Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global loop_ _publ_author_name 'Mitzel, Norbert W' 'Schier, Annette' 'Schmidbaur, Hubert' 'Wilton-Ely, James D.E.T.' _journal_coden_Cambridge 186 _publ_contact_author ;Prof Hubert Schmidbaur Anorganisch-chemisches Institut der Technischen Universitat Munchen Lichtenbergstrasse 4 D-85747 Garching GERMANY ; data_jam9 _database_code_CSD 155654 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H20 Au Cl3 N O2 P S' _chemical_formula_weight 732.77 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.3563(1) _cell_length_b 17.4820(3) _cell_length_c 19.2000(3) _cell_angle_alpha 104.530(1) _cell_angle_beta 90.423(1) _cell_angle_gamma 102.696(1) _cell_volume 2642.92(7) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour plate _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 6.033 _exptl_absorpt_correction_type DELABS _exptl_absorpt_correction_T_min 0.2648 _exptl_absorpt_correction_T_max 0.5837 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'NONIUS DIP2020H' _diffrn_measurement_method phi-rotation _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59270 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 31.67 _reflns_number_total 15978 _reflns_number_gt 13284 _reflns_threshold_expression >2sigma(I) _computing_data_collection XPRESS _computing_cell_refinement SCALEPACK _computing_data_reduction SCALEPACK _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0114P)^2^+6.9613P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens found _refine_ls_hydrogen_treatment 'riding (CH) isotropic (OH)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15978 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0939 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.735946(19) 0.555853(10) 0.052270(8) 0.02425(4) Uani 1 1 d . . . S1 S 0.52027(13) 0.46342(7) 0.07996(6) 0.0269(2) Uani 1 1 d . . . P1 P 0.94828(13) 0.64825(7) 0.02844(6) 0.0233(2) Uani 1 1 d . . . O1 O 0.6129(4) 0.5618(2) 0.44338(18) 0.0340(8) Uani 1 1 d . . . H1 H 0.606(8) 0.561(4) 0.481(3) 0.041(18) Uiso 1 1 d . . . O2 O 0.4060(4) 0.4515(2) 0.42342(17) 0.0329(7) Uani 1 1 d . . . Au2 Au 0.732908(19) 0.055227(10) 0.471424(8) 0.02404(4) Uani 1 1 d . . . P2 P 0.94207(13) 0.15315(7) 0.53573(6) 0.0224(2) Uani 1 1 d . . . S2 S 0.52037(14) -0.04209(7) 0.40195(6) 0.0281(2) Uani 1 1 d . . . O3 O 0.6079(5) 0.0569(2) 0.0857(2) 0.0424(9) Uani 1 1 d . . . H3 H 0.602(9) 0.059(4) 0.050(4) 0.05(2) Uiso 1 1 d . . . O4 O 0.4026(5) -0.0541(3) 0.05183(18) 0.0434(9) Uani 1 1 d . . . C11 C 0.5217(5) 0.4814(3) 0.1739(2) 0.0230(8) Uani 1 1 d . . . C12 C 0.4120(6) 0.4237(3) 0.2006(2) 0.0290(9) Uani 1 1 d . . . H12D H 0.3399 0.3793 0.1681 0.035 Uiso 1 1 calc R . . C13 C 0.4087(6) 0.4314(3) 0.2740(2) 0.0297(9) Uani 1 1 d . . . H13C H 0.3350 0.3916 0.2912 0.036 Uiso 1 1 calc R . . C14 C 0.5118(5) 0.4966(3) 0.3232(2) 0.0235(8) Uani 1 1 d . . . C15 C 0.6191(5) 0.5550(3) 0.2968(2) 0.0252(8) Uani 1 1 d . . . H15A H 0.6894 0.6000 0.3295 0.030 Uiso 1 1 calc R . . C16 C 0.6235(5) 0.5476(3) 0.2233(2) 0.0245(8) Uani 1 1 d . . . H16A H 0.6961 0.5878 0.2062 0.029 Uiso 1 1 calc R . . C17 C 0.5052(5) 0.5014(3) 0.4006(2) 0.0255(8) Uani 1 1 d . . . C21 C 0.5201(5) -0.0252(3) 0.3153(2) 0.0234(8) Uani 1 1 d . . . C22 C 0.4034(6) -0.0804(3) 0.2630(2) 0.0373(11) Uani 1 1 d . . . H22D H 0.3284 -0.1233 0.2757 0.045 Uiso 1 1 calc R . . C23 C 0.3973(6) -0.0728(3) 0.1936(3) 0.0374(11) Uani 1 1 d . . . H23D H 0.3177 -0.1105 0.1588 0.045 Uiso 1 1 calc R . . C24 C 0.5061(6) -0.0106(3) 0.1735(2) 0.0283(9) Uani 1 1 d . . . C25 C 0.6213(6) 0.0451(3) 0.2256(2) 0.0311(9) Uani 1 1 d . . . H25A H 0.6951 0.0884 0.2128 0.037 Uiso 1 1 calc R . . C26 C 0.6284(6) 0.0375(3) 0.2957(2) 0.0288(9) Uani 1 1 d . . . H26A H 0.7076 0.0753 0.3306 0.035 Uiso 1 1 calc R . . C27 C 0.5000(6) -0.0040(3) 0.0984(2) 0.0303(9) Uani 1 1 d . . . C111 C 0.9012(5) 0.7465(3) 0.0352(2) 0.0273(8) Uani 1 1 d . . . C112 C 1.0258(6) 0.8154(3) 0.0428(3) 0.0348(10) Uani 1 1 d . . . H11E H 1.1375 0.8118 0.0451 0.042 Uiso 1 1 calc R . . C113 C 0.9879(7) 0.8890(4) 0.0472(3) 0.0472(14) Uani 1 1 d . . . H11A H 1.0741 0.9358 0.0512 0.057 Uiso 1 1 calc R . . C114 C 0.8275(7) 0.8961(3) 0.0459(3) 0.0418(12) Uani 1 1 d . . . H11B H 0.8033 0.9477 0.0508 0.050 Uiso 1 1 calc R . . C115 C 0.7010(7) 0.8275(3) 0.0376(3) 0.0414(12) Uani 1 1 d . . . H11C H 0.5898 0.8319 0.0362 0.050 Uiso 1 1 calc R . . C116 C 0.7369(6) 0.7525(3) 0.0313(3) 0.0321(10) Uani 1 1 d . . . H11D H 0.6505 0.7052 0.0243 0.039 Uiso 1 1 calc R . . C121 C 1.1171(5) 0.6693(3) 0.0959(2) 0.0269(8) Uani 1 1 d . . . C122 C 1.2709(6) 0.6543(3) 0.0809(3) 0.0315(9) Uani 1 1 d . . . H12E H 1.2980 0.6368 0.0324 0.038 Uiso 1 1 calc R . . C123 C 1.3850(6) 0.6653(3) 0.1375(3) 0.0396(11) Uani 1 1 d . . . H12A H 1.4913 0.6557 0.1278 0.048 Uiso 1 1 calc R . . C124 C 1.3445(7) 0.6898(4) 0.2075(3) 0.0424(12) Uani 1 1 d . . . H12B H 1.4212 0.6959 0.2464 0.051 Uiso 1 1 calc R . . C125 C 1.1904(7) 0.7056(4) 0.2208(3) 0.0448(13) Uani 1 1 d . . . H12C H 1.1635 0.7242 0.2692 0.054 Uiso 1 1 calc R . . C126 C 1.0766(6) 0.6948(3) 0.1657(3) 0.0333(10) Uani 1 1 d . . . H12F H 0.9708 0.7049 0.1755 0.040 Uiso 1 1 calc R . . C131 C 1.0253(5) 0.6206(3) -0.0604(2) 0.0250(8) Uani 1 1 d . . . C132 C 0.9459(6) 0.5500(3) -0.1100(3) 0.0331(10) Uani 1 1 d . . . H13E H 0.8549 0.5141 -0.0971 0.040 Uiso 1 1 calc R . . C133 C 1.0021(7) 0.5320(4) -0.1799(3) 0.0421(12) Uani 1 1 d . . . H13A H 0.9504 0.4837 -0.2149 0.051 Uiso 1 1 calc R . . C134 C 1.1327(8) 0.5855(4) -0.1965(3) 0.0450(14) Uani 1 1 d . . . H13B H 1.1711 0.5749 -0.2436 0.054 Uiso 1 1 calc R . . C135 C 1.2087(7) 0.6549(4) -0.1448(3) 0.0475(14) Uani 1 1 d . . . H13D H 1.2998 0.6908 -0.1574 0.057 Uiso 1 1 calc R . . N136 N 1.1582(5) 0.6742(3) -0.0759(3) 0.0412(10) Uani 1 1 d . . . C211 C 0.8946(5) 0.2519(3) 0.5647(2) 0.0233(8) Uani 1 1 d . . . C212 C 1.0153(5) 0.3238(3) 0.5718(2) 0.0286(9) Uani 1 1 d . . . H21E H 1.1238 0.3215 0.5585 0.034 Uiso 1 1 calc R . . C213 C 0.9756(6) 0.3981(3) 0.5982(3) 0.0357(10) Uani 1 1 d . . . H21A H 1.0574 0.4467 0.6027 0.043 Uiso 1 1 calc R . . C214 C 0.8181(7) 0.4029(3) 0.6183(3) 0.0392(11) Uani 1 1 d . . . H21B H 0.7928 0.4542 0.6375 0.047 Uiso 1 1 calc R . . C215 C 0.6977(6) 0.3317(3) 0.6101(3) 0.0369(11) Uani 1 1 d . . . H21C H 0.5890 0.3345 0.6227 0.044 Uiso 1 1 calc R . . C216 C 0.7354(5) 0.2566(3) 0.5837(3) 0.0297(9) Uani 1 1 d . . . H21D H 0.6526 0.2083 0.5786 0.036 Uiso 1 1 calc R . . C221 C 1.0183(5) 0.1341(3) 0.6167(2) 0.0256(8) Uani 1 1 d . . . C222 C 0.9636(7) 0.0583(3) 0.6300(3) 0.0391(11) Uani 1 1 d . . . H22E H 0.8870 0.0170 0.5966 0.047 Uiso 1 1 calc R . . C223 C 1.0202(8) 0.0430(4) 0.6916(4) 0.0528(15) Uani 1 1 d . . . H22A H 0.9838 -0.0092 0.6998 0.063 Uiso 1 1 calc R . . C224 C 1.1282(8) 0.1021(4) 0.7410(3) 0.0468(14) Uani 1 1 d . . . H22B H 1.1634 0.0915 0.7841 0.056 Uiso 1 1 calc R . . C225 C 1.1861(8) 0.1773(4) 0.7282(3) 0.0516(15) Uani 1 1 d . . . H22C H 1.2637 0.2180 0.7617 0.062 Uiso 1 1 calc R . . C226 C 1.1306(8) 0.1933(3) 0.6659(3) 0.0455(13) Uani 1 1 d . . . H22F H 1.1700 0.2451 0.6572 0.055 Uiso 1 1 calc R . . C231 C 1.1140(5) 0.1679(3) 0.4790(2) 0.0244(8) Uani 1 1 d . . . N232 N 1.0756(5) 0.1915(3) 0.4211(2) 0.0366(9) Uani 1 1 d . . . C233 C 1.1904(7) 0.1986(4) 0.3736(3) 0.0439(13) Uani 1 1 d . . . H23A H 1.1651 0.2155 0.3323 0.053 Uiso 1 1 calc R . . C234 C 1.3445(7) 0.1829(4) 0.3810(3) 0.0454(13) Uani 1 1 d . . . H23B H 1.4220 0.1883 0.3456 0.054 Uiso 1 1 calc R . . C235 C 1.3818(6) 0.1593(4) 0.4412(3) 0.0420(12) Uani 1 1 d . . . H23C H 1.4861 0.1479 0.4479 0.050 Uiso 1 1 calc R . . C236 C 1.2657(6) 0.1521(3) 0.4921(3) 0.0308(9) Uani 1 1 d . . . H23E H 1.2894 0.1369 0.5345 0.037 Uiso 1 1 calc R . . C01 C 0.8490(6) 0.3144(3) 0.3926(3) 0.0365(11) Uani 1 1 d . . . H01A H 0.8620 0.2782 0.4242 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.7874(3) 0.25355(11) 0.30580(9) 0.0658(5) Uani 1 1 d . . . Cl2 Cl 0.6978(2) 0.36558(13) 0.42600(12) 0.0732(5) Uani 1 1 d . . . Cl3 Cl 1.03862(19) 0.38220(10) 0.39472(10) 0.0566(4) Uani 1 1 d . . . C02 C 0.8078(9) 0.8344(5) -0.1483(3) 0.0608(18) Uani 1 1 d . . . H02A H 0.8004 0.8494 -0.0948 0.073 Uiso 1 1 calc R . . Cl4 Cl 0.6109(2) 0.79485(15) -0.18959(16) 0.0904(8) Uani 1 1 d . . . Cl5 Cl 0.8997(4) 0.92126(12) -0.17533(16) 0.1068(9) Uani 1 1 d . . . Cl6 Cl 0.9246(2) 0.76178(15) -0.17100(17) 0.0938(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02422(8) 0.02632(8) 0.02090(8) 0.00558(6) 0.00427(6) 0.00355(6) S1 0.0277(5) 0.0308(5) 0.0187(4) 0.0058(4) 0.0023(4) 0.0001(4) P1 0.0226(4) 0.0238(5) 0.0225(5) 0.0037(4) 0.0049(4) 0.0058(4) O1 0.0354(17) 0.041(2) 0.0195(15) 0.0068(14) 0.0016(14) -0.0035(14) O2 0.0289(15) 0.045(2) 0.0220(15) 0.0107(13) 0.0045(13) -0.0007(14) Au2 0.02421(7) 0.02405(8) 0.02145(8) 0.00488(6) -0.00081(6) 0.00176(6) P2 0.0228(4) 0.0221(5) 0.0214(5) 0.0051(4) 0.0001(4) 0.0041(4) S2 0.0294(5) 0.0296(5) 0.0212(5) 0.0082(4) -0.0011(4) -0.0034(4) O3 0.059(2) 0.044(2) 0.0233(17) 0.0122(15) 0.0006(18) 0.0060(18) O4 0.043(2) 0.060(3) 0.0220(16) 0.0093(16) -0.0039(15) 0.0016(18) C11 0.0219(17) 0.027(2) 0.0205(18) 0.0077(15) 0.0040(15) 0.0054(15) C12 0.030(2) 0.030(2) 0.0225(19) 0.0056(16) 0.0019(17) -0.0014(17) C13 0.030(2) 0.030(2) 0.027(2) 0.0111(17) 0.0032(18) 0.0006(17) C14 0.0218(17) 0.030(2) 0.0191(18) 0.0062(15) 0.0036(15) 0.0061(15) C15 0.0232(18) 0.027(2) 0.0223(19) 0.0049(15) -0.0010(16) 0.0009(15) C16 0.0232(18) 0.025(2) 0.0239(19) 0.0062(15) 0.0017(16) 0.0021(15) C17 0.0221(17) 0.034(2) 0.0210(19) 0.0074(16) 0.0026(15) 0.0076(16) C21 0.0244(18) 0.026(2) 0.0177(17) 0.0036(14) -0.0027(15) 0.0049(15) C22 0.038(2) 0.040(3) 0.024(2) 0.0047(19) -0.0007(19) -0.010(2) C23 0.038(2) 0.044(3) 0.023(2) 0.0052(19) -0.003(2) -0.002(2) C24 0.032(2) 0.035(2) 0.0177(18) 0.0046(16) 0.0022(17) 0.0094(18) C25 0.039(2) 0.032(2) 0.0206(19) 0.0079(17) 0.0016(18) 0.0037(19) C26 0.033(2) 0.030(2) 0.0190(18) 0.0044(16) -0.0028(17) 0.0017(17) C27 0.033(2) 0.038(3) 0.023(2) 0.0073(17) 0.0045(18) 0.0155(19) C111 0.0278(19) 0.025(2) 0.028(2) 0.0036(16) 0.0043(17) 0.0069(16) C112 0.029(2) 0.024(2) 0.044(3) -0.0014(19) 0.000(2) 0.0035(17) C113 0.045(3) 0.033(3) 0.056(4) 0.000(2) 0.008(3) 0.007(2) C114 0.051(3) 0.029(3) 0.047(3) 0.007(2) 0.010(3) 0.015(2) C115 0.041(3) 0.037(3) 0.053(3) 0.014(2) 0.012(2) 0.019(2) C116 0.028(2) 0.035(2) 0.034(2) 0.0083(19) 0.0056(19) 0.0093(18) C121 0.0258(19) 0.024(2) 0.031(2) 0.0050(16) 0.0038(17) 0.0066(16) C122 0.029(2) 0.030(2) 0.034(2) 0.0048(18) 0.0054(19) 0.0075(18) C123 0.027(2) 0.048(3) 0.044(3) 0.008(2) 0.002(2) 0.014(2) C124 0.038(3) 0.052(3) 0.035(3) 0.007(2) -0.008(2) 0.010(2) C125 0.037(3) 0.057(4) 0.035(3) 0.002(2) 0.001(2) 0.013(2) C126 0.029(2) 0.041(3) 0.030(2) 0.0050(19) 0.0033(18) 0.0119(19) C131 0.0282(19) 0.025(2) 0.026(2) 0.0086(16) 0.0076(17) 0.0125(16) C132 0.040(2) 0.028(2) 0.029(2) 0.0045(18) 0.003(2) 0.0075(19) C133 0.055(3) 0.045(3) 0.028(2) 0.000(2) 0.006(2) 0.025(3) C134 0.058(3) 0.064(4) 0.030(2) 0.021(2) 0.022(2) 0.039(3) C135 0.047(3) 0.055(4) 0.056(4) 0.032(3) 0.024(3) 0.024(3) N136 0.037(2) 0.041(3) 0.049(3) 0.015(2) 0.017(2) 0.0105(19) C211 0.0255(18) 0.0221(19) 0.0221(18) 0.0048(14) -0.0017(15) 0.0062(15) C212 0.0258(19) 0.025(2) 0.032(2) 0.0046(17) -0.0001(17) 0.0046(16) C213 0.034(2) 0.027(2) 0.044(3) 0.006(2) -0.001(2) 0.0065(18) C214 0.042(3) 0.032(3) 0.048(3) 0.011(2) 0.007(2) 0.018(2) C215 0.032(2) 0.041(3) 0.045(3) 0.015(2) 0.012(2) 0.019(2) C216 0.0256(19) 0.031(2) 0.034(2) 0.0121(18) 0.0032(18) 0.0064(17) C221 0.030(2) 0.025(2) 0.0234(19) 0.0058(15) 0.0010(17) 0.0088(16) C222 0.046(3) 0.037(3) 0.031(2) 0.011(2) -0.006(2) 0.002(2) C223 0.060(4) 0.053(4) 0.057(4) 0.034(3) 0.000(3) 0.013(3) C224 0.055(3) 0.067(4) 0.030(3) 0.022(3) 0.002(3) 0.026(3) C225 0.063(4) 0.050(4) 0.038(3) -0.002(2) -0.019(3) 0.021(3) C226 0.056(3) 0.031(3) 0.044(3) 0.008(2) -0.019(3) 0.003(2) C231 0.0215(17) 0.0220(19) 0.029(2) 0.0049(15) 0.0018(16) 0.0045(15) N232 0.033(2) 0.052(3) 0.031(2) 0.0170(19) 0.0068(17) 0.0170(19) C233 0.040(3) 0.066(4) 0.037(3) 0.027(3) 0.014(2) 0.020(3) C234 0.036(3) 0.052(3) 0.051(3) 0.015(3) 0.015(2) 0.015(2) C235 0.026(2) 0.050(3) 0.053(3) 0.013(3) 0.007(2) 0.016(2) C236 0.030(2) 0.031(2) 0.033(2) 0.0080(18) -0.0010(19) 0.0105(18) C01 0.034(2) 0.037(3) 0.043(3) 0.019(2) 0.001(2) 0.008(2) Cl1 0.0795(12) 0.0545(10) 0.0513(9) 0.0056(7) -0.0006(9) -0.0002(9) Cl2 0.0578(10) 0.0785(13) 0.0902(14) 0.0175(11) 0.0214(10) 0.0348(9) Cl3 0.0435(7) 0.0443(8) 0.0781(11) 0.0223(7) 0.0061(7) -0.0056(6) C02 0.079(5) 0.073(5) 0.032(3) 0.016(3) 0.019(3) 0.018(4) Cl4 0.0545(10) 0.0901(16) 0.155(2) 0.0711(16) 0.0303(13) 0.0306(10) Cl5 0.145(2) 0.0326(9) 0.121(2) 0.0063(11) 0.0092(18) -0.0094(12) Cl6 0.0493(9) 0.0876(16) 0.170(3) 0.0754(17) 0.0136(13) 0.0215(10) _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 P1 2.2561(11) . ? Au1 S1 2.3036(10) . ? S1 C11 1.751(4) . ? P1 C131 1.816(4) . ? P1 C111 1.819(5) . ? P1 C121 1.819(5) . ? O1 C17 1.317(5) . ? O1 H1 0.73(6) . ? O2 C17 1.232(5) . ? Au2 P2 2.2588(11) . ? Au2 S2 2.3079(11) . ? P2 C211 1.808(4) . ? P2 C221 1.809(4) . ? P2 C231 1.821(4) . ? S2 C21 1.760(4) . ? O3 C27 1.311(6) . ? O3 H3 0.71(7) . ? O4 C27 1.229(6) . ? C11 C16 1.402(6) . ? C11 C12 1.407(6) . ? C12 C13 1.382(6) . ? C12 H12D 0.9500 . ? C13 C14 1.397(6) . ? C13 H13C 0.9500 . ? C14 C15 1.403(6) . ? C14 C17 1.469(6) . ? C15 C16 1.386(6) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C21 C26 1.392(6) . ? C21 C22 1.406(6) . ? C22 C23 1.374(7) . ? C22 H22D 0.9500 . ? C23 C24 1.393(7) . ? C23 H23D 0.9500 . ? C24 C25 1.400(6) . ? C24 C27 1.475(6) . ? C25 C26 1.389(6) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C111 C112 1.383(6) . ? C111 C116 1.403(6) . ? C112 C113 1.374(8) . ? C112 H11E 0.9500 . ? C113 C114 1.373(8) . ? C113 H11A 0.9500 . ? C114 C115 1.388(8) . ? C114 H11B 0.9500 . ? C115 C116 1.385(7) . ? C115 H11C 0.9500 . ? C116 H11D 0.9500 . ? C121 C126 1.371(6) . ? C121 C122 1.385(6) . ? C122 C123 1.389(7) . ? C122 H12E 0.9500 . ? C123 C124 1.373(8) . ? C123 H12A 0.9500 . ? C124 C125 1.388(8) . ? C124 H12B 0.9500 . ? C125 C126 1.367(7) . ? C125 H12C 0.9500 . ? C126 H12F 0.9500 . ? C131 N136 1.374(6) . ? C131 C132 1.382(6) . ? C132 C133 1.408(7) . ? C132 H13E 0.9500 . ? C133 C134 1.368(8) . ? C133 H13A 0.9500 . ? C134 C135 1.381(9) . ? C134 H13B 0.9500 . ? C135 N136 1.374(7) . ? C135 H13D 0.9500 . ? C211 C216 1.397(6) . ? C211 C212 1.404(6) . ? C212 C213 1.384(7) . ? C212 H21E 0.9500 . ? C213 C214 1.389(7) . ? C213 H21A 0.9500 . ? C214 C215 1.390(8) . ? C214 H21B 0.9500 . ? C215 C216 1.390(7) . ? C215 H21C 0.9500 . ? C216 H21D 0.9500 . ? C221 C226 1.383(7) . ? C221 C222 1.391(7) . ? C222 C223 1.377(8) . ? C222 H22E 0.9500 . ? C223 C224 1.367(9) . ? C223 H22A 0.9500 . ? C224 C225 1.381(9) . ? C224 H22B 0.9500 . ? C225 C226 1.393(8) . ? C225 H22C 0.9500 . ? C226 H22F 0.9500 . ? C231 N232 1.339(6) . ? C231 C236 1.389(6) . ? N232 C233 1.336(6) . ? C233 C234 1.388(8) . ? C233 H23A 0.9500 . ? C234 C235 1.377(8) . ? C234 H23B 0.9500 . ? C235 C236 1.391(7) . ? C235 H23C 0.9500 . ? C236 H23E 0.9500 . ? C01 Cl2 1.740(5) . ? C01 Cl1 1.742(6) . ? C01 Cl3 1.751(5) . ? C01 H01A 1.0000 . ? C02 Cl4 1.738(8) . ? C02 Cl6 1.739(8) . ? C02 Cl5 1.748(7) . ? C02 H02A 1.0000 . ? 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 P1 Au1 S1 178.40(4) . . ? C11 S1 Au1 108.37(14) . . ? C131 P1 C111 104.8(2) . . ? C131 P1 C121 108.6(2) . . ? C111 P1 C121 104.4(2) . . ? C131 P1 Au1 115.46(15) . . ? C111 P1 Au1 113.40(14) . . ? C121 P1 Au1 109.43(15) . . ? C17 O1 H1 112(5) . . ? P2 Au2 S2 177.63(4) . . ? C211 P2 C221 105.22(19) . . ? C211 P2 C231 104.51(19) . . ? C221 P2 C231 107.6(2) . . ? C211 P2 Au2 113.95(14) . . ? C221 P2 Au2 115.53(15) . . ? C231 P2 Au2 109.28(14) . . ? C21 S2 Au2 107.21(14) . . ? C27 O3 H3 113(6) . . ? C16 C11 C12 118.6(4) . . ? C16 C11 S1 125.1(3) . . ? C12 C11 S1 116.3(3) . . ? C13 C12 C11 120.3(4) . . ? C13 C12 H12D 119.8 . . ? C11 C12 H12D 119.8 . . ? C12 C13 C14 121.2(4) . . ? C12 C13 H13C 119.4 . . ? C14 C13 H13C 119.4 . . ? C13 C14 C15 118.6(4) . . ? C13 C14 C17 119.1(4) . . ? C15 C14 C17 122.4(4) . . ? C16 C15 C14 120.6(4) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C11 120.7(4) . . ? C15 C16 H16A 119.7 . . ? C11 C16 H16A 119.7 . . ? O2 C17 O1 122.7(4) . . ? O2 C17 C14 121.8(4) . . ? O1 C17 C14 115.5(4) . . ? C26 C21 C22 118.9(4) . . ? C26 C21 S2 124.4(3) . . ? C22 C21 S2 116.7(3) . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22D 119.8 . . ? C21 C22 H22D 119.8 . . ? C22 C23 C24 120.9(4) . . ? C22 C23 H23D 119.5 . . ? C24 C23 H23D 119.5 . . ? C23 C24 C25 118.9(4) . . ? C23 C24 C27 120.3(4) . . ? C25 C24 C27 120.8(4) . . ? C26 C25 C24 120.4(4) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C21 120.5(4) . . ? C25 C26 H26A 119.8 . . ? C21 C26 H26A 119.8 . . ? O4 C27 O3 123.7(4) . . ? O4 C27 C24 121.3(4) . . ? O3 C27 C24 115.0(4) . . ? C112 C111 C116 119.5(4) . . ? C112 C111 P1 120.7(3) . . ? C116 C111 P1 119.8(3) . . ? C113 C112 C111 119.9(5) . . ? C113 C112 H11E 120.0 . . ? C111 C112 H11E 120.0 . . ? C114 C113 C112 121.2(5) . . ? C114 C113 H11A 119.4 . . ? C112 C113 H11A 119.4 . . ? C113 C114 C115 119.6(5) . . ? C113 C114 H11B 120.2 . . ? C115 C114 H11B 120.2 . . ? C116 C115 C114 119.9(5) . . ? C116 C115 H11C 120.0 . . ? C114 C115 H11C 120.0 . . ? C115 C116 C111 119.8(5) . . ? C115 C116 H11D 120.1 . . ? C111 C116 H11D 120.1 . . ? C126 C121 C122 121.0(5) . . ? C126 C121 P1 114.4(3) . . ? C122 C121 P1 124.4(4) . . ? C121 C122 C123 119.2(5) . . ? C121 C122 H12E 120.4 . . ? C123 C122 H12E 120.4 . . ? C124 C123 C122 120.1(5) . . ? C124 C123 H12A 119.9 . . ? C122 C123 H12A 119.9 . . ? C123 C124 C125 119.3(5) . . ? C123 C124 H12B 120.4 . . ? C125 C124 H12B 120.4 . . ? C126 C125 C124 121.2(5) . . ? C126 C125 H12C 119.4 . . ? C124 C125 H12C 119.4 . . ? C125 C126 C121 119.1(5) . . ? C125 C126 H12F 120.4 . . ? C121 C126 H12F 120.4 . . ? N136 C131 C132 123.0(4) . . ? N136 C131 P1 117.0(3) . . ? C132 C131 P1 119.9(3) . . ? C131 C132 C133 118.9(5) . . ? C131 C132 H13E 120.6 . . ? C133 C132 H13E 120.6 . . ? C134 C133 C132 118.8(5) . . ? C134 C133 H13A 120.6 . . ? C132 C133 H13A 120.6 . . ? C133 C134 C135 120.1(5) . . ? C133 C134 H13B 120.0 . . ? C135 C134 H13B 120.0 . . ? N136 C135 C134 122.9(5) . . ? N136 C135 H13D 118.6 . . ? C134 C135 H13D 118.6 . . ? C131 N136 C135 116.4(5) . . ? C216 C211 C212 119.2(4) . . ? C216 C211 P2 118.9(3) . . ? C212 C211 P2 121.8(3) . . ? C213 C212 C211 119.7(4) . . ? C213 C212 H21E 120.1 . . ? C211 C212 H21E 120.1 . . ? C212 C213 C214 121.1(5) . . ? C212 C213 H21A 119.5 . . ? C214 C213 H21A 119.5 . . ? C213 C214 C215 119.3(5) . . ? C213 C214 H21B 120.4 . . ? C215 C214 H21B 120.4 . . ? C214 C215 C216 120.4(4) . . ? C214 C215 H21C 119.8 . . ? C216 C215 H21C 119.8 . . ? C215 C216 C211 120.2(4) . . ? C215 C216 H21D 119.9 . . ? C211 C216 H21D 119.9 . . ? C226 C221 C222 119.0(5) . . ? C226 C221 P2 121.4(4) . . ? C222 C221 P2 119.5(4) . . ? C223 C222 C221 120.2(5) . . ? C223 C222 H22E 119.9 . . ? C221 C222 H22E 119.9 . . ? C224 C223 C222 120.8(6) . . ? C224 C223 H22A 119.6 . . ? C222 C223 H22A 119.6 . . ? C223 C224 C225 119.9(5) . . ? C223 C224 H22B 120.1 . . ? C225 C224 H22B 120.1 . . ? C224 C225 C226 119.8(6) . . ? C224 C225 H22C 120.1 . . ? C226 C225 H22C 120.1 . . ? C221 C226 C225 120.3(5) . . ? C221 C226 H22F 119.9 . . ? C225 C226 H22F 119.9 . . ? N232 C231 C236 123.5(4) . . ? N232 C231 P2 112.6(3) . . ? C236 C231 P2 123.8(3) . . ? C233 N232 C231 117.1(4) . . ? N232 C233 C234 123.9(5) . . ? N232 C233 H23A 118.1 . . ? C234 C233 H23A 118.1 . . ? C235 C234 C233 118.1(5) . . ? C235 C234 H23B 121.0 . . ? C233 C234 H23B 121.0 . . ? C234 C235 C236 119.5(5) . . ? C234 C235 H23C 120.2 . . ? C236 C235 H23C 120.2 . . ? C231 C236 C235 117.9(4) . . ? C231 C236 H23E 121.0 . . ? C235 C236 H23E 121.0 . . ? Cl2 C01 Cl1 109.9(3) . . ? Cl2 C01 Cl3 111.2(3) . . ? Cl1 C01 Cl3 111.4(3) . . ? Cl2 C01 H01A 108.1 . . ? Cl1 C01 H01A 108.1 . . ? Cl3 C01 H01A 108.1 . . ? Cl4 C02 Cl6 109.8(4) . . ? Cl4 C02 Cl5 109.7(4) . . ? Cl6 C02 Cl5 110.3(4) . . ? Cl4 C02 H02A 109.0 . . ? Cl6 C02 H02A 109.0 . . ? Cl5 C02 H02A 109.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 S1 C11 -9.9(15) . . . . ? S1 Au1 P1 C131 166.6(14) . . . . ? S1 Au1 P1 C111 -72.5(15) . . . . ? S1 Au1 P1 C121 43.7(15) . . . . ? S2 Au2 P2 C211 67.0(10) . . . . ? S2 Au2 P2 C221 -170.9(10) . . . . ? S2 Au2 P2 C231 -49.4(10) . . . . ? P2 Au2 S2 C21 10.4(10) . . . . ? Au1 S1 C11 C16 7.8(4) . . . . ? Au1 S1 C11 C12 -171.7(3) . . . . ? C16 C11 C12 C13 -1.8(7) . . . . ? S1 C11 C12 C13 177.7(4) . . . . ? C11 C12 C13 C14 0.8(7) . . . . ? C12 C13 C14 C15 0.4(7) . . . . ? C12 C13 C14 C17 -179.2(4) . . . . ? C13 C14 C15 C16 -0.6(6) . . . . ? C17 C14 C15 C16 179.0(4) . . . . ? C14 C15 C16 C11 -0.5(6) . . . . ? C12 C11 C16 C15 1.6(6) . . . . ? S1 C11 C16 C15 -177.8(3) . . . . ? C13 C14 C17 O2 -3.3(7) . . . . ? C15 C14 C17 O2 177.1(4) . . . . ? C13 C14 C17 O1 176.1(4) . . . . ? C15 C14 C17 O1 -3.5(6) . . . . ? Au2 S2 C21 C26 -1.5(4) . . . . ? Au2 S2 C21 C22 177.4(3) . . . . ? C26 C21 C22 C23 0.4(8) . . . . ? S2 C21 C22 C23 -178.5(4) . . . . ? C21 C22 C23 C24 0.1(8) . . . . ? C22 C23 C24 C25 -0.8(8) . . . . ? C22 C23 C24 C27 178.9(5) . . . . ? C23 C24 C25 C26 1.0(7) . . . . ? C27 C24 C25 C26 -178.6(4) . . . . ? C24 C25 C26 C21 -0.6(7) . . . . ? C22 C21 C26 C25 -0.1(7) . . . . ? S2 C21 C26 C25 178.7(4) . . . . ? C23 C24 C27 O4 -2.0(7) . . . . ? C25 C24 C27 O4 177.7(5) . . . . ? C23 C24 C27 O3 179.9(5) . . . . ? C25 C24 C27 O3 -0.5(6) . . . . ? C131 P1 C111 C112 -71.8(4) . . . . ? C121 P1 C111 C112 42.3(4) . . . . ? Au1 P1 C111 C112 161.4(3) . . . . ? C131 P1 C111 C116 107.0(4) . . . . ? C121 P1 C111 C116 -138.8(4) . . . . ? Au1 P1 C111 C116 -19.8(4) . . . . ? C116 C111 C112 C113 0.6(8) . . . . ? P1 C111 C112 C113 179.4(4) . . . . ? C111 C112 C113 C114 1.7(9) . . . . ? C112 C113 C114 C115 -2.3(9) . . . . ? C113 C114 C115 C116 0.7(9) . . . . ? C114 C115 C116 C111 1.6(8) . . . . ? C112 C111 C116 C115 -2.2(7) . . . . ? P1 C111 C116 C115 179.0(4) . . . . ? C131 P1 C121 C126 177.0(4) . . . . ? C111 P1 C121 C126 65.6(4) . . . . ? Au1 P1 C121 C126 -56.1(4) . . . . ? C131 P1 C121 C122 -8.8(5) . . . . ? C111 P1 C121 C122 -120.3(4) . . . . ? Au1 P1 C121 C122 118.0(4) . . . . ? C126 C121 C122 C123 0.2(7) . . . . ? P1 C121 C122 C123 -173.6(4) . . . . ? C121 C122 C123 C124 0.7(8) . . . . ? C122 C123 C124 C125 -1.8(9) . . . . ? C123 C124 C125 C126 2.0(10) . . . . ? C124 C125 C126 C121 -1.2(9) . . . . ? C122 C121 C126 C125 0.1(8) . . . . ? P1 C121 C126 C125 174.4(4) . . . . ? C111 P1 C131 N136 56.7(4) . . . . ? C121 P1 C131 N136 -54.5(4) . . . . ? Au1 P1 C131 N136 -177.8(3) . . . . ? C111 P1 C131 C132 -120.5(4) . . . . ? C121 P1 C131 C132 128.3(4) . . . . ? Au1 P1 C131 C132 5.0(4) . . . . ? N136 C131 C132 C133 -0.6(8) . . . . ? P1 C131 C132 C133 176.4(4) . . . . ? C131 C132 C133 C134 -0.5(8) . . . . ? C132 C133 C134 C135 1.1(8) . . . . ? C133 C134 C135 N136 -0.6(9) . . . . ? C132 C131 N136 C135 1.0(7) . . . . ? P1 C131 N136 C135 -176.1(4) . . . . ? C134 C135 N136 C131 -0.4(8) . . . . ? C221 P2 C211 C216 -92.2(4) . . . . ? C231 P2 C211 C216 154.6(4) . . . . ? Au2 P2 C211 C216 35.3(4) . . . . ? C221 P2 C211 C212 84.7(4) . . . . ? C231 P2 C211 C212 -28.5(4) . . . . ? Au2 P2 C211 C212 -147.7(3) . . . . ? C216 C211 C212 C213 0.8(7) . . . . ? P2 C211 C212 C213 -176.2(4) . . . . ? C211 C212 C213 C214 0.3(8) . . . . ? C212 C213 C214 C215 -1.5(8) . . . . ? C213 C214 C215 C216 1.5(8) . . . . ? C214 C215 C216 C211 -0.4(8) . . . . ? C212 C211 C216 C215 -0.7(7) . . . . ? P2 C211 C216 C215 176.3(4) . . . . ? C211 P2 C221 C226 -44.7(5) . . . . ? C231 P2 C221 C226 66.3(5) . . . . ? Au2 P2 C221 C226 -171.3(4) . . . . ? C211 P2 C221 C222 135.4(4) . . . . ? C231 P2 C221 C222 -113.6(4) . . . . ? Au2 P2 C221 C222 8.8(4) . . . . ? C226 C221 C222 C223 0.3(8) . . . . ? P2 C221 C222 C223 -179.8(5) . . . . ? C221 C222 C223 C224 1.2(9) . . . . ? C222 C223 C224 C225 -2.3(10) . . . . ? C223 C224 C225 C226 1.8(10) . . . . ? C222 C221 C226 C225 -0.8(8) . . . . ? P2 C221 C226 C225 179.4(5) . . . . ? C224 C225 C226 C221 -0.3(10) . . . . ? C211 P2 C231 N232 -61.5(4) . . . . ? C221 P2 C231 N232 -173.0(3) . . . . ? Au2 P2 C231 N232 60.9(4) . . . . ? C211 P2 C231 C236 122.0(4) . . . . ? C221 P2 C231 C236 10.5(4) . . . . ? Au2 P2 C231 C236 -115.7(4) . . . . ? C236 C231 N232 C233 1.0(7) . . . . ? P2 C231 N232 C233 -175.6(4) . . . . ? C231 N232 C233 C234 0.2(9) . . . . ? N232 C233 C234 C235 -0.6(10) . . . . ? C233 C234 C235 C236 -0.1(9) . . . . ? N232 C231 C236 C235 -1.7(7) . . . . ? P2 C231 C236 C235 174.5(4) . . . . ? C234 C235 C236 C231 1.2(8) . . . . ? _diffrn_measured_fraction_theta_max 0.894 _diffrn_reflns_theta_full 31.67 _diffrn_measured_fraction_theta_full 0.894 _refine_diff_density_max 1.521 _refine_diff_density_min -1.784 _refine_diff_density_rms 0.150 data_jam11 _database_code_CSD 155655 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.50 H21 Au Cl O2 P S' _chemical_formula_weight 654.87 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 12.0102(2) _cell_length_b 13.3450(3) _cell_length_c 17.0602(3) _cell_angle_alpha 74.062(1) _cell_angle_beta 71.819(1) _cell_angle_gamma 86.963(1) _cell_volume 2496.37(8) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 6.168 _exptl_absorpt_correction_type 'DELABS (Platon)' _exptl_absorpt_correction_T_min 0.1325 _exptl_absorpt_correction_T_max 0.7479 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Nonius DIP 2020' _diffrn_measurement_method 'phi rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36359 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 26.31 _reflns_number_total 9408 _reflns_number_gt 8876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XPRESS (Nonius)' _computing_cell_refinement 'SCALEPACK (Nonius)' _computing_data_reduction 'DENZO (Nonius)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-PLUS _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Beside one molecule of methylenechloride which was found and refined without problems, the crystal contains another residual electron density which could not be identified. It was treated with 'SQUEEZE' from Platon. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.6785P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (CH), difmap (OH)' _refine_ls_hydrogen_treatment 'riding (CH), isotropic (OH)' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9408 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 1.455321(12) 0.293848(11) 0.907998(9) 0.01980(5) Uani 1 1 d . . . S1 S 1.63727(8) 0.37945(7) 0.84575(7) 0.0241(2) Uani 1 1 d . . . P1 P 1.27446(8) 0.22257(7) 0.99061(7) 0.0200(2) Uani 1 1 d . . . O1 O 2.0351(3) 0.2071(2) 0.5433(2) 0.0295(7) Uani 1 1 d . . . H1 H 2.073(6) 0.177(5) 0.520(5) 0.08(2) Uiso 1 1 d . . . O2 O 1.9624(2) 0.0511(2) 0.63062(19) 0.0283(6) Uani 1 1 d . . . C1 C 1.7308(3) 0.3079(3) 0.7802(2) 0.0199(8) Uani 1 1 d . . . C2 C 1.8273(3) 0.3613(3) 0.7136(3) 0.0230(8) Uani 1 1 d . . . H2A H 1.8409 0.4334 0.7057 0.028 Uiso 1 1 calc R . . C3 C 1.9028(3) 0.3100(3) 0.6594(3) 0.0257(9) Uani 1 1 d . . . H3A H 1.9664 0.3475 0.6133 0.031 Uiso 1 1 calc R . . C4 C 1.8865(3) 0.2034(3) 0.6718(3) 0.0205(8) Uani 1 1 d . . . C5 C 1.7927(3) 0.1497(3) 0.7395(3) 0.0224(8) Uani 1 1 d . . . H5A H 1.7816 0.0768 0.7494 0.027 Uiso 1 1 calc R . . C6 C 1.7156(3) 0.2015(3) 0.7924(3) 0.0218(8) Uani 1 1 d . . . H6A H 1.6513 0.1640 0.8379 0.026 Uiso 1 1 calc R . . C7 C 1.9641(3) 0.1477(3) 0.6138(3) 0.0215(8) Uani 1 1 d . . . C111 C 1.2439(3) 0.2354(3) 1.0986(3) 0.0219(8) Uani 1 1 d . . . C112 C 1.1827(3) 0.1605(3) 1.1717(3) 0.0252(9) Uani 1 1 d . . . H11A H 1.1538 0.0981 1.1671 0.030 Uiso 1 1 calc R . . C113 C 1.1636(4) 0.1768(3) 1.2516(3) 0.0294(9) Uani 1 1 d . . . H11B H 1.1234 0.1244 1.3017 0.035 Uiso 1 1 calc R . . C114 C 1.2024(4) 0.2679(3) 1.2592(3) 0.0310(9) Uani 1 1 d . . . H11C H 1.1888 0.2782 1.3143 0.037 Uiso 1 1 calc R . . C115 C 1.2610(4) 0.3442(3) 1.1867(3) 0.0339(10) Uani 1 1 d . . . H11D H 1.2858 0.4081 1.1914 0.041 Uiso 1 1 calc R . . C116 C 1.2833(4) 0.3269(3) 1.1073(3) 0.0311(10) Uani 1 1 d . . . H11E H 1.3264 0.3784 1.0576 0.037 Uiso 1 1 calc R . . C121 C 1.2571(3) 0.0851(3) 0.9998(3) 0.0220(8) Uani 1 1 d . . . C122 C 1.3567(4) 0.0278(3) 0.9770(3) 0.0240(8) Uani 1 1 d . . . H12A H 1.4325 0.0606 0.9567 0.029 Uiso 1 1 calc R . . C123 C 1.3444(4) -0.0772(3) 0.9841(3) 0.0307(9) Uani 1 1 d . . . H12B H 1.4122 -0.1162 0.9682 0.037 Uiso 1 1 calc R . . C124 C 1.2350(4) -0.1259(3) 1.0139(3) 0.0337(10) Uani 1 1 d . . . H12C H 1.2277 -0.1982 1.0193 0.040 Uiso 1 1 calc R . . C125 C 1.1364(4) -0.0693(3) 1.0358(3) 0.0337(10) Uani 1 1 d . . . H12D H 1.0610 -0.1028 1.0557 0.040 Uiso 1 1 calc R . . C126 C 1.1460(4) 0.0362(3) 1.0292(3) 0.0284(9) Uani 1 1 d . . . H12E H 1.0777 0.0748 1.0446 0.034 Uiso 1 1 calc R . . C131 C 1.1520(3) 0.2828(3) 0.9555(3) 0.0254(9) Uani 1 1 d . . . C132 C 1.0680(4) 0.3367(4) 1.0036(4) 0.0414(12) Uani 1 1 d . . . H13A H 1.0728 0.3422 1.0568 0.050 Uiso 1 1 calc R . . C133 C 0.9772(5) 0.3823(5) 0.9737(4) 0.0603(17) Uani 1 1 d . . . H13B H 0.9195 0.4185 1.0068 0.072 Uiso 1 1 calc R . . C134 C 0.9701(5) 0.3756(4) 0.8965(4) 0.0520(15) Uani 1 1 d . . . H13C H 0.9078 0.4074 0.8765 0.062 Uiso 1 1 calc R . . C135 C 1.0530(4) 0.3227(4) 0.8479(4) 0.0441(12) Uani 1 1 d . . . H13D H 1.0482 0.3184 0.7944 0.053 Uiso 1 1 calc R . . C136 C 1.1434(4) 0.2760(4) 0.8779(3) 0.0344(10) Uani 1 1 d . . . H13E H 1.2001 0.2389 0.8449 0.041 Uiso 1 1 calc R . . Au2 Au 1.426555(13) 0.359057(11) 0.728095(9) 0.02142(5) Uani 1 1 d . . . S2 S 1.42320(9) 0.17967(7) 0.76257(7) 0.0257(2) Uani 1 1 d . . . P2 P 1.41224(9) 0.53443(7) 0.69557(7) 0.0212(2) Uani 1 1 d . . . O3 O 1.8841(3) 0.0554(2) 0.4622(2) 0.0322(7) Uani 1 1 d . . . H3 H 1.932(5) 0.019(4) 0.435(4) 0.057(18) Uiso 1 1 d . . . O4 O 1.8150(3) -0.1028(2) 0.5469(2) 0.0336(7) Uani 1 1 d . . . C8 C 1.5399(3) 0.1345(3) 0.6910(3) 0.0213(8) Uani 1 1 d . . . C9 C 1.5506(4) 0.0253(3) 0.7104(3) 0.0260(9) Uani 1 1 d . . . H9A H 1.4973 -0.0183 0.7605 0.031 Uiso 1 1 calc R . . C10 C 1.6383(3) -0.0184(3) 0.6569(3) 0.0233(8) Uani 1 1 d . . . H10A H 1.6443 -0.0921 0.6702 0.028 Uiso 1 1 calc R . . C11 C 1.7176(3) 0.0438(3) 0.5841(3) 0.0225(8) Uani 1 1 d . . . C12 C 1.7078(3) 0.1520(3) 0.5647(3) 0.0228(8) Uani 1 1 d . . . H12F H 1.7615 0.1954 0.5148 0.027 Uiso 1 1 calc R . . C13 C 1.6196(3) 0.1962(3) 0.6181(3) 0.0225(8) Uani 1 1 d . . . H13F H 1.6137 0.2699 0.6044 0.027 Uiso 1 1 calc R . . C14 C 1.8094(3) -0.0070(3) 0.5292(3) 0.0237(8) Uani 1 1 d . . . C211 C 1.2815(3) 0.5783(3) 0.6662(3) 0.0261(9) Uani 1 1 d . . . C212 C 1.2481(5) 0.5337(4) 0.6124(4) 0.0453(13) Uani 1 1 d . . . H21A H 1.2928 0.4795 0.5928 0.054 Uiso 1 1 calc R . . C213 C 1.1503(5) 0.5669(4) 0.5864(4) 0.0539(15) Uani 1 1 d . . . H21B H 1.1299 0.5374 0.5478 0.065 Uiso 1 1 calc R . . C214 C 1.0837(4) 0.6425(4) 0.6170(4) 0.0457(13) Uani 1 1 d . . . H21C H 1.0150 0.6637 0.6014 0.055 Uiso 1 1 calc R . . C215 C 1.1162(5) 0.6883(4) 0.6709(4) 0.0491(14) Uani 1 1 d . . . H21D H 1.0705 0.7417 0.6912 0.059 Uiso 1 1 calc R . . C216 C 1.2147(4) 0.6564(4) 0.6948(3) 0.0410(12) Uani 1 1 d . . . H21E H 1.2370 0.6883 0.7313 0.049 Uiso 1 1 calc R . . C221 C 1.5360(3) 0.5975(3) 0.6049(3) 0.0240(8) Uani 1 1 d . . . C222 C 1.6484(4) 0.5711(4) 0.6084(3) 0.0317(10) Uani 1 1 d . . . H22A H 1.6584 0.5200 0.6566 0.038 Uiso 1 1 calc R . . C223 C 1.7446(4) 0.6187(4) 0.5425(3) 0.0370(11) Uani 1 1 d . . . H22B H 1.8210 0.6028 0.5464 0.044 Uiso 1 1 calc R . . C224 C 1.7311(4) 0.6893(4) 0.4706(3) 0.0364(11) Uani 1 1 d . . . H22C H 1.7982 0.7208 0.4246 0.044 Uiso 1 1 calc R . . C225 C 1.6206(4) 0.7143(4) 0.4652(3) 0.0350(10) Uani 1 1 d . . . H22D H 1.6115 0.7621 0.4151 0.042 Uiso 1 1 calc R . . C226 C 1.5230(4) 0.6699(3) 0.5325(3) 0.0302(9) Uani 1 1 d . . . H22E H 1.4469 0.6890 0.5295 0.036 Uiso 1 1 calc R . . C231 C 1.4093(4) 0.5929(3) 0.7806(3) 0.0241(8) Uani 1 1 d . . . C232 C 1.4699(4) 0.6867(3) 0.7632(3) 0.0302(9) Uani 1 1 d . . . H23A H 1.5131 0.7222 0.7059 0.036 Uiso 1 1 calc R . . C233 C 1.4664(4) 0.7277(3) 0.8306(3) 0.0366(11) Uani 1 1 d . . . H23B H 1.5081 0.7913 0.8192 0.044 Uiso 1 1 calc R . . C234 C 1.4039(4) 0.6779(3) 0.9128(3) 0.0345(10) Uani 1 1 d . . . H23C H 1.4030 0.7064 0.9583 0.041 Uiso 1 1 calc R . . C235 C 1.3420(4) 0.5860(3) 0.9300(3) 0.0347(10) Uani 1 1 d . . . H23D H 1.2977 0.5518 0.9873 0.042 Uiso 1 1 calc R . . C236 C 1.3444(4) 0.5436(3) 0.8638(3) 0.0285(9) Uani 1 1 d . . . H23E H 1.3013 0.4806 0.8758 0.034 Uiso 1 1 calc R . . C01 C 0.7868(7) 1.0133(7) 0.2159(7) 0.101(3) Uani 1 1 d . . . H01A H 0.7218 1.0089 0.2695 0.121 Uiso 1 1 calc R . . H01B H 0.7536 0.9983 0.1739 0.121 Uiso 1 1 calc R . . Cl1 Cl 0.8877(2) 0.92020(19) 0.23653(16) 0.1006(7) Uani 1 1 d . . . Cl2 Cl 0.85104(18) 1.14324(17) 0.17464(16) 0.0929(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01762(8) 0.02181(8) 0.01907(9) -0.00612(6) -0.00378(6) -0.00035(6) S1 0.0198(5) 0.0250(5) 0.0260(6) -0.0117(4) 0.0000(4) -0.0045(4) P1 0.0163(5) 0.0201(5) 0.0224(6) -0.0062(4) -0.0036(4) -0.0001(4) O1 0.0257(16) 0.0244(15) 0.0316(19) -0.0096(14) 0.0026(13) 0.0001(12) O2 0.0261(15) 0.0229(14) 0.0314(18) -0.0086(12) -0.0015(12) -0.0002(11) C1 0.0187(18) 0.0237(18) 0.021(2) -0.0075(16) -0.0090(15) -0.0009(15) C2 0.0170(18) 0.0220(18) 0.028(2) -0.0081(17) -0.0015(16) -0.0042(15) C3 0.0197(19) 0.0234(19) 0.031(3) -0.0061(17) -0.0034(17) -0.0047(15) C4 0.0160(18) 0.0248(19) 0.023(2) -0.0091(16) -0.0079(15) 0.0026(14) C5 0.025(2) 0.0182(18) 0.025(2) -0.0062(16) -0.0078(16) -0.0003(15) C6 0.0214(19) 0.0220(18) 0.021(2) -0.0043(16) -0.0053(16) -0.0043(15) C7 0.0163(18) 0.0241(19) 0.024(2) -0.0058(16) -0.0066(16) -0.0025(15) C111 0.0175(18) 0.0232(19) 0.026(2) -0.0090(17) -0.0072(16) 0.0026(15) C112 0.025(2) 0.0176(18) 0.030(2) -0.0030(16) -0.0064(17) -0.0037(15) C113 0.030(2) 0.028(2) 0.023(2) -0.0017(18) -0.0029(18) -0.0045(17) C114 0.031(2) 0.034(2) 0.027(3) -0.0137(19) -0.0042(18) 0.0024(18) C115 0.042(3) 0.026(2) 0.033(3) -0.0144(19) -0.005(2) -0.0035(19) C116 0.034(2) 0.023(2) 0.030(3) -0.0051(18) -0.0015(19) -0.0064(17) C121 0.0233(19) 0.0202(18) 0.025(2) -0.0074(16) -0.0095(16) 0.0007(15) C122 0.023(2) 0.028(2) 0.021(2) -0.0068(17) -0.0082(16) 0.0029(16) C123 0.033(2) 0.030(2) 0.032(3) -0.0119(19) -0.0143(19) 0.0110(18) C124 0.044(3) 0.023(2) 0.039(3) -0.0110(19) -0.018(2) 0.0024(19) C125 0.031(2) 0.031(2) 0.042(3) -0.010(2) -0.013(2) -0.0081(18) C126 0.022(2) 0.029(2) 0.036(3) -0.0138(19) -0.0083(18) 0.0013(16) C131 0.0207(19) 0.0233(19) 0.029(2) -0.0036(17) -0.0064(17) -0.0012(15) C132 0.038(3) 0.047(3) 0.052(3) -0.027(3) -0.023(2) 0.019(2) C133 0.052(3) 0.067(4) 0.083(5) -0.044(4) -0.035(3) 0.037(3) C134 0.045(3) 0.045(3) 0.082(5) -0.020(3) -0.042(3) 0.020(2) C135 0.038(3) 0.056(3) 0.042(3) -0.008(2) -0.021(2) 0.003(2) C136 0.021(2) 0.047(3) 0.035(3) -0.011(2) -0.0103(19) 0.0012(19) Au2 0.02396(8) 0.02053(8) 0.02181(10) -0.00868(6) -0.00794(6) 0.00416(6) S2 0.0279(5) 0.0216(5) 0.0237(6) -0.0080(4) -0.0015(4) 0.0033(4) P2 0.0218(5) 0.0199(5) 0.0235(6) -0.0077(4) -0.0081(4) 0.0030(4) O3 0.0271(16) 0.0302(16) 0.0318(19) -0.0100(14) 0.0024(13) 0.0016(13) O4 0.0356(17) 0.0280(15) 0.0309(19) -0.0122(13) 0.0013(13) 0.0051(13) C8 0.0204(19) 0.0254(19) 0.022(2) -0.0109(16) -0.0084(16) 0.0042(15) C9 0.024(2) 0.025(2) 0.027(2) -0.0081(17) -0.0045(17) -0.0003(16) C10 0.024(2) 0.0176(18) 0.029(2) -0.0066(16) -0.0104(17) 0.0023(15) C11 0.0213(19) 0.0252(19) 0.025(2) -0.0110(17) -0.0094(16) 0.0035(15) C12 0.0229(19) 0.0257(19) 0.018(2) -0.0037(16) -0.0057(16) -0.0040(15) C13 0.025(2) 0.0206(18) 0.024(2) -0.0068(16) -0.0102(17) 0.0015(15) C14 0.0217(19) 0.029(2) 0.022(2) -0.0091(17) -0.0066(16) 0.0011(16) C211 0.024(2) 0.026(2) 0.028(2) -0.0047(17) -0.0088(17) 0.0013(16) C212 0.043(3) 0.045(3) 0.067(4) -0.029(3) -0.033(3) 0.017(2) C213 0.046(3) 0.058(3) 0.077(4) -0.028(3) -0.038(3) 0.008(3) C214 0.027(2) 0.051(3) 0.058(4) -0.007(3) -0.021(2) 0.007(2) C215 0.036(3) 0.060(3) 0.057(4) -0.022(3) -0.022(3) 0.024(2) C216 0.038(3) 0.048(3) 0.046(3) -0.024(2) -0.017(2) 0.017(2) C221 0.024(2) 0.0257(19) 0.026(2) -0.0125(17) -0.0092(17) 0.0022(16) C222 0.028(2) 0.040(2) 0.027(3) -0.0046(19) -0.0121(19) 0.0016(18) C223 0.026(2) 0.054(3) 0.036(3) -0.017(2) -0.011(2) 0.000(2) C224 0.031(2) 0.046(3) 0.031(3) -0.013(2) -0.0028(19) -0.013(2) C225 0.038(3) 0.039(2) 0.025(3) -0.0017(19) -0.010(2) -0.005(2) C226 0.028(2) 0.032(2) 0.032(3) -0.0059(19) -0.0138(19) 0.0038(18) C231 0.027(2) 0.0209(18) 0.027(2) -0.0097(17) -0.0099(17) 0.0069(16) C232 0.039(2) 0.023(2) 0.028(3) -0.0072(18) -0.0079(19) -0.0030(17) C233 0.049(3) 0.029(2) 0.034(3) -0.011(2) -0.013(2) -0.004(2) C234 0.044(3) 0.033(2) 0.034(3) -0.017(2) -0.018(2) 0.012(2) C235 0.046(3) 0.029(2) 0.021(3) -0.0036(18) -0.004(2) 0.0097(19) C236 0.031(2) 0.0221(19) 0.027(3) -0.0069(17) -0.0006(18) 0.0003(16) C01 0.053(4) 0.111(7) 0.148(9) -0.060(6) -0.020(5) -0.006(4) Cl1 0.0903(15) 0.1247(18) 0.1057(18) -0.0279(14) -0.0606(14) 0.0113(13) Cl2 0.0798(13) 0.0955(14) 0.1259(19) -0.0693(14) -0.0293(12) 0.0053(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 P1 2.2764(10) . ? Au1 S1 2.3147(9) . ? Au1 Au2 3.0756(2) . ? S1 C1 1.765(4) . ? P1 C121 1.815(4) . ? P1 C111 1.817(4) . ? P1 C131 1.823(4) . ? O1 C7 1.308(5) . ? O1 H1 0.70(7) . ? O2 C7 1.241(5) . ? C1 C6 1.390(5) . ? C1 C2 1.401(5) . ? C2 C3 1.380(5) . ? C2 H2A 0.9500 . ? C3 C4 1.394(5) . ? C3 H3A 0.9500 . ? C4 C5 1.392(5) . ? C4 C7 1.468(5) . ? C5 C6 1.380(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C111 C112 1.384(6) . ? C111 C116 1.395(5) . ? C112 C113 1.385(6) . ? C112 H11A 0.9500 . ? C113 C114 1.378(6) . ? C113 H11B 0.9500 . ? C114 C115 1.380(6) . ? C114 H11C 0.9500 . ? C115 C116 1.377(6) . ? C115 H11D 0.9500 . ? C116 H11E 0.9500 . ? C121 C122 1.394(5) . ? C121 C126 1.397(6) . ? C122 C123 1.385(6) . ? C122 H12A 0.9500 . ? C123 C124 1.377(6) . ? C123 H12B 0.9500 . ? C124 C125 1.378(6) . ? C124 H12C 0.9500 . ? C125 C126 1.389(6) . ? C125 H12D 0.9500 . ? C126 H12E 0.9500 . ? C131 C136 1.388(6) . ? C131 C132 1.392(6) . ? C132 C133 1.389(7) . ? C132 H13A 0.9500 . ? C133 C134 1.372(8) . ? C133 H13B 0.9500 . ? C134 C135 1.382(8) . ? C134 H13C 0.9500 . ? C135 C136 1.390(6) . ? C135 H13D 0.9500 . ? C136 H13E 0.9500 . ? Au2 P2 2.2624(10) . ? Au2 S2 2.3023(10) . ? S2 C8 1.751(4) . ? P2 C211 1.814(4) . ? P2 C221 1.814(4) . ? P2 C231 1.817(4) . ? O3 C14 1.312(5) . ? O3 H3 0.84(6) . ? O4 C14 1.234(5) . ? C8 C13 1.386(6) . ? C8 C9 1.410(5) . ? C9 C10 1.384(5) . ? C9 H9A 0.9500 . ? C10 C11 1.386(6) . ? C10 H10A 0.9500 . ? C11 C12 1.397(5) . ? C11 C14 1.475(5) . ? C12 C13 1.388(5) . ? C12 H12F 0.9500 . ? C13 H13F 0.9500 . ? C211 C212 1.383(6) . ? C211 C216 1.384(6) . ? C212 C213 1.391(7) . ? C212 H21A 0.9500 . ? C213 C214 1.368(7) . ? C213 H21B 0.9500 . ? C214 C215 1.389(8) . ? C214 H21C 0.9500 . ? C215 C216 1.379(7) . ? C215 H21D 0.9500 . ? C216 H21E 0.9500 . ? C221 C226 1.390(6) . ? C221 C222 1.392(6) . ? C222 C223 1.370(6) . ? C222 H22A 0.9500 . ? C223 C224 1.375(7) . ? C223 H22B 0.9500 . ? C224 C225 1.377(6) . ? C224 H22C 0.9500 . ? C225 C226 1.379(6) . ? C225 H22D 0.9500 . ? C226 H22E 0.9500 . ? C231 C236 1.381(6) . ? C231 C232 1.393(6) . ? C232 C233 1.393(6) . ? C232 H23A 0.9500 . ? C233 C234 1.362(7) . ? C233 H23B 0.9500 . ? C234 C235 1.380(6) . ? C234 H23C 0.9500 . ? C235 C236 1.388(6) . ? C235 H23D 0.9500 . ? C236 H23E 0.9500 . ? C01 Cl1 1.732(9) . ? C01 Cl2 1.797(8) . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 S1 168.95(4) . . ? P1 Au1 Au2 101.69(3) . . ? S1 Au1 Au2 86.91(3) . . ? C1 S1 Au1 108.57(13) . . ? C121 P1 C111 107.17(18) . . ? C121 P1 C131 104.42(18) . . ? C111 P1 C131 104.89(18) . . ? C121 P1 Au1 114.15(13) . . ? C111 P1 Au1 109.86(13) . . ? C131 P1 Au1 115.60(14) . . ? C7 O1 H1 110(6) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 S1 123.7(3) . . ? C2 C1 S1 117.8(3) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 H2A 119.7 . . ? C1 C2 H2A 119.7 . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 119.0(3) . . ? C5 C4 C7 119.5(3) . . ? C3 C4 C7 121.5(4) . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C1 120.9(4) . . ? C5 C6 H6A 119.5 . . ? C1 C6 H6A 119.5 . . ? O2 C7 O1 122.4(4) . . ? O2 C7 C4 122.4(4) . . ? O1 C7 C4 115.2(3) . . ? C112 C111 C116 118.7(4) . . ? C112 C111 P1 123.8(3) . . ? C116 C111 P1 117.5(3) . . ? C111 C112 C113 119.8(4) . . ? C111 C112 H11A 120.1 . . ? C113 C112 H11A 120.1 . . ? C114 C113 C112 120.8(4) . . ? C114 C113 H11B 119.6 . . ? C112 C113 H11B 119.6 . . ? C113 C114 C115 119.9(4) . . ? C113 C114 H11C 120.0 . . ? C115 C114 H11C 120.0 . . ? C116 C115 C114 119.4(4) . . ? C116 C115 H11D 120.3 . . ? C114 C115 H11D 120.3 . . ? C115 C116 C111 121.3(4) . . ? C115 C116 H11E 119.4 . . ? C111 C116 H11E 119.4 . . ? C122 C121 C126 119.7(3) . . ? C122 C121 P1 119.1(3) . . ? C126 C121 P1 121.1(3) . . ? C123 C122 C121 119.6(4) . . ? C123 C122 H12A 120.2 . . ? C121 C122 H12A 120.2 . . ? C124 C123 C122 120.8(4) . . ? C124 C123 H12B 119.6 . . ? C122 C123 H12B 119.6 . . ? C123 C124 C125 119.8(4) . . ? C123 C124 H12C 120.1 . . ? C125 C124 H12C 120.1 . . ? C124 C125 C126 120.7(4) . . ? C124 C125 H12D 119.7 . . ? C126 C125 H12D 119.7 . . ? C125 C126 C121 119.4(4) . . ? C125 C126 H12E 120.3 . . ? C121 C126 H12E 120.3 . . ? C136 C131 C132 119.0(4) . . ? C136 C131 P1 118.9(3) . . ? C132 C131 P1 122.1(4) . . ? C133 C132 C131 119.9(5) . . ? C133 C132 H13A 120.0 . . ? C131 C132 H13A 120.0 . . ? C134 C133 C132 120.5(5) . . ? C134 C133 H13B 119.8 . . ? C132 C133 H13B 119.8 . . ? C133 C134 C135 120.3(5) . . ? C133 C134 H13C 119.8 . . ? C135 C134 H13C 119.8 . . ? C134 C135 C136 119.5(5) . . ? C134 C135 H13D 120.3 . . ? C136 C135 H13D 120.3 . . ? C131 C136 C135 120.8(4) . . ? C131 C136 H13E 119.6 . . ? C135 C136 H13E 119.6 . . ? P2 Au2 S2 174.78(4) . . ? P2 Au2 Au1 105.57(3) . . ? S2 Au2 Au1 76.11(3) . . ? C8 S2 Au2 111.40(14) . . ? C211 P2 C221 106.42(19) . . ? C211 P2 C231 105.11(18) . . ? C221 P2 C231 105.59(18) . . ? C211 P2 Au2 113.01(13) . . ? C221 P2 Au2 110.72(13) . . ? C231 P2 Au2 115.31(13) . . ? C14 O3 H3 109(4) . . ? C13 C8 C9 118.6(3) . . ? C13 C8 S2 125.7(3) . . ? C9 C8 S2 115.7(3) . . ? C10 C9 C8 120.2(4) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C9 C10 C11 120.8(4) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C10 C11 C12 119.2(4) . . ? C10 C11 C14 118.5(3) . . ? C12 C11 C14 122.3(4) . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12F 119.9 . . ? C11 C12 H12F 119.9 . . ? C8 C13 C12 120.9(4) . . ? C8 C13 H13F 119.5 . . ? C12 C13 H13F 119.5 . . ? O4 C14 O3 122.8(4) . . ? O4 C14 C11 121.0(4) . . ? O3 C14 C11 116.2(3) . . ? C212 C211 C216 118.6(4) . . ? C212 C211 P2 119.2(3) . . ? C216 C211 P2 122.1(3) . . ? C211 C212 C213 121.1(5) . . ? C211 C212 H21A 119.4 . . ? C213 C212 H21A 119.4 . . ? C214 C213 C212 119.4(5) . . ? C214 C213 H21B 120.3 . . ? C212 C213 H21B 120.3 . . ? C213 C214 C215 120.2(5) . . ? C213 C214 H21C 119.9 . . ? C215 C214 H21C 119.9 . . ? C216 C215 C214 119.9(5) . . ? C216 C215 H21D 120.0 . . ? C214 C215 H21D 120.0 . . ? C215 C216 C211 120.7(5) . . ? C215 C216 H21E 119.7 . . ? C211 C216 H21E 119.7 . . ? C226 C221 C222 119.0(4) . . ? C226 C221 P2 122.8(3) . . ? C222 C221 P2 118.1(3) . . ? C223 C222 C221 120.3(4) . . ? C223 C222 H22A 119.9 . . ? C221 C222 H22A 119.9 . . ? C222 C223 C224 120.4(4) . . ? C222 C223 H22B 119.8 . . ? C224 C223 H22B 119.8 . . ? C223 C224 C225 120.1(4) . . ? C223 C224 H22C 120.0 . . ? C225 C224 H22C 120.0 . . ? C224 C225 C226 120.1(4) . . ? C224 C225 H22D 120.0 . . ? C226 C225 H22D 120.0 . . ? C225 C226 C221 120.1(4) . . ? C225 C226 H22E 119.9 . . ? C221 C226 H22E 119.9 . . ? C236 C231 C232 119.7(4) . . ? C236 C231 P2 119.0(3) . . ? C232 C231 P2 121.3(3) . . ? C233 C232 C231 119.2(4) . . ? C233 C232 H23A 120.4 . . ? C231 C232 H23A 120.4 . . ? C234 C233 C232 120.9(4) . . ? C234 C233 H23B 119.6 . . ? C232 C233 H23B 119.6 . . ? C233 C234 C235 120.0(4) . . ? C233 C234 H23C 120.0 . . ? C235 C234 H23C 120.0 . . ? C234 C235 C236 120.1(4) . . ? C234 C235 H23D 119.9 . . ? C236 C235 H23D 119.9 . . ? C231 C236 C235 120.0(4) . . ? C231 C236 H23E 120.0 . . ? C235 C236 H23E 120.0 . . ? Cl1 C01 Cl2 112.3(4) . . ? Cl1 C01 H01A 109.1 . . ? Cl2 C01 H01A 109.1 . . ? Cl1 C01 H01B 109.1 . . ? Cl2 C01 H01B 109.1 . . ? H01A C01 H01B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au1 S1 C1 148.7(2) . . . . ? Au2 Au1 S1 C1 -69.80(14) . . . . ? S1 Au1 P1 C121 -132.3(2) . . . . ? Au2 Au1 P1 C121 87.14(14) . . . . ? S1 Au1 P1 C111 -11.9(2) . . . . ? Au2 Au1 P1 C111 -152.46(13) . . . . ? S1 Au1 P1 C131 106.6(2) . . . . ? Au2 Au1 P1 C131 -34.03(15) . . . . ? Au1 S1 C1 C6 -24.9(4) . . . . ? Au1 S1 C1 C2 156.9(3) . . . . ? C6 C1 C2 C3 2.5(6) . . . . ? S1 C1 C2 C3 -179.2(3) . . . . ? C1 C2 C3 C4 -2.1(6) . . . . ? C2 C3 C4 C5 0.2(6) . . . . ? C2 C3 C4 C7 178.5(4) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? C7 C4 C5 C6 -177.0(4) . . . . ? C4 C5 C6 C1 -1.0(6) . . . . ? C2 C1 C6 C5 -1.0(6) . . . . ? S1 C1 C6 C5 -179.2(3) . . . . ? C5 C4 C7 O2 -12.7(6) . . . . ? C3 C4 C7 O2 168.9(4) . . . . ? C5 C4 C7 O1 167.4(3) . . . . ? C3 C4 C7 O1 -11.0(5) . . . . ? C121 P1 C111 C112 -19.0(4) . . . . ? C131 P1 C111 C112 91.6(4) . . . . ? Au1 P1 C111 C112 -143.5(3) . . . . ? C121 P1 C111 C116 162.0(3) . . . . ? C131 P1 C111 C116 -87.4(3) . . . . ? Au1 P1 C111 C116 37.4(3) . . . . ? C116 C111 C112 C113 -1.1(6) . . . . ? P1 C111 C112 C113 179.8(3) . . . . ? C111 C112 C113 C114 1.6(6) . . . . ? C112 C113 C114 C115 -0.1(7) . . . . ? C113 C114 C115 C116 -2.0(7) . . . . ? C114 C115 C116 C111 2.5(7) . . . . ? C112 C111 C116 C115 -0.9(6) . . . . ? P1 C111 C116 C115 178.2(4) . . . . ? C111 P1 C121 C122 -105.7(3) . . . . ? C131 P1 C121 C122 143.4(3) . . . . ? Au1 P1 C121 C122 16.2(4) . . . . ? C111 P1 C121 C126 74.3(4) . . . . ? C131 P1 C121 C126 -36.6(4) . . . . ? Au1 P1 C121 C126 -163.8(3) . . . . ? C126 C121 C122 C123 -0.3(6) . . . . ? P1 C121 C122 C123 179.7(3) . . . . ? C121 C122 C123 C124 -0.4(6) . . . . ? C122 C123 C124 C125 0.9(7) . . . . ? C123 C124 C125 C126 -0.8(7) . . . . ? C124 C125 C126 C121 0.2(7) . . . . ? C122 C121 C126 C125 0.4(6) . . . . ? P1 C121 C126 C125 -179.6(3) . . . . ? C121 P1 C131 C136 -60.9(4) . . . . ? C111 P1 C131 C136 -173.4(3) . . . . ? Au1 P1 C131 C136 65.4(4) . . . . ? C121 P1 C131 C132 120.1(4) . . . . ? C111 P1 C131 C132 7.6(4) . . . . ? Au1 P1 C131 C132 -113.6(4) . . . . ? C136 C131 C132 C133 0.2(8) . . . . ? P1 C131 C132 C133 179.2(4) . . . . ? C131 C132 C133 C134 -0.6(9) . . . . ? C132 C133 C134 C135 0.4(10) . . . . ? C133 C134 C135 C136 0.3(9) . . . . ? C132 C131 C136 C135 0.5(7) . . . . ? P1 C131 C136 C135 -178.6(4) . . . . ? C134 C135 C136 C131 -0.7(8) . . . . ? P1 Au1 Au2 P2 105.08(4) . . . . ? S1 Au1 Au2 P2 -67.92(4) . . . . ? P1 Au1 Au2 S2 -69.81(4) . . . . ? S1 Au1 Au2 S2 117.19(4) . . . . ? P2 Au2 S2 C8 132.4(4) . . . . ? Au1 Au2 S2 C8 -118.09(14) . . . . ? S2 Au2 P2 C211 -17.2(5) . . . . ? Au1 Au2 P2 C211 -125.37(15) . . . . ? S2 Au2 P2 C221 -136.5(4) . . . . ? Au1 Au2 P2 C221 115.35(14) . . . . ? S2 Au2 P2 C231 103.7(4) . . . . ? Au1 Au2 P2 C231 -4.44(15) . . . . ? Au2 S2 C8 C13 -5.3(4) . . . . ? Au2 S2 C8 C9 175.5(3) . . . . ? C13 C8 C9 C10 -0.7(6) . . . . ? S2 C8 C9 C10 178.6(3) . . . . ? C8 C9 C10 C11 0.7(6) . . . . ? C9 C10 C11 C12 -0.4(6) . . . . ? C9 C10 C11 C14 180.0(4) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C14 C11 C12 C13 179.7(4) . . . . ? C9 C8 C13 C12 0.4(6) . . . . ? S2 C8 C13 C12 -178.7(3) . . . . ? C11 C12 C13 C8 -0.2(6) . . . . ? C10 C11 C14 O4 0.9(6) . . . . ? C12 C11 C14 O4 -178.7(4) . . . . ? C10 C11 C14 O3 -178.4(4) . . . . ? C12 C11 C14 O3 2.1(6) . . . . ? C221 P2 C211 C212 78.6(4) . . . . ? C231 P2 C211 C212 -169.7(4) . . . . ? Au2 P2 C211 C212 -43.1(4) . . . . ? C221 P2 C211 C216 -100.2(4) . . . . ? C231 P2 C211 C216 11.5(4) . . . . ? Au2 P2 C211 C216 138.0(4) . . . . ? C216 C211 C212 C213 0.6(8) . . . . ? P2 C211 C212 C213 -178.3(5) . . . . ? C211 C212 C213 C214 -2.2(9) . . . . ? C212 C213 C214 C215 2.4(9) . . . . ? C213 C214 C215 C216 -1.1(9) . . . . ? C214 C215 C216 C211 -0.5(9) . . . . ? C212 C211 C216 C215 0.7(8) . . . . ? P2 C211 C216 C215 179.6(4) . . . . ? C211 P2 C221 C226 4.1(4) . . . . ? C231 P2 C221 C226 -107.3(3) . . . . ? Au2 P2 C221 C226 127.2(3) . . . . ? C211 P2 C221 C222 -175.5(3) . . . . ? C231 P2 C221 C222 73.2(3) . . . . ? Au2 P2 C221 C222 -52.3(3) . . . . ? C226 C221 C222 C223 2.2(6) . . . . ? P2 C221 C222 C223 -178.3(3) . . . . ? C221 C222 C223 C224 -3.0(7) . . . . ? C222 C223 C224 C225 1.4(7) . . . . ? C223 C224 C225 C226 1.1(7) . . . . ? C224 C225 C226 C221 -2.0(7) . . . . ? C222 C221 C226 C225 0.3(6) . . . . ? P2 C221 C226 C225 -179.2(3) . . . . ? C211 P2 C231 C236 84.0(4) . . . . ? C221 P2 C231 C236 -163.7(3) . . . . ? Au2 P2 C231 C236 -41.1(4) . . . . ? C211 P2 C231 C232 -95.2(4) . . . . ? C221 P2 C231 C232 17.1(4) . . . . ? Au2 P2 C231 C232 139.6(3) . . . . ? C236 C231 C232 C233 1.7(6) . . . . ? P2 C231 C232 C233 -179.1(3) . . . . ? C231 C232 C233 C234 -0.5(7) . . . . ? C232 C233 C234 C235 -0.7(7) . . . . ? C233 C234 C235 C236 0.8(7) . . . . ? C232 C231 C236 C235 -1.6(6) . . . . ? P2 C231 C236 C235 179.1(3) . . . . ? C234 C235 C236 C231 0.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.31 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 1.255 _refine_diff_density_min -1.165 _refine_diff_density_rms 0.106 data_jam12 _database_code_CSD 155656 _audit_creation_method SHELXL-97 _chemical_name_systematic ; [4-Carboxyl-thiophenolato-gold(I)-triethylphosphane]-Dimer ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H20 Au O2 P S' _chemical_formula_weight 468.29 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.2190(1) _cell_length_b 14.0220(1) _cell_length_c 15.4040(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.094(5) _cell_angle_gamma 90.00 _cell_volume 1556.99(3) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 4807 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31.5 _exptl_crystal_description Block _exptl_crystal_colour Yellowish _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.998 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 9.677 _exptl_absorpt_correction_type 'DELABS from PLATON' _exptl_absorpt_correction_T_min 0.468 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'Nonius DIP 2020' _diffrn_measurement_method 'Phi scans 2.0 deg' _diffrn_detector_area_resol_mean '8 - 0.68' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 26047 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 31.53 _reflns_number_total 4807 _reflns_number_gt 4539 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius-DIP 2020 Software' _computing_cell_refinement 'SCALEPACK' _computing_data_reduction 'SCALEPACK, DIPSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0145P)^2^+5.4986P] 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 ride _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4807 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0717 _refine_ls_wR_factor_gt 0.0704 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _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 Au Au 0.931801(19) 0.600323(10) 0.065459(8) 0.02031(5) Uani 1 1 d . . . P P 1.12587(14) 0.62623(8) 0.18382(6) 0.02196(19) Uani 1 1 d . . . S S 0.72003(14) 0.57845(8) -0.05093(7) 0.0257(2) Uani 1 1 d . . . O1 O 0.2253(4) 0.9771(2) 0.0134(2) 0.0322(7) Uani 1 1 d . . . O2 O 0.0006(4) 0.8845(2) -0.0463(2) 0.0286(6) Uani 1 1 d . . . H2D H -0.0644 0.9317 -0.0338 0.043 Uiso 1 1 calc R . . C1 C 1.0491(7) 0.7260(3) 0.2488(3) 0.0318(9) Uani 1 1 d . . . H1A H 0.9329 0.7078 0.2758 0.038 Uiso 1 1 calc R . . H1B H 1.1440 0.7386 0.2962 0.038 Uiso 1 1 calc R . . C2 C 1.0150(9) 0.8178(4) 0.1966(3) 0.0444(12) Uani 1 1 d . . . H2A H 0.9744 0.8683 0.2352 0.067 Uiso 1 1 calc R . . H2B H 0.9188 0.8065 0.1504 0.067 Uiso 1 1 calc R . . H2C H 1.1301 0.8373 0.1707 0.067 Uiso 1 1 calc R . . C3 C 1.3617(6) 0.6550(3) 0.1572(3) 0.0283(8) Uani 1 1 d . . . H3A H 1.4114 0.6005 0.1249 0.034 Uiso 1 1 calc R . . H3B H 1.3568 0.7105 0.1175 0.034 Uiso 1 1 calc R . . C4 C 1.4981(8) 0.6778(6) 0.2334(4) 0.0585(18) Uani 1 1 d . . . H4A H 1.6199 0.6922 0.2115 0.088 Uiso 1 1 calc R . . H4B H 1.5086 0.6227 0.2725 0.088 Uiso 1 1 calc R . . H4C H 1.4535 0.7330 0.2651 0.088 Uiso 1 1 calc R . . C5 C 1.1443(7) 0.5278(4) 0.2604(3) 0.0333(10) Uani 1 1 d . . . H5A H 1.2237 0.4777 0.2366 0.040 Uiso 1 1 calc R . . H5B H 1.2063 0.5508 0.3154 0.040 Uiso 1 1 calc R . . C6 C 0.9578(9) 0.4840(4) 0.2803(4) 0.0480(14) Uani 1 1 d . . . H6A H 0.9777 0.4314 0.3216 0.072 Uiso 1 1 calc R . . H6B H 0.8965 0.4598 0.2264 0.072 Uiso 1 1 calc R . . H6C H 0.8795 0.5326 0.3055 0.072 Uiso 1 1 calc R . . C11 C 0.5615(5) 0.6731(3) -0.0428(2) 0.0179(6) Uani 1 1 d . . . C12 C 0.6184(5) 0.7638(3) -0.0136(2) 0.0207(7) Uani 1 1 d . . . H12A H 0.7454 0.7749 0.0027 0.025 Uiso 1 1 calc R . . C13 C 0.4918(5) 0.8371(3) -0.0081(2) 0.0212(7) Uani 1 1 d . . . H13A H 0.5321 0.8980 0.0123 0.025 Uiso 1 1 calc R . . C14 C 0.3047(5) 0.8223(3) -0.0325(2) 0.0197(7) Uani 1 1 d . . . C15 C 0.2476(5) 0.7326(3) -0.0641(2) 0.0204(7) Uani 1 1 d . . . H15A H 0.1212 0.7222 -0.0820 0.024 Uiso 1 1 calc R . . C16 C 0.3750(5) 0.6589(3) -0.0693(2) 0.0190(6) Uani 1 1 d . . . H16A H 0.3354 0.5984 -0.0910 0.023 Uiso 1 1 calc R . . C17 C 0.1716(5) 0.9001(3) -0.0213(2) 0.0215(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.02016(8) 0.02046(9) 0.02022(8) 0.00040(4) 0.00009(5) 0.00201(5) P 0.0220(5) 0.0266(5) 0.0174(4) 0.0002(3) 0.0017(3) 0.0015(4) S 0.0253(5) 0.0226(5) 0.0286(5) -0.0077(4) -0.0050(4) 0.0063(4) O1 0.0260(15) 0.0191(16) 0.0514(19) -0.0100(13) -0.0001(13) 0.0010(11) O2 0.0199(14) 0.0243(16) 0.0412(17) -0.0050(12) -0.0022(12) 0.0042(11) C1 0.035(2) 0.035(3) 0.0260(19) -0.0082(16) 0.0064(16) 0.0027(17) C2 0.060(4) 0.032(3) 0.042(3) -0.010(2) 0.006(2) 0.003(2) C3 0.0242(19) 0.038(3) 0.0229(18) -0.0030(15) 0.0021(14) -0.0019(16) C4 0.032(3) 0.106(6) 0.036(3) -0.003(3) -0.009(2) -0.016(3) C5 0.042(3) 0.036(3) 0.0218(18) 0.0066(16) 0.0011(17) 0.0049(19) C6 0.056(3) 0.049(4) 0.040(3) 0.014(2) 0.007(2) -0.013(3) C11 0.0207(16) 0.0160(18) 0.0168(14) 0.0001(11) 0.0001(12) 0.0044(12) C12 0.0180(16) 0.0209(19) 0.0234(16) 0.0009(13) 0.0014(13) -0.0015(13) C13 0.0211(17) 0.0169(19) 0.0257(17) -0.0011(13) 0.0009(13) -0.0023(13) C14 0.0219(17) 0.0172(18) 0.0200(15) 0.0020(12) 0.0009(12) 0.0018(12) C15 0.0212(17) 0.0204(19) 0.0194(15) 0.0008(12) -0.0014(12) -0.0036(13) C16 0.0205(16) 0.0170(18) 0.0194(15) 0.0003(12) 0.0000(12) -0.0013(12) C17 0.0197(17) 0.023(2) 0.0223(16) 0.0026(13) 0.0017(13) -0.0002(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au P 2.2679(10) . ? Au S 2.3130(10) . ? P C5 1.816(4) . ? P C3 1.817(4) . ? P C1 1.824(4) . ? S C11 1.761(4) . ? O1 C17 1.256(5) . ? O2 C17 1.292(5) . ? O2 H2D 0.8400 . ? C1 C2 1.530(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.524(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.526(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C16 1.400(5) . ? C11 C12 1.404(5) . ? C12 C13 1.381(5) . ? C12 H12A 0.9500 . ? C13 C14 1.397(5) . ? C13 H13A 0.9500 . ? C14 C15 1.403(5) . ? C14 C17 1.470(5) . ? C15 C16 1.389(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? 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 P Au S 176.57(4) . . ? C5 P C3 106.2(2) . . ? C5 P C1 103.9(2) . . ? C3 P C1 105.6(2) . . ? C5 P Au 114.91(17) . . ? C3 P Au 113.56(13) . . ? C1 P Au 111.78(16) . . ? C11 S Au 104.46(12) . . ? C17 O2 H2D 109.5 . . ? C2 C1 P 113.7(3) . . ? C2 C1 H1A 108.8 . . ? P C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 P 116.6(3) . . ? C4 C3 H3A 108.2 . . ? P C3 H3A 108.2 . . ? C4 C3 H3B 108.2 . . ? P C3 H3B 108.2 . . ? H3A C3 H3B 107.3 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 P 113.7(4) . . ? C6 C5 H5A 108.8 . . ? P C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? P C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C16 C11 C12 118.9(3) . . ? C16 C11 S 119.4(3) . . ? C12 C11 S 121.7(3) . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C14 120.4(3) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C13 C14 C15 119.2(3) . . ? C13 C14 C17 119.1(3) . . ? C15 C14 C17 121.6(3) . . ? C16 C15 C14 120.3(3) . . ? C16 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C15 C16 C11 120.4(3) . . ? C15 C16 H16A 119.8 . . ? C11 C16 H16A 119.8 . . ? O1 C17 O2 122.7(4) . . ? O1 C17 C14 119.9(4) . . ? O2 C17 C14 117.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S Au P C5 95.0(7) . . . . ? S Au P C3 -142.5(7) . . . . ? S Au P C1 -23.1(7) . . . . ? P Au S C11 27.1(7) . . . . ? C5 P C1 C2 -177.5(4) . . . . ? C3 P C1 C2 71.0(4) . . . . ? Au P C1 C2 -53.0(4) . . . . ? C5 P C3 C4 -55.4(5) . . . . ? C1 P C3 C4 54.5(5) . . . . ? Au P C3 C4 177.3(4) . . . . ? C3 P C5 C6 -171.5(4) . . . . ? C1 P C5 C6 77.3(4) . . . . ? Au P C5 C6 -45.1(4) . . . . ? Au S C11 C16 -147.0(3) . . . . ? Au S C11 C12 35.6(3) . . . . ? C16 C11 C12 C13 2.2(5) . . . . ? S C11 C12 C13 179.7(3) . . . . ? C11 C12 C13 C14 -0.6(6) . . . . ? C12 C13 C14 C15 -1.2(5) . . . . ? C12 C13 C14 C17 176.6(3) . . . . ? C13 C14 C15 C16 1.4(5) . . . . ? C17 C14 C15 C16 -176.3(3) . . . . ? C14 C15 C16 C11 0.3(5) . . . . ? C12 C11 C16 C15 -2.0(5) . . . . ? S C11 C16 C15 -179.6(3) . . . . ? C13 C14 C17 O1 -3.2(5) . . . . ? C15 C14 C17 O1 174.5(4) . . . . ? C13 C14 C17 O2 178.5(4) . . . . ? C15 C14 C17 O2 -3.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 31.53 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.739 _refine_diff_density_min -1.413 _refine_diff_density_rms 0.174