#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Peter Skabara' _publ_contact_author_email PETER.SKABARA@STRATH.AC.UK _publ_section_title ; Novel dithiolene complexes incorporating conjugated electroactive ligands ; loop_ _publ_author_name 'Peter Skabara' 'Elena Cerrada' 'W Clegg' 'Simon Coles' 'Bianca Gonzalez' 'Ross W Harrington' ; M.Hursthouse ; 'Mariano Laguna' 'Nora Lardies Miazza' 'Asuncion Luquin' 'Cristina Pozo-Gonzalo' # Attachment 'dalton.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 675707' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H42 Au N P2 S10' _chemical_formula_weight 1356.45 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2162(1) _cell_length_b 14.6583(2) _cell_length_c 15.0674(2) _cell_angle_alpha 76.383(1) _cell_angle_beta 80.037(1) _cell_angle_gamma 65.190(1) _cell_volume 2760.10(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 19560 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description lath _exptl_crystal_colour black _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 3.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.352 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38561 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0487 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.45 _reflns_number_total 12263 _reflns_number_gt 9692 _reflns_threshold_expression I>2\s(I) _computing_data_collection COLLECT _computing_cell_refinement DENZO _computing_data_reduction DENZO _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ; _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^)+(0.0650P)^2^+5.7933P] 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_number_reflns 12263 _refine_ls_number_parameters 671 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1076 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8257(5) 0.7695(6) 0.2156(5) 0.067(2) Uani 1 1 d . . . H1 H 0.8400 0.8237 0.1756 0.080 Uiso 1 1 calc R . . C2 C 0.8092(5) 0.6991(7) 0.1874(4) 0.063(2) Uani 1 1 d . . . H2 H 0.8121 0.6975 0.1243 0.076 Uiso 1 1 calc R . . C3 C 0.7873(3) 0.6278(4) 0.2563(3) 0.0268(10) Uani 1 1 d . . . H3 H 0.7717 0.5743 0.2462 0.032 Uiso 1 1 calc R . . C4 C 0.7914(4) 0.6454(4) 0.3443(3) 0.0328(11) Uani 1 1 d . . . C5 C 0.7724(4) 0.5898(4) 0.4345(3) 0.0258(10) Uani 1 1 d . . . C6 C 0.7035(3) 0.5429(3) 0.4616(3) 0.0232(9) Uani 1 1 d . . . C7 C 0.7055(3) 0.4969(3) 0.5569(3) 0.0218(9) Uani 1 1 d . . . C8 C 0.7777(3) 0.5072(4) 0.5998(3) 0.0245(9) Uani 1 1 d . . . C9 C 0.8068(4) 0.4703(4) 0.6933(3) 0.0269(10) Uani 1 1 d . . . C10 C 0.9100(4) 0.4378(4) 0.7230(3) 0.0258(10) Uani 1 1 d . . . H10 H 0.9708 0.4351 0.6838 0.031 Uiso 1 1 calc R . . C11 C 0.9050(5) 0.4110(5) 0.8196(4) 0.0480(16) Uani 1 1 d . . . H11 H 0.9635 0.3902 0.8532 0.058 Uiso 1 1 calc R . . C12 C 0.8127(6) 0.4170(6) 0.8598(4) 0.0547(17) Uani 1 1 d . . . H12 H 0.7995 0.3987 0.9241 0.066 Uiso 1 1 calc R . . C25 C 0.1327(4) 0.9571(4) 0.3423(3) 0.0255(10) Uani 1 1 d . . . C26 C 0.1803(4) 0.8524(4) 0.3388(4) 0.0309(11) Uani 1 1 d . . . H26 H 0.2431 0.8110 0.3670 0.037 Uiso 1 1 calc R . . C27 C 0.1363(4) 0.8091(4) 0.2944(4) 0.0366(12) Uani 1 1 d . . . H27 H 0.1694 0.7383 0.2922 0.044 Uiso 1 1 calc R . . C28 C 0.0455(5) 0.8677(5) 0.2537(4) 0.0396(13) Uani 1 1 d . . . H28 H 0.0158 0.8371 0.2237 0.048 Uiso 1 1 calc R . . C29 C -0.0028(5) 0.9705(5) 0.2560(4) 0.0413(13) Uani 1 1 d . . . H29 H -0.0656 1.0106 0.2273 0.050 Uiso 1 1 calc R . . C30 C 0.0398(4) 1.0167(4) 0.3005(3) 0.0311(11) Uani 1 1 d . . . H30 H 0.0060 1.0877 0.3022 0.037 Uiso 1 1 calc R . . C31 C 0.1091(3) 1.1467(4) 0.3934(3) 0.0251(10) Uani 1 1 d . . . C32 C 0.1144(4) 1.2205(4) 0.3173(3) 0.0322(11) Uani 1 1 d . . . H32 H 0.1640 1.2012 0.2668 0.039 Uiso 1 1 calc R . . C33 C 0.0474(5) 1.3219(4) 0.3152(4) 0.0386(13) Uani 1 1 d . . . H33 H 0.0499 1.3720 0.2629 0.046 Uiso 1 1 calc R . . C34 C -0.0236(4) 1.3499(4) 0.3898(4) 0.0377(12) Uani 1 1 d . . . H34 H -0.0695 1.4195 0.3886 0.045 Uiso 1 1 calc R . . C35 C -0.0278(4) 1.2771(4) 0.4659(4) 0.0375(12) Uani 1 1 d . . . H35 H -0.0761 1.2970 0.5169 0.045 Uiso 1 1 calc R . . C36 C 0.0378(4) 1.1755(4) 0.4684(3) 0.0308(11) Uani 1 1 d . . . H36 H 0.0345 1.1256 0.5207 0.037 Uiso 1 1 calc R . . C37 C 0.2154(4) 0.9511(4) 0.5084(3) 0.0249(10) Uani 1 1 d . . . C38 C 0.1913(4) 0.8682(4) 0.5475(4) 0.0335(11) Uani 1 1 d . . . H38 H 0.1588 0.8447 0.5130 0.040 Uiso 1 1 calc R . . C39 C 0.2137(4) 0.8177(4) 0.6375(4) 0.0401(13) Uani 1 1 d . . . H39 H 0.1960 0.7608 0.6640 0.048 Uiso 1 1 calc R . . C40 C 0.2619(5) 0.8517(4) 0.6872(4) 0.0391(13) Uani 1 1 d . . . H40 H 0.2785 0.8174 0.7479 0.047 Uiso 1 1 calc R . . C41 C 0.2857(5) 0.9356(4) 0.6484(4) 0.0404(13) Uani 1 1 d . . . H41 H 0.3178 0.9594 0.6829 0.048 Uiso 1 1 calc R . . C42 C 0.2632(4) 0.9851(4) 0.5594(4) 0.0336(11) Uani 1 1 d . . . H42 H 0.2803 1.0424 0.5332 0.040 Uiso 1 1 calc R . . C43 C 0.4807(3) 0.8650(4) 0.4059(3) 0.0233(9) Uani 1 1 d . . . C44 C 0.4536(4) 0.7860(4) 0.4566(3) 0.0300(11) Uani 1 1 d . . . H44 H 0.4061 0.7684 0.4343 0.036 Uiso 1 1 calc R . . C45 C 0.4951(4) 0.7325(4) 0.5394(3) 0.0311(11) Uani 1 1 d . . . H45 H 0.4750 0.6796 0.5743 0.037 Uiso 1 1 calc R . . C46 C 0.5652(4) 0.7567(4) 0.5705(3) 0.0324(11) Uani 1 1 d . . . H46 H 0.5948 0.7195 0.6266 0.039 Uiso 1 1 calc R . . C47 C 0.5934(5) 0.8350(5) 0.5206(4) 0.0477(16) Uani 1 1 d . . . H47 H 0.6424 0.8511 0.5423 0.057 Uiso 1 1 calc R . . C48 C 0.5502(4) 0.8896(5) 0.4392(4) 0.0389(13) Uani 1 1 d . . . H48 H 0.5684 0.9443 0.4059 0.047 Uiso 1 1 calc R . . C49 C 0.4810(4) 1.0205(4) 0.2438(3) 0.0258(10) Uani 1 1 d . . . C50 C 0.4426(4) 1.1232(4) 0.2471(3) 0.0269(10) Uani 1 1 d . . . H50 H 0.3794 1.1536 0.2827 0.032 Uiso 1 1 calc R . . C51 C 0.4964(4) 1.1826(4) 0.1984(3) 0.0342(12) Uani 1 1 d . . . H51 H 0.4710 1.2529 0.2022 0.041 Uiso 1 1 calc R . . C52 C 0.5863(4) 1.1391(4) 0.1450(3) 0.0354(12) Uani 1 1 d . . . H52 H 0.6223 1.1799 0.1112 0.042 Uiso 1 1 calc R . . C53 C 0.6246(4) 1.0376(5) 0.1401(4) 0.0392(13) Uani 1 1 d . . . H53 H 0.6869 1.0083 0.1032 0.047 Uiso 1 1 calc R . . C54 C 0.5725(4) 0.9773(4) 0.1890(4) 0.0364(12) Uani 1 1 d . . . H54 H 0.5988 0.9069 0.1853 0.044 Uiso 1 1 calc R . . C55 C 0.4210(4) 0.8589(3) 0.2332(3) 0.0236(9) Uani 1 1 d . . . C56 C 0.5072(4) 0.7673(4) 0.2314(3) 0.0319(11) Uani 1 1 d . . . H56 H 0.5595 0.7464 0.2721 0.038 Uiso 1 1 calc R . . C57 C 0.5165(5) 0.7066(4) 0.1700(4) 0.0390(13) Uani 1 1 d . . . H57 H 0.5764 0.6449 0.1673 0.047 Uiso 1 1 calc R . . C58 C 0.4390(5) 0.7352(4) 0.1128(4) 0.0399(13) Uani 1 1 d . . . H58 H 0.4449 0.6921 0.0720 0.048 Uiso 1 1 calc R . . C59 C 0.3529(5) 0.8262(5) 0.1143(3) 0.0384(13) Uani 1 1 d . . . H59 H 0.2998 0.8455 0.0747 0.046 Uiso 1 1 calc R . . C60 C 0.3443(4) 0.8889(4) 0.1734(3) 0.0327(11) Uani 1 1 d . . . H60 H 0.2863 0.9524 0.1733 0.039 Uiso 1 1 calc R . . N1 N 0.2977(3) 1.0183(3) 0.3321(3) 0.0255(8) Uani 1 1 d . . . P1 P 0.19478(9) 1.01544(9) 0.39151(8) 0.0222(2) Uani 1 1 d . . . P2 P 0.41243(9) 0.94305(9) 0.30665(8) 0.0218(2) Uani 1 1 d . . . S1 S 0.81838(14) 0.75172(13) 0.33105(12) 0.0553(4) Uani 1 1 d . . . S2 S 0.62076(9) 0.53866(9) 0.39061(7) 0.0261(2) Uani 1 1 d . . . S3 S 0.62037(9) 0.43655(9) 0.60969(7) 0.0248(2) Uani 1 1 d . . . S4 S 0.84232(9) 0.57550(10) 0.52392(8) 0.0295(3) Uani 1 1 d . . . S5 S 0.72027(12) 0.46064(15) 0.78500(10) 0.0521(4) Uani 1 1 d . . . Au1 Au 0.5000 0.5000 0.5000 0.02041(8) Uani 1 2 d S . . C13 C 0.3302(5) 0.2390(6) 0.0378(4) 0.0530(16) Uani 1 1 d . . . H13 H 0.4040 0.2121 0.0280 0.064 Uiso 1 1 calc R . . C14 C 0.2719(6) 0.3367(6) 0.0441(5) 0.0637(19) Uani 1 1 d . . . H14 H 0.3021 0.3845 0.0400 0.076 Uiso 1 1 calc R . . C15 C 0.1573(4) 0.3667(5) 0.0577(4) 0.0384(13) Uani 1 1 d . . . H15 H 0.1048 0.4322 0.0634 0.046 Uiso 1 1 calc R . . C16 C 0.1434(4) 0.2714(4) 0.0605(3) 0.0335(11) Uani 1 1 d . . . C17 C 0.0437(4) 0.2638(4) 0.0692(3) 0.0284(10) Uani 1 1 d . . . C18 C 0.0180(4) 0.1915(4) 0.0501(3) 0.0272(10) Uani 1 1 d . . . C19 C -0.0923(4) 0.2155(4) 0.0630(3) 0.0269(10) Uani 1 1 d . . . C20 C -0.1481(4) 0.3061(4) 0.0923(3) 0.0278(10) Uani 1 1 d . . . C21 C -0.2602(4) 0.3566(4) 0.1141(3) 0.0287(10) Uani 1 1 d . . . C22 C -0.3472(3) 0.3610(3) 0.0604(3) 0.0200(9) Uani 1 1 d U . . H22 H -0.3407 0.3357 0.0062 0.024 Uiso 1 1 calc R . . C23 C -0.4421(5) 0.4149(5) 0.1161(4) 0.0480(15) Uani 1 1 d . . . H23 H -0.5092 0.4267 0.1018 0.058 Uiso 1 1 calc R . . C24 C -0.4291(4) 0.4467(4) 0.1883(4) 0.0413(13) Uani 1 1 d . . . H24 H -0.4858 0.4817 0.2281 0.050 Uiso 1 1 calc R . . S6 S 0.25976(12) 0.16871(13) 0.04904(11) 0.0494(4) Uani 1 1 d . . . S7 S -0.06718(10) 0.36408(10) 0.10348(9) 0.0331(3) Uani 1 1 d . . . S8 S 0.10727(9) 0.07797(10) 0.01333(9) 0.0305(3) Uani 1 1 d . . . S9 S -0.14652(9) 0.13613(9) 0.04159(9) 0.0288(3) Uani 1 1 d . . . S10 S -0.30442(14) 0.41955(13) 0.20253(12) 0.0537(4) Uani 1 1 d . . . Au2 Au 0.0000 0.0000 0.0000 0.02258(8) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.036(4) 0.070(5) 0.067(5) 0.031(4) 0.002(3) -0.020(3) C2 0.033(3) 0.111(7) 0.031(3) 0.004(4) -0.001(2) -0.023(4) C3 0.017(2) 0.048(3) 0.019(2) -0.004(2) 0.0023(16) -0.017(2) C4 0.023(2) 0.039(3) 0.031(3) -0.003(2) 0.0024(19) -0.011(2) C5 0.022(2) 0.029(2) 0.025(2) -0.0087(19) -0.0011(18) -0.0074(19) C6 0.023(2) 0.024(2) 0.019(2) -0.0070(18) -0.0006(17) -0.0047(18) C7 0.019(2) 0.025(2) 0.021(2) -0.0070(18) 0.0024(16) -0.0083(18) C8 0.019(2) 0.028(2) 0.022(2) -0.0053(19) -0.0013(17) -0.0047(18) C9 0.025(2) 0.028(3) 0.026(2) -0.009(2) -0.0035(18) -0.0067(19) C10 0.030(3) 0.031(3) 0.020(2) 0.0004(19) -0.0069(18) -0.016(2) C11 0.032(3) 0.063(4) 0.042(3) -0.017(3) -0.020(3) -0.002(3) C12 0.064(4) 0.073(5) 0.024(3) 0.002(3) -0.013(3) -0.026(4) C25 0.026(2) 0.030(3) 0.021(2) -0.0029(19) 0.0004(17) -0.0134(19) C26 0.029(3) 0.030(3) 0.037(3) -0.006(2) 0.001(2) -0.017(2) C27 0.041(3) 0.037(3) 0.039(3) -0.012(2) 0.003(2) -0.023(2) C28 0.049(3) 0.052(4) 0.033(3) -0.013(3) 0.001(2) -0.034(3) C29 0.038(3) 0.063(4) 0.028(3) -0.011(3) -0.006(2) -0.023(3) C30 0.033(3) 0.041(3) 0.022(2) -0.008(2) -0.0025(19) -0.016(2) C31 0.021(2) 0.027(2) 0.027(2) -0.0034(19) -0.0039(17) -0.0084(18) C32 0.038(3) 0.029(3) 0.024(2) -0.003(2) -0.002(2) -0.008(2) C33 0.051(3) 0.025(3) 0.032(3) -0.002(2) -0.012(2) -0.007(2) C34 0.035(3) 0.024(3) 0.049(3) -0.013(2) -0.010(2) -0.002(2) C35 0.031(3) 0.038(3) 0.044(3) -0.018(3) 0.005(2) -0.012(2) C36 0.029(3) 0.033(3) 0.032(3) -0.011(2) 0.004(2) -0.014(2) C37 0.022(2) 0.027(2) 0.022(2) -0.0007(18) -0.0013(17) -0.0088(19) C38 0.030(3) 0.041(3) 0.033(3) 0.004(2) -0.008(2) -0.021(2) C39 0.042(3) 0.044(3) 0.036(3) 0.011(2) -0.013(2) -0.025(3) C40 0.046(3) 0.049(3) 0.026(3) 0.010(2) -0.011(2) -0.028(3) C41 0.049(3) 0.044(3) 0.035(3) 0.003(2) -0.017(2) -0.025(3) C42 0.041(3) 0.033(3) 0.034(3) 0.000(2) -0.009(2) -0.022(2) C43 0.020(2) 0.028(2) 0.022(2) -0.0100(18) 0.0021(16) -0.0082(18) C44 0.029(3) 0.026(3) 0.036(3) -0.008(2) -0.007(2) -0.008(2) C45 0.037(3) 0.023(2) 0.030(3) -0.008(2) -0.007(2) -0.006(2) C46 0.034(3) 0.042(3) 0.020(2) -0.009(2) -0.0026(19) -0.012(2) C47 0.044(3) 0.087(5) 0.029(3) 0.001(3) -0.011(2) -0.046(3) C48 0.046(3) 0.055(4) 0.027(3) -0.004(2) -0.002(2) -0.033(3) C49 0.022(2) 0.036(3) 0.022(2) -0.0050(19) -0.0021(17) -0.014(2) C50 0.028(2) 0.032(3) 0.023(2) -0.004(2) 0.0034(18) -0.016(2) C51 0.040(3) 0.035(3) 0.029(3) -0.002(2) 0.001(2) -0.019(2) C52 0.035(3) 0.053(3) 0.023(2) 0.002(2) -0.001(2) -0.026(3) C53 0.028(3) 0.057(4) 0.035(3) -0.014(3) 0.010(2) -0.021(3) C54 0.029(3) 0.037(3) 0.043(3) -0.013(2) 0.006(2) -0.013(2) C55 0.030(2) 0.025(2) 0.019(2) -0.0024(18) -0.0030(17) -0.0141(19) C56 0.038(3) 0.032(3) 0.026(2) -0.006(2) -0.008(2) -0.011(2) C57 0.050(3) 0.028(3) 0.035(3) -0.009(2) -0.009(2) -0.009(2) C58 0.058(4) 0.046(3) 0.028(3) -0.014(2) -0.002(2) -0.028(3) C59 0.047(3) 0.053(4) 0.024(3) -0.003(2) -0.011(2) -0.027(3) C60 0.032(3) 0.038(3) 0.028(3) -0.003(2) -0.006(2) -0.015(2) N1 0.021(2) 0.024(2) 0.029(2) -0.0012(16) 0.0012(15) -0.0090(16) P1 0.0202(6) 0.0229(6) 0.0227(6) -0.0020(5) -0.0012(4) -0.0090(5) P2 0.0202(6) 0.0233(6) 0.0223(6) -0.0046(5) -0.0013(4) -0.0088(5) S1 0.0545(10) 0.0504(10) 0.0569(10) -0.0022(8) 0.0099(8) -0.0263(8) S2 0.0275(6) 0.0345(6) 0.0172(5) -0.0058(5) -0.0011(4) -0.0130(5) S3 0.0248(6) 0.0301(6) 0.0200(5) -0.0005(5) -0.0056(4) -0.0121(5) S4 0.0252(6) 0.0396(7) 0.0271(6) -0.0066(5) -0.0020(4) -0.0159(5) S5 0.0396(8) 0.0902(13) 0.0254(7) -0.0046(7) -0.0047(6) -0.0269(8) Au1 0.02143(14) 0.02283(14) 0.01742(13) -0.00477(9) -0.00310(9) -0.00806(10) C13 0.048(4) 0.073(5) 0.052(4) -0.010(3) -0.012(3) -0.036(3) C14 0.066(5) 0.075(5) 0.074(5) -0.017(4) -0.005(4) -0.051(4) C15 0.040(3) 0.050(3) 0.044(3) -0.013(3) 0.000(2) -0.035(3) C16 0.040(3) 0.042(3) 0.026(3) -0.004(2) -0.007(2) -0.024(2) C17 0.034(3) 0.030(3) 0.024(2) -0.005(2) -0.0047(19) -0.015(2) C18 0.027(2) 0.033(3) 0.021(2) -0.006(2) -0.0024(18) -0.011(2) C19 0.032(3) 0.029(3) 0.021(2) -0.0013(19) -0.0054(18) -0.013(2) C20 0.032(3) 0.028(3) 0.023(2) -0.0042(19) -0.0064(18) -0.010(2) C21 0.032(3) 0.028(3) 0.025(2) -0.003(2) -0.0078(19) -0.010(2) C22 0.0191(12) 0.0181(12) 0.0234(12) -0.0077(9) 0.0037(8) -0.0080(9) C23 0.045(4) 0.050(4) 0.056(4) -0.011(3) 0.000(3) -0.026(3) C24 0.039(3) 0.033(3) 0.044(3) -0.011(2) 0.010(2) -0.010(2) S6 0.0409(8) 0.0619(10) 0.0490(9) 0.0015(7) -0.0101(6) -0.0275(7) S7 0.0377(7) 0.0330(7) 0.0338(7) -0.0104(5) -0.0073(5) -0.0149(5) S8 0.0242(6) 0.0337(7) 0.0375(7) -0.0117(5) 0.0024(5) -0.0144(5) S9 0.0220(6) 0.0301(6) 0.0364(7) -0.0124(5) -0.0009(5) -0.0096(5) S10 0.0546(10) 0.0479(9) 0.0488(9) -0.0143(7) 0.0038(7) -0.0111(8) Au2 0.02164(14) 0.02553(14) 0.02092(13) -0.00558(10) 0.00083(9) -0.00998(10) _geom_special_details ; ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.321(11) . ? C1 S1 1.689(8) . ? C1 H1 0.950 . ? C2 C3 1.384(9) . ? C2 H2 0.950 . ? C3 C4 1.424(7) . ? C3 H3 0.950 . ? C4 C5 1.456(7) . ? C4 S1 1.717(6) . ? C5 C6 1.376(7) . ? C5 S4 1.732(5) . ? C6 C7 1.434(6) . ? C6 S2 1.749(5) . ? C7 C8 1.378(6) . ? C7 S3 1.765(4) . ? C8 C9 1.451(6) . ? C8 S4 1.738(5) . ? C9 C10 1.456(6) . ? C9 S5 1.705(5) . ? C10 C11 1.414(7) . ? C10 H10 0.950 . ? C11 C12 1.322(9) . ? C11 H11 0.950 . ? C12 S5 1.695(6) . ? C12 H12 0.950 . ? C25 C26 1.403(7) . ? C25 C30 1.402(7) . ? C25 P1 1.795(5) . ? C26 C27 1.384(7) . ? C26 H26 0.950 . ? C27 C28 1.370(8) . ? C27 H27 0.950 . ? C28 C29 1.375(8) . ? C28 H28 0.950 . ? C29 C30 1.405(7) . ? C29 H29 0.950 . ? C30 H30 0.950 . ? C31 C32 1.395(7) . ? C31 C36 1.396(7) . ? C31 P1 1.798(5) . ? C32 C33 1.385(7) . ? C32 H32 0.950 . ? C33 C34 1.388(8) . ? C33 H33 0.950 . ? C34 C35 1.382(8) . ? C34 H34 0.950 . ? C35 C36 1.382(7) . ? C35 H35 0.950 . ? C36 H36 0.950 . ? C37 C38 1.373(7) . ? C37 C42 1.394(7) . ? C37 P1 1.801(5) . ? C38 C39 1.402(7) . ? C38 H38 0.950 . ? C39 C40 1.384(8) . ? C39 H39 0.950 . ? C40 C41 1.383(8) . ? C40 H40 0.950 . ? C41 C42 1.386(7) . ? C41 H41 0.950 . ? C42 H42 0.950 . ? C43 C48 1.384(7) . ? C43 C44 1.388(7) . ? C43 P2 1.803(5) . ? C44 C45 1.388(7) . ? C44 H44 0.950 . ? C45 C46 1.369(7) . ? C45 H45 0.950 . ? C46 C47 1.384(8) . ? C46 H46 0.950 . ? C47 C48 1.381(8) . ? C47 H47 0.950 . ? C48 H48 0.950 . ? C49 C50 1.380(7) . ? C49 C54 1.399(7) . ? C49 P2 1.800(5) . ? C50 C51 1.395(7) . ? C50 H50 0.950 . ? C51 C52 1.375(7) . ? C51 H51 0.950 . ? C52 C53 1.369(8) . ? C52 H52 0.950 . ? C53 C54 1.388(8) . ? C53 H53 0.950 . ? C54 H54 0.950 . ? C55 C56 1.390(7) . ? C55 C60 1.394(7) . ? C55 P2 1.797(5) . ? C56 C57 1.382(7) . ? C56 H56 0.950 . ? C57 C58 1.379(8) . ? C57 H57 0.950 . ? C58 C59 1.383(8) . ? C58 H58 0.950 . ? C59 C60 1.382(7) . ? C59 H59 0.950 . ? C60 H60 0.950 . ? N1 P2 1.580(4) . ? N1 P1 1.589(4) . ? S2 Au1 2.3200(11) . ? S3 Au1 2.3332(11) . ? Au1 S2 2.3200(11) 2_666 ? Au1 S3 2.3332(11) 2_666 ? C13 C14 1.337(10) . ? C13 S6 1.679(6) . ? C13 H13 0.950 . ? C14 C15 1.488(9) . ? C14 H14 0.950 . ? C15 C16 1.481(7) . ? C15 H15 0.950 . ? C16 C17 1.449(7) . ? C16 S6 1.723(6) . ? C17 C18 1.359(7) . ? C17 S7 1.744(5) . ? C18 C19 1.444(7) . ? C18 S8 1.762(5) . ? C19 C20 1.364(7) . ? C19 S9 1.751(5) . ? C20 C21 1.463(7) . ? C20 S7 1.740(5) . ? C21 C22 1.562(6) . ? C21 S10 1.681(5) . ? C22 C23 1.474(7) . ? C22 H22 0.950 . ? C23 C24 1.346(9) . ? C23 H23 0.950 . ? C24 S10 1.687(6) . ? C24 H24 0.950 . ? S8 Au2 2.3127(12) . ? S9 Au2 2.3156(12) . ? Au2 S8 2.3127(12) 2 ? Au2 S9 2.3156(12) 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 C2 C1 S1 111.9(5) . . ? C2 C1 H1 124.0 . . ? S1 C1 H1 124.0 . . ? C1 C2 C3 115.3(6) . . ? C1 C2 H2 122.4 . . ? C3 C2 H2 122.3 . . ? C2 C3 C4 111.0(6) . . ? C2 C3 H3 124.5 . . ? C4 C3 H3 124.5 . . ? C3 C4 C5 129.2(5) . . ? C3 C4 S1 109.1(4) . . ? C5 C4 S1 121.7(4) . . ? C6 C5 C4 128.3(4) . . ? C6 C5 S4 111.6(3) . . ? C4 C5 S4 120.1(4) . . ? C5 C6 C7 112.4(4) . . ? C5 C6 S2 125.2(4) . . ? C7 C6 S2 122.4(3) . . ? C8 C7 C6 113.0(4) . . ? C8 C7 S3 125.7(3) . . ? C6 C7 S3 121.3(3) . . ? C7 C8 C9 131.0(4) . . ? C7 C8 S4 110.9(3) . . ? C9 C8 S4 118.1(4) . . ? C8 C9 C10 126.4(4) . . ? C8 C9 S5 123.0(4) . . ? C10 C9 S5 110.7(3) . . ? C11 C10 C9 108.8(4) . . ? C11 C10 H10 125.6 . . ? C9 C10 H10 125.6 . . ? C12 C11 C10 115.0(5) . . ? C12 C11 H11 122.5 . . ? C10 C11 H11 122.5 . . ? C11 C12 S5 113.2(5) . . ? C11 C12 H12 123.4 . . ? S5 C12 H12 123.4 . . ? C26 C25 C30 118.8(4) . . ? C26 C25 P1 120.5(4) . . ? C30 C25 P1 120.5(4) . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C26 120.5(5) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.3(5) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 120.6(5) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C25 C30 C29 119.3(5) . . ? C25 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C32 C31 C36 120.0(4) . . ? C32 C31 P1 118.4(4) . . ? C36 C31 P1 121.6(4) . . ? C33 C32 C31 120.0(5) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 119.8(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 120.3(5) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C36 C35 C34 120.5(5) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C35 C36 C31 119.5(5) . . ? C35 C36 H36 120.3 . . ? C31 C36 H36 120.3 . . ? C38 C37 C42 119.1(4) . . ? C38 C37 P1 123.3(4) . . ? C42 C37 P1 117.5(4) . . ? C37 C38 C39 121.1(5) . . ? C37 C38 H38 119.5 . . ? C39 C38 H38 119.5 . . ? C40 C39 C38 119.3(5) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? C41 C40 C39 119.9(5) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.5(5) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 120.2(5) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C48 C43 C44 118.8(4) . . ? C48 C43 P2 121.5(4) . . ? C44 C43 P2 119.2(4) . . ? C45 C44 C43 120.9(5) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C46 C45 C44 119.5(5) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C47 120.4(5) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C48 120.0(5) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C47 C48 C43 120.4(5) . . ? C47 C48 H48 119.8 . . ? C43 C48 H48 119.8 . . ? C50 C49 C54 119.5(4) . . ? C50 C49 P2 120.5(4) . . ? C54 C49 P2 120.0(4) . . ? C49 C50 C51 120.2(5) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C52 C51 C50 119.7(5) . . ? C52 C51 H51 120.1 . . ? C50 C51 H51 120.1 . . ? C53 C52 C51 120.7(5) . . ? C53 C52 H52 119.6 . . ? C51 C52 H52 119.6 . . ? C52 C53 C54 120.2(5) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C53 C54 C49 119.7(5) . . ? C53 C54 H54 120.1 . . ? C49 C54 H54 120.1 . . ? C56 C55 C60 119.8(4) . . ? C56 C55 P2 120.2(4) . . ? C60 C55 P2 119.8(4) . . ? C57 C56 C55 119.7(5) . . ? C57 C56 H56 120.1 . . ? C55 C56 H56 120.1 . . ? C58 C57 C56 120.2(5) . . ? C58 C57 H57 119.9 . . ? C56 C57 H57 119.9 . . ? C57 C58 C59 120.4(5) . . ? C57 C58 H58 119.8 . . ? C59 C58 H58 119.8 . . ? C60 C59 C58 119.8(5) . . ? C60 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C59 C60 C55 119.9(5) . . ? C59 C60 H60 120.0 . . ? C55 C60 H60 120.0 . . ? P2 N1 P1 139.7(3) . . ? N1 P1 C25 112.3(2) . . ? N1 P1 C31 105.8(2) . . ? C25 P1 C31 109.1(2) . . ? N1 P1 C37 113.6(2) . . ? C25 P1 C37 108.3(2) . . ? C31 P1 C37 107.6(2) . . ? N1 P2 C55 114.1(2) . . ? N1 P2 C49 107.2(2) . . ? C55 P2 C49 106.3(2) . . ? N1 P2 C43 113.0(2) . . ? C55 P2 C43 107.5(2) . . ? C49 P2 C43 108.4(2) . . ? C1 S1 C4 92.7(4) . . ? C6 S2 Au1 100.17(15) . . ? C7 S3 Au1 100.14(15) . . ? C5 S4 C8 92.1(2) . . ? C12 S5 C9 92.2(3) . . ? S2 Au1 S2 180.0 . 2_666 ? S2 Au1 S3 90.09(4) . 2_666 ? S2 Au1 S3 89.91(4) 2_666 2_666 ? S2 Au1 S3 89.91(4) . . ? S2 Au1 S3 90.09(4) 2_666 . ? S3 Au1 S3 180.0 2_666 . ? C14 C13 S6 113.0(5) . . ? C14 C13 H13 123.5 . . ? S6 C13 H13 123.5 . . ? C13 C14 C15 116.6(6) . . ? C13 C14 H14 121.7 . . ? C15 C14 H14 121.7 . . ? C16 C15 C14 104.6(5) . . ? C16 C15 H15 127.7 . . ? C14 C15 H15 127.7 . . ? C17 C16 C15 124.8(5) . . ? C17 C16 S6 122.6(4) . . ? C15 C16 S6 112.7(4) . . ? C18 C17 C16 130.7(5) . . ? C18 C17 S7 110.7(4) . . ? C16 C17 S7 118.5(4) . . ? C17 C18 C19 113.5(4) . . ? C17 C18 S8 125.0(4) . . ? C19 C18 S8 121.6(4) . . ? C20 C19 C18 112.6(4) . . ? C20 C19 S9 124.6(4) . . ? C18 C19 S9 122.8(4) . . ? C19 C20 C21 129.5(5) . . ? C19 C20 S7 111.1(4) . . ? C21 C20 S7 119.4(4) . . ? C20 C21 C22 126.1(4) . . ? C20 C21 S10 119.4(4) . . ? C22 C21 S10 114.5(3) . . ? C23 C22 C21 101.6(4) . . ? C23 C22 H22 129.2 . . ? C21 C22 H22 129.2 . . ? C24 C23 C22 116.9(5) . . ? C24 C23 H23 121.6 . . ? C22 C23 H23 121.6 . . ? C23 C24 S10 114.8(5) . . ? C23 C24 H24 122.6 . . ? S10 C24 H24 122.6 . . ? C13 S6 C16 93.1(3) . . ? C20 S7 C17 92.1(2) . . ? C18 S8 Au2 102.22(17) . . ? C19 S9 Au2 101.93(17) . . ? C21 S10 C24 91.9(3) . . ? S8 Au2 S8 180.0 2 . ? S8 Au2 S9 88.54(4) 2 . ? S8 Au2 S9 91.46(4) . . ? S8 Au2 S9 91.46(4) 2 2 ? S8 Au2 S9 88.54(4) . 2 ? S9 Au2 S9 180.0 . 2 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 2.210 _refine_diff_density_min -2.549 _refine_diff_density_rms 0.152 #===END data_12 _database_code_depnum_ccdc_archive 'CCDC 675708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 C16 H36 N +, C28 H20 S10 Ni 2-' _chemical_formula_sum 'C60 H92 N2 Ni S10' _chemical_formula_weight 1220.67 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7090(7) _cell_length_b 21.2066(16) _cell_length_c 17.7517(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.521(2) _cell_angle_gamma 90.00 _cell_volume 3187.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6070 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 23.81 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 0.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6868 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX2 CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5 _diffrn_reflns_number 22238 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 23.81 _reflns_number_total 5371 _reflns_number_gt 4828 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; ; _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^)+(0.0394P)^2^+1.8924P] 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 5371 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0805 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Ni Ni 0.5000 0.5000 0.5000 0.02672(10) Uani 1 2 d S . . S1 S 0.61106(6) 0.59247(2) 0.52162(3) 0.03285(12) Uani 1 1 d . . . S2 S 0.60020(5) 0.46885(2) 0.61930(3) 0.03037(12) Uani 1 1 d . . . S3 S 0.87519(6) 0.61386(2) 0.75648(3) 0.03707(13) Uani 1 1 d . . . S4 S 0.73950(7) 0.73186(3) 0.54977(3) 0.04532(15) Uani 1 1 d . . . S5 S 0.70719(6) 0.42402(2) 0.79582(3) 0.03661(13) Uani 1 1 d . . . C1 C 0.8270(4) 0.85082(12) 0.50629(17) 0.0688(8) Uani 1 1 d . . . H1A H 0.8874 0.8883 0.5279 0.103 Uiso 1 1 calc R . . H1B H 0.7143 0.8612 0.4919 0.103 Uiso 1 1 calc R . . H1C H 0.8612 0.8367 0.4603 0.103 Uiso 1 1 calc R . . C2 C 0.8546(3) 0.79928(10) 0.56563(14) 0.0508(6) Uani 1 1 d . . . C3 C 0.9663(3) 0.79449(11) 0.63225(14) 0.0513(6) Uani 1 1 d . . . H3 H 1.0409 0.8269 0.6508 0.062 Uiso 1 1 calc R . . C4 C 0.9625(3) 0.73718(10) 0.67185(14) 0.0450(5) Uani 1 1 d . . . H4 H 1.0346 0.7271 0.7193 0.054 Uiso 1 1 calc R . . C5 C 0.8444(2) 0.69747(10) 0.63515(12) 0.0374(5) Uani 1 1 d . . . C6 C 0.8024(2) 0.63646(9) 0.66003(11) 0.0336(4) Uani 1 1 d . . . C7 C 0.7101(2) 0.58981(9) 0.61889(11) 0.0305(4) Uani 1 1 d . . . C8 C 0.7001(2) 0.53497(9) 0.66410(11) 0.0289(4) Uani 1 1 d . . . C9 C 0.7793(2) 0.54095(9) 0.74050(11) 0.0312(4) Uani 1 1 d . . . C10 C 0.7863(2) 0.49969(9) 0.80574(11) 0.0335(4) Uani 1 1 d . . . C11 C 0.8454(2) 0.51280(11) 0.88290(12) 0.0410(5) Uani 1 1 d . . . H11 H 0.8963 0.5514 0.9011 0.049 Uiso 1 1 calc R . . C12 C 0.8230(3) 0.46319(12) 0.93273(12) 0.0465(5) Uani 1 1 d . . . H12 H 0.8572 0.4656 0.9875 0.056 Uiso 1 1 calc R . . C13 C 0.7489(3) 0.41233(11) 0.89547(12) 0.0438(5) Uani 1 1 d . . . C14 C 0.6993(3) 0.35273(13) 0.92837(14) 0.0583(6) Uani 1 1 d . . . H14A H 0.7498 0.3503 0.9838 0.087 Uiso 1 1 calc R . . H14B H 0.7315 0.3164 0.9016 0.087 Uiso 1 1 calc R . . H14C H 0.5843 0.3525 0.9213 0.087 Uiso 1 1 calc R . . N N 0.1652(2) 0.40573(9) 0.68450(11) 0.0427(4) Uani 1 1 d . . . C15 C 0.1679(2) 0.43219(11) 0.76388(13) 0.0465(5) Uani 1 1 d . . . H15A H 0.1778 0.3967 0.8009 0.056 Uiso 1 1 calc R . . H15B H 0.0652 0.4530 0.7619 0.056 Uiso 1 1 calc R . . C16 C 0.2983(3) 0.47903(12) 0.79503(15) 0.0520(6) Uani 1 1 d . . . H16A H 0.4015 0.4597 0.7945 0.062 Uiso 1 1 calc R . . H16B H 0.2845 0.5165 0.7609 0.062 Uiso 1 1 calc R . . C17 C 0.2983(3) 0.49912(15) 0.87588(15) 0.0640(7) Uani 1 1 d . . . H17A H 0.3199 0.4620 0.9105 0.077 Uiso 1 1 calc R . . H17B H 0.1921 0.5152 0.8769 0.077 Uiso 1 1 calc R . . C18 C 0.4193(3) 0.54957(14) 0.90630(17) 0.0663(7) Uani 1 1 d . . . H18A H 0.4145 0.5609 0.9592 0.099 Uiso 1 1 calc R . . H18B H 0.3970 0.5869 0.8730 0.099 Uiso 1 1 calc R . . H18C H 0.5250 0.5336 0.9064 0.099 Uiso 1 1 calc R . . C19 C 0.1756(2) 0.45804(10) 0.62735(13) 0.0428(5) Uani 1 1 d . . . H19A H 0.2817 0.4774 0.6431 0.051 Uiso 1 1 calc R . . H19B H 0.1667 0.4388 0.5757 0.051 Uiso 1 1 calc R . . C20 C 0.0533(3) 0.51007(11) 0.61938(14) 0.0499(6) Uani 1 1 d . . . H20A H 0.0395 0.5222 0.6712 0.060 Uiso 1 1 calc R . . H20B H -0.0495 0.4948 0.5883 0.060 Uiso 1 1 calc R . . C21 C 0.1074(3) 0.56723(12) 0.57984(16) 0.0608(7) Uani 1 1 d . . . H21A H 0.1416 0.5528 0.5333 0.073 Uiso 1 1 calc R . . H21B H 0.0164 0.5960 0.5623 0.073 Uiso 1 1 calc R . . C22 C 0.2417(4) 0.60377(13) 0.63147(18) 0.0703(8) Uani 1 1 d . . . H22A H 0.2702 0.6396 0.6026 0.106 Uiso 1 1 calc R . . H22B H 0.3334 0.5760 0.6480 0.106 Uiso 1 1 calc R . . H22C H 0.2081 0.6193 0.6771 0.106 Uiso 1 1 calc R . . C23 C 0.0116(2) 0.36835(12) 0.65845(14) 0.0500(6) Uani 1 1 d . . . H23A H -0.0014 0.3413 0.7020 0.060 Uiso 1 1 calc R . . H23B H -0.0776 0.3985 0.6475 0.060 Uiso 1 1 calc R . . C24 C 0.0002(3) 0.32708(12) 0.58786(15) 0.0542(6) Uani 1 1 d . . . H24A H 0.0719 0.2906 0.6021 0.065 Uiso 1 1 calc R . . H24B H 0.0359 0.3514 0.5475 0.065 Uiso 1 1 calc R . . C25 C -0.1680(3) 0.30296(14) 0.55429(17) 0.0673(7) Uani 1 1 d . . . H25A H -0.2410 0.3394 0.5440 0.081 Uiso 1 1 calc R . . H25B H -0.1713 0.2818 0.5042 0.081 Uiso 1 1 calc R . . C26 C -0.2242(4) 0.25812(18) 0.60635(19) 0.0912(11) Uani 1 1 d . . . H26A H -0.3323 0.2449 0.5822 0.137 Uiso 1 1 calc R . . H26B H -0.2223 0.2788 0.6559 0.137 Uiso 1 1 calc R . . H26C H -0.1549 0.2211 0.6153 0.137 Uiso 1 1 calc R . . C27 C 0.3077(3) 0.36404(11) 0.68637(15) 0.0490(6) Uani 1 1 d . . . H27A H 0.3008 0.3481 0.6333 0.059 Uiso 1 1 calc R . . H27B H 0.4037 0.3906 0.7007 0.059 Uiso 1 1 calc R . . C28 C 0.3288(3) 0.30809(13) 0.7410(2) 0.0676(8) Uani 1 1 d . A . H28A H 0.2314 0.2823 0.7302 0.081 Uiso 1 1 calc R . . H28B H 0.3491 0.3230 0.7952 0.081 Uiso 1 1 calc R . . C29 C 0.4673(3) 0.26846(14) 0.7296(3) 0.1005(13) Uani 1 1 d . . . H29A H 0.4466 0.2591 0.6735 0.121 Uiso 0.557(6) 1 calc PR A 1 H29B H 0.5610 0.2963 0.7416 0.121 Uiso 0.557(6) 1 calc PR A 1 H29C H 0.5459 0.2969 0.7152 0.121 Uiso 0.443(6) 1 calc PR A 2 H29D H 0.5181 0.2488 0.7798 0.121 Uiso 0.443(6) 1 calc PR A 2 C30 C 0.5120(6) 0.2137(2) 0.7665(3) 0.0678(18) Uani 0.557(6) 1 d P A 1 H30A H 0.6038 0.1969 0.7501 0.102 Uiso 0.557(6) 1 calc PR A 1 H30B H 0.4249 0.1833 0.7536 0.102 Uiso 0.557(6) 1 calc PR A 1 H30C H 0.5398 0.2209 0.8225 0.102 Uiso 0.557(6) 1 calc PR A 1 C30A C 0.4331(9) 0.2243(3) 0.6777(5) 0.081(2) Uani 0.443(6) 1 d P A 2 H30D H 0.5297 0.2017 0.6748 0.121 Uiso 0.443(6) 1 calc PR A 2 H30E H 0.3858 0.2431 0.6272 0.121 Uiso 0.443(6) 1 calc PR A 2 H30F H 0.3581 0.1948 0.6920 0.121 Uiso 0.443(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.02618(17) 0.02898(18) 0.02583(17) -0.00231(13) 0.00774(13) -0.00390(13) S1 0.0377(3) 0.0318(3) 0.0289(2) -0.00174(19) 0.00756(19) -0.0072(2) S2 0.0304(2) 0.0316(2) 0.0289(2) -0.00116(18) 0.00662(18) -0.00479(18) S3 0.0369(3) 0.0399(3) 0.0331(3) -0.0094(2) 0.0057(2) -0.0046(2) S4 0.0567(3) 0.0340(3) 0.0455(3) -0.0012(2) 0.0124(3) -0.0107(2) S5 0.0356(3) 0.0417(3) 0.0326(3) 0.0029(2) 0.0081(2) 0.0037(2) C1 0.097(2) 0.0420(14) 0.0713(18) 0.0017(13) 0.0269(16) -0.0171(14) C2 0.0686(16) 0.0318(11) 0.0591(15) -0.0060(10) 0.0291(13) -0.0122(11) C3 0.0576(14) 0.0402(12) 0.0613(15) -0.0171(11) 0.0245(12) -0.0181(11) C4 0.0451(12) 0.0412(12) 0.0501(13) -0.0123(10) 0.0138(10) -0.0085(10) C5 0.0389(11) 0.0358(11) 0.0406(11) -0.0109(9) 0.0155(9) -0.0061(9) C6 0.0334(10) 0.0337(10) 0.0346(10) -0.0074(8) 0.0097(8) -0.0019(8) C7 0.0283(9) 0.0347(10) 0.0304(10) -0.0059(8) 0.0104(8) -0.0010(8) C8 0.0245(9) 0.0328(10) 0.0308(9) -0.0052(8) 0.0091(7) -0.0002(7) C9 0.0259(9) 0.0358(10) 0.0326(10) -0.0057(8) 0.0086(7) 0.0002(8) C10 0.0253(9) 0.0425(11) 0.0330(10) -0.0031(8) 0.0072(8) 0.0046(8) C11 0.0347(11) 0.0532(13) 0.0334(11) -0.0042(9) 0.0047(9) 0.0044(9) C12 0.0436(12) 0.0654(15) 0.0294(11) 0.0038(10) 0.0062(9) 0.0111(11) C13 0.0404(11) 0.0565(14) 0.0353(11) 0.0078(10) 0.0103(9) 0.0111(10) C14 0.0629(16) 0.0662(16) 0.0473(13) 0.0158(12) 0.0159(12) 0.0057(13) N 0.0328(9) 0.0468(10) 0.0531(11) 0.0031(8) 0.0194(8) 0.0034(8) C15 0.0338(11) 0.0572(14) 0.0523(13) 0.0075(11) 0.0179(10) 0.0090(10) C16 0.0438(12) 0.0576(14) 0.0605(15) -0.0047(12) 0.0242(11) 0.0060(11) C17 0.0483(14) 0.092(2) 0.0517(15) -0.0022(14) 0.0110(12) 0.0003(13) C18 0.0601(16) 0.0762(19) 0.0637(16) -0.0133(14) 0.0165(13) 0.0093(14) C19 0.0401(11) 0.0440(12) 0.0504(13) 0.0022(10) 0.0229(10) 0.0016(9) C20 0.0486(13) 0.0544(14) 0.0523(14) 0.0049(11) 0.0233(11) 0.0100(11) C21 0.0742(17) 0.0519(15) 0.0651(16) 0.0100(12) 0.0342(14) 0.0162(13) C22 0.093(2) 0.0467(14) 0.085(2) 0.0044(14) 0.0480(18) 0.0043(14) C23 0.0312(11) 0.0576(14) 0.0644(15) 0.0148(12) 0.0179(10) -0.0003(10) C24 0.0522(14) 0.0465(13) 0.0651(16) 0.0004(12) 0.0162(12) -0.0049(11) C25 0.0599(16) 0.0723(18) 0.0677(17) -0.0035(14) 0.0110(13) -0.0054(14) C26 0.075(2) 0.122(3) 0.081(2) -0.023(2) 0.0287(17) -0.046(2) C27 0.0351(11) 0.0439(12) 0.0735(16) -0.0009(11) 0.0239(11) 0.0029(9) C28 0.0397(13) 0.0535(15) 0.111(2) 0.0164(15) 0.0196(14) 0.0082(11) C29 0.0453(16) 0.0499(17) 0.200(4) -0.015(2) 0.016(2) 0.0106(13) C30 0.049(3) 0.056(3) 0.101(4) 0.025(3) 0.021(3) 0.010(2) C30A 0.083(5) 0.065(5) 0.097(6) -0.010(4) 0.026(4) -0.001(4) _geom_special_details ; ; 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 Ni S1 2.1806(5) . ? Ni S1 2.1806(5) 3_666 ? Ni S2 2.1952(5) . ? Ni S2 2.1952(5) 3_666 ? S1 C7 1.7413(19) . ? S2 C8 1.7411(18) . ? S3 C6 1.748(2) . ? S3 C9 1.7488(19) . ? S4 C2 1.731(2) . ? S4 C5 1.737(2) . ? S5 C10 1.739(2) . ? S5 C13 1.738(2) . ? C1 C2 1.498(3) . ? C2 C3 1.348(4) . ? C3 C4 1.408(3) . ? C4 C5 1.370(3) . ? C5 C6 1.442(3) . ? C6 C7 1.373(3) . ? C7 C8 1.427(3) . ? C8 C9 1.376(3) . ? C9 C10 1.441(3) . ? C10 C11 1.374(3) . ? C11 C12 1.417(3) . ? C12 C13 1.348(3) . ? C13 C14 1.498(3) . ? N C15 1.512(3) . ? N C19 1.520(3) . ? N C23 1.531(3) . ? N C27 1.518(3) . ? C15 C16 1.513(3) . ? C16 C17 1.497(3) . ? C17 C18 1.511(4) . ? C19 C20 1.517(3) . ? C20 C21 1.529(3) . ? C21 C22 1.519(4) . ? C23 C24 1.513(3) . ? C24 C25 1.534(4) . ? C25 C26 1.486(4) . ? C27 C28 1.516(4) . ? C28 C29 1.522(4) . ? C29 C30 1.346(6) . ? C29 C30A 1.298(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Ni S1 180.0 . 3_666 ? S1 Ni S2 92.343(17) . . ? S1 Ni S2 87.657(17) 3_666 . ? S1 Ni S2 92.343(17) 3_666 3_666 ? S1 Ni S2 87.657(17) . 3_666 ? S2 Ni S2 180.0 . 3_666 ? Ni S1 C7 103.99(7) . . ? Ni S2 C8 103.99(7) . . ? C6 S3 C9 91.92(9) . . ? C2 S4 C5 92.20(11) . . ? C10 S5 C13 92.57(10) . . ? S4 C2 C1 119.8(2) . . ? S4 C2 C3 110.61(18) . . ? C1 C2 C3 129.5(2) . . ? C2 C3 C4 114.0(2) . . ? C3 C4 C5 113.3(2) . . ? S4 C5 C4 109.89(17) . . ? S4 C5 C6 121.65(15) . . ? C4 C5 C6 128.4(2) . . ? S3 C6 C5 119.09(14) . . ? S3 C6 C7 110.90(15) . . ? C5 C6 C7 130.01(19) . . ? S1 C7 C6 126.65(16) . . ? S1 C7 C8 120.18(14) . . ? C6 C7 C8 113.17(17) . . ? S2 C8 C7 119.28(14) . . ? S2 C8 C9 127.30(15) . . ? C7 C8 C9 113.37(17) . . ? S3 C9 C8 110.59(14) . . ? S3 C9 C10 118.52(14) . . ? C8 C9 C10 130.79(18) . . ? S5 C10 C9 122.51(14) . . ? S5 C10 C11 109.57(16) . . ? C9 C10 C11 127.85(19) . . ? C10 C11 C12 113.4(2) . . ? C11 C12 C13 114.05(19) . . ? S5 C13 C12 110.33(17) . . ? S5 C13 C14 120.43(18) . . ? C12 C13 C14 129.2(2) . . ? C15 N C19 111.15(17) . . ? C15 N C23 107.20(16) . . ? C15 N C27 111.20(17) . . ? C19 N C23 111.13(17) . . ? C19 N C27 105.28(15) . . ? C23 N C27 110.94(17) . . ? N C15 C16 115.53(17) . . ? C15 C16 C17 111.6(2) . . ? C16 C17 C18 112.8(2) . . ? N C19 C20 116.29(17) . . ? C19 C20 C21 109.56(19) . . ? C20 C21 C22 113.8(2) . . ? N C23 C24 115.68(18) . . ? C23 C24 C25 112.7(2) . . ? C24 C25 C26 113.3(2) . . ? N C27 C28 116.51(19) . . ? C27 C28 C29 109.2(3) . . ? C28 C29 C30 124.1(4) . . ? C28 C29 C30A 115.8(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ni S1 C7 -1.11(6) . . . . ? S2 Ni S1 C7 178.89(6) 3_666 . . . ? S1 Ni S2 C8 3.03(6) . . . . ? S1 Ni S2 C8 -176.97(6) 3_666 . . . ? C5 S4 C2 C1 177.2(2) . . . . ? C5 S4 C2 C3 0.38(19) . . . . ? S4 C2 C3 C4 0.0(3) . . . . ? C1 C2 C3 C4 -176.4(2) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C3 C4 C5 S4 0.8(2) . . . . ? C3 C4 C5 C6 -177.7(2) . . . . ? C2 S4 C5 C4 -0.70(17) . . . . ? C2 S4 C5 C6 177.95(17) . . . . ? S4 C5 C6 S3 -162.92(11) . . . . ? S4 C5 C6 C7 17.4(3) . . . . ? C4 C5 C6 S3 15.5(3) . . . . ? C4 C5 C6 C7 -164.2(2) . . . . ? C9 S3 C6 C5 -179.84(16) . . . . ? C9 S3 C6 C7 -0.09(15) . . . . ? S3 C6 C7 S1 178.83(11) . . . . ? S3 C6 C7 C8 -1.4(2) . . . . ? C5 C6 C7 S1 -1.5(3) . . . . ? C5 C6 C7 C8 178.34(18) . . . . ? Ni S1 C7 C6 178.07(16) . . . . ? Ni S1 C7 C8 -1.73(16) . . . . ? S1 C7 C8 S2 4.7(2) . . . . ? S1 C7 C8 C9 -177.55(13) . . . . ? C6 C7 C8 S2 -175.10(13) . . . . ? C6 C7 C8 C9 2.6(2) . . . . ? Ni S2 C8 C7 -4.99(15) . . . . ? Ni S2 C8 C9 177.63(15) . . . . ? S2 C8 C9 S3 174.89(11) . . . . ? S2 C8 C9 C10 -8.9(3) . . . . ? C7 C8 C9 S3 -2.6(2) . . . . ? C7 C8 C9 C10 173.58(18) . . . . ? C6 S3 C9 C8 1.56(14) . . . . ? C6 S3 C9 C10 -175.16(15) . . . . ? S3 C9 C10 S5 -175.44(10) . . . . ? S3 C9 C10 C11 8.0(3) . . . . ? C8 C9 C10 S5 8.6(3) . . . . ? C8 C9 C10 C11 -168.0(2) . . . . ? C13 S5 C10 C9 -175.25(16) . . . . ? C13 S5 C10 C11 1.87(15) . . . . ? S5 C10 C11 C12 -1.6(2) . . . . ? C9 C10 C11 C12 175.32(19) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? C11 C12 C13 S5 1.1(2) . . . . ? C11 C12 C13 C14 -177.2(2) . . . . ? C10 S5 C13 C12 -1.70(17) . . . . ? C10 S5 C13 C14 176.78(19) . . . . ? C19 N C15 C16 -49.4(2) . . . . ? C23 N C15 C16 -171.05(19) . . . . ? C27 N C15 C16 67.5(2) . . . . ? N C15 C16 C17 -176.0(2) . . . . ? C15 C16 C17 C18 -175.7(2) . . . . ? C15 N C19 C20 -54.5(2) . . . . ? C23 N C19 C20 64.8(2) . . . . ? C27 N C19 C20 -175.0(2) . . . . ? N C19 C20 C21 163.3(2) . . . . ? C19 C20 C21 C22 -73.5(3) . . . . ? C15 N C23 C24 -168.13(19) . . . . ? C19 N C23 C24 70.2(2) . . . . ? C27 N C23 C24 -46.5(3) . . . . ? N C23 C24 C25 -167.1(2) . . . . ? C23 C24 C25 C26 -67.1(3) . . . . ? C15 N C27 C28 58.2(3) . . . . ? C19 N C27 C28 178.7(2) . . . . ? C23 N C27 C28 -61.0(3) . . . . ? N C27 C28 C29 174.6(2) . . . . ? C27 C28 C29 C30 -176.4(4) . . . . ? C27 C28 C29 C30A -89.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.81 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.694 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.041 # Attachment '16 new.cif' data_16 _database_code_depnum_ccdc_archive 'CCDC 675709' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H58 Au N O4 P2 S6' _chemical_formula_weight 1452.46 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.101(3) _cell_length_b 15.888(4) _cell_length_c 19.945(5) _cell_angle_alpha 105.418(4) _cell_angle_beta 100.449(4) _cell_angle_gamma 99.858(4) _cell_volume 3244.5(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4513 _cell_measurement_theta_min 2.177 _cell_measurement_theta_max 23.18 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 2.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.713576 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _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 'CCD area Detector' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14816 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0852 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 23.30 _reflns_number_total 9255 _reflns_number_gt 6391 _reflns_threshold_expression >2sigma(I) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.500 0.000 106.0 38.7 _platon_squeeze_details ; ? ; _computing_data_collection 'DENZO & COLLECT' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'WinGX v1.10.01' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0576P)^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 9255 _refine_ls_number_parameters 785 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1068 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.009 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 0.5000 0.0000 0.5000 0.03146(15) Uani 1 2 d S . . Au2 Au 0.5000 0.5000 0.0000 0.02946(14) Uani 1 2 d S . . S1 S 0.3425(2) 0.03830(16) 0.42984(11) 0.0394(6) Uani 1 1 d . . . S2 S 0.39813(19) 0.02703(15) 0.59158(11) 0.0357(5) Uani 1 1 d . . . S3 S 0.37070(18) -0.02981(13) 0.21140(11) 0.0301(5) Uani 1 1 d . . . S4 S 0.61367(18) 0.39044(14) -0.00172(11) 0.0339(5) Uani 1 1 d . . . S5 S 0.39752(19) 0.45768(14) 0.08076(11) 0.0340(5) Uani 1 1 d . . . S6 S 0.4631(2) 0.20740(14) 0.10133(12) 0.0396(5) Uani 1 1 d . . . P1 P 0.74886(18) 0.39416(13) 0.55353(11) 0.0266(5) Uani 1 1 d . . . P2 P 0.96719(18) 0.35234(13) 0.64181(11) 0.0266(5) Uani 1 1 d . . . O1 O 0.1498(5) 0.2313(4) 0.8396(3) 0.0575(18) Uani 1 1 d . . . O2 O -0.1715(5) 0.0965(3) 0.2302(3) 0.0326(13) Uani 1 1 d . . . O3 O 0.0014(5) 0.2881(4) 0.2572(3) 0.0388(14) Uani 1 1 d . . . O4 O 0.9391(12) 0.0704(9) -0.0270(8) 0.038(4) Uani 0.50 1 d P . . O4' O 0.8793(13) 0.0289(9) -0.0363(8) 0.033(3) Uani 0.50 1 d P . . N1 N 0.8861(5) 0.3873(4) 0.5864(3) 0.0284(15) Uani 1 1 d . . . C1 C 0.5128(7) 0.0223(5) 0.6645(4) 0.031(2) Uani 1 1 d . . . C2 C 0.3781(7) 0.0082(5) 0.3457(4) 0.0297(19) Uani 1 1 d . . . C3 C 0.3041(7) 0.0086(5) 0.2830(4) 0.0248(18) Uani 1 1 d . . . C4 C 0.1797(7) 0.0331(5) 0.2679(4) 0.0252(18) Uani 1 1 d . . . C5 C 0.1304(7) 0.0784(5) 0.3226(4) 0.0319(19) Uani 1 1 d . . . H5 H 0.1780 0.0957 0.3708 0.038 Uiso 1 1 calc R . . C6 C 0.0141(7) 0.0987(5) 0.3088(4) 0.0290(19) Uani 1 1 d . . . H6 H -0.0178 0.1293 0.3470 0.035 Uiso 1 1 calc R . . C7 C -0.0561(7) 0.0739(5) 0.2383(4) 0.0306(19) Uani 1 1 d . . . C8 C -0.2494(7) 0.0672(6) 0.1597(4) 0.041(2) Uani 1 1 d . . . H8A H -0.2665 0.0017 0.1409 0.061 Uiso 1 1 calc R . . H8B H -0.2066 0.0939 0.1288 0.061 Uiso 1 1 calc R . . H8C H -0.3290 0.0858 0.1606 0.061 Uiso 1 1 calc R . . C9 C -0.0094(8) 0.0300(6) 0.1839(4) 0.046(2) Uani 1 1 d . . . H9 H -0.0561 0.0136 0.1357 0.055 Uiso 1 1 calc R . . C10 C 0.1069(8) 0.0095(6) 0.1997(5) 0.048(2) Uani 1 1 d . . . H10 H 0.1374 -0.0223 0.1613 0.058 Uiso 1 1 calc R . . C11 C 0.5038(7) 0.0497(5) 0.7335(4) 0.0290(18) Uani 1 1 d . . . C12 C 0.4116(7) 0.0947(5) 0.7645(4) 0.0285(18) Uani 1 1 d . . . C13 C 0.2852(7) 0.0734(5) 0.7276(4) 0.0296(18) Uani 1 1 d . . . H13 H 0.2567 0.0265 0.6833 0.036 Uiso 1 1 calc R . . C14 C 0.2011(7) 0.1198(5) 0.7547(4) 0.032(2) Uani 1 1 d . . . H14 H 0.1158 0.1047 0.7285 0.039 Uiso 1 1 calc R . . C15 C 0.2388(7) 0.1868(6) 0.8182(5) 0.042(2) Uani 1 1 d . . . C16 C 0.1865(10) 0.3033(8) 0.9047(6) 0.086(4) Uani 1 1 d . . . H16A H 0.2074 0.2800 0.9450 0.129 Uiso 1 1 calc R . . H16B H 0.1170 0.3332 0.9101 0.129 Uiso 1 1 calc R . . H16C H 0.2603 0.3464 0.9038 0.129 Uiso 1 1 calc R . . C17 C 0.3627(9) 0.2087(6) 0.8576(5) 0.051(3) Uani 1 1 d . . . H17 H 0.3891 0.2545 0.9025 0.062 Uiso 1 1 calc R . . C18 C 0.4482(7) 0.1622(5) 0.8301(4) 0.036(2) Uani 1 1 d . . . H18 H 0.5331 0.1770 0.8568 0.043 Uiso 1 1 calc R . . C19 C 0.5367(7) 0.3266(5) 0.0445(4) 0.0315(19) Uani 1 1 d . . . C20 C 0.5583(7) 0.2475(5) 0.0513(4) 0.0327(19) Uani 1 1 d . . . C21 C 0.6463(12) 0.1961(8) 0.0242(5) 0.074(2) Uani 1 1 d . . . C22 C 0.7696(9) 0.2395(7) 0.0281(5) 0.056(3) Uani 1 1 d . A . H22 H 0.7946 0.3032 0.0445 0.067 Uiso 1 1 calc R . . C23 C 0.8560(11) 0.1887(8) 0.0077(5) 0.074(2) Uani 1 1 d . . . H23 H 0.9399 0.2171 0.0101 0.088 Uiso 1 1 calc R A . C24 C 0.8158(12) 0.0965(8) -0.0159(5) 0.074(2) Uani 1 1 d . A . C25 C 0.8398(15) -0.0666(10) -0.0606(9) 0.035(4) Uani 0.50 1 d P A 1 H25A H 0.8101 -0.0876 -0.0232 0.052 Uiso 0.50 1 calc PR A 1 H25B H 0.9109 -0.0923 -0.0713 0.052 Uiso 0.50 1 calc PR A 1 H25C H 0.7714 -0.0855 -0.1039 0.052 Uiso 0.50 1 calc PR A 1 C25' C 1.0695(14) 0.1211(11) -0.0079(10) 0.049(5) Uani 0.50 1 d P B 2 H25D H 1.0794 0.1600 -0.0382 0.074 Uiso 0.50 1 calc PR B 2 H25E H 1.1250 0.0794 -0.0151 0.074 Uiso 0.50 1 calc PR B 2 H25F H 1.0917 0.1579 0.0425 0.074 Uiso 0.50 1 calc PR B 2 C26 C 0.6973(12) 0.0528(8) -0.0230(5) 0.074(2) Uani 1 1 d . . . H26 H 0.6719 -0.0108 -0.0415 0.088 Uiso 1 1 calc R A . C27 C 0.6145(11) 0.1035(6) -0.0026(4) 0.059(3) Uani 1 1 d . A . H27 H 0.5304 0.0734 -0.0071 0.071 Uiso 1 1 calc R . . C28 C 0.4396(6) 0.3559(5) 0.0793(4) 0.0266(18) Uani 1 1 d . . . C29 C 0.3906(7) 0.2966(5) 0.1120(4) 0.0291(18) Uani 1 1 d . . . C30 C 0.2919(7) 0.3008(5) 0.1522(4) 0.0264(18) Uani 1 1 d . . . C31 C 0.1893(7) 0.3344(6) 0.1327(5) 0.040(2) Uani 1 1 d . . . H31 H 0.1854 0.3597 0.0945 0.048 Uiso 1 1 calc R . . C32 C 0.0921(7) 0.3326(6) 0.1669(4) 0.041(2) Uani 1 1 d . . . H32 H 0.0229 0.3568 0.1524 0.049 Uiso 1 1 calc R . . C33 C 0.0951(7) 0.2963(5) 0.2212(4) 0.034(2) Uani 1 1 d . . . C34 C -0.1130(7) 0.3117(6) 0.2287(5) 0.046(2) Uani 1 1 d . . . H34A H -0.0959 0.3762 0.2351 0.068 Uiso 1 1 calc R . . H34B H -0.1771 0.2962 0.2542 0.068 Uiso 1 1 calc R . . H34C H -0.1437 0.2784 0.1776 0.068 Uiso 1 1 calc R . . C35 C 0.1975(8) 0.2635(5) 0.2440(4) 0.040(2) Uani 1 1 d . . . H35 H 0.2015 0.2401 0.2832 0.047 Uiso 1 1 calc R . . C36 C 0.2936(8) 0.2652(5) 0.2089(4) 0.036(2) Uani 1 1 d . . . H36 H 0.3630 0.2414 0.2238 0.044 Uiso 1 1 calc R . . C37 C 0.7601(7) 0.5026(5) 0.5417(4) 0.0279(18) Uani 1 1 d . . . C38 C 0.8627(7) 0.5733(5) 0.5849(4) 0.0320(19) Uani 1 1 d . . . H38 H 0.9252 0.5627 0.6190 0.038 Uiso 1 1 calc R . . C39 C 0.8717(8) 0.6581(5) 0.5773(5) 0.039(2) Uani 1 1 d . . . H39 H 0.9396 0.7059 0.6073 0.046 Uiso 1 1 calc R . . C40 C 0.7830(7) 0.6741(6) 0.5267(4) 0.035(2) Uani 1 1 d . . . H40 H 0.7913 0.7322 0.5211 0.042 Uiso 1 1 calc R . . C41 C 0.6820(8) 0.6050(5) 0.4842(4) 0.033(2) Uani 1 1 d . . . H41 H 0.6209 0.6161 0.4496 0.040 Uiso 1 1 calc R . . C42 C 0.6693(7) 0.5207(5) 0.4915(4) 0.0270(18) Uani 1 1 d . . . H42 H 0.5989 0.4742 0.4626 0.032 Uiso 1 1 calc R . . C43 C 0.6843(7) 0.3144(5) 0.4670(4) 0.0281(18) Uani 1 1 d . . . C44 C 0.7639(8) 0.2815(5) 0.4248(4) 0.033(2) Uani 1 1 d . . . H44 H 0.8525 0.3007 0.4433 0.040 Uiso 1 1 calc R . . C45 C 0.7170(9) 0.2227(5) 0.3579(5) 0.038(2) Uani 1 1 d . . . H45 H 0.7728 0.2012 0.3302 0.045 Uiso 1 1 calc R . . C46 C 0.5881(9) 0.1938(5) 0.3300(5) 0.044(2) Uani 1 1 d . . . H46 H 0.5554 0.1519 0.2834 0.053 Uiso 1 1 calc R . . C47 C 0.5075(8) 0.2260(5) 0.3700(4) 0.037(2) Uani 1 1 d . . . H47 H 0.4192 0.2083 0.3500 0.045 Uiso 1 1 calc R . . C48 C 0.5535(8) 0.2832(5) 0.4382(4) 0.038(2) Uani 1 1 d . . . H48 H 0.4969 0.3020 0.4663 0.045 Uiso 1 1 calc R . . C49 C 0.6418(7) 0.3818(5) 0.6094(4) 0.0288(19) Uani 1 1 d . . . C50 C 0.5877(7) 0.2967(5) 0.6115(4) 0.036(2) Uani 1 1 d . . . H50 H 0.5983 0.2447 0.5784 0.043 Uiso 1 1 calc R . . C51 C 0.5187(7) 0.2876(6) 0.6615(5) 0.044(2) Uani 1 1 d . . . H51 H 0.4821 0.2297 0.6630 0.053 Uiso 1 1 calc R . . C52 C 0.5037(8) 0.3630(7) 0.7090(5) 0.047(2) Uani 1 1 d . . . H52 H 0.4572 0.3568 0.7437 0.057 Uiso 1 1 calc R . . C53 C 0.5545(8) 0.4469(6) 0.7073(5) 0.042(2) Uani 1 1 d . . . H53 H 0.5429 0.4984 0.7405 0.051 Uiso 1 1 calc R . . C54 C 0.6231(7) 0.4568(5) 0.6571(4) 0.035(2) Uani 1 1 d . . . H54 H 0.6572 0.5150 0.6553 0.043 Uiso 1 1 calc R . . C55 C 1.1118(6) 0.4362(5) 0.6874(4) 0.0250(18) Uani 1 1 d . . . C56 C 1.1659(7) 0.4884(5) 0.6488(4) 0.0309(19) Uani 1 1 d . . . H56 H 1.1271 0.4798 0.6002 0.037 Uiso 1 1 calc R . . C57 C 1.2765(7) 0.5525(5) 0.6830(5) 0.034(2) Uani 1 1 d . . . H57 H 1.3151 0.5875 0.6575 0.041 Uiso 1 1 calc R . . C58 C 1.3308(7) 0.5659(5) 0.7534(5) 0.036(2) Uani 1 1 d . . . H58 H 1.4060 0.6109 0.7768 0.043 Uiso 1 1 calc R . . C59 C 1.2762(8) 0.5139(6) 0.7908(5) 0.043(2) Uani 1 1 d . . . H59 H 1.3142 0.5236 0.8397 0.051 Uiso 1 1 calc R . . C60 C 1.1677(7) 0.4486(5) 0.7577(4) 0.0304(19) Uani 1 1 d . . . H60 H 1.1316 0.4123 0.7832 0.036 Uiso 1 1 calc R . . C61 C 1.0105(7) 0.2527(5) 0.5951(4) 0.0252(18) Uani 1 1 d . . . C62 C 0.9241(7) 0.1896(5) 0.5380(4) 0.0320(19) Uani 1 1 d . . . H62 H 0.8398 0.1956 0.5265 0.038 Uiso 1 1 calc R . . C63 C 0.9603(7) 0.1172(5) 0.4974(4) 0.0309(19) Uani 1 1 d . . . H63 H 0.9009 0.0740 0.4576 0.037 Uiso 1 1 calc R . . C64 C 1.0825(8) 0.1077(5) 0.5148(5) 0.035(2) Uani 1 1 d . . . H64 H 1.1073 0.0585 0.4863 0.042 Uiso 1 1 calc R . . C65 C 1.1669(8) 0.1683(5) 0.5722(5) 0.036(2) Uani 1 1 d . . . H65 H 1.2499 0.1601 0.5846 0.043 Uiso 1 1 calc R . . C66 C 1.1343(7) 0.2414(5) 0.6130(4) 0.0309(19) Uani 1 1 d . . . H66 H 1.1946 0.2839 0.6528 0.037 Uiso 1 1 calc R . . C67 C 0.8947(7) 0.3286(5) 0.7102(4) 0.0292(19) Uani 1 1 d . . . C68 C 0.8577(7) 0.3989(6) 0.7551(4) 0.041(2) Uani 1 1 d . . . H68 H 0.8718 0.4568 0.7491 0.049 Uiso 1 1 calc R . . C69 C 0.8008(8) 0.3833(7) 0.8082(5) 0.049(2) Uani 1 1 d . . . H69 H 0.7728 0.4300 0.8375 0.059 Uiso 1 1 calc R . . C70 C 0.7844(9) 0.3003(8) 0.8187(5) 0.061(3) Uani 1 1 d . . . H70 H 0.7473 0.2903 0.8561 0.074 Uiso 1 1 calc R . . C71 C 0.8219(10) 0.2312(7) 0.7749(6) 0.067(3) Uani 1 1 d . . . H71 H 0.8095 0.1736 0.7816 0.080 Uiso 1 1 calc R . . C72 C 0.8779(8) 0.2469(6) 0.7211(5) 0.049(2) Uani 1 1 d . . . H72 H 0.9048 0.1999 0.6915 0.058 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 0.0269(3) 0.0427(3) 0.0341(3) 0.0188(2) 0.0094(2) 0.0191(2) Au2 0.0175(3) 0.0306(3) 0.0438(3) 0.0141(2) 0.0117(2) 0.0059(2) S1 0.0366(13) 0.0597(15) 0.0352(13) 0.0234(11) 0.0105(10) 0.0292(12) S2 0.0270(12) 0.0547(15) 0.0369(13) 0.0231(11) 0.0090(10) 0.0242(11) S3 0.0218(11) 0.0334(12) 0.0359(12) 0.0118(10) 0.0056(9) 0.0077(9) S4 0.0193(11) 0.0326(12) 0.0554(14) 0.0172(11) 0.0148(10) 0.0083(9) S5 0.0293(12) 0.0304(12) 0.0551(14) 0.0220(10) 0.0222(11) 0.0141(10) S6 0.0490(14) 0.0303(13) 0.0430(14) 0.0127(11) 0.0117(11) 0.0150(11) P1 0.0152(10) 0.0244(12) 0.0380(13) 0.0072(10) 0.0027(9) 0.0066(9) P2 0.0150(10) 0.0255(12) 0.0400(13) 0.0104(10) 0.0051(9) 0.0078(9) O1 0.026(3) 0.055(4) 0.074(5) -0.009(4) 0.008(3) 0.015(3) O2 0.021(3) 0.040(3) 0.037(3) 0.013(3) 0.002(3) 0.012(3) O3 0.036(3) 0.042(3) 0.050(4) 0.025(3) 0.020(3) 0.012(3) O4 0.027(9) 0.030(9) 0.058(9) 0.011(8) 0.013(8) 0.011(6) O4' 0.029(9) 0.026(9) 0.045(8) 0.004(7) 0.016(7) 0.009(6) N1 0.016(3) 0.024(4) 0.043(4) 0.011(3) 0.005(3) 0.002(3) C1 0.021(4) 0.044(5) 0.045(5) 0.030(4) 0.008(4) 0.020(4) C2 0.028(5) 0.028(5) 0.036(5) 0.015(4) 0.005(4) 0.006(4) C3 0.015(4) 0.024(5) 0.037(5) 0.008(4) 0.011(4) 0.007(3) C4 0.016(4) 0.031(5) 0.030(5) 0.012(4) 0.004(4) 0.005(4) C5 0.036(5) 0.026(5) 0.032(5) 0.009(4) -0.002(4) 0.014(4) C6 0.030(5) 0.024(4) 0.035(5) 0.011(4) 0.008(4) 0.009(4) C7 0.024(4) 0.029(5) 0.042(5) 0.015(4) 0.006(4) 0.009(4) C8 0.021(5) 0.059(6) 0.041(5) 0.015(5) -0.001(4) 0.015(4) C9 0.035(5) 0.071(7) 0.028(5) 0.008(5) 0.001(4) 0.026(5) C10 0.044(6) 0.071(7) 0.034(6) 0.007(5) 0.016(5) 0.034(5) C11 0.022(4) 0.032(5) 0.032(5) 0.010(4) 0.004(4) 0.005(4) C12 0.019(4) 0.031(5) 0.033(5) 0.011(4) 0.004(4) 0.001(4) C13 0.023(4) 0.025(4) 0.037(5) 0.008(4) 0.005(4) 0.000(4) C14 0.013(4) 0.039(5) 0.043(5) 0.012(4) 0.004(4) 0.006(4) C15 0.021(5) 0.045(6) 0.057(6) 0.006(5) 0.014(5) 0.010(4) C16 0.049(7) 0.103(10) 0.078(9) -0.025(7) 0.012(6) 0.032(7) C17 0.042(6) 0.054(6) 0.048(6) -0.005(5) 0.007(5) 0.020(5) C18 0.015(4) 0.041(5) 0.045(6) 0.008(4) 0.000(4) 0.006(4) C19 0.014(4) 0.029(5) 0.043(5) 0.006(4) 0.003(4) -0.005(3) C20 0.028(5) 0.023(5) 0.043(5) 0.008(4) 0.000(4) 0.008(4) C21 0.108(5) 0.103(5) 0.038(3) 0.026(3) 0.022(3) 0.086(5) C22 0.045(6) 0.094(8) 0.054(6) 0.035(6) 0.024(5) 0.050(6) C23 0.108(5) 0.103(5) 0.038(3) 0.026(3) 0.022(3) 0.086(5) C24 0.108(5) 0.103(5) 0.038(3) 0.026(3) 0.022(3) 0.086(5) C25 0.037(10) 0.027(10) 0.051(11) 0.015(8) 0.021(9) 0.018(8) C25' 0.017(9) 0.042(11) 0.088(15) 0.014(10) 0.019(10) 0.007(8) C26 0.108(5) 0.103(5) 0.038(3) 0.026(3) 0.022(3) 0.086(5) C27 0.093(8) 0.059(7) 0.033(6) 0.013(5) -0.001(5) 0.050(6) C28 0.013(4) 0.029(5) 0.036(5) 0.013(4) 0.001(4) 0.000(3) C29 0.024(4) 0.031(5) 0.029(5) 0.007(4) 0.004(4) 0.006(4) C30 0.019(4) 0.019(4) 0.036(5) 0.011(4) 0.002(4) -0.006(3) C31 0.017(4) 0.055(6) 0.061(6) 0.042(5) 0.008(4) 0.003(4) C32 0.014(4) 0.059(6) 0.059(6) 0.038(5) 0.006(4) 0.002(4) C33 0.021(4) 0.034(5) 0.047(5) 0.014(4) 0.011(4) 0.002(4) C34 0.029(5) 0.052(6) 0.074(7) 0.033(5) 0.026(5) 0.019(4) C35 0.040(5) 0.048(6) 0.045(6) 0.027(5) 0.013(4) 0.021(5) C36 0.032(5) 0.036(5) 0.051(6) 0.023(4) 0.008(4) 0.017(4) C37 0.030(5) 0.030(5) 0.027(5) 0.006(4) 0.006(4) 0.020(4) C38 0.022(4) 0.021(5) 0.047(5) 0.006(4) 0.000(4) 0.005(4) C39 0.032(5) 0.026(5) 0.058(6) 0.013(4) 0.013(5) 0.004(4) C40 0.032(5) 0.039(5) 0.048(6) 0.022(4) 0.018(4) 0.018(4) C41 0.030(5) 0.035(5) 0.046(5) 0.023(4) 0.011(4) 0.020(4) C42 0.015(4) 0.034(5) 0.033(5) 0.011(4) 0.007(4) 0.006(4) C43 0.021(4) 0.024(4) 0.036(5) 0.007(4) 0.003(4) 0.005(4) C44 0.030(5) 0.034(5) 0.043(5) 0.017(4) 0.011(4) 0.018(4) C45 0.055(6) 0.024(5) 0.038(6) 0.009(4) 0.014(5) 0.017(5) C46 0.058(7) 0.025(5) 0.038(6) 0.004(4) 0.002(5) -0.002(5) C47 0.025(5) 0.032(5) 0.044(6) 0.009(4) -0.002(4) -0.004(4) C48 0.036(5) 0.040(5) 0.033(5) 0.009(4) 0.005(4) 0.006(4) C49 0.016(4) 0.038(5) 0.036(5) 0.014(4) 0.005(4) 0.013(4) C50 0.019(4) 0.036(5) 0.053(6) 0.013(4) 0.005(4) 0.011(4) C51 0.016(5) 0.048(6) 0.069(7) 0.028(5) 0.010(5) -0.007(4) C52 0.018(5) 0.072(7) 0.051(6) 0.014(5) 0.013(4) 0.013(5) C53 0.025(5) 0.055(6) 0.048(6) 0.009(5) 0.012(4) 0.016(5) C54 0.023(5) 0.036(5) 0.046(5) 0.011(4) 0.004(4) 0.010(4) C55 0.014(4) 0.020(4) 0.036(5) 0.002(4) 0.003(4) 0.005(3) C56 0.014(4) 0.032(5) 0.047(5) 0.009(4) 0.010(4) 0.008(4) C57 0.014(4) 0.026(5) 0.061(6) 0.009(4) 0.013(4) 0.006(4) C58 0.010(4) 0.031(5) 0.055(6) -0.003(4) 0.003(4) 0.004(4) C59 0.028(5) 0.045(6) 0.048(6) 0.004(5) -0.002(5) 0.019(5) C60 0.022(4) 0.026(5) 0.038(5) 0.003(4) 0.003(4) 0.005(4) C61 0.022(4) 0.021(4) 0.036(5) 0.013(4) 0.007(4) 0.007(4) C62 0.021(4) 0.030(5) 0.047(5) 0.014(4) 0.004(4) 0.011(4) C63 0.035(5) 0.011(4) 0.048(5) 0.009(4) 0.015(4) 0.004(4) C64 0.039(5) 0.022(5) 0.053(6) 0.014(4) 0.026(5) 0.015(4) C65 0.026(5) 0.028(5) 0.065(6) 0.022(5) 0.019(5) 0.017(4) C66 0.019(4) 0.025(5) 0.046(5) 0.012(4) -0.001(4) 0.005(4) C67 0.018(4) 0.025(5) 0.044(5) 0.013(4) 0.007(4) 0.000(4) C68 0.021(5) 0.052(6) 0.048(6) 0.012(5) 0.007(4) 0.012(4) C69 0.036(5) 0.070(7) 0.053(6) 0.022(5) 0.019(5) 0.027(5) C70 0.044(6) 0.087(9) 0.071(7) 0.038(7) 0.035(6) 0.018(6) C71 0.084(8) 0.056(7) 0.084(8) 0.038(6) 0.048(7) 0.018(6) C72 0.049(6) 0.043(6) 0.057(6) 0.014(5) 0.020(5) 0.014(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 S2 2.302(2) 2_656 ? Au1 S2 2.302(2) . ? Au1 S1 2.3055(19) 2_656 ? Au1 S1 2.3055(19) . ? Au2 S5 2.3064(19) 2_665 ? Au2 S5 2.3064(19) . ? Au2 S4 2.3151(19) 2_665 ? Au2 S4 2.3151(19) . ? S1 C2 1.756(8) . ? S2 C1 1.777(7) . ? S3 C11 1.740(7) 2_656 ? S3 C3 1.742(7) . ? S4 C19 1.760(8) . ? S5 C28 1.753(7) . ? S6 C29 1.730(7) . ? S6 C20 1.734(8) . ? P1 N1 1.579(6) . ? P1 C43 1.782(8) . ? P1 C37 1.787(7) . ? P1 C49 1.792(7) . ? P2 N1 1.574(6) . ? P2 C67 1.794(7) . ? P2 C61 1.801(7) . ? P2 C55 1.809(7) . ? O1 C15 1.374(9) . ? O1 C16 1.421(11) . ? O2 C7 1.383(8) . ? O2 C8 1.419(8) . ? O3 C33 1.374(8) . ? O3 C34 1.445(9) . ? O4 C25' 1.458(19) . ? O4 C24 1.533(17) . ? O4' C24 1.395(16) . ? O4' C25 1.426(19) . ? C1 C11 1.356(10) . ? C1 C2 1.408(10) 2_656 ? C2 C3 1.367(10) . ? C2 C1 1.408(10) 2_656 ? C3 C4 1.499(10) . ? C4 C10 1.369(10) . ? C4 C5 1.393(10) . ? C5 C6 1.381(10) . ? C6 C7 1.393(10) . ? C7 C9 1.363(10) . ? C9 C10 1.386(11) . ? C11 C12 1.479(10) . ? C11 S3 1.740(7) 2_656 ? C12 C18 1.392(10) . ? C12 C13 1.399(10) . ? C13 C14 1.383(10) . ? C14 C15 1.361(11) . ? C15 C17 1.389(12) . ? C17 C18 1.400(11) . ? C19 C20 1.355(10) . ? C19 C28 1.461(10) . ? C20 C21 1.464(11) . ? C21 C27 1.382(14) . ? C21 C22 1.402(15) . ? C22 C23 1.403(12) . ? C23 C24 1.378(15) . ? C24 C26 1.342(16) . ? C26 C27 1.370(12) . ? C28 C29 1.373(10) . ? C29 C30 1.472(10) . ? C30 C31 1.375(10) . ? C30 C36 1.391(10) . ? C31 C32 1.377(10) . ? C32 C33 1.353(10) . ? C33 C35 1.383(10) . ? C35 C36 1.378(10) . ? C37 C42 1.409(10) . ? C37 C38 1.411(10) . ? C38 C39 1.383(10) . ? C39 C40 1.384(11) . ? C40 C41 1.386(11) . ? C41 C42 1.372(10) . ? C43 C44 1.399(10) . ? C43 C48 1.408(11) . ? C44 C45 1.358(11) . ? C45 C46 1.385(12) . ? C46 C47 1.378(11) . ? C47 C48 1.367(11) . ? C49 C54 1.386(10) . ? C49 C50 1.397(10) . ? C50 C51 1.386(11) . ? C51 C52 1.371(12) . ? C52 C53 1.368(12) . ? C53 C54 1.388(11) . ? C55 C60 1.374(10) . ? C55 C56 1.406(10) . ? C56 C57 1.382(10) . ? C57 C58 1.367(11) . ? C58 C59 1.388(11) . ? C59 C60 1.372(11) . ? C61 C62 1.374(10) . ? C61 C66 1.411(10) . ? C62 C63 1.386(10) . ? C63 C64 1.382(10) . ? C64 C65 1.354(11) . ? C65 C66 1.375(10) . ? C67 C72 1.360(10) . ? C67 C68 1.406(11) . ? C68 C69 1.381(11) . ? C69 C70 1.377(12) . ? C70 C71 1.385(13) . ? C71 C72 1.390(12) . ? 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 S2 180.0 2_656 . ? S2 Au1 S1 89.08(7) 2_656 2_656 ? S2 Au1 S1 90.92(7) . 2_656 ? S2 Au1 S1 90.92(7) 2_656 . ? S2 Au1 S1 89.08(7) . . ? S1 Au1 S1 180.00(9) 2_656 . ? S5 Au2 S5 180.00(10) 2_665 . ? S5 Au2 S4 91.61(7) 2_665 2_665 ? S5 Au2 S4 88.39(7) . 2_665 ? S5 Au2 S4 88.39(7) 2_665 . ? S5 Au2 S4 91.61(7) . . ? S4 Au2 S4 180.0 2_665 . ? C2 S1 Au1 102.0(3) . . ? C1 S2 Au1 101.6(3) . . ? C11 S3 C3 92.1(4) 2_656 . ? C19 S4 Au2 101.6(3) . . ? C28 S5 Au2 101.3(2) . . ? C29 S6 C20 93.3(4) . . ? N1 P1 C43 111.6(3) . . ? N1 P1 C37 107.6(3) . . ? C43 P1 C37 106.5(3) . . ? N1 P1 C49 113.5(3) . . ? C43 P1 C49 109.1(4) . . ? C37 P1 C49 108.1(3) . . ? N1 P2 C67 115.7(3) . . ? N1 P2 C61 109.7(3) . . ? C67 P2 C61 108.5(3) . . ? N1 P2 C55 109.0(3) . . ? C67 P2 C55 106.5(4) . . ? C61 P2 C55 107.1(3) . . ? C15 O1 C16 118.5(7) . . ? C7 O2 C8 116.7(6) . . ? C33 O3 C34 116.0(6) . . ? C25' O4 C24 133.2(13) . . ? C24 O4' C25 132.7(13) . . ? P2 N1 P1 144.9(4) . . ? C11 C1 C2 115.2(7) . 2_656 ? C11 C1 S2 123.1(6) . . ? C2 C1 S2 121.7(6) 2_656 . ? C3 C2 C1 112.3(7) . 2_656 ? C3 C2 S1 125.2(6) . . ? C1 C2 S1 122.4(6) 2_656 . ? C2 C3 C4 130.9(7) . . ? C2 C3 S3 110.7(5) . . ? C4 C3 S3 118.4(6) . . ? C10 C4 C5 116.6(7) . . ? C10 C4 C3 121.5(7) . . ? C5 C4 C3 121.8(7) . . ? C6 C5 C4 121.8(7) . . ? C5 C6 C7 119.5(7) . . ? C9 C7 O2 125.2(7) . . ? C9 C7 C6 119.8(7) . . ? O2 C7 C6 115.0(7) . . ? C7 C9 C10 119.4(8) . . ? C4 C10 C9 123.0(7) . . ? C1 C11 C12 129.9(7) . . ? C1 C11 S3 109.6(5) . 2_656 ? C12 C11 S3 120.5(6) . 2_656 ? C18 C12 C13 117.5(7) . . ? C18 C12 C11 121.4(7) . . ? C13 C12 C11 121.1(7) . . ? C14 C13 C12 120.8(7) . . ? C15 C14 C13 121.0(7) . . ? C14 C15 O1 116.8(7) . . ? C14 C15 C17 120.2(7) . . ? O1 C15 C17 123.0(8) . . ? C15 C17 C18 119.0(8) . . ? C12 C18 C17 121.5(7) . . ? C20 C19 C28 113.5(7) . . ? C20 C19 S4 125.3(6) . . ? C28 C19 S4 121.2(6) . . ? C19 C20 C21 130.2(8) . . ? C19 C20 S6 110.4(6) . . ? C21 C20 S6 119.4(7) . . ? C27 C21 C22 117.3(9) . . ? C27 C21 C20 122.0(11) . . ? C22 C21 C20 120.6(10) . . ? C21 C22 C23 119.8(11) . . ? C22 C23 C24 118.2(12) . . ? C26 C24 O4' 104.7(12) . . ? C26 C24 C23 123.6(10) . . ? O4' C24 C23 131.7(13) . . ? C26 C24 O4 136.2(12) . . ? O4' C24 O4 31.6(6) . . ? C23 C24 O4 100.2(11) . . ? C24 C26 C27 117.3(12) . . ? C26 C27 C21 123.7(12) . . ? C29 C28 C19 112.2(6) . . ? C29 C28 S5 125.3(6) . . ? C19 C28 S5 122.5(5) . . ? C28 C29 C30 129.4(7) . . ? C28 C29 S6 110.5(6) . . ? C30 C29 S6 120.0(5) . . ? C31 C30 C36 116.7(7) . . ? C31 C30 C29 121.8(7) . . ? C36 C30 C29 121.4(7) . . ? C30 C31 C32 122.1(7) . . ? C33 C32 C31 120.0(7) . . ? C32 C33 O3 124.9(7) . . ? C32 C33 C35 120.1(7) . . ? O3 C33 C35 115.0(7) . . ? C36 C35 C33 119.1(7) . . ? C35 C36 C30 121.9(7) . . ? C42 C37 C38 118.6(7) . . ? C42 C37 P1 122.5(6) . . ? C38 C37 P1 118.9(5) . . ? C39 C38 C37 119.7(7) . . ? C38 C39 C40 120.9(8) . . ? C39 C40 C41 119.7(7) . . ? C42 C41 C40 120.6(7) . . ? C41 C42 C37 120.5(7) . . ? C44 C43 C48 117.7(7) . . ? C44 C43 P1 120.2(6) . . ? C48 C43 P1 122.1(6) . . ? C45 C44 C43 121.3(8) . . ? C44 C45 C46 120.2(8) . . ? C47 C46 C45 119.7(8) . . ? C48 C47 C46 120.5(8) . . ? C47 C48 C43 120.5(8) . . ? C54 C49 C50 119.1(7) . . ? C54 C49 P1 120.2(6) . . ? C50 C49 P1 120.3(6) . . ? C51 C50 C49 120.3(8) . . ? C52 C51 C50 119.4(8) . . ? C53 C52 C51 121.2(8) . . ? C52 C53 C54 119.9(8) . . ? C49 C54 C53 120.1(8) . . ? C60 C55 C56 120.7(7) . . ? C60 C55 P2 121.1(6) . . ? C56 C55 P2 118.2(6) . . ? C57 C56 C55 118.7(8) . . ? C58 C57 C56 120.5(8) . . ? C57 C58 C59 120.1(8) . . ? C60 C59 C58 120.6(8) . . ? C55 C60 C59 119.3(8) . . ? C62 C61 C66 119.4(7) . . ? C62 C61 P2 119.5(5) . . ? C66 C61 P2 121.0(6) . . ? C61 C62 C63 119.9(7) . . ? C64 C63 C62 120.2(8) . . ? C65 C64 C63 120.2(7) . . ? C64 C65 C66 121.0(7) . . ? C65 C66 C61 119.4(7) . . ? C72 C67 C68 119.5(7) . . ? C72 C67 P2 122.6(6) . . ? C68 C67 P2 117.9(6) . . ? C69 C68 C67 119.7(8) . . ? C70 C69 C68 120.2(9) . . ? C69 C70 C71 120.2(9) . . ? C70 C71 C72 119.4(9) . . ? C67 C72 C71 121.0(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.659 _refine_diff_density_min -1.364 _refine_diff_density_rms 0.123