# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lang, Jian-Ping' _publ_contact_author_email jplang@suda.edu.cn _publ_section_title ; Reactions of a gold(I) thiolate complex [Au(Tab)2]2(PF6)2 (Tab = 4-(trimethylammonio)benzenethiolate) with diphosphine ligands ; loop_ _publ_author_name 'Ai-Xia Zheng' 'Zhi-Gang Ren' 'Ling-Ling Li' 'Hai Shang' 'Hong-Xi Li' ; Jian-Ping Lang ; # Attachment '- JPLangCIF (re-revised).cif' #============================================================================== data_1^.^2MeOH _database_code_depnum_ccdc_archive 'CCDC 779817' #TrackingRef '- JPLangCIF (re-revised).cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C44 H50 Au2 N2 P2 S2), 4(F6 P), 2(C H4 O)' _chemical_formula_sum 'C90 H108 Au4 F24 N4 O2 P8 S4' _chemical_formula_weight 2897.72 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' 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' F F 0.0171 0.0103 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.318(3) _cell_length_b 20.583(4) _cell_length_c 20.796(4) _cell_angle_alpha 81.10(3) _cell_angle_beta 70.71(3) _cell_angle_gamma 81.21(3) _cell_volume 5681(2) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 18381 _cell_measurement_theta_min 3.0178 _cell_measurement_theta_max 27.4623 _exptl_crystal_description club _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 5.418 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2205 _exptl_absorpt_correction_T_max 0.4104 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39095 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0938 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 19635 _reflns_number_gt 15373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0761P)^2^+17.3506P] 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 19635 _refine_ls_number_parameters 1052 _refine_ls_number_restraints 103 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.2021 _refine_ls_wR_factor_gt 0.1879 _refine_ls_goodness_of_fit_ref 1.159 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.006 _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 -0.19021(4) 0.70733(3) 0.22085(3) 0.04704(16) Uani 1 1 d . . . Au2 Au 0.19187(4) 0.56056(3) 0.31349(4) 0.0631(2) Uani 1 1 d . . . Au3 Au 0.18259(4) 0.66645(2) 0.40563(3) 0.04160(15) Uani 1 1 d . A . Au4 Au 0.69666(4) 0.58592(3) 0.28677(3) 0.04067(14) Uani 1 1 d . . . S1 S -0.3154(3) 0.74918(17) 0.31353(18) 0.0467(8) Uani 1 1 d . A . S2 S 0.1756(3) 0.5062(2) 0.4214(2) 0.0711(12) Uani 1 1 d . A . S3 S 0.0191(2) 0.67133(17) 0.4067(2) 0.0507(9) Uani 1 1 d . . . S4 S 0.8198(3) 0.58299(19) 0.3371(2) 0.0511(9) Uani 1 1 d . . . N2 N 1.0038(10) 0.2993(7) 0.3672(7) 0.067(4) Uani 1 1 d . . . N3 N -0.1255(9) 0.9615(6) 0.3513(6) 0.052(3) Uani 1 1 d . A . N4 N 0.3817(9) 0.2275(6) 0.4297(6) 0.049(3) Uani 1 1 d . . . C1 C -0.3583(10) 0.8283(7) 0.2855(7) 0.049(3) Uani 1 1 d . . . C2 C -0.4406(14) 0.8632(9) 0.3306(10) 0.082(6) Uani 1 1 d . A . H2 H -0.4709 0.8420 0.3744 0.098 Uiso 1 1 calc R . . C3 C -0.4780(12) 0.9259(8) 0.3137(8) 0.070(5) Uani 1 1 d . . . H3 H -0.5334 0.9464 0.3456 0.083 Uiso 1 1 calc R A . C4 C -0.4367(12) 0.9594(7) 0.2515(8) 0.059(4) Uani 1 1 d . A . C5 C -0.3534(14) 0.9277(10) 0.2039(9) 0.095(7) Uani 1 1 d . . . H5 H -0.3221 0.9495 0.1605 0.114 Uiso 1 1 calc R A . C6 C -0.3197(13) 0.8633(8) 0.2235(8) 0.078(6) Uani 1 1 d . A . H6 H -0.2657 0.8421 0.1913 0.094 Uiso 1 1 calc R . . C10 C 0.8747(11) 0.5007(8) 0.3412(8) 0.059(3) Uani 1 1 d U . . C11 C 0.9352(11) 0.4812(8) 0.3845(8) 0.059(3) Uani 1 1 d U . . H11 H 0.9460 0.5129 0.4086 0.071 Uiso 1 1 calc R . . C12 C 0.9794(11) 0.4158(8) 0.3922(9) 0.066(4) Uani 1 1 d U . . H12 H 1.0200 0.4037 0.4205 0.079 Uiso 1 1 calc R . . C13 C 0.9617(11) 0.3697(8) 0.3570(9) 0.063(4) Uani 1 1 d U . . C14 C 0.9023(14) 0.3883(9) 0.3174(10) 0.085(4) Uani 1 1 d U . . H14 H 0.8885 0.3560 0.2953 0.102 Uiso 1 1 calc R . . C15 C 0.8605(13) 0.4530(8) 0.3078(9) 0.077(4) Uani 1 1 d U . . H15 H 0.8221 0.4640 0.2779 0.093 Uiso 1 1 calc R . . C16 C 1.0433(17) 0.2704(10) 0.3000(10) 0.114(9) Uani 1 1 d . . . H16A H 1.0720 0.3041 0.2637 0.171 Uiso 1 1 calc R . . H16B H 0.9895 0.2544 0.2905 0.171 Uiso 1 1 calc R . . H16C H 1.0941 0.2339 0.3025 0.171 Uiso 1 1 calc R . . C17 C 0.9205(13) 0.2573(9) 0.4105(10) 0.084(6) Uani 1 1 d . . . H17A H 0.8916 0.2723 0.4557 0.125 Uiso 1 1 calc R . . H17B H 0.9476 0.2113 0.4149 0.125 Uiso 1 1 calc R . . H17C H 0.8695 0.2617 0.3884 0.125 Uiso 1 1 calc R . . C18 C 1.0787(13) 0.2917(8) 0.4041(11) 0.086(6) Uani 1 1 d . . . H18A H 1.1381 0.3110 0.3745 0.130 Uiso 1 1 calc R . . H18B H 1.0957 0.2451 0.4167 0.130 Uiso 1 1 calc R . . H18C H 1.0512 0.3141 0.4451 0.130 Uiso 1 1 calc R . . C19 C -0.0185(9) 0.7563(6) 0.3921(7) 0.041(3) Uani 1 1 d . A . C20 C -0.0991(9) 0.7734(7) 0.3646(7) 0.048(3) Uani 1 1 d . . . H20 H -0.1303 0.7401 0.3562 0.058 Uiso 1 1 calc R A . C21 C -0.1315(10) 0.8401(7) 0.3502(7) 0.052(4) Uani 1 1 d . A . H21 H -0.1814 0.8515 0.3290 0.062 Uiso 1 1 calc R . . C22 C -0.0905(10) 0.8902(7) 0.3670(6) 0.047(3) Uani 1 1 d . . . C23 C -0.0154(9) 0.8734(7) 0.3962(7) 0.049(3) Uani 1 1 d . A . H23 H 0.0116 0.9067 0.4084 0.058 Uiso 1 1 calc R . . C24 C 0.0208(10) 0.8074(7) 0.4080(8) 0.052(4) Uani 1 1 d . . . H24 H 0.0731 0.7970 0.4270 0.062 Uiso 1 1 calc R A . C25 C -0.0427(13) 0.9942(8) 0.2973(9) 0.077(5) Uani 1 1 d . . . H25A H -0.0136 0.9668 0.2601 0.115 Uiso 1 1 calc R A . H25B H 0.0079 0.9997 0.3171 0.115 Uiso 1 1 calc R . . H25C H -0.0688 1.0371 0.2800 0.115 Uiso 1 1 calc R . . C26 C -0.1538(14) 0.9971(8) 0.4144(9) 0.078(5) Uani 1 1 d . . . H26A H -0.1731 1.0436 0.4029 0.117 Uiso 1 1 calc R A . H26B H -0.0974 0.9926 0.4314 0.117 Uiso 1 1 calc R . . H26C H -0.2092 0.9779 0.4495 0.117 Uiso 1 1 calc R . . C27 C -0.2118(13) 0.9726(8) 0.3261(11) 0.089(6) Uani 1 1 d . . . H27A H -0.1988 0.9468 0.2881 0.134 Uiso 1 1 calc R A . H27B H -0.2234 1.0192 0.3106 0.134 Uiso 1 1 calc R . . H27C H -0.2701 0.9591 0.3627 0.134 Uiso 1 1 calc R . . C28 C 0.2367(10) 0.4242(7) 0.4182(7) 0.049(3) Uani 1 1 d . . . C29 C 0.2999(14) 0.3982(8) 0.3602(8) 0.069(5) Uani 1 1 d . A . H29 H 0.3122 0.4242 0.3175 0.083 Uiso 1 1 calc R . . C30 C 0.3445(13) 0.3355(7) 0.3639(8) 0.073(5) Uani 1 1 d . . . H30 H 0.3874 0.3190 0.3234 0.087 Uiso 1 1 calc R A . C31 C 0.3298(10) 0.2953(7) 0.4238(8) 0.050(3) Uani 1 1 d . A . C32 C 0.2653(11) 0.3213(8) 0.4818(8) 0.060(4) Uani 1 1 d . . . H32 H 0.2532 0.2949 0.5242 0.072 Uiso 1 1 calc R A . C33 C 0.2186(10) 0.3843(8) 0.4793(8) 0.061(4) Uani 1 1 d . A . H33 H 0.1741 0.4003 0.5195 0.073 Uiso 1 1 calc R . . C7 C -0.562(4) 1.053(3) 0.289(2) 0.089(5) Uiso 0.427(6) 1 d P A 1 H7A H -0.5399 1.0644 0.3249 0.134 Uiso 0.427(6) 1 calc PR A 1 H7B H -0.6058 1.0181 0.3084 0.134 Uiso 0.427(6) 1 calc PR A 1 H7C H -0.5988 1.0916 0.2721 0.134 Uiso 0.427(6) 1 calc PR A 1 C8 C -0.507(4) 1.027(3) 0.171(2) 0.089(5) Uiso 0.427(6) 1 d P A 1 H8A H -0.5020 1.0700 0.1438 0.134 Uiso 0.427(6) 1 calc PR A 1 H8B H -0.5749 1.0167 0.1860 0.134 Uiso 0.427(6) 1 calc PR A 1 H8C H -0.4634 0.9936 0.1442 0.134 Uiso 0.427(6) 1 calc PR A 1 C9 C -0.400(4) 1.075(3) 0.234(3) 0.089(5) Uiso 0.427(6) 1 d P A 1 H9A H -0.3890 1.1077 0.1936 0.134 Uiso 0.427(6) 1 calc PR A 1 H9B H -0.3377 1.0491 0.2336 0.134 Uiso 0.427(6) 1 calc PR A 1 H9C H -0.4263 1.0979 0.2748 0.134 Uiso 0.427(6) 1 calc PR A 1 C34 C 0.328(3) 0.185(2) 0.411(2) 0.081(5) Uiso 0.427(6) 1 d P A 1 H34A H 0.3337 0.1414 0.4354 0.121 Uiso 0.427(6) 1 calc PR A 1 H34B H 0.3559 0.1820 0.3617 0.121 Uiso 0.427(6) 1 calc PR A 1 H34C H 0.2588 0.2029 0.4216 0.121 Uiso 0.427(6) 1 calc PR A 1 C35 C 0.399(3) 0.210(2) 0.502(2) 0.081(5) Uiso 0.427(6) 1 d P A 1 H35A H 0.4396 0.1672 0.5026 0.121 Uiso 0.427(6) 1 calc PR A 1 H35B H 0.3355 0.2069 0.5375 0.121 Uiso 0.427(6) 1 calc PR A 1 H35C H 0.4332 0.2435 0.5095 0.121 Uiso 0.427(6) 1 calc PR A 1 C36 C 0.490(3) 0.226(2) 0.376(2) 0.081(5) Uiso 0.427(6) 1 d P A 1 H36A H 0.5284 0.2549 0.3876 0.121 Uiso 0.427(6) 1 calc PR A 1 H36B H 0.4859 0.2411 0.3303 0.121 Uiso 0.427(6) 1 calc PR A 1 H36C H 0.5232 0.1812 0.3766 0.121 Uiso 0.427(6) 1 calc PR A 1 C89 C 0.124(4) 0.429(3) 0.188(3) 0.098(15) Uiso 0.427(6) 1 d P A 1 O1 O 0.117(4) 0.381(3) 0.137(3) 0.19(2) Uiso 0.427(6) 1 d P A 1 P1 P -0.0724(9) 0.6540(6) 0.1408(6) 0.0520(9) Uiso 0.427(6) 1 d P A 1 P2 P 0.1972(8) 0.6377(6) 0.2079(5) 0.0520(9) Uiso 0.427(6) 1 d P A 1 C85 C 0.033(3) 0.6095(17) 0.1771(18) 0.0520(9) Uiso 0.427(6) 1 d P A 1 H85A H 0.0067 0.5789 0.2181 0.062 Uiso 0.427(6) 1 calc PR A 1 H85B H 0.0851 0.5852 0.1427 0.062 Uiso 0.427(6) 1 calc PR A 1 C86 C 0.074(2) 0.6694(18) 0.1948(18) 0.0520(9) Uiso 0.427(6) 1 d P A 1 H86A H 0.0270 0.6862 0.2366 0.062 Uiso 0.427(6) 1 calc PR A 1 H86B H 0.0817 0.7053 0.1572 0.062 Uiso 0.427(6) 1 calc PR A 1 C37 C -0.0180(16) 0.7107(10) 0.0656(9) 0.0520(9) Uiso 0.427(6) 1 d PG A 1 C38 C -0.0464(14) 0.7784(10) 0.0588(9) 0.0520(9) Uiso 0.427(6) 1 d PG A 1 H38 H -0.0962 0.7980 0.0947 0.062 Uiso 0.427(6) 1 calc PR A 1 C39 C -0.0012(16) 0.8172(8) -0.0013(11) 0.0520(9) Uiso 0.427(6) 1 d PG A 1 H39 H -0.0204 0.8630 -0.0060 0.062 Uiso 0.427(6) 1 calc PR A 1 C40 C 0.0724(15) 0.7882(9) -0.0545(9) 0.0520(9) Uiso 0.427(6) 1 d PG A 1 H40 H 0.1030 0.8145 -0.0952 0.062 Uiso 0.427(6) 1 calc PR A 1 C41 C 0.1009(14) 0.7205(10) -0.0477(9) 0.0520(9) Uiso 0.427(6) 1 d PG A 1 H41 H 0.1507 0.7010 -0.0837 0.062 Uiso 0.427(6) 1 calc PR A 1 C42 C 0.0557(16) 0.6818(8) 0.0124(11) 0.0520(9) Uiso 0.427(6) 1 d PG A 1 H42 H 0.0749 0.6360 0.0171 0.062 Uiso 0.427(6) 1 calc PR A 1 C43 C -0.111(3) 0.5905(17) 0.1088(19) 0.105(4) Uiso 0.427(6) 1 d PG A 1 C44 C -0.092(3) 0.525(2) 0.1344(16) 0.105(4) Uiso 0.427(6) 1 d PG A 1 H44 H -0.0611 0.5151 0.1685 0.126 Uiso 0.427(6) 1 calc PR A 1 C45 C -0.120(3) 0.4744(14) 0.1095(17) 0.105(4) Uiso 0.427(6) 1 d PG A 1 H45 H -0.1068 0.4302 0.1267 0.126 Uiso 0.427(6) 1 calc PR A 1 C46 C -0.166(3) 0.4892(17) 0.0589(18) 0.105(4) Uiso 0.427(6) 1 d PG A 1 H46 H -0.1842 0.4550 0.0421 0.126 Uiso 0.427(6) 1 calc PR A 1 C47 C -0.185(2) 0.5547(19) 0.0334(15) 0.105(4) Uiso 0.427(6) 1 d PG A 1 H47 H -0.2160 0.5647 -0.0008 0.126 Uiso 0.427(6) 1 calc PR A 1 C48 C -0.158(3) 0.6053(14) 0.0583(19) 0.105(4) Uiso 0.427(6) 1 d PG A 1 H48 H -0.1704 0.6495 0.0410 0.126 Uiso 0.427(6) 1 calc PR A 1 C49 C 0.2366(18) 0.7165(10) 0.2065(13) 0.054(9) Uiso 0.427(6) 1 d PG A 1 C50 C 0.1641(14) 0.7671(13) 0.2327(13) 0.058(9) Uiso 0.427(6) 1 d PG A 1 H50 H 0.0972 0.7588 0.2527 0.069 Uiso 0.427(6) 1 calc PR A 1 C51 C 0.1904(18) 0.8301(11) 0.2295(15) 0.077(12) Uiso 0.427(6) 1 d PG A 1 H51 H 0.1413 0.8643 0.2472 0.092 Uiso 0.427(6) 1 calc PR A 1 C52 C 0.289(2) 0.8425(10) 0.2000(15) 0.071(11) Uiso 0.427(6) 1 d PG A 1 H52 H 0.3070 0.8851 0.1978 0.085 Uiso 0.427(6) 1 calc PR A 1 C53 C 0.3618(15) 0.7919(13) 0.1737(14) 0.060(9) Uiso 0.427(6) 1 d PG A 1 H53 H 0.4286 0.8003 0.1538 0.072 Uiso 0.427(6) 1 calc PR A 1 C54 C 0.3355(16) 0.7289(11) 0.1770(14) 0.052(9) Uiso 0.427(6) 1 d PG A 1 H54 H 0.3845 0.6947 0.1592 0.063 Uiso 0.427(6) 1 calc PR A 1 C55 C 0.273(2) 0.6042(14) 0.1271(11) 0.076(3) Uiso 0.427(6) 1 d PG A 1 C56 C 0.297(2) 0.6490(11) 0.0684(14) 0.076(3) Uiso 0.427(6) 1 d PG A 1 H56 H 0.2786 0.6945 0.0714 0.091 Uiso 0.427(6) 1 calc PR A 1 C57 C 0.350(2) 0.6265(13) 0.0052(11) 0.076(3) Uiso 0.427(6) 1 d PG A 1 H57 H 0.3662 0.6569 -0.0345 0.091 Uiso 0.427(6) 1 calc PR A 1 C58 C 0.377(2) 0.5593(14) 0.0008(11) 0.076(3) Uiso 0.427(6) 1 d PG A 1 H58 H 0.4127 0.5441 -0.0420 0.091 Uiso 0.427(6) 1 calc PR A 1 C59 C 0.353(2) 0.5144(11) 0.0595(14) 0.076(3) Uiso 0.427(6) 1 d PG A 1 H59 H 0.3717 0.4689 0.0564 0.091 Uiso 0.427(6) 1 calc PR A 1 C60 C 0.301(2) 0.5369(13) 0.1226(11) 0.076(3) Uiso 0.427(6) 1 d PG A 1 H60 H 0.2841 0.5066 0.1623 0.091 Uiso 0.427(6) 1 calc PR A 1 C7' C -0.589(3) 1.0368(19) 0.2604(19) 0.089(5) Uiso 0.573(6) 1 d P A 2 H7'1 H -0.6109 1.0067 0.3019 0.134 Uiso 0.573(6) 1 calc PR A 2 H7'2 H -0.6156 1.0264 0.2262 0.134 Uiso 0.573(6) 1 calc PR A 2 H7'3 H -0.6138 1.0819 0.2705 0.134 Uiso 0.573(6) 1 calc PR A 2 C8' C -0.448(3) 1.0472(19) 0.1552(17) 0.089(5) Uiso 0.573(6) 1 d P A 2 H8'1 H -0.4756 1.0920 0.1450 0.134 Uiso 0.573(6) 1 calc PR A 2 H8'2 H -0.4740 1.0168 0.1360 0.134 Uiso 0.573(6) 1 calc PR A 2 H8'3 H -0.3758 1.0437 0.1354 0.134 Uiso 0.573(6) 1 calc PR A 2 C9' C -0.432(3) 1.074(2) 0.2616(19) 0.089(5) Uiso 0.573(6) 1 d P A 2 H9'1 H -0.4231 1.1155 0.2319 0.134 Uiso 0.573(6) 1 calc PR A 2 H9'2 H -0.3680 1.0533 0.2650 0.134 Uiso 0.573(6) 1 calc PR A 2 H9'3 H -0.4763 1.0827 0.3069 0.134 Uiso 0.573(6) 1 calc PR A 2 O1' O 0.302(6) 0.788(4) -0.074(4) 0.36(4) Uiso 0.573(6) 1 d P A 2 C89' C 0.251(6) 0.792(4) 0.002(4) 0.23(3) Uiso 0.573(6) 1 d P A 2 C34' C 0.307(2) 0.1774(17) 0.4603(17) 0.081(5) Uiso 0.573(6) 1 d P A 2 H34D H 0.3408 0.1331 0.4552 0.121 Uiso 0.573(6) 1 calc PR A 2 H34E H 0.2573 0.1851 0.4367 0.121 Uiso 0.573(6) 1 calc PR A 2 H34F H 0.2745 0.1821 0.5086 0.121 Uiso 0.573(6) 1 calc PR A 2 C35' C 0.452(3) 0.2209(18) 0.4640(17) 0.081(5) Uiso 0.573(6) 1 d P A 2 H35D H 0.4180 0.2254 0.5122 0.121 Uiso 0.573(6) 1 calc PR A 2 H35E H 0.4963 0.2549 0.4445 0.121 Uiso 0.573(6) 1 calc PR A 2 H35F H 0.4897 0.1776 0.4594 0.121 Uiso 0.573(6) 1 calc PR A 2 C36' C 0.436(3) 0.2010(17) 0.3614(16) 0.081(5) Uiso 0.573(6) 1 d P A 2 H36D H 0.4824 0.2314 0.3328 0.121 Uiso 0.573(6) 1 calc PR A 2 H36E H 0.3879 0.1967 0.3389 0.121 Uiso 0.573(6) 1 calc PR A 2 H36F H 0.4717 0.1581 0.3690 0.121 Uiso 0.573(6) 1 calc PR A 2 P1' P -0.0643(7) 0.6706(4) 0.1272(4) 0.0520(9) Uiso 0.573(6) 1 d P A 2 P2' P 0.1832(6) 0.6116(4) 0.2193(4) 0.0520(9) Uiso 0.573(6) 1 d P A 2 C85' C 0.0569(18) 0.6545(13) 0.1403(12) 0.0520(9) Uiso 0.573(6) 1 d P A 2 H85C H 0.1010 0.6276 0.1048 0.062 Uiso 0.573(6) 1 calc PR A 2 H85D H 0.0842 0.6969 0.1328 0.062 Uiso 0.573(6) 1 calc PR A 2 C86' C 0.0613(18) 0.6197(13) 0.2101(13) 0.0520(9) Uiso 0.573(6) 1 d P A 2 H86C H 0.0397 0.5756 0.2165 0.062 Uiso 0.573(6) 1 calc PR A 2 H86D H 0.0144 0.6447 0.2462 0.062 Uiso 0.573(6) 1 calc PR A 2 C37' C -0.0506(12) 0.7187(7) 0.0469(6) 0.0520(9) Uiso 0.573(6) 1 d PG A 2 C38' C -0.0914(11) 0.7845(8) 0.0460(6) 0.0520(9) Uiso 0.573(6) 1 d PG A 2 H38' H -0.1362 0.8002 0.0863 0.062 Uiso 0.573(6) 1 calc PR A 2 C39' C -0.0661(12) 0.8270(6) -0.0145(8) 0.0520(9) Uiso 0.573(6) 1 d PG A 2 H39' H -0.0938 0.8714 -0.0150 0.062 Uiso 0.573(6) 1 calc PR A 2 C40' C 0.0000(12) 0.8037(7) -0.0740(6) 0.0520(9) Uiso 0.573(6) 1 d PG A 2 H40' H 0.0171 0.8324 -0.1149 0.062 Uiso 0.573(6) 1 calc PR A 2 C41' C 0.0409(11) 0.7379(8) -0.0732(6) 0.0520(9) Uiso 0.573(6) 1 d PG A 2 H41' H 0.0856 0.7222 -0.1135 0.062 Uiso 0.573(6) 1 calc PR A 2 C42' C 0.0156(12) 0.6955(6) -0.0127(8) 0.0520(9) Uiso 0.573(6) 1 d PG A 2 H42' H 0.0432 0.6510 -0.0122 0.062 Uiso 0.573(6) 1 calc PR A 2 C43' C -0.084(2) 0.5855(12) 0.1117(14) 0.105(4) Uiso 0.573(6) 1 d PG A 2 C44' C -0.0223(17) 0.5267(15) 0.1155(12) 0.105(4) Uiso 0.573(6) 1 d PG A 2 H44' H 0.0341 0.5258 0.1295 0.126 Uiso 0.573(6) 1 calc PR A 2 C45' C -0.0443(19) 0.4693(12) 0.0987(13) 0.105(4) Uiso 0.573(6) 1 d PG A 2 H45' H -0.0028 0.4296 0.1013 0.126 Uiso 0.573(6) 1 calc PR A 2 C46' C -0.128(2) 0.4707(12) 0.0781(13) 0.105(4) Uiso 0.573(6) 1 d PG A 2 H46' H -0.1425 0.4318 0.0667 0.126 Uiso 0.573(6) 1 calc PR A 2 C47' C -0.1889(16) 0.5294(15) 0.0743(12) 0.105(4) Uiso 0.573(6) 1 d PG A 2 H47' H -0.2453 0.5304 0.0603 0.126 Uiso 0.573(6) 1 calc PR A 2 C48' C -0.1669(19) 0.5868(12) 0.0911(13) 0.105(4) Uiso 0.573(6) 1 d PG A 2 H48' H -0.2084 0.6266 0.0885 0.126 Uiso 0.573(6) 1 calc PR A 2 C49' C 0.2108(15) 0.6949(8) 0.2084(10) 0.045(6) Uiso 0.573(6) 1 d PG A 2 C50' C 0.1324(11) 0.7437(10) 0.2300(11) 0.074(9) Uiso 0.573(6) 1 d PG A 2 H50' H 0.0664 0.7330 0.2454 0.089 Uiso 0.573(6) 1 calc PR A 2 C51' C 0.1514(15) 0.8081(9) 0.2287(12) 0.076(9) Uiso 0.573(6) 1 d PG A 2 H51' H 0.0983 0.8411 0.2433 0.091 Uiso 0.573(6) 1 calc PR A 2 C52' C 0.2489(18) 0.8239(9) 0.2060(13) 0.091(11) Uiso 0.573(6) 1 d PG A 2 H52' H 0.2618 0.8675 0.2052 0.109 Uiso 0.573(6) 1 calc PR A 2 C53' C 0.3274(13) 0.7751(12) 0.1844(13) 0.091(11) Uiso 0.573(6) 1 d PG A 2 H53' H 0.3933 0.7858 0.1690 0.109 Uiso 0.573(6) 1 calc PR A 2 C54' C 0.3083(13) 0.7107(10) 0.1856(12) 0.077(10) Uiso 0.573(6) 1 d PG A 2 H54' H 0.3614 0.6777 0.1711 0.093 Uiso 0.573(6) 1 calc PR A 2 C55' C 0.2655(16) 0.5751(10) 0.1432(9) 0.076(3) Uiso 0.573(6) 1 d PG A 2 C56' C 0.3090(17) 0.6134(8) 0.0823(11) 0.076(3) Uiso 0.573(6) 1 d PG A 2 H56' H 0.3044 0.6596 0.0812 0.091 Uiso 0.573(6) 1 calc PR A 2 C57' C 0.3593(16) 0.5834(10) 0.0231(8) 0.076(3) Uiso 0.573(6) 1 d PG A 2 H57' H 0.3887 0.6093 -0.0181 0.091 Uiso 0.573(6) 1 calc PR A 2 C58' C 0.3661(16) 0.5151(10) 0.0247(8) 0.076(3) Uiso 0.573(6) 1 d PG A 2 H58' H 0.4001 0.4948 -0.0153 0.091 Uiso 0.573(6) 1 calc PR A 2 C59' C 0.3226(16) 0.4768(8) 0.0856(11) 0.076(3) Uiso 0.573(6) 1 d PG A 2 H59' H 0.3272 0.4306 0.0867 0.091 Uiso 0.573(6) 1 calc PR A 2 C60' C 0.2723(16) 0.5069(10) 0.1449(8) 0.076(3) Uiso 0.573(6) 1 d PG A 2 H60' H 0.2429 0.4810 0.1860 0.091 Uiso 0.573(6) 1 calc PR A 2 C61 C 0.5821(10) 0.6400(8) 0.1637(7) 0.050(4) Uani 1 1 d . . . C62 C 0.5670(12) 0.6210(8) 0.1073(7) 0.057(4) Uani 1 1 d . . . H62 H 0.5499 0.5783 0.1089 0.068 Uiso 1 1 calc R . . C63 C 0.5769(15) 0.6643(11) 0.0494(9) 0.086(6) Uani 1 1 d . . . H63 H 0.5675 0.6510 0.0109 0.103 Uiso 1 1 calc R . . C64 C 0.6007(16) 0.7283(11) 0.0466(10) 0.089(6) Uani 1 1 d . . . H64 H 0.6085 0.7576 0.0062 0.106 Uiso 1 1 calc R . . C65 C 0.6127(15) 0.7480(10) 0.1026(9) 0.082(5) Uani 1 1 d . . . H65 H 0.6258 0.7916 0.1016 0.098 Uiso 1 1 calc R . . C66 C 0.6055(11) 0.7033(8) 0.1620(8) 0.056(4) Uani 1 1 d . . . H66 H 0.6164 0.7162 0.2001 0.068 Uiso 1 1 calc R . . C67 C 0.5675(10) 0.5010(6) 0.2232(6) 0.041(3) Uani 1 1 d . . . C68 C 0.6475(14) 0.4522(8) 0.2242(11) 0.086(6) Uani 1 1 d . . . H68 H 0.7018 0.4622 0.2354 0.103 Uiso 1 1 calc R . . C69 C 0.6462(18) 0.3886(10) 0.2084(13) 0.111(8) Uani 1 1 d . . . H69 H 0.7014 0.3568 0.2064 0.133 Uiso 1 1 calc R . . C70 C 0.5674(18) 0.3732(8) 0.1963(10) 0.084(6) Uani 1 1 d . . . H70 H 0.5651 0.3295 0.1893 0.101 Uiso 1 1 calc R . . C71 C 0.4886(14) 0.4204(9) 0.1939(9) 0.076(5) Uani 1 1 d . . . H71 H 0.4356 0.4093 0.1820 0.091 Uiso 1 1 calc R . . C72 C 0.4873(12) 0.4834(7) 0.2088(8) 0.064(4) Uani 1 1 d . . . H72 H 0.4320 0.5147 0.2091 0.077 Uiso 1 1 calc R . . C73 C 0.3269(9) 0.7652(6) 0.4230(6) 0.039(3) Uani 1 1 d U A . C74 C 0.2979(11) 0.8142(7) 0.3769(8) 0.055(4) Uani 1 1 d U . . H74 H 0.2925 0.8033 0.3361 0.066 Uiso 1 1 calc R . . C75 C 0.2770(12) 0.8797(8) 0.3921(8) 0.061(4) Uani 1 1 d U . . H75 H 0.2565 0.9131 0.3617 0.073 Uiso 1 1 calc R . . C76 C 0.2865(12) 0.8959(7) 0.4529(8) 0.061(4) Uani 1 1 d U . . H76 H 0.2731 0.9401 0.4628 0.073 Uiso 1 1 calc R . . C77 C 0.3152(11) 0.8475(7) 0.4976(8) 0.057(4) Uani 1 1 d U . . H77 H 0.3221 0.8580 0.5381 0.069 Uiso 1 1 calc R . . C78 C 0.3343(9) 0.7812(7) 0.4819(7) 0.045(3) Uani 1 1 d U . . H78 H 0.3526 0.7476 0.5130 0.054 Uiso 1 1 calc R . . C79 C 0.3891(9) 0.6308(6) 0.4658(7) 0.039(3) Uani 1 1 d . A . C80 C 0.4853(10) 0.6329(7) 0.4645(8) 0.053(4) Uani 1 1 d . . . H80 H 0.5257 0.6604 0.4293 0.063 Uiso 1 1 calc R . . C81 C 0.5251(13) 0.5960(9) 0.5129(10) 0.073(5) Uani 1 1 d . . . H81 H 0.5919 0.5977 0.5093 0.087 Uiso 1 1 calc R . . C82 C 0.4672(17) 0.5574(9) 0.5657(10) 0.083(6) Uani 1 1 d . . . H82 H 0.4922 0.5343 0.6003 0.100 Uiso 1 1 calc R . . C83 C 0.3706(14) 0.5526(10) 0.5677(10) 0.089(6) Uani 1 1 d . . . H83 H 0.3312 0.5245 0.6028 0.106 Uiso 1 1 calc R . . C84 C 0.3313(12) 0.5886(8) 0.5188(9) 0.069(5) Uani 1 1 d . . . H84 H 0.2657 0.5849 0.5212 0.082 Uiso 1 1 calc R . . C87 C 0.4518(9) 0.6037(6) 0.3021(6) 0.040(3) Uani 1 1 d . . . H87A H 0.4007 0.5988 0.2819 0.048 Uiso 1 1 calc R . . H87B H 0.4430 0.5720 0.3435 0.048 Uiso 1 1 calc R . . C88 C 0.4352(9) 0.6742(7) 0.3229(6) 0.043(3) Uani 1 1 d . A . H88A H 0.4167 0.7057 0.2876 0.051 Uiso 1 1 calc R . . H88B H 0.4973 0.6857 0.3263 0.051 Uiso 1 1 calc R . . P3 P 0.3369(2) 0.68042(16) 0.40537(17) 0.0371(7) Uani 1 1 d . . . P4 P 0.5730(2) 0.58306(16) 0.24179(18) 0.0389(8) Uani 1 1 d . . . P5 P -0.2321(4) 1.1952(3) 0.2818(3) 0.0751(13) Uani 1 1 d . . . F1 F -0.3133(12) 1.2235(7) 0.2470(8) 0.141(6) Uani 1 1 d . . . F2 F -0.2999(11) 1.1404(6) 0.3267(7) 0.119(4) Uani 1 1 d . . . F3 F -0.1823(11) 1.1462(7) 0.2262(6) 0.134(5) Uani 1 1 d . . . F4 F -0.1545(10) 1.1658(6) 0.3215(7) 0.123(5) Uani 1 1 d . . . F5 F -0.1660(12) 1.2496(7) 0.2377(8) 0.141(5) Uani 1 1 d . . . F6 F -0.2812(10) 1.2437(6) 0.3394(6) 0.112(4) Uani 1 1 d . . . P6 P -0.5000 1.0000 0.5000 0.0524(13) Uani 1 2 d S . . F7 F -0.4399(12) 1.0489(7) 0.4441(7) 0.152(6) Uani 1 1 d . . . F8 F -0.5822(11) 1.0138(7) 0.4658(9) 0.151(6) Uani 1 1 d . . . F9 F -0.4502(11) 0.9410(6) 0.4579(6) 0.117(5) Uani 1 1 d . . . P7 P -0.6278(5) 1.2520(3) 0.1681(3) 0.0850(16) Uani 1 1 d . . . F10 F -0.6945(15) 1.2053(11) 0.2243(10) 0.225(11) Uani 1 1 d . . . F11 F -0.7065(14) 1.2718(10) 0.1307(10) 0.194(8) Uani 1 1 d . . . F12 F -0.5801(16) 1.1952(8) 0.1228(10) 0.191(8) Uani 1 1 d . . . F13 F -0.5482(12) 1.2378(9) 0.2040(8) 0.164(7) Uani 1 1 d . . . F14 F -0.6755(14) 1.3085(9) 0.2158(8) 0.166(7) Uani 1 1 d . . . F15 F -0.5622(13) 1.3025(7) 0.1150(7) 0.143(6) Uani 1 1 d . . . P8 P 0.1391(4) 0.0750(2) 0.3871(3) 0.0681(12) Uani 1 1 d . . . F16 F 0.0460(8) 0.1006(6) 0.3634(7) 0.111(4) Uani 1 1 d . . . F17 F 0.0870(9) 0.0151(7) 0.4347(7) 0.124(5) Uani 1 1 d . . . F18 F 0.1825(10) 0.0327(6) 0.3258(6) 0.113(4) Uani 1 1 d . . . F19 F 0.2341(9) 0.0509(5) 0.4108(7) 0.108(4) Uani 1 1 d . . . F20 F 0.1937(9) 0.1332(5) 0.3400(6) 0.101(4) Uani 1 1 d . . . F21 F 0.0983(11) 0.1196(7) 0.4469(6) 0.124(5) Uani 1 1 d . . . O3 O -0.848(4) 1.115(3) 0.176(2) 0.187(18) Uiso 0.50 1 d P . . C91 C -0.794(4) 1.049(3) 0.176(3) 0.132(19) Uiso 0.50 1 d P . . P9 P 0.8963(18) 0.9933(12) 0.1069(11) 0.291(10) Uiso 0.50 1 d PD . . F22 F 0.982(3) 0.982(2) 0.0380(14) 0.291(10) Uiso 0.50 1 d PD . . F23 F 0.856(3) 1.0596(15) 0.0708(19) 0.291(10) Uiso 0.50 1 d PD . . F24 F 0.810(2) 1.006(2) 0.1753(15) 0.291(10) Uiso 0.50 1 d PD . . F25 F 0.937(3) 0.9266(15) 0.1423(19) 0.291(10) Uiso 0.50 1 d PD . . F26 F 0.827(3) 0.9549(18) 0.084(2) 0.291(10) Uiso 0.50 1 d PD . . F27 F 0.964(3) 1.0332(19) 0.129(2) 0.291(10) Uiso 0.50 1 d PD . . C90 C 0.636(6) 0.917(5) 0.020(5) 0.26(4) Uiso 0.50 1 d PD . . O2 O 0.526(6) 0.920(4) 0.051(4) 0.33(4) Uiso 0.50 1 d PD . . N1A N -0.4756(13) 1.0297(7) 0.2328(8) 0.079(4) 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 0.0385(3) 0.0434(3) 0.0605(4) -0.0145(3) -0.0179(2) 0.0060(2) Au2 0.0493(3) 0.0619(4) 0.0858(5) -0.0358(3) -0.0267(3) 0.0110(3) Au3 0.0352(3) 0.0341(3) 0.0583(3) -0.0150(2) -0.0180(2) 0.0055(2) Au4 0.0366(3) 0.0357(3) 0.0509(3) -0.0074(2) -0.0189(2) 0.0065(2) S1 0.0426(18) 0.0392(19) 0.058(2) -0.0146(16) -0.0136(16) 0.0004(15) S2 0.076(3) 0.036(2) 0.094(3) -0.020(2) -0.014(2) 0.0030(19) S3 0.0332(16) 0.0379(19) 0.083(3) -0.0111(18) -0.0217(17) 0.0035(14) S4 0.0473(19) 0.049(2) 0.064(2) -0.0066(17) -0.0313(18) 0.0068(16) N2 0.073(9) 0.053(8) 0.078(9) -0.025(7) -0.031(8) 0.028(7) N3 0.055(7) 0.037(6) 0.056(7) -0.008(5) -0.015(6) 0.014(5) N4 0.059(7) 0.036(6) 0.053(7) -0.013(5) -0.024(6) 0.013(5) C1 0.041(7) 0.052(9) 0.059(9) -0.022(7) -0.023(7) 0.011(6) C2 0.083(13) 0.060(11) 0.084(12) -0.026(10) 0.003(10) -0.002(10) C3 0.064(10) 0.066(11) 0.057(10) -0.016(8) -0.003(8) 0.033(9) C4 0.066(10) 0.040(8) 0.066(10) -0.017(7) -0.017(8) 0.010(7) C5 0.089(14) 0.079(14) 0.070(12) -0.005(10) 0.018(10) 0.033(11) C6 0.090(13) 0.052(10) 0.061(10) 0.000(8) -0.003(9) 0.035(9) C10 0.059(8) 0.054(8) 0.078(9) -0.020(7) -0.043(7) 0.013(6) C11 0.053(7) 0.055(8) 0.085(9) -0.014(7) -0.045(7) 0.005(6) C12 0.057(8) 0.062(8) 0.092(9) -0.027(7) -0.049(7) 0.028(7) C13 0.055(7) 0.052(8) 0.089(9) -0.021(7) -0.046(7) 0.035(6) C14 0.104(10) 0.064(9) 0.107(10) -0.044(8) -0.071(8) 0.045(8) C15 0.100(10) 0.059(8) 0.097(10) -0.033(7) -0.074(8) 0.042(8) C16 0.14(2) 0.077(15) 0.103(16) -0.018(12) -0.031(14) 0.060(14) C17 0.064(11) 0.067(12) 0.112(15) -0.009(11) -0.027(11) 0.013(9) C18 0.072(11) 0.053(10) 0.160(19) -0.012(11) -0.080(13) 0.016(9) C19 0.027(6) 0.040(7) 0.058(8) -0.024(6) -0.010(6) 0.005(5) C20 0.040(7) 0.044(8) 0.073(10) -0.021(7) -0.025(7) -0.009(6) C21 0.038(7) 0.058(9) 0.066(9) -0.007(7) -0.032(7) 0.011(6) C22 0.044(7) 0.048(8) 0.039(7) -0.010(6) -0.006(6) 0.011(6) C23 0.036(7) 0.044(8) 0.075(10) -0.020(7) -0.025(7) 0.000(6) C24 0.038(7) 0.044(8) 0.083(10) -0.021(7) -0.033(7) 0.010(6) C25 0.072(12) 0.059(11) 0.087(13) -0.007(9) -0.018(10) 0.007(9) C26 0.086(13) 0.051(10) 0.091(13) -0.020(9) -0.024(11) 0.016(9) C27 0.076(12) 0.050(10) 0.159(19) -0.021(11) -0.067(13) 0.018(9) C28 0.043(7) 0.040(8) 0.060(9) -0.022(7) -0.004(7) -0.005(6) C29 0.096(13) 0.053(10) 0.051(9) 0.002(8) -0.018(9) -0.001(9) C30 0.102(13) 0.041(9) 0.048(9) -0.011(7) -0.005(9) 0.035(9) C31 0.049(8) 0.037(8) 0.067(10) -0.014(7) -0.023(7) 0.005(6) C32 0.064(10) 0.048(9) 0.064(10) -0.008(8) -0.020(8) 0.010(8) C33 0.040(8) 0.064(10) 0.063(10) -0.013(8) 0.001(7) 0.008(7) C61 0.046(8) 0.064(10) 0.037(7) -0.015(7) -0.010(6) 0.008(7) C62 0.076(11) 0.059(10) 0.033(8) -0.001(7) -0.017(7) -0.005(8) C63 0.105(16) 0.110(17) 0.051(11) -0.022(11) -0.033(10) -0.002(13) C64 0.116(17) 0.089(16) 0.064(12) 0.015(11) -0.045(12) -0.006(13) C65 0.101(15) 0.070(13) 0.073(12) -0.001(10) -0.030(11) -0.004(11) C66 0.053(9) 0.055(10) 0.066(10) -0.006(8) -0.023(8) -0.015(7) C67 0.044(7) 0.030(7) 0.044(7) -0.009(6) -0.008(6) 0.005(6) C68 0.073(12) 0.049(10) 0.153(19) -0.029(11) -0.057(13) 0.009(9) C69 0.111(18) 0.049(12) 0.18(2) -0.060(14) -0.050(17) 0.027(11) C70 0.137(19) 0.030(9) 0.093(14) -0.008(9) -0.038(13) -0.028(11) C71 0.075(12) 0.073(13) 0.084(12) -0.035(10) -0.013(10) -0.019(10) C72 0.065(10) 0.038(8) 0.095(12) -0.033(8) -0.026(9) 0.003(7) C73 0.041(6) 0.031(6) 0.044(6) -0.015(5) -0.011(5) 0.007(5) C74 0.062(7) 0.030(6) 0.071(7) -0.008(6) -0.023(6) 0.010(5) C75 0.071(8) 0.045(7) 0.066(7) -0.004(6) -0.029(6) 0.012(6) C76 0.071(8) 0.039(7) 0.070(8) -0.015(6) -0.022(6) 0.009(6) C77 0.068(7) 0.048(7) 0.058(7) -0.018(6) -0.018(6) -0.004(6) C78 0.044(6) 0.038(6) 0.054(7) -0.008(5) -0.021(5) 0.008(5) C79 0.043(7) 0.028(6) 0.053(8) -0.014(6) -0.024(6) 0.011(5) C80 0.043(8) 0.051(9) 0.074(10) -0.008(7) -0.029(7) -0.009(7) C81 0.066(11) 0.065(11) 0.108(14) -0.013(10) -0.059(11) 0.006(9) C82 0.118(17) 0.065(12) 0.070(12) 0.005(10) -0.042(12) -0.006(12) C83 0.065(12) 0.076(13) 0.104(15) 0.031(11) -0.021(11) 0.002(10) C84 0.053(9) 0.053(10) 0.090(12) 0.011(9) -0.019(9) 0.001(8) C87 0.043(7) 0.030(7) 0.049(8) -0.005(6) -0.020(6) 0.002(5) C88 0.041(7) 0.047(8) 0.037(7) -0.006(6) -0.013(6) 0.008(6) P3 0.0349(16) 0.0287(16) 0.050(2) -0.0144(14) -0.0167(15) 0.0061(13) P4 0.0360(17) 0.0326(17) 0.051(2) -0.0129(15) -0.0185(15) 0.0084(14) P5 0.091(4) 0.057(3) 0.082(3) -0.002(2) -0.040(3) 0.002(3) F1 0.179(14) 0.108(11) 0.185(14) -0.026(10) -0.137(12) 0.030(10) F2 0.147(12) 0.073(8) 0.135(10) -0.009(7) -0.039(9) -0.023(8) F3 0.165(14) 0.110(11) 0.106(9) -0.045(8) -0.017(9) 0.018(10) F4 0.134(11) 0.091(9) 0.176(13) -0.009(9) -0.106(10) 0.022(8) F5 0.157(14) 0.095(10) 0.154(12) 0.009(9) -0.024(11) -0.039(10) F6 0.127(10) 0.082(9) 0.119(9) -0.038(7) -0.021(8) 0.002(8) P6 0.058(3) 0.036(3) 0.067(4) -0.010(3) -0.024(3) 0.000(2) F7 0.192(16) 0.087(10) 0.126(11) 0.003(8) 0.022(11) -0.036(10) F8 0.138(12) 0.124(12) 0.249(18) -0.062(12) -0.143(13) 0.041(10) F9 0.188(13) 0.069(8) 0.090(8) -0.040(6) -0.047(8) 0.040(8) P7 0.112(4) 0.073(4) 0.084(4) 0.007(3) -0.050(3) -0.022(3) F10 0.22(2) 0.27(3) 0.182(17) 0.078(17) -0.045(16) -0.16(2) F11 0.202(19) 0.21(2) 0.232(19) -0.015(15) -0.164(17) 0.008(15) F12 0.25(2) 0.123(14) 0.24(2) -0.102(14) -0.124(18) 0.050(14) F13 0.160(15) 0.208(19) 0.153(13) 0.040(12) -0.106(12) -0.041(13) F14 0.203(18) 0.178(17) 0.127(12) -0.058(12) -0.055(12) -0.001(14) F15 0.212(17) 0.119(12) 0.098(9) 0.019(8) -0.044(10) -0.057(11) P8 0.074(3) 0.042(2) 0.093(3) -0.002(2) -0.040(3) 0.005(2) F16 0.089(8) 0.075(8) 0.180(12) -0.009(8) -0.073(8) 0.019(6) F17 0.102(9) 0.102(10) 0.170(13) 0.037(9) -0.055(9) -0.043(8) F18 0.145(11) 0.096(9) 0.116(9) -0.045(7) -0.070(9) 0.038(8) F19 0.096(8) 0.071(8) 0.173(12) 0.020(7) -0.083(8) -0.001(6) F20 0.096(8) 0.069(7) 0.135(10) 0.018(7) -0.046(8) -0.012(6) F21 0.143(12) 0.127(12) 0.092(8) -0.040(8) -0.026(8) 0.015(9) N1A 0.100(12) 0.061(10) 0.077(10) -0.014(8) -0.037(9) 0.016(8) _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 2.229(12) . ? Au1 P1' 2.309(9) . ? Au1 S1 2.330(4) . ? Au1 Au4 3.0753(13) 1_455 ? Au2 P2' 2.107(8) . ? Au2 S2 2.303(5) . ? Au2 P2 2.489(11) . ? Au2 Au3 3.0782(11) . ? Au3 P3 2.269(3) . ? Au3 S3 2.321(3) . ? Au4 P4 2.270(3) . ? Au4 S4 2.318(3) . ? Au4 Au1 3.0753(13) 1_655 ? S1 C1 1.734(14) . ? S2 C28 1.779(14) . ? S3 C19 1.759(13) . ? S4 C10 1.756(15) . ? N2 C18 1.491(18) . ? N2 C13 1.494(17) . ? N2 C16 1.50(2) . ? N2 C17 1.53(2) . ? N3 C27 1.470(19) . ? N3 C25 1.499(19) . ? N3 C22 1.500(16) . ? N3 C26 1.509(19) . ? N4 C35' 1.39(3) . ? N4 C34 1.42(4) . ? N4 C31 1.486(16) . ? N4 C36' 1.51(3) . ? N4 C34' 1.52(3) . ? N4 C35 1.58(4) . ? N4 C36 1.59(4) . ? C1 C6 1.36(2) . ? C1 C2 1.42(2) . ? C2 C3 1.36(2) . ? C2 H2 0.9400 . ? C3 C4 1.36(2) . ? C3 H3 0.9400 . ? C4 C5 1.42(2) . ? C4 N1A 1.508(19) . ? C5 C6 1.39(2) . ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? C10 C15 1.36(2) . ? C10 C11 1.422(18) . ? C11 C12 1.407(19) . ? C11 H11 0.9400 . ? C12 C13 1.38(2) . ? C12 H12 0.9400 . ? C13 C14 1.35(2) . ? C14 C15 1.39(2) . ? C14 H14 0.9400 . ? C15 H15 0.9400 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C24 1.394(17) . ? C19 C20 1.426(17) . ? C20 C21 1.400(18) . ? C20 H20 0.9400 . ? C21 C22 1.401(19) . ? C21 H21 0.9400 . ? C22 C23 1.377(18) . ? C23 C24 1.393(18) . ? C23 H23 0.9400 . ? C24 H24 0.9400 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 H25C 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C26 H26C 0.9700 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 H27C 0.9700 . ? C28 C33 1.37(2) . ? C28 C29 1.38(2) . ? C29 C30 1.35(2) . ? C29 H29 0.9400 . ? C30 C31 1.36(2) . ? C30 H30 0.9400 . ? C31 C32 1.380(19) . ? C32 C33 1.37(2) . ? C32 H32 0.9400 . ? C33 H33 0.9400 . ? C7 N1A 1.48(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 N1A 1.50(5) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 N1A 1.54(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 H35C 0.9700 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C89 O1 1.58(7) . ? P1 C43 1.79(3) . ? P1 C37 1.821(17) . ? P1 C85 1.95(4) . ? P2 C49 1.79(2) . ? P2 C55 1.84(2) . ? P2 C86 1.88(3) . ? C85 C86 1.58(5) . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C38 H38 0.9400 . ? C39 C40 1.3900 . ? C39 H39 0.9400 . ? C40 C41 1.3900 . ? C40 H40 0.9400 . ? C41 C42 1.3900 . ? C41 H41 0.9400 . ? C42 H42 0.9400 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C44 H44 0.9400 . ? C45 C46 1.3900 . ? C45 H45 0.9400 . ? C46 C47 1.3900 . ? C46 H46 0.9400 . ? C47 C48 1.3900 . ? C47 H47 0.9400 . ? C48 H48 0.9400 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C50 H50 0.9400 . ? C51 C52 1.3900 . ? C51 H51 0.9400 . ? C52 C53 1.3900 . ? C52 H52 0.9400 . ? C53 C54 1.3900 . ? C53 H53 0.9400 . ? C54 H54 0.9400 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C56 H56 0.9400 . ? C57 C58 1.3900 . ? C57 H57 0.9400 . ? C58 C59 1.3900 . ? C58 H58 0.9400 . ? C59 C60 1.3900 . ? C59 H59 0.9400 . ? C60 H60 0.9400 . ? C7' N1A 1.53(4) . ? C7' H7'1 0.9700 . ? C7' H7'2 0.9700 . ? C7' H7'3 0.9700 . ? C8' N1A 1.53(3) . ? C8' H8'1 0.9700 . ? C8' H8'2 0.9700 . ? C8' H8'3 0.9700 . ? C9' N1A 1.47(4) . ? C9' H9'1 0.9700 . ? C9' H9'2 0.9700 . ? C9' H9'3 0.9700 . ? O1' C89' 1.52(8) . ? C34' H34D 0.9700 . ? C34' H34E 0.9700 . ? C34' H34F 0.9700 . ? C35' H35D 0.9700 . ? C35' H35E 0.9700 . ? C35' H35F 0.9700 . ? C36' H36D 0.9700 . ? C36' H36E 0.9700 . ? C36' H36F 0.9700 . ? P1' C37' 1.772(13) . ? P1' C85' 1.82(3) . ? P1' C43' 1.91(2) . ? P2' C49' 1.781(17) . ? P2' C86' 1.80(3) . ? P2' C55' 1.823(16) . ? C85' C86' 1.53(3) . ? C85' H85C 0.9800 . ? C85' H85D 0.9800 . ? C86' H86C 0.9800 . ? C86' H86D 0.9800 . ? C37' C38' 1.3900 . ? C37' C42' 1.3900 . ? C38' C39' 1.3900 . ? C38' H38' 0.9400 . ? C39' C40' 1.3900 . ? C39' H39' 0.9400 . ? C40' C41' 1.3900 . ? C40' H40' 0.9400 . ? C41' C42' 1.3900 . ? C41' H41' 0.9400 . ? C42' H42' 0.9400 . ? C43' C44' 1.3900 . ? C43' C48' 1.3900 . ? C44' C45' 1.3900 . ? C44' H44' 0.9400 . ? C45' C46' 1.3900 . ? C45' H45' 0.9400 . ? C46' C47' 1.3900 . ? C46' H46' 0.9400 . ? C47' C48' 1.3900 . ? C47' H47' 0.9400 . ? C48' H48' 0.9400 . ? C49' C50' 1.3900 . ? C49' C54' 1.3900 . ? C50' C51' 1.3900 . ? C50' H50' 0.9400 . ? C51' C52' 1.3900 . ? C51' H51' 0.9400 . ? C52' C53' 1.3900 . ? C52' H52' 0.9400 . ? C53' C54' 1.3900 . ? C53' H53' 0.9400 . ? C54' H54' 0.9400 . ? C55' C56' 1.3900 . ? C55' C60' 1.3900 . ? C56' C57' 1.3900 . ? C56' H56' 0.9400 . ? C57' C58' 1.3900 . ? C57' H57' 0.9400 . ? C58' C59' 1.3900 . ? C58' H58' 0.9400 . ? C59' C60' 1.3900 . ? C59' H59' 0.9400 . ? C60' H60' 0.9400 . ? C61 C62 1.383(19) . ? C61 C66 1.39(2) . ? C61 P4 1.828(14) . ? C62 C63 1.36(2) . ? C62 H62 0.9400 . ? C63 C64 1.40(3) . ? C63 H63 0.9400 . ? C64 C65 1.36(2) . ? C64 H64 0.9400 . ? C65 C66 1.40(2) . ? C65 H65 0.9400 . ? C66 H66 0.9400 . ? C67 C72 1.388(19) . ? C67 C68 1.41(2) . ? C67 P4 1.809(13) . ? C68 C69 1.40(2) . ? C68 H68 0.9400 . ? C69 C70 1.33(3) . ? C69 H69 0.9400 . ? C70 C71 1.38(3) . ? C70 H70 0.9400 . ? C71 C72 1.38(2) . ? C71 H71 0.9400 . ? C72 H72 0.9400 . ? C73 C78 1.359(17) . ? C73 C74 1.393(18) . ? C73 P3 1.813(12) . ? C74 C75 1.399(19) . ? C74 H74 0.9400 . ? C75 C76 1.41(2) . ? C75 H75 0.9400 . ? C76 C77 1.37(2) . ? C76 H76 0.9400 . ? C77 C78 1.416(18) . ? C77 H77 0.9400 . ? C78 H78 0.9400 . ? C79 C80 1.376(17) . ? C79 C84 1.405(19) . ? C79 P3 1.781(12) . ? C80 C81 1.39(2) . ? C80 H80 0.9400 . ? C81 C82 1.36(2) . ? C81 H81 0.9400 . ? C82 C83 1.39(2) . ? C82 H82 0.9400 . ? C83 C84 1.38(2) . ? C83 H83 0.9400 . ? C84 H84 0.9400 . ? C87 C88 1.540(17) . ? C87 P4 1.808(12) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C88 P3 1.833(12) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? P5 F5 1.556(13) . ? P5 F1 1.559(12) . ? P5 F3 1.568(13) . ? P5 F2 1.580(13) . ? P5 F6 1.589(12) . ? P5 F4 1.590(11) . ? P6 F7 1.531(12) 2_476 ? P6 F7 1.531(12) . ? P6 F8 1.536(12) . ? P6 F8 1.536(12) 2_476 ? P6 F9 1.551(10) 2_476 ? P6 F9 1.551(10) . ? P7 F13 1.527(14) . ? P7 F11 1.544(15) . ? P7 F10 1.548(15) . ? P7 F12 1.548(16) . ? P7 F15 1.563(14) . ? P7 F14 1.572(17) . ? P8 F20 1.557(11) . ? P8 F18 1.557(12) . ? P8 F16 1.561(11) . ? P8 F21 1.562(13) . ? P8 F17 1.573(12) . ? P8 F19 1.582(11) . ? O3 C91 1.46(6) . ? P9 F27 1.569(9) . ? P9 F24 1.571(9) . ? P9 F22 1.573(9) . ? P9 F26 1.575(9) . ? P9 F25 1.578(9) . ? P9 F23 1.580(9) . ? F22 F22 1.59(6) 2_775 ? C90 O2 1.48(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 P1' 10.2(4) . . ? P1 Au1 S1 172.2(3) . . ? P1' Au1 S1 177.4(2) . . ? P1 Au1 Au4 94.9(3) . 1_455 ? P1' Au1 Au4 104.3(2) . 1_455 ? S1 Au1 Au4 78.25(9) . 1_455 ? P2' Au2 S2 171.4(2) . . ? P2' Au2 P2 11.2(3) . . ? S2 Au2 P2 169.6(3) . . ? P2' Au2 Au3 106.6(2) . . ? S2 Au2 Au3 73.48(11) . . ? P2 Au2 Au3 96.7(3) . . ? P3 Au3 S3 170.30(12) . . ? P3 Au3 Au2 111.28(9) . . ? S3 Au3 Au2 76.61(10) . . ? P4 Au4 S4 176.48(13) . . ? P4 Au4 Au1 110.72(9) . 1_655 ? S4 Au4 Au1 72.80(10) . 1_655 ? C1 S1 Au1 107.5(5) . . ? C28 S2 Au2 111.8(5) . . ? C19 S3 Au3 104.6(4) . . ? C10 S4 Au4 106.6(5) . . ? C18 N2 C13 112.0(13) . . ? C18 N2 C16 112.9(15) . . ? C13 N2 C16 110.5(13) . . ? C18 N2 C17 107.1(13) . . ? C13 N2 C17 109.8(13) . . ? C16 N2 C17 104.2(16) . . ? C27 N3 C25 107.2(13) . . ? C27 N3 C22 114.7(12) . . ? C25 N3 C22 109.3(11) . . ? C27 N3 C26 107.1(13) . . ? C25 N3 C26 108.0(13) . . ? C22 N3 C26 110.4(11) . . ? C35' N4 C34 137(3) . . ? C35' N4 C31 114.3(18) . . ? C34 N4 C31 107(2) . . ? C35' N4 C36' 106(2) . . ? C34 N4 C36' 66(2) . . ? C31 N4 C36' 114.0(16) . . ? C35' N4 C34' 112(2) . . ? C34 N4 C34' 38.5(19) . . ? C31 N4 C34' 110.4(16) . . ? C36' N4 C34' 99(2) . . ? C35' N4 C35 35.3(18) . . ? C34 N4 C35 118(3) . . ? C31 N4 C35 110.9(19) . . ? C36' N4 C35 131(2) . . ? C34' N4 C35 82(2) . . ? C35' N4 C36 70(2) . . ? C34 N4 C36 108(3) . . ? C31 N4 C36 108.7(19) . . ? C36' N4 C36 42.9(18) . . ? C34' N4 C36 135(2) . . ? C35 N4 C36 105(2) . . ? C6 C1 C2 113.8(15) . . ? C6 C1 S1 127.1(11) . . ? C2 C1 S1 119.1(13) . . ? C3 C2 C1 123.3(17) . . ? C3 C2 H2 118.3 . . ? C1 C2 H2 118.3 . . ? C4 C3 C2 121.1(15) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 118.7(15) . . ? C3 C4 N1A 121.6(14) . . ? C5 C4 N1A 119.7(15) . . ? C6 C5 C4 117.6(16) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C1 C6 C5 125.5(15) . . ? C1 C6 H6 117.2 . . ? C5 C6 H6 117.2 . . ? C15 C10 C11 116.9(14) . . ? C15 C10 S4 124.7(11) . . ? C11 C10 S4 118.3(12) . . ? C12 C11 C10 121.8(15) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C11 118.4(14) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C12 119.6(14) . . ? C14 C13 N2 121.1(15) . . ? C12 C13 N2 119.2(13) . . ? C13 C14 C15 122.7(17) . . ? C13 C14 H14 118.7 . . ? C15 C14 H14 118.7 . . ? C10 C15 C14 120.7(15) . . ? C10 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 117.9(12) . . ? C24 C19 S3 125.5(10) . . ? C20 C19 S3 116.5(10) . . ? C21 C20 C19 119.7(12) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.7(12) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 119.4(13) . . ? C23 C22 N3 120.2(13) . . ? C21 C22 N3 120.4(12) . . ? C22 C23 C24 120.5(13) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 121.6(12) . . ? C23 C24 H24 119.2 . . ? C19 C24 H24 119.2 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 118.1(14) . . ? C33 C28 S2 116.3(10) . . ? C29 C28 S2 125.6(12) . . ? C30 C29 C28 120.6(15) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 122.5(14) . . ? C29 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C30 C31 C32 116.7(13) . . ? C30 C31 N4 123.5(13) . . ? C32 C31 N4 119.8(13) . . ? C33 C32 C31 121.9(15) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C32 C33 C28 120.1(14) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? N1A C7 H7A 109.5 . . ? N1A C7 H7B 109.5 . . ? N1A C7 H7C 109.5 . . ? N1A C8 H8A 109.5 . . ? N1A C8 H8B 109.5 . . ? N1A C8 H8C 109.5 . . ? N1A C9 H9A 109.5 . . ? N1A C9 H9B 109.5 . . ? N1A C9 H9C 109.5 . . ? N4 C34 H34A 109.5 . . ? N4 C34 H34B 109.5 . . ? N4 C34 H34C 109.5 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? C43 P1 C37 105.4(15) . . ? C43 P1 C85 104.9(18) . . ? C37 P1 C85 108.7(14) . . ? C43 P1 Au1 115.9(14) . . ? C37 P1 Au1 111.3(9) . . ? C85 P1 Au1 110.2(12) . . ? C49 P2 C55 107.5(13) . . ? C49 P2 C86 97.1(14) . . ? C55 P2 C86 104.6(15) . . ? C49 P2 Au2 114.8(10) . . ? C55 P2 Au2 114.8(10) . . ? C86 P2 Au2 116.1(12) . . ? C86 C85 P1 102(2) . . ? C86 C85 H85A 111.3 . . ? P1 C85 H85A 111.3 . . ? C86 C85 H85B 111.3 . . ? P1 C85 H85B 111.3 . . ? H85A C85 H85B 109.2 . . ? C85 C86 P2 107(2) . . ? C85 C86 H86A 110.3 . . ? P2 C86 H86A 110.3 . . ? C85 C86 H86B 110.3 . . ? P2 C86 H86B 110.3 . . ? H86A C86 H86B 108.5 . . ? C38 C37 C42 120.0 . . ? C38 C37 P1 124.5(13) . . ? C42 C37 P1 115.5(13) . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 120.0 . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 120.0 . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C44 C43 C48 120.0 . . ? C44 C43 P1 119(2) . . ? C48 C43 P1 121(2) . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C50 C49 C54 120.0 . . ? C50 C49 P2 117.9(14) . . ? C54 C49 P2 122.0(14) . . ? C51 C50 C49 120.0 . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 120.0 . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 H54 120.0 . . ? C49 C54 H54 120.0 . . ? C56 C55 C60 120.0 . . ? C56 C55 P2 117.1(16) . . ? C60 C55 P2 122.8(17) . . ? C57 C56 C55 120.0 . . ? C57 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C58 C57 C56 120.0 . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C59 C58 C57 120.0 . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.0 . . ? C58 C59 H59 120.0 . . ? C60 C59 H59 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? N1A C7' H7'1 109.5 . . ? N1A C7' H7'2 109.5 . . ? H7'1 C7' H7'2 109.5 . . ? N1A C7' H7'3 109.5 . . ? H7'1 C7' H7'3 109.5 . . ? H7'2 C7' H7'3 109.5 . . ? N1A C8' H8'1 109.5 . . ? N1A C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? N1A C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? N1A C9' H9'1 109.5 . . ? N1A C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? N1A C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? N4 C34' H34D 109.5 . . ? N4 C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? N4 C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? N4 C35' H35D 109.5 . . ? N4 C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? N4 C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? N4 C36' H36D 109.5 . . ? N4 C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? N4 C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? C37' P1' C85' 108.1(11) . . ? C37' P1' C43' 103.9(11) . . ? C85' P1' C43' 101.7(13) . . ? C37' P1' Au1 117.4(7) . . ? C85' P1' Au1 113.5(9) . . ? C43' P1' Au1 110.7(9) . . ? C49' P2' C86' 103.7(12) . . ? C49' P2' C55' 105.9(10) . . ? C86' P2' C55' 104.6(12) . . ? C49' P2' Au2 112.3(7) . . ? C86' P2' Au2 114.0(9) . . ? C55' P2' Au2 115.3(8) . . ? C86' C85' P1' 117.4(18) . . ? C86' C85' H85C 108.0 . . ? P1' C85' H85C 108.0 . . ? C86' C85' H85D 108.0 . . ? P1' C85' H85D 108.0 . . ? H85C C85' H85D 107.2 . . ? C85' C86' P2' 113.5(17) . . ? C85' C86' H86C 108.9 . . ? P2' C86' H86C 108.9 . . ? C85' C86' H86D 108.9 . . ? P2' C86' H86D 108.9 . . ? H86C C86' H86D 107.7 . . ? C38' C37' C42' 120.0 . . ? C38' C37' P1' 118.5(10) . . ? C42' C37' P1' 120.3(9) . . ? C37' C38' C39' 120.0 . . ? C37' C38' H38' 120.0 . . ? C39' C38' H38' 120.0 . . ? C38' C39' C40' 120.0 . . ? C38' C39' H39' 120.0 . . ? C40' C39' H39' 120.0 . . ? C39' C40' C41' 120.0 . . ? C39' C40' H40' 120.0 . . ? C41' C40' H40' 120.0 . . ? C40' C41' C42' 120.0 . . ? C40' C41' H41' 120.0 . . ? C42' C41' H41' 120.0 . . ? C41' C42' C37' 120.0 . . ? C41' C42' H42' 120.0 . . ? C37' C42' H42' 120.0 . . ? C44' C43' C48' 120.0 . . ? C44' C43' P1' 127.3(17) . . ? C48' C43' P1' 112.6(17) . . ? C45' C44' C43' 120.0 . . ? C45' C44' H44' 120.0 . . ? C43' C44' H44' 120.0 . . ? C44' C45' C46' 120.0 . . ? C44' C45' H45' 120.0 . . ? C46' C45' H45' 120.0 . . ? C45' C46' C47' 120.0 . . ? C45' C46' H46' 120.0 . . ? C47' C46' H46' 120.0 . . ? C48' C47' C46' 120.0 . . ? C48' C47' H47' 120.0 . . ? C46' C47' H47' 120.0 . . ? C47' C48' C43' 120.0 . . ? C47' C48' H48' 120.0 . . ? C43' C48' H48' 120.0 . . ? C50' C49' C54' 120.0 . . ? C50' C49' P2' 118.1(12) . . ? C54' C49' P2' 121.6(12) . . ? C51' C50' C49' 120.0 . . ? C51' C50' H50' 120.0 . . ? C49' C50' H50' 120.0 . . ? C52' C51' C50' 120.0 . . ? C52' C51' H51' 120.0 . . ? C50' C51' H51' 120.0 . . ? C51' C52' C53' 120.0 . . ? C51' C52' H52' 120.0 . . ? C53' C52' H52' 120.0 . . ? C54' C53' C52' 120.0 . . ? C54' C53' H53' 120.0 . . ? C52' C53' H53' 120.0 . . ? C53' C54' C49' 120.0 . . ? C53' C54' H54' 120.0 . . ? C49' C54' H54' 120.0 . . ? C56' C55' C60' 120.0 . . ? C56' C55' P2' 122.3(12) . . ? C60' C55' P2' 117.1(12) . . ? C55' C56' C57' 120.0 . . ? C55' C56' H56' 120.0 . . ? C57' C56' H56' 120.0 . . ? C58' C57' C56' 120.0 . . ? C58' C57' H57' 120.0 . . ? C56' C57' H57' 120.0 . . ? C57' C58' C59' 120.0 . . ? C57' C58' H58' 120.0 . . ? C59' C58' H58' 120.0 . . ? C60' C59' C58' 120.0 . . ? C60' C59' H59' 120.0 . . ? C58' C59' H59' 120.0 . . ? C59' C60' C55' 120.0 . . ? C59' C60' H60' 120.0 . . ? C55' C60' H60' 120.0 . . ? C62 C61 C66 120.2(14) . . ? C62 C61 P4 121.5(12) . . ? C66 C61 P4 118.3(11) . . ? C63 C62 C61 119.8(16) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 120.8(16) . . ? C62 C63 H63 119.6 . . ? C64 C63 H63 119.6 . . ? C65 C64 C63 119.7(17) . . ? C65 C64 H64 120.2 . . ? C63 C64 H64 120.2 . . ? C64 C65 C66 120.2(19) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C61 C66 C65 119.3(15) . . ? C61 C66 H66 120.4 . . ? C65 C66 H66 120.4 . . ? C72 C67 C68 118.1(13) . . ? C72 C67 P4 123.1(10) . . ? C68 C67 P4 118.7(12) . . ? C69 C68 C67 119.9(17) . . ? C69 C68 H68 120.0 . . ? C67 C68 H68 120.0 . . ? C70 C69 C68 120.2(19) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C69 C70 C71 121.0(16) . . ? C69 C70 H70 119.5 . . ? C71 C70 H70 119.5 . . ? C72 C71 C70 120.3(17) . . ? C72 C71 H71 119.8 . . ? C70 C71 H71 119.8 . . ? C71 C72 C67 120.2(16) . . ? C71 C72 H72 119.9 . . ? C67 C72 H72 119.9 . . ? C78 C73 C74 120.2(12) . . ? C78 C73 P3 122.8(10) . . ? C74 C73 P3 116.5(10) . . ? C73 C74 C75 119.1(14) . . ? C73 C74 H74 120.4 . . ? C75 C74 H74 120.4 . . ? C74 C75 C76 120.2(14) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C77 C76 C75 120.0(14) . . ? C77 C76 H76 120.0 . . ? C75 C76 H76 120.0 . . ? C76 C77 C78 119.0(14) . . ? C76 C77 H77 120.5 . . ? C78 C77 H77 120.5 . . ? C73 C78 C77 121.4(13) . . ? C73 C78 H78 119.3 . . ? C77 C78 H78 119.3 . . ? C80 C79 C84 116.9(13) . . ? C80 C79 P3 122.6(11) . . ? C84 C79 P3 120.5(11) . . ? C79 C80 C81 122.7(15) . . ? C79 C80 H80 118.6 . . ? C81 C80 H80 118.6 . . ? C82 C81 C80 119.9(17) . . ? C82 C81 H81 120.0 . . ? C80 C81 H81 120.0 . . ? C81 C82 C83 118.9(17) . . ? C81 C82 H82 120.5 . . ? C83 C82 H82 120.5 . . ? C84 C83 C82 121.1(18) . . ? C84 C83 H83 119.5 . . ? C82 C83 H83 119.5 . . ? C83 C84 C79 120.4(16) . . ? C83 C84 H84 119.8 . . ? C79 C84 H84 119.8 . . ? C88 C87 P4 114.0(9) . . ? C88 C87 H87A 108.8 . . ? P4 C87 H87A 108.8 . . ? C88 C87 H87B 108.8 . . ? P4 C87 H87B 108.8 . . ? H87A C87 H87B 107.6 . . ? C87 C88 P3 110.8(9) . . ? C87 C88 H88A 109.5 . . ? P3 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? P3 C88 H88B 109.5 . . ? H88A C88 H88B 108.1 . . ? C79 P3 C73 106.1(6) . . ? C79 P3 C88 104.2(6) . . ? C73 P3 C88 105.6(6) . . ? C79 P3 Au3 119.8(5) . . ? C73 P3 Au3 104.8(4) . . ? C88 P3 Au3 115.2(5) . . ? C87 P4 C67 103.9(6) . . ? C87 P4 C61 106.9(6) . . ? C67 P4 C61 108.1(6) . . ? C87 P4 Au4 111.5(4) . . ? C67 P4 Au4 112.3(4) . . ? C61 P4 Au4 113.5(5) . . ? F5 P5 F1 89.6(9) . . ? F5 P5 F3 91.2(8) . . ? F1 P5 F3 91.3(8) . . ? F5 P5 F2 179.6(10) . . ? F1 P5 F2 90.2(9) . . ? F3 P5 F2 89.1(8) . . ? F5 P5 F6 89.3(8) . . ? F1 P5 F6 90.1(8) . . ? F3 P5 F6 178.6(9) . . ? F2 P5 F6 90.4(7) . . ? F5 P5 F4 93.0(9) . . ? F1 P5 F4 176.5(9) . . ? F3 P5 F4 90.9(8) . . ? F2 P5 F4 87.2(8) . . ? F6 P5 F4 87.7(7) . . ? F7 P6 F7 180.0(8) 2_476 . ? F7 P6 F8 91.0(9) 2_476 . ? F7 P6 F8 89.0(9) . . ? F7 P6 F8 89.0(9) 2_476 2_476 ? F7 P6 F8 91.0(9) . 2_476 ? F8 P6 F8 180.000(5) . 2_476 ? F7 P6 F9 92.0(7) 2_476 2_476 ? F7 P6 F9 88.0(7) . 2_476 ? F8 P6 F9 88.9(7) . 2_476 ? F8 P6 F9 91.1(7) 2_476 2_476 ? F7 P6 F9 88.0(7) 2_476 . ? F7 P6 F9 92.0(7) . . ? F8 P6 F9 91.1(7) . . ? F8 P6 F9 88.9(7) 2_476 . ? F9 P6 F9 180.000(4) 2_476 . ? F13 P7 F11 175.7(11) . . ? F13 P7 F10 90.5(10) . . ? F11 P7 F10 92.8(12) . . ? F13 P7 F12 92.4(11) . . ? F11 P7 F12 90.2(10) . . ? F10 P7 F12 91.6(13) . . ? F13 P7 F15 88.4(9) . . ? F11 P7 F15 88.1(10) . . ? F10 P7 F15 176.2(12) . . ? F12 P7 F15 92.0(11) . . ? F13 P7 F14 86.4(10) . . ? F11 P7 F14 91.1(11) . . ? F10 P7 F14 87.5(12) . . ? F12 P7 F14 178.5(11) . . ? F15 P7 F14 88.9(9) . . ? F20 P8 F18 88.5(8) . . ? F20 P8 F16 89.5(7) . . ? F18 P8 F16 90.2(7) . . ? F20 P8 F21 89.3(8) . . ? F18 P8 F21 177.7(9) . . ? F16 P8 F21 90.2(8) . . ? F20 P8 F17 178.2(7) . . ? F18 P8 F17 91.0(8) . . ? F16 P8 F17 92.2(7) . . ? F21 P8 F17 91.3(8) . . ? F20 P8 F19 89.3(6) . . ? F18 P8 F19 90.4(7) . . ? F16 P8 F19 178.6(7) . . ? F21 P8 F19 89.1(8) . . ? F17 P8 F19 89.0(6) . . ? F27 P9 F24 89.4(10) . . ? F27 P9 F22 90.1(10) . . ? F24 P9 F22 179.0(12) . . ? F27 P9 F26 178.6(12) . . ? F24 P9 F26 90.5(10) . . ? F22 P9 F26 89.9(10) . . ? F27 P9 F25 91.0(10) . . ? F24 P9 F25 91.0(10) . . ? F22 P9 F25 90.0(10) . . ? F26 P9 F25 90.4(10) . . ? F27 P9 F23 89.6(10) . . ? F24 P9 F23 89.4(10) . . ? F22 P9 F23 89.7(9) . . ? F26 P9 F23 89.0(9) . . ? F25 P9 F23 179.3(12) . . ? P9 F22 F22 138(4) . 2_775 ? C9' N1A C7 78(2) . . ? C9' N1A C8 140(3) . . ? C7 N1A C8 110(3) . . ? C9' N1A C4 108(2) . . ? C7 N1A C4 111(2) . . ? C8 N1A C4 105(2) . . ? C9' N1A C8' 109(2) . . ? C7 N1A C8' 132(3) . . ? C8 N1A C8' 36(2) . . ? C4 N1A C8' 111.5(19) . . ? C9' N1A C7' 112(2) . . ? C7 N1A C7' 36(2) . . ? C8 N1A C7' 76(2) . . ? C4 N1A C7' 108.9(19) . . ? C8' N1A C7' 107(2) . . ? C9' N1A C9 23(2) . . ? C7 N1A C9 100(3) . . ? C8 N1A C9 123(3) . . ? C4 N1A C9 108(3) . . ? C8' N1A C9 89(3) . . ? C7' N1A C9 131(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 C8' H8'1 F12 0.97 2.48 3.43(4) 167.5 . C5 H5 F24 0.94 2.49 2.89(5) 105.9 1_455 C5 H5 F26 0.94 2.21 3.00(4) 140.1 1_455 C27 H27A F24 0.97 2.44 3.02(4) 118.1 1_455 C16 H16C F20 0.97 2.50 3.45(2) 164.9 1_655 C34' H34D F8 0.97 2.54 3.50(4) 169.4 1_645 C41' H41' F5 0.94 2.47 3.286(19) 145.0 2_575 C76 H76 F19 0.94 2.43 3.216(18) 140.5 1_565 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.432 _refine_diff_density_min -3.494 _refine_diff_density_rms 0.174 #===END #============================================================================== data_2^.^0.5MeOH^.^4H~2~O _database_code_depnum_ccdc_archive 'CCDC 779818' #TrackingRef '- JPLangCIF (re-revised).cif' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C45 H52 Au2 N2 P2 S2), 4(H2 O), 0.5(C H4 O), 2(Cl)' _chemical_formula_sum 'C45.50 H62 Au2 Cl2 N2 O4.50 P2 S2' _chemical_formula_weight 1299.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.706(3) _cell_length_b 29.885(8) _cell_length_c 21.926(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.251(11) _cell_angle_gamma 90.00 _cell_volume 5529(3) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14352 _cell_measurement_theta_min 3.0140 _cell_measurement_theta_max 27.5087 _exptl_crystal_description prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2556 _exptl_absorpt_coefficient_mu 5.570 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1349 _exptl_absorpt_correction_T_max 0.6642 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23216 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.1119 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.45 _reflns_number_total 11978 _reflns_number_gt 7547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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^)+(0.0731P)^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 11978 _refine_ls_number_parameters 544 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.086 _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 0.08570(5) 0.757142(15) 0.24529(2) 0.04094(15) Uani 1 1 d . . . Au2 Au 0.72752(5) 0.754747(14) 0.24318(2) 0.03860(15) Uani 1 1 d . . . S1 S 0.1022(3) 0.80586(12) 0.32868(16) 0.0557(9) Uani 1 1 d . . . S2 S 0.7351(3) 0.81968(10) 0.18573(17) 0.0523(8) Uani 1 1 d . . . P1 P 0.0820(3) 0.70726(10) 0.16606(14) 0.0390(7) Uani 1 1 d . . . P2 P 0.7026(3) 0.68824(10) 0.29077(14) 0.0393(7) Uani 1 1 d . . . C1 C 0.2981(11) 0.8277(4) 0.3543(5) 0.042(3) Uani 1 1 d . . . C2 C 0.3250(13) 0.8628(4) 0.3974(6) 0.051(3) Uani 1 1 d . . . H2C H 0.2394 0.8727 0.4130 0.061 Uiso 1 1 calc R . . C3 C 0.4649(12) 0.8835(4) 0.4181(6) 0.051(3) Uani 1 1 d . . . H3C H 0.4773 0.9067 0.4478 0.061 Uiso 1 1 calc R . . C4 C 0.5899(13) 0.8697(4) 0.3948(5) 0.043(3) Uani 1 1 d . . . C5 C 0.5718(14) 0.8350(4) 0.3518(6) 0.054(3) Uani 1 1 d . . . H5A H 0.6578 0.8257 0.3361 0.065 Uiso 1 1 calc R . . C6 C 0.4282(13) 0.8145(4) 0.3324(6) 0.054(3) Uani 1 1 d . . . H6A H 0.4167 0.7908 0.3035 0.065 Uiso 1 1 calc R . . C7 C 0.8653(12) 0.8563(4) 0.4552(6) 0.055(3) Uani 1 1 d . . . H7A H 0.8709 0.8295 0.4307 0.082 Uiso 1 1 calc R . . H7B H 0.8253 0.8486 0.4914 0.082 Uiso 1 1 calc R . . H7C H 0.9703 0.8692 0.4693 0.082 Uiso 1 1 calc R . . C8 C 0.7520(13) 0.9321(4) 0.4523(7) 0.062(4) Uani 1 1 d . . . H8A H 0.6846 0.9545 0.4268 0.093 Uiso 1 1 calc R . . H8B H 0.8590 0.9437 0.4662 0.093 Uiso 1 1 calc R . . H8C H 0.7117 0.9251 0.4887 0.093 Uiso 1 1 calc R . . C9 C 0.8149(15) 0.9048(5) 0.3584(7) 0.074(4) Uani 1 1 d . . . H9A H 0.7447 0.9272 0.3343 0.111 Uiso 1 1 calc R . . H9B H 0.8193 0.8791 0.3319 0.111 Uiso 1 1 calc R . . H9C H 0.9203 0.9174 0.3733 0.111 Uiso 1 1 calc R . . C10 C 0.5649(12) 0.8514(4) 0.1881(6) 0.046(3) Uani 1 1 d . . . C11 C 0.5818(13) 0.8962(4) 0.1999(7) 0.060(4) Uani 1 1 d . . . H11A H 0.6818 0.9095 0.2045 0.072 Uiso 1 1 calc R . . C12 C 0.4533(13) 0.9228(4) 0.2053(6) 0.058(4) Uani 1 1 d . . . H12A H 0.4660 0.9538 0.2117 0.070 Uiso 1 1 calc R . . C13 C 0.3063(12) 0.9028(4) 0.2012(6) 0.045(3) Uani 1 1 d . . . C14 C 0.2909(12) 0.8596(4) 0.1889(7) 0.058(4) Uani 1 1 d . . . H14A H 0.1915 0.8461 0.1853 0.069 Uiso 1 1 calc R . . C15 C 0.4142(13) 0.8336(4) 0.1814(7) 0.058(4) Uani 1 1 d . . . H15A H 0.3968 0.8031 0.1715 0.070 Uiso 1 1 calc R . . C16 C 0.0272(15) 0.9059(5) 0.2095(9) 0.096(6) Uani 1 1 d . . . H16A H -0.0526 0.9257 0.2185 0.145 Uiso 1 1 calc R . . H16B H 0.0506 0.8824 0.2410 0.145 Uiso 1 1 calc R . . H16C H -0.0119 0.8927 0.1682 0.145 Uiso 1 1 calc R . . C17 C 0.2202(16) 0.9528(5) 0.2770(7) 0.084(5) Uani 1 1 d . . . H17A H 0.1329 0.9710 0.2829 0.126 Uiso 1 1 calc R . . H17B H 0.3141 0.9712 0.2818 0.126 Uiso 1 1 calc R . . H17C H 0.2410 0.9290 0.3082 0.126 Uiso 1 1 calc R . . C18 C 0.1436(15) 0.9671(5) 0.1647(6) 0.068(4) Uani 1 1 d . . . H18A H 0.0605 0.9862 0.1726 0.103 Uiso 1 1 calc R . . H18B H 0.1091 0.9540 0.1231 0.103 Uiso 1 1 calc R . . H18C H 0.2385 0.9847 0.1671 0.103 Uiso 1 1 calc R . . C19 C -0.1032(11) 0.6771(4) 0.1360(5) 0.036(2) Uani 1 1 d . . . C20 C -0.2397(13) 0.7022(4) 0.1102(5) 0.048(3) Uani 1 1 d . . . H20A H -0.2327 0.7335 0.1101 0.058 Uiso 1 1 calc R . . C21 C -0.3830(14) 0.6823(5) 0.0850(6) 0.065(4) Uani 1 1 d . . . H21A H -0.4729 0.6996 0.0672 0.078 Uiso 1 1 calc R . . C22 C -0.3920(15) 0.6371(5) 0.0865(6) 0.064(4) Uani 1 1 d . . . H22A H -0.4900 0.6231 0.0697 0.077 Uiso 1 1 calc R . . C23 C -0.2637(15) 0.6117(5) 0.1114(6) 0.066(4) Uani 1 1 d . . . H23A H -0.2741 0.5804 0.1130 0.079 Uiso 1 1 calc R . . C24 C -0.1132(14) 0.6319(4) 0.1353(6) 0.056(3) Uani 1 1 d . . . H24A H -0.0223 0.6143 0.1503 0.067 Uiso 1 1 calc R . . C25 C 0.1219(13) 0.7331(4) 0.0958(6) 0.047(3) Uani 1 1 d . . . C26 C 0.0807(18) 0.7775(5) 0.0841(8) 0.076(4) Uani 1 1 d . . . H26 H 0.0333 0.7937 0.1114 0.091 Uiso 1 1 calc R . . C27 C 0.111(2) 0.7984(7) 0.0297(10) 0.115(7) Uani 1 1 d . . . H27A H 0.0875 0.8287 0.0202 0.138 Uiso 1 1 calc R . . C28 C 0.180(2) 0.7710(9) -0.0091(9) 0.105(8) Uani 1 1 d . . . H28A H 0.2059 0.7838 -0.0444 0.126 Uiso 1 1 calc R . . C29 C 0.2086(19) 0.7288(7) 0.0024(8) 0.086(5) Uani 1 1 d . . . H29A H 0.2480 0.7117 -0.0263 0.103 Uiso 1 1 calc R . . C30 C 0.1833(14) 0.7085(5) 0.0546(6) 0.064(4) Uani 1 1 d . . . H30A H 0.2075 0.6780 0.0623 0.077 Uiso 1 1 calc R . . C31 C 0.8737(12) 0.6521(4) 0.3026(5) 0.040(3) Uani 1 1 d . . . C32 C 0.8661(13) 0.6091(4) 0.2825(6) 0.047(3) Uani 1 1 d . . . H32A H 0.7675 0.5966 0.2626 0.056 Uiso 1 1 calc R . . C33 C 1.0016(16) 0.5836(4) 0.2911(6) 0.064(4) Uani 1 1 d . . . H33A H 0.9961 0.5543 0.2753 0.077 Uiso 1 1 calc R . . C34 C 1.1476(14) 0.6016(5) 0.3234(7) 0.069(4) Uani 1 1 d . . . H34A H 1.2404 0.5843 0.3296 0.082 Uiso 1 1 calc R . . C35 C 1.1543(14) 0.6450(5) 0.3462(6) 0.058(3) Uani 1 1 d . . . H35A H 1.2505 0.6573 0.3694 0.069 Uiso 1 1 calc R . . C36 C 1.0167(13) 0.6699(4) 0.3341(6) 0.051(3) Uani 1 1 d . . . H36 H 1.0209 0.6998 0.3477 0.062 Uiso 1 1 calc R . . C37 C 0.6664(12) 0.6930(4) 0.3681(5) 0.043(2) Uani 1 1 d U . . C38 C 0.715(2) 0.7305(5) 0.4031(7) 0.083(4) Uani 1 1 d U . . H38A H 0.7622 0.7540 0.3859 0.099 Uiso 1 1 calc R . . C39 C 0.695(3) 0.7344(6) 0.4626(8) 0.105(6) Uani 1 1 d U . . H39A H 0.7324 0.7601 0.4864 0.126 Uiso 1 1 calc R . . C40 C 0.622(2) 0.7017(7) 0.4880(7) 0.095(5) Uani 1 1 d U . . H40A H 0.6058 0.7053 0.5285 0.114 Uiso 1 1 calc R . . C41 C 0.5733(19) 0.6637(7) 0.4547(7) 0.099(5) Uani 1 1 d U . . H41A H 0.5229 0.6411 0.4724 0.119 Uiso 1 1 calc R . . C42 C 0.5973(18) 0.6576(6) 0.3934(6) 0.084(5) Uani 1 1 d U . . H42A H 0.5680 0.6310 0.3708 0.100 Uiso 1 1 calc R . . C43 C 0.2372(11) 0.6660(4) 0.1928(5) 0.042(3) Uani 1 1 d . . . H43A H 0.2048 0.6448 0.2213 0.050 Uiso 1 1 calc R . . H43B H 0.2544 0.6492 0.1566 0.050 Uiso 1 1 calc R . . C44 C 0.3907(11) 0.6891(4) 0.2267(5) 0.048(3) Uani 1 1 d . . . H44A H 0.3759 0.7024 0.2657 0.057 Uiso 1 1 calc R . . H44B H 0.4125 0.7135 0.2002 0.057 Uiso 1 1 calc R . . C45 C 0.5350(11) 0.6578(4) 0.2428(5) 0.046(3) Uani 1 1 d . . . H45A H 0.5604 0.6473 0.2040 0.055 Uiso 1 1 calc R . . H45B H 0.5114 0.6316 0.2659 0.055 Uiso 1 1 calc R . . N1 N 0.7531(11) 0.8905(3) 0.4140(5) 0.047(2) Uani 1 1 d . . . N2 N 0.1771(11) 0.9323(3) 0.2109(6) 0.061(3) Uani 1 1 d . . . Cl1 Cl -0.4913(5) 0.54307(13) 0.2903(3) 0.133(2) Uani 1 1 d . . . Cl2 Cl 0.2113(5) 0.92178(19) 0.5389(3) 0.145(3) Uani 1 1 d . . . O1 O -0.1820(10) 0.9897(3) 0.2539(5) 0.087(3) Uani 1 1 d . . . H1A H -0.1871 0.9896 0.2921 0.131 Uiso 1 1 d R . . H1B H -0.2757 0.9958 0.2331 0.131 Uiso 1 1 d R . . O2 O 0.0389(12) 0.9772(4) 0.6251(6) 0.115(4) Uani 1 1 d . . . O4 O -0.256(3) 1.0118(8) 0.5725(8) 0.130(11) Uani 0.50 1 d P A 1 H4A H -0.2802 1.0150 0.5327 0.195 Uiso 0.50 1 d PR A 1 H4B H -0.1592 1.0042 0.5815 0.195 Uiso 0.50 1 d PR A 1 O3 O -0.5369(18) 0.9783(6) 0.6375(10) 0.260(13) Uani 1 1 d . B 1 H3A H -0.5628 0.9810 0.5977 0.390 Uiso 1 1 d R B 1 H3B H -0.4406 0.9701 0.6456 0.390 Uiso 1 1 d R B 1 O5 O 0.055(4) 1.0789(13) -0.0101(19) 0.197(15) Uiso 0.50 1 d P C 1 O6 O -0.287(4) 1.0715(14) -0.0184(19) 0.216(17) Uiso 0.50 1 d P D 1 C46 C 0.116(5) 1.0658(16) 0.050(2) 0.142(17) Uiso 0.50 1 d P . . 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 0.0312(2) 0.0438(3) 0.0460(3) -0.00881(19) 0.0059(2) -0.00258(18) Au2 0.0315(2) 0.0349(2) 0.0485(3) 0.00076(18) 0.0082(2) 0.00380(17) S1 0.0389(15) 0.066(2) 0.062(2) -0.0310(18) 0.0115(14) -0.0055(15) S2 0.0451(16) 0.0382(15) 0.078(2) 0.0125(16) 0.0243(15) 0.0069(13) P1 0.0366(14) 0.0390(15) 0.0399(17) -0.0060(13) 0.0064(12) -0.0054(12) P2 0.0336(14) 0.0372(15) 0.0437(17) 0.0037(13) 0.0027(12) 0.0038(12) C1 0.031(5) 0.055(7) 0.040(7) -0.013(6) 0.007(5) -0.004(5) C2 0.048(7) 0.054(7) 0.052(8) -0.015(6) 0.015(6) 0.001(6) C3 0.040(6) 0.051(7) 0.064(8) -0.022(6) 0.013(6) 0.002(6) C4 0.046(6) 0.050(7) 0.030(6) 0.002(5) 0.003(5) 0.003(5) C5 0.048(7) 0.056(8) 0.059(8) -0.019(7) 0.013(6) -0.005(6) C6 0.043(6) 0.059(8) 0.057(8) -0.028(7) 0.006(6) 0.001(6) C7 0.037(6) 0.065(8) 0.061(8) -0.009(7) 0.008(6) 0.007(6) C8 0.045(7) 0.059(8) 0.082(10) -0.014(8) 0.014(7) -0.003(6) C9 0.067(9) 0.077(10) 0.084(11) -0.004(9) 0.031(8) -0.014(8) C10 0.041(6) 0.039(6) 0.060(8) 0.000(6) 0.013(5) -0.005(5) C11 0.042(6) 0.037(6) 0.111(12) -0.010(7) 0.036(7) -0.018(5) C12 0.044(7) 0.037(6) 0.088(10) -0.006(7) 0.006(7) -0.010(6) C13 0.032(5) 0.045(6) 0.064(8) 0.010(6) 0.020(5) 0.004(5) C14 0.028(5) 0.036(6) 0.111(12) 0.000(7) 0.020(6) -0.002(5) C15 0.041(6) 0.034(6) 0.104(11) -0.001(7) 0.027(7) -0.004(5) C16 0.052(8) 0.057(9) 0.185(19) 0.018(11) 0.038(10) 0.003(7) C17 0.061(9) 0.095(13) 0.098(13) -0.016(11) 0.022(8) 0.011(9) C18 0.069(8) 0.074(10) 0.067(9) 0.025(8) 0.026(7) 0.025(8) C19 0.030(5) 0.049(6) 0.030(6) -0.012(5) 0.010(4) -0.003(5) C20 0.051(7) 0.055(7) 0.039(7) 0.005(6) 0.012(5) -0.007(6) C21 0.034(6) 0.095(12) 0.062(9) -0.024(9) 0.005(6) -0.018(7) C22 0.048(7) 0.097(12) 0.051(8) -0.009(8) 0.018(6) -0.036(8) C23 0.065(8) 0.070(9) 0.059(9) -0.013(7) 0.008(7) -0.039(8) C24 0.056(7) 0.054(8) 0.054(8) 0.006(7) 0.007(6) -0.011(6) C25 0.032(6) 0.063(8) 0.049(7) -0.003(6) 0.017(5) -0.001(6) C26 0.098(11) 0.051(8) 0.085(12) 0.020(8) 0.035(9) 0.003(8) C27 0.127(17) 0.089(14) 0.116(18) 0.052(13) 0.005(13) -0.024(13) C28 0.067(11) 0.18(2) 0.069(13) 0.040(16) 0.016(9) -0.014(14) C29 0.076(11) 0.127(17) 0.048(10) 0.015(11) 0.004(8) 0.006(12) C30 0.049(7) 0.095(11) 0.045(8) 0.023(8) 0.008(6) 0.018(7) C31 0.046(6) 0.038(6) 0.041(7) -0.003(5) 0.021(5) 0.001(5) C32 0.045(6) 0.037(6) 0.058(8) 0.007(6) 0.011(6) 0.002(5) C33 0.090(10) 0.042(7) 0.070(10) 0.015(7) 0.039(8) 0.018(7) C34 0.039(7) 0.084(11) 0.089(11) 0.020(9) 0.029(7) 0.028(7) C35 0.039(6) 0.065(9) 0.062(9) -0.004(7) -0.001(6) 0.006(6) C36 0.048(7) 0.049(7) 0.057(8) 0.008(6) 0.013(6) 0.014(6) C37 0.034(5) 0.060(7) 0.033(6) 0.004(5) 0.007(4) 0.013(5) C38 0.144(13) 0.064(8) 0.040(7) -0.003(6) 0.024(8) -0.003(8) C39 0.192(17) 0.079(10) 0.053(9) -0.010(8) 0.047(10) 0.010(10) C40 0.109(12) 0.141(14) 0.046(9) -0.013(8) 0.039(8) 0.003(10) C41 0.104(11) 0.148(14) 0.056(9) -0.005(9) 0.042(9) -0.043(11) C42 0.098(10) 0.114(11) 0.039(7) -0.003(7) 0.020(7) -0.041(9) C43 0.043(6) 0.043(6) 0.038(6) -0.002(5) 0.006(5) -0.001(5) C44 0.047(6) 0.050(7) 0.050(7) -0.002(6) 0.018(5) 0.008(6) C45 0.033(5) 0.059(7) 0.043(7) -0.012(6) 0.003(5) 0.009(5) N1 0.050(5) 0.046(6) 0.045(6) -0.006(5) 0.014(5) 0.003(5) N2 0.046(6) 0.045(6) 0.087(9) 0.006(6) 0.009(6) -0.005(5) Cl1 0.063(2) 0.047(2) 0.287(8) 0.014(3) 0.041(3) 0.005(2) Cl2 0.080(3) 0.115(4) 0.207(6) -0.065(4) -0.025(3) 0.014(3) O1 0.069(6) 0.069(7) 0.130(10) 0.000(7) 0.038(6) -0.006(6) O2 0.097(8) 0.107(10) 0.128(11) -0.005(9) 0.001(7) -0.034(7) O4 0.22(2) 0.13(2) 0.031(11) 0.007(12) 0.021(13) 0.14(2) O3 0.175(14) 0.148(16) 0.35(3) -0.113(17) -0.129(16) 0.071(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.283(3) . ? Au1 S1 2.314(3) . ? Au1 Au2 3.1080(12) 1_455 ? Au2 P2 2.280(3) . ? Au2 S2 2.323(3) . ? Au2 Au1 3.1080(12) 1_655 ? S1 C1 1.783(10) . ? S2 C10 1.771(11) . ? P1 C43 1.818(11) . ? P1 C19 1.822(10) . ? P1 C25 1.830(13) . ? P2 C37 1.804(12) . ? P2 C31 1.805(11) . ? P2 C45 1.819(11) . ? C1 C6 1.391(14) . ? C1 C2 1.394(14) . ? C2 C3 1.341(14) . ? C2 H2C 0.9400 . ? C3 C4 1.375(14) . ? C3 H3C 0.9400 . ? C4 C5 1.383(15) . ? C4 N1 1.513(14) . ? C5 C6 1.363(15) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 N1 1.545(14) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 N1 1.502(14) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 N1 1.510(15) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C10 C11 1.363(15) . ? C10 C15 1.390(14) . ? C11 C12 1.401(15) . ? C11 H11A 0.9400 . ? C12 C13 1.396(14) . ? C12 H12A 0.9400 . ? C13 C14 1.319(15) . ? C13 N2 1.486(14) . ? C14 C15 1.368(15) . ? C14 H14A 0.9400 . ? C15 H15A 0.9400 . ? C16 N2 1.519(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 N2 1.532(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 N2 1.431(15) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 C24 1.354(15) . ? C19 C20 1.400(14) . ? C20 C21 1.369(15) . ? C20 H20A 0.9400 . ? C21 C22 1.352(19) . ? C21 H21A 0.9400 . ? C22 C23 1.351(18) . ? C22 H22A 0.9400 . ? C23 C24 1.422(15) . ? C23 H23A 0.9400 . ? C24 H24A 0.9400 . ? C25 C30 1.371(17) . ? C25 C26 1.383(18) . ? C26 C27 1.43(2) . ? C26 H26 0.9400 . ? C27 C28 1.41(3) . ? C27 H27A 0.9400 . ? C28 C29 1.30(3) . ? C28 H28A 0.9400 . ? C29 C30 1.361(19) . ? C29 H29A 0.9400 . ? C30 H30A 0.9400 . ? C31 C32 1.355(14) . ? C31 C36 1.373(15) . ? C32 C33 1.378(15) . ? C32 H32A 0.9400 . ? C33 C34 1.401(18) . ? C33 H33A 0.9400 . ? C34 C35 1.387(18) . ? C34 H34A 0.9400 . ? C35 C36 1.378(15) . ? C35 H35A 0.9400 . ? C36 H36 0.9400 . ? C37 C38 1.365(17) . ? C37 C42 1.396(18) . ? C38 C39 1.36(2) . ? C38 H38A 0.9400 . ? C39 C40 1.36(2) . ? C39 H39A 0.9400 . ? C40 C41 1.36(2) . ? C40 H40A 0.9400 . ? C41 C42 1.422(19) . ? C41 H41A 0.9400 . ? C42 H42A 0.9400 . ? C43 C44 1.525(14) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C44 C45 1.536(14) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? O1 H1A 0.8503 . ? O1 H1B 0.8500 . ? O4 H4A 0.8499 . ? O4 H4B 0.8500 . ? O3 H3A 0.8501 . ? O3 H3B 0.8499 . ? O5 C46 1.34(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 P1 Au1 S1 176.85(11) . . ? P1 Au1 Au2 98.47(7) . 1_455 ? S1 Au1 Au2 83.86(7) . 1_455 ? P2 Au2 S2 174.23(11) . . ? P2 Au2 Au1 102.79(7) . 1_655 ? S2 Au2 Au1 80.01(7) . 1_655 ? C1 S1 Au1 110.3(4) . . ? C10 S2 Au2 107.2(4) . . ? C43 P1 C19 107.6(5) . . ? C43 P1 C25 106.1(5) . . ? C19 P1 C25 103.8(5) . . ? C43 P1 Au1 109.2(4) . . ? C19 P1 Au1 116.3(3) . . ? C25 P1 Au1 113.2(4) . . ? C37 P2 C31 103.9(5) . . ? C37 P2 C45 106.4(5) . . ? C31 P2 C45 107.4(5) . . ? C37 P2 Au2 114.8(4) . . ? C31 P2 Au2 114.8(4) . . ? C45 P2 Au2 109.0(4) . . ? C6 C1 C2 115.6(10) . . ? C6 C1 S1 125.8(9) . . ? C2 C1 S1 118.5(8) . . ? C3 C2 C1 124.2(11) . . ? C3 C2 H2C 117.9 . . ? C1 C2 H2C 117.9 . . ? C2 C3 C4 118.2(11) . . ? C2 C3 H3C 120.9 . . ? C4 C3 H3C 120.9 . . ? C3 C4 C5 120.7(11) . . ? C3 C4 N1 123.2(11) . . ? C5 C4 N1 116.1(10) . . ? C6 C5 C4 119.5(12) . . ? C6 C5 H5A 120.3 . . ? C4 C5 H5A 120.3 . . ? C5 C6 C1 121.8(11) . . ? C5 C6 H6A 119.1 . . ? C1 C6 H6A 119.1 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 116.9(11) . . ? C11 C10 S2 118.6(8) . . ? C15 C10 S2 124.4(9) . . ? C10 C11 C12 121.4(10) . . ? C10 C11 H11A 119.3 . . ? C12 C11 H11A 119.3 . . ? C13 C12 C11 119.4(11) . . ? C13 C12 H12A 120.3 . . ? C11 C12 H12A 120.3 . . ? C14 C13 C12 118.6(11) . . ? C14 C13 N2 124.7(10) . . ? C12 C13 N2 116.8(11) . . ? C13 C14 C15 122.5(11) . . ? C13 C14 H14A 118.7 . . ? C15 C14 H14A 118.7 . . ? C14 C15 C10 121.1(11) . . ? C14 C15 H15A 119.4 . . ? C10 C15 H15A 119.4 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 118.9(10) . . ? C24 C19 P1 123.1(9) . . ? C20 C19 P1 118.0(9) . . ? C21 C20 C19 122.0(12) . . ? C21 C20 H20A 119.0 . . ? C19 C20 H20A 119.0 . . ? C22 C21 C20 118.4(13) . . ? C22 C21 H21A 120.8 . . ? C20 C21 H21A 120.8 . . ? C23 C22 C21 121.7(12) . . ? C23 C22 H22A 119.2 . . ? C21 C22 H22A 119.2 . . ? C22 C23 C24 120.3(13) . . ? C22 C23 H23A 119.9 . . ? C24 C23 H23A 119.9 . . ? C19 C24 C23 118.7(12) . . ? C19 C24 H24A 120.6 . . ? C23 C24 H24A 120.6 . . ? C30 C25 C26 121.1(13) . . ? C30 C25 P1 120.9(11) . . ? C26 C25 P1 117.9(10) . . ? C25 C26 C27 118.8(16) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? C28 C27 C26 116.2(18) . . ? C28 C27 H27A 121.9 . . ? C26 C27 H27A 121.9 . . ? C29 C28 C27 122.4(18) . . ? C29 C28 H28A 118.8 . . ? C27 C28 H28A 118.8 . . ? C28 C29 C30 122.2(19) . . ? C28 C29 H29A 118.9 . . ? C30 C29 H29A 118.9 . . ? C29 C30 C25 119.1(16) . . ? C29 C30 H30A 120.5 . . ? C25 C30 H30A 120.5 . . ? C32 C31 C36 119.7(11) . . ? C32 C31 P2 123.2(9) . . ? C36 C31 P2 117.1(9) . . ? C31 C32 C33 120.6(11) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C32 C33 C34 119.8(12) . . ? C32 C33 H33A 120.1 . . ? C34 C33 H33A 120.1 . . ? C35 C34 C33 119.5(12) . . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 120.2 . . ? C36 C35 C34 118.5(12) . . ? C36 C35 H35A 120.7 . . ? C34 C35 H35A 120.7 . . ? C31 C36 C35 121.8(12) . . ? C31 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? C38 C37 C42 120.1(13) . . ? C38 C37 P2 119.5(11) . . ? C42 C37 P2 120.4(10) . . ? C39 C38 C37 121.0(17) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C40 C39 C38 120.9(18) . . ? C40 C39 H39A 119.5 . . ? C38 C39 H39A 119.5 . . ? C39 C40 C41 119.8(16) . . ? C39 C40 H40A 120.1 . . ? C41 C40 H40A 120.1 . . ? C40 C41 C42 120.9(16) . . ? C40 C41 H41A 119.5 . . ? C42 C41 H41A 119.5 . . ? C37 C42 C41 117.2(16) . . ? C37 C42 H42A 121.4 . . ? C41 C42 H42A 121.4 . . ? C44 C43 P1 110.0(8) . . ? C44 C43 H43A 109.7 . . ? P1 C43 H43A 109.7 . . ? C44 C43 H43B 109.7 . . ? P1 C43 H43B 109.7 . . ? H43A C43 H43B 108.2 . . ? C43 C44 C45 113.9(10) . . ? C43 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? C43 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C44 C45 P2 108.8(8) . . ? C44 C45 H45A 109.9 . . ? P2 C45 H45A 109.9 . . ? C44 C45 H45B 109.9 . . ? P2 C45 H45B 109.9 . . ? H45A C45 H45B 108.3 . . ? C8 N1 C9 105.7(10) . . ? C8 N1 C4 111.2(9) . . ? C9 N1 C4 112.9(9) . . ? C8 N1 C7 108.1(9) . . ? C9 N1 C7 111.1(9) . . ? C4 N1 C7 107.7(9) . . ? C18 N2 C13 111.1(11) . . ? C18 N2 C16 109.8(10) . . ? C13 N2 C16 111.4(10) . . ? C18 N2 C17 109.8(11) . . ? C13 N2 C17 110.8(9) . . ? C16 N2 C17 103.7(12) . . ? H1A O1 H1B 104.6 . . ? H4A O4 H4B 104.4 . . ? H3A O3 H3B 103.9 . . ? 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 O1 H1B Cl1 0.85 2.42 3.197(10) 151.9 2_455 O4 H4B O2 0.85 1.93 2.75(2) 160.5 . C7 H7C Cl2 0.97 2.76 3.681(12) 158.6 1_655 C45 H45B Cl1 0.98 2.70 3.607(13) 153.8 1_655 C12 H12A Cl1 0.94 2.68 3.609(13) 170.8 2 C16 H16A O1 0.97 2.44 3.378(18) 162.4 . C18 H18C Cl1 0.97 2.78 3.717(15) 162.0 2 O1 H1A O2 0.85 2.19 2.818(16) 130.8 3_576 O4 H4A Cl2 0.85 2.62 3.24(2) 131.3 3_576 O3 H3A Cl2 0.85 2.72 3.163(14) 113.7 1_455 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 2.530 _refine_diff_density_min -2.912 _refine_diff_density_rms 0.182 #===END #============================================================================== data_3^.^4DMF _database_code_depnum_ccdc_archive 'CCDC 779819' #TrackingRef '- JPLangCIF (re-revised).cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H80 Au4 N4 P2 S4, C5 H11 N2 O2, 2(C3 H7 N O), 4(F6 P)' _chemical_formula_sum 'C75 H105 Au4 F24 N8 O4 P6 S4' _chemical_formula_weight 2740.60 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.778(3) _cell_length_b 37.260(8) _cell_length_c 8.9963(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.35(3) _cell_angle_gamma 90.00 _cell_volume 4873.0(17) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 9973 _cell_measurement_theta_min 3.0083 _cell_measurement_theta_max 27.4971 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.868 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2658 _exptl_absorpt_coefficient_mu 6.281 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1988 _exptl_absorpt_correction_T_max 0.5723 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16366 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8421 _reflns_number_gt 6452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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. Since the methyl groups of DMF are likely to rotate over the symmetry axis, the C---N bond length was refined as 1.45\%A. The thermal parameter for the disordered methyl groups and one DMF solvent molecule were refined the same. One phenyl group of the dppb ligand for C7 to C12 and one phenyl group of the Tab ligand for C24, C27, C28 were refined the same in the style of movement as they are likely to rotate. ; _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^)+(0.0380P)^2^+18.4985P] 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 8421 _refine_ls_number_parameters 563 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.1086 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.1545 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.002 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 0.45757(4) 0.452642(15) 0.00189(6) 0.04407(17) Uani 1 1 d . . . Au2 Au 0.65122(4) 0.481674(14) 0.12801(6) 0.04216(16) Uani 1 1 d . . . N1 N 0.1592(10) 0.3039(3) 0.0429(16) 0.065(4) Uani 1 1 d . . . N2 N 0.7409(13) 0.3025(4) -0.085(2) 0.089(6) Uani 1 1 d . . . N3 N 0.5460(15) 0.1548(7) -0.237(3) 0.146(8) Uani 1 1 d U . . N4 N 1.0148(15) 0.4281(7) 0.082(3) 0.159(14) Uani 1 1 d D . . P1 P 0.7042(2) 0.50206(10) 0.3656(4) 0.0393(8) Uani 1 1 d . . . P2 P 0.3686(4) 0.1858(2) 0.0971(7) 0.0901(18) Uani 1 1 d . . . P3 P -0.0502(4) 0.19300(13) -0.0229(6) 0.0688(13) Uani 1 1 d . . . F1 F 0.0543(9) 0.1922(5) -0.0001(18) 0.174(7) Uani 1 1 d . . . F2 F -0.1543(9) 0.1977(5) -0.0375(18) 0.161(7) Uani 1 1 d . . . F3 F -0.0397(11) 0.2233(3) 0.1020(16) 0.144(6) Uani 1 1 d . . . F4 F -0.0623(16) 0.1628(3) -0.1391(15) 0.198(9) Uani 1 1 d . . . F5 F -0.0496(9) 0.2209(3) -0.1532(15) 0.121(5) Uani 1 1 d . . . F6 F -0.0494(9) 0.1649(3) 0.1116(12) 0.104(4) Uani 1 1 d . . . F7 F 0.3923(16) 0.2243(6) 0.129(4) 0.283(14) Uani 1 1 d . . . F8 F 0.2728(11) 0.1911(6) 0.138(2) 0.216(10) Uani 1 1 d . . . F9 F 0.4056(13) 0.1708(9) 0.2510(19) 0.275(15) Uani 1 1 d . . . F10 F 0.4660(11) 0.1826(6) 0.0568(19) 0.206(10) Uani 1 1 d . . . F11 F 0.3283(11) 0.1999(6) -0.0585(16) 0.190(8) Uani 1 1 d . . . F12 F 0.3480(19) 0.1479(5) 0.049(4) 0.305(15) Uani 1 1 d . . . O1 O 0.6419(17) 0.1978(7) -0.209(4) 0.276(16) Uani 1 1 d U . . O2 O 0.9683(11) 0.3708(5) 0.008(2) 0.118(6) Uani 1 1 d . . . C1 C 0.7530(9) 0.4669(4) 0.4963(15) 0.039(3) Uani 1 1 d . . . C2 C 0.7681(10) 0.4334(4) 0.4414(19) 0.056(4) Uani 1 1 d . . . H2A H 0.7544 0.4285 0.3373 0.067 Uiso 1 1 calc R . . C3 C 0.8050(11) 0.4064(5) 0.547(2) 0.072(5) Uani 1 1 d . . . H3A H 0.8140 0.3830 0.5129 0.087 Uiso 1 1 calc R . . C4 C 0.8274(11) 0.4139(5) 0.698(2) 0.074(6) Uani 1 1 d . . . H4A H 0.8532 0.3960 0.7660 0.089 Uiso 1 1 calc R . . C5 C 0.8125(11) 0.4469(5) 0.7475(19) 0.065(5) Uani 1 1 d . . . H5A H 0.8273 0.4517 0.8516 0.078 Uiso 1 1 calc R . . C6 C 0.7762(10) 0.4738(4) 0.6507(17) 0.056(4) Uani 1 1 d . . . H6A H 0.7670 0.4968 0.6884 0.067 Uiso 1 1 calc R . . C7 C 0.7936(9) 0.5359(4) 0.3789(16) 0.044(3) Uani 1 1 d U . . C8 C 0.7767(12) 0.5722(4) 0.4000(16) 0.057(4) Uani 1 1 d U . . H8A H 0.7169 0.5795 0.4077 0.068 Uiso 1 1 calc R . . C9 C 0.8451(11) 0.5974(4) 0.4097(19) 0.063(5) Uani 1 1 d . . . H9A H 0.8321 0.6218 0.4218 0.075 Uiso 1 1 calc R . . C10 C 0.9326(13) 0.5865(5) 0.402(2) 0.085(6) Uani 1 1 d . . . H10A H 0.9796 0.6037 0.4054 0.102 Uiso 1 1 calc R . . C11 C 0.9519(12) 0.5510(5) 0.388(3) 0.108(8) Uani 1 1 d U . . H11A H 1.0127 0.5438 0.3866 0.129 Uiso 1 1 calc R . . C12 C 0.8836(10) 0.5257(5) 0.376(2) 0.089(6) Uani 1 1 d U . . H12A H 0.8978 0.5013 0.3664 0.106 Uiso 1 1 calc R . . C13 C 0.6112(8) 0.5206(4) 0.4486(14) 0.040(3) Uani 1 1 d . . . H13A H 0.6362 0.5304 0.5486 0.048 Uiso 1 1 calc R . . H13B H 0.5822 0.5404 0.3852 0.048 Uiso 1 1 calc R . . C14 C 0.5401(8) 0.4928(4) 0.4635(15) 0.042(3) Uani 1 1 d . . . H14A H 0.5698 0.4729 0.5248 0.050 Uiso 1 1 calc R . . H14B H 0.5149 0.4833 0.3629 0.050 Uiso 1 1 calc R . . C15 C 0.2856(10) 0.4081(4) 0.0979(16) 0.049(4) Uani 1 1 d . . . C16 C 0.2897(11) 0.3877(4) -0.0279(17) 0.059(4) Uani 1 1 d . A . H16A H 0.3208 0.3966 -0.1026 0.071 Uiso 1 1 calc R . . C17 C 0.2478(11) 0.3536(4) -0.0467(18) 0.061(4) Uani 1 1 d . . . H17A H 0.2499 0.3401 -0.1341 0.073 Uiso 1 1 calc R A . C18 C 0.2039(10) 0.3404(4) 0.0636(17) 0.048(4) Uani 1 1 d . A . C19 C 0.2018(11) 0.3610(4) 0.1904(18) 0.062(4) Uani 1 1 d . . . H19A H 0.1717 0.3522 0.2666 0.074 Uiso 1 1 calc R A . C20 C 0.2436(11) 0.3943(4) 0.2067(15) 0.054(4) Uani 1 1 d . A . H20A H 0.2428 0.4077 0.2952 0.064 Uiso 1 1 calc R . . C21 C 0.2361(18) 0.2768(7) 0.064(3) 0.052(8) Uiso 0.60(4) 1 d PU A 1 H21A H 0.2604 0.2739 0.1705 0.078 Uiso 0.60(4) 1 calc PR A 1 H21B H 0.2846 0.2850 0.0123 0.078 Uiso 0.60(4) 1 calc PR A 1 H21C H 0.2129 0.2539 0.0213 0.078 Uiso 0.60(4) 1 calc PR A 1 C22 C 0.094(2) 0.2986(8) 0.159(3) 0.057(8) Uiso 0.60(4) 1 d PU A 1 H22A H 0.0571 0.3201 0.1622 0.086 Uiso 0.60(4) 1 calc PR A 1 H22B H 0.1300 0.2941 0.2584 0.086 Uiso 0.60(4) 1 calc PR A 1 H22C H 0.0535 0.2783 0.1289 0.086 Uiso 0.60(4) 1 calc PR A 1 C23 C 0.107(3) 0.3003(11) -0.109(4) 0.070(11) Uiso 0.60(4) 1 d PU A 1 H23A H 0.0545 0.3161 -0.1222 0.105 Uiso 0.60(4) 1 calc PR A 1 H23B H 0.0868 0.2756 -0.1263 0.105 Uiso 0.60(4) 1 calc PR A 1 H23C H 0.1462 0.3066 -0.1815 0.105 Uiso 0.60(4) 1 calc PR A 1 C21A C 0.221(5) 0.2765(19) -0.022(10) 0.14(3) Uiso 0.40(4) 1 d PU A 2 H21D H 0.2509 0.2883 -0.0962 0.216 Uiso 0.40(4) 1 calc PR A 2 H21E H 0.1834 0.2568 -0.0694 0.216 Uiso 0.40(4) 1 calc PR A 2 H21F H 0.2672 0.2672 0.0593 0.216 Uiso 0.40(4) 1 calc PR A 2 C22A C 0.137(4) 0.2898(14) 0.177(5) 0.074(15) Uiso 0.40(4) 1 d PU A 2 H22D H 0.0927 0.3054 0.2128 0.111 Uiso 0.40(4) 1 calc PR A 2 H22E H 0.1923 0.2883 0.2539 0.111 Uiso 0.40(4) 1 calc PR A 2 H22F H 0.1108 0.2660 0.1583 0.111 Uiso 0.40(4) 1 calc PR A 2 C23A C 0.080(4) 0.3057(17) -0.085(7) 0.078(17) Uiso 0.40(4) 1 d PU A 2 H23D H 0.0357 0.3233 -0.0623 0.117 Uiso 0.40(4) 1 calc PR A 2 H23E H 0.0504 0.2824 -0.0996 0.117 Uiso 0.40(4) 1 calc PR A 2 H23F H 0.1013 0.3127 -0.1765 0.117 Uiso 0.40(4) 1 calc PR A 2 C24 C 0.6299(8) 0.4092(3) -0.0906(14) 0.033(3) Uani 1 1 d . . . C25 C 0.7058(11) 0.3990(4) 0.0116(18) 0.063(5) Uani 1 1 d . A . H25A H 0.7365 0.4158 0.0809 0.076 Uiso 1 1 calc R . . C26 C 0.7373(13) 0.3639(5) 0.0127(19) 0.080(6) Uani 1 1 d . . . H26A H 0.7882 0.3572 0.0858 0.096 Uiso 1 1 calc R A . C27 C 0.6983(12) 0.3394(4) -0.086(2) 0.062(4) Uani 1 1 d U A . C28 C 0.6262(14) 0.3498(4) -0.192(3) 0.107(8) Uani 1 1 d U . . H28A H 0.5991 0.3332 -0.2647 0.129 Uiso 1 1 calc R A . C29 C 0.5917(12) 0.3840(5) -0.195(2) 0.083(6) Uani 1 1 d . A . H29A H 0.5413 0.3903 -0.2701 0.099 Uiso 1 1 calc R . . C30 C 0.784(3) 0.2892(12) 0.050(5) 0.112(16) Uiso 0.60(4) 1 d P A 1 H30A H 0.7419 0.2899 0.1213 0.168 Uiso 0.60(4) 1 calc PR A 1 H30B H 0.8376 0.3037 0.0878 0.168 Uiso 0.60(4) 1 calc PR A 1 H30C H 0.8025 0.2646 0.0370 0.168 Uiso 0.60(4) 1 calc PR A 1 C31 C 0.812(3) 0.3041(11) -0.200(4) 0.103(14) Uiso 0.60(4) 1 d P A 1 H31A H 0.8554 0.3235 -0.1711 0.154 Uiso 0.60(4) 1 calc PR A 1 H31B H 0.7787 0.3082 -0.3017 0.154 Uiso 0.60(4) 1 calc PR A 1 H31C H 0.8450 0.2815 -0.1969 0.154 Uiso 0.60(4) 1 calc PR A 1 C32 C 0.682(3) 0.2784(13) -0.152(6) 0.126(17) Uiso 0.60(4) 1 d P A 1 H32A H 0.6354 0.2740 -0.0912 0.188 Uiso 0.60(4) 1 calc PR A 1 H32B H 0.7144 0.2562 -0.1640 0.188 Uiso 0.60(4) 1 calc PR A 1 H32C H 0.6532 0.2872 -0.2509 0.188 Uiso 0.60(4) 1 calc PR A 1 C30A C 0.826(4) 0.2981(14) 0.034(6) 0.074(15) Uiso 0.40(4) 1 d P A 2 H30D H 0.8088 0.2964 0.1324 0.111 Uiso 0.40(4) 1 calc PR A 2 H30E H 0.8661 0.3187 0.0314 0.111 Uiso 0.40(4) 1 calc PR A 2 H30F H 0.8583 0.2764 0.0137 0.111 Uiso 0.40(4) 1 calc PR A 2 C31A C 0.753(4) 0.2915(14) -0.229(5) 0.079(17) Uiso 0.40(4) 1 d P A 2 H31D H 0.7022 0.2765 -0.2741 0.119 Uiso 0.40(4) 1 calc PR A 2 H31E H 0.8102 0.2780 -0.2200 0.119 Uiso 0.40(4) 1 calc PR A 2 H31F H 0.7566 0.3124 -0.2917 0.119 Uiso 0.40(4) 1 calc PR A 2 C32A C 0.656(3) 0.2761(14) -0.063(6) 0.079(16) Uiso 0.40(4) 1 d P A 2 H32D H 0.6325 0.2832 0.0273 0.118 Uiso 0.40(4) 1 calc PR A 2 H32E H 0.6771 0.2515 -0.0519 0.118 Uiso 0.40(4) 1 calc PR A 2 H32F H 0.6066 0.2780 -0.1500 0.118 Uiso 0.40(4) 1 calc PR A 2 C33 C 0.478(3) 0.1628(15) -0.340(6) 0.138(15) Uani 0.50 1 d PU . . H33A H 0.4874 0.1862 -0.3815 0.207 Uiso 0.50 1 calc PR . . H33B H 0.4219 0.1632 -0.2974 0.207 Uiso 0.50 1 calc PR . . H33C H 0.4715 0.1450 -0.4202 0.207 Uiso 0.50 1 calc PR . . C34 C 0.5332(18) 0.1182(8) -0.164(3) 0.167(11) Uani 1 1 d U . . H34A H 0.4773 0.1069 -0.2160 0.251 Uiso 1 1 calc R . . H34B H 0.5287 0.1218 -0.0584 0.251 Uiso 1 1 calc R . . H34C H 0.5855 0.1029 -0.1700 0.251 Uiso 1 1 calc R . . C35 C 0.622(2) 0.1689(9) -0.169(4) 0.174(12) Uani 1 1 d U . . H35A H 0.6603 0.1566 -0.0912 0.209 Uiso 1 1 calc R . . C36 C 1.077(2) 0.4566(8) 0.059(6) 0.35(4) Uani 1 1 d D . . H36A H 1.1119 0.4495 -0.0175 0.528 Uiso 1 1 calc R . . H36B H 1.1185 0.4615 0.1530 0.528 Uiso 1 1 calc R . . H36C H 1.0418 0.4781 0.0261 0.528 Uiso 1 1 calc R . . C37 C 0.950(3) 0.4293(12) 0.184(3) 0.25(3) Uani 1 1 d D . . H37A H 0.9580 0.4516 0.2404 0.378 Uiso 1 1 calc R . . H37B H 0.9616 0.4093 0.2539 0.378 Uiso 1 1 calc R . . H37C H 0.8882 0.4278 0.1273 0.378 Uiso 1 1 calc R . . C38 C 1.017(2) 0.3996(11) 0.001(5) 0.169(16) Uani 1 1 d . . . H38A H 1.0572 0.3996 -0.0687 0.203 Uiso 1 1 calc R . . S1 S 0.3337(3) 0.45187(11) 0.1222(5) 0.0547(10) Uani 1 1 d . . . S2 S 0.5899(3) 0.45429(10) -0.1055(4) 0.0449(9) 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 0.0494(3) 0.0367(3) 0.0460(3) -0.0001(3) 0.0083(3) 0.0047(3) Au2 0.0470(3) 0.0370(3) 0.0430(3) -0.0034(3) 0.0097(2) 0.0036(3) N1 0.077(10) 0.042(8) 0.072(10) 0.007(7) 0.008(8) -0.010(7) N2 0.143(16) 0.032(8) 0.087(12) -0.017(8) 0.006(11) 0.020(9) N3 0.094(13) 0.190(19) 0.16(2) -0.060(16) 0.042(12) -0.069(14) N4 0.094(16) 0.097(17) 0.26(4) -0.07(2) -0.037(19) 0.055(14) P1 0.0383(19) 0.0355(19) 0.044(2) -0.0029(16) 0.0072(16) 0.0012(16) P2 0.079(4) 0.109(5) 0.083(4) 0.014(4) 0.017(3) 0.012(4) P3 0.074(3) 0.047(3) 0.084(4) 0.003(3) 0.011(3) 0.003(2) F1 0.085(9) 0.27(2) 0.176(15) 0.079(15) 0.056(10) 0.041(11) F2 0.085(9) 0.237(19) 0.158(14) 0.034(13) 0.013(9) 0.014(10) F3 0.210(16) 0.072(8) 0.139(12) -0.019(9) -0.002(11) -0.023(9) F4 0.45(3) 0.054(8) 0.093(10) -0.032(7) 0.051(14) -0.002(13) F5 0.142(11) 0.094(9) 0.127(11) 0.052(8) 0.026(9) 0.006(8) F6 0.157(11) 0.060(7) 0.088(8) 0.002(6) 0.000(8) -0.010(7) F7 0.24(2) 0.139(18) 0.46(4) -0.13(2) 0.03(3) -0.020(17) F8 0.143(13) 0.26(2) 0.28(2) 0.173(18) 0.127(14) 0.087(14) F9 0.177(17) 0.54(4) 0.117(13) 0.13(2) 0.063(12) 0.19(2) F10 0.126(13) 0.33(3) 0.180(16) 0.114(17) 0.063(12) 0.101(16) F11 0.166(15) 0.31(3) 0.091(10) 0.065(14) 0.000(10) 0.032(15) F12 0.33(3) 0.097(15) 0.46(5) -0.05(2) 0.00(3) -0.005(17) O1 0.16(2) 0.16(2) 0.48(4) -0.03(2) -0.02(2) -0.069(16) O2 0.100(12) 0.119(14) 0.131(14) -0.014(12) 0.011(11) 0.006(10) C1 0.035(7) 0.041(7) 0.039(8) 0.002(6) 0.006(6) -0.008(6) C2 0.053(9) 0.041(8) 0.066(11) -0.012(8) -0.009(8) 0.007(7) C3 0.053(10) 0.049(10) 0.112(16) 0.021(11) 0.007(11) -0.001(8) C4 0.051(10) 0.068(12) 0.099(15) 0.038(12) 0.000(11) -0.001(9) C5 0.053(10) 0.091(14) 0.050(10) 0.009(10) 0.004(8) 0.003(10) C6 0.052(9) 0.064(11) 0.050(9) 0.007(8) 0.002(8) 0.009(8) C7 0.047(6) 0.037(7) 0.051(8) -0.003(6) 0.013(7) 0.000(6) C8 0.084(11) 0.041(7) 0.040(8) -0.006(7) -0.003(8) 0.007(7) C9 0.069(11) 0.038(9) 0.083(13) -0.017(8) 0.020(10) -0.003(8) C10 0.079(13) 0.079(14) 0.094(15) 0.009(12) 0.012(12) -0.042(12) C11 0.056(9) 0.060(11) 0.21(2) -0.003(14) 0.027(13) -0.024(9) C12 0.044(8) 0.049(9) 0.178(17) 0.000(11) 0.032(11) -0.010(6) C13 0.040(7) 0.045(8) 0.038(7) -0.010(6) 0.016(6) 0.003(6) C14 0.046(8) 0.046(8) 0.035(7) 0.000(6) 0.011(6) 0.006(7) C15 0.061(10) 0.038(8) 0.045(9) -0.003(7) -0.004(7) 0.006(7) C16 0.076(11) 0.058(10) 0.045(9) -0.002(8) 0.017(8) -0.021(9) C17 0.073(11) 0.056(10) 0.059(10) -0.016(8) 0.023(9) -0.011(9) C18 0.056(9) 0.033(8) 0.050(9) 0.010(7) -0.003(8) -0.005(7) C19 0.080(12) 0.053(10) 0.057(10) -0.007(8) 0.025(9) -0.010(9) C20 0.091(12) 0.047(9) 0.033(8) -0.012(7) 0.038(8) 0.000(8) C24 0.033(7) 0.031(7) 0.036(7) 0.002(6) 0.009(6) 0.006(6) C25 0.079(12) 0.047(9) 0.060(10) -0.023(8) -0.002(9) 0.012(9) C26 0.103(15) 0.074(13) 0.054(11) -0.008(10) -0.007(10) 0.035(11) C27 0.072(11) 0.033(8) 0.081(12) -0.005(8) 0.017(8) 0.011(8) C28 0.124(16) 0.036(9) 0.136(18) -0.038(11) -0.044(13) 0.008(10) C29 0.069(12) 0.078(13) 0.086(14) -0.031(11) -0.028(11) 0.014(10) C33 0.06(2) 0.22(4) 0.15(4) -0.05(3) 0.052(15) -0.08(3) C34 0.13(2) 0.17(2) 0.22(3) -0.06(2) 0.07(2) -0.037(18) C35 0.111(18) 0.16(2) 0.23(3) -0.06(2) -0.012(18) -0.043(17) C36 0.18(3) 0.08(2) 0.73(11) 0.06(4) -0.09(5) -0.02(2) C37 0.24(4) 0.42(7) 0.10(2) -0.03(3) 0.04(3) 0.15(5) C38 0.09(2) 0.17(3) 0.23(4) 0.09(3) -0.02(3) 0.02(2) S1 0.059(2) 0.042(2) 0.066(3) -0.008(2) 0.020(2) -0.0020(19) S2 0.057(2) 0.0387(19) 0.0391(19) 0.0000(16) 0.0097(17) 0.0065(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 S1 2.289(4) . ? Au1 S2 2.333(4) . ? Au1 Au2 3.0439(9) 3_665 ? Au1 Au2 3.0791(11) . ? Au2 P1 2.271(4) . ? Au2 S2 2.365(3) . ? Au2 Au1 3.0439(9) 3_665 ? N1 C22A 1.41(5) . ? N1 C23 1.45(4) . ? N1 C23A 1.49(5) . ? N1 C21 1.51(3) . ? N1 C18 1.512(17) . ? N1 C21A 1.55(7) . ? N1 C22 1.56(3) . ? N2 C32 1.32(4) . ? N2 C30 1.36(4) . ? N2 C31A 1.40(5) . ? N2 C30A 1.51(5) . ? N2 C27 1.515(18) . ? N2 C31 1.60(4) . ? N2 C32A 1.64(5) . ? N3 C33 1.28(5) . ? N3 C35 1.29(3) . ? N3 C34 1.54(3) . ? N4 C38 1.29(4) . ? N4 C37 1.439(10) . ? N4 C36 1.443(10) . ? P1 C7 1.814(14) . ? P1 C13 1.815(12) . ? P1 C1 1.820(13) . ? P2 F7 1.491(18) . ? P2 F12 1.493(19) . ? P2 F9 1.502(15) . ? P2 F11 1.512(13) . ? P2 F8 1.536(15) . ? P2 F10 1.551(16) . ? P3 F1 1.521(13) . ? P3 F4 1.523(12) . ? P3 F2 1.529(13) . ? P3 F5 1.569(12) . ? P3 F3 1.582(13) . ? P3 F6 1.599(11) . ? O1 C35 1.19(4) . ? O2 C38 1.30(3) . ? C1 C2 1.377(18) . ? C1 C6 1.393(18) . ? C2 C3 1.43(2) . ? C2 H2A 0.9400 . ? C3 C4 1.36(2) . ? C3 H3A 0.9400 . ? C4 C5 1.34(2) . ? C4 H4A 0.9400 . ? C5 C6 1.37(2) . ? C5 H5A 0.9400 . ? C6 H6A 0.9400 . ? C7 C12 1.39(2) . ? C7 C8 1.393(18) . ? C8 C9 1.37(2) . ? C8 H8A 0.9400 . ? C9 C10 1.37(2) . ? C9 H9A 0.9400 . ? C10 C11 1.36(2) . ? C10 H10A 0.9400 . ? C11 C12 1.37(2) . ? C11 H11A 0.9400 . ? C12 H12A 0.9400 . ? C13 C14 1.500(18) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C14 1.55(2) 3_666 ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C20 1.351(19) . ? C15 C16 1.373(19) . ? C15 S1 1.777(14) . ? C16 C17 1.410(19) . ? C16 H16A 0.9400 . ? C17 C18 1.37(2) . ? C17 H17A 0.9400 . ? C18 C19 1.38(2) . ? C19 C20 1.384(19) . ? C19 H19A 0.9400 . ? C20 H20A 0.9400 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? C21A H21D 0.9700 . ? C21A H21E 0.9700 . ? C21A H21F 0.9700 . ? C22A H22D 0.9700 . ? C22A H22E 0.9700 . ? C22A H22F 0.9700 . ? C23A H23D 0.9700 . ? C23A H23E 0.9700 . ? C23A H23F 0.9700 . ? C24 C25 1.370(17) . ? C24 C29 1.376(18) . ? C24 S2 1.779(12) . ? C25 C26 1.39(2) . ? C25 H25A 0.9400 . ? C26 C27 1.33(2) . ? C26 H26A 0.9400 . ? C27 C28 1.35(2) . ? C28 C29 1.37(2) . ? C28 H28A 0.9400 . ? C29 H29A 0.9400 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C30 H30C 0.9700 . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 H32C 0.9700 . ? C30A H30D 0.9700 . ? C30A H30E 0.9700 . ? C30A H30F 0.9700 . ? C31A H31D 0.9700 . ? C31A H31E 0.9700 . ? C31A H31F 0.9700 . ? C32A H32D 0.9700 . ? C32A H32E 0.9700 . ? C32A H32F 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C33 H33C 0.9700 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 H34C 0.9700 . ? C35 H35A 0.9400 . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C36 H36C 0.9700 . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C37 H37C 0.9700 . ? C38 H38A 0.9400 . ? 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 S1 Au1 S2 176.24(13) . . ? S1 Au1 Au2 77.26(10) . 3_665 ? S2 Au1 Au2 104.13(9) . 3_665 ? S1 Au1 Au2 126.85(10) . . ? S2 Au1 Au2 49.49(9) . . ? Au2 Au1 Au2 104.53(3) 3_665 . ? P1 Au2 S2 173.13(13) . . ? P1 Au2 Au1 99.30(9) . 3_665 ? S2 Au2 Au1 85.07(9) . 3_665 ? P1 Au2 Au1 127.23(10) . . ? S2 Au2 Au1 48.59(10) . . ? Au1 Au2 Au1 75.47(3) 3_665 . ? C22A N1 C23 128(3) . . ? C22A N1 C23A 114(3) . . ? C23 N1 C23A 21(3) . . ? C22A N1 C21 86(2) . . ? C23 N1 C21 108(2) . . ? C23A N1 C21 127(3) . . ? C22A N1 C18 113(2) . . ? C23 N1 C18 110.2(18) . . ? C23A N1 C18 109(3) . . ? C21 N1 C18 106.6(14) . . ? C22A N1 C21A 109(3) . . ? C23 N1 C21A 80(3) . . ? C23A N1 C21A 100(4) . . ? C21 N1 C21A 29(3) . . ? C18 N1 C21A 111(3) . . ? C22A N1 C22 27(2) . . ? C23 N1 C22 110(2) . . ? C23A N1 C22 91(3) . . ? C21 N1 C22 112.2(18) . . ? C18 N1 C22 109.9(16) . . ? C21A N1 C22 130(3) . . ? C32 N2 C30 109(3) . . ? C32 N2 C31A 64(3) . . ? C30 N2 C31A 127(3) . . ? C32 N2 C30A 130(3) . . ? C30 N2 C30A 30(3) . . ? C31A N2 C30A 113(3) . . ? C32 N2 C27 112(2) . . ? C30 N2 C27 117(2) . . ? C31A N2 C27 113(2) . . ? C30A N2 C27 113(2) . . ? C32 N2 C31 101(3) . . ? C30 N2 C31 110(3) . . ? C31A N2 C31 37(2) . . ? C30A N2 C31 84(3) . . ? C27 N2 C31 106.6(19) . . ? C32 N2 C32A 36(3) . . ? C30 N2 C32A 85(3) . . ? C31A N2 C32A 100(3) . . ? C30A N2 C32A 114(3) . . ? C27 N2 C32A 102(2) . . ? C31 N2 C32A 135(3) . . ? C33 N3 C35 139(4) . . ? C33 N3 C34 112(3) . . ? C35 N3 C34 109(3) . . ? C38 N4 C37 118(3) . . ? C38 N4 C36 117(3) . . ? C37 N4 C36 125(3) . . ? C7 P1 C13 107.7(6) . . ? C7 P1 C1 104.9(6) . . ? C13 P1 C1 104.5(6) . . ? C7 P1 Au2 114.8(5) . . ? C13 P1 Au2 110.8(4) . . ? C1 P1 Au2 113.4(5) . . ? F7 P2 F12 174.0(19) . . ? F7 P2 F9 98.4(16) . . ? F12 P2 F9 86.2(15) . . ? F7 P2 F11 83.5(14) . . ? F12 P2 F11 92.1(14) . . ? F9 P2 F11 177.8(16) . . ? F7 P2 F8 91.4(13) . . ? F12 P2 F8 92.4(14) . . ? F9 P2 F8 91.6(9) . . ? F11 P2 F8 87.1(9) . . ? F7 P2 F10 85.6(13) . . ? F12 P2 F10 90.5(14) . . ? F9 P2 F10 89.2(9) . . ? F11 P2 F10 92.2(9) . . ? F8 P2 F10 177.0(14) . . ? F1 P3 F4 93.9(11) . . ? F1 P3 F2 173.9(11) . . ? F4 P3 F2 91.9(11) . . ? F1 P3 F5 88.4(8) . . ? F4 P3 F5 89.6(8) . . ? F2 P3 F5 90.0(8) . . ? F1 P3 F3 87.2(9) . . ? F4 P3 F3 177.7(10) . . ? F2 P3 F3 87.0(9) . . ? F5 P3 F3 92.5(8) . . ? F1 P3 F6 90.8(8) . . ? F4 P3 F6 91.1(7) . . ? F2 P3 F6 90.6(8) . . ? F5 P3 F6 179.0(8) . . ? F3 P3 F6 86.8(7) . . ? C2 C1 C6 119.9(14) . . ? C2 C1 P1 119.5(11) . . ? C6 C1 P1 120.6(11) . . ? C1 C2 C3 118.0(15) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C4 C3 C2 120.8(17) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C5 C4 C3 119.8(17) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 121.8(17) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C5 C6 C1 119.6(16) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? C12 C7 C8 117.7(15) . . ? C12 C7 P1 119.8(11) . . ? C8 C7 P1 122.4(12) . . ? C9 C8 C7 121.7(16) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C10 C9 C8 119.1(16) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C11 C10 C9 120.4(17) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.7(19) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 120.3(17) . . ? C11 C12 H12A 119.9 . . ? C7 C12 H12A 119.9 . . ? C14 C13 P1 111.5(9) . . ? C14 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 108.0 . . ? C13 C14 C14 113.5(14) . 3_666 ? C13 C14 H14A 108.9 . . ? C14 C14 H14A 108.9 3_666 . ? C13 C14 H14B 108.9 . . ? C14 C14 H14B 108.9 3_666 . ? H14A C14 H14B 107.7 . . ? C20 C15 C16 118.8(14) . . ? C20 C15 S1 119.0(12) . . ? C16 C15 S1 122.2(13) . . ? C15 C16 C17 120.9(15) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 119.4(15) . . ? C18 C17 H17A 120.3 . . ? C16 C17 H17A 120.3 . . ? C17 C18 C19 118.9(14) . . ? C17 C18 N1 119.2(14) . . ? C19 C18 N1 121.9(15) . . ? C18 C19 C20 120.7(15) . . ? C18 C19 H19A 119.7 . . ? C20 C19 H19A 119.7 . . ? C15 C20 C19 121.2(14) . . ? C15 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 H22A 109.4 . . ? N1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C21A H21D 109.5 . . ? N1 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? N1 C21A H21F 109.4 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? N1 C22A H22D 109.4 . . ? N1 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? N1 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? N1 C23A H23D 109.5 . . ? N1 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? N1 C23A H23F 109.4 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C25 C24 C29 117.2(13) . . ? C25 C24 S2 122.1(10) . . ? C29 C24 S2 120.2(11) . . ? C24 C25 C26 119.8(14) . . ? C24 C25 H25A 120.1 . . ? C26 C25 H25A 120.1 . . ? C27 C26 C25 122.6(16) . . ? C27 C26 H26A 118.7 . . ? C25 C26 H26A 118.7 . . ? C26 C27 C28 117.7(15) . . ? C26 C27 N2 119.6(16) . . ? C28 C27 N2 122.4(15) . . ? C27 C28 C29 121.8(16) . . ? C27 C28 H28A 119.1 . . ? C29 C28 H28A 119.1 . . ? C28 C29 C24 120.8(15) . . ? C28 C29 H29A 119.6 . . ? C24 C29 H29A 119.6 . . ? N2 C30 H30A 109.4 . . ? N2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N2 C30 H30C 109.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 H31A 109.4 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N2 C32 H32A 109.6 . . ? N2 C32 H32B 109.4 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.4 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C30A H30D 109.4 . . ? N2 C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? N2 C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? N2 C31A H31D 109.6 . . ? N2 C31A H31E 109.4 . . ? H31D C31A H31E 109.5 . . ? N2 C31A H31F 109.4 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? N2 C32A H32D 109.5 . . ? N2 C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? N2 C32A H32F 109.4 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? N3 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O1 C35 N3 118(4) . . ? O1 C35 H35A 120.9 . . ? N3 C35 H35A 120.9 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 O2 126(4) . . ? N4 C38 H38A 117.2 . . ? O2 C38 H38A 117.2 . . ? C15 S1 Au1 106.8(6) . . ? C24 S2 Au1 103.6(4) . . ? C24 S2 Au2 105.8(4) . . ? Au1 S2 Au2 81.91(12) . . ? 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 C10 H10A F6 0.94 2.52 3.40(2) 157.1 2_655 C17 H17A F8 0.94 2.44 3.37(2) 173.0 4_565 C28 H28A F10 0.94 2.38 3.20(2) 146.3 4_565 C30A H30F F3 0.97 2.53 3.41(5) 151.5 1_655 C31 H31B F2 0.97 2.51 3.16(4) 125.0 4_665 C32A H32E O1 0.97 2.45 3.19(6) 133.1 . _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.120 _refine_diff_density_min -1.026 _refine_diff_density_rms 0.164 #===END #============================================================================== data_4^.^2DMF^.^4H~2~O _database_code_depnum_ccdc_archive 'CCDC 779820' #TrackingRef '- JPLangCIF (re-revised).cif' #============================================================================== # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H39 Au2 N3 S3, C3 H7 N O, 2(H2 O), 2(Cl)' _chemical_formula_sum 'C30 H50 Au2 Cl2 N4 O3 S3' _chemical_formula_weight 1075.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.740(3) _cell_length_b 9.0476(18) _cell_length_c 30.106(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.61(2) _cell_angle_gamma 90.00 _cell_volume 3799.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10967 _cell_measurement_theta_min 3.0546 _cell_measurement_theta_max 27.6491 _exptl_crystal_description prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2087 _exptl_absorpt_coefficient_mu 8.055 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.1191 _exptl_absorpt_correction_T_max 0.3098 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _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 'Rigaku MercuryCCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17747 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8660 _reflns_number_gt 7002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_cell_refinement 'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)' _computing_data_reduction 'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _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. As the methyl groups of the two Tab ligands are likely to rotate along the N center, the thermal parameter of them were refined the same. ; _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^)+(0.0441P)^2^+5.7880P] 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 8660 _refine_ls_number_parameters 357 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1183 _refine_ls_wR_factor_gt 0.1086 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.009 _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 0.86231(2) 0.67185(3) 0.478698(11) 0.03400(10) Uani 1 1 d . . . Au2 Au 1.11062(2) 0.66513(3) 0.518599(11) 0.03186(10) Uani 1 1 d . . . S1 S 0.96827(14) 0.66262(19) 0.44538(7) 0.0329(4) Uani 1 1 d . . . S2 S 0.75167(19) 0.6703(2) 0.50772(10) 0.0540(6) Uani 1 1 d . . . S3 S 1.25002(16) 0.6315(2) 0.59043(8) 0.0432(5) Uani 1 1 d . . . N1 N 0.9038(5) 1.2286(7) 0.3276(2) 0.0379(15) Uani 1 1 d . . . N2 N 0.8056(5) 1.2400(7) 0.6232(3) 0.0430(17) Uani 1 1 d . . . N3 N 1.4586(5) 1.2068(7) 0.6718(2) 0.0380(16) Uani 1 1 d . . . C1 C 0.9505(6) 0.8344(7) 0.4132(3) 0.0315(16) Uani 1 1 d . . . C2 C 0.9991(5) 0.9623(8) 0.4362(3) 0.0319(17) Uani 1 1 d . . . H2A H 1.0429 0.9617 0.4701 0.038 Uiso 1 1 calc R . . C3 C 0.9820(5) 1.0923(7) 0.4084(3) 0.0308(16) Uani 1 1 d . . . H3A H 1.0128 1.1793 0.4240 0.037 Uiso 1 1 calc R . . C4 C 0.9200(5) 1.0918(8) 0.3583(3) 0.0314(16) Uani 1 1 d . . . C5 C 0.8731(6) 0.9652(8) 0.3344(3) 0.0354(18) Uani 1 1 d . . . H5A H 0.8315 0.9660 0.3001 0.042 Uiso 1 1 calc R . . C6 C 0.8885(5) 0.8358(7) 0.3619(3) 0.0319(16) Uani 1 1 d . . . H6A H 0.8572 0.7494 0.3460 0.038 Uiso 1 1 calc R . . C7 C 0.9499(9) 1.3641(11) 0.3589(4) 0.0828(13) Uani 1 1 d . . . H7A H 0.9238 1.3810 0.3816 0.124 Uiso 1 1 calc R . . H7B H 0.9373 1.4483 0.3373 0.124 Uiso 1 1 calc R . . H7C H 1.0179 1.3491 0.3775 0.124 Uiso 1 1 calc R . . C8 C 0.9472(9) 1.2051(12) 0.2922(5) 0.0828(13) Uani 1 1 d . . . H8A H 0.9181 1.1205 0.2715 0.124 Uiso 1 1 calc R . . H8B H 1.0150 1.1891 0.3114 0.124 Uiso 1 1 calc R . . H8C H 0.9358 1.2910 0.2715 0.124 Uiso 1 1 calc R . . C9 C 0.7993(8) 1.2607(12) 0.2977(4) 0.0828(13) Uani 1 1 d . . . H9A H 0.7675 1.1769 0.2772 0.124 Uiso 1 1 calc R . . H9B H 0.7905 1.3454 0.2768 0.124 Uiso 1 1 calc R . . H9C H 0.7725 1.2806 0.3200 0.124 Uiso 1 1 calc R . . C10 C 0.7683(6) 0.8401(8) 0.5406(3) 0.041(2) Uani 1 1 d . . . C11 C 0.7520(7) 0.9755(9) 0.5169(3) 0.048(2) Uani 1 1 d . . . H11A H 0.7332 0.9784 0.4828 0.058 Uiso 1 1 calc R . . C12 C 0.7626(7) 1.1070(9) 0.5423(3) 0.046(2) Uani 1 1 d . . . H12A H 0.7513 1.1968 0.5255 0.056 Uiso 1 1 calc R . . C13 C 0.7904(6) 1.1031(9) 0.5932(3) 0.0396(19) Uani 1 1 d . . . C14 C 0.8068(7) 0.9701(10) 0.6175(3) 0.049(2) Uani 1 1 d . . . H14A H 0.8263 0.9678 0.6518 0.059 Uiso 1 1 calc R . . C15 C 0.7946(7) 0.8393(9) 0.5914(3) 0.046(2) Uani 1 1 d . . . H15A H 0.8043 0.7496 0.6082 0.056 Uiso 1 1 calc R . . C16 C 0.7425(7) 1.2382(10) 0.6481(4) 0.055(2) Uani 1 1 d . . . H16A H 0.7556 1.1510 0.6685 0.082 Uiso 1 1 calc R . . H16B H 0.6766 1.2380 0.6231 0.082 Uiso 1 1 calc R . . H16C H 0.7550 1.3243 0.6689 0.082 Uiso 1 1 calc R . . C17 C 0.9073(6) 1.2492(11) 0.6631(4) 0.063(3) Uani 1 1 d . . . H17A H 0.9491 1.2508 0.6479 0.095 Uiso 1 1 calc R . . H17B H 0.9220 1.1648 0.6848 0.095 Uiso 1 1 calc R . . H17C H 0.9161 1.3378 0.6823 0.095 Uiso 1 1 calc R . . C18 C 0.7847(8) 1.3772(9) 0.5920(4) 0.070(3) Uani 1 1 d . . . H18A H 0.8250 1.3801 0.5759 0.105 Uiso 1 1 calc R . . H18B H 0.7968 1.4625 0.6130 0.105 Uiso 1 1 calc R . . H18C H 0.7187 1.3768 0.5669 0.105 Uiso 1 1 calc R . . C19 C 1.3052(5) 0.8036(8) 0.6136(3) 0.0334(17) Uani 1 1 d . . . C20 C 1.4019(6) 0.8046(8) 0.6479(3) 0.043(2) Uani 1 1 d . . . H20A H 1.4341 0.7150 0.6581 0.051 Uiso 1 1 calc R . . C21 C 1.4511(6) 0.9323(9) 0.6672(3) 0.0399(19) Uani 1 1 d . . . H21A H 1.5162 0.9298 0.6898 0.048 Uiso 1 1 calc R . . C22 C 1.4032(5) 1.0656(8) 0.6528(3) 0.0314(16) Uani 1 1 d . . . C23 C 1.3070(5) 1.0685(8) 0.6202(3) 0.0346(17) Uani 1 1 d . . . H23A H 1.2739 1.1577 0.6114 0.042 Uiso 1 1 calc R . . C24 C 1.2601(6) 0.9371(8) 0.6006(3) 0.0363(18) Uani 1 1 d . . . H24A H 1.1953 0.9397 0.5777 0.044 Uiso 1 1 calc R . . C25 C 1.5133(9) 1.2292(12) 0.6430(4) 0.0828(13) Uani 1 1 d . . . H25A H 1.5506 1.3180 0.6542 0.124 Uiso 1 1 calc R . . H25B H 1.4693 1.2375 0.6079 0.124 Uiso 1 1 calc R . . H25C H 1.5551 1.1465 0.6482 0.124 Uiso 1 1 calc R . . C26 C 1.5277(9) 1.1980(11) 0.7245(4) 0.0828(13) Uani 1 1 d . . . H26A H 1.5617 1.2899 0.7349 0.124 Uiso 1 1 calc R . . H26B H 1.5722 1.1195 0.7294 0.124 Uiso 1 1 calc R . . H26C H 1.4948 1.1787 0.7439 0.124 Uiso 1 1 calc R . . C27 C 1.3995(9) 1.3362(11) 0.6647(5) 0.0828(13) Uani 1 1 d . . . H27A H 1.4397 1.4215 0.6777 0.124 Uiso 1 1 calc R . . H27B H 1.3619 1.3229 0.6820 0.124 Uiso 1 1 calc R . . H27C H 1.3577 1.3498 0.6295 0.124 Uiso 1 1 calc R . . O3 O 0.5484(7) 0.2647(12) 0.5409(4) 0.110(3) Uani 1 1 d . . . N4 N 0.4875(7) 0.2618(14) 0.4568(4) 0.094(3) Uani 1 1 d . . . C28 C 0.4324(9) 0.1764(11) 0.4124(5) 0.0828(13) Uani 1 1 d . . . H28A H 0.3973 0.1015 0.4196 0.124 Uiso 1 1 calc R . . H28B H 0.4746 0.1306 0.4016 0.124 Uiso 1 1 calc R . . H28C H 0.3883 0.2399 0.3864 0.124 Uiso 1 1 calc R . . C29 C 0.5408(9) 0.3810(12) 0.4525(4) 0.0828(13) Uani 1 1 d . . . H29A H 0.5741 0.4298 0.4844 0.124 Uiso 1 1 calc R . . H29B H 0.4983 0.4498 0.4280 0.124 Uiso 1 1 calc R . . H29C H 0.5864 0.3448 0.4423 0.124 Uiso 1 1 calc R . . C30 C 0.4984(10) 0.218(2) 0.5020(6) 0.102(5) Uani 1 1 d . . . H30 H 0.4603 0.1384 0.5016 0.122 Uiso 1 1 calc R . . Cl1 Cl 0.63307(18) 0.5569(3) 0.71645(10) 0.0670(7) Uani 1 1 d . . . Cl2 Cl 0.88879(16) 0.5869(2) 0.24776(8) 0.0478(5) Uani 1 1 d . . . O1 O 0.3136(5) 0.3938(8) 0.7587(4) 0.136(5) Uani 1 1 d D . . H1O1 H 0.3407 0.3202 0.7750 0.164 Uiso 1 1 d RD . . H2O1 H 0.2612 0.4019 0.7581 0.164 Uiso 1 1 d RD . . O2 O 0.8180(6) 0.5898(8) 0.6985(3) 0.073(2) Uani 1 1 d D . . H2O2 H 0.7749 0.5807 0.7063 0.08(4) Uiso 1 1 d RD . . H1O2 H 0.8429 0.6710 0.7077 0.12(5) Uiso 1 1 d RD . . 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 0.0430(2) 0.02379(15) 0.03240(17) -0.00215(11) 0.01505(14) -0.00204(12) Au2 0.03635(18) 0.02368(15) 0.03215(17) 0.00142(11) 0.01300(14) -0.00096(12) S1 0.0370(11) 0.0241(8) 0.0307(10) 0.0004(7) 0.0100(8) 0.0001(8) S2 0.0719(17) 0.0395(12) 0.0696(16) -0.0168(11) 0.0489(14) -0.0166(11) S3 0.0420(12) 0.0280(9) 0.0422(12) 0.0021(9) 0.0048(10) -0.0031(9) N1 0.040(4) 0.036(3) 0.040(4) 0.004(3) 0.021(3) 0.002(3) N2 0.052(4) 0.035(3) 0.049(4) -0.010(3) 0.029(4) -0.009(3) N3 0.039(4) 0.033(3) 0.042(4) 0.003(3) 0.018(3) -0.003(3) C1 0.039(4) 0.026(3) 0.032(4) 0.004(3) 0.019(4) -0.001(3) C2 0.027(4) 0.030(4) 0.036(4) 0.008(3) 0.012(3) -0.003(3) C3 0.034(4) 0.023(3) 0.035(4) -0.003(3) 0.017(3) -0.003(3) C4 0.038(4) 0.029(4) 0.029(4) 0.005(3) 0.016(3) 0.005(3) C5 0.042(5) 0.031(4) 0.028(4) -0.001(3) 0.011(3) 0.000(3) C6 0.032(4) 0.025(3) 0.036(4) -0.008(3) 0.014(3) -0.009(3) C7 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C8 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C9 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C10 0.042(5) 0.033(4) 0.058(5) -0.010(4) 0.031(4) -0.006(4) C11 0.067(6) 0.047(5) 0.032(4) -0.005(4) 0.024(4) -0.004(5) C12 0.064(6) 0.040(4) 0.045(5) -0.004(4) 0.033(5) -0.005(4) C13 0.040(5) 0.044(5) 0.040(4) -0.013(4) 0.023(4) -0.005(4) C14 0.061(6) 0.055(5) 0.037(5) 0.004(4) 0.028(4) 0.012(5) C15 0.063(6) 0.038(4) 0.040(5) 0.005(4) 0.026(5) 0.006(4) C16 0.060(6) 0.050(5) 0.065(6) -0.013(5) 0.038(5) -0.001(5) C17 0.047(6) 0.082(7) 0.057(6) -0.018(6) 0.021(5) -0.004(5) C18 0.110(9) 0.035(5) 0.076(7) -0.007(5) 0.052(7) -0.014(6) C19 0.034(4) 0.029(4) 0.034(4) 0.004(3) 0.013(3) -0.004(3) C20 0.041(5) 0.029(4) 0.052(5) 0.006(4) 0.017(4) 0.005(4) C21 0.033(4) 0.039(4) 0.042(5) -0.002(4) 0.012(4) -0.002(4) C22 0.035(4) 0.026(3) 0.029(4) -0.001(3) 0.012(3) -0.004(3) C23 0.032(4) 0.033(4) 0.040(4) 0.003(3) 0.018(4) 0.003(3) C24 0.031(4) 0.034(4) 0.044(5) 0.001(4) 0.017(4) -0.005(3) C25 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C26 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C27 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) O3 0.081(7) 0.156(9) 0.074(6) -0.008(6) 0.019(5) -0.009(7) N4 0.075(7) 0.137(10) 0.081(7) -0.038(7) 0.046(6) -0.047(7) C28 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C29 0.094(3) 0.062(2) 0.092(3) -0.008(2) 0.043(3) -0.013(2) C30 0.076(10) 0.143(14) 0.092(12) -0.006(10) 0.043(9) -0.029(9) Cl1 0.0544(15) 0.0511(13) 0.0793(18) 0.0013(13) 0.0172(13) -0.0137(12) Cl2 0.0516(13) 0.0460(11) 0.0492(12) 0.0084(10) 0.0263(10) 0.0036(10) O1 0.052(5) 0.067(5) 0.266(13) 0.076(7) 0.053(7) 0.008(4) O2 0.090(5) 0.054(4) 0.091(6) -0.029(4) 0.056(5) -0.005(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 S2 2.282(3) . ? Au1 S1 2.312(2) . ? Au1 Au2 3.0744(7) 3_766 ? Au2 S3 2.277(2) . ? Au2 S1 2.303(2) . ? Au2 Au1 3.0744(7) 3_766 ? S1 C1 1.783(7) . ? S2 C10 1.780(8) . ? S3 C19 1.761(7) . ? N1 C9 1.493(12) . ? N1 C4 1.495(9) . ? N1 C7 1.511(11) . ? N1 C8 1.523(13) . ? N2 C13 1.486(9) . ? N2 C17 1.493(11) . ? N2 C16 1.497(11) . ? N2 C18 1.499(11) . ? N3 C27 1.447(12) . ? N3 C26 1.451(12) . ? N3 C25 1.493(13) . ? N3 C22 1.502(9) . ? C1 C2 1.383(10) . ? C1 C6 1.393(10) . ? C2 C3 1.397(9) . ? C2 H2A 0.9300 . ? C3 C4 1.365(10) . ? C3 H3A 0.9300 . ? C4 C5 1.372(10) . ? C5 C6 1.389(9) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.380(11) . ? C10 C15 1.389(12) . ? C11 C12 1.381(11) . ? C11 H11A 0.9300 . ? C12 C13 1.384(11) . ? C12 H12A 0.9300 . ? C13 C14 1.370(11) . ? C14 C15 1.384(11) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C24 1.363(10) . ? C19 C20 1.388(10) . ? C20 C21 1.363(10) . ? C20 H20A 0.9300 . ? C21 C22 1.382(10) . ? C21 H21A 0.9300 . ? C22 C23 1.370(10) . ? C23 C24 1.379(10) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? O3 C30 1.147(14) . ? N4 C30 1.352(15) . ? N4 C29 1.409(14) . ? N4 C28 1.435(13) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30 0.9300 . ? O1 H1O1 0.8200 . ? O1 H2O1 0.8201 . ? O2 H2O2 0.8184 . ? O2 H1O2 0.8184 . ? 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 S2 Au1 S1 176.30(7) . . ? S2 Au1 Au2 96.01(6) . 3_766 ? S1 Au1 Au2 81.76(4) . 3_766 ? S3 Au2 S1 171.76(7) . . ? S3 Au2 Au1 77.39(5) . 3_766 ? S1 Au2 Au1 94.42(4) . 3_766 ? C1 S1 Au2 110.5(3) . . ? C1 S1 Au1 103.9(3) . . ? Au2 S1 Au1 99.31(8) . . ? C10 S2 Au1 105.4(3) . . ? C19 S3 Au2 109.8(3) . . ? C9 N1 C4 111.0(7) . . ? C9 N1 C7 107.1(7) . . ? C4 N1 C7 113.1(7) . . ? C9 N1 C8 109.4(8) . . ? C4 N1 C8 108.3(7) . . ? C7 N1 C8 107.9(8) . . ? C13 N2 C17 110.3(7) . . ? C13 N2 C16 109.8(6) . . ? C17 N2 C16 108.0(7) . . ? C13 N2 C18 112.4(7) . . ? C17 N2 C18 107.5(7) . . ? C16 N2 C18 108.6(7) . . ? C27 N3 C26 108.2(8) . . ? C27 N3 C25 107.9(8) . . ? C26 N3 C25 107.5(8) . . ? C27 N3 C22 114.3(7) . . ? C26 N3 C22 112.2(7) . . ? C25 N3 C22 106.5(7) . . ? C2 C1 C6 119.2(6) . . ? C2 C1 S1 123.1(6) . . ? C6 C1 S1 117.6(5) . . ? C1 C2 C3 119.7(7) . . ? C1 C2 H2A 120.1 . . ? C3 C2 H2A 120.1 . . ? C4 C3 C2 120.0(7) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 121.2(7) . . ? C3 C4 N1 120.7(6) . . ? C5 C4 N1 118.0(6) . . ? C4 C5 C6 119.1(7) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C5 C6 C1 120.6(6) . . ? C5 C6 H6A 119.7 . . ? C1 C6 H6A 119.7 . . ? N1 C7 H7A 109.5 . . ? N1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.5(7) . . ? C11 C10 S2 122.4(7) . . ? C15 C10 S2 120.0(6) . . ? C10 C11 C12 122.3(8) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? C11 C12 C13 119.0(8) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 120.0(8) . . ? C14 C13 N2 117.9(8) . . ? C12 C13 N2 122.1(8) . . ? C13 C14 C15 120.3(8) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C15 C10 120.9(8) . . ? C14 C15 H15A 119.6 . . ? C10 C15 H15A 119.6 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 116.9(7) . . ? C24 C19 S3 125.1(6) . . ? C20 C19 S3 118.0(6) . . ? C21 C20 C19 122.3(7) . . ? C21 C20 H20A 118.9 . . ? C19 C20 H20A 118.9 . . ? C20 C21 C22 119.1(7) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C23 C22 C21 120.2(7) . . ? C23 C22 N3 120.7(6) . . ? C21 C22 N3 119.1(7) . . ? C22 C23 C24 119.0(7) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C19 C24 C23 122.5(7) . . ? C19 C24 H24A 118.8 . . ? C23 C24 H24A 118.8 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 N4 C29 121.0(11) . . ? C30 N4 C28 121.2(12) . . ? C29 N4 C28 117.1(11) . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O3 C30 N4 128.5(16) . . ? O3 C30 H30 115.8 . . ? N4 C30 H30 115.8 . . ? H1O1 O1 H2O1 108.9 . . ? H2O2 O2 H1O2 108.9 . . ? 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 O1 H1O1 Cl1 0.82 2.41 3.158(7) 151.8 2_646 O1 H2O1 Cl2 0.82 2.29 3.105(8) 176.1 3_666 O2 H2O2 Cl1 0.82 2.40 3.211(10) 171.7 . O2 H1O2 Cl2 0.82 2.44 3.236(7) 163.3 4_576 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.773 _refine_diff_density_min -2.047 _refine_diff_density_rms 0.167 #===END