -0.015(4) 0.005(3) F6 0.209(10) 0.099(5) 0.067(4) 0.033(4) 0.059(5) 0.120(6) N1 0.027(4) 0.039(4) 0.019(4) -0.002(3) 0.000(3) 0.012(3) N2 0.029(2) 0.025(2) 0.028(2) 0.0030(18) 0.0062(19) 0.0089(19) N3 0.021(3) 0.042(4) 0.029(4) 0.005(3) 0.008(3) 0.023(3) N4 0.027(2) 0.027(3) 0.027(3) 0.001(2) 0.009(2) 0.015(2) O1 0.033(3) 0.060(4) 0.046(3) 0.003(3) -0.004(3) 0.014(3) O2 0.041(3) 0.068(4) 0.030(3) -0.002(3) 0.009(3) 0.030(3) O3 0.030(3) 0.055(4) 0.033(3) 0.001(3) 0.008(3) 0.020(3) O4 0.055(4) 0.069(5) 0.027(3) -0.007(3) 0.000(3) 0.040(4) O5 0.031(3) 0.046(3) 0.053(4) 0.003(3) -0.004(3) 0.005(2) O6 0.027(3) 0.081(5) 0.044(4) 0.015(4) 0.012(3) 0.036(3) P1 0.0259(11) 0.0223(10) 0.0271(11) 0.0036(8) 0.0087(8) 0.0115(8) P52 0.0176(9) 0.0260(10) 0.0221(10) 0.0048(8) 0.0053(8) 0.0105(8) S1 0.0287(11) 0.0394(12) 0.0273(11) -0.0019(9) -0.0013(8) 0.0154(9) S51 0.0282(11) 0.0388(11) 0.0297(11) 0.0007(9) 0.0014(8) 0.0179(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.394(11) . ? C1 C6 1.399(11) . ? C1 P1 1.809(9) . ? C2 C3 1.368(12) . ? C2 H2 0.95 . ? C3 C4 1.384(12) . ? C3 H3 0.95 . ? C4 C5 1.368(12) . ? C4 H4 0.95 . ? C5 C6 1.376(12) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.363(13) . ? C7 C12 1.395(13) . ? C7 P1 1.833(9) . ? C8 C9 1.401(14) . ? C8 H8 0.95 . ? C9 C10 1.363(13) . ? C9 H9 0.95 . ? C10 C11 1.362(13) . ? C10 H10 0.95 . ? C11 C12 1.385(13) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.562(8) . ? C13 P1 1.827(7) . ? C14 N2 1.458(7) . ? C14 C15 1.554(9) . ? C14 H14 1 . ? C15 C16 1.515(10) . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.510(10) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 N2 1.466(7) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 N2 1.457(7) . ? C18 C19 1.539(10) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.508(13) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 O6 1.225(11) . ? C20 N3 1.400(11) . ? C21 C26 1.360(11) . ? C21 C22 1.404(11) . ? C21 P52 1.825(8) . ? C22 C23 1.392(12) . ? C22 H22 0.95 . ? C23 C24 1.382(12) . ? C23 H23 0.95 . ? C24 C25 1.362(13) . ? C24 H24 0.95 . ? C25 C26 1.410(12) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C27 C28 1.380(12) . ? C27 C32 1.417(11) . ? C27 P52 1.811(9) . ? C28 C29 1.387(12) . ? C28 H28 0.95 . ? C29 C30 1.380(12) . ? C29 H29 0.95 . ? C30 C31 1.389(13) . ? C30 H30 0.95 . ? C31 C32 1.376(13) . ? C31 H31 0.95 . ? C32 H32 0.95 . ? C33 C34 1.536(8) . ? C33 P52 1.850(7) . ? C34 N4 1.489(6) . ? C34 C35 1.536(9) . ? C34 H34 1 . ? C35 C36 1.532(9) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.475(10) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 N4 1.460(7) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 N4 1.457(7) . ? C38 C39 1.521(9) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 C40 1.514(12) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 O3 1.187(11) . ? C40 N1 1.394(12) . ? C41 F2 1.287(11) . ? C41 F1 1.309(11) . ? C41 F3 1.317(11) . ? C41 S51 1.838(10) . ? C42 F6 1.290(12) . ? C42 F4 1.316(11) . ? C42 F5 1.333(12) . ? C42 S1 1.842(10) . ? C101 C106 1.392(15) . ? C101 C102 1.395(16) . ? C101 H101 0.95 . ? C102 C103 1.401(16) . ? C102 H102 0.95 . ? C103 C104 1.340(15) . ? C103 H103 0.95 . ? C104 C105 1.355(15) . ? C104 H104 0.95 . ? C105 C106 1.368(15) . ? C105 H105 0.95 . ? C106 H106 0.95 . ? C111 C116 1.345(16) . ? C111 C112 1.353(17) . ? C111 H111 0.95 . ? C112 C113 1.41(2) . ? C112 H112 0.95 . ? C113 C114 1.37(2) . ? C113 H113 0.95 . ? C114 C115 1.34(2) . ? C114 H114 0.95 . ? C115 C116 1.346(18) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C122 1.382(19) . ? C121 C126 1.399(18) . ? C121 H121 0.95 . ? C122 C123 1.370(17) . ? C122 H122 0.95 . ? C123 C124 1.389(16) . ? C123 H123 0.95 . ? C124 C125 1.381(15) . ? C124 H124 0.95 . ? C125 C126 1.368(16) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C131 C136 1.30(2) . ? C131 C132 1.34(2) . ? C131 H131 0.95 . ? C132 C133 1.31(2) . ? C132 H132 0.95 . ? C133 C134 1.38(2) . ? C133 H133 0.95 . ? C134 C135 1.35(2) . ? C134 H134 0.95 . ? C135 C136 1.39(2) . ? C135 H135 0.95 . ? C136 H136 0.95 . ? C141 C146 1.36(3) . ? C141 C142 1.39(3) . ? C141 H141 0.95 . ? C142 C143 1.32(3) . ? C142 H142 0.95 . ? C143 C144 1.35(2) . ? C143 H143 0.95 . ? C144 C145 1.324(19) . ? C144 H144 0.95 . ? C145 C146 1.360(18) . ? C145 H145 0.95 . ? C146 H146 0.95 . ? Au1 N1 2.094(8) . ? Au1 P1 2.236(3) . ? Au52 N3 2.091(7) . ? Au52 P52 2.242(2) . ? N1 S1 1.601(8) . ? N3 S51 1.627(8) . ? O1 S1 1.418(8) . ? O2 S1 1.436(7) . ? O4 S51 1.405(8) . ? O5 S51 1.419(7) . ? 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 C6 119.9(8) . . ? C2 C1 P1 119.0(6) . . ? C6 C1 P1 121.0(6) . . ? C3 C2 C1 119.4(8) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 121.0(7) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.3(8) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.5(8) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.8(7) . . ? C5 C6 H6 120.6 . . ? C1 C6 H6 120.6 . . ? C8 C7 C12 119.2(9) . . ? C8 C7 P1 119.0(8) . . ? C12 C7 P1 121.8(7) . . ? C7 C8 C9 121.2(9) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 118.7(9) . . ? C10 C9 H9 120.6 . . ? C8 C9 H9 120.6 . . ? C11 C10 C9 120.7(9) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.9(9) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 119.1(9) . . ? C11 C12 H12 120.4 . . ? C7 C12 H12 120.4 . . ? C14 C13 P1 109.4(4) . . ? N2 C14 C15 102.1(5) . . ? N2 C14 C13 116.2(5) . . ? C15 C14 C13 111.7(6) . . ? N2 C14 H14 108.8 . . ? C15 C14 H14 108.8 . . ? C13 C14 H14 108.8 . . ? C16 C15 C14 104.5(6) . . ? C16 C15 H15A 110.8 . . ? C14 C15 H15A 110.8 . . ? C16 C15 H15B 110.8 . . ? C14 C15 H15B 110.8 . . ? H15A C15 H15B 108.9 . . ? C17 C16 C15 105.3(5) . . ? C17 C16 H16A 110.7 . . ? C15 C16 H16A 110.7 . . ? C17 C16 H16B 110.7 . . ? C15 C16 H16B 110.7 . . ? H16A C16 H16B 108.8 . . ? N2 C17 C16 104.7(5) . . ? N2 C17 H17A 110.8 . . ? C16 C17 H17A 110.8 . . ? N2 C17 H17B 110.8 . . ? C16 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? N2 C18 C19 117.0(5) . . ? N2 C18 H18A 108 . . ? C19 C18 H18A 108 . . ? N2 C18 H18B 108 . . ? C19 C18 H18B 108 . . ? H18A C18 H18B 107.3 . . ? C20 C19 C18 109.5(6) . . ? C20 C19 H19A 109.8 . . ? C18 C19 H19A 109.8 . . ? C20 C19 H19B 109.8 . . ? C18 C19 H19B 109.8 . . ? H19A C19 H19B 108.2 . . ? O6 C20 N3 122.6(9) . . ? O6 C20 C19 122.9(8) . . ? N3 C20 C19 114.4(8) . . ? C26 C21 C22 120.2(8) . . ? C26 C21 P52 121.0(7) . . ? C22 C21 P52 118.7(6) . . ? C23 C22 C21 119.5(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 119.2(8) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 121.8(8) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 119.0(8) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 120.4(8) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C32 118.0(8) . . ? C28 C27 P52 125.2(7) . . ? C32 C27 P52 116.7(6) . . ? C27 C28 C29 121.2(8) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.9(9) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.4(9) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 119.5(8) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C27 121.0(8) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C34 C33 P52 114.5(4) . . ? N4 C34 C33 113.5(5) . . ? N4 C34 C35 103.3(5) . . ? C33 C34 C35 114.4(5) . . ? N4 C34 H34 108.4 . . ? C33 C34 H34 108.4 . . ? C35 C34 H34 108.4 . . ? C36 C35 C34 103.8(5) . . ? C36 C35 H35A 111 . . ? C34 C35 H35A 111 . . ? C36 C35 H35B 111 . . ? C34 C35 H35B 111 . . ? H35A C35 H35B 109 . . ? C37 C36 C35 106.5(6) . . ? C37 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? C37 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? N4 C37 C36 108.4(5) . . ? N4 C37 H37A 110 . . ? C36 C37 H37A 110 . . ? N4 C37 H37B 110 . . ? C36 C37 H37B 110 . . ? H37A C37 H37B 108.4 . . ? N4 C38 C39 109.7(5) . . ? N4 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? N4 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C40 C39 C38 114.8(7) . . ? C40 C39 H39A 108.6 . . ? C38 C39 H39A 108.6 . . ? C40 C39 H39B 108.6 . . ? C38 C39 H39B 108.6 . . ? H39A C39 H39B 107.5 . . ? O3 C40 N1 125.4(9) . . ? O3 C40 C39 122.7(8) . . ? N1 C40 C39 111.9(7) . . ? F2 C41 F1 106.7(10) . . ? F2 C41 F3 108.0(9) . . ? F1 C41 F3 107.9(9) . . ? F2 C41 S51 114.8(7) . . ? F1 C41 S51 110.9(7) . . ? F3 C41 S51 108.4(7) . . ? F6 C42 F4 107.8(9) . . ? F6 C42 F5 108.1(10) . . ? F4 C42 F5 106.6(9) . . ? F6 C42 S1 112.6(8) . . ? F4 C42 S1 110.2(7) . . ? F5 C42 S1 111.2(7) . . ? C106 C101 C102 119.3(11) . . ? C106 C101 H101 120.4 . . ? C102 C101 H101 120.4 . . ? C101 C102 C103 118.9(10) . . ? C101 C102 H102 120.6 . . ? C103 C102 H102 120.6 . . ? C104 C103 C102 119.4(10) . . ? C104 C103 H103 120.3 . . ? C102 C103 H103 120.3 . . ? C103 C104 C105 123.0(10) . . ? C103 C104 H104 118.5 . . ? C105 C104 H104 118.5 . . ? C104 C105 C106 119.2(10) . . ? C104 C105 H105 120.4 . . ? C106 C105 H105 120.4 . . ? C105 C106 C101 120.3(10) . . ? C105 C106 H106 119.9 . . ? C101 C106 H106 119.9 . . ? C116 C111 C112 122.6(13) . . ? C116 C111 H111 118.7 . . ? C112 C111 H111 118.7 . . ? C111 C112 C113 116.5(13) . . ? C111 C112 H112 121.8 . . ? C113 C112 H112 121.8 . . ? C114 C113 C112 120.3(13) . . ? C114 C113 H113 119.8 . . ? C112 C113 H113 119.8 . . ? C115 C114 C113 119.3(13) . . ? C115 C114 H114 120.4 . . ? C113 C114 H114 120.4 . . ? C114 C115 C116 121.2(12) . . ? C114 C115 H115 119.4 . . ? C116 C115 H115 119.4 . . ? C111 C116 C115 119.6(12) . . ? C111 C116 H116 120.2 . . ? C115 C116 H116 120.2 . . ? C122 C121 C126 116.2(12) . . ? C122 C121 H121 121.9 . . ? C126 C121 H121 121.9 . . ? C123 C122 C121 122.6(12) . . ? C123 C122 H122 118.7 . . ? C121 C122 H122 118.7 . . ? C122 C123 C124 119.0(11) . . ? C122 C123 H123 120.5 . . ? C124 C123 H123 120.5 . . ? C125 C124 C123 120.1(11) . . ? C125 C124 H124 119.9 . . ? C123 C124 H124 119.9 . . ? C126 C125 C124 119.1(11) . . ? C126 C125 H125 120.4 . . ? C124 C125 H125 120.4 . . ? C125 C126 C121 122.4(11) . . ? C125 C126 H126 118.8 . . ? C121 C126 H126 118.8 . . ? C136 C131 C132 120.5(14) . . ? C136 C131 H131 119.8 . . ? C132 C131 H131 119.8 . . ? C133 C132 C131 120.5(14) . . ? C133 C132 H132 119.8 . . ? C131 C132 H132 119.8 . . ? C132 C133 C134 120.7(12) . . ? C132 C133 H133 119.7 . . ? C134 C133 H133 119.7 . . ? C135 C134 C133 119.1(14) . . ? C135 C134 H134 120.4 . . ? C133 C134 H134 120.4 . . ? C134 C135 C136 117.8(14) . . ? C134 C135 H135 121.1 . . ? C136 C135 H135 121.1 . . ? C131 C136 C135 121.4(14) . . ? C131 C136 H136 119.3 . . ? C135 C136 H136 119.3 . . ? C146 C141 C142 117.9(16) . . ? C146 C141 H141 121 . . ? C142 C141 H141 121 . . ? C143 C142 C141 119.0(15) . . ? C143 C142 H142 120.5 . . ? C141 C142 H142 120.5 . . ? C142 C143 C144 123.7(15) . . ? C142 C143 H143 118.1 . . ? C144 C143 H143 118.1 . . ? C145 C144 C143 117.1(15) . . ? C145 C144 H144 121.4 . . ? C143 C144 H144 121.4 . . ? C144 C145 C146 122.2(15) . . ? C144 C145 H145 118.9 . . ? C146 C145 H145 118.9 . . ? C145 C146 C141 120.0(17) . . ? C145 C146 H146 120 . . ? C141 C146 H146 120 . . ? N1 Au1 P1 173.9(2) . . ? N3 Au52 P52 177.4(2) . . ? C40 N1 S1 120.8(7) . . ? C40 N1 Au1 122.8(6) . . ? S1 N1 Au1 116.4(4) . . ? C18 N2 C14 116.0(5) . . ? C18 N2 C17 114.4(5) . . ? C14 N2 C17 104.3(5) . . ? C20 N3 S51 119.3(6) . . ? C20 N3 Au52 125.5(6) . . ? S51 N3 Au52 114.5(4) . . ? C38 N4 C37 114.1(5) . . ? C38 N4 C34 112.9(4) . . ? C37 N4 C34 106.6(5) . . ? C1 P1 C13 107.7(3) . . ? C1 P1 C7 105.4(4) . . ? C13 P1 C7 108.1(4) . . ? C1 P1 Au1 114.3(3) . . ? C13 P1 Au1 109.5(2) . . ? C7 P1 Au1 111.7(3) . . ? C27 P52 C21 104.1(4) . . ? C27 P52 C33 109.9(4) . . ? C21 P52 C33 102.5(3) . . ? C27 P52 Au52 110.2(3) . . ? C21 P52 Au52 112.8(3) . . ? C33 P52 Au52 116.6(2) . . ? O1 S1 O2 120.5(5) . . ? O1 S1 N1 114.7(4) . . ? O2 S1 N1 106.8(4) . . ? O1 S1 C42 105.2(5) . . ? O2 S1 C42 103.3(5) . . ? N1 S1 C42 104.7(5) . . ? O4 S51 O5 118.8(5) . . ? O4 S51 N3 107.5(4) . . ? O5 S51 N3 114.0(4) . . ? O4 S51 C41 104.4(5) . . ? O5 S51 C41 104.8(4) . . ? N3 S51 C41 106.2(5) . . ? # END of CIF