Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Jorge Morgado' 'Isabel C. Santos' 'Luis F. Veiros' 'Cesar Rodrigues' 'Rui T. Henriques' 'M. Teresa Duarte' 'Luis Alcacera' 'Manuel Almeida' _publ_contact_author_name 'Prof M Almeida' _publ_contact_author_address ; Prof M Almeida Department Quimica Instituto Tecnologico e Nuclear Sacavem P-2686-953 PORTUGAL ; _publ_contact_author_email 'MALMEIDA@ITN.PT' _publ_section_title ; Preparation, structural, electrical and magnetic properties of tetrathiafulvalene-Au(pds)2 radical-cation salts (pds=pyrazine-2,3-diselenolate). ; data_(ttf)2[Au(pds)2]2 _database_code_CSD 159179 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H16 Au2 N8 S8 Se8' _chemical_formula_weight 1746.58 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' 'Se' 'Se' -0.0929 2.2259 '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 9.2248(15) _cell_length_b 14.095(2) _cell_length_c 17.050(2) _cell_angle_alpha 92.524(10) _cell_angle_beta 105.622(9) _cell_angle_gamma 101.51 _cell_volume 2080.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.65 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.788 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 14.477 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9278 _exptl_absorpt_correction_T_max 0.9991 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10351 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.1102 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 27.96 _reflns_number_total 10019 _reflns_number_gt 5041 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+65.5396P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00266(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10019 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1838 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2207 _refine_ls_wR_factor_gt 0.1506 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.36235(9) 0.91778(6) 0.30273(5) 0.0325(2) Uani 1 d . . . Se1 Se 0.1954(3) 0.87422(16) 0.38931(14) 0.0417(5) Uani 1 d . . . Se2 Se 0.4509(3) 1.08248(15) 0.36988(14) 0.0397(5) Uani 1 d . . . Se3 Se 0.2844(3) 0.75217(16) 0.23570(15) 0.0463(6) Uani 1 d . . . Se4 Se 0.5293(3) 0.96664(17) 0.21734(15) 0.0470(6) Uani 1 d . . . C1 C 0.246(2) 0.9870(13) 0.4606(12) 0.033(4) Uani 1 d . . . N1 N 0.173(2) 0.9927(15) 0.5201(11) 0.045(4) Uani 1 d . . . C3 C 0.206(3) 1.071(2) 0.5677(14) 0.061(7) Uani 1 d . . . H3 H 0.1620 1.0731 0.6106 0.073 Uiso 1 calc R . . C2 C 0.348(2) 1.0781(15) 0.4498(13) 0.038(5) Uani 1 d . . . N2 N 0.378(2) 1.1587(15) 0.5012(11) 0.051(5) Uani 1 d . . . C4 C 0.307(3) 1.1542(18) 0.5569(18) 0.063(7) Uani 1 d . . . H4 H 0.3234 1.2101 0.5922 0.076 Uiso 1 calc R . . C5 C 0.408(2) 0.7605(15) 0.1616(13) 0.037(5) Uani 1 d . . . C6 C 0.514(2) 0.8440(18) 0.1567(15) 0.051(6) Uani 1 d . . . N3 N 0.392(2) 0.6779(12) 0.1172(11) 0.041(4) Uani 1 d . . . N4 N 0.599(2) 0.8494(13) 0.1066(13) 0.048(5) Uani 1 d . . . C7 C 0.485(3) 0.6845(16) 0.0662(16) 0.054(6) Uani 1 d . . . H7 H 0.4772 0.6289 0.0325 0.064 Uiso 1 calc R . . C8 C 0.585(3) 0.7654(18) 0.0614(14) 0.055(6) Uani 1 d . . . H8 H 0.6467 0.7637 0.0264 0.066 Uiso 1 calc R . . Au2 Au 0.39241(9) 0.35161(6) 0.22103(5) 0.0376(2) Uani 1 d . . . Se5 Se 0.3334(3) 0.19160(17) 0.14687(15) 0.0473(6) Uani 1 d . . . Se6 Se 0.5815(3) 0.40768(17) 0.14793(14) 0.0432(5) Uani 1 d . . . Se7 Se 0.4432(3) 0.51166(18) 0.29338(14) 0.0452(6) Uani 1 d . . . Se8 Se 0.2143(3) 0.2961(2) 0.29975(16) 0.0573(7) Uani 1 d . . . C9 C 0.176(2) 0.1250(18) 0.1877(12) 0.041(5) Uani 1 d . . . N5 N 0.106(2) 0.0329(15) 0.1519(13) 0.052(5) Uani 1 d . . . C10 C 0.129(2) 0.1650(19) 0.2510(15) 0.049(6) Uani 1 d . . . N6 N 0.022(2) 0.117(2) 0.2832(15) 0.076(8) Uani 1 d . . . C11 C 0.001(3) -0.016(2) 0.1860(18) 0.077(10) Uani 1 d . . . H11 H -0.0408 -0.0813 0.1677 0.092 Uiso 1 calc R . . C12 C -0.048(3) 0.026(2) 0.2479(15) 0.066(8) Uani 1 d . . . H12 H -0.1296 -0.0086 0.2644 0.079 Uiso 1 calc R . . C13 C 0.669(2) 0.5358(16) 0.2019(13) 0.040(5) Uani 1 d . . . N7 N 0.787(2) 0.5825(16) 0.1771(14) 0.061(6) Uani 1 d . . . C14 C 0.622(2) 0.5759(17) 0.2622(13) 0.042(5) Uani 1 d . . . N8 N 0.684(2) 0.6671(16) 0.3002(13) 0.056(5) Uani 1 d . . . C15 C 0.847(3) 0.6742(17) 0.2190(19) 0.063(8) Uani 1 d . . . H15 H 0.9252 0.7136 0.2032 0.075 Uiso 1 calc R . . C16 C 0.804(3) 0.711(2) 0.2783(16) 0.063(7) Uani 1 d . . . H16 H 0.8610 0.7711 0.3061 0.076 Uiso 1 calc R . . S1 S 0.7053(6) 0.5086(4) 0.4678(4) 0.0441(13) Uani 1 d . . . S2 S 0.8544(7) 0.4119(5) 0.6047(4) 0.0491(14) Uani 1 d . . . S3 S 0.9821(7) 0.6994(4) 0.5280(4) 0.0471(14) Uani 1 d . . . S4 S 1.1373(6) 0.6028(4) 0.6613(3) 0.0438(13) Uani 1 d . . . C17 C 0.860(2) 0.5136(16) 0.5535(12) 0.038(5) Uani 1 d . . . C18 C 0.983(2) 0.5969(14) 0.5770(11) 0.035(4) Uani 1 d . . . C19 C 0.611(3) 0.3963(17) 0.4811(13) 0.044(5) Uani 1 d . . . H19 H 0.5149 0.3665 0.4459 0.053 Uiso 1 calc R . . C20 C 0.678(2) 0.3542(14) 0.5419(14) 0.041(6) Uani 1 d . . . H20 H 0.6306 0.2929 0.5514 0.050 Uiso 1 calc R . . C21 C 1.149(3) 0.7631(17) 0.5932(15) 0.050(6) Uani 1 d . . . H21 H 1.1891 0.8271 0.5865 0.060 Uiso 1 calc R . . C22 C 1.220(3) 0.7194(18) 0.6538(15) 0.054(6) Uani 1 d . . . H22 H 1.3118 0.7514 0.6913 0.065 Uiso 1 calc R . . S5 S 0.1166(7) 0.8697(5) 0.0325(4) 0.0538(15) Uani 1 d . . . S6 S 0.2416(8) 0.8134(5) -0.0962(4) 0.0599(17) Uani 1 d . . . S7 S 0.0211(9) 0.5979(5) -0.1191(4) 0.0651(19) Uani 1 d . . . S8 S -0.0924(8) 0.6546(5) 0.0136(5) 0.068(2) Uani 1 d . . . C24 C 0.117(3) 0.7806(15) -0.0368(12) 0.040(5) Uani 1 d . . . C25 C 0.030(3) 0.6878(14) -0.0454(14) 0.045(5) Uani 1 d . . . C26 C 0.248(3) 0.9550(15) 0.0064(15) 0.061(8) Uani 1 d . . . H26 H 0.2805 1.0175 0.0336 0.073 Uiso 1 calc R . . C27 C 0.304(3) 0.9288(17) -0.0564(15) 0.058(7) Uani 1 d . . . H27 H 0.3726 0.9730 -0.0754 0.069 Uiso 1 calc R . . C28 C -0.175(4) 0.542(2) -0.037(2) 0.082(11) Uani 1 d . . . H28 H -0.2507 0.4997 -0.0206 0.098 Uiso 1 calc R . . C29 C -0.129(3) 0.5159(18) -0.097(2) 0.082(12) Uani 1 d . . . H29 H -0.1727 0.4559 -0.1278 0.098 Uiso 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 0.0355(4) 0.0310(4) 0.0336(4) 0.0054(3) 0.0145(3) 0.0064(3) Se1 0.0471(12) 0.0349(12) 0.0492(13) 0.0067(10) 0.0263(10) 0.0048(9) Se2 0.0470(12) 0.0293(11) 0.0444(12) 0.0017(9) 0.0210(10) 0.0012(9) Se3 0.0574(13) 0.0311(12) 0.0562(14) 0.0003(10) 0.0340(11) -0.0008(10) Se4 0.0559(13) 0.0337(12) 0.0587(15) 0.0029(11) 0.0361(12) 0.0001(10) C1 0.055(12) 0.020(9) 0.042(11) 0.012(8) 0.031(9) 0.023(9) N1 0.047(10) 0.057(12) 0.038(10) 0.001(9) 0.019(8) 0.017(9) C3 0.091(19) 0.068(18) 0.029(12) -0.018(12) 0.014(12) 0.038(15) C2 0.043(11) 0.038(12) 0.042(12) 0.017(10) 0.016(9) 0.022(9) N2 0.055(11) 0.062(14) 0.031(10) -0.008(9) 0.002(9) 0.019(10) C4 0.10(2) 0.028(13) 0.070(18) 0.005(12) 0.023(16) 0.030(14) C5 0.047(11) 0.030(11) 0.038(11) 0.003(9) 0.010(9) 0.020(9) C6 0.021(9) 0.049(14) 0.063(15) 0.007(12) -0.006(9) -0.009(9) N3 0.046(10) 0.032(10) 0.038(10) -0.004(8) 0.012(8) -0.001(8) N4 0.046(10) 0.031(10) 0.076(14) 0.018(10) 0.036(10) 0.006(8) C7 0.065(15) 0.027(12) 0.076(18) 0.007(11) 0.023(13) 0.022(11) C8 0.093(19) 0.051(15) 0.036(12) 0.024(11) 0.029(12) 0.030(14) Au2 0.0409(4) 0.0428(5) 0.0332(4) 0.0041(4) 0.0125(3) 0.0159(4) Se5 0.0591(14) 0.0362(12) 0.0526(14) 0.0036(10) 0.0307(11) 0.0036(10) Se6 0.0488(12) 0.0407(12) 0.0445(12) -0.0044(10) 0.0221(10) 0.0095(10) Se7 0.0526(13) 0.0494(14) 0.0389(12) -0.0050(10) 0.0164(10) 0.0210(11) Se8 0.0700(16) 0.0683(18) 0.0547(15) 0.0137(13) 0.0402(13) 0.0309(14) C9 0.044(11) 0.068(16) 0.025(10) 0.023(10) 0.018(9) 0.026(11) N5 0.055(12) 0.042(12) 0.070(14) 0.018(10) 0.025(10) 0.021(9) C10 0.029(10) 0.061(16) 0.059(15) 0.011(12) 0.010(10) 0.019(10) N6 0.042(12) 0.14(3) 0.070(15) 0.046(17) 0.035(11) 0.037(14) C11 0.052(15) 0.08(2) 0.064(18) 0.036(16) -0.012(13) -0.027(14) C12 0.077(18) 0.08(2) 0.032(13) 0.017(13) 0.018(12) -0.006(16) C13 0.040(11) 0.043(12) 0.046(12) -0.004(10) 0.025(10) 0.013(9) N7 0.041(11) 0.060(14) 0.069(14) -0.009(11) 0.006(10) -0.005(10) C14 0.043(11) 0.051(14) 0.035(11) 0.027(10) 0.005(9) 0.019(10) N8 0.060(13) 0.051(13) 0.061(13) -0.004(10) 0.016(11) 0.021(10) C15 0.038(12) 0.037(14) 0.10(2) -0.022(14) 0.015(13) -0.006(10) C16 0.058(16) 0.071(19) 0.052(16) -0.003(14) 0.002(13) 0.014(14) S1 0.043(3) 0.043(3) 0.049(3) 0.008(3) 0.013(2) 0.015(2) S2 0.054(3) 0.049(4) 0.050(3) 0.021(3) 0.019(3) 0.017(3) S3 0.048(3) 0.045(3) 0.057(4) 0.015(3) 0.020(3) 0.019(3) S4 0.045(3) 0.049(3) 0.039(3) 0.012(3) 0.010(2) 0.015(2) C17 0.047(12) 0.045(13) 0.027(10) 0.002(9) 0.014(9) 0.015(10) C18 0.060(13) 0.031(10) 0.023(9) 0.016(8) 0.020(9) 0.022(9) C19 0.048(12) 0.052(14) 0.037(12) 0.010(11) 0.017(10) 0.015(11) C20 0.047(12) 0.026(10) 0.058(14) -0.022(10) 0.037(11) -0.002(9) C21 0.064(15) 0.036(12) 0.065(16) 0.017(11) 0.039(13) 0.015(11) C22 0.057(14) 0.050(15) 0.042(13) -0.013(11) 0.001(11) 0.002(12) S5 0.061(4) 0.037(3) 0.065(4) 0.006(3) 0.021(3) 0.009(3) S6 0.068(4) 0.059(4) 0.057(4) 0.018(3) 0.026(3) 0.008(3) S7 0.076(5) 0.049(4) 0.058(4) -0.001(3) 0.001(3) 0.011(3) S8 0.059(4) 0.052(4) 0.107(6) 0.028(4) 0.043(4) 0.014(3) C24 0.056(13) 0.031(11) 0.027(10) 0.007(8) 0.004(9) 0.005(9) C25 0.077(16) 0.019(10) 0.055(14) 0.012(9) 0.032(12) 0.025(10) C26 0.090(19) 0.016(10) 0.054(15) 0.025(10) -0.009(13) -0.002(11) C27 0.073(16) 0.042(14) 0.047(14) 0.025(12) 0.012(12) -0.013(12) C28 0.071(19) 0.045(17) 0.10(3) 0.025(17) -0.031(18) 0.015(14) C29 0.08(2) 0.021(12) 0.09(2) -0.012(14) -0.054(18) -0.002(12) _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 Se4 2.416(2) . ? Au1 Se1 2.420(2) . ? Au1 Se2 2.423(2) . ? Au1 Se3 2.434(3) . ? Se1 C1 1.858(19) . ? Se2 C2 1.86(2) . ? Se3 C5 1.91(2) . ? Se4 C6 1.93(3) . ? C1 N1 1.36(2) . ? C1 C2 1.48(3) . ? N1 C3 1.28(3) . ? C3 C4 1.39(4) . ? C2 N2 1.34(3) . ? N2 C4 1.29(3) . ? C5 N3 1.32(3) . ? C5 C6 1.40(3) . ? C6 N4 1.30(3) . ? N3 C7 1.37(3) . ? N4 C8 1.35(3) . ? C7 C8 1.34(3) . ? Au2 Se7 2.419(3) . ? Au2 Se5 2.423(3) . ? Au2 Se8 2.425(3) . ? Au2 Se6 2.435(2) . ? Se5 C9 1.88(2) . ? Se6 C13 1.90(2) . ? Se7 C14 1.93(2) . ? Se8 C10 1.91(3) . ? C9 N5 1.36(3) . ? C9 C10 1.40(3) . ? N5 C11 1.35(3) . ? C10 N6 1.33(3) . ? N6 C12 1.35(4) . ? C11 C12 1.41(4) . ? C13 N7 1.34(3) . ? C13 C14 1.36(3) . ? N7 C15 1.38(3) . ? C14 N8 1.35(3) . ? N8 C16 1.31(3) . ? C15 C16 1.30(4) . ? S1 C19 1.70(2) . ? S1 C17 1.74(2) . ? S2 C20 1.71(2) . ? S2 C17 1.71(2) . ? S3 C21 1.69(3) . ? S3 C18 1.702(19) . ? S4 C22 1.69(3) . ? S4 C18 1.71(2) . ? C17 C18 1.41(3) . ? C19 C20 1.29(3) . ? C21 C22 1.32(3) . ? S5 C24 1.69(2) . ? S5 C26 1.69(2) . ? S6 C27 1.66(3) . ? S6 C24 1.74(2) . ? S7 C25 1.72(2) . ? S7 C29 1.75(4) . ? S8 C28 1.70(3) . ? S8 C25 1.72(2) . ? C24 C25 1.37(3) . ? C26 C27 1.38(4) . ? C28 C29 1.28(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Se4 Au1 Se1 178.19(9) . . ? Se4 Au1 Se2 86.83(8) . . ? Se1 Au1 Se2 91.46(8) . . ? Se4 Au1 Se3 91.53(8) . . ? Se1 Au1 Se3 90.19(8) . . ? Se2 Au1 Se3 177.63(9) . . ? C1 Se1 Au1 101.5(6) . . ? C2 Se2 Au1 102.2(7) . . ? C5 Se3 Au1 100.9(6) . . ? C6 Se4 Au1 101.6(7) . . ? N1 C1 C2 116.5(18) . . ? N1 C1 Se1 120.0(15) . . ? C2 C1 Se1 122.9(14) . . ? C3 N1 C1 120(2) . . ? N1 C3 C4 122(2) . . ? N2 C2 C1 121.0(19) . . ? N2 C2 Se2 117.3(16) . . ? C1 C2 Se2 121.5(15) . . ? C4 N2 C2 117(2) . . ? N2 C4 C3 124(2) . . ? N3 C5 C6 121(2) . . ? N3 C5 Se3 114.6(16) . . ? C6 C5 Se3 124.1(17) . . ? N4 C6 C5 124(2) . . ? N4 C6 Se4 114.3(16) . . ? C5 C6 Se4 121.2(18) . . ? C5 N3 C7 113.8(19) . . ? C6 N4 C8 115(2) . . ? C8 C7 N3 125(2) . . ? C7 C8 N4 121(2) . . ? Se7 Au2 Se5 178.25(9) . . ? Se7 Au2 Se8 87.85(9) . . ? Se5 Au2 Se8 91.33(9) . . ? Se7 Au2 Se6 91.34(8) . . ? Se5 Au2 Se6 89.55(8) . . ? Se8 Au2 Se6 177.22(10) . . ? C9 Se5 Au2 101.4(8) . . ? C13 Se6 Au2 100.3(6) . . ? C14 Se7 Au2 100.6(7) . . ? C10 Se8 Au2 101.1(7) . . ? N5 C9 C10 120(2) . . ? N5 C9 Se5 116.4(15) . . ? C10 C9 Se5 123.8(19) . . ? C11 N5 C9 115(2) . . ? N6 C10 C9 125(3) . . ? N6 C10 Se8 113(2) . . ? C9 C10 Se8 122.1(18) . . ? C10 N6 C12 116(3) . . ? N5 C11 C12 124(3) . . ? N6 C12 C11 120(2) . . ? N7 C13 C14 122(2) . . ? N7 C13 Se6 113.2(15) . . ? C14 C13 Se6 124.6(16) . . ? C13 N7 C15 111(2) . . ? N8 C14 C13 124(2) . . ? N8 C14 Se7 113.4(17) . . ? C13 C14 Se7 122.1(18) . . ? C16 N8 C14 113(2) . . ? C16 C15 N7 127(3) . . ? C15 C16 N8 122(3) . . ? C19 S1 C17 94.0(11) . . ? C20 S2 C17 93.5(11) . . ? C21 S3 C18 94.5(11) . . ? C22 S4 C18 94.1(11) . . ? C18 C17 S2 123.6(15) . . ? C18 C17 S1 120.8(16) . . ? S2 C17 S1 115.5(12) . . ? C17 C18 S3 122.8(15) . . ? C17 C18 S4 121.4(14) . . ? S3 C18 S4 115.7(12) . . ? C20 C19 S1 117.4(18) . . ? C19 C20 S2 119.5(17) . . ? C22 C21 S3 117.9(18) . . ? C21 C22 S4 117.7(19) . . ? C24 S5 C26 95.2(13) . . ? C27 S6 C24 96.0(12) . . ? C25 S7 C29 94.4(14) . . ? C28 S8 C25 96.1(16) . . ? C25 C24 S5 123.7(17) . . ? C25 C24 S6 121.2(17) . . ? S5 C24 S6 115.1(12) . . ? C24 C25 S8 121.5(17) . . ? C24 C25 S7 124.3(17) . . ? S8 C25 S7 114.0(13) . . ? C27 C26 S5 117.8(18) . . ? C26 C27 S6 115.8(17) . . ? C29 C28 S8 118(3) . . ? C28 C29 S7 117(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.866 _refine_diff_density_min -4.621 _refine_diff_density_rms 0.385 data_(ttf)3[Au(pds)2]2 _database_code_CSD 159180 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.50 H5 Au0.50 N2 S3 Se2' _chemical_formula_weight 487.73 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x, y, -z' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 22.437(9) _cell_length_b 10.9810(10) _cell_length_c 10.854(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.79(2) _cell_angle_gamma 90.00 _cell_volume 2672.9(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 11.435 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8278 _exptl_absorpt_correction_T_max 0.9991 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3807 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 13.5433 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.98 _reflns_number_total 3392 _reflns_number_gt 1768 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3392 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1646 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1412 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.18212(3) 0.0000 0.44764(7) 0.0346(2) Uani 1 d S . . Se1 Se 0.16297(7) 0.15663(11) 0.29326(12) 0.0473(4) Uani 1 d . . . Se2 Se 0.20048(7) 0.15752(11) 0.60145(12) 0.0473(4) Uani 1 d . . . C1 C 0.1246(5) 0.0633(10) 0.1655(10) 0.038(3) Uani 1 d . . . N1 N 0.1019(5) 0.1273(10) 0.0742(9) 0.047(3) Uani 1 d . . . C2 C 0.0796(6) 0.0649(13) -0.0181(13) 0.061(4) Uani 1 d . . . H2 H 0.0632 0.1061 -0.0859 0.073 Uiso 1 calc R . . C3 C 0.2132(6) 0.0670(11) 0.7457(11) 0.046(3) Uani 1 d . . . N2 N 0.2234(5) 0.1283(12) 0.8497(10) 0.056(3) Uani 1 d . . . C4 C 0.2332(6) 0.0594(12) 0.9538(12) 0.058(4) Uani 1 d . . . H4 H 0.2402 0.0995 1.0283 0.070 Uiso 1 calc R . . C5 C 0.4375(8) 0.0000 0.1940(17) 0.043(4) Uani 1 d S . . C6 C 0.4991(8) 0.0000 0.1733(15) 0.042(4) Uani 1 d S . . S1 S 0.53959(15) 0.1339(3) 0.1532(3) 0.0439(8) Uani 1 d . . . C7 C 0.6065(6) 0.0598(12) 0.1215(11) 0.052(4) Uani 1 d . . . H7 H 0.6408 0.1037 0.1052 0.063 Uiso 1 calc R . . S2 S 0.39924(15) 0.1335(3) 0.2085(3) 0.0470(8) Uani 1 d . . . C8 C 0.3286(6) 0.0603(11) 0.2263(11) 0.052(3) Uani 1 d . . . H8 H 0.2937 0.1047 0.2351 0.062 Uiso 1 calc R . . S3 S 0.42995(14) 0.1326(3) 0.5279(3) 0.0402(7) Uani 1 d . . . C9 C 0.4693(7) 0.0000 0.5123(13) 0.030(3) Uani 1 d S . . C10 C 0.3618(5) 0.0611(11) 0.5473(10) 0.039(3) Uani 1 d . . . H10 H 0.3270 0.1054 0.5573 0.047 Uiso 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 Au 0.0363(4) 0.0300(3) 0.0375(4) 0.000 0.0020(3) 0.005 Se1 0.0662(10) 0.0269(7) 0.0483(8) -0.0016(5) -0.0068(7) 0.0022(6) Se2 0.0636(10) 0.0341(8) 0.0441(8) -0.0066(5) -0.0012(7) 0.0049(6) C1 0.043(7) 0.029(6) 0.041(6) 0.001(5) -0.001(5) 0.004(5) N1 0.052(7) 0.042(6) 0.046(6) -0.007(5) -0.006(5) 0.002(5) C2 0.068(10) 0.061(9) 0.053(8) 0.009(7) -0.016(7) -0.005(8) C3 0.052(8) 0.045(8) 0.041(7) -0.004(6) 0.004(6) 0.005(6) N2 0.050(7) 0.074(8) 0.044(6) -0.023(6) 0.008(5) 0.005(6) C4 0.060(9) 0.078(10) 0.038(7) -0.005(7) 0.012(6) -0.002(8) C5 0.049(11) 0.023(8) 0.058(11) 0.000 0.008(9) 0.000 C6 0.042(10) 0.048(11) 0.037(9) 0.000 0.001(8) 0.000 S1 0.0477(19) 0.0351(16) 0.0488(18) -0.0017(14) 0.0000(15) -0.0093(15) C7 0.047(8) 0.066(9) 0.042(7) -0.001(6) -0.013(6) -0.005(7) S2 0.049(2) 0.0351(16) 0.057(2) -0.0053(15) 0.0013(16) 0.0059(15) C8 0.052(8) 0.049(8) 0.055(8) -0.001(6) -0.003(6) -0.009(6) S3 0.0366(16) 0.0302(15) 0.0538(18) -0.0008(14) 0.0023(14) 0.0009(13) C9 0.040(9) 0.031(8) 0.018(7) 0.000 -0.009(7) 0.000 C10 0.034(6) 0.047(7) 0.037(6) 0.000(5) 0.010(5) -0.002(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 Au Se2 2.4302(15) . ? Au Se2 2.4302(15) 2 ? Au Se1 2.4301(15) 2 ? Au Se1 2.4301(15) . ? Se1 C1 1.909(11) . ? Se2 C3 1.869(12) . ? C1 N1 1.305(14) . ? C1 C1 1.39(2) 2 ? N1 C2 1.301(15) . ? C2 C2 1.43(3) 2 ? C3 N2 1.328(15) . ? C3 C3 1.47(3) 2 ? N2 C4 1.371(16) . ? C4 C4 1.30(3) 2 ? C5 C6 1.41(2) . ? C5 S2 1.708(10) 2 ? C5 S2 1.708(10) . ? C6 S1 1.746(10) . ? C6 S1 1.746(10) 2 ? S1 C7 1.750(13) . ? C7 C7 1.31(3) 2 ? S2 C8 1.792(13) . ? C8 C8 1.32(3) 2 ? S3 C9 1.714(8) . ? S3 C10 1.737(11) . ? C9 C9 1.41(3) 5_656 ? C9 S3 1.714(8) 2 ? C10 C10 1.34(2) 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 Se2 Au Se2 90.76(7) . 2 ? Se2 Au Se1 179.50(6) . 2 ? Se2 Au Se1 89.57(5) 2 2 ? Se2 Au Se1 89.57(5) . . ? Se2 Au Se1 179.50(6) 2 . ? Se1 Au Se1 90.10(7) 2 . ? C1 Se1 Au 100.8(3) . . ? C3 Se2 Au 102.4(4) . . ? N1 C1 C1 122.6(7) . 2 ? N1 C1 Se1 114.8(8) . . ? C1 C1 Se1 122.5(3) 2 . ? C2 N1 C1 115.6(11) . . ? N1 C2 C2 121.8(8) . 2 ? N2 C3 C3 120.4(8) . 2 ? N2 C3 Se2 117.4(10) . . ? C3 C3 Se2 122.1(4) 2 . ? C3 N2 C4 116.1(12) . . ? C4 C4 N2 123.5(7) 2 . ? C6 C5 S2 120.9(5) . 2 ? C6 C5 S2 120.9(5) . . ? S2 C5 S2 118.2(11) 2 . ? C5 C6 S1 122.5(5) . . ? C5 C6 S1 122.5(5) . 2 ? S1 C6 S1 114.7(10) . 2 ? C6 S1 C7 94.9(7) . . ? C7 C7 S1 117.7(4) 2 . ? C5 S2 C8 94.2(7) . . ? C8 C8 S2 116.7(4) 2 . ? C9 S3 C10 94.9(6) . . ? C9 C9 S3 121.8(4) 5_656 2 ? C9 C9 S3 121.8(4) 5_656 . ? S3 C9 S3 116.4(9) 2 . ? C10 C10 S3 116.9(4) 2 . ? _diffrn_measured_fraction_theta_max 0.499 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.499 _refine_diff_density_max 2.416 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.247 data_(ttf)3[Au(pds)2]3 _database_code_CSD 159181 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H12 Au1.50 N6 S6 Se6' _chemical_formula_weight 1309.94 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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.775(2) _cell_length_b 20.404(2) _cell_length_c 15.424(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.25(2) _cell_angle_gamma 90.00 _cell_volume 3063.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 13 _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.840 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2394 _exptl_absorpt_coefficient_mu 14.751 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.6183 _exptl_absorpt_correction_T_max 0.9995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6311 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0561 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.93 _reflns_number_total 5953 _reflns_number_gt 4202 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+133.4530P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5953 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1573 _refine_ls_wR_factor_gt 0.1402 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.0000 0.0000 0.0000 0.0380(3) Uani 1 d S . . Se1 Se 0.0203(2) 0.11506(11) -0.03753(14) 0.0493(5) Uani 1 d . . . Se2 Se -0.0167(2) 0.02706(10) 0.15186(13) 0.0457(5) Uani 1 d . . . C1 C 0.0066(17) 0.1572(14) 0.0720(12) 0.054(7) Uani 1 d . . . N1 N 0.0116(16) 0.2218(8) 0.0685(13) 0.051(5) Uani 1 d . . . C2 C 0.0034(19) 0.2496(12) 0.1477(16) 0.059(6) Uani 1 d . . . H2 H 0.0085 0.2950 0.1508 0.071 Uiso 1 calc R . . C3 C -0.0111(16) 0.1196(11) 0.1474(13) 0.043(5) Uani 1 d . . . N2 N -0.0184(16) 0.1500(9) 0.2232(11) 0.048(4) Uani 1 d . . . C4 C -0.012(2) 0.2165(13) 0.2238(17) 0.068(7) Uani 1 d . . . H4 H -0.0179 0.2395 0.2753 0.081 Uiso 1 calc R . . Au2 Au -0.00709(7) 0.80385(4) 0.23792(5) 0.03436(19) Uani 1 d . . . Se3 Se 0.16792(18) 0.87185(10) 0.31460(14) 0.0444(5) Uani 1 d . . . Se4 Se 0.17445(18) 0.73834(10) 0.18369(13) 0.0410(5) Uani 1 d . . . Se5 Se -0.18116(19) 0.73477(10) 0.16213(13) 0.0448(5) Uani 1 d . . . Se6 Se -0.18782(19) 0.87018(10) 0.29207(14) 0.0453(5) Uani 1 d . . . C5 C 0.0595(14) 0.9423(9) 0.3507(11) 0.032(4) Uani 1 d . . . N11 N 0.1294(16) 0.9951(8) 0.3830(10) 0.045(4) Uani 1 d . . . C6 C -0.0873(18) 0.9424(9) 0.3409(11) 0.034(4) Uani 1 d . . . N12 N -0.1570(16) 0.9913(9) 0.3686(12) 0.054(5) Uani 1 d . . . C7 C -0.0854(19) 1.0439(12) 0.4007(15) 0.057(6) Uani 1 d . . . H7 H -0.1333 1.0804 0.4179 0.068 Uiso 1 calc R . . C8 C 0.055(2) 1.0454(11) 0.4088(14) 0.051(5) Uani 1 d . . . H8 H 0.0995 1.0822 0.4328 0.062 Uiso 1 calc R . . C9 C -0.0736(17) 0.6790(9) 0.0963(11) 0.037(4) Uani 1 d . . . N13 N -0.1422(16) 0.6363(8) 0.0449(11) 0.046(4) Uani 1 d . . . C10 C -0.069(2) 0.5974(12) -0.0006(14) 0.055(6) Uani 1 d . . . H10 H -0.1139 0.5667 -0.0374 0.066 Uiso 1 calc R . . C11 C 0.0758(15) 0.6816(9) 0.1057(11) 0.030(4) Uani 1 d . . . N14 N 0.1438(17) 0.6426(8) 0.0563(10) 0.044(4) Uani 1 d . . . C12 C 0.075(2) 0.6005(12) 0.0042(16) 0.061(6) Uani 1 d . . . H12 H 0.1226 0.5724 -0.0299 0.073 Uiso 1 calc R . . C13 C 0.0117(16) 0.6138(10) 0.3389(14) 0.047(5) Uani 1 d . . . S1 S 0.1691(5) 0.5862(3) 0.3198(4) 0.0512(14) Uani 1 d . . . S2 S -0.1259(5) 0.5762(3) 0.2788(4) 0.0492(13) Uani 1 d . . . C14 C 0.111(2) 0.5318(11) 0.2412(14) 0.055(6) Uani 1 d . . . H14 H 0.1729 0.5067 0.2126 0.066 Uiso 1 calc R . . C15 C -0.024(2) 0.5259(10) 0.2215(13) 0.048(5) Uani 1 d . . . H15 H -0.0606 0.4965 0.1796 0.058 Uiso 1 calc R . . C16 C -0.0064(17) 0.6665(10) 0.3934(12) 0.037(4) Uani 1 d . . . S3 S -0.1670(5) 0.6967(3) 0.4105(3) 0.0479(13) Uani 1 d . . . S4 S 0.1273(5) 0.7067(3) 0.4469(4) 0.0545(14) Uani 1 d . . . C17 C 0.028(2) 0.7633(13) 0.4945(17) 0.069(7) Uani 1 d . . . H17 H 0.0673 0.7965 0.5299 0.083 Uiso 1 calc R . . C18 C -0.106(2) 0.7575(11) 0.4786(14) 0.059(6) Uani 1 d . . . H18 H -0.1653 0.7858 0.5038 0.071 Uiso 1 calc R . . C19 C 0.0162(18) 0.4739(12) 0.4754(13) 0.054(6) Uani 1 d . . . S5 S 0.1759(5) 0.4473(3) 0.4608(4) 0.0524(14) Uani 1 d . . . S6 S -0.1167(5) 0.4343(3) 0.4104(3) 0.0501(13) Uani 1 d . . . C20 C 0.128(2) 0.3893(12) 0.3827(14) 0.056(6) Uani 1 d . . . H20 H 0.1920 0.3643 0.3564 0.067 Uiso 1 calc R . . C21 C -0.003(3) 0.3826(10) 0.3626(14) 0.058(6) Uani 1 d . . . H21 H -0.0362 0.3505 0.3232 0.069 Uiso 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 0.0225(5) 0.0443(6) 0.0478(6) 0.0176(5) 0.0057(4) 0.0040(4) Se1 0.0494(12) 0.0468(13) 0.0528(12) 0.0205(10) 0.0100(9) 0.0013(10) Se2 0.0428(11) 0.0477(12) 0.0470(11) 0.0191(9) 0.0068(9) -0.0001(9) C1 0.012(8) 0.12(2) 0.035(10) 0.006(12) 0.008(7) -0.005(11) N1 0.030(9) 0.031(10) 0.094(15) 0.018(9) 0.018(9) 0.005(7) C2 0.028(10) 0.065(16) 0.085(18) -0.019(14) 0.004(11) -0.016(10) C3 0.009(7) 0.070(14) 0.052(12) -0.014(10) 0.003(7) -0.009(8) N2 0.040(9) 0.046(11) 0.055(11) 0.001(8) -0.008(8) -0.001(8) C4 0.052(14) 0.080(19) 0.072(17) -0.017(14) 0.010(12) 0.021(13) Au2 0.0286(3) 0.0345(4) 0.0395(4) 0.0073(3) 0.0005(3) -0.0017(3) Se3 0.0268(9) 0.0447(12) 0.0608(13) -0.0086(10) -0.0016(8) 0.0001(8) Se4 0.0260(9) 0.0372(11) 0.0590(12) -0.0007(9) -0.0002(8) -0.0034(8) Se5 0.0278(9) 0.0480(12) 0.0577(12) -0.0004(10) -0.0009(8) -0.0061(9) Se6 0.0278(9) 0.0468(12) 0.0609(13) -0.0015(10) 0.0029(8) -0.0009(9) C5 0.006(7) 0.049(11) 0.041(10) 0.007(8) -0.006(6) -0.007(7) N11 0.041(9) 0.041(10) 0.053(10) 0.010(8) -0.002(7) 0.005(8) C6 0.035(9) 0.042(11) 0.027(9) 0.010(8) 0.007(7) 0.006(8) N12 0.031(9) 0.054(12) 0.076(13) 0.008(10) 0.001(8) 0.005(9) C7 0.022(10) 0.065(15) 0.081(16) -0.001(12) -0.006(10) 0.018(10) C8 0.047(12) 0.051(14) 0.059(13) -0.005(11) 0.020(10) -0.005(10) C9 0.029(9) 0.037(11) 0.042(10) 0.015(8) -0.008(7) -0.011(8) N13 0.045(9) 0.041(10) 0.049(10) 0.003(8) -0.013(8) -0.004(8) C10 0.047(12) 0.065(15) 0.052(13) -0.012(11) 0.002(10) -0.021(11) C11 0.016(7) 0.042(11) 0.034(9) 0.001(8) 0.006(6) -0.001(7) N14 0.048(10) 0.045(10) 0.040(9) -0.007(8) 0.004(7) -0.009(8) C12 0.059(14) 0.051(14) 0.073(16) 0.005(12) 0.004(12) -0.006(12) C13 0.005(7) 0.054(13) 0.082(15) 0.021(11) 0.001(8) 0.011(8) S1 0.028(2) 0.040(3) 0.086(4) 0.006(3) 0.013(2) 0.002(2) S2 0.031(2) 0.054(3) 0.061(3) 0.011(3) -0.003(2) -0.001(2) C14 0.033(11) 0.062(15) 0.071(15) 0.001(12) 0.019(10) 0.013(10) C15 0.056(13) 0.040(12) 0.049(12) -0.008(9) 0.006(10) -0.001(10) C16 0.027(9) 0.044(11) 0.041(10) 0.005(9) 0.005(8) 0.009(8) S3 0.024(2) 0.063(3) 0.057(3) 0.009(3) 0.004(2) 0.008(2) S4 0.034(3) 0.053(4) 0.075(4) 0.007(3) -0.005(2) 0.001(2) C17 0.039(13) 0.083(19) 0.083(17) -0.022(15) -0.009(12) -0.009(12) C18 0.074(16) 0.059(15) 0.048(12) -0.006(11) 0.021(11) 0.007(13) C19 0.020(9) 0.083(19) 0.058(14) 0.017(11) 0.003(9) -0.015(11) S5 0.020(2) 0.081(4) 0.056(3) -0.002(3) 0.003(2) -0.002(2) S6 0.029(2) 0.068(4) 0.051(3) 0.003(3) -0.005(2) -0.007(2) C20 0.046(12) 0.066(16) 0.057(13) 0.007(12) 0.009(10) -0.005(11) C21 0.086(18) 0.030(11) 0.055(13) 0.004(10) -0.003(12) -0.005(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 Se2 2.427(2) 3 ? Au1 Se2 2.427(2) . ? Au1 Se1 2.431(2) . ? Au1 Se1 2.431(2) 3 ? Se1 C1 1.91(2) . ? Se2 C3 1.89(2) . ? C1 N1 1.32(3) . ? C1 C3 1.42(3) . ? N1 C2 1.35(3) . ? C2 C4 1.37(3) . ? C3 N2 1.33(2) . ? N2 C4 1.36(3) . ? Au2 Se3 2.425(2) . ? Au2 Se5 2.426(2) . ? Au2 Se4 2.431(2) . ? Au2 Se6 2.433(2) . ? Se3 C5 1.899(18) . ? Se4 C11 1.872(17) . ? Se5 C9 1.90(2) . ? Se6 C6 1.889(19) . ? C5 N11 1.35(2) . ? C5 C6 1.43(2) . ? N11 C8 1.34(3) . ? C6 N12 1.30(2) . ? N12 C7 1.35(3) . ? C7 C8 1.36(3) . ? C9 N13 1.32(2) . ? C9 C11 1.46(2) . ? N13 C10 1.31(3) . ? C10 C12 1.40(3) . ? C11 N14 1.32(2) . ? N14 C12 1.32(3) . ? C13 C16 1.39(3) . ? C13 S1 1.689(17) . ? C13 S2 1.74(2) . ? S1 C14 1.70(2) . ? S2 C15 1.73(2) . ? C14 C15 1.33(3) . ? C16 S4 1.693(19) . ? C16 S3 1.729(17) . ? S3 C18 1.70(2) . ? S4 C17 1.71(3) . ? C17 C18 1.32(3) . ? C19 C19 1.36(5) 3_566 ? C19 S5 1.69(2) . ? C19 S6 1.76(2) . ? S5 C20 1.72(2) . ? S6 C21 1.74(2) . ? C20 C21 1.30(3) . ? 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 Se2 Au1 Se2 180.0 3 . ? Se2 Au1 Se1 88.61(7) 3 . ? Se2 Au1 Se1 91.39(7) . . ? Se2 Au1 Se1 91.39(7) 3 3 ? Se2 Au1 Se1 88.61(7) . 3 ? Se1 Au1 Se1 180.0 . 3 ? C1 Se1 Au1 102.1(8) . . ? C3 Se2 Au1 100.8(6) . . ? N1 C1 C3 126(2) . . ? N1 C1 Se1 114.0(16) . . ? C3 C1 Se1 120.4(19) . . ? C1 N1 C2 112(2) . . ? N1 C2 C4 126(2) . . ? N2 C3 C1 119(2) . . ? N2 C3 Se2 115.4(15) . . ? C1 C3 Se2 125.2(16) . . ? C3 N2 C4 118(2) . . ? N2 C4 C2 120(2) . . ? Se3 Au2 Se5 179.36(8) . . ? Se3 Au2 Se4 88.73(7) . . ? Se5 Au2 Se4 90.95(7) . . ? Se3 Au2 Se6 90.93(7) . . ? Se5 Au2 Se6 89.39(7) . . ? Se4 Au2 Se6 179.57(7) . . ? C5 Se3 Au2 100.9(5) . . ? C11 Se4 Au2 102.2(5) . . ? C9 Se5 Au2 102.0(5) . . ? C6 Se6 Au2 101.7(5) . . ? N11 C5 C6 120.6(17) . . ? N11 C5 Se3 115.9(11) . . ? C6 C5 Se3 123.5(14) . . ? C8 N11 C5 116.8(16) . . ? N12 C6 C5 121.1(18) . . ? N12 C6 Se6 117.4(14) . . ? C5 C6 Se6 121.5(14) . . ? C6 N12 C7 117.5(16) . . ? N12 C7 C8 122(2) . . ? N11 C8 C7 122(2) . . ? N13 C9 C11 122.3(18) . . ? N13 C9 Se5 116.1(13) . . ? C11 C9 Se5 121.5(13) . . ? C9 N13 C10 116.5(17) . . ? N13 C10 C12 123(2) . . ? N14 C11 C9 118.3(16) . . ? N14 C11 Se4 119.1(12) . . ? C9 C11 Se4 122.7(13) . . ? C12 N14 C11 119.3(18) . . ? N14 C12 C10 121(2) . . ? C16 C13 S1 122.2(14) . . ? C16 C13 S2 122.0(13) . . ? S1 C13 S2 115.6(13) . . ? C13 S1 C14 95.4(10) . . ? C15 S2 C13 94.5(10) . . ? C15 C14 S1 118.5(16) . . ? C14 C15 S2 115.9(16) . . ? C13 C16 S4 122.4(13) . . ? C13 C16 S3 122.5(14) . . ? S4 C16 S3 115.1(11) . . ? C18 S3 C16 94.7(11) . . ? C16 S4 C17 95.3(10) . . ? C18 C17 S4 116.8(19) . . ? C17 C18 S3 118.0(19) . . ? C19 C19 S5 126(2) 3_566 . ? C19 C19 S6 118.6(19) 3_566 . ? S5 C19 S6 114.8(13) . . ? C19 S5 C20 96.8(11) . . ? C21 S6 C19 93.1(11) . . ? C21 C20 S5 116.1(19) . . ? C20 C21 S6 119.2(19) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 2.280 _refine_diff_density_min -1.366 _refine_diff_density_rms 0.299