# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Tzi Sum Andy Hor' _publ_contact_author_email ANDYHOR@NUS.EDU.SG _publ_section_title ; Isolation of Cationic Digold-Frame with Free Carboxylic Acid Pendants ; loop_ _publ_author_name 'Andy Hor' 'L. L. Koh' 'Peili Teo.' 'Jing Wang.' # Attachment 'complex_1.cif' data_6344a _database_code_depnum_ccdc_archive 'CCDC 715600' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H35 Au2 Cl3 F6 N2 O11 P2 S2' _chemical_formula_weight 1460.04 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.6477(17) _cell_length_b 13.0358(10) _cell_length_c 18.1681(15) _cell_angle_alpha 90.00 _cell_angle_beta 101.712(2) _cell_angle_gamma 90.00 _cell_volume 5020.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5052 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.95 _exptl_crystal_description 'Thin Plate' _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2808 _exptl_absorpt_coefficient_mu 6.223 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1541 _exptl_absorpt_correction_T_max 0.7889 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33235 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11502 _reflns_number_gt 7541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atoms of the two waters were located from different map and refined with restraints in bond length and thermal parameters. The three Cl of the ; _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^)+(0.0703P)^2^+6.0017P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11502 _refine_ls_number_parameters 621 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1619 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.185476(18) 0.81577(3) 0.68176(2) 0.05039(13) Uani 1 1 d . . . Au2 Au 0.25138(2) 1.00124(3) 0.61831(2) 0.05126(13) Uani 1 1 d . . . P1 P 0.29292(12) 0.89379(18) 0.54562(14) 0.0463(6) Uani 1 1 d . . . P2 P 0.24398(11) 0.71161(17) 0.62546(13) 0.0423(5) Uani 1 1 d . . . O1 O -0.0430(4) 1.1321(7) 0.7893(5) 0.078(2) Uani 1 1 d . . . O2 O 0.0327(4) 1.1407(7) 0.8914(5) 0.080(2) Uani 1 1 d . . . H2 H 0.0073 1.1784 0.9070 0.120 Uiso 1 1 calc R . . O3 O 0.0887(4) 1.3514(7) 0.8014(5) 0.099(3) Uani 1 1 d . . . O4 O 0.1678(4) 1.3099(6) 0.8941(4) 0.066(2) Uani 1 1 d . . . H4A H 0.1494 1.3481 0.9192 0.099 Uiso 1 1 calc R . . N1 N 0.1265(4) 0.9083(6) 0.7322(4) 0.0496(19) Uani 1 1 d . . . N2 N 0.2168(4) 1.1091(5) 0.6838(4) 0.052(2) Uani 1 1 d . . . C1 C 0.1482(5) 0.9527(7) 0.7975(6) 0.050(2) Uani 1 1 d . . . H1 H 0.1898 0.9393 0.8226 0.061 Uiso 1 1 calc R . . C2 C 0.1115(5) 1.0183(7) 0.8299(6) 0.053(2) Uani 1 1 d . . . H2A H 0.1278 1.0490 0.8766 0.063 Uiso 1 1 calc R . . C3 C 0.0505(4) 1.0382(7) 0.7932(5) 0.047(2) Uani 1 1 d . . . C4 C 0.0282(5) 0.9896(8) 0.7253(6) 0.060(3) Uani 1 1 d . . . H4 H -0.0135 0.9999 0.6990 0.072 Uiso 1 1 calc R . . C5 C 0.0684(5) 0.9261(8) 0.6974(6) 0.064(3) Uani 1 1 d . . . H5 H 0.0535 0.8937 0.6510 0.077 Uiso 1 1 calc R . . C6 C 0.0075(5) 1.1086(8) 0.8234(6) 0.055(3) Uani 1 1 d . . . C7 C 0.2506(5) 1.1390(7) 0.7504(5) 0.050(2) Uani 1 1 d . . . H7 H 0.2919 1.1138 0.7658 0.060 Uiso 1 1 calc R . . C8 C 0.2275(5) 1.2048(7) 0.7968(6) 0.054(2) Uani 1 1 d . . . H8 H 0.2524 1.2246 0.8432 0.065 Uiso 1 1 calc R . . C9 C 0.1671(5) 1.2415(6) 0.7742(6) 0.048(2) Uani 1 1 d . . . C10 C 0.1327(5) 1.2135(7) 0.7060(6) 0.060(3) Uani 1 1 d . . . H10 H 0.0920 1.2403 0.6887 0.072 Uiso 1 1 calc R . . C11 C 0.1581(6) 1.1454(8) 0.6629(6) 0.067(3) Uani 1 1 d . . . H11 H 0.1334 1.1234 0.6170 0.080 Uiso 1 1 calc R . . C12 C 0.1372(5) 1.3077(7) 0.8258(6) 0.055(2) Uani 1 1 d . . . C13 C 0.2569(4) 0.7664(6) 0.5381(5) 0.041(2) Uani 1 1 d . . . H13A H 0.2163 0.7702 0.5028 0.050 Uiso 1 1 calc R . . H13B H 0.2840 0.7196 0.5166 0.050 Uiso 1 1 calc R . . C1A C 0.2058(4) 0.5905(7) 0.5973(5) 0.045(2) Uani 1 1 d . . . C2A C 0.1539(5) 0.5642(7) 0.6269(5) 0.052(2) Uani 1 1 d . . . H2A1 H 0.1387 0.6093 0.6594 0.062 Uiso 1 1 calc R . . C3A C 0.1241(6) 0.4684(10) 0.6078(7) 0.075(3) Uani 1 1 d . . . H3A H 0.0901 0.4480 0.6294 0.090 Uiso 1 1 calc R . . C4A C 0.1447(6) 0.4068(9) 0.5582(7) 0.071(3) Uani 1 1 d . . . H4A H 0.1239 0.3443 0.5445 0.085 Uiso 1 1 calc R . . C5A C 0.1954(6) 0.4331(7) 0.5274(6) 0.065(3) Uani 1 1 d . . . H5A H 0.2095 0.3887 0.4935 0.078 Uiso 1 1 calc R . . C6A C 0.2252(5) 0.5255(7) 0.5468(6) 0.055(2) Uani 1 1 d . . . H6A H 0.2594 0.5444 0.5252 0.066 Uiso 1 1 calc R . . C1B C 0.3214(5) 0.6827(7) 0.6819(6) 0.053(2) Uani 1 1 d . . . C2B C 0.3640(5) 0.6252(9) 0.6531(6) 0.069(3) Uani 1 1 d . . . H2B H 0.3534 0.6002 0.6036 0.083 Uiso 1 1 calc R . . C3B C 0.4218(6) 0.6044(10) 0.6967(8) 0.085(4) Uani 1 1 d . . . H3B H 0.4517 0.5664 0.6773 0.102 Uiso 1 1 calc R . . C4B C 0.4360(7) 0.6409(10) 0.7717(8) 0.088(4) Uani 1 1 d . . . H4B H 0.4753 0.6251 0.8022 0.106 Uiso 1 1 calc R . . C5B C 0.3953(6) 0.6965(10) 0.7997(7) 0.080(4) Uani 1 1 d . . . H5B H 0.4058 0.7213 0.8493 0.096 Uiso 1 1 calc R . . C6B C 0.3368(5) 0.7179(8) 0.7551(6) 0.062(3) Uani 1 1 d . . . H6B H 0.3073 0.7566 0.7748 0.074 Uiso 1 1 calc R . . C1C C 0.3754(5) 0.8744(7) 0.5776(6) 0.052(2) Uani 1 1 d . . . C2C C 0.4092(5) 0.8172(9) 0.5349(7) 0.069(3) Uani 1 1 d . . . H2C H 0.3893 0.7912 0.4877 0.083 Uiso 1 1 calc R . . C3C C 0.4728(6) 0.7988(11) 0.5626(10) 0.095(4) Uani 1 1 d . . . H3C H 0.4959 0.7619 0.5329 0.114 Uiso 1 1 calc R . . C4C C 0.5033(7) 0.8330(13) 0.6326(12) 0.110(5) Uani 1 1 d . . . H4C H 0.5461 0.8183 0.6518 0.132 Uiso 1 1 calc R . . C5C C 0.4675(8) 0.8902(12) 0.6732(9) 0.108(5) Uani 1 1 d . . . H5C H 0.4871 0.9161 0.7204 0.130 Uiso 1 1 calc R . . C6C C 0.4059(6) 0.9100(9) 0.6476(7) 0.076(3) Uani 1 1 d . . . H6C H 0.3834 0.9481 0.6774 0.091 Uiso 1 1 calc R . . C1D C 0.2803(5) 0.9367(7) 0.4482(5) 0.051(2) Uani 1 1 d . . . C2D C 0.3284(6) 0.9914(8) 0.4249(7) 0.073(3) Uani 1 1 d . . . H2D H 0.3674 1.0025 0.4577 0.087 Uiso 1 1 calc R . . C3D C 0.3168(7) 1.0298(9) 0.3500(8) 0.085(4) Uani 1 1 d . . . H3D H 0.3481 1.0678 0.3331 0.101 Uiso 1 1 calc R . . C4D C 0.2602(7) 1.0118(8) 0.3023(7) 0.073(3) Uani 1 1 d . . . H4D H 0.2533 1.0356 0.2524 0.087 Uiso 1 1 calc R . . C5D C 0.2136(6) 0.9588(9) 0.3273(6) 0.070(3) Uani 1 1 d . . . H5D H 0.1744 0.9477 0.2951 0.084 Uiso 1 1 calc R . . C6D C 0.2248(5) 0.9220(8) 0.4003(6) 0.060(3) Uani 1 1 d . . . H6D H 0.1927 0.8857 0.4169 0.072 Uiso 1 1 calc R . . S1 S 0.33848(16) 0.9682(3) 0.9012(2) 0.0800(10) Uani 1 1 d . . . C14 C 0.4207(14) 1.014(2) 0.8971(15) 0.173(13) Uani 1 1 d . . . F1 F 0.4106(7) 1.0750(14) 0.8450(13) 0.262(10) Uani 1 1 d . . . F2 F 0.4467(9) 1.0346(19) 0.9571(15) 0.346(17) Uani 1 1 d . . . F3 F 0.4490(5) 0.9287(12) 0.8820(10) 0.214(7) Uani 1 1 d . . . S2 S 0.04706(13) 0.8157(2) 0.48197(15) 0.0583(6) Uani 1 1 d . . . O5 O 0.3446(8) 0.8844(10) 0.9455(9) 0.205(8) Uani 1 1 d . . . O6 O 0.3132(6) 0.9421(9) 0.8233(7) 0.149(5) Uani 1 1 d . . . O7 O 0.3110(5) 1.0576(8) 0.9234(6) 0.111(3) Uani 1 1 d . . . O8 O -0.0071(6) 0.8651(11) 0.4467(7) 0.176(7) Uani 1 1 d . . . O9 O 0.0443(6) 0.7671(8) 0.5503(5) 0.123(4) Uani 1 1 d . . . O10 O 0.1033(4) 0.8721(7) 0.4915(6) 0.105(3) Uani 1 1 d . . . C15 C 0.0577(6) 0.7105(10) 0.4220(7) 0.072(3) Uani 1 1 d . . . F4 F 0.1084(5) 0.6630(7) 0.4432(6) 0.141(4) Uani 1 1 d . . . F5 F 0.0590(8) 0.7399(10) 0.3561(5) 0.198(7) Uani 1 1 d . . . F6 F 0.0119(5) 0.6499(10) 0.4110(8) 0.194(7) Uani 1 1 d . . . C1S C 0.6418(8) 0.8022(13) 0.9197(10) 0.116(5) Uani 1 1 d . . . H1S H 0.6484 0.8670 0.9487 0.139 Uiso 1 1 calc R A 1 Cl1A Cl 0.6891(4) 0.7126(4) 0.9705(4) 0.198(3) Uani 1 1 d U B . Cl1B Cl 0.6659(4) 0.8237(5) 0.8363(4) 0.181(3) Uani 1 1 d U B . Cl1C Cl 0.5659(4) 0.7764(12) 0.9049(6) 0.362(8) Uani 1 1 d U B 1 O1W O 0.1114(4) 1.4150(6) 0.9829(5) 0.066(2) Uani 1 1 d D C 2 H1W H 0.109(4) 1.4801(10) 0.983(7) 0.080 Uiso 1 1 d D . . H2W H 0.0718(10) 1.412(7) 0.980(7) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0566(2) 0.0485(2) 0.0528(2) -0.00546(17) 0.02685(18) 0.00292(18) Au2 0.0719(3) 0.0396(2) 0.0471(2) -0.00614(15) 0.02340(19) 0.00205(18) P1 0.0582(15) 0.0408(12) 0.0451(14) -0.0072(10) 0.0224(11) -0.0036(11) P2 0.0456(13) 0.0401(12) 0.0441(13) -0.0035(10) 0.0159(10) -0.0010(10) O1 0.064(5) 0.099(6) 0.078(6) -0.012(5) 0.031(4) 0.014(5) O2 0.091(6) 0.084(6) 0.067(5) -0.022(4) 0.021(4) 0.033(5) O3 0.088(6) 0.114(7) 0.091(7) -0.026(5) 0.009(5) 0.058(6) O4 0.081(5) 0.066(5) 0.054(5) -0.012(3) 0.022(4) 0.014(4) N1 0.055(5) 0.047(4) 0.051(5) 0.001(4) 0.020(4) 0.003(4) N2 0.081(6) 0.035(4) 0.044(5) -0.005(3) 0.017(4) 0.006(4) C1 0.050(6) 0.050(5) 0.055(6) -0.009(5) 0.019(5) -0.004(5) C2 0.066(7) 0.045(5) 0.050(6) -0.005(4) 0.019(5) 0.002(5) C3 0.049(6) 0.052(5) 0.044(5) -0.001(4) 0.022(4) -0.002(4) C4 0.044(6) 0.070(7) 0.069(7) -0.001(5) 0.019(5) 0.000(5) C5 0.051(6) 0.080(8) 0.065(7) -0.028(6) 0.018(5) -0.007(6) C6 0.051(6) 0.059(6) 0.065(7) -0.003(5) 0.032(5) 0.003(5) C7 0.050(5) 0.050(5) 0.050(6) 0.003(4) 0.008(4) 0.011(5) C8 0.071(7) 0.048(5) 0.046(6) -0.006(4) 0.020(5) 0.003(5) C9 0.058(6) 0.028(4) 0.061(6) -0.006(4) 0.015(5) 0.006(4) C10 0.077(7) 0.054(6) 0.046(6) -0.004(5) 0.007(5) 0.019(5) C11 0.101(9) 0.051(6) 0.051(6) -0.006(5) 0.018(6) 0.003(6) C12 0.062(6) 0.046(6) 0.060(7) 0.001(5) 0.017(5) 0.013(5) C13 0.044(5) 0.038(4) 0.044(5) 0.001(4) 0.013(4) 0.004(4) C1A 0.044(5) 0.042(5) 0.052(6) 0.009(4) 0.014(4) 0.001(4) C2A 0.059(6) 0.047(5) 0.052(6) 0.001(4) 0.014(5) -0.006(5) C3A 0.064(7) 0.084(8) 0.080(9) 0.002(7) 0.021(6) -0.028(7) C4A 0.073(8) 0.062(7) 0.072(8) -0.006(6) -0.002(6) -0.020(6) C5A 0.090(8) 0.043(6) 0.065(7) -0.011(5) 0.020(6) -0.004(6) C6A 0.059(6) 0.048(5) 0.061(7) -0.005(5) 0.022(5) -0.005(5) C1B 0.063(6) 0.040(5) 0.053(6) -0.003(4) 0.008(5) -0.007(5) C2B 0.063(7) 0.080(8) 0.063(7) -0.017(6) 0.012(6) 0.016(6) C3B 0.074(8) 0.090(9) 0.086(10) -0.006(7) 0.007(7) 0.026(7) C4B 0.077(9) 0.075(8) 0.097(11) 0.009(8) -0.017(8) 0.011(7) C5B 0.082(9) 0.091(9) 0.057(7) -0.003(6) -0.008(7) -0.015(8) C6B 0.071(7) 0.057(6) 0.058(7) -0.006(5) 0.015(6) -0.010(5) C1C 0.055(6) 0.048(5) 0.055(6) -0.002(5) 0.016(5) -0.013(5) C2C 0.067(7) 0.076(8) 0.070(8) -0.008(6) 0.025(6) -0.013(6) C3C 0.056(8) 0.095(10) 0.139(14) -0.006(9) 0.033(8) 0.006(7) C4C 0.062(9) 0.114(13) 0.153(17) 0.007(11) 0.016(10) -0.016(9) C5C 0.106(12) 0.101(11) 0.101(12) -0.029(9) -0.016(10) -0.034(10) C6C 0.068(8) 0.068(7) 0.087(9) -0.013(6) 0.003(7) -0.017(6) C1D 0.074(7) 0.043(5) 0.043(5) -0.008(4) 0.031(5) 0.004(5) C2D 0.091(9) 0.070(7) 0.057(7) 0.006(5) 0.017(6) -0.015(6) C3D 0.115(11) 0.071(8) 0.077(9) 0.012(7) 0.042(8) -0.030(8) C4D 0.109(10) 0.055(7) 0.062(8) 0.012(5) 0.036(7) 0.004(7) C5D 0.081(8) 0.071(7) 0.059(7) 0.016(6) 0.015(6) 0.013(6) C6D 0.071(7) 0.059(6) 0.054(6) -0.001(5) 0.023(5) -0.002(6) S1 0.076(2) 0.0687(19) 0.105(3) 0.0266(18) 0.0388(19) 0.0106(17) C14 0.22(3) 0.20(2) 0.14(2) 0.079(18) 0.11(2) 0.12(2) F1 0.123(10) 0.27(2) 0.42(3) 0.10(2) 0.110(15) -0.036(12) F2 0.204(16) 0.39(3) 0.36(3) -0.20(2) -0.151(19) 0.062(17) F3 0.094(7) 0.233(15) 0.33(2) -0.083(14) 0.087(10) 0.016(9) S2 0.0568(15) 0.0698(16) 0.0527(15) -0.0023(13) 0.0211(12) -0.0081(14) O5 0.261(17) 0.155(11) 0.258(18) 0.145(12) 0.191(15) 0.098(12) O6 0.166(11) 0.100(8) 0.148(11) -0.033(7) -0.047(9) 0.018(8) O7 0.126(8) 0.115(8) 0.105(8) 0.017(6) 0.054(6) 0.045(7) O8 0.147(10) 0.223(14) 0.132(10) -0.083(10) -0.033(8) 0.122(10) O9 0.199(11) 0.113(7) 0.076(6) -0.025(5) 0.075(7) -0.076(8) O10 0.093(6) 0.070(5) 0.168(10) -0.024(6) 0.066(6) -0.037(5) C15 0.072(8) 0.083(9) 0.053(7) -0.012(6) -0.010(6) 0.004(7) F4 0.131(8) 0.113(7) 0.150(9) -0.061(6) -0.041(7) 0.055(6) F5 0.336(18) 0.206(12) 0.065(6) 0.007(7) 0.076(8) 0.126(13) F6 0.138(9) 0.197(11) 0.265(16) -0.166(11) 0.083(9) -0.090(9) C1S 0.110(12) 0.118(13) 0.123(14) -0.026(10) 0.034(10) 0.000(10) Cl1A 0.326(9) 0.092(3) 0.173(6) 0.012(3) 0.045(6) 0.052(5) Cl1B 0.250(7) 0.179(5) 0.126(5) -0.001(4) 0.071(5) -0.011(5) Cl1C 0.130(6) 0.68(2) 0.289(12) -0.166(13) 0.070(6) -0.127(9) O1W 0.080(5) 0.058(4) 0.071(5) -0.004(4) 0.040(4) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.097(7) . ? Au1 P2 2.241(2) . ? Au1 Au2 3.1429(5) . ? Au2 N2 2.077(7) . ? Au2 P1 2.235(2) . ? P1 C1C 1.780(10) . ? P1 C1D 1.822(10) . ? P1 C13 1.827(9) . ? P2 C1A 1.808(9) . ? P2 C13 1.813(8) . ? P2 C1B 1.817(10) . ? O1 C6 1.182(12) . ? O2 C6 1.313(13) . ? O3 C12 1.197(12) . ? O4 C12 1.284(12) . ? N1 C5 1.309(12) . ? N1 C1 1.318(12) . ? N2 C11 1.337(14) . ? N2 C7 1.338(12) . ? C1 C2 1.378(13) . ? C2 C3 1.377(14) . ? C3 C4 1.384(14) . ? C3 C6 1.489(13) . ? C4 C5 1.371(13) . ? C7 C8 1.367(12) . ? C8 C9 1.375(13) . ? C9 C10 1.359(13) . ? C9 C12 1.513(13) . ? C10 C11 1.371(14) . ? C1A C6A 1.377(13) . ? C1A C2A 1.382(12) . ? C2A C3A 1.416(14) . ? C3A C4A 1.350(16) . ? C4A C5A 1.372(15) . ? C5A C6A 1.378(13) . ? C1B C2B 1.371(14) . ? C1B C6B 1.382(14) . ? C2B C3B 1.366(15) . ? C3B C4B 1.416(18) . ? C4B C5B 1.321(18) . ? C5B C6B 1.386(16) . ? C1C C2C 1.387(14) . ? C1C C6C 1.390(15) . ? C2C C3C 1.388(17) . ? C3C C4C 1.38(2) . ? C4C C5C 1.39(2) . ? C5C C6C 1.344(19) . ? C1D C6D 1.346(14) . ? C1D C2D 1.398(14) . ? C2D C3D 1.424(16) . ? C3D C4D 1.369(18) . ? C4D C5D 1.374(16) . ? C5D C6D 1.384(14) . ? S1 O5 1.348(10) . ? S1 O7 1.405(10) . ? S1 O6 1.450(12) . ? S1 C14 1.89(3) . ? C14 F2 1.15(3) . ? C14 F1 1.22(2) . ? C14 F3 1.33(2) . ? S2 O8 1.376(10) . ? S2 O10 1.403(8) . ? S2 O9 1.406(9) . ? S2 C15 1.795(12) . ? C15 F6 1.252(14) . ? C15 F4 1.252(13) . ? C15 F5 1.263(15) . ? C1S Cl1C 1.645(17) . ? C1S Cl1A 1.697(18) . ? C1S Cl1B 1.722(18) . ? 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 N1 Au1 P2 176.9(2) . . ? N1 Au1 Au2 94.6(2) . . ? P2 Au1 Au2 87.59(6) . . ? N2 Au2 P1 176.0(2) . . ? N2 Au2 Au1 93.9(2) . . ? P1 Au2 Au1 90.10(6) . . ? C1C P1 C1D 107.7(5) . . ? C1C P1 C13 106.2(4) . . ? C1D P1 C13 103.2(4) . . ? C1C P1 Au2 113.2(3) . . ? C1D P1 Au2 112.5(3) . . ? C13 P1 Au2 113.4(3) . . ? C1A P2 C13 103.9(4) . . ? C1A P2 C1B 107.2(4) . . ? C13 P2 C1B 106.7(4) . . ? C1A P2 Au1 112.9(3) . . ? C13 P2 Au1 111.3(3) . . ? C1B P2 Au1 114.2(3) . . ? C5 N1 C1 119.2(8) . . ? C5 N1 Au1 120.1(7) . . ? C1 N1 Au1 120.5(7) . . ? C11 N2 C7 117.9(8) . . ? C11 N2 Au2 120.6(7) . . ? C7 N2 Au2 121.4(7) . . ? N1 C1 C2 121.7(9) . . ? C3 C2 C1 119.3(9) . . ? C2 C3 C4 118.2(9) . . ? C2 C3 C6 123.2(9) . . ? C4 C3 C6 118.6(9) . . ? C5 C4 C3 118.2(10) . . ? N1 C5 C4 123.3(10) . . ? O1 C6 O2 125.1(9) . . ? O1 C6 C3 123.2(10) . . ? O2 C6 C3 111.8(9) . . ? N2 C7 C8 122.7(9) . . ? C7 C8 C9 118.6(9) . . ? C10 C9 C8 119.4(9) . . ? C10 C9 C12 119.6(9) . . ? C8 C9 C12 120.9(9) . . ? C9 C10 C11 119.0(10) . . ? N2 C11 C10 122.4(11) . . ? O3 C12 O4 126.1(10) . . ? O3 C12 C9 119.7(10) . . ? O4 C12 C9 114.2(9) . . ? P2 C13 P1 115.6(5) . . ? C6A C1A C2A 119.3(9) . . ? C6A C1A P2 122.8(7) . . ? C2A C1A P2 117.9(7) . . ? C1A C2A C3A 119.3(10) . . ? C4A C3A C2A 119.5(10) . . ? C3A C4A C5A 121.6(11) . . ? C4A C5A C6A 119.0(10) . . ? C1A C6A C5A 121.2(9) . . ? C2B C1B C6B 119.9(10) . . ? C2B C1B P2 120.9(8) . . ? C6B C1B P2 119.3(8) . . ? C3B C2B C1B 119.8(11) . . ? C2B C3B C4B 119.0(12) . . ? C5B C4B C3B 121.6(12) . . ? C4B C5B C6B 119.1(12) . . ? C1B C6B C5B 120.7(11) . . ? C2C C1C C6C 119.0(10) . . ? C2C C1C P1 120.2(8) . . ? C6C C1C P1 120.7(8) . . ? C1C C2C C3C 119.1(12) . . ? C4C C3C C2C 122.2(14) . . ? C3C C4C C5C 116.5(14) . . ? C6C C5C C4C 122.8(14) . . ? C5C C6C C1C 120.4(13) . . ? C6D C1D C2D 119.9(10) . . ? C6D C1D P1 121.6(8) . . ? C2D C1D P1 118.5(9) . . ? C1D C2D C3D 118.1(12) . . ? C4D C3D C2D 120.5(11) . . ? C3D C4D C5D 119.9(11) . . ? C4D C5D C6D 119.6(12) . . ? C1D C6D C5D 122.0(10) . . ? O5 S1 O7 119.8(8) . . ? O5 S1 O6 111.4(10) . . ? O7 S1 O6 112.1(6) . . ? O5 S1 C14 107.5(10) . . ? O7 S1 C14 101.8(10) . . ? O6 S1 C14 102.0(10) . . ? F2 C14 F1 124(4) . . ? F2 C14 F3 103(2) . . ? F1 C14 F3 114(2) . . ? F2 C14 S1 109(2) . . ? F1 C14 S1 102(2) . . ? F3 C14 S1 103(2) . . ? O8 S2 O10 116.6(9) . . ? O8 S2 O9 115.9(9) . . ? O10 S2 O9 108.6(7) . . ? O8 S2 C15 106.0(6) . . ? O10 S2 C15 105.1(6) . . ? O9 S2 C15 103.0(6) . . ? F6 C15 F4 110.7(13) . . ? F6 C15 F5 102.1(13) . . ? F4 C15 F5 104.7(13) . . ? F6 C15 S2 112.6(10) . . ? F4 C15 S2 113.8(8) . . ? F5 C15 S2 112.0(10) . . ? Cl1C C1S Cl1A 114.8(12) . . ? Cl1C C1S Cl1B 111.0(11) . . ? Cl1A C1S Cl1B 109.5(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O9 0.83 1.88 2.708(11) 174.8 2_556 O4 H4A O1W 0.83 1.78 2.602(9) 171.6 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.001 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.167 # Attachment 'complex_2.cif' data_8487 _database_code_depnum_ccdc_archive 'CCDC 715601' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H34 Au2 Cl2 F6 N2 O10 P2 S2' _chemical_formula_weight 1407.59 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3909(10) _cell_length_b 10.8057(11) _cell_length_c 21.649(2) _cell_angle_alpha 79.284(2) _cell_angle_beta 84.081(2) _cell_angle_gamma 80.780(2) _cell_volume 2350.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5631 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 27.43 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.989 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 6.584 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1374 _exptl_absorpt_correction_T_max 0.7786 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16415 _diffrn_reflns_av_R_equivalents 0.0384 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10680 _reflns_number_gt 7932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. H atom of O1 and O3 were located from different map and refined with restraints in bond length and thermal parameters. One phenyl ring and one Cl of the solvent CH2Cl2 are disordered into two positions with occupancy ratios 56:44 and 60:40 respectively. Restraints in bond distances and thermal parameters were applied to these disordered parts. ; _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^)+(0.1024P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10680 _refine_ls_number_parameters 630 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.33862(3) 0.51408(3) 0.784229(15) 0.03817(12) Uani 1 1 d . A . Au2 Au 0.33567(3) 0.41909(3) 0.654551(15) 0.03732(12) Uani 1 1 d . A . P1 P 0.1633(2) 0.4195(2) 0.82216(10) 0.0350(5) Uani 1 1 d . . . P2 P 0.1705(2) 0.3139(2) 0.69785(10) 0.0334(4) Uani 1 1 d . . . N1 N 0.4889(7) 0.6227(7) 0.7537(3) 0.0379(16) Uani 1 1 d . . . N2 N 0.4926(7) 0.5119(7) 0.6134(4) 0.0406(17) Uani 1 1 d . . . O1 O 0.4271(8) 0.9317(8) 0.6131(4) 0.068(2) Uani 1 1 d D . . H1 H 0.409(11) 0.996(6) 0.581(2) 0.080 Uiso 1 1 d D . . O2 O 0.6105(8) 1.0015(8) 0.6292(4) 0.072(2) Uani 1 1 d D . . O3 O 0.4415(8) 0.8004(8) 0.4597(4) 0.076(3) Uani 1 1 d D . . H3 H 0.405(10) 0.853(8) 0.427(2) 0.080 Uiso 1 1 d D . . O4 O 0.6281(7) 0.8646(8) 0.4733(4) 0.071(2) Uani 1 1 d D . . C1 C 0.4693(9) 0.7283(8) 0.7094(4) 0.0398(19) Uani 1 1 d . A . H1A H 0.3887 0.7485 0.6911 0.048 Uiso 1 1 calc R . . C2 C 0.5617(9) 0.8073(9) 0.6901(4) 0.043(2) Uani 1 1 d . . . C3 C 0.6800(10) 0.7804(11) 0.7178(5) 0.055(3) Uani 1 1 d . A . H3A H 0.7444 0.8341 0.7060 0.066 Uiso 1 1 calc R . . C4 C 0.7002(10) 0.6741(11) 0.7625(5) 0.059(3) Uani 1 1 d . . . H4 H 0.7810 0.6524 0.7806 0.070 Uiso 1 1 calc R A . C5 C 0.6040(10) 0.5977(11) 0.7818(5) 0.057(3) Uani 1 1 d . A . H5 H 0.6180 0.5277 0.8146 0.069 Uiso 1 1 calc R . . C6 C 0.5307(10) 0.9227(10) 0.6408(5) 0.052(2) Uani 1 1 d D A . C7 C 0.4746(9) 0.6098(9) 0.5646(4) 0.043(2) Uani 1 1 d . A . H7 H 0.3924 0.6307 0.5478 0.052 Uiso 1 1 calc R . . C8 C 0.5705(9) 0.6783(9) 0.5391(5) 0.046(2) Uani 1 1 d . . . C9 C 0.6924(10) 0.6533(10) 0.5654(5) 0.054(2) Uani 1 1 d . A . H9 H 0.7581 0.7041 0.5501 0.064 Uiso 1 1 calc R . . C10 C 0.7122(9) 0.5519(10) 0.6142(5) 0.051(2) Uani 1 1 d . . . H10 H 0.7940 0.5301 0.6313 0.061 Uiso 1 1 calc R A . C11 C 0.6119(9) 0.4818(9) 0.6380(5) 0.044(2) Uani 1 1 d . A . H11 H 0.6261 0.4131 0.6714 0.053 Uiso 1 1 calc R . . C12 C 0.5448(9) 0.7914(10) 0.4875(5) 0.049(2) Uani 1 1 d D A . C13 C 0.0744(8) 0.3890(8) 0.7594(4) 0.0347(17) Uani 1 1 d . A . H13A H 0.0086 0.3351 0.7787 0.042 Uiso 1 1 calc R . . H13B H 0.0275 0.4704 0.7395 0.042 Uiso 1 1 calc R . . C1B C 0.1944(9) 0.2720(8) 0.8769(4) 0.040(2) Uani 1 1 d . A . C2B C 0.1023(10) 0.1870(10) 0.8902(5) 0.056(3) Uani 1 1 d . . . H2B H 0.0239 0.2039 0.8700 0.067 Uiso 1 1 calc R A . C3B C 0.1311(13) 0.0753(11) 0.9349(6) 0.067(3) Uani 1 1 d . A . H3B H 0.0705 0.0174 0.9453 0.080 Uiso 1 1 calc R . . C4B C 0.2452(13) 0.0507(11) 0.9628(6) 0.068(3) Uani 1 1 d . . . H4B H 0.2624 -0.0252 0.9918 0.082 Uiso 1 1 calc R A . C5B C 0.3375(13) 0.1331(12) 0.9504(5) 0.067(3) Uani 1 1 d . A . H5B H 0.4155 0.1155 0.9710 0.081 Uiso 1 1 calc R . . C6B C 0.3095(10) 0.2443(10) 0.9057(5) 0.051(2) Uani 1 1 d . . . H6B H 0.3713 0.3010 0.8953 0.061 Uiso 1 1 calc R A . C1C C 0.0517(8) 0.3055(8) 0.6447(4) 0.0369(18) Uani 1 1 d . A . C2C C -0.0661(9) 0.2561(9) 0.6671(5) 0.043(2) Uani 1 1 d . . . H2C H -0.0869 0.2357 0.7108 0.052 Uiso 1 1 calc R A . C3C C -0.1507(9) 0.2375(9) 0.6256(5) 0.044(2) Uani 1 1 d . A . H3C H -0.2265 0.2007 0.6407 0.053 Uiso 1 1 calc R . . C4C C -0.1226(10) 0.2735(10) 0.5621(5) 0.055(3) Uani 1 1 d . . . H4C H -0.1809 0.2609 0.5342 0.066 Uiso 1 1 calc R A . C5C C -0.0124(10) 0.3274(11) 0.5373(5) 0.054(3) Uani 1 1 d . A . H5C H 0.0042 0.3527 0.4936 0.065 Uiso 1 1 calc R . . C6C C 0.0745(9) 0.3429(10) 0.5808(4) 0.048(2) Uani 1 1 d . . . H6C H 0.1500 0.3798 0.5654 0.058 Uiso 1 1 calc R A . C1D C 0.2316(8) 0.1540(8) 0.7352(4) 0.0389(19) Uani 1 1 d . A . C2D C 0.1584(12) 0.0532(10) 0.7393(6) 0.064(3) Uani 1 1 d . . . H2D H 0.0802 0.0658 0.7193 0.077 Uiso 1 1 calc R A . C3D C 0.2042(13) -0.0663(10) 0.7739(6) 0.072(3) Uani 1 1 d . A . H3D H 0.1561 -0.1342 0.7771 0.086 Uiso 1 1 calc R . . C4D C 0.3163(12) -0.0846(11) 0.8025(5) 0.063(3) Uani 1 1 d . . . H4D H 0.3449 -0.1646 0.8263 0.075 Uiso 1 1 calc R A . C5D C 0.3891(11) 0.0121(12) 0.7973(6) 0.064(3) Uani 1 1 d . A . H5D H 0.4678 -0.0019 0.8170 0.077 Uiso 1 1 calc R . . C6D C 0.3470(10) 0.1313(10) 0.7627(5) 0.056(3) Uani 1 1 d . . . H6D H 0.3988 0.1967 0.7583 0.067 Uiso 1 1 calc R A . S1 S 0.0890(2) 0.7062(2) 0.63758(11) 0.0434(5) Uani 1 1 d . . . O5 O -0.0274(8) 0.6512(8) 0.6536(4) 0.075(2) Uani 1 1 d . . . O6 O 0.1644(9) 0.7087(8) 0.6889(4) 0.079(3) Uani 1 1 d . . . O7 O 0.1666(8) 0.6662(9) 0.5837(4) 0.080(3) Uani 1 1 d . . . C14 C 0.0320(12) 0.8749(12) 0.6104(6) 0.067(3) Uani 1 1 d . . . F1 F -0.0399(8) 0.9242(8) 0.6576(5) 0.096(3) Uani 1 1 d . . . F2 F -0.0467(10) 0.8875(8) 0.5641(4) 0.109(3) Uani 1 1 d . . . F3 F 0.1250(9) 0.9412(8) 0.5923(6) 0.127(4) Uani 1 1 d . . . S2 S 0.6891(3) 0.2463(3) 0.83206(16) 0.0678(8) Uani 1 1 d . . . O8 O 0.6298(15) 0.2677(17) 0.8911(7) 0.161(7) Uani 1 1 d . . . O9 O 0.5958(11) 0.2666(11) 0.7861(6) 0.117(4) Uani 1 1 d . . . O10 O 0.8034(7) 0.3043(9) 0.8106(5) 0.080(3) Uani 1 1 d . . . C15 C 0.7464(14) 0.0817(15) 0.8398(7) 0.085(4) Uani 1 1 d . . . F4 F 0.6620(10) 0.0072(10) 0.8689(5) 0.130(4) Uani 1 1 d . . . F5 F 0.8465(11) 0.0484(10) 0.8767(7) 0.150(5) Uani 1 1 d . . . F6 F 0.7872(16) 0.0430(10) 0.7861(6) 0.163(6) Uani 1 1 d . . . C1Y C 0.0482(7) 0.5260(7) 0.8622(4) 0.040(5) Uani 0.56(2) 1 d PGU A 1 C2Y C -0.0128(14) 0.4904(8) 0.9217(4) 0.070(6) Uani 0.56(2) 1 d PGU A 1 H2YA H 0.0019 0.4053 0.9422 0.084 Uiso 0.56(2) 1 calc PR A 1 C3Y C -0.0955(15) 0.5806(12) 0.9507(4) 0.092(7) Uani 0.56(2) 1 d PGU A 1 H3YA H -0.1368 0.5565 0.9909 0.110 Uiso 0.56(2) 1 calc PR A 1 C4Y C -0.1172(11) 0.7064(9) 0.9203(6) 0.075(6) Uani 0.56(2) 1 d PGU A 1 H4YA H -0.1731 0.7674 0.9400 0.090 Uiso 0.56(2) 1 calc PR A 1 C5Y C -0.0561(12) 0.7420(6) 0.8609(7) 0.072(6) Uani 0.56(2) 1 d PGU A 1 H5YA H -0.0708 0.8271 0.8403 0.087 Uiso 0.56(2) 1 calc PR A 1 C6Y C 0.0266(11) 0.6518(8) 0.8318(5) 0.052(5) Uani 0.56(2) 1 d PGU A 1 H6YA H 0.0678 0.6759 0.7916 0.063 Uiso 0.56(2) 1 calc PR A 1 C1X C 0.0393(8) 0.5238(7) 0.8626(4) 0.055(8) Uani 0.44(2) 1 d PGU A 2 C2X C 0.0623(8) 0.6464(8) 0.8641(7) 0.069(7) Uani 0.44(2) 1 d PGU A 2 H2XA H 0.1393 0.6749 0.8439 0.083 Uiso 0.44(2) 1 calc PR A 2 C3X C -0.0287(11) 0.7268(8) 0.8954(7) 0.080(7) Uani 0.44(2) 1 d PGU A 2 H3XA H -0.0131 0.8098 0.8964 0.096 Uiso 0.44(2) 1 calc PR A 2 C4X C -0.1426(11) 0.6847(10) 0.9252(5) 0.074(7) Uani 0.44(2) 1 d PGU A 2 H4XA H -0.2041 0.7391 0.9464 0.089 Uiso 0.44(2) 1 calc PR A 2 C5X C -0.1656(11) 0.5621(10) 0.9238(8) 0.067(7) Uani 0.44(2) 1 d PGU A 2 H5XA H -0.2426 0.5336 0.9440 0.080 Uiso 0.44(2) 1 calc PR A 2 C6X C -0.0746(11) 0.4816(7) 0.8925(7) 0.067(7) Uani 0.44(2) 1 d PGU A 2 H6XA H -0.0902 0.3987 0.8915 0.080 Uiso 0.44(2) 1 calc PR A 2 C1S C 0.4067(14) 0.6517(13) 0.9806(5) 0.239(17) Uani 1 1 d DU . . H1SA H 0.3234 0.7028 0.9912 0.287 Uiso 0.590(10) 1 calc PR B 3 H1SB H 0.4454 0.6085 1.0198 0.287 Uiso 0.590(10) 1 calc PR B 3 H1SA H 0.4384 0.5616 0.9796 0.287 Uiso 0.410(10) 1 d PR B 4 H1SB H 0.4009 0.6650 1.0245 0.287 Uiso 0.410(10) 1 d PR B 4 Cl1 Cl 0.5130(9) 0.7472(10) 0.9339(4) 0.251(5) Uani 1 1 d D B . Cl2 Cl 0.3841(17) 0.5413(13) 0.9344(5) 0.204(6) Uani 0.590(10) 1 d PD B 3 Cl3 Cl 0.2538(12) 0.695(2) 0.9499(8) 0.204(6) Uani 0.410(10) 1 d PD B 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03747(19) 0.0427(2) 0.0369(2) -0.00321(14) -0.00230(13) -0.01773(14) Au2 0.03300(18) 0.0420(2) 0.0386(2) -0.00558(14) 0.00118(13) -0.01446(14) P1 0.0348(11) 0.0379(11) 0.0337(11) -0.0045(9) -0.0018(8) -0.0121(9) P2 0.0311(10) 0.0356(11) 0.0349(11) -0.0050(8) -0.0023(8) -0.0103(8) N1 0.039(4) 0.041(4) 0.036(4) -0.002(3) -0.002(3) -0.017(3) N2 0.031(4) 0.043(4) 0.047(4) -0.004(3) 0.003(3) -0.010(3) O1 0.060(5) 0.062(5) 0.079(6) 0.015(4) -0.020(4) -0.021(4) O2 0.073(5) 0.070(5) 0.076(6) 0.015(4) -0.006(4) -0.049(4) O3 0.070(5) 0.074(5) 0.087(6) 0.022(4) -0.039(5) -0.037(4) O4 0.052(4) 0.067(5) 0.088(6) 0.024(4) -0.014(4) -0.035(4) C1 0.038(4) 0.041(5) 0.042(5) -0.005(4) -0.005(4) -0.012(4) C2 0.043(5) 0.038(5) 0.047(5) 0.004(4) 0.003(4) -0.018(4) C3 0.047(5) 0.063(7) 0.057(7) -0.001(5) -0.003(5) -0.026(5) C4 0.040(5) 0.073(7) 0.066(7) -0.002(6) -0.012(5) -0.024(5) C5 0.046(5) 0.071(7) 0.051(6) 0.010(5) -0.008(4) -0.020(5) C6 0.051(6) 0.048(5) 0.053(6) 0.010(4) -0.003(4) -0.018(5) C7 0.039(5) 0.049(5) 0.045(5) -0.012(4) -0.003(4) -0.011(4) C8 0.041(5) 0.042(5) 0.051(6) 0.000(4) 0.004(4) -0.012(4) C9 0.040(5) 0.060(6) 0.062(7) -0.007(5) 0.002(4) -0.019(5) C10 0.033(5) 0.052(6) 0.067(7) -0.003(5) 0.002(4) -0.014(4) C11 0.037(5) 0.038(5) 0.061(6) -0.013(4) -0.003(4) -0.009(4) C12 0.040(5) 0.057(6) 0.051(6) -0.009(4) 0.006(4) -0.013(4) C13 0.036(4) 0.034(4) 0.034(4) 0.002(3) -0.002(3) -0.014(3) C1B 0.043(5) 0.039(5) 0.035(5) 0.007(4) -0.002(4) -0.011(4) C2B 0.053(6) 0.051(6) 0.056(6) 0.009(5) 0.000(5) -0.012(5) C3B 0.081(8) 0.049(6) 0.064(8) 0.008(5) 0.010(6) -0.024(6) C4B 0.088(9) 0.050(6) 0.058(7) 0.010(5) -0.010(6) -0.003(6) C5B 0.080(8) 0.067(7) 0.051(7) -0.002(5) -0.018(6) 0.003(6) C6B 0.050(6) 0.057(6) 0.045(6) -0.005(4) -0.010(4) -0.009(5) C1C 0.032(4) 0.038(4) 0.040(5) -0.008(4) -0.002(3) -0.003(3) C2C 0.040(5) 0.041(5) 0.047(5) -0.003(4) -0.004(4) -0.011(4) C3C 0.041(5) 0.042(5) 0.053(6) -0.009(4) -0.011(4) -0.014(4) C4C 0.049(6) 0.060(6) 0.062(7) -0.014(5) -0.020(5) -0.013(5) C5C 0.058(6) 0.079(7) 0.031(5) -0.014(5) -0.001(4) -0.026(5) C6C 0.040(5) 0.070(6) 0.035(5) -0.003(4) -0.001(4) -0.017(5) C1D 0.039(4) 0.038(4) 0.039(5) -0.003(4) -0.001(4) -0.010(4) C2D 0.060(7) 0.048(6) 0.087(9) 0.004(5) -0.027(6) -0.020(5) C3D 0.090(9) 0.037(5) 0.089(9) 0.007(5) -0.015(7) -0.028(6) C4D 0.081(8) 0.045(6) 0.056(7) -0.004(5) -0.014(6) 0.009(6) C5D 0.054(6) 0.067(7) 0.065(7) -0.005(6) -0.021(5) 0.010(6) C6D 0.045(5) 0.051(6) 0.075(8) -0.013(5) -0.014(5) -0.008(5) S1 0.0405(11) 0.0456(12) 0.0451(13) -0.0007(10) -0.0130(9) -0.0112(10) O5 0.053(5) 0.067(5) 0.108(7) 0.002(5) -0.019(4) -0.026(4) O6 0.089(6) 0.070(5) 0.083(6) 0.009(4) -0.050(5) -0.022(5) O7 0.065(5) 0.100(7) 0.066(6) -0.016(5) 0.000(4) 0.013(5) C14 0.058(7) 0.059(7) 0.076(8) 0.007(6) -0.015(6) -0.006(6) F1 0.089(6) 0.068(5) 0.140(8) -0.042(5) -0.015(5) -0.002(4) F2 0.124(7) 0.088(6) 0.112(7) 0.004(5) -0.075(6) 0.015(5) F3 0.096(6) 0.066(5) 0.206(11) 0.049(6) -0.031(6) -0.040(5) S2 0.0449(14) 0.082(2) 0.082(2) -0.0211(16) 0.0082(13) -0.0265(14) O8 0.153(12) 0.206(16) 0.147(13) -0.097(11) 0.096(10) -0.086(12) O9 0.092(8) 0.099(8) 0.170(12) 0.002(7) -0.061(8) -0.038(7) O10 0.049(4) 0.083(6) 0.112(7) -0.019(5) 0.022(4) -0.031(4) C15 0.081(9) 0.100(11) 0.075(9) 0.013(8) -0.010(7) -0.049(8) F4 0.118(7) 0.122(8) 0.149(9) 0.044(7) -0.041(6) -0.076(7) F5 0.109(8) 0.101(7) 0.246(14) 0.010(8) -0.086(9) -0.035(6) F6 0.267(17) 0.081(7) 0.140(11) -0.037(6) 0.030(10) -0.033(9) C1Y 0.051(10) 0.056(11) 0.023(9) -0.021(8) -0.003(8) -0.023(9) C2Y 0.082(12) 0.065(10) 0.065(11) -0.027(9) 0.026(9) -0.019(9) C3Y 0.095(13) 0.089(12) 0.085(12) -0.027(10) 0.053(11) -0.020(11) C4Y 0.083(12) 0.068(11) 0.079(12) -0.027(10) 0.033(10) -0.032(10) C5Y 0.075(11) 0.079(12) 0.068(11) -0.020(9) -0.011(9) -0.017(10) C6Y 0.059(10) 0.060(10) 0.044(9) -0.020(7) -0.009(7) -0.013(8) C1X 0.045(13) 0.046(13) 0.071(16) -0.001(13) 0.001(13) -0.009(12) C2X 0.069(13) 0.035(10) 0.104(16) -0.004(10) 0.017(12) -0.035(9) C3X 0.097(14) 0.035(10) 0.120(17) -0.040(10) 0.023(13) -0.037(10) C4X 0.073(13) 0.045(11) 0.102(16) -0.021(11) 0.033(12) -0.018(11) C5X 0.065(13) 0.055(11) 0.079(14) -0.024(10) 0.027(11) -0.007(10) C6X 0.059(12) 0.061(12) 0.072(14) -0.017(10) 0.019(11) 0.007(10) C1S 0.242(19) 0.238(19) 0.248(19) -0.044(10) -0.031(10) -0.055(10) Cl1 0.184(8) 0.381(15) 0.173(8) 0.043(8) -0.063(6) -0.073(9) Cl2 0.322(17) 0.212(11) 0.103(6) -0.007(6) -0.027(8) -0.132(11) Cl3 0.322(17) 0.212(11) 0.103(6) -0.007(6) -0.027(8) -0.132(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.083(7) . ? Au1 P1 2.239(2) . ? Au1 Au2 3.1680(5) . ? Au2 N2 2.086(7) . ? Au2 P2 2.239(2) . ? P1 C1Y 1.795(6) . ? P1 C1B 1.805(8) . ? P1 C13 1.825(9) . ? P1 C1X 1.835(6) . ? P2 C1C 1.795(9) . ? P2 C1D 1.810(9) . ? P2 C13 1.816(9) . ? N1 C1 1.350(11) . ? N1 C5 1.362(12) . ? N2 C7 1.354(12) . ? N2 C11 1.367(12) . ? O1 C6 1.268(12) . ? O2 C6 1.257(11) . ? O3 C12 1.267(12) . ? O4 C12 1.242(12) . ? C1 C2 1.369(12) . ? C2 C3 1.388(14) . ? C2 C6 1.498(13) . ? C3 C4 1.361(15) . ? C4 C5 1.380(14) . ? C7 C8 1.347(12) . ? C8 C9 1.408(14) . ? C8 C12 1.504(14) . ? C9 C10 1.379(15) . ? C10 C11 1.386(12) . ? C1B C6B 1.371(13) . ? C1B C2B 1.403(13) . ? C2B C3B 1.412(14) . ? C3B C4B 1.352(18) . ? C4B C5B 1.385(18) . ? C5B C6B 1.407(15) . ? C1C C6C 1.375(12) . ? C1C C2C 1.418(12) . ? C2C C3C 1.381(13) . ? C3C C4C 1.372(14) . ? C4C C5C 1.382(14) . ? C5C C6C 1.418(13) . ? C1D C6D 1.361(13) . ? C1D C2D 1.410(13) . ? C2D C3D 1.404(15) . ? C3D C4D 1.345(17) . ? C4D C5D 1.367(17) . ? C5D C6D 1.393(15) . ? S1 O5 1.415(8) . ? S1 O6 1.430(8) . ? S1 O7 1.442(9) . ? S1 C14 1.830(12) . ? C14 F3 1.280(14) . ? C14 F2 1.331(14) . ? C14 F1 1.342(16) . ? S2 O8 1.404(11) . ? S2 O9 1.424(11) . ? S2 O10 1.427(7) . ? S2 C15 1.766(17) . ? C15 F6 1.315(19) . ? C15 F4 1.318(14) . ? C15 F5 1.339(16) . ? C1Y C2Y 1.3900 . ? C1Y C6Y 1.3900 . ? C2Y C3Y 1.3900 . ? C3Y C4Y 1.3900 . ? C4Y C5Y 1.3900 . ? C5Y C6Y 1.3900 . ? C1X C2X 1.3900 . ? C1X C6X 1.3900 . ? C2X C3X 1.3900 . ? C3X C4X 1.3900 . ? C4X C5X 1.3900 . ? C5X C6X 1.3900 . ? C1S Cl3 1.747(5) . ? C1S Cl1 1.748(5) . ? C1S Cl2 1.750(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Au1 P1 172.5(2) . . ? N1 Au1 Au2 95.2(2) . . ? P1 Au1 Au2 89.95(6) . . ? N2 Au2 P2 178.2(2) . . ? N2 Au2 Au1 92.8(2) . . ? P2 Au2 Au1 88.25(6) . . ? C1Y P1 C1B 107.0(4) . . ? C1Y P1 C13 104.5(4) . . ? C1B P1 C13 107.6(4) . . ? C1Y P1 C1X 2.9 . . ? C1B P1 C1X 106.2(4) . . ? C13 P1 C1X 102.3(4) . . ? C1Y P1 Au1 109.2(3) . . ? C1B P1 Au1 115.8(3) . . ? C13 P1 Au1 112.1(3) . . ? C1X P1 Au1 111.8(3) . . ? C1C P2 C1D 108.8(4) . . ? C1C P2 C13 103.6(4) . . ? C1D P2 C13 105.9(4) . . ? C1C P2 Au2 115.1(3) . . ? C1D P2 Au2 110.8(3) . . ? C13 P2 Au2 112.1(3) . . ? C1 N1 C5 117.9(8) . . ? C1 N1 Au1 120.1(6) . . ? C5 N1 Au1 121.6(6) . . ? C7 N2 C11 118.9(8) . . ? C7 N2 Au2 120.0(6) . . ? C11 N2 Au2 120.9(6) . . ? N1 C1 C2 122.8(8) . . ? C1 C2 C3 119.2(8) . . ? C1 C2 C6 118.9(9) . . ? C3 C2 C6 121.8(8) . . ? C4 C3 C2 118.2(9) . . ? C3 C4 C5 121.1(10) . . ? N1 C5 C4 120.7(9) . . ? O2 C6 O1 125.1(9) . . ? O2 C6 C2 117.7(9) . . ? O1 C6 C2 117.2(8) . . ? C8 C7 N2 122.3(9) . . ? C7 C8 C9 120.0(9) . . ? C7 C8 C12 120.9(9) . . ? C9 C8 C12 118.8(8) . . ? C10 C9 C8 117.9(9) . . ? C9 C10 C11 120.2(9) . . ? N2 C11 C10 120.6(9) . . ? O4 C12 O3 125.0(10) . . ? O4 C12 C8 118.5(9) . . ? O3 C12 C8 116.4(9) . . ? P2 C13 P1 116.8(5) . . ? C6B C1B C2B 120.2(8) . . ? C6B C1B P1 119.0(7) . . ? C2B C1B P1 120.8(7) . . ? C1B C2B C3B 117.9(10) . . ? C4B C3B C2B 120.6(11) . . ? C3B C4B C5B 122.5(10) . . ? C4B C5B C6B 117.0(11) . . ? C1B C6B C5B 121.7(10) . . ? C6C C1C C2C 118.0(8) . . ? C6C C1C P2 120.8(7) . . ? C2C C1C P2 121.1(7) . . ? C3C C2C C1C 120.8(9) . . ? C4C C3C C2C 119.1(9) . . ? C3C C4C C5C 123.0(9) . . ? C4C C5C C6C 116.9(9) . . ? C1C C6C C5C 122.1(9) . . ? C6D C1D C2D 119.0(9) . . ? C6D C1D P2 119.7(7) . . ? C2D C1D P2 121.2(7) . . ? C3D C2D C1D 119.0(10) . . ? C4D C3D C2D 120.6(11) . . ? C3D C4D C5D 120.5(10) . . ? C4D C5D C6D 120.2(10) . . ? C1D C6D C5D 120.6(10) . . ? O5 S1 O6 116.1(6) . . ? O5 S1 O7 114.3(6) . . ? O6 S1 O7 113.5(6) . . ? O5 S1 C14 104.2(5) . . ? O6 S1 C14 102.9(6) . . ? O7 S1 C14 103.8(6) . . ? F3 C14 F2 110.1(11) . . ? F3 C14 F1 107.5(12) . . ? F2 C14 F1 106.5(11) . . ? F3 C14 S1 113.4(9) . . ? F2 C14 S1 109.8(9) . . ? F1 C14 S1 109.3(8) . . ? O8 S2 O9 111.7(10) . . ? O8 S2 O10 116.1(7) . . ? O9 S2 O10 113.8(7) . . ? O8 S2 C15 106.8(9) . . ? O9 S2 C15 103.3(7) . . ? O10 S2 C15 103.7(6) . . ? F6 C15 F4 106.9(14) . . ? F6 C15 F5 106.8(16) . . ? F4 C15 F5 102.0(11) . . ? F6 C15 S2 114.1(10) . . ? F4 C15 S2 114.8(12) . . ? F5 C15 S2 111.2(12) . . ? C2Y C1Y C6Y 120.0 . . ? C2Y C1Y P1 123.7(5) . . ? C6Y C1Y P1 116.2(5) . . ? C3Y C2Y C1Y 120.0 . . ? C2Y C3Y C4Y 120.0 . . ? C3Y C4Y C5Y 120.0 . . ? C6Y C5Y C4Y 120.0 . . ? C5Y C6Y C1Y 120.0 . . ? C2X C1X C6X 120.0 . . ? C2X C1X P1 118.6(5) . . ? C6X C1X P1 121.4(5) . . ? C1X C2X C3X 120.0 . . ? C2X C3X C4X 120.0 . . ? C3X C4X C5X 120.0 . . ? C6X C5X C4X 120.0 . . ? C5X C6X C1X 120.0 . . ? Cl3 C1S Cl1 107.2(4) . . ? Cl3 C1S Cl2 70.8(11) . . ? Cl1 C1S Cl2 104.9(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.90(2) 1.74(3) 2.637(10) 171(8) 2_676 O3 H3 O2 0.90(2) 1.79(6) 2.624(11) 153(12) 2_676 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.293 _refine_diff_density_min -1.628 _refine_diff_density_rms 0.216 # Attachment 'complex_3.cif' data_7338 _database_code_depnum_ccdc_archive 'CCDC 715602' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H34 Au2 F6 N2 O10 P2 S2' _chemical_formula_weight 1336.69 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' 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 11.5340(8) _cell_length_b 14.5704(11) _cell_length_c 15.1800(11) _cell_angle_alpha 99.0260(10) _cell_angle_beta 99.8100(10) _cell_angle_gamma 111.1180(10) _cell_volume 2277.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 8235 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.51 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'Not Measured' _exptl_crystal_density_diffrn 1.949 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 6.676 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1082 _exptl_absorpt_correction_T_max 0.7761 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29720 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10434 _reflns_number_gt 8018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One of the Otf had very bad thermal parameters and was refined with restraints in bond lengths and thermal parameters. ; _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^)+(0.0672P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10434 _refine_ls_number_parameters 579 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1207 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.050 _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 0.47208(2) 0.455754(18) 0.264519(15) 0.03797(9) Uani 1 1 d . . . Au2 Au 0.59350(2) 0.895049(19) 0.269314(16) 0.04176(9) Uani 1 1 d . . . P1 P 0.40620(14) 0.80728(13) 0.29785(10) 0.0374(3) Uani 1 1 d . . . P2 P 0.33756(14) 0.49173(12) 0.16572(10) 0.0329(3) Uani 1 1 d . . . N1 N 0.6019(5) 0.4272(4) 0.3567(3) 0.0415(12) Uani 1 1 d . . . N2 N 0.7667(5) 0.9692(4) 0.2381(4) 0.0422(12) Uani 1 1 d . . . O1 O 0.9728(5) 0.3685(5) 0.5061(3) 0.0657(15) Uani 1 1 d . . . H1 H 1.0251 0.3586 0.5441 0.099 Uiso 1 1 calc R . . O2 O 0.8912(5) 0.3955(4) 0.6264(3) 0.0615(14) Uani 1 1 d . . . O3 O 1.2111(5) 1.1116(5) 0.2080(4) 0.0779(18) Uani 1 1 d . . . H3 H 1.2767 1.1469 0.1942 0.117 Uiso 1 1 calc R . . O4 O 1.1137(6) 1.1567(7) 0.0967(6) 0.121(3) Uani 1 1 d . . . C1 C 0.5871(7) 0.4152(7) 0.4392(5) 0.059(2) Uani 1 1 d . . . H1A H 0.5108 0.4128 0.4548 0.071 Uiso 1 1 calc R . . C2 C 0.6800(7) 0.4062(7) 0.5025(5) 0.062(2) Uani 1 1 d . . . H2 H 0.6702 0.4039 0.5624 0.074 Uiso 1 1 calc R . . C3 C 0.7873(6) 0.4006(5) 0.4788(4) 0.0374(13) Uani 1 1 d . . . C4 C 0.7992(8) 0.4093(7) 0.3917(5) 0.065(2) Uani 1 1 d . . . H4 H 0.8708 0.4057 0.3722 0.078 Uiso 1 1 calc R . . C5 C 0.7064(8) 0.4232(7) 0.3341(5) 0.069(2) Uani 1 1 d . . . H5 H 0.7168 0.4304 0.2751 0.082 Uiso 1 1 calc R . . C6 C 0.8886(6) 0.3878(6) 0.5464(5) 0.0468(16) Uani 1 1 d . . . C7 C 0.8682(6) 0.9482(6) 0.2652(5) 0.0479(16) Uani 1 1 d . . . H7 H 0.8624 0.9008 0.3014 0.057 Uiso 1 1 calc R . . C8 C 0.9827(6) 0.9947(5) 0.2410(5) 0.0476(16) Uani 1 1 d . . . H8 H 1.0533 0.9788 0.2612 0.057 Uiso 1 1 calc R . . C9 C 0.9922(6) 1.0637(5) 0.1878(5) 0.0466(15) Uani 1 1 d . . . C10 C 0.8878(7) 1.0858(6) 0.1627(6) 0.064(2) Uani 1 1 d . . . H10 H 0.8921 1.1339 0.1274 0.077 Uiso 1 1 calc R . . C11 C 0.7758(7) 1.0385(6) 0.1885(6) 0.060(2) Uani 1 1 d . . . H11 H 0.7052 1.0553 0.1708 0.072 Uiso 1 1 calc R . . C12 C 1.1124(7) 1.1161(7) 0.1579(6) 0.062(2) Uani 1 1 d . . . C13 C 0.3773(6) 0.6271(5) 0.1836(4) 0.0376(13) Uani 1 1 d . . . H13A H 0.4610 0.6603 0.1708 0.045 Uiso 1 1 calc R . . H13B H 0.3133 0.6384 0.1402 0.045 Uiso 1 1 calc R . . C14 C 0.3813(5) 0.6748(4) 0.2812(4) 0.0345(12) Uani 1 1 d . . . H14A H 0.4506 0.6689 0.3241 0.041 Uiso 1 1 calc R . . H14B H 0.3003 0.6372 0.2958 0.041 Uiso 1 1 calc R . . C1A C 0.3990(6) 0.8427(5) 0.4150(4) 0.0435(15) Uani 1 1 d . . . C2A C 0.2959(7) 0.8558(6) 0.4399(5) 0.0543(17) Uani 1 1 d . . . H2A H 0.2269 0.8523 0.3945 0.065 Uiso 1 1 calc R . . C3A C 0.2932(9) 0.8746(6) 0.5332(6) 0.069(2) Uani 1 1 d . . . H3A H 0.2226 0.8831 0.5503 0.083 Uiso 1 1 calc R . . C4A C 0.3933(10) 0.8801(6) 0.5979(6) 0.074(3) Uani 1 1 d . . . H4A H 0.3904 0.8915 0.6601 0.089 Uiso 1 1 calc R . . C5A C 0.4959(9) 0.8698(7) 0.5762(5) 0.067(2) Uani 1 1 d . . . H5A H 0.5649 0.8753 0.6228 0.081 Uiso 1 1 calc R . . C6A C 0.5005(8) 0.8506(7) 0.4833(5) 0.064(2) Uani 1 1 d . . . H6A H 0.5727 0.8432 0.4677 0.077 Uiso 1 1 calc R . . C1B C 0.2687(6) 0.8081(5) 0.2213(4) 0.0430(15) Uani 1 1 d . . . C2B C 0.2857(7) 0.8823(6) 0.1707(5) 0.0527(17) Uani 1 1 d . . . H2B H 0.3673 0.9339 0.1801 0.063 Uiso 1 1 calc R . . C3B C 0.1830(8) 0.8800(7) 0.1068(6) 0.065(2) Uani 1 1 d . . . H3B H 0.1948 0.9296 0.0724 0.078 Uiso 1 1 calc R . . C4B C 0.0628(8) 0.8043(8) 0.0937(6) 0.070(2) Uani 1 1 d . . . H4B H -0.0067 0.8024 0.0498 0.083 Uiso 1 1 calc R . . C5B C 0.0435(7) 0.7324(7) 0.1433(6) 0.070(2) Uani 1 1 d . . . H5B H -0.0390 0.6819 0.1340 0.084 Uiso 1 1 calc R . . C6B C 0.1455(6) 0.7334(6) 0.2080(5) 0.0552(19) Uani 1 1 d . . . H6B H 0.1318 0.6841 0.2426 0.066 Uiso 1 1 calc R . . C1C C 0.1744(5) 0.4377(5) 0.1772(4) 0.0425(14) Uani 1 1 d . . . C2C C 0.0764(7) 0.4404(8) 0.1151(6) 0.072(3) Uani 1 1 d . . . H2C H 0.0932 0.4703 0.0656 0.086 Uiso 1 1 calc R . . C3C C -0.0493(7) 0.3990(9) 0.1245(7) 0.094(4) Uani 1 1 d . . . H3C H -0.1167 0.4018 0.0818 0.112 Uiso 1 1 calc R . . C4C C -0.0734(8) 0.3557(9) 0.1942(7) 0.095(4) Uani 1 1 d . . . H4C H -0.1583 0.3273 0.1998 0.113 Uiso 1 1 calc R . . C5C C 0.0222(9) 0.3519(8) 0.2570(7) 0.084(3) Uani 1 1 d . . . H5C H 0.0035 0.3216 0.3060 0.101 Uiso 1 1 calc R . . C6C C 0.1488(7) 0.3930(6) 0.2491(5) 0.059(2) Uani 1 1 d . . . H6C H 0.2155 0.3902 0.2924 0.071 Uiso 1 1 calc R . . C1D C 0.3267(5) 0.4437(5) 0.0458(4) 0.0380(13) Uani 1 1 d . . . C2D C 0.3426(6) 0.5077(6) -0.0164(4) 0.0467(16) Uani 1 1 d . . . H2D H 0.3622 0.5772 0.0039 0.056 Uiso 1 1 calc R . . C3D C 0.3287(7) 0.4662(8) -0.1064(5) 0.061(2) Uani 1 1 d . . . H3D H 0.3358 0.5075 -0.1486 0.073 Uiso 1 1 calc R . . C4D C 0.3047(7) 0.3656(9) -0.1375(5) 0.071(3) Uani 1 1 d . . . H4D H 0.2988 0.3395 -0.1995 0.085 Uiso 1 1 calc R . . C5D C 0.2897(8) 0.3055(7) -0.0787(6) 0.073(2) Uani 1 1 d . . . H5D H 0.2690 0.2361 -0.1009 0.088 Uiso 1 1 calc R . . C6D C 0.3043(6) 0.3438(6) 0.0172(5) 0.0491(16) Uani 1 1 d . . . H6D H 0.2988 0.3018 0.0588 0.059 Uiso 1 1 calc R . . S1 S 0.75735(18) 0.71460(14) 0.42694(12) 0.0524(4) Uani 1 1 d . . . O5 O 0.7114(6) 0.7581(5) 0.3613(4) 0.087(2) Uani 1 1 d . . . O6 O 0.8338(6) 0.6630(5) 0.3980(4) 0.0792(18) Uani 1 1 d . . . O7 O 0.6645(9) 0.6622(6) 0.4699(7) 0.146(4) Uani 1 1 d . . . C15 C 0.8644(11) 0.8183(10) 0.5200(9) 0.107(4) Uani 1 1 d . . . F1 F 0.8127(7) 0.8763(6) 0.5517(5) 0.156(4) Uani 1 1 d . . . F2 F 0.9585(9) 0.8775(8) 0.4839(9) 0.200(5) Uani 1 1 d . . . F3 F 0.9268(10) 0.7968(8) 0.5825(5) 0.188(5) Uani 1 1 d . . . S2 S 0.5239(2) 0.1957(2) 0.13435(17) 0.0764(7) Uani 1 1 d DU . . C16 C 0.4954(11) 0.1463(7) 0.0140(5) 0.177(7) Uani 1 1 d DU . . O8 O 0.4161(8) 0.2048(8) 0.1533(7) 0.169(5) Uani 1 1 d DU . . F4 F 0.4922(15) 0.2137(10) -0.0295(6) 0.260(7) Uani 1 1 d DU . . O9 O 0.5732(11) 0.1439(9) 0.1813(5) 0.224(7) Uani 1 1 d DU . . F5 F 0.5905(15) 0.1236(11) 0.0024(7) 0.284(8) Uani 1 1 d DU . . O10 O 0.6162(10) 0.2972(6) 0.1421(9) 0.284(9) Uani 1 1 d DU . . F6 F 0.3903(13) 0.0696(11) -0.0088(9) 0.414(12) Uani 1 1 d DU . . 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 0.03928(14) 0.04604(16) 0.03461(13) 0.01648(10) 0.00889(10) 0.02105(11) Au2 0.03598(14) 0.04631(17) 0.04560(15) 0.01227(11) 0.01461(10) 0.01671(11) P1 0.0350(8) 0.0442(9) 0.0371(8) 0.0107(7) 0.0108(6) 0.0191(7) P2 0.0320(7) 0.0424(9) 0.0293(7) 0.0134(6) 0.0109(6) 0.0169(6) N1 0.047(3) 0.044(3) 0.040(3) 0.017(2) 0.008(2) 0.023(2) N2 0.036(3) 0.046(3) 0.050(3) 0.014(2) 0.018(2) 0.017(2) O1 0.068(3) 0.109(5) 0.049(3) 0.030(3) 0.014(2) 0.063(3) O2 0.055(3) 0.095(4) 0.046(3) 0.034(3) 0.013(2) 0.036(3) O3 0.050(3) 0.105(5) 0.090(4) 0.045(4) 0.033(3) 0.028(3) O4 0.069(4) 0.193(9) 0.147(7) 0.129(7) 0.056(4) 0.053(5) C1 0.047(4) 0.095(6) 0.057(4) 0.046(4) 0.025(3) 0.036(4) C2 0.054(4) 0.105(7) 0.053(4) 0.052(4) 0.027(3) 0.042(4) C3 0.039(3) 0.037(3) 0.039(3) 0.013(3) 0.009(2) 0.017(3) C4 0.074(5) 0.110(7) 0.043(4) 0.031(4) 0.022(4) 0.064(5) C5 0.076(5) 0.119(8) 0.040(4) 0.030(4) 0.025(4) 0.062(5) C6 0.038(3) 0.060(4) 0.052(4) 0.025(3) 0.012(3) 0.025(3) C7 0.047(4) 0.054(4) 0.046(4) 0.018(3) 0.012(3) 0.021(3) C8 0.035(3) 0.054(4) 0.058(4) 0.023(3) 0.015(3) 0.019(3) C9 0.041(3) 0.050(4) 0.052(4) 0.019(3) 0.017(3) 0.017(3) C10 0.061(5) 0.067(5) 0.082(6) 0.042(4) 0.026(4) 0.032(4) C11 0.046(4) 0.070(5) 0.087(6) 0.040(4) 0.023(4) 0.035(4) C12 0.051(4) 0.075(6) 0.070(5) 0.034(4) 0.025(4) 0.025(4) C13 0.039(3) 0.045(4) 0.037(3) 0.017(3) 0.012(2) 0.022(3) C14 0.027(3) 0.046(4) 0.034(3) 0.015(3) 0.011(2) 0.015(3) C1A 0.046(4) 0.044(4) 0.047(4) 0.013(3) 0.023(3) 0.020(3) C2A 0.057(4) 0.059(5) 0.052(4) 0.005(3) 0.019(3) 0.030(4) C3A 0.077(6) 0.068(6) 0.065(5) 0.002(4) 0.040(5) 0.028(4) C4A 0.116(8) 0.050(5) 0.044(4) -0.001(3) 0.027(5) 0.022(5) C5A 0.086(6) 0.072(6) 0.043(4) 0.003(4) 0.011(4) 0.038(5) C6A 0.058(5) 0.086(6) 0.043(4) 0.005(4) 0.010(3) 0.030(4) C1B 0.042(3) 0.054(4) 0.041(3) 0.010(3) 0.010(3) 0.028(3) C2B 0.052(4) 0.056(5) 0.056(4) 0.019(3) 0.014(3) 0.026(4) C3B 0.065(5) 0.077(6) 0.065(5) 0.036(4) 0.016(4) 0.035(5) C4B 0.060(5) 0.099(7) 0.064(5) 0.028(5) 0.007(4) 0.049(5) C5B 0.041(4) 0.087(6) 0.086(6) 0.027(5) 0.011(4) 0.029(4) C6B 0.042(4) 0.073(5) 0.064(5) 0.029(4) 0.014(3) 0.032(4) C1C 0.029(3) 0.052(4) 0.042(3) 0.009(3) 0.011(2) 0.010(3) C2C 0.044(4) 0.119(8) 0.057(5) 0.030(5) 0.016(4) 0.032(5) C3C 0.034(4) 0.157(11) 0.073(6) 0.010(6) 0.010(4) 0.027(5) C4C 0.044(5) 0.133(10) 0.079(7) -0.007(6) 0.027(5) 0.011(5) C5C 0.070(6) 0.088(7) 0.090(7) 0.023(5) 0.048(5) 0.013(5) C6C 0.052(4) 0.070(5) 0.057(4) 0.015(4) 0.031(3) 0.015(4) C1D 0.031(3) 0.053(4) 0.035(3) 0.013(3) 0.012(2) 0.019(3) C2D 0.045(4) 0.062(4) 0.043(3) 0.024(3) 0.019(3) 0.025(3) C3D 0.046(4) 0.104(7) 0.042(4) 0.029(4) 0.021(3) 0.030(4) C4D 0.048(4) 0.141(9) 0.027(3) 0.009(5) 0.016(3) 0.043(5) C5D 0.063(5) 0.081(6) 0.058(5) -0.022(4) 0.010(4) 0.028(4) C6D 0.053(4) 0.055(4) 0.042(3) 0.006(3) 0.011(3) 0.027(3) S1 0.0583(10) 0.0563(11) 0.0482(9) 0.0131(8) 0.0130(8) 0.0289(9) O5 0.105(5) 0.104(5) 0.073(4) 0.023(4) 0.006(3) 0.074(4) O6 0.088(4) 0.111(5) 0.059(3) 0.007(3) 0.005(3) 0.074(4) O7 0.176(8) 0.087(6) 0.172(8) 0.033(5) 0.128(7) 0.010(5) C15 0.079(7) 0.097(9) 0.120(10) -0.023(7) -0.015(7) 0.043(7) F1 0.124(6) 0.138(6) 0.158(7) -0.084(5) -0.051(5) 0.085(5) F2 0.110(7) 0.140(8) 0.249(12) -0.014(7) -0.009(7) -0.017(6) F3 0.229(10) 0.246(10) 0.087(5) -0.045(5) -0.074(6) 0.177(9) S2 0.0460(11) 0.0983(18) 0.0864(16) 0.0094(13) 0.0205(10) 0.0336(12) C16 0.288(18) 0.150(12) 0.154(13) 0.086(11) 0.079(12) 0.127(13) O8 0.103(6) 0.239(12) 0.246(12) 0.136(10) 0.113(7) 0.095(7) F4 0.48(2) 0.235(13) 0.187(10) 0.136(10) 0.155(12) 0.215(14) O9 0.383(16) 0.418(18) 0.099(6) 0.139(9) 0.120(8) 0.360(15) F5 0.51(2) 0.392(18) 0.230(11) 0.191(12) 0.291(14) 0.357(17) O10 0.210(13) 0.146(11) 0.318(19) -0.029(11) 0.005(13) -0.071(9) F6 0.42(2) 0.38(2) 0.223(14) -0.118(14) -0.068(15) 0.050(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.071(5) . ? Au1 P2 2.2296(14) . ? Au2 N2 2.076(5) . ? Au2 P1 2.2342(16) . ? P1 C1A 1.797(7) . ? P1 C1B 1.804(6) . ? P1 C14 1.815(6) . ? P2 C1D 1.810(6) . ? P2 C1C 1.811(6) . ? P2 C13 1.821(6) . ? N1 C1 1.322(8) . ? N1 C5 1.327(9) . ? N2 C7 1.328(8) . ? N2 C11 1.338(8) . ? O1 C6 1.320(8) . ? O2 C6 1.195(8) . ? O3 C12 1.285(9) . ? O4 C12 1.177(9) . ? C1 C2 1.371(9) . ? C2 C3 1.372(9) . ? C3 C4 1.372(9) . ? C3 C6 1.503(8) . ? C4 C5 1.358(9) . ? C7 C8 1.391(9) . ? C8 C9 1.372(9) . ? C9 C10 1.363(9) . ? C9 C12 1.507(9) . ? C10 C11 1.383(10) . ? C13 C14 1.520(8) . ? C1A C2A 1.375(9) . ? C1A C6A 1.382(10) . ? C2A C3A 1.407(10) . ? C3A C4A 1.351(12) . ? C4A C5A 1.333(12) . ? C5A C6A 1.409(10) . ? C1B C2B 1.398(9) . ? C1B C6B 1.401(10) . ? C2B C3B 1.384(10) . ? C3B C4B 1.383(12) . ? C4B C5B 1.360(12) . ? C5B C6B 1.392(10) . ? C1C C2C 1.360(10) . ? C1C C6C 1.378(9) . ? C2C C3C 1.397(11) . ? C3C C4C 1.334(14) . ? C4C C5C 1.353(14) . ? C5C C6C 1.400(11) . ? C1D C6D 1.366(9) . ? C1D C2D 1.418(8) . ? C2D C3D 1.362(10) . ? C3D C4D 1.376(12) . ? C4D C5D 1.335(13) . ? C5D C6D 1.433(10) . ? S1 O5 1.391(6) . ? S1 O7 1.400(7) . ? S1 O6 1.429(5) . ? S1 C15 1.787(11) . ? C15 F3 1.240(13) . ? C15 F1 1.279(12) . ? C15 F2 1.377(17) . ? S2 O9 1.319(6) . ? S2 O8 1.369(6) . ? S2 O10 1.450(7) . ? S2 C16 1.782(7) . ? C16 F6 1.265(9) . ? C16 F4 1.275(8) . ? C16 F5 1.285(9) . ? 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 N1 Au1 P2 178.03(15) . . ? N2 Au2 P1 176.80(16) . . ? C1A P1 C1B 109.4(3) . . ? C1A P1 C14 103.9(3) . . ? C1B P1 C14 105.1(3) . . ? C1A P1 Au2 114.0(2) . . ? C1B P1 Au2 114.0(2) . . ? C14 P1 Au2 109.51(18) . . ? C1D P2 C1C 104.6(3) . . ? C1D P2 C13 107.4(3) . . ? C1C P2 C13 104.9(3) . . ? C1D P2 Au1 114.3(2) . . ? C1C P2 Au1 112.2(2) . . ? C13 P2 Au1 112.7(2) . . ? C1 N1 C5 117.8(5) . . ? C1 N1 Au1 122.7(4) . . ? C5 N1 Au1 119.5(4) . . ? C7 N2 C11 119.2(6) . . ? C7 N2 Au2 121.5(4) . . ? C11 N2 Au2 119.3(4) . . ? N1 C1 C2 121.8(6) . . ? C1 C2 C3 120.3(6) . . ? C4 C3 C2 117.2(6) . . ? C4 C3 C6 121.7(6) . . ? C2 C3 C6 121.1(6) . . ? C5 C4 C3 119.4(7) . . ? N1 C5 C4 123.4(6) . . ? O2 C6 O1 125.4(6) . . ? O2 C6 C3 123.3(6) . . ? O1 C6 C3 111.3(5) . . ? N2 C7 C8 121.6(6) . . ? C9 C8 C7 119.8(6) . . ? C10 C9 C8 117.5(6) . . ? C10 C9 C12 119.6(6) . . ? C8 C9 C12 122.9(6) . . ? C9 C10 C11 121.0(7) . . ? N2 C11 C10 120.8(6) . . ? O4 C12 O3 125.2(7) . . ? O4 C12 C9 123.1(7) . . ? O3 C12 C9 111.7(6) . . ? C14 C13 P2 112.1(4) . . ? C13 C14 P1 112.9(4) . . ? C2A C1A C6A 118.8(6) . . ? C2A C1A P1 123.9(5) . . ? C6A C1A P1 117.2(5) . . ? C1A C2A C3A 120.2(7) . . ? C4A C3A C2A 119.4(8) . . ? C5A C4A C3A 121.9(8) . . ? C4A C5A C6A 119.8(8) . . ? C1A C6A C5A 120.0(7) . . ? C2B C1B C6B 118.8(6) . . ? C2B C1B P1 119.5(5) . . ? C6B C1B P1 121.6(5) . . ? C3B C2B C1B 120.4(7) . . ? C4B C3B C2B 119.6(7) . . ? C5B C4B C3B 121.1(7) . . ? C4B C5B C6B 120.2(8) . . ? C5B C6B C1B 119.9(7) . . ? C2C C1C C6C 119.5(6) . . ? C2C C1C P2 120.6(5) . . ? C6C C1C P2 119.9(5) . . ? C1C C2C C3C 120.4(8) . . ? C4C C3C C2C 119.8(9) . . ? C3C C4C C5C 121.1(8) . . ? C4C C5C C6C 120.1(9) . . ? C1C C6C C5C 119.1(8) . . ? C6D C1D C2D 120.8(6) . . ? C6D C1D P2 117.9(5) . . ? C2D C1D P2 121.2(5) . . ? C3D C2D C1D 118.4(7) . . ? C2D C3D C4D 122.1(7) . . ? C5D C4D C3D 119.3(7) . . ? C4D C5D C6D 121.9(9) . . ? C1D C6D C5D 117.4(7) . . ? O5 S1 O7 113.4(6) . . ? O5 S1 O6 114.2(4) . . ? O7 S1 O6 115.4(5) . . ? O5 S1 C15 105.5(6) . . ? O7 S1 C15 101.5(7) . . ? O6 S1 C15 105.0(5) . . ? F3 C15 F1 111.7(12) . . ? F3 C15 F2 102.6(11) . . ? F1 C15 F2 105.3(12) . . ? F3 C15 S1 116.1(10) . . ? F1 C15 S1 113.4(8) . . ? F2 C15 S1 106.2(10) . . ? O9 S2 O8 117.2(5) . . ? O9 S2 O10 112.5(5) . . ? O8 S2 O10 106.9(5) . . ? O9 S2 C16 110.1(5) . . ? O8 S2 C16 109.7(5) . . ? O10 S2 C16 99.0(5) . . ? F6 C16 F4 112.3(8) . . ? F6 C16 F5 112.5(8) . . ? F4 C16 F5 108.8(7) . . ? F6 C16 S2 106.2(7) . . ? F4 C16 S2 110.0(7) . . ? F5 C16 S2 106.8(7) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O6 0.83 1.87 2.673(7) 163.5 2_766 O3 H3 O8 0.83 1.79 2.615(8) 171.0 1_665 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.975 _refine_diff_density_min -1.236 _refine_diff_density_rms 0.163 # Attachment 'complex_4.cif' data_8523 _database_code_depnum_ccdc_archive 'CCDC 715603' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H38 Au2 F6 N2 O13 P2 S2' _chemical_formula_weight 1388.72 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.6240(5) _cell_length_b 20.5776(11) _cell_length_c 20.8821(11) _cell_angle_alpha 90.00 _cell_angle_beta 93.5220(10) _cell_angle_gamma 90.00 _cell_volume 4556.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8252 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.51 _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 6.684 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1752 _exptl_absorpt_correction_T_max 0.5546 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16020 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5230 _reflns_number_gt 4770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Hydrogen atoms of the waters were located from different map and refined with restriants in bond length and thermal parameters. ; _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^)+(0.0326P)^2^+12.1783P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5230 _refine_ls_number_parameters 313 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0614 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.968749(11) 0.325366(6) 0.822464(6) 0.01549(5) Uani 1 1 d . . . P1 P 0.84831(8) 0.40702(4) 0.78353(4) 0.01541(16) Uani 1 1 d . . . N1 N 1.0843(3) 0.25079(14) 0.85765(13) 0.0184(6) Uani 1 1 d . . . O1 O 1.3676(2) 0.10527(12) 0.99102(12) 0.0248(5) Uani 1 1 d . . . O2 O 1.3923(2) 0.07198(12) 0.88988(12) 0.0225(5) Uani 1 1 d . . . H2 H 1.4475 0.0489 0.9070 0.034 Uiso 1 1 calc R . . C1 C 1.1046(3) 0.24295(17) 0.92105(17) 0.0204(7) Uani 1 1 d . . . H1 H 1.0633 0.2699 0.9487 0.024 Uiso 1 1 calc R . . C2 C 1.1857(3) 0.19552(18) 0.94636(17) 0.0202(7) Uani 1 1 d . . . H2A H 1.1965 0.1897 0.9905 0.024 Uiso 1 1 calc R . . C3 C 1.2504(3) 0.15688(16) 0.90512(17) 0.0184(7) Uani 1 1 d . . . C4 C 1.2275(3) 0.16469(17) 0.83935(17) 0.0206(7) Uani 1 1 d . . . H4 H 1.2680 0.1386 0.8106 0.025 Uiso 1 1 calc R . . C5 C 1.1432(3) 0.21197(17) 0.81766(17) 0.0226(7) Uani 1 1 d . . . H5 H 1.1267 0.2171 0.7737 0.027 Uiso 1 1 calc R . . C6 C 1.3431(3) 0.10813(16) 0.93320(17) 0.0195(7) Uani 1 1 d . . . C7 C 0.9424(3) 0.47601(17) 0.76068(16) 0.0194(6) Uani 1 1 d . . . H7 H 0.9050 0.5166 0.7644 0.023 Uiso 1 1 calc R . . C1A C 0.7472(3) 0.38267(18) 0.71488(16) 0.0202(7) Uani 1 1 d . . . C2A C 0.7435(4) 0.4159(2) 0.65724(18) 0.0289(8) Uani 1 1 d . . . H2A1 H 0.7960 0.4515 0.6521 0.035 Uiso 1 1 calc R . . C3A C 0.6605(4) 0.3956(2) 0.60704(19) 0.0382(10) Uani 1 1 d . . . H3A H 0.6576 0.4177 0.5682 0.046 Uiso 1 1 calc R . . C4A C 0.5830(4) 0.3432(3) 0.6144(2) 0.0415(11) Uani 1 1 d . . . H4A H 0.5276 0.3302 0.5806 0.050 Uiso 1 1 calc R . . C5A C 0.5869(4) 0.3096(2) 0.6718(2) 0.0394(11) Uani 1 1 d . . . H5A H 0.5345 0.2740 0.6766 0.047 Uiso 1 1 calc R . . C6A C 0.6687(4) 0.3292(2) 0.7220(2) 0.0305(9) Uani 1 1 d . . . H6A H 0.6716 0.3066 0.7606 0.037 Uiso 1 1 calc R . . C1B C 0.7425(3) 0.44270(17) 0.83801(17) 0.0190(7) Uani 1 1 d . . . C2B C 0.6532(3) 0.48789(18) 0.81351(18) 0.0233(7) Uani 1 1 d . . . H2B H 0.6468 0.4972 0.7699 0.028 Uiso 1 1 calc R . . C3B C 0.5747(3) 0.51854(19) 0.85445(19) 0.0274(8) Uani 1 1 d . . . H3B H 0.5157 0.5488 0.8385 0.033 Uiso 1 1 calc R . . C4B C 0.5843(4) 0.5039(2) 0.9193(2) 0.0325(9) Uani 1 1 d . . . H4B H 0.5317 0.5248 0.9468 0.039 Uiso 1 1 calc R . . C5B C 0.6702(4) 0.4590(2) 0.94364(19) 0.0307(9) Uani 1 1 d . . . H5B H 0.6746 0.4492 0.9872 0.037 Uiso 1 1 calc R . . C6B C 0.7507(3) 0.42800(19) 0.90310(17) 0.0232(7) Uani 1 1 d . . . H6B H 0.8093 0.3978 0.9195 0.028 Uiso 1 1 calc R . . S1 S 0.76164(9) 0.12772(5) 0.85676(5) 0.0305(2) Uani 1 1 d . . . O3 O 0.8728(3) 0.15190(16) 0.82886(14) 0.0345(6) Uani 1 1 d . . . O4 O 0.7818(3) 0.07147(15) 0.89718(16) 0.0439(8) Uani 1 1 d . . . O5 O 0.6515(3) 0.1233(2) 0.81402(17) 0.0661(12) Uani 1 1 d . . . C8 C 0.7244(4) 0.1904(2) 0.9138(2) 0.0296(8) Uani 1 1 d . . . F1 F 0.8193(2) 0.19895(15) 0.95791(13) 0.0468(7) Uani 1 1 d . . . F2 F 0.6229(3) 0.17561(13) 0.94486(15) 0.0468(7) Uani 1 1 d . . . F3 F 0.7030(3) 0.24727(14) 0.88529(16) 0.0563(8) Uani 1 1 d . . . O1W O 0.5721(3) 0.00220(16) 0.93266(16) 0.0364(7) Uani 1 1 d . . . H1W H 0.636(5) 0.025(3) 0.929(3) 0.055 Uiso 1 1 d . . . H2W H 0.580(6) -0.022(3) 0.955(3) 0.055 Uiso 1 1 d . . . O2W O 0.5000 0.1959(11) 0.7500 0.212(7) Uani 1 2 d SD . . H3W H 0.542(15) 0.169(6) 0.774(7) 0.200 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01356(7) 0.01496(8) 0.01774(8) 0.00188(4) -0.00082(5) 0.00176(4) P1 0.0123(4) 0.0171(4) 0.0169(4) 0.0014(3) 0.0014(3) 0.0020(3) N1 0.0171(13) 0.0173(14) 0.0203(14) 0.0003(11) -0.0017(10) 0.0015(11) O1 0.0276(13) 0.0251(13) 0.0213(13) 0.0039(10) -0.0020(10) 0.0081(11) O2 0.0213(13) 0.0224(13) 0.0235(13) 0.0002(10) -0.0014(10) 0.0087(10) C1 0.0223(17) 0.0170(16) 0.0219(17) -0.0022(13) 0.0017(13) 0.0021(13) C2 0.0224(17) 0.0210(17) 0.0169(16) 0.0016(13) -0.0026(13) 0.0034(14) C3 0.0167(16) 0.0146(15) 0.0235(17) 0.0021(13) -0.0004(13) 0.0006(13) C4 0.0243(18) 0.0167(16) 0.0209(17) -0.0012(13) 0.0022(14) 0.0047(13) C5 0.0259(18) 0.0229(18) 0.0185(17) 0.0000(14) -0.0023(13) 0.0023(14) C6 0.0162(16) 0.0151(16) 0.0271(18) 0.0011(13) 0.0000(13) 0.0000(12) C7 0.0216(16) 0.0156(15) 0.0213(16) 0.0020(13) 0.0028(13) 0.0031(13) C1A 0.0134(15) 0.0250(18) 0.0219(17) -0.0031(14) -0.0005(12) 0.0062(13) C2A 0.028(2) 0.036(2) 0.0225(18) 0.0011(16) -0.0006(15) 0.0070(16) C3A 0.036(2) 0.058(3) 0.0197(19) 0.0002(19) -0.0034(16) 0.013(2) C4A 0.020(2) 0.072(3) 0.032(2) -0.021(2) -0.0050(16) 0.013(2) C5A 0.021(2) 0.055(3) 0.043(3) -0.016(2) 0.0015(17) -0.0075(19) C6A 0.0210(19) 0.040(2) 0.030(2) 0.0006(17) -0.0022(15) -0.0063(16) C1B 0.0134(15) 0.0195(17) 0.0243(17) -0.0017(13) 0.0027(12) 0.0001(12) C2B 0.0185(17) 0.0256(19) 0.0259(18) -0.0002(14) 0.0017(13) 0.0037(14) C3B 0.0174(17) 0.0260(19) 0.040(2) -0.0064(16) 0.0067(15) 0.0009(14) C4B 0.0215(19) 0.035(2) 0.042(2) -0.0118(18) 0.0155(16) -0.0023(16) C5B 0.029(2) 0.039(2) 0.0258(19) -0.0023(17) 0.0118(15) -0.0062(17) C6B 0.0208(17) 0.0288(19) 0.0201(17) -0.0008(14) 0.0031(13) -0.0034(14) S1 0.0281(5) 0.0369(5) 0.0273(5) -0.0052(4) 0.0080(4) -0.0099(4) O3 0.0285(15) 0.0418(17) 0.0346(16) 0.0029(13) 0.0135(12) -0.0036(13) O4 0.057(2) 0.0254(16) 0.053(2) -0.0023(14) 0.0296(16) -0.0038(14) O5 0.0362(19) 0.117(4) 0.044(2) -0.022(2) -0.0037(15) -0.025(2) C8 0.0231(19) 0.028(2) 0.038(2) 0.0018(17) 0.0043(16) -0.0008(15) F1 0.0388(15) 0.0561(17) 0.0448(16) -0.0219(14) -0.0025(12) -0.0025(13) F2 0.0387(16) 0.0463(17) 0.0582(18) -0.0100(13) 0.0260(13) -0.0071(11) F3 0.0521(18) 0.0350(15) 0.084(2) 0.0185(15) 0.0183(15) 0.0160(13) O1W 0.0234(14) 0.0354(17) 0.051(2) 0.0244(14) 0.0085(13) 0.0107(12) O2W 0.229(19) 0.203(18) 0.195(17) 0.000 -0.065(13) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.071(3) . ? Au1 P1 2.2347(8) . ? Au1 Au1 3.1380(3) 2_756 ? P1 C1B 1.804(3) . ? P1 C1A 1.809(3) . ? P1 C7 1.817(3) . ? N1 C1 1.338(4) . ? N1 C5 1.338(4) . ? O1 C6 1.221(4) . ? O2 C6 1.305(4) . ? C1 C2 1.385(5) . ? C2 C3 1.386(5) . ? C3 C4 1.389(5) . ? C3 C6 1.500(4) . ? C4 C5 1.380(5) . ? C7 C7 1.329(7) 2_756 ? C1A C2A 1.383(5) . ? C1A C6A 1.394(5) . ? C2A C3A 1.392(6) . ? C3A C4A 1.370(7) . ? C4A C5A 1.382(7) . ? C5A C6A 1.380(6) . ? C1B C6B 1.390(5) . ? C1B C2B 1.403(5) . ? C2B C3B 1.383(5) . ? C3B C4B 1.385(6) . ? C4B C5B 1.375(6) . ? C5B C6B 1.394(5) . ? S1 O5 1.430(4) . ? S1 O3 1.438(3) . ? S1 O4 1.441(3) . ? S1 C8 1.815(4) . ? C8 F3 1.326(5) . ? C8 F2 1.328(5) . ? C8 F1 1.336(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Au1 P1 178.57(8) . . ? N1 Au1 Au1 100.74(8) . 2_756 ? P1 Au1 Au1 78.44(2) . 2_756 ? C1B P1 C1A 104.47(16) . . ? C1B P1 C7 102.82(16) . . ? C1A P1 C7 108.54(16) . . ? C1B P1 Au1 116.21(12) . . ? C1A P1 Au1 112.27(12) . . ? C7 P1 Au1 111.79(11) . . ? C1 N1 C5 119.5(3) . . ? C1 N1 Au1 119.8(2) . . ? C5 N1 Au1 120.7(2) . . ? N1 C1 C2 121.4(3) . . ? C1 C2 C3 119.2(3) . . ? C2 C3 C4 119.0(3) . . ? C2 C3 C6 118.7(3) . . ? C4 C3 C6 122.3(3) . . ? C5 C4 C3 118.5(3) . . ? N1 C5 C4 122.3(3) . . ? O1 C6 O2 126.0(3) . . ? O1 C6 C3 120.9(3) . . ? O2 C6 C3 113.1(3) . . ? C7 C7 P1 128.42(11) 2_756 . ? C2A C1A C6A 119.9(4) . . ? C2A C1A P1 122.4(3) . . ? C6A C1A P1 117.7(3) . . ? C1A C2A C3A 119.3(4) . . ? C4A C3A C2A 120.6(4) . . ? C3A C4A C5A 120.3(4) . . ? C6A C5A C4A 119.8(4) . . ? C5A C6A C1A 120.2(4) . . ? C6B C1B C2B 120.1(3) . . ? C6B C1B P1 121.6(3) . . ? C2B C1B P1 118.3(3) . . ? C3B C2B C1B 119.8(3) . . ? C2B C3B C4B 119.6(4) . . ? C5B C4B C3B 121.0(4) . . ? C4B C5B C6B 120.1(4) . . ? C1B C6B C5B 119.4(4) . . ? O5 S1 O3 115.5(2) . . ? O5 S1 O4 113.6(2) . . ? O3 S1 O4 114.78(19) . . ? O5 S1 C8 104.6(2) . . ? O3 S1 C8 103.75(19) . . ? O4 S1 C8 102.53(19) . . ? F3 C8 F2 107.4(3) . . ? F3 C8 F1 107.1(4) . . ? F2 C8 F1 107.1(4) . . ? F3 C8 S1 111.8(3) . . ? F2 C8 S1 112.0(3) . . ? F1 C8 S1 111.1(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1W 0.82 1.70 2.510(4) 171.9 1_655 O1W H1W O4 0.83(6) 1.97(6) 2.783(4) 165(5) . O1W H2W O1 0.69(6) 2.11(6) 2.778(4) 166(7) 5_757 O2W H3W O5 0.854(5) 1.68(5) 2.518(14) 167(18) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.049 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.129 # Attachment 'complex_5.cif' data_8475 _database_code_depnum_ccdc_archive 'CCDC 715604' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H54 Au4 Cl2 F6 N2 O10 P4 S2' _chemical_formula_weight 2207.89 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.6177(15) _cell_length_b 11.4930(5) _cell_length_c 35.2363(16) _cell_angle_alpha 90.00 _cell_angle_beta 92.2930(10) _cell_angle_gamma 90.00 _cell_volume 14007.9(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5200 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 26.69 _exptl_crystal_description ROD _exptl_crystal_colour COLOURLESS _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.094 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8368 _exptl_absorpt_coefficient_mu 8.654 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2119 _exptl_absorpt_correction_T_max 0.4782 _exptl_absorpt_process_details 'Sadabs, (Sheldrick 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48781 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16062 _reflns_number_gt 13087 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The dichloromethane was disordered into three positions with occupancy ratio 20:20:60. Restraints in bond length and distances were applied to the disordered solvent. ; _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^)+(0.0412P)^2^+156.7116P] 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 16062 _refine_ls_number_parameters 896 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1157 _refine_ls_wR_factor_gt 0.1111 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.157 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.611536(8) 0.20544(3) 0.248116(10) 0.02322(8) Uani 1 1 d . . . Au2 Au 0.618828(9) 0.07853(3) 0.323441(10) 0.02485(8) Uani 1 1 d . . . Au3 Au 0.495451(9) 0.47371(3) 0.139476(9) 0.02384(8) Uani 1 1 d . . . Au4 Au 0.574476(9) 0.59941(3) 0.137566(9) 0.02457(8) Uani 1 1 d . . . P1 P 0.65958(6) 0.31562(19) 0.27226(7) 0.0234(5) Uani 1 1 d . . . P2 P 0.68189(6) 0.08735(19) 0.33671(7) 0.0245(5) Uani 1 1 d . . . P3 P 0.52016(6) 0.38714(18) 0.08938(6) 0.0210(4) Uani 1 1 d . . . P4 P 0.57956(6) 0.63399(18) 0.07618(6) 0.0233(4) Uani 1 1 d . . . O1 O 0.43895(16) 0.0412(5) 0.18343(19) 0.0307(14) Uani 1 1 d . . . O2 O 0.45904(15) 0.2255(5) 0.19537(18) 0.0281(13) Uani 1 1 d . . . O3 O 0.44948(18) 0.4346(5) 0.28930(17) 0.0298(14) Uani 1 1 d . . . O4 O 0.42605(18) 0.6107(5) 0.30477(17) 0.0328(14) Uani 1 1 d . . . N1 N 0.56909(18) 0.1001(6) 0.22099(19) 0.0233(15) Uani 1 1 d . . . N2 N 0.46520(19) 0.5634(6) 0.1800(2) 0.0239(15) Uani 1 1 d . . . C1 C 0.4644(2) 0.1191(8) 0.1920(2) 0.0267(19) Uani 1 1 d . . . C2 C 0.5336(2) 0.1411(7) 0.2133(2) 0.0231(17) Uani 1 1 d . . . H2 H 0.5281 0.2202 0.2187 0.028 Uiso 1 1 calc R . . C3 C 0.5048(2) 0.0710(7) 0.1977(2) 0.0223(17) Uani 1 1 d . . . C4 C 0.5134(3) -0.0442(8) 0.1892(3) 0.036(2) Uani 1 1 d . . . H4 H 0.4941 -0.0949 0.1787 0.043 Uiso 1 1 calc R . . C5 C 0.5506(3) -0.0825(8) 0.1966(3) 0.038(2) Uani 1 1 d . . . H5 H 0.5575 -0.1597 0.1900 0.046 Uiso 1 1 calc R . . C6 C 0.5774(3) -0.0114(8) 0.2132(3) 0.036(2) Uani 1 1 d . . . H6 H 0.6025 -0.0407 0.2194 0.043 Uiso 1 1 calc R . . C7 C 0.7043(2) 0.2317(7) 0.2772(3) 0.0240(18) Uani 1 1 d . . . H7 H 0.7242 0.2524 0.2606 0.029 Uiso 1 1 calc R . . C8 C 0.7122(2) 0.1463(8) 0.3009(3) 0.0285(19) Uani 1 1 d . . . H8 H 0.7369 0.1112 0.2990 0.034 Uiso 1 1 calc R . . C9 C 0.4610(2) 0.5199(7) 0.2154(2) 0.0216(16) Uani 1 1 d . . . H9 H 0.4723 0.4469 0.2220 0.026 Uiso 1 1 calc R . . C10 C 0.4406(2) 0.5802(7) 0.2421(2) 0.0227(17) Uani 1 1 d . . . C11 C 0.4232(2) 0.6859(8) 0.2311(3) 0.0291(19) Uani 1 1 d . . . H11 H 0.4084 0.7281 0.2486 0.035 Uiso 1 1 calc R . . C12 C 0.4274(3) 0.7284(8) 0.1951(3) 0.036(2) Uani 1 1 d . . . H12 H 0.4157 0.7997 0.1873 0.044 Uiso 1 1 calc R . . C13 C 0.4492(3) 0.6647(8) 0.1704(3) 0.033(2) Uani 1 1 d . . . H13 H 0.4528 0.6946 0.1457 0.039 Uiso 1 1 calc R . . C14 C 0.4390(2) 0.5319(8) 0.2816(2) 0.0252(18) Uani 1 1 d . . . C15 C 0.5181(2) 0.4888(7) 0.0500(2) 0.0231(17) Uani 1 1 d . . . H15 H 0.4986 0.4752 0.0308 0.028 Uiso 1 1 calc R . . C16 C 0.5410(2) 0.5813(7) 0.0452(2) 0.0268(18) Uani 1 1 d . . . H16 H 0.5362 0.6243 0.0225 0.032 Uiso 1 1 calc R . . C1A C 0.6717(2) 0.4305(7) 0.2397(3) 0.0255(18) Uani 1 1 d . . . C2A C 0.6661(2) 0.5469(8) 0.2482(3) 0.034(2) Uani 1 1 d . . . H2A H 0.6571 0.5691 0.2723 0.041 Uiso 1 1 calc R . . C3A C 0.6739(3) 0.6306(9) 0.2212(3) 0.042(3) Uani 1 1 d . . . H3A H 0.6707 0.7107 0.2270 0.050 Uiso 1 1 calc R . . C4A C 0.6863(3) 0.5979(9) 0.1858(3) 0.040(2) Uani 1 1 d . . . H4A H 0.6912 0.6557 0.1673 0.048 Uiso 1 1 calc R . . C5A C 0.6917(3) 0.4817(9) 0.1773(3) 0.039(2) Uani 1 1 d . . . H5A H 0.7005 0.4597 0.1531 0.047 Uiso 1 1 calc R . . C6A C 0.6841(2) 0.3976(8) 0.2042(3) 0.030(2) Uani 1 1 d . . . H6A H 0.6875 0.3176 0.1984 0.036 Uiso 1 1 calc R . . C1B C 0.6527(2) 0.3816(7) 0.3180(3) 0.0260(18) Uani 1 1 d . . . C2B C 0.6833(2) 0.4354(8) 0.3374(3) 0.032(2) Uani 1 1 d . . . H2B H 0.7078 0.4391 0.3263 0.039 Uiso 1 1 calc R . . C3B C 0.6784(3) 0.4840(8) 0.3729(3) 0.038(2) Uani 1 1 d . . . H3B H 0.6995 0.5202 0.3862 0.045 Uiso 1 1 calc R . . C4B C 0.6427(3) 0.4795(8) 0.3888(3) 0.036(2) Uani 1 1 d . . . H4B H 0.6393 0.5121 0.4132 0.043 Uiso 1 1 calc R . . C5B C 0.6119(3) 0.4278(8) 0.3693(3) 0.034(2) Uani 1 1 d . . . H5B H 0.5873 0.4269 0.3803 0.041 Uiso 1 1 calc R . . C6B C 0.6162(2) 0.3771(8) 0.3339(3) 0.030(2) Uani 1 1 d . . . H6B H 0.5950 0.3405 0.3208 0.036 Uiso 1 1 calc R . . C1C C 0.7028(2) -0.0569(7) 0.3435(3) 0.0282(19) Uani 1 1 d . . . C2C C 0.7167(3) -0.0946(9) 0.3786(3) 0.040(2) Uani 1 1 d . . . H2C H 0.7144 -0.0466 0.4003 0.048 Uiso 1 1 calc R . . C3C C 0.7342(3) -0.2029(10) 0.3820(3) 0.048(3) Uani 1 1 d . . . H3C H 0.7439 -0.2286 0.4062 0.058 Uiso 1 1 calc R . . C4C C 0.7375(3) -0.2724(9) 0.3513(3) 0.045(3) Uani 1 1 d . . . H4C H 0.7499 -0.3458 0.3540 0.054 Uiso 1 1 calc R . . C5C C 0.7229(3) -0.2374(8) 0.3162(3) 0.039(2) Uani 1 1 d . . . H5C H 0.7247 -0.2874 0.2949 0.047 Uiso 1 1 calc R . . C6C C 0.7052(3) -0.1259(8) 0.3120(3) 0.034(2) Uani 1 1 d . . . H6C H 0.6953 -0.1002 0.2880 0.040 Uiso 1 1 calc R . . C1D C 0.6944(3) 0.1665(8) 0.3795(3) 0.031(2) Uani 1 1 d . . . C2D C 0.6678(3) 0.1752(10) 0.4083(3) 0.046(3) Uani 1 1 d . . . H2D H 0.6428 0.1424 0.4049 0.055 Uiso 1 1 calc R . . C3D C 0.6784(4) 0.2321(11) 0.4419(3) 0.053(3) Uani 1 1 d . . . H3D H 0.6600 0.2404 0.4610 0.064 Uiso 1 1 calc R . . C4D C 0.7149(3) 0.2764(11) 0.4478(3) 0.058(3) Uani 1 1 d . . . H4D H 0.7222 0.3097 0.4717 0.069 Uiso 1 1 calc R . . C5D C 0.7412(3) 0.2729(10) 0.4189(4) 0.053(3) Uani 1 1 d . . . H5D H 0.7657 0.3091 0.4222 0.063 Uiso 1 1 calc R . . C6D C 0.7309(3) 0.2155(9) 0.3852(3) 0.042(3) Uani 1 1 d . . . H6D H 0.7491 0.2098 0.3658 0.050 Uiso 1 1 calc R . . C1E C 0.4919(2) 0.2687(7) 0.0718(3) 0.0262(18) Uani 1 1 d . . . C2E C 0.4965(2) 0.2224(7) 0.0350(3) 0.0260(18) Uani 1 1 d . . . H2E H 0.5147 0.2575 0.0191 0.031 Uiso 1 1 calc R . . C3E C 0.4756(3) 0.1286(7) 0.0216(3) 0.030(2) Uani 1 1 d . . . H3E H 0.4778 0.1037 -0.0039 0.036 Uiso 1 1 calc R . . C4E C 0.4511(3) 0.0702(8) 0.0455(3) 0.039(2) Uani 1 1 d . . . H4E H 0.4374 0.0032 0.0368 0.047 Uiso 1 1 calc R . . C5E C 0.4469(3) 0.1107(9) 0.0823(3) 0.037(2) Uani 1 1 d . . . H5E H 0.4304 0.0706 0.0988 0.045 Uiso 1 1 calc R . . C6E C 0.4665(3) 0.2086(8) 0.0950(3) 0.032(2) Uani 1 1 d . . . H6E H 0.4628 0.2361 0.1200 0.039 Uiso 1 1 calc R . . C1F C 0.5693(2) 0.3369(7) 0.0955(2) 0.0228(17) Uani 1 1 d . . . C2F C 0.5824(2) 0.3062(7) 0.1323(3) 0.0249(18) Uani 1 1 d . . . H2F H 0.5663 0.3149 0.1533 0.030 Uiso 1 1 calc R . . C3F C 0.6201(3) 0.2623(8) 0.1372(3) 0.035(2) Uani 1 1 d . . . H3F H 0.6295 0.2398 0.1618 0.043 Uiso 1 1 calc R . . C4F C 0.6438(3) 0.2513(8) 0.1066(3) 0.039(2) Uani 1 1 d . . . H4F H 0.6695 0.2236 0.1106 0.047 Uiso 1 1 calc R . . C5F C 0.6305(3) 0.2800(7) 0.0711(3) 0.035(2) Uani 1 1 d . . . H5F H 0.6469 0.2715 0.0503 0.042 Uiso 1 1 calc R . . C6F C 0.5927(2) 0.3222(7) 0.0649(3) 0.0283(19) Uani 1 1 d . . . H6F H 0.5833 0.3406 0.0399 0.034 Uiso 1 1 calc R . . C1G C 0.5778(3) 0.7908(7) 0.0686(3) 0.0283(19) Uani 1 1 d . . . C2G C 0.6046(3) 0.8472(9) 0.0473(3) 0.047(3) Uani 1 1 d . . . H2G H 0.6250 0.8058 0.0361 0.056 Uiso 1 1 calc R . . C3G C 0.6007(3) 0.9660(10) 0.0428(5) 0.066(4) Uani 1 1 d . . . H3G H 0.6190 1.0060 0.0283 0.080 Uiso 1 1 calc R . . C4G C 0.5718(4) 1.0285(10) 0.0583(4) 0.064(4) Uani 1 1 d . . . H4G H 0.5696 1.1099 0.0541 0.077 Uiso 1 1 calc R . . C5G C 0.5464(3) 0.9717(9) 0.0799(3) 0.049(3) Uani 1 1 d . . . H5G H 0.5267 1.0145 0.0916 0.059 Uiso 1 1 calc R . . C6G C 0.5485(3) 0.8520(8) 0.0851(3) 0.039(2) Uani 1 1 d . . . H6G H 0.5301 0.8129 0.0998 0.047 Uiso 1 1 calc R . . C1H C 0.6239(3) 0.5847(7) 0.0561(2) 0.0268(18) Uani 1 1 d . . . C2H C 0.6264(3) 0.5527(9) 0.0182(3) 0.038(2) Uani 1 1 d . . . H2H H 0.6042 0.5577 0.0015 0.045 Uiso 1 1 calc R . . C3H C 0.6605(3) 0.5141(10) 0.0048(3) 0.049(3) Uani 1 1 d . . . H3H H 0.6619 0.4922 -0.0211 0.059 Uiso 1 1 calc R . . C4H C 0.6929(3) 0.5068(10) 0.0285(4) 0.053(3) Uani 1 1 d . . . H4H H 0.7165 0.4789 0.0191 0.063 Uiso 1 1 calc R . . C5H C 0.6913(3) 0.5392(10) 0.0654(4) 0.047(3) Uani 1 1 d . . . H5H H 0.7139 0.5359 0.0815 0.056 Uiso 1 1 calc R . . C6H C 0.6568(3) 0.5770(8) 0.0796(3) 0.035(2) Uani 1 1 d . . . H6H H 0.6557 0.5978 0.1056 0.043 Uiso 1 1 calc R . . S1 S 0.30925(7) 0.9804(2) 0.30643(8) 0.0408(6) Uani 1 1 d . . . O5 O 0.3118(3) 1.1041(7) 0.3073(3) 0.070(3) Uani 1 1 d . . . O6 O 0.33335(19) 0.9266(6) 0.2797(2) 0.0445(18) Uani 1 1 d . . . O7 O 0.2731(3) 0.9282(12) 0.3085(3) 0.115(5) Uani 1 1 d . . . C17 C 0.3329(6) 0.9417(11) 0.3525(4) 0.079(5) Uani 1 1 d . . . F1 F 0.3673(3) 0.9840(7) 0.3565(2) 0.081(2) Uani 1 1 d . . . F2 F 0.3126(3) 0.9891(8) 0.3807(3) 0.109(4) Uani 1 1 d . . . F3 F 0.3353(5) 0.8298(7) 0.3575(3) 0.177(7) Uani 1 1 d . . . S2 S 0.42807(8) 0.7198(2) 0.05819(8) 0.0448(6) Uani 1 1 d . . . O8 O 0.4568(2) 0.7686(8) 0.0850(2) 0.062(2) Uani 1 1 d . . . O9 O 0.4305(3) 0.7696(8) 0.0215(2) 0.070(3) Uani 1 1 d . . . O10 O 0.4242(2) 0.5980(7) 0.0609(3) 0.074(3) Uani 1 1 d . . . C18 C 0.3837(3) 0.7771(9) 0.0761(4) 0.048(3) Uani 1 1 d . . . F4 F 0.3806(2) 0.8934(6) 0.0721(2) 0.067(2) Uani 1 1 d . . . F5 F 0.37779(19) 0.7516(6) 0.1113(2) 0.0571(18) Uani 1 1 d . . . F6 F 0.3529(2) 0.7322(6) 0.0557(2) 0.072(2) Uani 1 1 d . . . C2S C 0.7046(10) 1.008(2) 0.5271(10) 0.129(13) Uani 0.592(9) 1 d PDU A 1 H2S1 H 0.6840 1.0230 0.5452 0.155 Uiso 0.592(9) 1 calc PR A 1 H2S2 H 0.7158 1.0827 0.5189 0.155 Uiso 0.592(9) 1 calc PR A 1 Cl3 Cl 0.7408(7) 0.910(3) 0.5462(7) 0.328(10) Uani 0.592(9) 1 d PDU A 1 Cl4 Cl 0.6877(7) 0.922(2) 0.4878(7) 0.328(10) Uani 0.592(9) 1 d PDU A 1 C1S C 0.7007(13) 0.908(2) 0.5262(11) 0.110(15) Uani 0.408(9) 1 d PDU A 2 H1S1 H 0.7114 0.9268 0.5519 0.132 Uiso 0.408(9) 1 calc PR A 2 H1S2 H 0.6740 0.8791 0.5287 0.132 Uiso 0.408(9) 1 calc PR A 2 Cl1A Cl 0.7279(5) 0.8014(14) 0.5069(8) 0.216(14) Uani 0.408(9) 1 d PD . 2 Cl2A Cl 0.6997(3) 1.0374(11) 0.4976(5) 0.115(6) Uani 0.408(9) 1 d PD A 2 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 0.01550(14) 0.02611(16) 0.02795(17) 0.00177(13) -0.00034(13) -0.00146(12) Au2 0.01572(14) 0.02869(17) 0.03009(18) 0.00356(14) 0.00031(13) 0.00146(12) Au3 0.02239(16) 0.02656(17) 0.02263(16) -0.00239(13) 0.00179(13) -0.00018(12) Au4 0.02780(17) 0.02402(16) 0.02180(16) 0.00012(13) -0.00016(13) -0.00399(12) P1 0.0156(9) 0.0224(10) 0.0322(12) 0.0032(9) -0.0003(9) -0.0013(8) P2 0.0189(10) 0.0263(11) 0.0282(12) 0.0004(9) -0.0007(9) 0.0025(8) P3 0.0223(10) 0.0193(10) 0.0210(10) -0.0004(8) -0.0014(9) -0.0015(8) P4 0.0291(11) 0.0173(10) 0.0233(11) 0.0012(8) -0.0015(9) -0.0031(8) O1 0.017(3) 0.031(3) 0.044(4) -0.012(3) -0.001(3) 0.001(2) O2 0.016(3) 0.029(3) 0.039(4) 0.001(3) -0.001(3) 0.004(2) O3 0.034(3) 0.028(3) 0.027(3) 0.004(3) 0.001(3) 0.003(3) O4 0.039(4) 0.038(4) 0.021(3) 0.003(3) -0.001(3) 0.009(3) N1 0.017(3) 0.033(4) 0.021(4) 0.001(3) 0.005(3) -0.004(3) N2 0.023(3) 0.021(3) 0.027(4) -0.005(3) 0.001(3) -0.003(3) C1 0.016(4) 0.040(5) 0.024(4) 0.005(4) 0.003(3) 0.004(3) C2 0.026(4) 0.022(4) 0.023(4) 0.005(3) 0.010(4) 0.002(3) C3 0.016(4) 0.030(4) 0.021(4) -0.006(3) 0.002(3) 0.003(3) C4 0.027(5) 0.033(5) 0.046(6) -0.017(4) -0.004(4) -0.002(4) C5 0.035(5) 0.026(5) 0.052(6) -0.012(4) -0.007(5) 0.014(4) C6 0.028(5) 0.030(5) 0.048(6) -0.006(4) -0.006(4) 0.003(4) C7 0.011(3) 0.029(4) 0.031(5) -0.002(4) -0.003(3) 0.001(3) C8 0.014(4) 0.033(5) 0.038(5) -0.003(4) 0.004(4) -0.002(3) C9 0.017(4) 0.022(4) 0.025(4) 0.002(3) -0.003(3) 0.003(3) C10 0.018(4) 0.027(4) 0.023(4) -0.002(3) -0.002(3) 0.003(3) C11 0.027(4) 0.028(5) 0.033(5) -0.004(4) 0.001(4) 0.008(4) C12 0.050(6) 0.031(5) 0.028(5) -0.001(4) 0.001(5) 0.017(4) C13 0.035(5) 0.029(5) 0.033(5) -0.001(4) 0.002(4) 0.003(4) C14 0.019(4) 0.032(5) 0.024(4) -0.001(4) 0.001(3) 0.004(3) C15 0.027(4) 0.018(4) 0.023(4) 0.001(3) -0.005(4) 0.004(3) C16 0.033(5) 0.024(4) 0.023(4) 0.011(4) -0.008(4) -0.001(3) C1A 0.018(4) 0.025(4) 0.034(5) 0.009(4) -0.006(4) -0.001(3) C2A 0.017(4) 0.033(5) 0.053(6) 0.004(4) 0.001(4) 0.003(3) C3A 0.027(5) 0.030(5) 0.067(8) 0.012(5) -0.004(5) 0.003(4) C4A 0.028(5) 0.044(6) 0.048(6) 0.018(5) 0.000(5) -0.002(4) C5A 0.029(5) 0.054(6) 0.034(5) 0.010(5) 0.000(4) -0.004(4) C6A 0.027(4) 0.033(5) 0.031(5) 0.004(4) -0.006(4) -0.002(4) C1B 0.022(4) 0.020(4) 0.035(5) -0.001(4) -0.001(4) -0.002(3) C2B 0.021(4) 0.029(5) 0.048(6) 0.001(4) 0.004(4) 0.001(3) C3B 0.032(5) 0.028(5) 0.052(6) -0.005(5) -0.009(5) 0.000(4) C4B 0.036(5) 0.027(5) 0.044(6) -0.008(4) -0.006(5) 0.007(4) C5B 0.022(4) 0.032(5) 0.049(6) 0.002(4) 0.007(4) 0.004(4) C6B 0.024(4) 0.037(5) 0.030(5) 0.002(4) -0.001(4) 0.001(4) C1C 0.016(4) 0.028(4) 0.041(5) -0.001(4) 0.004(4) 0.001(3) C2C 0.037(5) 0.039(6) 0.044(6) 0.001(5) -0.006(5) -0.001(4) C3C 0.040(6) 0.050(7) 0.055(7) 0.021(6) -0.007(5) 0.009(5) C4C 0.034(5) 0.035(6) 0.065(8) 0.009(5) 0.003(5) 0.001(4) C5C 0.038(5) 0.026(5) 0.054(7) -0.007(5) 0.013(5) -0.005(4) C6C 0.033(5) 0.029(5) 0.039(5) 0.007(4) 0.007(4) -0.009(4) C1D 0.031(5) 0.035(5) 0.028(5) 0.002(4) 0.002(4) 0.004(4) C2D 0.035(5) 0.063(7) 0.039(6) -0.009(5) 0.001(5) -0.001(5) C3D 0.055(7) 0.075(8) 0.028(5) -0.013(6) -0.003(5) -0.003(6) C4D 0.049(7) 0.073(8) 0.049(7) -0.027(6) -0.026(6) 0.017(6) C5D 0.046(6) 0.048(7) 0.065(8) -0.005(6) -0.001(6) -0.012(5) C6D 0.036(5) 0.044(6) 0.045(6) -0.026(5) -0.003(5) 0.004(4) C1E 0.027(4) 0.024(4) 0.028(5) -0.008(4) -0.001(4) -0.003(3) C2E 0.027(4) 0.023(4) 0.029(5) 0.006(4) 0.004(4) 0.002(3) C3E 0.041(5) 0.023(4) 0.026(5) 0.001(4) 0.006(4) -0.001(4) C4E 0.042(6) 0.028(5) 0.046(6) 0.003(4) -0.005(5) -0.016(4) C5E 0.032(5) 0.045(6) 0.036(5) 0.000(5) 0.006(4) -0.012(4) C6E 0.032(5) 0.034(5) 0.031(5) -0.001(4) 0.009(4) -0.002(4) C1F 0.021(4) 0.018(4) 0.029(5) -0.001(3) 0.004(4) 0.000(3) C2F 0.027(4) 0.014(4) 0.033(5) 0.003(3) -0.004(4) -0.001(3) C3F 0.031(5) 0.030(5) 0.044(6) 0.002(4) -0.013(5) -0.002(4) C4F 0.025(4) 0.023(4) 0.069(8) 0.008(5) -0.005(5) 0.001(4) C5F 0.028(5) 0.023(4) 0.055(6) 0.003(4) 0.014(5) -0.004(4) C6F 0.032(5) 0.015(4) 0.038(5) -0.001(4) 0.002(4) 0.000(3) C1G 0.037(5) 0.020(4) 0.026(4) 0.001(4) -0.014(4) -0.005(4) C2G 0.052(6) 0.031(5) 0.057(7) 0.012(5) -0.009(6) -0.003(5) C3G 0.043(6) 0.032(6) 0.122(13) 0.018(7) -0.012(7) -0.011(5) C4G 0.065(8) 0.031(6) 0.093(10) 0.013(6) -0.033(8) -0.017(6) C5G 0.062(7) 0.038(6) 0.046(6) -0.008(5) -0.021(6) 0.024(5) C6G 0.052(6) 0.032(5) 0.032(5) -0.005(4) -0.008(5) 0.009(4) C1H 0.032(4) 0.023(4) 0.026(4) 0.005(4) 0.002(4) -0.004(3) C2H 0.042(6) 0.041(5) 0.030(5) 0.011(4) 0.002(5) -0.003(4) C3H 0.053(7) 0.059(7) 0.037(6) -0.007(5) 0.025(6) -0.001(5) C4H 0.044(6) 0.057(7) 0.059(8) 0.009(6) 0.022(6) 0.007(5) C5H 0.025(5) 0.052(7) 0.064(8) 0.012(6) 0.000(5) -0.005(4) C6H 0.035(5) 0.030(5) 0.041(6) -0.004(4) 0.002(5) -0.004(4) S1 0.0255(11) 0.0410(14) 0.0564(17) -0.0080(12) 0.0068(12) -0.0026(10) O5 0.104(7) 0.044(5) 0.060(6) -0.007(4) -0.013(5) 0.028(5) O6 0.029(3) 0.054(4) 0.051(5) -0.015(4) 0.001(3) 0.000(3) O7 0.044(5) 0.200(13) 0.103(9) -0.063(9) 0.029(6) -0.057(7) C17 0.148(16) 0.042(7) 0.048(8) -0.001(6) -0.001(10) -0.038(9) F1 0.084(6) 0.077(5) 0.079(6) -0.030(5) -0.033(5) 0.019(5) F2 0.166(10) 0.101(7) 0.063(5) -0.016(5) 0.036(6) -0.060(7) F3 0.39(2) 0.032(4) 0.101(8) 0.009(5) -0.116(11) -0.019(8) S2 0.0503(16) 0.0465(15) 0.0386(14) 0.0035(12) 0.0157(13) -0.0090(12) O8 0.046(4) 0.083(6) 0.057(5) 0.009(5) 0.002(4) -0.019(4) O9 0.090(7) 0.080(6) 0.042(5) 0.006(5) 0.015(5) -0.024(5) O10 0.056(5) 0.054(5) 0.117(9) 0.012(5) 0.047(6) 0.014(4) C18 0.044(6) 0.041(6) 0.060(8) -0.004(5) 0.011(6) -0.005(5) F4 0.064(4) 0.041(4) 0.095(6) 0.007(4) 0.005(4) -0.007(3) F5 0.057(4) 0.062(4) 0.055(4) 0.001(3) 0.026(4) -0.010(3) F6 0.056(4) 0.062(5) 0.098(6) 0.001(4) -0.013(4) -0.007(4) C2S 0.13(2) 0.118(19) 0.14(2) -0.012(17) -0.013(17) -0.020(16) Cl3 0.344(17) 0.339(18) 0.303(16) 0.081(14) 0.043(13) 0.025(15) Cl4 0.344(17) 0.339(18) 0.303(16) 0.081(14) 0.043(13) 0.025(15) C1S 0.12(2) 0.10(2) 0.11(2) 0.024(17) -0.004(17) -0.030(17) Cl1A 0.124(12) 0.115(12) 0.41(4) 0.121(18) -0.040(17) -0.026(9) Cl2A 0.053(5) 0.111(9) 0.182(14) 0.089(9) 0.021(7) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 N1 2.104(7) . ? Au1 P1 2.232(2) . ? Au1 Au2 3.0302(5) . ? Au2 O1 2.051(6) 2_655 ? Au2 P2 2.217(2) . ? Au3 N2 2.078(7) . ? Au3 P3 2.227(2) . ? Au3 Au4 3.0968(5) . ? Au4 O4 2.037(6) 2_655 ? Au4 P4 2.213(2) . ? P1 C1B 1.807(9) . ? P1 C1A 1.808(8) . ? P1 C7 1.826(8) . ? P2 C1D 1.800(10) . ? P2 C8 1.805(9) . ? P2 C1C 1.820(9) . ? P3 C1E 1.773(8) . ? P3 C1F 1.800(8) . ? P3 C15 1.812(8) . ? P4 C16 1.798(9) . ? P4 C1H 1.805(9) . ? P4 C1G 1.822(9) . ? O1 C1 1.284(10) . ? O1 Au2 2.051(6) 2_655 ? O2 C1 1.244(10) . ? O3 C14 1.203(10) . ? O4 C14 1.311(10) . ? O4 Au4 2.037(6) 2_655 ? N1 C2 1.332(10) . ? N1 C6 1.344(11) . ? N2 C13 1.328(11) . ? N2 C9 1.357(11) . ? C1 C3 1.508(11) . ? C2 C3 1.380(11) . ? C3 C4 1.392(12) . ? C4 C5 1.375(13) . ? C5 C6 1.352(13) . ? C7 C8 1.311(12) . ? C9 C10 1.384(11) . ? C10 C11 1.404(11) . ? C10 C14 1.504(12) . ? C11 C12 1.371(13) . ? C12 C13 1.383(12) . ? C15 C16 1.340(11) . ? C1A C2A 1.386(12) . ? C1A C6A 1.393(13) . ? C2A C3A 1.386(14) . ? C3A C4A 1.388(15) . ? C4A C5A 1.383(14) . ? C5A C6A 1.386(13) . ? C1B C2B 1.383(12) . ? C1B C6B 1.404(12) . ? C2B C3B 1.387(14) . ? C3B C4B 1.378(13) . ? C4B C5B 1.379(13) . ? C5B C6B 1.391(13) . ? C1C C6C 1.367(13) . ? C1C C2C 1.380(14) . ? C2C C3C 1.387(14) . ? C3C C4C 1.353(16) . ? C4C C5C 1.375(15) . ? C5C C6C 1.425(13) . ? C1D C6D 1.391(13) . ? C1D C2D 1.400(13) . ? C2D C3D 1.385(15) . ? C3D C4D 1.371(16) . ? C4D C5D 1.392(17) . ? C5D C6D 1.393(15) . ? C1E C6E 1.406(12) . ? C1E C2E 1.416(12) . ? C2E C3E 1.373(12) . ? C3E C4E 1.392(12) . ? C4E C5E 1.390(14) . ? C5E C6E 1.380(13) . ? C1F C6F 1.387(12) . ? C1F C2F 1.404(12) . ? C2F C3F 1.403(12) . ? C3F C4F 1.386(14) . ? C4F C5F 1.358(15) . ? C5F C6F 1.404(12) . ? C1G C2G 1.378(14) . ? C1G C6G 1.380(13) . ? C2G C3G 1.380(15) . ? C3G C4G 1.363(18) . ? C4G C5G 1.353(17) . ? C5G C6G 1.390(14) . ? C1H C6H 1.384(13) . ? C1H C2H 1.394(13) . ? C2H C3H 1.362(14) . ? C3H C4H 1.375(17) . ? C4H C5H 1.353(17) . ? C5H C6H 1.385(14) . ? S1 O7 1.393(9) . ? S1 O6 1.423(7) . ? S1 O5 1.425(8) . ? S1 C17 1.843(16) . ? C17 F1 1.289(18) . ? C17 F3 1.301(15) . ? C17 F2 1.354(17) . ? S2 O10 1.409(9) . ? S2 O9 1.418(9) . ? S2 O8 1.457(9) . ? S2 C18 1.807(11) . ? C18 F5 1.302(13) . ? C18 F4 1.348(12) . ? C18 F6 1.363(13) . ? C2S Cl4 1.784(19) . ? C2S Cl3 1.797(19) . ? C1S Cl1A 1.702(19) . ? C1S Cl2A 1.797(19) . ? Cl1A Cl1A 2.01(4) 7_666 ? 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 N1 Au1 P1 174.92(18) . . ? N1 Au1 Au2 98.80(19) . . ? P1 Au1 Au2 84.52(6) . . ? O1 Au2 P2 169.21(17) 2_655 . ? O1 Au2 Au1 87.16(17) 2_655 . ? P2 Au2 Au1 102.10(6) . . ? N2 Au3 P3 170.6(2) . . ? N2 Au3 Au4 104.68(18) . . ? P3 Au3 Au4 79.83(5) . . ? O4 Au4 P4 165.40(18) 2_655 . ? O4 Au4 Au3 87.99(17) 2_655 . ? P4 Au4 Au3 102.12(6) . . ? C1B P1 C1A 107.6(4) . . ? C1B P1 C7 106.2(4) . . ? C1A P1 C7 103.2(4) . . ? C1B P1 Au1 117.1(3) . . ? C1A P1 Au1 111.1(3) . . ? C7 P1 Au1 110.7(3) . . ? C1D P2 C8 105.6(4) . . ? C1D P2 C1C 105.7(4) . . ? C8 P2 C1C 101.2(4) . . ? C1D P2 Au2 113.7(3) . . ? C8 P2 Au2 117.7(3) . . ? C1C P2 Au2 111.6(3) . . ? C1E P3 C1F 107.5(4) . . ? C1E P3 C15 102.9(4) . . ? C1F P3 C15 107.9(4) . . ? C1E P3 Au3 113.4(3) . . ? C1F P3 Au3 116.1(3) . . ? C15 P3 Au3 108.2(3) . . ? C16 P4 C1H 106.2(4) . . ? C16 P4 C1G 103.0(4) . . ? C1H P4 C1G 106.1(4) . . ? C16 P4 Au4 116.6(3) . . ? C1H P4 Au4 115.4(3) . . ? C1G P4 Au4 108.5(3) . . ? C1 O1 Au2 122.7(5) . 2_655 ? C14 O4 Au4 126.4(5) . 2_655 ? C2 N1 C6 119.9(7) . . ? C2 N1 Au1 120.6(6) . . ? C6 N1 Au1 119.4(6) . . ? C13 N2 C9 119.9(7) . . ? C13 N2 Au3 118.5(6) . . ? C9 N2 Au3 121.6(5) . . ? O2 C1 O1 127.1(8) . . ? O2 C1 C3 119.3(8) . . ? O1 C1 C3 113.6(7) . . ? N1 C2 C3 121.4(8) . . ? C2 C3 C4 118.9(8) . . ? C2 C3 C1 119.4(7) . . ? C4 C3 C1 121.7(8) . . ? C5 C4 C3 118.1(8) . . ? C6 C5 C4 120.7(8) . . ? N1 C6 C5 121.0(8) . . ? C8 C7 P1 127.6(7) . . ? C7 C8 P2 127.9(7) . . ? N2 C9 C10 121.0(7) . . ? C9 C10 C11 118.2(8) . . ? C9 C10 C14 118.9(7) . . ? C11 C10 C14 122.9(7) . . ? C12 C11 C10 120.1(8) . . ? C11 C12 C13 118.3(8) . . ? N2 C13 C12 122.4(9) . . ? O3 C14 O4 127.6(8) . . ? O3 C14 C10 122.0(8) . . ? O4 C14 C10 110.4(7) . . ? C16 C15 P3 127.1(7) . . ? C15 C16 P4 128.2(7) . . ? C2A C1A C6A 120.4(8) . . ? C2A C1A P1 122.0(7) . . ? C6A C1A P1 117.4(7) . . ? C3A C2A C1A 119.3(10) . . ? C2A C3A C4A 120.2(10) . . ? C5A C4A C3A 120.4(9) . . ? C4A C5A C6A 119.6(10) . . ? C5A C6A C1A 120.0(9) . . ? C2B C1B C6B 120.3(9) . . ? C2B C1B P1 120.1(7) . . ? C6B C1B P1 119.5(7) . . ? C1B C2B C3B 120.3(8) . . ? C4B C3B C2B 119.8(9) . . ? C3B C4B C5B 120.2(9) . . ? C4B C5B C6B 121.2(9) . . ? C5B C6B C1B 118.2(9) . . ? C6C C1C C2C 120.8(9) . . ? C6C C1C P2 117.4(8) . . ? C2C C1C P2 121.7(7) . . ? C1C C2C C3C 119.7(10) . . ? C4C C3C C2C 120.7(11) . . ? C3C C4C C5C 120.4(10) . . ? C4C C5C C6C 119.7(10) . . ? C1C C6C C5C 118.6(10) . . ? C6D C1D C2D 119.1(9) . . ? C6D C1D P2 120.8(7) . . ? C2D C1D P2 120.1(7) . . ? C3D C2D C1D 119.6(10) . . ? C4D C3D C2D 120.9(11) . . ? C3D C4D C5D 120.3(11) . . ? C4D C5D C6D 119.0(10) . . ? C1D C6D C5D 120.9(10) . . ? C6E C1E C2E 116.4(8) . . ? C6E C1E P3 121.5(7) . . ? C2E C1E P3 121.8(7) . . ? C3E C2E C1E 122.2(8) . . ? C2E C3E C4E 119.8(9) . . ? C5E C4E C3E 119.5(9) . . ? C6E C5E C4E 120.5(9) . . ? C5E C6E C1E 121.5(9) . . ? C6F C1F C2F 120.7(8) . . ? C6F C1F P3 121.7(7) . . ? C2F C1F P3 117.4(6) . . ? C3F C2F C1F 117.9(8) . . ? C4F C3F C2F 121.1(9) . . ? C5F C4F C3F 120.3(9) . . ? C4F C5F C6F 120.5(9) . . ? C1F C6F C5F 119.4(9) . . ? C2G C1G C6G 120.7(9) . . ? C2G C1G P4 121.7(8) . . ? C6G C1G P4 117.6(7) . . ? C1G C2G C3G 117.6(11) . . ? C4G C3G C2G 123.0(12) . . ? C5G C4G C3G 118.3(11) . . ? C4G C5G C6G 121.3(11) . . ? C1G C6G C5G 119.0(10) . . ? C6H C1H C2H 118.4(9) . . ? C6H C1H P4 118.5(7) . . ? C2H C1H P4 123.1(7) . . ? C3H C2H C1H 120.4(10) . . ? C2H C3H C4H 120.4(10) . . ? C5H C4H C3H 120.2(10) . . ? C4H C5H C6H 120.2(11) . . ? C1H C6H C5H 120.3(10) . . ? O7 S1 O6 113.5(6) . . ? O7 S1 O5 118.8(7) . . ? O6 S1 O5 114.3(5) . . ? O7 S1 C17 102.7(8) . . ? O6 S1 C17 103.0(7) . . ? O5 S1 C17 101.4(6) . . ? F1 C17 F3 107.7(17) . . ? F1 C17 F2 105.8(11) . . ? F3 C17 F2 109.3(13) . . ? F1 C17 S1 112.4(10) . . ? F3 C17 S1 112.5(10) . . ? F2 C17 S1 108.9(13) . . ? O10 S2 O9 118.2(6) . . ? O10 S2 O8 113.8(6) . . ? O9 S2 O8 111.8(5) . . ? O10 S2 C18 104.8(5) . . ? O9 S2 C18 104.6(6) . . ? O8 S2 C18 101.6(5) . . ? F5 C18 F4 107.8(9) . . ? F5 C18 F6 105.5(9) . . ? F4 C18 F6 105.2(10) . . ? F5 C18 S2 114.8(9) . . ? F4 C18 S2 113.1(8) . . ? F6 C18 S2 109.6(8) . . ? Cl4 C2S Cl3 98.3(12) . . ? Cl1A C1S Cl2A 111.8(16) . . ? C1S Cl1A Cl1A 163(3) . 7_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.162 _refine_diff_density_min -1.528 _refine_diff_density_rms 0.219