# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2008 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Manuel Almeida' _publ_contact_author_email MALMEIDA@ITN.PT loop_ _publ_author_name M.Almeida H.Alves J.S.Brooks E.Canadell D.Graf E.B.Lopes ; I.C.Santos ; data_ni25-120 _database_code_depnum_ccdc_archive 'CCDC 670913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (n-Bu!4$N)!2$(Ni(dcbdt)!2$)!5$! _chemical_melting_point ? _chemical_formula_moiety 'C32 H8 N8 Ni2 S8, 2(C16 H36 N), 3(C16 H4 N4 Ni S4)' _chemical_formula_sum 'C112 H92 N22 Ni5 S20' _chemical_formula_weight 2680.83 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9605(5) _cell_length_b 17.0682(13) _cell_length_c 22.3270(17) _cell_angle_alpha 69.628(4) _cell_angle_beta 89.239(4) _cell_angle_gamma 79.236(4) _cell_volume 2789.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1378 _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8044 _exptl_absorpt_correction_T_max 0.9752 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS APEX- CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19519 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_av_sigmaI/netI 0.2301 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.38 _reflns_number_total 10020 _reflns_number_gt 3981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART, (Bruker, 2004)' _computing_cell_refinement 'Bruker SMART, (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT, (Bruker, 2004)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL(Keller, 1989),ORTEP3 (Farrugia,1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. Due to problems with anisotropy, restraints for displacement parameters were applied for some C atoms using ISOR instructions in SHELXL97 (Sheldrick, 1997). ; _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^)+(0.0387P)^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 10020 _refine_ls_number_parameters 722 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.2184 _refine_ls_R_factor_gt 0.0726 _refine_ls_wR_factor_ref 0.1472 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.880 _refine_ls_shift/su_max 0.000 _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 Ni1 Ni 1.0000 0.0000 1.0000 0.0168(5) Uani 1 2 d S . . Ni3 Ni 0.14220(14) 0.43879(7) 0.98509(6) 0.0112(3) Uani 1 1 d . . . Ni2 Ni 0.55926(15) 0.20787(8) 0.99139(6) 0.0137(3) Uani 1 1 d . . . S1 S 0.7349(3) 0.00856(15) 0.97988(12) 0.0184(6) Uani 1 1 d . . . S2 S 1.0300(3) 0.08458(15) 0.90639(12) 0.0175(6) Uani 1 1 d . . . S3 S 0.2925(3) 0.21426(14) 0.97288(12) 0.0147(6) Uani 1 1 d . . . S4 S 0.5797(3) 0.30032(15) 0.89916(12) 0.0170(6) Uani 1 1 d . . . S5 S 0.5325(3) 0.12021(15) 1.08497(12) 0.0155(6) Uani 1 1 d . . . S6 S 0.8245(3) 0.20416(15) 1.01214(12) 0.0165(6) Uani 1 1 d . . . S7 S -0.1331(3) 0.45633(14) 0.96528(11) 0.0112(5) Uani 1 1 d . . . S8 S 0.1753(3) 0.51638(15) 0.88622(11) 0.0138(5) Uani 1 1 d . . . S9 S 0.1197(3) 0.32565(14) 1.06748(12) 0.0139(5) Uani 1 1 d . . . S10 S 0.4223(3) 0.40612(14) 0.99892(11) 0.0145(5) Uani 1 1 d . . . C1 C 0.6921(12) 0.0750(6) 0.9033(5) 0.019(2) Uani 1 1 d U . . C2 C 0.8301(12) 0.1091(6) 0.8682(5) 0.020(2) Uani 1 1 d . . . C3 C 0.5315(12) 0.0986(6) 0.8724(5) 0.021(2) Uani 1 1 d . . . H3 H 0.4393 0.0770 0.8956 0.025 Uiso 1 1 calc R . . C4 C 0.7987(12) 0.1631(6) 0.8030(5) 0.020(2) Uani 1 1 d . . . H4 H 0.8894 0.1859 0.7794 0.024 Uiso 1 1 calc R . . C5 C 0.4985(12) 0.1519(6) 0.8095(5) 0.021(3) Uani 1 1 d . . . C6 C 0.6403(11) 0.1822(6) 0.7744(4) 0.013(2) Uani 1 1 d . . . C7 C 0.3327(12) 0.1743(6) 0.7795(5) 0.020(2) Uani 1 1 d . . . C8 C 0.6084(12) 0.2338(6) 0.7068(5) 0.022(2) Uani 1 1 d . . . C9 C 0.2490(11) 0.2850(5) 0.8973(5) 0.015(2) Uani 1 1 d U . . C10 C 0.3760(11) 0.3274(6) 0.8600(5) 0.018(2) Uani 1 1 d . . . C11 C 0.0828(11) 0.3067(5) 0.8673(4) 0.015(2) Uani 1 1 d U . . H11 H -0.0072 0.2827 0.8906 0.018 Uiso 1 1 calc R . . C12 C 0.3411(11) 0.3814(5) 0.7991(4) 0.014(2) Uani 1 1 d . . . H12 H 0.4295 0.4066 0.7756 0.017 Uiso 1 1 calc R . . C13 C 0.0488(12) 0.3612(5) 0.8054(5) 0.016(2) Uani 1 1 d . . . C14 C 0.1779(11) 0.4005(6) 0.7702(5) 0.017(2) Uani 1 1 d . . . C15 C -0.1239(11) 0.3826(6) 0.7744(5) 0.015(2) Uani 1 1 d . . . C16 C 0.1399(11) 0.4608(6) 0.7075(5) 0.021(2) Uani 1 1 d . . . C17 C 0.7305(11) 0.0983(5) 1.1225(4) 0.013(2) Uani 1 1 d . . . C18 C 0.8679(11) 0.1341(6) 1.0893(4) 0.015(2) Uani 1 1 d U . . C19 C 0.7603(11) 0.0406(5) 1.1868(4) 0.012(2) Uani 1 1 d U . . H19 H 0.6709 0.0151 1.2093 0.014 Uiso 1 1 calc R . . C20 C 1.0312(11) 0.1122(5) 1.1201(5) 0.017(2) Uani 1 1 d . . . H20 H 1.1234 0.1348 1.0975 0.021 Uiso 1 1 calc R . . C21 C 0.9227(12) 0.0226(6) 1.2161(5) 0.019(2) Uani 1 1 d . . . C22 C 1.0594(11) 0.0574(5) 1.1838(5) 0.013(2) Uani 1 1 d U . . C23 C 0.9556(11) -0.0353(6) 1.2818(5) 0.018(2) Uani 1 1 d . . . C24 C 1.2281(12) 0.0346(6) 1.2123(5) 0.017(2) Uani 1 1 d . . . C25 C -0.1634(10) 0.5126(5) 0.8819(4) 0.009(2) Uani 1 1 d U . . C26 C -0.0228(11) 0.5400(5) 0.8476(5) 0.016(2) Uani 1 1 d . . . C27 C -0.3269(10) 0.5291(5) 0.8518(4) 0.012(2) Uani 1 1 d . . . H27 H -0.4195 0.5086 0.8756 0.015 Uiso 1 1 calc R . . C28 C -0.0540(10) 0.5883(5) 0.7827(4) 0.012(2) Uani 1 1 d . . . H28 H 0.0368 0.6107 0.7589 0.014 Uiso 1 1 calc R . . C29 C -0.3495(11) 0.5749(5) 0.7882(4) 0.011(2) Uani 1 1 d . . . C30 C -0.2116(11) 0.6044(5) 0.7522(4) 0.015(2) Uani 1 1 d . . . C31 C -0.5173(12) 0.5918(6) 0.7566(4) 0.015(2) Uani 1 1 d . . . C32 C -0.2385(10) 0.6507(5) 0.6842(5) 0.013(2) Uani 1 1 d . . . C33 C 0.3177(11) 0.3016(5) 1.1095(5) 0.019(2) Uani 1 1 d . . . C34 C 0.4524(11) 0.3383(5) 1.0769(4) 0.017(2) Uani 1 1 d U . . C35 C 0.3402(10) 0.2448(5) 1.1723(4) 0.0082(19) Uani 1 1 d U . . H35 H 0.2488 0.2193 1.1930 0.010 Uiso 1 1 calc R . . C36 C 0.6167(10) 0.3164(5) 1.1095(4) 0.013(2) Uani 1 1 d . . . H36 H 0.7097 0.3398 1.0881 0.016 Uiso 1 1 calc R . . C37 C 0.5011(10) 0.2260(5) 1.2042(5) 0.012(2) Uani 1 1 d . . . C38 C 0.6394(10) 0.2628(5) 1.1700(4) 0.0079(19) Uani 1 1 d U . . C39 C 0.5268(12) 0.1703(6) 1.2702(5) 0.022(2) Uani 1 1 d . . . C40 C 0.8063(11) 0.2416(6) 1.2037(4) 0.016(2) Uani 1 1 d U . . N1 N 0.1987(11) 0.1941(6) 0.7550(4) 0.035(2) Uani 1 1 d . . . N2 N 0.5801(11) 0.2711(6) 0.6548(5) 0.040(3) Uani 1 1 d . . . N3 N -0.2583(9) 0.3970(5) 0.7511(4) 0.027(2) Uani 1 1 d . . . N4 N 0.0985(10) 0.5098(5) 0.6569(4) 0.033(2) Uani 1 1 d . . . N5 N 0.9883(10) -0.0805(5) 1.3329(4) 0.028(2) Uani 1 1 d . . . N6 N 1.3616(10) 0.0155(5) 1.2381(4) 0.023(2) Uani 1 1 d . . . N7 N -0.6524(9) 0.6089(5) 0.7322(4) 0.0208(19) Uani 1 1 d . . . N8 N -0.2630(10) 0.6904(5) 0.6322(4) 0.031(2) Uani 1 1 d . . . N9 N 0.5470(11) 0.1275(6) 1.3216(4) 0.035(2) Uani 1 1 d . . . N10 N 0.9408(9) 0.2260(5) 1.2272(4) 0.022(2) Uani 1 1 d . . . N11 N 0.7588(9) 0.2487(4) 0.4828(4) 0.0238(19) Uani 1 1 d . . . C41 C 0.8447(12) 0.2621(6) 0.5369(4) 0.032(3) Uani 1 1 d . . . H41A H 0.9004 0.2057 0.5673 0.038 Uiso 1 1 calc R . . H41B H 0.7549 0.2871 0.5597 0.038 Uiso 1 1 calc R . . C42 C 0.9764(13) 0.3178(6) 0.5196(5) 0.038(3) Uani 1 1 d . . . H42A H 0.9204 0.3776 0.4960 0.045 Uiso 1 1 calc R . . H42B H 1.0601 0.2988 0.4919 0.045 Uiso 1 1 calc R . . C43 C 1.0697(14) 0.3114(7) 0.5828(6) 0.051(4) Uani 1 1 d . . . H43A H 0.9829 0.3201 0.6132 0.061 Uiso 1 1 calc R . . H43B H 1.1394 0.2533 0.6025 0.061 Uiso 1 1 calc R . . C44 C 1.1805(15) 0.3735(8) 0.5725(7) 0.077(5) Uani 1 1 d . . . H44A H 1.1165 0.4303 0.5472 0.115 Uiso 1 1 calc R . . H44B H 1.2797 0.3584 0.5495 0.115 Uiso 1 1 calc R . . H44C H 1.2196 0.3735 0.6139 0.115 Uiso 1 1 calc R . . C51 C 0.6111(12) 0.2028(6) 0.5095(5) 0.037(3) Uani 1 1 d . . . H51A H 0.5379 0.2367 0.5315 0.044 Uiso 1 1 calc R . . H51B H 0.5411 0.2044 0.4726 0.044 Uiso 1 1 calc R . . C52 C 0.6510(13) 0.1135(6) 0.5541(6) 0.056(4) Uani 1 1 d . . . H52A H 0.7423 0.1069 0.5862 0.068 Uiso 1 1 calc R . . H52B H 0.6930 0.0752 0.5302 0.068 Uiso 1 1 calc R . . C53 C 0.4833(15) 0.0878(8) 0.5895(6) 0.074(5) Uani 1 1 d . . . H53A H 0.5145 0.0303 0.6227 0.089 Uiso 1 1 calc R . . H53B H 0.4387 0.1284 0.6113 0.089 Uiso 1 1 calc R . . C54 C 0.3507(15) 0.0876(7) 0.5465(6) 0.065(4) Uani 1 1 d . . . H54A H 0.3976 0.0526 0.5212 0.098 Uiso 1 1 calc R . . H54B H 0.3063 0.1460 0.5178 0.098 Uiso 1 1 calc R . . H54C H 0.2576 0.0640 0.5712 0.098 Uiso 1 1 calc R . . C60 C 0.8884(11) 0.1952(6) 0.4575(5) 0.030(3) Uani 1 1 d . . . H60A H 0.9382 0.1428 0.4936 0.036 Uiso 1 1 calc R . . H60B H 0.9819 0.2266 0.4412 0.036 Uiso 1 1 calc R . . C61 C 0.8251(12) 0.1692(6) 0.4048(5) 0.040(3) Uani 1 1 d . . . H61A H 0.8066 0.2189 0.3644 0.047 Uiso 1 1 calc R . . H61B H 0.7136 0.1516 0.4157 0.047 Uiso 1 1 calc R . . C62 C 0.9525(12) 0.0952(6) 0.3946(5) 0.040(3) Uani 1 1 d . . . H62A H 0.9664 0.0450 0.4346 0.048 Uiso 1 1 calc R . . H62B H 0.9029 0.0798 0.3608 0.048 Uiso 1 1 calc R . . C63 C 1.1257(12) 0.1151(7) 0.3760(5) 0.048(3) Uani 1 1 d . . . H63A H 1.1128 0.1676 0.3385 0.071 Uiso 1 1 calc R . . H63B H 1.1948 0.0680 0.3658 0.071 Uiso 1 1 calc R . . H63C H 1.1828 0.1227 0.4117 0.071 Uiso 1 1 calc R . . C70 C 0.6818(11) 0.3328(5) 0.4301(4) 0.021(2) Uani 1 1 d . . . H70A H 0.7741 0.3653 0.4143 0.025 Uiso 1 1 calc R . . H70B H 0.6376 0.3202 0.3939 0.025 Uiso 1 1 calc R . . C71 C 0.5408(13) 0.3876(6) 0.4501(5) 0.040(3) Uani 1 1 d . . . H71A H 0.5799 0.3951 0.4893 0.048 Uiso 1 1 calc R . . H71B H 0.4419 0.3586 0.4605 0.048 Uiso 1 1 calc R . . C72 C 0.4845(12) 0.4734(6) 0.3994(5) 0.035(3) Uani 1 1 d . . . H72A H 0.5770 0.5063 0.3948 0.042 Uiso 1 1 calc R . . H72B H 0.4670 0.4658 0.3581 0.042 Uiso 1 1 calc R . . C73 C 0.3247(13) 0.5233(7) 0.4128(5) 0.050(3) Uani 1 1 d . . . H73A H 0.2274 0.4979 0.4079 0.074 Uiso 1 1 calc R . . H73B H 0.3075 0.5821 0.3827 0.074 Uiso 1 1 calc R . . H73C H 0.3334 0.5228 0.4567 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0207(10) 0.0141(10) 0.0172(12) -0.0064(9) -0.0003(9) -0.0056(8) Ni3 0.0103(6) 0.0100(6) 0.0112(8) -0.0008(6) -0.0002(5) -0.0025(5) Ni2 0.0143(6) 0.0126(7) 0.0127(8) -0.0026(6) 0.0006(5) -0.0022(5) S1 0.0167(14) 0.0209(15) 0.0163(16) -0.0050(13) 0.0033(12) -0.0040(11) S2 0.0183(13) 0.0187(14) 0.0147(16) -0.0027(12) -0.0001(11) -0.0078(11) S3 0.0136(12) 0.0144(13) 0.0142(15) -0.0023(11) 0.0001(11) -0.0034(10) S4 0.0159(13) 0.0189(14) 0.0136(15) -0.0015(12) -0.0017(11) -0.0058(11) S5 0.0130(12) 0.0134(13) 0.0183(16) -0.0033(12) 0.0005(11) -0.0027(10) S6 0.0192(13) 0.0125(13) 0.0147(15) -0.0008(11) -0.0032(11) -0.0025(10) S7 0.0113(11) 0.0102(12) 0.0090(13) 0.0004(10) -0.0013(10) -0.0018(9) S8 0.0094(12) 0.0178(13) 0.0127(14) -0.0033(11) -0.0008(10) -0.0028(10) S9 0.0128(12) 0.0110(12) 0.0157(14) -0.0008(11) -0.0004(10) -0.0047(10) S10 0.0118(12) 0.0145(13) 0.0134(14) -0.0002(11) 0.0015(10) -0.0029(10) C1 0.021(3) 0.018(3) 0.020(3) -0.0081(19) 0.0009(19) -0.0042(19) C2 0.026(6) 0.007(5) 0.024(7) -0.006(5) -0.008(5) 0.003(4) C3 0.018(5) 0.025(6) 0.023(7) -0.013(5) -0.004(5) -0.005(5) C4 0.023(6) 0.013(5) 0.027(7) -0.011(5) 0.005(5) -0.005(4) C5 0.021(6) 0.029(6) 0.025(7) -0.018(5) 0.009(5) -0.020(5) C6 0.017(5) 0.018(5) 0.009(6) -0.010(5) 0.005(4) -0.006(4) C7 0.022(6) 0.025(6) 0.020(7) -0.012(5) 0.006(5) -0.010(5) C8 0.013(5) 0.022(6) 0.021(7) 0.002(5) 0.006(5) 0.004(4) C9 0.015(3) 0.014(3) 0.016(3) -0.0062(19) 0.0014(18) -0.0057(18) C10 0.019(5) 0.020(6) 0.018(7) -0.011(5) 0.004(5) -0.003(4) C11 0.015(3) 0.015(3) 0.014(3) -0.0047(19) -0.0002(18) -0.0023(18) C12 0.016(5) 0.007(5) 0.015(6) 0.001(4) 0.010(4) -0.005(4) C13 0.031(6) 0.005(5) 0.012(6) -0.003(4) -0.007(5) -0.003(4) C14 0.007(5) 0.021(6) 0.022(6) -0.008(5) -0.001(4) -0.004(4) C15 0.010(5) 0.015(5) 0.018(6) -0.006(5) -0.002(4) 0.000(4) C16 0.012(5) 0.024(6) 0.028(7) -0.012(5) 0.008(5) -0.003(4) C17 0.017(5) 0.012(5) 0.011(6) -0.005(5) 0.008(4) -0.006(4) C18 0.017(3) 0.014(3) 0.015(3) -0.0071(19) 0.0015(18) -0.0008(18) C19 0.012(3) 0.010(3) 0.013(3) -0.0032(19) 0.0006(18) -0.0033(18) C20 0.011(5) 0.013(5) 0.028(7) -0.005(5) 0.002(5) -0.006(4) C21 0.030(6) 0.013(5) 0.009(6) -0.003(5) 0.002(5) 0.002(5) C22 0.013(3) 0.011(3) 0.013(3) -0.0038(19) 0.0014(18) -0.0012(18) C23 0.017(5) 0.023(6) 0.017(6) -0.010(5) 0.003(5) -0.003(4) C24 0.020(5) 0.016(5) 0.020(6) -0.010(5) 0.007(5) -0.008(4) C25 0.010(3) 0.010(3) 0.008(3) -0.0039(18) -0.0008(18) -0.0008(18) C26 0.011(5) 0.013(5) 0.024(7) -0.007(5) 0.001(4) -0.003(4) C27 0.003(4) 0.012(5) 0.030(6) -0.016(5) 0.002(4) -0.002(4) C28 0.007(5) 0.015(5) 0.012(6) -0.002(5) -0.001(4) -0.004(4) C29 0.018(5) 0.008(5) 0.006(5) 0.001(4) -0.007(4) -0.007(4) C30 0.014(5) 0.010(5) 0.017(6) -0.003(4) -0.004(4) -0.001(4) C31 0.022(5) 0.015(5) 0.011(6) -0.007(5) 0.004(4) -0.002(4) C32 0.004(4) 0.012(5) 0.019(6) -0.002(5) -0.003(4) -0.001(4) C33 0.020(5) 0.010(5) 0.033(7) -0.013(5) 0.004(5) -0.008(4) C34 0.018(3) 0.016(3) 0.017(3) -0.0083(19) 0.0028(18) -0.0006(18) C35 0.009(2) 0.006(2) 0.009(3) -0.0017(18) 0.0001(18) -0.0008(18) C36 0.010(5) 0.009(5) 0.021(6) -0.009(5) -0.001(4) 0.001(4) C37 0.010(5) 0.009(5) 0.018(6) -0.009(5) -0.008(4) 0.006(4) C38 0.008(3) 0.007(2) 0.009(3) -0.0036(18) -0.0012(18) -0.0004(18) C39 0.016(5) 0.022(6) 0.033(8) -0.014(6) -0.002(5) -0.007(5) C40 0.017(3) 0.017(3) 0.015(3) -0.0055(19) 0.0004(19) -0.0024(18) N1 0.030(5) 0.044(6) 0.030(7) -0.007(5) -0.001(5) -0.012(5) N2 0.035(6) 0.045(6) 0.030(7) -0.004(5) -0.009(5) -0.003(5) N3 0.019(5) 0.035(6) 0.029(6) -0.009(5) 0.005(4) -0.012(4) N4 0.036(5) 0.038(6) 0.019(6) -0.003(5) -0.007(4) -0.009(4) N5 0.037(5) 0.025(5) 0.012(5) 0.006(4) -0.006(4) -0.001(4) N6 0.025(5) 0.024(5) 0.020(6) -0.008(4) -0.010(4) 0.003(4) N7 0.025(5) 0.021(5) 0.013(5) 0.001(4) 0.000(4) -0.010(4) N8 0.025(5) 0.037(6) 0.029(6) -0.009(5) 0.000(4) -0.008(4) N9 0.037(6) 0.037(6) 0.026(6) 0.000(5) -0.004(5) -0.015(5) N10 0.022(5) 0.021(5) 0.019(5) 0.000(4) -0.003(4) -0.004(4) N11 0.021(4) 0.015(4) 0.028(5) 0.003(4) -0.003(4) -0.005(4) C41 0.036(6) 0.031(6) 0.021(6) -0.007(5) -0.011(5) 0.007(5) C42 0.057(7) 0.028(6) 0.035(7) -0.016(6) -0.016(6) -0.012(6) C43 0.043(7) 0.040(8) 0.073(11) -0.029(8) -0.006(7) 0.003(6) C44 0.069(9) 0.065(10) 0.117(14) -0.060(10) -0.013(9) -0.006(8) C51 0.038(7) 0.030(7) 0.029(7) 0.006(6) -0.006(5) -0.008(5) C52 0.038(7) 0.034(7) 0.078(11) 0.008(7) -0.012(7) -0.011(6) C53 0.060(9) 0.051(9) 0.087(13) 0.022(8) -0.024(8) -0.035(7) C54 0.064(9) 0.062(9) 0.073(11) -0.014(8) -0.004(8) -0.036(8) C60 0.024(6) 0.031(6) 0.035(7) -0.010(6) 0.000(5) -0.011(5) C61 0.031(6) 0.027(6) 0.063(9) -0.019(6) -0.017(6) -0.003(5) C62 0.042(7) 0.035(7) 0.050(8) -0.023(6) -0.013(6) -0.007(5) C63 0.049(8) 0.040(7) 0.044(8) -0.012(6) -0.022(6) 0.011(6) C70 0.026(5) 0.025(6) 0.011(5) -0.003(5) -0.009(4) -0.003(4) C71 0.056(7) 0.029(7) 0.034(7) -0.011(6) 0.006(6) -0.003(6) C72 0.036(6) 0.024(6) 0.041(8) -0.013(6) 0.007(6) 0.006(5) C73 0.060(8) 0.041(8) 0.035(8) -0.005(6) -0.014(6) 0.008(6) _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 Ni1 S2 2.127(3) 2_757 ? Ni1 S2 2.127(3) . ? Ni1 S1 2.131(2) . ? Ni1 S1 2.131(2) 2_757 ? Ni3 S8 2.185(3) . ? Ni3 S7 2.185(2) . ? Ni3 S9 2.189(3) . ? Ni3 S10 2.193(3) . ? Ni3 S7 2.402(2) 2_567 ? Ni2 S5 2.140(3) . ? Ni2 S4 2.141(3) . ? Ni2 S3 2.145(3) . ? Ni2 S6 2.152(3) . ? S1 C1 1.687(10) . ? S2 C2 1.724(9) . ? S3 C9 1.693(9) . ? S4 C10 1.756(9) . ? S5 C17 1.709(9) . ? S6 C18 1.716(9) . ? S7 C25 1.769(9) . ? S7 Ni3 2.402(2) 2_567 ? S8 C26 1.718(9) . ? S9 C33 1.751(9) . ? S10 C34 1.713(9) . ? C1 C3 1.382(11) . ? C1 C2 1.434(12) . ? C2 C4 1.423(13) . ? C3 C5 1.377(13) . ? C4 C6 1.352(11) . ? C5 C7 1.412(12) . ? C5 C6 1.438(12) . ? C6 C8 1.455(13) . ? C7 N1 1.142(11) . ? C8 N2 1.116(12) . ? C9 C11 1.416(11) . ? C9 C10 1.438(12) . ? C10 C12 1.349(12) . ? C11 C13 1.367(12) . ? C12 C14 1.388(11) . ? C13 C14 1.411(12) . ? C13 C15 1.471(11) . ? C14 C16 1.416(13) . ? C15 N3 1.141(10) . ? C16 N4 1.155(12) . ? C17 C19 1.423(12) . ? C17 C18 1.425(11) . ? C18 C20 1.402(11) . ? C19 C21 1.388(11) . ? C20 C22 1.397(12) . ? C21 C22 1.406(12) . ? C21 C23 1.451(13) . ? C22 C24 1.420(11) . ? C23 N5 1.133(11) . ? C24 N6 1.150(11) . ? C25 C27 1.407(10) . ? C25 C26 1.408(11) . ? C26 C28 1.393(12) . ? C27 C29 1.358(12) . ? C28 C30 1.370(10) . ? C29 C30 1.416(11) . ? C29 C31 1.450(11) . ? C30 C32 1.445(12) . ? C31 N7 1.152(10) . ? C32 N8 1.121(11) . ? C33 C35 1.389(12) . ? C33 C34 1.409(12) . ? C34 C36 1.425(11) . ? C35 C37 1.401(10) . ? C36 C38 1.334(11) . ? C37 C39 1.442(13) . ? C37 C38 1.447(11) . ? C38 C40 1.456(11) . ? C39 N9 1.119(12) . ? C40 N10 1.141(10) . ? N11 C60 1.485(11) . ? N11 C41 1.501(11) . ? N11 C70 1.528(10) . ? N11 C51 1.534(11) . ? C41 C42 1.503(12) . ? C42 C43 1.563(13) . ? C43 C44 1.459(14) . ? C51 C52 1.480(12) . ? C52 C53 1.596(14) . ? C53 C54 1.438(14) . ? C60 C61 1.517(12) . ? C61 C62 1.546(12) . ? C62 C63 1.500(12) . ? C70 C71 1.489(11) . ? C71 C72 1.496(13) . ? C72 C73 1.482(11) . ? 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 Ni1 S2 180.000(1) 2_757 . ? S2 Ni1 S1 87.58(9) 2_757 . ? S2 Ni1 S1 92.42(9) . . ? S2 Ni1 S1 92.42(9) 2_757 2_757 ? S2 Ni1 S1 87.58(9) . 2_757 ? S1 Ni1 S1 180.00(14) . 2_757 ? S8 Ni3 S7 91.24(10) . . ? S8 Ni3 S9 158.82(10) . . ? S7 Ni3 S9 87.39(9) . . ? S8 Ni3 S10 87.64(10) . . ? S7 Ni3 S10 171.47(10) . . ? S9 Ni3 S10 90.61(10) . . ? S8 Ni3 S7 99.69(9) . 2_567 ? S7 Ni3 S7 97.92(8) . 2_567 ? S9 Ni3 S7 101.43(9) . 2_567 ? S10 Ni3 S7 90.60(8) . 2_567 ? S5 Ni2 S4 177.29(11) . . ? S5 Ni2 S3 86.85(10) . . ? S4 Ni2 S3 92.42(11) . . ? S5 Ni2 S6 92.55(11) . . ? S4 Ni2 S6 88.09(11) . . ? S3 Ni2 S6 177.93(12) . . ? C1 S1 Ni1 105.9(3) . . ? C2 S2 Ni1 104.3(4) . . ? C9 S3 Ni2 104.2(3) . . ? C10 S4 Ni2 105.9(3) . . ? C17 S5 Ni2 103.9(3) . . ? C18 S6 Ni2 104.9(3) . . ? C25 S7 Ni3 104.2(3) . . ? C25 S7 Ni3 106.6(3) . 2_567 ? Ni3 S7 Ni3 82.08(8) . 2_567 ? C26 S8 Ni3 105.3(3) . . ? C33 S9 Ni3 102.4(3) . . ? C34 S10 Ni3 102.3(3) . . ? C3 C1 C2 118.0(9) . . ? C3 C1 S1 123.8(8) . . ? C2 C1 S1 118.2(7) . . ? C4 C2 C1 119.3(9) . . ? C4 C2 S2 121.4(8) . . ? C1 C2 S2 119.2(8) . . ? C5 C3 C1 123.3(9) . . ? C6 C4 C2 120.3(9) . . ? C3 C5 C7 121.6(9) . . ? C3 C5 C6 117.7(9) . . ? C7 C5 C6 120.6(10) . . ? C4 C6 C5 121.2(10) . . ? C4 C6 C8 120.8(9) . . ? C5 C6 C8 118.0(9) . . ? N1 C7 C5 178.5(11) . . ? N2 C8 C6 177.2(11) . . ? C11 C9 C10 116.0(9) . . ? C11 C9 S3 121.3(7) . . ? C10 C9 S3 122.7(7) . . ? C12 C10 C9 122.1(9) . . ? C12 C10 S4 123.1(7) . . ? C9 C10 S4 114.8(7) . . ? C13 C11 C9 121.5(9) . . ? C10 C12 C14 120.9(9) . . ? C11 C13 C14 120.6(9) . . ? C11 C13 C15 121.0(9) . . ? C14 C13 C15 118.3(9) . . ? C12 C14 C13 118.8(9) . . ? C12 C14 C16 120.6(8) . . ? C13 C14 C16 120.5(8) . . ? N3 C15 C13 178.3(11) . . ? N4 C16 C14 175.9(11) . . ? C19 C17 C18 119.6(8) . . ? C19 C17 S5 119.5(6) . . ? C18 C17 S5 120.9(7) . . ? C20 C18 C17 119.9(9) . . ? C20 C18 S6 122.4(7) . . ? C17 C18 S6 117.7(7) . . ? C21 C19 C17 118.6(8) . . ? C22 C20 C18 120.5(8) . . ? C19 C21 C22 122.3(9) . . ? C19 C21 C23 119.6(9) . . ? C22 C21 C23 118.1(9) . . ? C20 C22 C21 119.0(8) . . ? C20 C22 C24 118.5(8) . . ? C21 C22 C24 122.3(9) . . ? N5 C23 C21 177.2(11) . . ? N6 C24 C22 176.9(11) . . ? C27 C25 C26 121.9(9) . . ? C27 C25 S7 119.2(7) . . ? C26 C25 S7 118.8(6) . . ? C28 C26 C25 117.1(8) . . ? C28 C26 S8 122.8(7) . . ? C25 C26 S8 120.1(7) . . ? C29 C27 C25 118.5(8) . . ? C30 C28 C26 121.9(8) . . ? C27 C29 C30 121.1(8) . . ? C27 C29 C31 119.0(8) . . ? C30 C29 C31 119.9(8) . . ? C28 C30 C29 119.2(9) . . ? C28 C30 C32 120.9(8) . . ? C29 C30 C32 119.8(8) . . ? N7 C31 C29 176.6(9) . . ? N8 C32 C30 176.3(10) . . ? C35 C33 C34 122.0(8) . . ? C35 C33 S9 119.9(7) . . ? C34 C33 S9 118.0(8) . . ? C33 C34 C36 118.8(9) . . ? C33 C34 S10 121.0(7) . . ? C36 C34 S10 120.1(7) . . ? C33 C35 C37 118.4(8) . . ? C38 C36 C34 119.7(8) . . ? C35 C37 C39 119.8(8) . . ? C35 C37 C38 119.2(9) . . ? C39 C37 C38 121.0(8) . . ? C36 C38 C37 121.8(8) . . ? C36 C38 C40 119.8(8) . . ? C37 C38 C40 118.3(8) . . ? N9 C39 C37 179.5(11) . . ? N10 C40 C38 176.5(11) . . ? C60 N11 C41 107.6(7) . . ? C60 N11 C70 111.2(7) . . ? C41 N11 C70 112.1(7) . . ? C60 N11 C51 110.6(7) . . ? C41 N11 C51 107.9(7) . . ? C70 N11 C51 107.3(6) . . ? N11 C41 C42 116.8(8) . . ? C41 C42 C43 108.3(9) . . ? C44 C43 C42 112.9(11) . . ? C52 C51 N11 119.1(8) . . ? C51 C52 C53 109.8(9) . . ? C54 C53 C52 112.8(11) . . ? N11 C60 C61 116.3(8) . . ? C60 C61 C62 112.3(8) . . ? C63 C62 C61 114.2(8) . . ? C71 C70 N11 114.7(8) . . ? C70 C71 C72 112.6(8) . . ? C73 C72 C71 113.8(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.887 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.147 data_Au295K _database_code_depnum_ccdc_archive 'CCDC 670914' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (n-Bu!4$N)!2$(Au(dcbdt)!2$)!5$! _chemical_melting_point ? _chemical_formula_moiety '2(C16 H36 N), 5(C16 H4 Au N4 S4)' _chemical_formula_sum 'C112 H92 Au5 N22 S20' _chemical_formula_weight 3372.11 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.973(4) _cell_length_b 17.322(3) _cell_length_c 23.171(4) _cell_angle_alpha 68.119(9) _cell_angle_beta 88.882(8) _cell_angle_gamma 78.409(9) _cell_volume 2903.6(16) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 12 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.928 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1633 _exptl_absorpt_coefficient_mu 6.713 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details 'psi-scan (North,1968)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'cad4-enraf nonius' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 5 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% ? _diffrn_reflns_number 11007 _diffrn_reflns_av_R_equivalents 0.0871 _diffrn_reflns_av_sigmaI/netI 0.2273 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 24.98 _reflns_number_total 10206 _reflns_number_gt 3725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software (Enraf-Nonius,1994) ' _computing_cell_refinement 'CAD4 Software (Enraf-Nonius,1994) ' _computing_data_reduction 'process-MolEN, (Fair, 1990) ' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL(Keller, 1989),ORTEP3 (Farrugia, 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. For a completely anisotropic refinement of all non-H atoms the ISOR restraint on displacement parameters had to be used, as a consequence of the low number of observed reflection [I>2\s(I)] (3725) and a large number of refined parameters (722) . ; _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^)+(0.0280P)^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 10206 _refine_ls_number_parameters 722 _refine_ls_number_restraints 200 _refine_ls_R_factor_all 0.2473 _refine_ls_R_factor_gt 0.0801 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 1.0000 0.0000 1.0000 0.0298(5) Uani 1 2 d S . . Au3 Au 0.12187(13) 0.42891(6) 0.96246(5) 0.0250(3) Uani 1 1 d . . . Au2 Au 0.55375(17) 0.21460(8) 0.98147(6) 0.0290(3) Uani 1 1 d . . . S1 S 0.7191(10) 0.0058(5) 0.9751(4) 0.031(2) Uani 1 1 d . . . S2 S 1.0256(10) 0.0898(5) 0.8990(4) 0.029(2) Uani 1 1 d . . . S3 S 0.2732(10) 0.2163(5) 0.9554(4) 0.035(2) Uani 1 1 d . . . S4 S 0.5736(11) 0.3071(5) 0.8815(4) 0.039(2) Uani 1 1 d . . . S5 S 0.5273(10) 0.1239(5) 1.0817(4) 0.037(2) Uani 1 1 d . . . S6 S 0.8375(9) 0.2100(5) 1.0072(4) 0.037(2) Uani 1 1 d . . . S7 S -0.1564(10) 0.4352(5) 0.9370(4) 0.034(2) Uani 1 1 d . . . S8 S 0.1489(10) 0.5227(5) 0.8652(4) 0.035(2) Uani 1 1 d . . . S9 S 0.1001(10) 0.3342(5) 1.0613(4) 0.043(2) Uani 1 1 d . . . S10 S 0.3972(10) 0.4252(5) 0.9868(3) 0.039(2) Uani 1 1 d . . . C1 C 0.696(3) 0.0733(15) 0.8984(12) 0.019(7) Uani 1 1 d U . . C2 C 0.831(3) 0.1091(17) 0.8643(13) 0.029(8) Uani 1 1 d U . . C3 C 0.530(4) 0.0956(16) 0.8720(13) 0.028(8) Uani 1 1 d U . . H3 H 0.4399 0.0796 0.8964 0.034 Uiso 1 1 calc R . . C4 C 0.801(3) 0.1584(14) 0.8007(12) 0.014(6) Uani 1 1 d U . . H4 H 0.8925 0.1741 0.7770 0.017 Uiso 1 1 calc R . . C5 C 0.500(4) 0.1444(17) 0.8056(14) 0.036(8) Uani 1 1 d U . . C6 C 0.637(4) 0.1847(17) 0.7718(13) 0.028(7) Uani 1 1 d U . . C7 C 0.328(4) 0.1716(17) 0.7789(14) 0.028(8) Uani 1 1 d U . . C8 C 0.610(3) 0.2267(14) 0.7044(12) 0.026(6) Uani 1 1 d U . . C9 C 0.228(3) 0.2852(16) 0.8785(14) 0.034(8) Uani 1 1 d . . . C10 C 0.369(3) 0.3323(15) 0.8449(12) 0.015(6) Uani 1 1 d U . . C11 C 0.076(4) 0.3075(17) 0.8465(14) 0.030(8) Uani 1 1 d U . . H11 H -0.0111 0.2799 0.8657 0.037 Uiso 1 1 calc R . . C12 C 0.330(3) 0.3844(15) 0.7848(12) 0.020(6) Uani 1 1 d U . . H12 H 0.4171 0.4090 0.7630 0.024 Uiso 1 1 calc R . . C13 C 0.041(4) 0.3650(19) 0.7905(15) 0.043(9) Uani 1 1 d U . . C14 C 0.177(4) 0.4047(16) 0.7532(13) 0.028(7) Uani 1 1 d . . . C15 C -0.125(4) 0.382(2) 0.7598(14) 0.047(9) Uani 1 1 d . . . C16 C 0.132(3) 0.4670(19) 0.6928(13) 0.040(7) Uani 1 1 d . . . C17 C 0.735(4) 0.102(2) 1.1172(16) 0.051(10) Uani 1 1 d . . . C18 C 0.871(4) 0.1383(16) 1.0822(13) 0.024(7) Uani 1 1 d U . . C19 C 0.763(4) 0.0484(19) 1.1816(15) 0.039(10) Uani 1 1 d U . . H19 H 0.6737 0.0269 1.2037 0.047 Uiso 1 1 calc R . . C20 C 1.031(3) 0.1138(14) 1.1208(11) 0.016(6) Uani 1 1 d U . . H20 H 1.1227 0.1379 1.1030 0.020 Uiso 1 1 calc R . . C21 C 0.914(4) 0.030(2) 1.2093(16) 0.051(10) Uani 1 1 d U . . C22 C 1.052(3) 0.0605(14) 1.1784(11) 0.014(6) Uani 1 1 d U . . C23 C 0.958(4) -0.0276(19) 1.2754(16) 0.047(10) Uani 1 1 d U . . C24 C 1.224(3) 0.0436(16) 1.2119(12) 0.024(7) Uani 1 1 d . . . C25 C -0.180(3) 0.5096(14) 0.8607(11) 0.008(5) Uani 1 1 d U . . C26 C -0.052(4) 0.5389(17) 0.8305(14) 0.030(8) Uani 1 1 d . . . C27 C -0.348(4) 0.5296(16) 0.8309(13) 0.027(8) Uani 1 1 d . . . H27 H -0.4361 0.5060 0.8525 0.032 Uiso 1 1 calc R . . C28 C -0.072(4) 0.594(2) 0.7692(17) 0.056(11) Uani 1 1 d . . . H28 H 0.0196 0.6153 0.7488 0.067 Uiso 1 1 calc R . . C29 C -0.375(3) 0.5860(13) 0.7681(12) 0.031(7) Uani 1 1 d D . . C30 C -0.240(3) 0.6175(18) 0.7371(15) 0.051(9) Uani 1 1 d . . . C31 C -0.542(3) 0.6045(15) 0.7391(12) 0.032(7) Uani 1 1 d DU . . C32 C -0.264(4) 0.6706(18) 0.6734(15) 0.048(8) Uani 1 1 d U . . C33 C 0.298(3) 0.3201(13) 1.0980(11) 0.015(5) Uani 1 1 d U . . C34 C 0.428(3) 0.3556(15) 1.0667(12) 0.032(7) Uani 1 1 d U . . C35 C 0.328(4) 0.2613(18) 1.1591(14) 0.043(10) Uani 1 1 d . . . H35 H 0.2431 0.2337 1.1803 0.051 Uiso 1 1 calc R . . C36 C 0.587(4) 0.3372(17) 1.0911(14) 0.036(9) Uani 1 1 d U . . H36 H 0.6722 0.3588 1.0657 0.044 Uiso 1 1 calc R . . C37 C 0.496(4) 0.2460(17) 1.1876(13) 0.027(7) Uani 1 1 d U . . C38 C 0.632(4) 0.2847(18) 1.1556(14) 0.039(9) Uani 1 1 d . . . C39 C 0.518(4) 0.1866(17) 1.2515(14) 0.035(8) Uani 1 1 d U . . C40 C 0.794(5) 0.259(2) 1.1820(15) 0.052(11) Uani 1 1 d . . . N1 N 0.196(3) 0.1888(15) 0.7517(12) 0.058(8) Uani 1 1 d . . . N2 N 0.576(4) 0.2717(17) 0.6548(14) 0.091(10) Uani 1 1 d U . . N3 N -0.260(3) 0.4003(14) 0.7387(10) 0.041(6) Uani 1 1 d . . . N4 N 0.102(3) 0.5159(15) 0.6453(10) 0.067(8) Uani 1 1 d . . . N5 N 0.970(3) -0.0616(15) 1.3259(13) 0.069(8) Uani 1 1 d U . . N6 N 1.354(3) 0.0312(18) 1.2282(13) 0.082(10) Uani 1 1 d . . . N7 N -0.676(3) 0.6249(15) 0.7153(11) 0.066(8) Uani 1 1 d . . . N8 N -0.289(3) 0.7139(15) 0.6200(11) 0.066(7) Uani 1 1 d . . . N9 N 0.551(3) 0.1427(15) 1.3043(12) 0.073(8) Uani 1 1 d U . . N10 N 0.923(3) 0.2418(12) 1.2114(10) 0.052(7) Uani 1 1 d . . . N11 N 0.758(3) 0.2368(12) 0.4899(8) 0.052(5) Uani 1 1 d . . . C41 C 0.850(3) 0.2466(17) 0.5421(10) 0.065(8) Uani 1 1 d . . . H41A H 0.7655 0.2698 0.5651 0.078 Uiso 1 1 calc R . . H41B H 0.9075 0.1905 0.5703 0.078 Uiso 1 1 calc R . . C42 C 0.976(4) 0.300(2) 0.5240(16) 0.100(12) Uani 1 1 d U . . H42A H 0.9241 0.3576 0.4967 0.120 Uiso 1 1 calc R . . H42B H 1.0684 0.2771 0.5031 0.120 Uiso 1 1 calc R . . C43 C 1.044(5) 0.298(2) 0.5876(19) 0.16(2) Uani 1 1 d D . . H43A H 0.9478 0.3154 0.6094 0.190 Uiso 1 1 calc R . . H43B H 1.0996 0.2399 0.6132 0.190 Uiso 1 1 calc R . . C51 C 0.610(3) 0.1946(16) 0.5183(12) 0.070(8) Uani 1 1 d . . . H51A H 0.5396 0.2301 0.5373 0.084 Uiso 1 1 calc R . . H51B H 0.5404 0.1940 0.4848 0.084 Uiso 1 1 calc R . . C52 C 0.654(4) 0.109(2) 0.5642(16) 0.094(11) Uani 1 1 d U . . H52A H 0.7441 0.1064 0.5928 0.113 Uiso 1 1 calc R . . H52B H 0.6987 0.0710 0.5434 0.113 Uiso 1 1 calc R . . C53 C 0.501(5) 0.078(2) 0.6026(17) 0.106(16) Uani 1 1 d . . . H53A H 0.5407 0.0242 0.6372 0.128 Uiso 1 1 calc R . . H53B H 0.4399 0.1194 0.6183 0.128 Uiso 1 1 calc R . . C54 C 0.395(6) 0.067(3) 0.5564(19) 0.20(3) Uani 1 1 d . . . H54A H 0.3432 0.1223 0.5262 0.294 Uiso 1 1 calc R . . H54B H 0.3066 0.0385 0.5769 0.294 Uiso 1 1 calc R . . H54C H 0.4646 0.0346 0.5359 0.294 Uiso 1 1 calc R . . C60 C 0.885(3) 0.1838(14) 0.4638(12) 0.059(8) Uani 1 1 d . . . H60A H 0.9754 0.2143 0.4469 0.071 Uiso 1 1 calc R . . H60B H 0.9365 0.1316 0.4978 0.071 Uiso 1 1 calc R . . C61 C 0.817(4) 0.1612(19) 0.4148(16) 0.117(14) Uani 1 1 d . . . H61A H 0.7863 0.2124 0.3775 0.140 Uiso 1 1 calc R . . H61B H 0.7119 0.1411 0.4284 0.140 Uiso 1 1 calc R . . C63 C 1.092(5) 0.1222(18) 0.3689(17) 0.127(16) Uani 1 1 d . . . H63A H 1.0746 0.1421 0.3244 0.191 Uiso 1 1 calc R . . H63B H 1.1872 0.0748 0.3830 0.191 Uiso 1 1 calc R . . H63C H 1.1142 0.1672 0.3803 0.191 Uiso 1 1 calc R . . C62 C 0.935(5) 0.095(2) 0.3982(17) 0.122(15) Uani 1 1 d . . . H62A H 0.9689 0.0448 0.4357 0.147 Uiso 1 1 calc R . . H62B H 0.8730 0.0801 0.3698 0.147 Uiso 1 1 calc R . . C70 C 0.680(3) 0.3202(14) 0.4401(11) 0.051(7) Uani 1 1 d U . . H70A H 0.7722 0.3485 0.4218 0.061 Uiso 1 1 calc R . . H70B H 0.6263 0.3087 0.4078 0.061 Uiso 1 1 calc R . . C71 C 0.554(4) 0.3790(17) 0.4576(15) 0.117(14) Uani 1 1 d . . . H71A H 0.6082 0.3921 0.4891 0.141 Uiso 1 1 calc R . . H71B H 0.4626 0.3507 0.4767 0.141 Uiso 1 1 calc R . . C72 C 0.479(4) 0.4585(16) 0.4075(15) 0.102(12) Uani 1 1 d . . . H72A H 0.4334 0.4451 0.3747 0.123 Uiso 1 1 calc R . . H72B H 0.5704 0.4884 0.3905 0.123 Uiso 1 1 calc R . . C73 C 0.340(5) 0.5181(19) 0.4233(14) 0.128(16) Uani 1 1 d . . . H73A H 0.2399 0.4940 0.4327 0.193 Uiso 1 1 calc R . . H73B H 0.3131 0.5714 0.3884 0.193 Uiso 1 1 calc R . . H73C H 0.3783 0.5273 0.4588 0.193 Uiso 1 1 calc R . . C44 C 1.165(5) 0.354(3) 0.579(2) 0.22(2) Uani 1 1 d DU . . H44A H 1.1711 0.3849 0.5349 0.333 Uiso 1 1 calc R . . H44B H 1.2767 0.3200 0.5960 0.333 Uiso 1 1 calc R . . H44C H 1.1278 0.3926 0.5991 0.333 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.0268(11) 0.0308(10) 0.0310(12) -0.0112(9) 0.0022(9) -0.0053(8) Au3 0.0204(6) 0.0279(7) 0.0272(7) -0.0110(6) -0.0008(6) -0.0048(5) Au2 0.0246(7) 0.0278(7) 0.0312(8) -0.0077(6) -0.0006(6) -0.0045(6) S1 0.023(4) 0.039(5) 0.026(5) -0.003(4) 0.000(4) -0.014(4) S2 0.020(4) 0.035(5) 0.030(5) -0.005(4) 0.006(4) -0.011(3) S3 0.033(5) 0.031(4) 0.036(6) -0.006(4) 0.006(4) -0.009(4) S4 0.044(6) 0.046(5) 0.025(5) -0.005(4) 0.007(4) -0.022(4) S5 0.030(5) 0.042(5) 0.032(5) -0.008(4) -0.002(4) -0.006(4) S6 0.021(4) 0.033(5) 0.052(6) -0.016(4) -0.009(4) 0.002(4) S7 0.028(4) 0.049(5) 0.022(4) -0.006(4) 0.000(3) -0.016(4) S8 0.022(4) 0.043(5) 0.037(5) -0.009(4) -0.010(3) -0.011(3) S9 0.031(5) 0.044(5) 0.049(6) -0.012(4) 0.000(4) -0.009(4) S10 0.040(5) 0.048(5) 0.025(5) -0.003(4) 0.012(4) -0.022(4) C1 0.019(7) 0.019(7) 0.019(7) -0.007(3) 0.001(2) -0.003(2) C2 0.029(8) 0.029(8) 0.029(8) -0.011(3) 0.001(2) -0.006(3) C3 0.028(8) 0.028(8) 0.028(8) -0.010(3) 0.001(2) -0.007(3) C4 0.014(6) 0.014(6) 0.014(6) -0.005(3) 0.001(2) -0.003(2) C5 0.036(8) 0.036(8) 0.036(8) -0.013(4) 0.002(2) -0.008(3) C6 0.027(8) 0.028(8) 0.027(8) -0.010(3) 0.002(2) -0.005(2) C7 0.028(8) 0.028(8) 0.029(8) -0.011(3) 0.002(2) -0.006(3) C8 0.025(6) 0.026(6) 0.026(6) -0.008(3) 0.002(2) -0.006(2) C9 0.024(15) 0.035(14) 0.046(17) -0.013(12) 0.006(12) -0.018(11) C10 0.015(6) 0.015(6) 0.015(6) -0.006(3) 0.000(2) -0.003(2) C11 0.030(8) 0.030(8) 0.030(8) -0.011(4) 0.002(2) -0.006(3) C12 0.019(7) 0.020(6) 0.020(7) -0.007(3) 0.002(2) -0.005(2) C13 0.043(9) 0.043(9) 0.043(9) -0.016(4) 0.003(2) -0.009(3) C14 0.031(16) 0.025(14) 0.024(16) -0.007(12) -0.002(12) -0.002(11) C15 0.043(18) 0.09(2) 0.024(16) -0.031(15) 0.010(13) -0.031(16) C16 0.026(14) 0.08(2) 0.027(15) -0.026(15) 0.022(12) -0.023(14) C17 0.042(17) 0.053(18) 0.044(19) -0.007(14) 0.022(14) -0.001(13) C18 0.024(7) 0.024(7) 0.024(7) -0.009(3) 0.002(2) -0.005(2) C19 0.039(10) 0.039(10) 0.040(10) -0.014(4) 0.003(2) -0.008(3) C20 0.017(6) 0.016(6) 0.017(6) -0.007(3) 0.002(2) -0.003(2) C21 0.051(10) 0.051(10) 0.051(10) -0.019(4) 0.003(2) -0.011(3) C22 0.015(6) 0.014(6) 0.014(6) -0.005(3) 0.001(2) -0.003(2) C23 0.047(10) 0.047(10) 0.046(10) -0.017(4) 0.003(2) -0.010(3) C24 0.014(13) 0.033(14) 0.014(14) 0.002(11) 0.001(11) 0.001(10) C25 0.008(6) 0.009(6) 0.008(6) -0.003(3) 0.001(2) -0.001(2) C26 0.021(14) 0.026(14) 0.041(17) -0.010(12) -0.021(12) -0.003(10) C27 0.026(15) 0.034(16) 0.020(16) -0.009(12) -0.011(12) -0.008(12) C28 0.034(17) 0.051(19) 0.09(3) -0.025(17) 0.023(17) -0.021(14) C29 0.053(16) 0.011(10) 0.039(15) -0.017(10) -0.002(12) -0.011(10) C30 0.027(16) 0.057(19) 0.06(2) -0.011(17) -0.028(15) -0.010(14) C31 0.032(7) 0.033(7) 0.032(7) -0.012(3) 0.002(2) -0.007(2) C32 0.047(8) 0.048(8) 0.048(8) -0.018(3) 0.002(2) -0.010(3) C33 0.015(6) 0.015(6) 0.015(6) -0.005(3) 0.001(2) -0.004(2) C34 0.032(7) 0.031(7) 0.032(7) -0.012(3) 0.002(2) -0.006(2) C35 0.029(17) 0.043(17) 0.034(18) 0.004(13) 0.002(14) 0.005(12) C36 0.037(9) 0.036(9) 0.037(9) -0.014(4) 0.003(2) -0.008(3) C37 0.027(8) 0.027(8) 0.027(8) -0.010(3) 0.001(2) -0.006(3) C38 0.039(17) 0.055(18) 0.043(19) -0.028(15) 0.022(14) -0.036(14) C39 0.034(8) 0.035(8) 0.035(8) -0.013(4) 0.002(2) -0.008(3) C40 0.08(3) 0.06(2) 0.03(2) -0.012(17) 0.015(18) -0.05(2) N1 0.038(16) 0.077(19) 0.07(2) -0.035(17) -0.001(15) -0.024(14) N2 0.090(10) 0.092(10) 0.090(10) -0.033(4) 0.006(2) -0.019(3) N3 0.022(12) 0.065(16) 0.029(14) -0.006(12) -0.010(11) -0.015(11) N4 0.053(15) 0.083(18) 0.024(14) 0.028(13) -0.010(12) -0.019(13) N5 0.068(9) 0.069(9) 0.068(9) -0.024(4) 0.004(2) -0.015(3) N6 0.016(14) 0.14(3) 0.08(2) -0.03(2) -0.005(15) -0.021(16) N7 0.027(13) 0.089(18) 0.064(18) -0.003(14) -0.004(13) -0.025(13) N8 0.060(16) 0.092(18) 0.040(16) -0.009(14) 0.005(13) -0.035(14) N9 0.072(8) 0.073(8) 0.072(8) -0.026(3) 0.004(2) -0.016(3) N10 0.073(19) 0.039(13) 0.026(14) 0.002(11) -0.022(13) -0.001(13) N11 0.057(14) 0.059(13) 0.029(12) -0.004(10) -0.008(11) -0.011(11) C41 0.036(15) 0.11(2) 0.025(15) -0.008(15) 0.013(12) -0.006(15) C42 0.100(12) 0.100(12) 0.100(12) -0.037(5) 0.006(2) -0.021(3) C43 0.16(4) 0.11(4) 0.17(5) -0.01(3) -0.13(4) -0.04(3) C51 0.052(18) 0.09(2) 0.07(2) -0.018(17) -0.003(16) -0.023(16) C52 0.094(11) 0.094(11) 0.094(11) -0.035(5) 0.005(2) -0.020(3) C53 0.17(4) 0.06(2) 0.09(3) -0.03(2) 0.07(3) -0.02(3) C54 0.30(8) 0.14(4) 0.13(5) -0.01(3) 0.01(5) -0.08(5) C60 0.09(2) 0.034(14) 0.07(2) -0.030(15) 0.022(17) -0.023(14) C61 0.09(3) 0.12(3) 0.18(4) -0.11(3) -0.04(3) 0.02(2) C63 0.15(4) 0.05(2) 0.15(4) -0.04(2) 0.01(3) 0.03(2) C62 0.11(3) 0.13(3) 0.13(4) -0.04(3) 0.05(3) -0.05(3) C70 0.051(7) 0.051(7) 0.050(7) -0.018(3) 0.003(2) -0.011(2) C71 0.16(4) 0.06(2) 0.10(3) -0.03(2) -0.03(3) 0.04(2) C72 0.14(3) 0.039(17) 0.11(3) -0.026(19) -0.01(2) 0.022(19) C73 0.20(4) 0.07(2) 0.09(3) -0.02(2) -0.01(3) 0.01(3) C44 0.22(2) 0.22(2) 0.22(2) -0.084(9) 0.013(2) -0.046(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 S1 2.297(8) . ? Au1 S1 2.297(8) 2_757 ? Au1 S2 2.309(8) . ? Au1 S2 2.309(8) 2_757 ? Au3 S10 2.259(8) . ? Au3 S8 2.271(8) . ? Au3 S7 2.278(8) . ? Au3 S9 2.295(8) . ? Au2 S4 2.297(8) . ? Au2 S5 2.303(8) . ? Au2 S3 2.320(9) . ? Au2 S6 2.329(8) . ? S1 C1 1.71(3) . ? S2 C2 1.67(3) . ? S3 C9 1.73(3) . ? S4 C10 1.75(2) . ? S5 C17 1.77(3) . ? S6 C18 1.71(3) . ? S7 C25 1.74(2) . ? S8 C26 1.73(3) . ? S9 C33 1.74(2) . ? S10 C34 1.78(3) . ? C1 C3 1.39(3) . ? C1 C2 1.43(3) . ? C2 C4 1.40(3) . ? C3 C5 1.45(4) . ? C4 C6 1.39(3) . ? C5 C7 1.43(4) . ? C5 C6 1.47(4) . ? C6 C8 1.46(3) . ? C7 N1 1.16(3) . ? C8 N2 1.12(3) . ? C9 C11 1.34(4) . ? C9 C10 1.55(3) . ? C10 C12 1.35(3) . ? C11 C13 1.30(4) . ? C12 C14 1.35(3) . ? C13 C15 1.44(4) . ? C13 C14 1.49(4) . ? C14 C16 1.41(4) . ? C15 N3 1.12(3) . ? C16 N4 1.10(3) . ? C17 C19 1.42(4) . ? C17 C18 1.45(4) . ? C18 C20 1.46(3) . ? C19 C21 1.30(4) . ? C20 C22 1.30(3) . ? C21 C22 1.39(4) . ? C21 C23 1.49(4) . ? C22 C24 1.51(3) . ? C23 N5 1.09(4) . ? C24 N6 1.07(3) . ? C25 C26 1.30(3) . ? C25 C27 1.43(3) . ? C26 C28 1.37(4) . ? C27 C29 1.41(3) . ? C28 C30 1.45(4) . ? C29 C30 1.37(4) . ? C29 C31 1.423(18) . ? C30 C32 1.41(4) . ? C31 N7 1.14(3) . ? C32 N8 1.18(3) . ? C33 C34 1.37(3) . ? C33 C35 1.39(3) . ? C34 C36 1.33(4) . ? C35 C37 1.44(4) . ? C36 C38 1.44(4) . ? C37 C38 1.44(3) . ? C37 C39 1.44(4) . ? C38 C40 1.36(4) . ? C39 N9 1.18(3) . ? C40 N10 1.17(4) . ? N11 C70 1.49(3) . ? N11 C60 1.50(3) . ? N11 C41 1.51(3) . ? N11 C51 1.52(3) . ? C41 C42 1.45(3) . ? C42 C43 1.56(4) . ? C43 C44 1.461(19) . ? C51 C52 1.44(3) . ? C52 C53 1.56(4) . ? C53 C54 1.46(5) . ? C60 C61 1.48(3) . ? C61 C62 1.49(4) . ? C63 C62 1.49(4) . ? C70 C71 1.44(3) . ? C71 C72 1.45(3) . ? C72 C73 1.49(4) . ? 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 S1 180.000(1) . 2_757 ? S1 Au1 S2 89.6(3) . . ? S1 Au1 S2 90.4(3) 2_757 . ? S1 Au1 S2 90.4(3) . 2_757 ? S1 Au1 S2 89.6(3) 2_757 2_757 ? S2 Au1 S2 180.000(2) . 2_757 ? S10 Au3 S8 88.7(3) . . ? S10 Au3 S7 179.0(3) . . ? S8 Au3 S7 90.5(3) . . ? S10 Au3 S9 90.1(3) . . ? S8 Au3 S9 178.8(3) . . ? S7 Au3 S9 90.7(3) . . ? S4 Au2 S5 178.6(3) . . ? S4 Au2 S3 89.1(3) . . ? S5 Au2 S3 89.9(3) . . ? S4 Au2 S6 91.1(3) . . ? S5 Au2 S6 90.0(3) . . ? S3 Au2 S6 178.7(3) . . ? C1 S1 Au1 101.4(10) . . ? C2 S2 Au1 103.9(10) . . ? C9 S3 Au2 107.1(9) . . ? C10 S4 Au2 105.7(9) . . ? C17 S5 Au2 103.0(11) . . ? C18 S6 Au2 103.5(10) . . ? C25 S7 Au3 100.8(8) . . ? C26 S8 Au3 101.1(11) . . ? C33 S9 Au3 103.0(8) . . ? C34 S10 Au3 103.1(9) . . ? C3 C1 C2 121(3) . . ? C3 C1 S1 114(2) . . ? C2 C1 S1 124(2) . . ? C4 C2 C1 119(3) . . ? C4 C2 S2 120(2) . . ? C1 C2 S2 121(2) . . ? C1 C3 C5 119(3) . . ? C6 C4 C2 122(3) . . ? C7 C5 C3 119(3) . . ? C7 C5 C6 120(3) . . ? C3 C5 C6 118(3) . . ? C4 C6 C8 121(3) . . ? C4 C6 C5 118(3) . . ? C8 C6 C5 117(3) . . ? N1 C7 C5 171(3) . . ? N2 C8 C6 167(3) . . ? C11 C9 C10 116(3) . . ? C11 C9 S3 126(2) . . ? C10 C9 S3 117(2) . . ? C12 C10 C9 116(2) . . ? C12 C10 S4 124(2) . . ? C9 C10 S4 120.3(19) . . ? C13 C11 C9 125(3) . . ? C10 C12 C14 127(3) . . ? C11 C13 C15 120(3) . . ? C11 C13 C14 121(3) . . ? C15 C13 C14 118(3) . . ? C12 C14 C16 126(3) . . ? C12 C14 C13 115(3) . . ? C16 C14 C13 119(3) . . ? N3 C15 C13 174(3) . . ? N4 C16 C14 177(3) . . ? C19 C17 C18 121(3) . . ? C19 C17 S5 118(3) . . ? C18 C17 S5 121(2) . . ? C17 C18 C20 112(3) . . ? C17 C18 S6 122(2) . . ? C20 C18 S6 125(2) . . ? C21 C19 C17 120(4) . . ? C22 C20 C18 124(3) . . ? C19 C21 C22 122(3) . . ? C19 C21 C23 124(3) . . ? C22 C21 C23 114(3) . . ? C20 C22 C21 120(3) . . ? C20 C22 C24 118(2) . . ? C21 C22 C24 122(3) . . ? N5 C23 C21 169(4) . . ? N6 C24 C22 170(3) . . ? C26 C25 C27 122(3) . . ? C26 C25 S7 123(2) . . ? C27 C25 S7 114.7(19) . . ? C25 C26 C28 122(3) . . ? C25 C26 S8 124(2) . . ? C28 C26 S8 114(2) . . ? C29 C27 C25 118(3) . . ? C26 C28 C30 118(3) . . ? C30 C29 C27 119(2) . . ? C30 C29 C31 123(3) . . ? C27 C29 C31 118(2) . . ? C29 C30 C32 120(3) . . ? C29 C30 C28 120(3) . . ? C32 C30 C28 120(3) . . ? N7 C31 C29 175(3) . . ? N8 C32 C30 177(3) . . ? C34 C33 C35 121(2) . . ? C34 C33 S9 122(2) . . ? C35 C33 S9 117(2) . . ? C36 C34 C33 124(3) . . ? C36 C34 S10 115(2) . . ? C33 C34 S10 121(2) . . ? C33 C35 C37 116(3) . . ? C34 C36 C38 122(3) . . ? C35 C37 C38 124(3) . . ? C35 C37 C39 114(3) . . ? C38 C37 C39 122(3) . . ? C40 C38 C36 124(3) . . ? C40 C38 C37 121(3) . . ? C36 C38 C37 114(3) . . ? N9 C39 C37 172(3) . . ? N10 C40 C38 169(4) . . ? C70 N11 C60 110.8(18) . . ? C70 N11 C41 112.7(19) . . ? C60 N11 C41 107.3(18) . . ? C70 N11 C51 106.7(18) . . ? C60 N11 C51 112.8(19) . . ? C41 N11 C51 106.5(18) . . ? C42 C41 N11 116(2) . . ? C41 C42 C43 103(3) . . ? C44 C43 C42 111(4) . . ? C52 C51 N11 117(2) . . ? C51 C52 C53 115(3) . . ? C54 C53 C52 102(3) . . ? C61 C60 N11 116(2) . . ? C60 C61 C62 115(3) . . ? C63 C62 C61 114(3) . . ? C71 C70 N11 118(2) . . ? C70 C71 C72 116(3) . . ? C71 C72 C73 117(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.428 _refine_diff_density_min -1.709 _refine_diff_density_rms 0.229 data_au120k _database_code_depnum_ccdc_archive 'CCDC 670915' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (n-Bu!4$N)!2$(Au(dcbdt)!2$)!5$! _chemical_melting_point ? _chemical_formula_moiety '2(C16 H36 N), 5(C16 H4 Au N4 S4)' _chemical_formula_sum 'C112 H92 Au5 N22 S20' _chemical_formula_weight 3372.11 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9351(1) _cell_length_b 17.0822(3) _cell_length_c 22.9746(4) _cell_angle_alpha 68.763(2) _cell_angle_beta 88.809(1) _cell_angle_gamma 78.163(1) _cell_volume 2836.08(9) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1633 _exptl_absorpt_coefficient_mu 6.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2323 _exptl_absorpt_correction_T_max 0.8204 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS APEX- CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70525 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.68 _reflns_number_total 10747 _reflns_number_gt 8677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART, (Bruker, 2004)' _computing_cell_refinement 'Bruker SMART, (Bruker, 2004)' _computing_data_reduction 'Bruker SAINT, (Bruker, 2004)' _computing_structure_solution 'SIR97 (Altomare, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SCHAKAL(Keller,1989),ORTEP3(Farrugia,1997) _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0263P)^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 10747 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0565 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 1.0000 0.0000 1.0000 0.01222(5) Uani 1 2 d S . . Au3 Au 0.120643(18) 0.428853(9) 0.961991(7) 0.01059(5) Uani 1 1 d . . . Au2 Au 0.552743(17) 0.215498(8) 0.980065(6) 0.01126(4) Uani 1 1 d . . . S1 S 0.71821(12) 0.00435(6) 0.97469(4) 0.0153(2) Uani 1 1 d . . . S2 S 1.02722(12) 0.08976(6) 0.89921(5) 0.0160(2) Uani 1 1 d . . . S3 S 0.27297(12) 0.21697(6) 0.95452(4) 0.0148(2) Uani 1 1 d . . . S4 S 0.57607(12) 0.30851(6) 0.87974(4) 0.0158(2) Uani 1 1 d . . . S5 S 0.52566(12) 0.12449(6) 1.08046(4) 0.0149(2) Uani 1 1 d . . . S6 S 0.83369(12) 0.21222(6) 1.00637(4) 0.0148(2) Uani 1 1 d . . . S7 S -0.16114(12) 0.43454(6) 0.93602(4) 0.0134(2) Uani 1 1 d . . . S8 S 0.14857(12) 0.52315(6) 0.86318(4) 0.0144(2) Uani 1 1 d . . . S9 S 0.09630(12) 0.33503(6) 1.06180(4) 0.0135(2) Uani 1 1 d . . . S10 S 0.40153(12) 0.42542(6) 0.98681(4) 0.0136(2) Uani 1 1 d . . . C1 C 0.6901(5) 0.0744(2) 0.89701(17) 0.0133(8) Uani 1 1 d . . . C2 C 0.8234(5) 0.1091(2) 0.86417(18) 0.0151(8) Uani 1 1 d . . . C3 C 0.5243(5) 0.0953(2) 0.86757(18) 0.0146(8) Uani 1 1 d . . . H3 H 0.4324 0.0734 0.8905 0.017 Uiso 1 1 calc R . . C4 C 0.7946(5) 0.1620(2) 0.80027(19) 0.0175(9) Uani 1 1 d . . . H4 H 0.8860 0.1847 0.7775 0.021 Uiso 1 1 calc R . . C5 C 0.4960(5) 0.1480(2) 0.80507(19) 0.0174(9) Uani 1 1 d . . . C6 C 0.6336(5) 0.1808(2) 0.77090(19) 0.0179(9) Uani 1 1 d . . . C7 C 0.3270(5) 0.1696(2) 0.77448(18) 0.0170(9) Uani 1 1 d . . . C8 C 0.6022(5) 0.2329(3) 0.7053(2) 0.0235(10) Uani 1 1 d . . . C9 C 0.2400(5) 0.2895(2) 0.87772(17) 0.0130(8) Uani 1 1 d . . . C10 C 0.3712(5) 0.3283(2) 0.84452(18) 0.0152(8) Uani 1 1 d . . . C11 C 0.0751(5) 0.3095(2) 0.84850(18) 0.0141(8) Uani 1 1 d . . . H11 H -0.0141 0.2839 0.8707 0.017 Uiso 1 1 calc R . . C12 C 0.3382(5) 0.3861(2) 0.78219(18) 0.0154(9) Uani 1 1 d . . . H12 H 0.4273 0.4115 0.7598 0.018 Uiso 1 1 calc R . . C13 C 0.0421(4) 0.3669(2) 0.78697(18) 0.0134(8) Uani 1 1 d . . . C14 C 0.1741(5) 0.4058(2) 0.75366(18) 0.0152(8) Uani 1 1 d . . . C15 C -0.1272(5) 0.3862(2) 0.75769(18) 0.0181(9) Uani 1 1 d . . . C16 C 0.1335(5) 0.4688(2) 0.6911(2) 0.0188(9) Uani 1 1 d . . . C17 C 0.7283(5) 0.1055(2) 1.11599(17) 0.0135(8) Uani 1 1 d . . . C18 C 0.8635(5) 0.1411(2) 1.08342(17) 0.0129(8) Uani 1 1 d . . . C19 C 0.7558(5) 0.0518(2) 1.17957(18) 0.0156(9) Uani 1 1 d . . . H19 H 0.6636 0.0293 1.2018 0.019 Uiso 1 1 calc R . . C20 C 1.0273(5) 0.1197(2) 1.11391(18) 0.0138(8) Uani 1 1 d . . . H20 H 1.1196 0.1423 1.0917 0.017 Uiso 1 1 calc R . . C21 C 0.9172(5) 0.0318(2) 1.20976(18) 0.0160(8) Uani 1 1 d . . . C22 C 1.0549(5) 0.0659(2) 1.17624(19) 0.0165(9) Uani 1 1 d . . . C23 C 0.9472(5) -0.0224(2) 1.27480(19) 0.0193(9) Uani 1 1 d . . . C24 C 1.2224(5) 0.0450(2) 1.20712(18) 0.0175(9) Uani 1 1 d . . . C25 C -0.1912(5) 0.5087(2) 0.85919(18) 0.0147(8) Uani 1 1 d . . . C26 C -0.0542(5) 0.5447(2) 0.82649(18) 0.0154(8) Uani 1 1 d . . . C27 C -0.3523(5) 0.5301(2) 0.82874(18) 0.0149(9) Uani 1 1 d . . . H27 H -0.4448 0.5074 0.8506 0.018 Uiso 1 1 calc R . . C28 C -0.0818(5) 0.5982(2) 0.76358(18) 0.0144(8) Uani 1 1 d . . . H28 H 0.0100 0.6215 0.7416 0.017 Uiso 1 1 calc R . . C29 C -0.3795(5) 0.5844(2) 0.76657(17) 0.0130(8) Uani 1 1 d . . . C30 C -0.2422(5) 0.6177(2) 0.73284(18) 0.0151(8) Uani 1 1 d . . . C31 C -0.5488(5) 0.6061(2) 0.73652(17) 0.0150(8) Uani 1 1 d . . . C32 C -0.2681(5) 0.6697(2) 0.66724(19) 0.0174(9) Uani 1 1 d . . . C33 C 0.2978(5) 0.3184(2) 1.09714(17) 0.0104(8) Uani 1 1 d . . . C34 C 0.4307(4) 0.3564(2) 1.06475(17) 0.0109(8) Uani 1 1 d . . . C35 C 0.3296(5) 0.2635(2) 1.16093(18) 0.0150(8) Uani 1 1 d . . . H35 H 0.2392 0.2395 1.1834 0.018 Uiso 1 1 calc R . . C36 C 0.5952(5) 0.3363(2) 1.09561(17) 0.0120(8) Uani 1 1 d . . . H36 H 0.6856 0.3611 1.0737 0.014 Uiso 1 1 calc R . . C37 C 0.4887(5) 0.2448(2) 1.19041(18) 0.0135(8) Uani 1 1 d . . . C38 C 0.6257(5) 0.2814(2) 1.15674(18) 0.0148(8) Uani 1 1 d . . . C39 C 0.5203(5) 0.1895(3) 1.2555(2) 0.0214(9) Uani 1 1 d . . . C40 C 0.7932(5) 0.2597(2) 1.18721(18) 0.0161(9) Uani 1 1 d . . . N1 N 0.1918(4) 0.1878(2) 0.75064(17) 0.0294(9) Uani 1 1 d . . . N2 N 0.5753(5) 0.2727(3) 0.65325(17) 0.0371(10) Uani 1 1 d . . . N3 N -0.2624(4) 0.4027(2) 0.73438(16) 0.0260(8) Uani 1 1 d . . . N4 N 0.0950(4) 0.5199(2) 0.64246(16) 0.0271(8) Uani 1 1 d . . . N5 N 0.9760(5) -0.0653(2) 1.32633(16) 0.0302(9) Uani 1 1 d . . . N6 N 1.3565(4) 0.0282(2) 1.23192(16) 0.0263(8) Uani 1 1 d . . . N7 N -0.6858(4) 0.6233(2) 0.71433(15) 0.0233(8) Uani 1 1 d . . . N8 N -0.2892(4) 0.7103(2) 0.61499(16) 0.0281(8) Uani 1 1 d . . . N9 N 0.5450(4) 0.1467(2) 1.30686(16) 0.0306(9) Uani 1 1 d . . . N10 N 0.9285(4) 0.2415(2) 1.21130(15) 0.0216(8) Uani 1 1 d . . . N11 N 0.7548(4) 0.23434(18) 0.49121(14) 0.0192(7) Uani 1 1 d . . . C41 C 0.8469(5) 0.2450(2) 0.54423(18) 0.0246(9) Uani 1 1 d . . . H41A H 0.7582 0.2676 0.5684 0.030 Uiso 1 1 calc R . . H41B H 0.9076 0.1873 0.5725 0.030 Uiso 1 1 calc R . . C42 C 0.9745(6) 0.3021(3) 0.5272(2) 0.0317(11) Uani 1 1 d . . . H42A H 0.9149 0.3622 0.5037 0.038 Uiso 1 1 calc R . . H42B H 1.0608 0.2837 0.5005 0.038 Uiso 1 1 calc R . . C43 C 1.0646(6) 0.2957(3) 0.5882(2) 0.0430(13) Uani 1 1 d . . . H43A H 0.9758 0.3035 0.6177 0.052 Uiso 1 1 calc R . . H43B H 1.1378 0.2374 0.6078 0.052 Uiso 1 1 calc R . . C44 C 1.1707(7) 0.3587(3) 0.5786(3) 0.0637(17) Uani 1 1 d . . . H44A H 1.2556 0.3534 0.5479 0.096 Uiso 1 1 calc R . . H44B H 1.2308 0.3487 0.6183 0.096 Uiso 1 1 calc R . . H44C H 1.0975 0.4166 0.5631 0.096 Uiso 1 1 calc R . . C51 C 0.6053(5) 0.1918(2) 0.5174(2) 0.0270(10) Uani 1 1 d . . . H51A H 0.5344 0.2256 0.5396 0.032 Uiso 1 1 calc R . . H51B H 0.5324 0.1949 0.4818 0.032 Uiso 1 1 calc R . . C52 C 0.6524(5) 0.0988(3) 0.5617(2) 0.0398(12) Uani 1 1 d . . . H52A H 0.7435 0.0919 0.5930 0.048 Uiso 1 1 calc R . . H52B H 0.6977 0.0615 0.5380 0.048 Uiso 1 1 calc R . . C53 C 0.4906(6) 0.0719(3) 0.5951(2) 0.0452(14) Uani 1 1 d . . . H53A H 0.5247 0.0129 0.6265 0.054 Uiso 1 1 calc R . . H53B H 0.4453 0.1107 0.6177 0.054 Uiso 1 1 calc R . . C54 C 0.3504(6) 0.0743(3) 0.5519(3) 0.0530(15) Uani 1 1 d . . . H54A H 0.3116 0.1332 0.5219 0.079 Uiso 1 1 calc R . . H54B H 0.2534 0.0553 0.5761 0.079 Uiso 1 1 calc R . . H54C H 0.3940 0.0361 0.5293 0.079 Uiso 1 1 calc R . . C60 C 0.8831(5) 0.1812(2) 0.46340(18) 0.0220(9) Uani 1 1 d . . . H60A H 0.9360 0.1267 0.4974 0.026 Uiso 1 1 calc R . . H60B H 0.9761 0.2125 0.4467 0.026 Uiso 1 1 calc R . . C61 C 0.8113(5) 0.1596(3) 0.4116(2) 0.0317(11) Uani 1 1 d . . . H61A H 0.7766 0.2128 0.3742 0.038 Uiso 1 1 calc R . . H61B H 0.7074 0.1358 0.4255 0.038 Uiso 1 1 calc R . . C62 C 0.9447(5) 0.0946(3) 0.3945(2) 0.0308(11) Uani 1 1 d . . . H62A H 0.9804 0.0424 0.4325 0.037 Uiso 1 1 calc R . . H62B H 0.8896 0.0778 0.3639 0.037 Uiso 1 1 calc R . . C63 C 1.1048(6) 0.1267(3) 0.3672(2) 0.0371(12) Uani 1 1 d . . . H63A H 1.0704 0.1818 0.3324 0.056 Uiso 1 1 calc R . . H63B H 1.1759 0.0847 0.3521 0.056 Uiso 1 1 calc R . . H63C H 1.1712 0.1341 0.3996 0.056 Uiso 1 1 calc R . . C70 C 0.6813(5) 0.3213(2) 0.44070(18) 0.0204(9) Uani 1 1 d . . . H70A H 0.6373 0.3118 0.4043 0.025 Uiso 1 1 calc R . . H70B H 0.7757 0.3526 0.4267 0.025 Uiso 1 1 calc R . . C71 C 0.5359(6) 0.3776(2) 0.46149(19) 0.0311(10) Uani 1 1 d . . . H71A H 0.4342 0.3508 0.4696 0.037 Uiso 1 1 calc R . . H71B H 0.5738 0.3815 0.5010 0.037 Uiso 1 1 calc R . . C72 C 0.4859(5) 0.4671(2) 0.4121(2) 0.0313(11) Uani 1 1 d . . . H72A H 0.5803 0.4978 0.4100 0.038 Uiso 1 1 calc R . . H72B H 0.4709 0.4626 0.3708 0.038 Uiso 1 1 calc R . . C73 C 0.3209(6) 0.5185(3) 0.4256(2) 0.0453(13) Uani 1 1 d . . . H73A H 0.2239 0.4929 0.4217 0.068 Uiso 1 1 calc R . . H73B H 0.3012 0.5778 0.3956 0.068 Uiso 1 1 calc R . . H73C H 0.3306 0.5180 0.4682 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01189(11) 0.01224(10) 0.01187(11) -0.00414(8) -0.00015(8) -0.00152(8) Au3 0.00956(8) 0.01099(8) 0.01049(8) -0.00339(6) -0.00084(6) -0.00147(6) Au2 0.01090(8) 0.01116(8) 0.01057(8) -0.00333(6) -0.00082(6) -0.00091(6) S1 0.0130(5) 0.0165(5) 0.0140(5) -0.0025(4) 0.0003(4) -0.0035(4) S2 0.0124(5) 0.0182(5) 0.0150(5) -0.0027(4) 0.0000(4) -0.0042(4) S3 0.0126(5) 0.0153(5) 0.0137(5) -0.0011(4) 0.0001(4) -0.0043(4) S4 0.0124(5) 0.0192(5) 0.0131(5) -0.0019(4) -0.0004(4) -0.0046(4) S5 0.0120(5) 0.0172(5) 0.0125(5) -0.0013(4) -0.0013(4) -0.0038(4) S6 0.0120(5) 0.0160(5) 0.0126(5) -0.0008(4) -0.0009(4) -0.0030(4) S7 0.0107(5) 0.0153(5) 0.0116(5) -0.0015(4) 0.0001(4) -0.0036(4) S8 0.0100(5) 0.0175(5) 0.0132(5) -0.0020(4) -0.0007(4) -0.0038(4) S9 0.0115(5) 0.0151(5) 0.0121(5) -0.0021(4) -0.0006(4) -0.0039(4) S10 0.0114(5) 0.0168(5) 0.0114(5) -0.0030(4) -0.0004(4) -0.0045(4) C1 0.017(2) 0.0129(19) 0.011(2) -0.0069(16) -0.0029(16) 0.0002(16) C2 0.0131(19) 0.0126(19) 0.018(2) -0.0064(17) 0.0007(17) 0.0019(16) C3 0.0142(19) 0.0121(19) 0.017(2) -0.0055(17) 0.0029(16) -0.0017(16) C4 0.016(2) 0.018(2) 0.018(2) -0.0062(17) 0.0030(17) -0.0046(17) C5 0.016(2) 0.015(2) 0.021(2) -0.0074(17) -0.0019(17) -0.0015(17) C6 0.016(2) 0.016(2) 0.018(2) -0.0039(17) 0.0013(17) 0.0004(17) C7 0.018(2) 0.015(2) 0.016(2) -0.0041(17) 0.0042(17) -0.0025(17) C8 0.013(2) 0.030(2) 0.025(3) -0.007(2) 0.0004(18) -0.0044(18) C9 0.017(2) 0.0086(18) 0.0110(19) -0.0020(15) -0.0019(16) 0.0005(16) C10 0.017(2) 0.0132(19) 0.016(2) -0.0080(17) -0.0031(16) 0.0002(16) C11 0.015(2) 0.0142(19) 0.013(2) -0.0048(16) -0.0001(16) -0.0026(16) C12 0.0127(19) 0.017(2) 0.016(2) -0.0059(17) 0.0027(16) -0.0048(16) C13 0.0096(18) 0.0140(19) 0.016(2) -0.0066(16) -0.0007(16) 0.0010(16) C14 0.017(2) 0.0135(19) 0.015(2) -0.0060(16) -0.0016(16) -0.0011(16) C15 0.021(2) 0.019(2) 0.013(2) -0.0039(17) 0.0027(17) -0.0053(18) C16 0.013(2) 0.019(2) 0.024(2) -0.0058(19) 0.0035(17) -0.0070(17) C17 0.0119(19) 0.0133(19) 0.014(2) -0.0057(16) 0.0003(16) 0.0020(16) C18 0.0144(19) 0.0144(19) 0.013(2) -0.0078(16) 0.0014(16) -0.0053(16) C19 0.017(2) 0.0122(19) 0.017(2) -0.0031(16) 0.0023(17) -0.0046(17) C20 0.0093(18) 0.0141(19) 0.019(2) -0.0072(17) 0.0037(16) -0.0035(16) C21 0.021(2) 0.0137(19) 0.012(2) -0.0044(16) 0.0006(17) -0.0008(17) C22 0.0110(19) 0.018(2) 0.021(2) -0.0097(17) -0.0015(17) -0.0005(16) C23 0.017(2) 0.020(2) 0.019(2) -0.0044(18) -0.0033(17) -0.0034(17) C24 0.017(2) 0.018(2) 0.017(2) -0.0046(17) -0.0006(17) -0.0049(17) C25 0.018(2) 0.0117(19) 0.014(2) -0.0052(16) -0.0002(16) 0.0001(16) C26 0.015(2) 0.0151(19) 0.016(2) -0.0059(17) -0.0024(16) -0.0016(16) C27 0.0129(19) 0.017(2) 0.021(2) -0.0121(17) 0.0042(17) -0.0075(16) C28 0.014(2) 0.0141(19) 0.015(2) -0.0055(17) 0.0039(16) -0.0033(16) C29 0.0133(19) 0.0116(18) 0.015(2) -0.0057(16) 0.0017(16) -0.0027(16) C30 0.0142(19) 0.0160(19) 0.014(2) -0.0040(16) -0.0031(16) -0.0031(16) C31 0.019(2) 0.017(2) 0.010(2) -0.0057(16) 0.0015(16) -0.0063(17) C32 0.0106(19) 0.020(2) 0.022(2) -0.0054(18) 0.0001(17) -0.0066(17) C33 0.0146(19) 0.0047(17) 0.0096(19) -0.0004(15) 0.0046(15) -0.0014(15) C34 0.0065(18) 0.0147(18) 0.0121(19) -0.0064(15) -0.0021(15) -0.0006(15) C35 0.013(2) 0.016(2) 0.017(2) -0.0069(17) 0.0004(16) -0.0040(16) C36 0.0116(19) 0.0146(19) 0.010(2) -0.0029(16) 0.0015(15) -0.0057(16) C37 0.015(2) 0.0075(18) 0.015(2) -0.0016(16) 0.0035(16) -0.0016(16) C38 0.0126(19) 0.017(2) 0.016(2) -0.0075(17) -0.0021(16) -0.0015(16) C39 0.020(2) 0.020(2) 0.024(3) -0.0066(19) -0.0012(18) -0.0067(18) C40 0.015(2) 0.015(2) 0.015(2) -0.0034(16) 0.0023(17) -0.0023(17) N1 0.0162(18) 0.041(2) 0.026(2) -0.0070(17) -0.0032(16) -0.0052(17) N2 0.029(2) 0.053(3) 0.018(2) 0.0009(19) -0.0029(16) -0.0090(19) N3 0.0157(18) 0.036(2) 0.0216(19) -0.0055(16) -0.0011(15) -0.0045(16) N4 0.0254(19) 0.030(2) 0.019(2) -0.0013(17) -0.0030(15) -0.0070(16) N5 0.035(2) 0.029(2) 0.020(2) -0.0007(17) -0.0053(16) -0.0059(17) N6 0.0203(19) 0.034(2) 0.024(2) -0.0085(16) -0.0039(16) -0.0066(16) N7 0.0146(18) 0.035(2) 0.0169(18) -0.0045(16) -0.0014(14) -0.0059(15) N8 0.028(2) 0.033(2) 0.018(2) 0.0016(16) -0.0041(16) -0.0121(17) N9 0.030(2) 0.035(2) 0.022(2) 0.0000(18) -0.0061(16) -0.0150(18) N10 0.0165(18) 0.0241(18) 0.0225(19) -0.0074(15) -0.0015(15) -0.0024(15) N11 0.0213(17) 0.0143(16) 0.0155(17) 0.0015(13) -0.0045(14) -0.0019(14) C41 0.030(2) 0.026(2) 0.016(2) -0.0060(18) -0.0087(18) -0.0032(19) C42 0.041(3) 0.031(2) 0.024(2) -0.009(2) -0.006(2) -0.012(2) C43 0.042(3) 0.040(3) 0.045(3) -0.012(2) -0.015(2) -0.009(2) C44 0.058(4) 0.064(4) 0.077(5) -0.039(3) -0.020(3) -0.002(3) C51 0.017(2) 0.024(2) 0.029(2) 0.0017(19) -0.0023(18) -0.0040(18) C52 0.025(2) 0.029(3) 0.047(3) 0.009(2) -0.008(2) -0.008(2) C53 0.038(3) 0.035(3) 0.046(3) 0.010(2) -0.006(2) -0.016(2) C54 0.036(3) 0.057(3) 0.064(4) -0.013(3) 0.008(3) -0.024(3) C60 0.019(2) 0.020(2) 0.023(2) -0.0040(17) -0.0044(17) -0.0006(17) C61 0.027(2) 0.031(2) 0.039(3) -0.018(2) -0.011(2) 0.002(2) C62 0.026(2) 0.028(2) 0.041(3) -0.020(2) -0.008(2) 0.001(2) C63 0.045(3) 0.033(3) 0.033(3) -0.012(2) 0.001(2) -0.007(2) C70 0.024(2) 0.015(2) 0.015(2) 0.0014(16) -0.0053(17) -0.0025(17) C71 0.040(3) 0.023(2) 0.026(2) -0.0093(19) -0.003(2) 0.004(2) C72 0.035(3) 0.021(2) 0.028(3) 0.0000(19) 0.003(2) -0.001(2) C73 0.060(3) 0.029(3) 0.039(3) -0.014(2) -0.005(3) 0.011(2) _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 2.3018(10) 2_757 ? Au1 S1 2.3018(9) . ? Au1 S2 2.3027(10) 2_757 ? Au1 S2 2.3027(10) . ? Au3 S10 2.2959(9) . ? Au3 S8 2.2965(10) . ? Au3 S7 2.2999(9) . ? Au3 S9 2.3045(9) . ? Au2 S3 2.3009(10) . ? Au2 S5 2.3026(10) . ? Au2 S6 2.3062(9) . ? Au2 S4 2.3068(10) . ? S1 C1 1.740(4) . ? S2 C2 1.736(4) . ? S3 C9 1.738(4) . ? S4 C10 1.745(4) . ? S5 C17 1.734(4) . ? S6 C18 1.734(4) . ? S7 C25 1.747(4) . ? S8 C26 1.739(4) . ? S9 C33 1.731(4) . ? S10 C34 1.740(4) . ? C1 C2 1.393(5) . ? C1 C3 1.409(5) . ? C2 C4 1.412(5) . ? C3 C5 1.384(5) . ? C4 C6 1.379(5) . ? C5 C6 1.421(5) . ? C5 C7 1.441(5) . ? C6 C8 1.442(6) . ? C7 N1 1.146(5) . ? C8 N2 1.140(5) . ? C9 C11 1.403(5) . ? C9 C10 1.410(5) . ? C10 C12 1.407(5) . ? C11 C13 1.391(5) . ? C12 C14 1.391(5) . ? C13 C14 1.417(5) . ? C13 C15 1.436(5) . ? C14 C16 1.445(5) . ? C15 N3 1.144(5) . ? C16 N4 1.140(5) . ? C17 C19 1.408(5) . ? C17 C18 1.409(5) . ? C18 C20 1.404(5) . ? C19 C21 1.387(5) . ? C20 C22 1.386(5) . ? C21 C22 1.423(5) . ? C21 C23 1.439(5) . ? C22 C24 1.435(5) . ? C23 N5 1.142(5) . ? C24 N6 1.149(5) . ? C25 C27 1.385(5) . ? C25 C26 1.425(5) . ? C26 C28 1.395(5) . ? C27 C29 1.385(5) . ? C28 C30 1.386(5) . ? C29 C30 1.418(5) . ? C29 C31 1.438(5) . ? C30 C32 1.439(5) . ? C31 N7 1.145(5) . ? C32 N8 1.144(5) . ? C33 C34 1.410(5) . ? C33 C35 1.419(5) . ? C34 C36 1.415(5) . ? C35 C37 1.367(5) . ? C36 C38 1.370(5) . ? C37 C38 1.437(5) . ? C37 C39 1.444(5) . ? C38 C40 1.430(5) . ? C39 N9 1.136(5) . ? C40 N10 1.148(5) . ? N11 C60 1.511(5) . ? N11 C51 1.518(5) . ? N11 C41 1.518(5) . ? N11 C70 1.522(4) . ? C41 C42 1.497(5) . ? C42 C43 1.544(6) . ? C43 C44 1.452(6) . ? C51 C52 1.517(5) . ? C52 C53 1.547(6) . ? C53 C54 1.491(7) . ? C60 C61 1.519(5) . ? C61 C62 1.525(5) . ? C62 C63 1.520(6) . ? C70 C71 1.529(5) . ? C71 C72 1.515(5) . ? C72 C73 1.513(6) . ? 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 S1 180.000(1) 2_757 . ? S1 Au1 S2 90.03(3) 2_757 2_757 ? S1 Au1 S2 89.97(3) . 2_757 ? S1 Au1 S2 89.97(3) 2_757 . ? S1 Au1 S2 90.03(3) . . ? S2 Au1 S2 180.000(1) 2_757 . ? S10 Au3 S8 88.72(3) . . ? S10 Au3 S7 179.07(4) . . ? S8 Au3 S7 90.48(3) . . ? S10 Au3 S9 90.38(3) . . ? S8 Au3 S9 179.00(4) . . ? S7 Au3 S9 90.41(3) . . ? S3 Au2 S5 89.58(3) . . ? S3 Au2 S6 179.29(3) . . ? S5 Au2 S6 89.89(3) . . ? S3 Au2 S4 89.95(3) . . ? S5 Au2 S4 178.99(3) . . ? S6 Au2 S4 90.59(3) . . ? C1 S1 Au1 102.39(13) . . ? C2 S2 Au1 102.67(14) . . ? C9 S3 Au2 102.80(13) . . ? C10 S4 Au2 103.09(14) . . ? C17 S5 Au2 102.81(13) . . ? C18 S6 Au2 102.86(13) . . ? C25 S7 Au3 102.54(13) . . ? C26 S8 Au3 103.20(13) . . ? C33 S9 Au3 102.45(12) . . ? C34 S10 Au3 102.56(12) . . ? C2 C1 C3 120.3(3) . . ? C2 C1 S1 122.6(3) . . ? C3 C1 S1 117.1(3) . . ? C1 C2 C4 119.8(3) . . ? C1 C2 S2 122.2(3) . . ? C4 C2 S2 118.0(3) . . ? C5 C3 C1 119.7(4) . . ? C6 C4 C2 120.0(4) . . ? C3 C5 C6 120.1(4) . . ? C3 C5 C7 120.1(4) . . ? C6 C5 C7 119.8(4) . . ? C4 C6 C5 120.1(4) . . ? C4 C6 C8 120.9(4) . . ? C5 C6 C8 118.9(4) . . ? N1 C7 C5 178.9(5) . . ? N2 C8 C6 178.3(5) . . ? C11 C9 C10 119.6(3) . . ? C11 C9 S3 117.6(3) . . ? C10 C9 S3 122.7(3) . . ? C12 C10 C9 120.5(3) . . ? C12 C10 S4 118.2(3) . . ? C9 C10 S4 121.3(3) . . ? C13 C11 C9 119.9(4) . . ? C14 C12 C10 119.5(4) . . ? C11 C13 C14 120.4(3) . . ? C11 C13 C15 119.1(4) . . ? C14 C13 C15 120.5(3) . . ? C12 C14 C13 120.1(3) . . ? C12 C14 C16 120.7(4) . . ? C13 C14 C16 119.1(3) . . ? N3 C15 C13 179.0(4) . . ? N4 C16 C14 177.1(4) . . ? C19 C17 C18 120.0(3) . . ? C19 C17 S5 117.7(3) . . ? C18 C17 S5 122.4(3) . . ? C20 C18 C17 119.7(3) . . ? C20 C18 S6 118.4(3) . . ? C17 C18 S6 121.9(3) . . ? C21 C19 C17 120.1(4) . . ? C22 C20 C18 120.3(4) . . ? C19 C21 C22 119.7(3) . . ? C19 C21 C23 120.8(4) . . ? C22 C21 C23 119.4(3) . . ? C20 C22 C21 120.2(3) . . ? C20 C22 C24 119.8(4) . . ? C21 C22 C24 120.0(4) . . ? N5 C23 C21 178.0(4) . . ? N6 C24 C22 179.9(7) . . ? C27 C25 C26 119.5(3) . . ? C27 C25 S7 118.3(3) . . ? C26 C25 S7 122.1(3) . . ? C28 C26 C25 119.7(3) . . ? C28 C26 S8 118.8(3) . . ? C25 C26 S8 121.4(3) . . ? C29 C27 C25 120.4(4) . . ? C30 C28 C26 120.6(4) . . ? C27 C29 C30 120.6(3) . . ? C27 C29 C31 119.0(3) . . ? C30 C29 C31 120.4(3) . . ? C28 C30 C29 119.2(3) . . ? C28 C30 C32 120.4(4) . . ? C29 C30 C32 120.4(3) . . ? N7 C31 C29 177.8(4) . . ? N8 C32 C30 179.3(4) . . ? C34 C33 C35 119.2(3) . . ? C34 C33 S9 122.5(3) . . ? C35 C33 S9 118.3(3) . . ? C33 C34 C36 119.5(3) . . ? C33 C34 S10 122.1(3) . . ? C36 C34 S10 118.4(3) . . ? C37 C35 C33 120.8(4) . . ? C38 C36 C34 120.7(4) . . ? C35 C37 C38 119.8(3) . . ? C35 C37 C39 120.7(4) . . ? C38 C37 C39 119.4(3) . . ? C36 C38 C40 120.5(4) . . ? C36 C38 C37 119.8(3) . . ? C40 C38 C37 119.7(3) . . ? N9 C39 C37 179.3(4) . . ? N10 C40 C38 179.0(4) . . ? C60 N11 C51 112.1(3) . . ? C60 N11 C41 108.4(3) . . ? C51 N11 C41 108.3(3) . . ? C60 N11 C70 109.3(3) . . ? C51 N11 C70 107.9(3) . . ? C41 N11 C70 110.8(3) . . ? C42 C41 N11 117.5(3) . . ? C41 C42 C43 108.3(4) . . ? C44 C43 C42 113.4(4) . . ? C52 C51 N11 116.3(3) . . ? C51 C52 C53 109.5(4) . . ? C54 C53 C52 113.7(4) . . ? N11 C60 C61 115.9(3) . . ? C60 C61 C62 111.1(3) . . ? C63 C62 C61 114.5(4) . . ? N11 C70 C71 114.2(3) . . ? C72 C71 C70 111.2(3) . . ? C73 C72 C71 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.958 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.117