# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Batail, Patrick' _publ_contact_author_email patrick.batail@univ-angers.fr _publ_section_title ; The Layered Topology of a Five Components Melaminium-Melamine Hybrid Salt of a Functional Gold(III) Dithiolene Complex ; loop_ _publ_author_name P.Batail A.Ranganathan A.El-Ghayoury L.Zorina # Attachment '1.cif' data_sad _database_code_depnum_ccdc_archive 'CCDC 764008' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'gold phosphonium' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H22 Au N2 O4 P S4' _chemical_formula_weight 854.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.901(1) _cell_length_b 11.972(1) _cell_length_c 13.205(1) _cell_angle_alpha 77.164(4) _cell_angle_beta 76.256(3) _cell_angle_gamma 74.665(4) _cell_volume 1590.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 400 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description hexagonal-shaped _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.784 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 4.977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.702 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KappaCCD' _diffrn_measurement_method 'combined \f-\w-scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44232 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5588 _reflns_number_gt 4503 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND 3.1 (Crystal Impact GbR 2005)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0105P)^2^+4.0050P] 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 5588 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.17280(2) 0.44587(2) 0.215255(17) 0.03495(8) Uani 1 1 d . . . S1 S 0.17669(16) 0.33006(13) 0.38248(11) 0.0428(4) Uani 1 1 d . . . S2 S 0.15085(16) 0.61690(13) 0.28108(11) 0.0423(4) Uani 1 1 d . . . S3 S 0.16435(16) 0.56166(13) 0.04859(11) 0.0450(4) Uani 1 1 d . . . S4 S 0.2026(2) 0.27379(14) 0.14882(12) 0.0583(5) Uani 1 1 d . . . O1 O 0.1981(4) 0.3287(3) 0.6268(3) 0.0495(11) Uani 1 1 d . . . O2 O 0.1733(4) 0.7161(4) 0.4873(3) 0.0521(11) Uani 1 1 d . . . O3 O 0.1631(4) 0.5568(4) -0.1993(3) 0.0507(11) Uani 1 1 d . . . O4 O 0.2047(7) 0.1682(4) -0.0605(3) 0.097(2) Uani 1 1 d . . . C1 C 0.1735(5) 0.4391(5) 0.4505(4) 0.0337(13) Uani 1 1 d . . . C2 C 0.1640(5) 0.5521(5) 0.4099(4) 0.0342(13) Uani 1 1 d . . . C3 C 0.1727(5) 0.6151(5) 0.4930(4) 0.0378(14) Uani 1 1 d . . . C4 C 0.1864(5) 0.4195(5) 0.5629(4) 0.0362(14) Uani 1 1 d . . . C5 C 0.1910(6) 0.3371(5) 0.0196(4) 0.0432(15) Uani 1 1 d . . . C6 C 0.1768(5) 0.4510(5) -0.0206(4) 0.0359(14) Uani 1 1 d . . . C7 C 0.1754(5) 0.4670(5) -0.1355(4) 0.0390(14) Uani 1 1 d . . . C8 C 0.1958(7) 0.2718(6) -0.0659(4) 0.0559(18) Uani 1 1 d . . . N1 N 0.1840(5) 0.5288(4) 0.5825(3) 0.0411(12) Uani 1 1 d . . . H1 H 0.1888 0.5420 0.6427 0.049 Uiso 1 1 calc R . . N2 N 0.1891(5) 0.3552(4) -0.1562(4) 0.0524(14) Uani 1 1 d . . . H2 H 0.1928 0.3399 -0.2177 0.063 Uiso 1 1 calc R . . P1 P 0.33961(14) 0.87187(13) 0.77545(11) 0.0339(3) Uani 1 1 d . . . C9 C 0.1957(5) 0.9295(5) 0.7191(4) 0.0334(13) Uani 1 1 d . . . C10 C 0.1202(6) 0.8558(5) 0.7147(5) 0.0516(16) Uani 1 1 d . . . H10 H 0.1411 0.7762 0.7426 0.062 Uiso 1 1 calc R . . C11 C 0.0118(6) 0.9027(6) 0.6679(5) 0.0611(19) Uani 1 1 d . . . H11 H -0.0398 0.8537 0.6639 0.073 Uiso 1 1 calc R . . C12 C -0.0199(6) 1.0205(6) 0.6275(5) 0.0502(17) Uani 1 1 d . . . H12 H -0.0919 1.0508 0.5956 0.060 Uiso 1 1 calc R . . C13 C 0.0535(6) 1.0918(6) 0.6344(5) 0.0501(16) Uani 1 1 d . . . H13 H 0.0306 1.1718 0.6087 0.060 Uiso 1 1 calc R . . C14 C 0.1617(6) 1.0479(5) 0.6788(4) 0.0451(15) Uani 1 1 d . . . H14 H 0.2125 1.0979 0.6819 0.054 Uiso 1 1 calc R . . C15 C 0.4044(5) 0.7230(5) 0.7551(5) 0.0412(14) Uani 1 1 d . . . C16 C 0.4204(7) 0.6968(6) 0.6551(5) 0.0624(19) Uani 1 1 d . . . H16 H 0.3963 0.7557 0.5998 0.075 Uiso 1 1 calc R . . C17 C 0.4726(7) 0.5821(8) 0.6381(8) 0.082(3) Uani 1 1 d . . . H17 H 0.4832 0.5637 0.5713 0.099 Uiso 1 1 calc R . . C18 C 0.5085(7) 0.4957(8) 0.7202(10) 0.092(3) Uani 1 1 d . . . H18 H 0.5430 0.4188 0.7086 0.110 Uiso 1 1 calc R . . C19 C 0.4946(7) 0.5208(6) 0.8162(8) 0.079(3) Uani 1 1 d . . . H19 H 0.5211 0.4616 0.8706 0.095 Uiso 1 1 calc R . . C20 C 0.4410(6) 0.6340(5) 0.8355(6) 0.0563(17) Uani 1 1 d . . . H20 H 0.4296 0.6502 0.9032 0.068 Uiso 1 1 calc R . . C21 C 0.3032(6) 0.8777(5) 0.9136(4) 0.0397(14) Uani 1 1 d . . . C22 C 0.1791(7) 0.8812(5) 0.9717(5) 0.0539(17) Uani 1 1 d . . . H22 H 0.1126 0.8807 0.9390 0.065 Uiso 1 1 calc R . . C23 C 0.1543(8) 0.8854(6) 1.0793(5) 0.070(2) Uani 1 1 d . . . H23 H 0.0708 0.8890 1.1185 0.085 Uiso 1 1 calc R . . C24 C 0.2511(11) 0.8844(7) 1.1267(6) 0.088(3) Uani 1 1 d . . . H24 H 0.2333 0.8877 1.1985 0.105 Uiso 1 1 calc R . . C25 C 0.3742(10) 0.8786(8) 1.0720(6) 0.091(3) Uani 1 1 d . . . H25 H 0.4398 0.8767 1.1067 0.110 Uiso 1 1 calc R . . C26 C 0.4024(7) 0.8754(6) 0.9638(5) 0.067(2) Uani 1 1 d . . . H26 H 0.4866 0.8718 0.9259 0.080 Uiso 1 1 calc R . . C27 C 0.4557(5) 0.9610(5) 0.7126(4) 0.0371(13) Uani 1 1 d . . . C28 C 0.5615(6) 0.9234(6) 0.6385(5) 0.0545(17) Uani 1 1 d . . . H28 H 0.5774 0.8487 0.6220 0.065 Uiso 1 1 calc R . . C29 C 0.6447(7) 0.9970(8) 0.5882(6) 0.076(2) Uani 1 1 d . . . H29 H 0.7175 0.9715 0.5387 0.092 Uiso 1 1 calc R . . C30 C 0.6193(8) 1.1078(8) 0.6120(6) 0.076(2) Uani 1 1 d . . . H30 H 0.6753 1.1572 0.5782 0.091 Uiso 1 1 calc R . . C31 C 0.5133(8) 1.1464(6) 0.6843(6) 0.071(2) Uani 1 1 d . . . H31 H 0.4959 1.2225 0.6982 0.085 Uiso 1 1 calc R . . C32 C 0.4310(6) 1.0725(5) 0.7374(5) 0.0503(16) Uani 1 1 d . . . H32 H 0.3603 1.0973 0.7889 0.060 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 0.04113(13) 0.03337(13) 0.02791(11) -0.00439(8) -0.00490(8) -0.00632(9) S1 0.0645(11) 0.0301(9) 0.0343(8) -0.0052(6) -0.0096(7) -0.0117(8) S2 0.0585(11) 0.0316(9) 0.0346(8) -0.0010(7) -0.0138(7) -0.0058(8) S3 0.0700(11) 0.0351(9) 0.0317(8) -0.0029(7) -0.0126(7) -0.0148(8) S4 0.1028(15) 0.0348(10) 0.0308(8) -0.0034(7) -0.0089(9) -0.0094(10) O1 0.079(3) 0.034(3) 0.035(2) 0.0004(19) -0.015(2) -0.015(2) O2 0.078(3) 0.035(3) 0.052(3) -0.006(2) -0.022(2) -0.020(2) O3 0.078(3) 0.038(3) 0.038(2) -0.001(2) -0.019(2) -0.013(2) O4 0.206(7) 0.030(3) 0.047(3) -0.006(2) -0.020(3) -0.016(3) C1 0.034(3) 0.037(4) 0.028(3) -0.007(3) -0.004(2) -0.004(3) C2 0.037(3) 0.035(4) 0.030(3) -0.005(3) -0.005(2) -0.009(3) C3 0.038(3) 0.036(4) 0.042(3) -0.010(3) -0.007(3) -0.009(3) C4 0.040(4) 0.029(4) 0.039(3) -0.008(3) -0.005(3) -0.006(3) C5 0.058(4) 0.036(4) 0.031(3) -0.009(3) -0.003(3) -0.004(3) C6 0.047(4) 0.034(4) 0.027(3) -0.003(3) -0.008(3) -0.010(3) C7 0.042(4) 0.039(4) 0.035(3) -0.004(3) -0.008(3) -0.010(3) C8 0.090(5) 0.038(4) 0.034(3) -0.005(3) -0.008(3) -0.008(4) N1 0.064(3) 0.035(3) 0.031(3) -0.003(2) -0.019(2) -0.016(3) N2 0.086(4) 0.038(3) 0.031(3) -0.012(2) -0.007(3) -0.008(3) P1 0.0383(9) 0.0311(9) 0.0319(8) -0.0040(6) -0.0070(6) -0.0080(7) C9 0.036(4) 0.028(3) 0.036(3) -0.008(2) -0.004(2) -0.007(3) C10 0.056(4) 0.038(4) 0.067(4) 0.001(3) -0.022(3) -0.021(3) C11 0.055(4) 0.064(5) 0.077(5) -0.008(4) -0.020(4) -0.032(4) C12 0.042(4) 0.058(5) 0.051(4) -0.008(3) -0.022(3) -0.003(3) C13 0.045(4) 0.042(4) 0.059(4) -0.006(3) -0.015(3) 0.001(3) C14 0.051(4) 0.031(4) 0.055(4) -0.011(3) -0.015(3) -0.005(3) C15 0.040(4) 0.029(3) 0.055(4) -0.009(3) -0.015(3) -0.003(3) C16 0.068(5) 0.056(5) 0.069(5) -0.027(4) -0.021(4) -0.003(4) C17 0.065(5) 0.084(7) 0.111(7) -0.066(6) -0.003(5) -0.009(5) C18 0.042(5) 0.044(5) 0.197(11) -0.053(7) -0.016(6) -0.002(4) C19 0.064(5) 0.031(5) 0.144(8) -0.005(5) -0.041(5) -0.002(4) C20 0.047(4) 0.042(4) 0.079(5) -0.002(3) -0.018(3) -0.009(3) C21 0.049(4) 0.032(3) 0.034(3) -0.001(2) -0.002(3) -0.010(3) C22 0.065(5) 0.045(4) 0.047(4) -0.001(3) -0.009(3) -0.011(3) C23 0.083(6) 0.062(5) 0.047(4) -0.002(3) 0.012(4) -0.010(4) C24 0.133(9) 0.088(6) 0.040(4) -0.012(4) -0.005(5) -0.027(6) C25 0.129(8) 0.121(8) 0.042(4) 0.003(4) -0.038(5) -0.051(6) C26 0.081(5) 0.088(6) 0.041(4) -0.003(4) -0.013(4) -0.039(4) C27 0.041(3) 0.039(4) 0.034(3) -0.001(3) -0.012(3) -0.014(3) C28 0.044(4) 0.056(4) 0.058(4) -0.010(3) 0.001(3) -0.008(3) C29 0.052(5) 0.099(7) 0.069(5) -0.003(5) 0.005(4) -0.027(5) C30 0.059(5) 0.095(7) 0.074(5) 0.032(5) -0.025(4) -0.044(5) C31 0.087(6) 0.053(5) 0.088(5) 0.001(4) -0.036(5) -0.035(5) C32 0.053(4) 0.053(4) 0.051(4) -0.011(3) -0.007(3) -0.023(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S4 2.3309(17) . ? Au1 S2 2.3321(15) . ? Au1 S3 2.3339(14) . ? Au1 S1 2.3352(14) . ? S1 C1 1.730(5) . ? S2 C2 1.728(5) . ? S3 C6 1.730(5) . ? S4 C5 1.726(6) . ? O1 C4 1.216(6) . ? O2 C3 1.197(6) . ? O3 C7 1.208(6) . ? O4 C8 1.206(7) . ? C1 C2 1.327(7) . ? C1 C4 1.486(7) . ? C2 C3 1.495(7) . ? C3 N1 1.392(7) . ? C4 N1 1.382(7) . ? C5 C6 1.331(7) . ? C5 C8 1.493(8) . ? C6 C7 1.490(7) . ? C7 N2 1.388(7) . ? C8 N2 1.378(7) . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? P1 C21 1.786(5) . ? P1 C15 1.790(6) . ? P1 C9 1.801(5) . ? P1 C27 1.803(5) . ? C9 C10 1.375(7) . ? C9 C14 1.382(7) . ? C10 C11 1.391(8) . ? C10 H10 0.9300 . ? C11 C12 1.374(8) . ? C11 H11 0.9300 . ? C12 C13 1.345(8) . ? C12 H12 0.9300 . ? C13 C14 1.369(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C20 1.377(8) . ? C15 C16 1.385(8) . ? C16 C17 1.386(10) . ? C16 H16 0.9300 . ? C17 C18 1.375(12) . ? C17 H17 0.9300 . ? C18 C19 1.331(12) . ? C18 H18 0.9300 . ? C19 C20 1.382(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.382(8) . ? C21 C26 1.389(8) . ? C22 C23 1.392(9) . ? C22 H22 0.9300 . ? C23 C24 1.344(11) . ? C23 H23 0.9300 . ? C24 C25 1.356(11) . ? C24 H24 0.9300 . ? C25 C26 1.395(9) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.369(8) . ? C27 C32 1.387(8) . ? C28 C29 1.385(9) . ? C28 H28 0.9300 . ? C29 C30 1.373(11) . ? C29 H29 0.9300 . ? C30 C31 1.360(10) . ? C30 H30 0.9300 . ? C31 C32 1.388(9) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? 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 S4 Au1 S2 178.00(7) . . ? S4 Au1 S3 92.10(5) . . ? S2 Au1 S3 88.08(5) . . ? S4 Au1 S1 87.77(5) . . ? S2 Au1 S1 92.09(5) . . ? S3 Au1 S1 178.81(7) . . ? C1 S1 Au1 97.89(18) . . ? C2 S2 Au1 97.69(19) . . ? C6 S3 Au1 97.95(18) . . ? C5 S4 Au1 97.9(2) . . ? C2 C1 C4 109.3(5) . . ? C2 C1 S1 125.6(4) . . ? C4 C1 S1 125.0(4) . . ? C1 C2 C3 108.7(5) . . ? C1 C2 S2 126.4(4) . . ? C3 C2 S2 124.8(4) . . ? O2 C3 N1 125.3(5) . . ? O2 C3 C2 129.8(5) . . ? N1 C3 C2 104.9(5) . . ? O1 C4 N1 125.3(5) . . ? O1 C4 C1 129.4(5) . . ? N1 C4 C1 105.3(5) . . ? C6 C5 C8 108.8(5) . . ? C6 C5 S4 126.1(4) . . ? C8 C5 S4 125.1(5) . . ? C5 C6 C7 108.5(5) . . ? C5 C6 S3 125.7(4) . . ? C7 C6 S3 125.7(4) . . ? O3 C7 N2 125.5(5) . . ? O3 C7 C6 128.8(5) . . ? N2 C7 C6 105.6(5) . . ? O4 C8 N2 125.5(6) . . ? O4 C8 C5 128.9(6) . . ? N2 C8 C5 105.6(5) . . ? C4 N1 C3 111.8(4) . . ? C4 N1 H1 124.1 . . ? C3 N1 H1 124.1 . . ? C8 N2 C7 111.4(5) . . ? C8 N2 H2 124.3 . . ? C7 N2 H2 124.3 . . ? C21 P1 C15 109.9(3) . . ? C21 P1 C9 110.6(3) . . ? C15 P1 C9 108.9(3) . . ? C21 P1 C27 107.8(3) . . ? C15 P1 C27 110.6(3) . . ? C9 P1 C27 109.1(2) . . ? C10 C9 C14 119.7(5) . . ? C10 C9 P1 120.2(4) . . ? C14 C9 P1 120.1(4) . . ? C9 C10 C11 118.7(6) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 120.8(6) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 119.8(6) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.7(6) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C9 120.3(6) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? C20 C15 C16 118.9(6) . . ? C20 C15 P1 122.0(5) . . ? C16 C15 P1 119.1(5) . . ? C15 C16 C17 119.5(7) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 119.8(8) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 120.8(8) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 120.4(8) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C15 C20 C19 120.4(7) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C22 C21 C26 119.6(6) . . ? C22 C21 P1 121.2(5) . . ? C26 C21 P1 119.1(5) . . ? C21 C22 C23 119.7(6) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C24 C23 C22 120.1(7) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 121.5(7) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C26 120.1(8) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 119.1(7) . . ? C21 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C28 C27 C32 120.5(5) . . ? C28 C27 P1 121.7(5) . . ? C32 C27 P1 117.8(4) . . ? C27 C28 C29 119.8(7) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C30 C29 C28 119.6(7) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 120.9(7) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C30 C31 C32 120.1(7) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C27 C32 C31 119.1(6) . . ? C27 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.630 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.113 data_c_ _database_code_depnum_ccdc_archive 'CCDC 764009' #TrackingRef '21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'gold(iii) bis(4,5-diamido-2-oxo-1,3-dithiolate) melaminium' _chemical_melting_point ? _chemical_formula_moiety 'C8 H2 Au N2 O4 S4, C3 H7 N6, C3 H6 N6, 2(C3 H7 N O), 2(H2 O)' _chemical_formula_sum 'C20 H33 Au N16 O8 S4' _chemical_formula_weight 950.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0130(10) _cell_length_b 13.0590(10) _cell_length_c 17.0873(16) _cell_angle_alpha 101.236(8) _cell_angle_beta 96.662(7) _cell_angle_gamma 100.106(6) _cell_volume 1705.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 34822 _cell_measurement_theta_min 3 _cell_measurement_theta_max 35 _exptl_crystal_description parallelogram-shaped _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 4.626 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.242 _exptl_absorpt_correction_T_max 0.600 _exptl_absorpt_process_details 'SADABS (Sheldrick, Bruker, 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker KappaCCD' _diffrn_measurement_method 'combined \f-\w-scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 69722 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0365 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 35.02 _reflns_number_total 14794 _reflns_number_gt 11334 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.1 (Crystal Impact GbR 2005)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), enCIFer: a program for viewing, editing and visualising CIFs (F. H. Allen et al., 2004) ; _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^ > 2\s(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^)+(0.0163P)^2^+1.1736P] 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 14794 _refine_ls_number_parameters 461 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0553 _refine_ls_wR_factor_gt 0.0500 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.718891(11) 0.335564(7) 0.049391(5) 0.02675(2) Uani 1 1 d . . . S1 S 0.81403(9) 0.22881(5) -0.05535(3) 0.03606(13) Uani 1 1 d . . . S2 S 0.74359(9) 0.47892(5) -0.01366(3) 0.03786(14) Uani 1 1 d . . . S3 S 0.68589(8) 0.19176(5) 0.11141(3) 0.03549(13) Uani 1 1 d . . . S4 S 0.61860(9) 0.44100(5) 0.15199(4) 0.04103(15) Uani 1 1 d . . . C1 C 0.8502(3) 0.32175(17) -0.11391(12) 0.0278(4) Uani 1 1 d . . . C2 C 0.8233(3) 0.42145(17) -0.09687(12) 0.0283(4) Uani 1 1 d . . . C3 C 0.5945(3) 0.24707(17) 0.19126(12) 0.0288(4) Uani 1 1 d . . . C4 C 0.5701(3) 0.34751(18) 0.20869(12) 0.0297(4) Uani 1 1 d . . . C5 C 0.9167(3) 0.30447(18) -0.19188(12) 0.0301(4) Uani 1 1 d . . . C6 C 0.8715(3) 0.47435(17) -0.16267(13) 0.0304(4) Uani 1 1 d . . . C7 C 0.5302(3) 0.19132(19) 0.25319(13) 0.0334(5) Uani 1 1 d . . . C8 C 0.4908(3) 0.3627(2) 0.28379(13) 0.0347(5) Uani 1 1 d . . . O1 O 0.9561(2) 0.22505(14) -0.22808(10) 0.0429(4) Uani 1 1 d . . . O2 O 0.8657(3) 0.56465(14) -0.16853(10) 0.0436(4) Uani 1 1 d . . . O3 O 0.5299(3) 0.10081(15) 0.25928(11) 0.0496(5) Uani 1 1 d . . . O4 O 0.4546(3) 0.44242(15) 0.32136(11) 0.0520(5) Uani 1 1 d . . . N1 N 0.9256(3) 0.39922(15) -0.21769(11) 0.0354(4) Uani 1 1 d . . . H1 H 0.9600 0.4099 -0.2618 0.042 Uiso 1 1 calc R . . N2 N 0.4677(3) 0.26546(16) 0.30515(12) 0.0397(5) Uani 1 1 d . . . H2 H 0.4204 0.2524 0.3458 0.048 Uiso 1 1 calc R . . N11 N 0.3468(3) 0.22812(15) 0.44723(11) 0.0334(4) Uani 1 1 d . . . C12 C 0.2826(3) 0.30097(17) 0.49514(13) 0.0295(4) Uani 1 1 d . . . N12 N 0.3111(3) 0.39973(16) 0.48241(13) 0.0432(5) Uani 1 1 d . . . H12A H 0.2722 0.4489 0.5116 0.052 Uiso 1 1 calc R . . H12B H 0.3683 0.4142 0.4450 0.052 Uiso 1 1 calc R . . N13 N 0.2281(2) 0.10073(14) 0.51886(10) 0.0278(4) Uani 1 1 d . . . C14 C 0.1688(3) 0.17982(17) 0.56266(12) 0.0272(4) Uani 1 1 d . . . N14 N 0.0778(3) 0.15484(16) 0.61894(12) 0.0377(5) Uani 1 1 d . . . H14B H 0.0594 0.0906 0.6259 0.045 Uiso 1 1 calc R . . H14A H 0.0373 0.2029 0.6484 0.045 Uiso 1 1 calc R . . N15 N 0.1929(2) 0.28147(15) 0.55397(11) 0.0305(4) Uani 1 1 d . . . C16 C 0.3149(3) 0.12903(17) 0.46148(12) 0.0284(4) Uani 1 1 d . . . N16 N 0.3733(3) 0.05409(16) 0.41412(12) 0.0409(5) Uani 1 1 d . . . H16A H 0.3548 -0.0103 0.4209 0.049 Uiso 1 1 calc R . . H16B H 0.4296 0.0700 0.3768 0.049 Uiso 1 1 calc R . . N21 N 1.0284(2) 0.18421(15) 0.26265(11) 0.0318(4) Uani 1 1 d . . . H21 H 1.0747 0.1988 0.2221 0.038 Uiso 1 1 calc R . . C22 C 0.9748(3) 0.26134(17) 0.31355(13) 0.0286(4) Uani 1 1 d . . . N22 N 0.9996(3) 0.35779(16) 0.29942(12) 0.0397(5) Uani 1 1 d . . . H22A H 0.9675 0.4083 0.3306 0.048 Uiso 1 1 calc R . . H22B H 1.0480 0.3704 0.2590 0.048 Uiso 1 1 calc R . . N23 N 0.9005(2) 0.24011(14) 0.37551(11) 0.0300(4) Uani 1 1 d . . . C24 C 0.8835(3) 0.13837(17) 0.38500(12) 0.0270(4) Uani 1 1 d . . . N24 N 0.8083(3) 0.11398(16) 0.44562(11) 0.0352(4) Uani 1 1 d . . . H24A H 0.7956 0.0501 0.4533 0.042 Uiso 1 1 calc R . . H24B H 0.7720 0.1620 0.4774 0.042 Uiso 1 1 calc R . . N25 N 0.9374(2) 0.05890(14) 0.33753(11) 0.0299(4) Uani 1 1 d . . . C26 C 1.0082(3) 0.08381(17) 0.27626(13) 0.0286(4) Uani 1 1 d . . . N26 N 1.0645(3) 0.01256(17) 0.22541(12) 0.0424(5) Uani 1 1 d . . . H26A H 1.0552 -0.0517 0.2320 0.051 Uiso 1 1 calc R . . H26B H 1.1104 0.0305 0.1857 0.051 Uiso 1 1 calc R . . O31 O 0.6609(3) 0.18537(17) 0.59687(12) 0.0523(5) Uani 1 1 d . . . C31 C 0.5999(3) 0.2517(2) 0.63937(15) 0.0407(5) Uani 1 1 d . . . H31 H 0.6100 0.3185 0.6269 0.049 Uiso 1 1 calc R . . N31 N 0.5210(3) 0.23685(16) 0.70137(12) 0.0369(4) Uani 1 1 d . . . C32 C 0.4976(4) 0.1346(2) 0.72391(18) 0.0518(7) Uani 1 1 d . . . H32A H 0.4810 0.1440 0.7794 0.078 Uiso 1 1 calc R . . H32B H 0.5975 0.1047 0.7171 0.078 Uiso 1 1 calc R . . H32C H 0.3989 0.0874 0.6902 0.078 Uiso 1 1 calc R . . C33 C 0.4492(4) 0.3200(2) 0.74698(17) 0.0483(6) Uani 1 1 d . . . H33A H 0.4741 0.3835 0.7265 0.072 Uiso 1 1 calc R . . H33B H 0.4988 0.3348 0.8029 0.072 Uiso 1 1 calc R . . H33C H 0.3271 0.2967 0.7417 0.072 Uiso 1 1 calc R . . O41 O 0.1703(3) 0.16367(17) 0.12729(12) 0.0522(5) Uani 1 1 d . . . C41 C 0.2021(3) 0.2084(2) 0.07196(14) 0.0372(5) Uani 1 1 d . . . H41 H 0.1969 0.2802 0.0792 0.045 Uiso 1 1 calc R . . N41 N 0.2428(3) 0.16210(17) 0.00352(12) 0.0376(4) Uani 1 1 d . . . C42 C 0.2542(5) 0.0509(3) -0.0126(2) 0.0681(9) Uani 1 1 d . . . H42A H 0.3490 0.0415 -0.0410 0.102 Uiso 1 1 calc R . . H42B H 0.1499 0.0088 -0.0451 0.102 Uiso 1 1 calc R . . H42C H 0.2715 0.0285 0.0375 0.102 Uiso 1 1 calc R . . C43 C 0.2757(4) 0.2193(3) -0.05972(17) 0.0539(7) Uani 1 1 d . . . H43A H 0.1908 0.1883 -0.1067 0.081 Uiso 1 1 calc R . . H43B H 0.3876 0.2147 -0.0731 0.081 Uiso 1 1 calc R . . H43C H 0.2705 0.2928 -0.0411 0.081 Uiso 1 1 calc R . . O51 O 0.0061(3) 0.42548(16) 0.62619(12) 0.0474(5) Uani 1 1 d D . . H51A H -0.074(4) 0.417(3) 0.5892(17) 0.071 Uiso 1 1 d D . . H51B H 0.081(4) 0.393(3) 0.614(2) 0.071 Uiso 1 1 d D . . O52 O 0.2526(3) 0.62462(18) 0.51460(13) 0.0541(5) Uani 1 1 d D . . H52A H 0.199(4) 0.655(3) 0.5460(19) 0.081 Uiso 1 1 d D . . H52B H 0.349(3) 0.659(3) 0.518(2) 0.081 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03520(4) 0.02763(4) 0.02141(3) 0.00775(3) 0.01240(3) 0.00911(3) S1 0.0585(4) 0.0305(3) 0.0295(3) 0.0125(2) 0.0231(3) 0.0191(3) S2 0.0634(4) 0.0290(3) 0.0308(3) 0.0108(2) 0.0259(3) 0.0182(3) S3 0.0563(4) 0.0289(3) 0.0295(3) 0.0108(2) 0.0198(2) 0.0171(3) S4 0.0711(4) 0.0287(3) 0.0354(3) 0.0137(2) 0.0324(3) 0.0193(3) C1 0.0349(11) 0.0294(11) 0.0220(9) 0.0079(8) 0.0113(8) 0.0075(9) C2 0.0379(11) 0.0268(10) 0.0231(9) 0.0071(8) 0.0129(8) 0.0067(9) C3 0.0368(11) 0.0302(11) 0.0232(9) 0.0095(8) 0.0115(8) 0.0083(9) C4 0.0391(12) 0.0299(11) 0.0237(9) 0.0077(8) 0.0143(8) 0.0085(9) C5 0.0378(12) 0.0312(11) 0.0232(9) 0.0060(8) 0.0122(8) 0.0079(9) C6 0.0388(12) 0.0280(11) 0.0264(10) 0.0079(8) 0.0129(9) 0.0052(9) C7 0.0424(13) 0.0339(12) 0.0265(10) 0.0121(9) 0.0110(9) 0.0052(10) C8 0.0437(13) 0.0379(12) 0.0271(10) 0.0101(9) 0.0168(9) 0.0104(10) O1 0.0647(12) 0.0392(10) 0.0336(9) 0.0084(7) 0.0260(8) 0.0214(9) O2 0.0688(12) 0.0308(9) 0.0397(9) 0.0155(7) 0.0257(9) 0.0127(8) O3 0.0783(14) 0.0339(10) 0.0454(10) 0.0200(8) 0.0246(10) 0.0128(9) O4 0.0835(14) 0.0440(11) 0.0423(10) 0.0147(8) 0.0374(10) 0.0259(10) N1 0.0530(12) 0.0319(10) 0.0260(9) 0.0091(7) 0.0212(8) 0.0084(9) N2 0.0594(13) 0.0372(11) 0.0312(10) 0.0152(8) 0.0257(9) 0.0119(10) N11 0.0490(11) 0.0284(9) 0.0324(9) 0.0136(7) 0.0240(8) 0.0142(8) C12 0.0363(11) 0.0275(10) 0.0280(10) 0.0091(8) 0.0105(8) 0.0086(9) N12 0.0661(14) 0.0271(10) 0.0467(12) 0.0146(9) 0.0299(11) 0.0159(10) N13 0.0364(10) 0.0252(8) 0.0273(8) 0.0093(7) 0.0153(7) 0.0101(7) C14 0.0327(11) 0.0306(10) 0.0223(9) 0.0084(8) 0.0110(8) 0.0095(8) N14 0.0546(12) 0.0335(10) 0.0352(10) 0.0132(8) 0.0293(9) 0.0154(9) N15 0.0407(10) 0.0286(9) 0.0280(9) 0.0091(7) 0.0162(8) 0.0126(8) C16 0.0340(11) 0.0302(10) 0.0259(9) 0.0091(8) 0.0136(8) 0.0108(9) N16 0.0629(14) 0.0298(10) 0.0417(11) 0.0128(8) 0.0351(10) 0.0177(9) N21 0.0407(10) 0.0313(10) 0.0270(9) 0.0112(7) 0.0142(8) 0.0057(8) C22 0.0315(11) 0.0278(10) 0.0273(10) 0.0086(8) 0.0069(8) 0.0038(8) N22 0.0608(14) 0.0279(10) 0.0361(10) 0.0132(8) 0.0216(10) 0.0077(9) N23 0.0374(10) 0.0262(9) 0.0296(9) 0.0091(7) 0.0139(7) 0.0061(7) C24 0.0284(10) 0.0279(10) 0.0264(9) 0.0095(8) 0.0075(8) 0.0046(8) N24 0.0467(11) 0.0310(10) 0.0363(10) 0.0143(8) 0.0229(9) 0.0113(8) N25 0.0369(10) 0.0268(9) 0.0297(9) 0.0098(7) 0.0127(7) 0.0075(7) C26 0.0319(11) 0.0294(11) 0.0263(10) 0.0083(8) 0.0081(8) 0.0063(8) N26 0.0658(14) 0.0335(11) 0.0368(11) 0.0110(8) 0.0265(10) 0.0175(10) O31 0.0603(12) 0.0545(12) 0.0454(11) 0.0062(9) 0.0251(9) 0.0148(10) C31 0.0471(14) 0.0361(13) 0.0389(13) 0.0092(10) 0.0095(11) 0.0053(11) N31 0.0454(11) 0.0291(10) 0.0377(10) 0.0048(8) 0.0132(9) 0.0098(8) C32 0.0685(19) 0.0378(14) 0.0547(17) 0.0149(12) 0.0236(14) 0.0112(13) C33 0.0558(17) 0.0393(14) 0.0497(15) -0.0016(12) 0.0146(13) 0.0175(13) O41 0.0670(13) 0.0574(12) 0.0433(10) 0.0199(9) 0.0280(9) 0.0200(10) C41 0.0444(13) 0.0356(12) 0.0344(12) 0.0068(10) 0.0135(10) 0.0122(10) N41 0.0456(12) 0.0385(11) 0.0318(10) 0.0052(8) 0.0125(8) 0.0154(9) C42 0.088(3) 0.0407(17) 0.074(2) -0.0036(15) 0.0173(19) 0.0256(17) C43 0.0613(18) 0.070(2) 0.0353(13) 0.0161(13) 0.0178(13) 0.0142(15) O51 0.0661(14) 0.0425(11) 0.0413(10) 0.0080(8) 0.0253(9) 0.0225(10) O52 0.0658(14) 0.0485(12) 0.0533(12) 0.0066(10) 0.0228(11) 0.0221(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 S3 2.3207(6) . ? Au1 S4 2.3215(6) . ? Au1 S2 2.3260(6) . ? Au1 S1 2.3335(6) . ? S1 C1 1.725(2) . ? S2 C2 1.719(2) . ? S3 C3 1.718(2) . ? S4 C4 1.721(2) . ? C1 C2 1.338(3) . ? C1 C5 1.483(3) . ? C2 C6 1.483(3) . ? C3 C4 1.341(3) . ? C3 C7 1.487(3) . ? C4 C8 1.491(3) . ? C5 O1 1.212(3) . ? C5 N1 1.385(3) . ? C6 O2 1.211(3) . ? C6 N1 1.385(3) . ? C7 O3 1.206(3) . ? C7 N2 1.383(3) . ? C8 O4 1.212(3) . ? C8 N2 1.377(3) . ? N1 H1 0.8600 . ? N2 H2 0.8600 . ? N11 C12 1.344(3) . ? N11 C16 1.349(3) . ? C12 N12 1.334(3) . ? C12 N15 1.340(3) . ? N12 H12A 0.8600 . ? N12 H12B 0.8600 . ? N13 C16 1.339(2) . ? N13 C14 1.344(3) . ? C14 N14 1.328(2) . ? C14 N15 1.347(3) . ? N14 H14B 0.8600 . ? N14 H14A 0.8600 . ? C16 N16 1.331(3) . ? N16 H16A 0.8600 . ? N16 H16B 0.8600 . ? N21 C22 1.361(3) . ? N21 C26 1.361(3) . ? N21 H21 0.8600 . ? C22 N22 1.314(3) . ? C22 N23 1.325(3) . ? N22 H22A 0.8600 . ? N22 H22B 0.8600 . ? N23 C24 1.355(3) . ? C24 N24 1.320(3) . ? C24 N25 1.353(3) . ? N24 H24A 0.8600 . ? N24 H24B 0.8600 . ? N25 C26 1.315(3) . ? C26 N26 1.322(3) . ? N26 H26A 0.8600 . ? N26 H26B 0.8600 . ? O31 C31 1.225(3) . ? C31 N31 1.324(3) . ? C31 H31 0.9300 . ? N31 C32 1.447(3) . ? N31 C33 1.453(3) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? O41 C41 1.233(3) . ? C41 N41 1.312(3) . ? C41 H41 0.9300 . ? N41 C42 1.446(4) . ? N41 C43 1.452(3) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? O51 H51A 0.82(2) . ? O51 H51B 0.82(2) . ? O52 H52A 0.81(2) . ? O52 H52B 0.81(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 S3 Au1 S4 92.20(2) . . ? S3 Au1 S2 178.38(2) . . ? S4 Au1 S2 87.30(2) . . ? S3 Au1 S1 87.98(2) . . ? S4 Au1 S1 178.80(3) . . ? S2 Au1 S1 92.49(2) . . ? C1 S1 Au1 97.55(7) . . ? C2 S2 Au1 97.80(7) . . ? C3 S3 Au1 98.03(7) . . ? C4 S4 Au1 98.32(7) . . ? C2 C1 C5 108.42(18) . . ? C2 C1 S1 125.97(15) . . ? C5 C1 S1 125.60(16) . . ? C1 C2 C6 108.56(17) . . ? C1 C2 S2 126.13(16) . . ? C6 C2 S2 125.31(16) . . ? C4 C3 C7 108.47(18) . . ? C4 C3 S3 126.04(16) . . ? C7 C3 S3 125.49(17) . . ? C3 C4 C8 108.41(18) . . ? C3 C4 S4 125.21(15) . . ? C8 C4 S4 126.37(17) . . ? O1 C5 N1 124.99(19) . . ? O1 C5 C1 128.8(2) . . ? N1 C5 C1 106.20(18) . . ? O2 C6 N1 125.91(19) . . ? O2 C6 C2 128.0(2) . . ? N1 C6 C2 106.12(18) . . ? O3 C7 N2 125.2(2) . . ? O3 C7 C3 129.0(2) . . ? N2 C7 C3 105.71(19) . . ? O4 C8 N2 124.9(2) . . ? O4 C8 C4 129.4(2) . . ? N2 C8 C4 105.72(19) . . ? C6 N1 C5 110.70(17) . . ? C6 N1 H1 124.6 . . ? C5 N1 H1 124.6 . . ? C8 N2 C7 111.64(17) . . ? C8 N2 H2 124.2 . . ? C7 N2 H2 124.2 . . ? C12 N11 C16 115.28(17) . . ? N12 C12 N15 118.27(19) . . ? N12 C12 N11 116.84(19) . . ? N15 C12 N11 124.89(19) . . ? C12 N12 H12A 120.0 . . ? C12 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C16 N13 C14 114.62(17) . . ? N14 C14 N13 116.79(19) . . ? N14 C14 N15 117.58(19) . . ? N13 C14 N15 125.63(17) . . ? C14 N14 H14B 120.0 . . ? C14 N14 H14A 120.0 . . ? H14B N14 H14A 120.0 . . ? C12 N15 C14 114.65(17) . . ? N16 C16 N13 118.01(19) . . ? N16 C16 N11 117.08(18) . . ? N13 C16 N11 124.91(19) . . ? C16 N16 H16A 120.0 . . ? C16 N16 H16B 120.0 . . ? H16A N16 H16B 120.0 . . ? C22 N21 C26 119.58(17) . . ? C22 N21 H21 120.2 . . ? C26 N21 H21 120.2 . . ? N22 C22 N23 121.0(2) . . ? N22 C22 N21 117.83(19) . . ? N23 C22 N21 121.18(19) . . ? C22 N22 H22A 120.0 . . ? C22 N22 H22B 120.0 . . ? H22A N22 H22B 120.0 . . ? C22 N23 C24 115.98(18) . . ? N24 C24 N25 116.76(19) . . ? N24 C24 N23 117.67(19) . . ? N25 C24 N23 125.57(18) . . ? C24 N24 H24A 120.0 . . ? C24 N24 H24B 120.0 . . ? H24A N24 H24B 120.0 . . ? C26 N25 C24 116.01(18) . . ? N25 C26 N26 121.5(2) . . ? N25 C26 N21 121.65(19) . . ? N26 C26 N21 116.89(19) . . ? C26 N26 H26A 120.0 . . ? C26 N26 H26B 120.0 . . ? H26A N26 H26B 120.0 . . ? O31 C31 N31 126.0(2) . . ? O31 C31 H31 117.0 . . ? N31 C31 H31 117.0 . . ? C31 N31 C32 120.5(2) . . ? C31 N31 C33 121.8(2) . . ? C32 N31 C33 117.7(2) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O41 C41 N41 124.7(2) . . ? O41 C41 H41 117.6 . . ? N41 C41 H41 117.6 . . ? C41 N41 C42 121.2(2) . . ? C41 N41 C43 121.8(2) . . ? C42 N41 C43 117.0(2) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N41 C43 H43A 109.5 . . ? N41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? H51A O51 H51B 114(4) . . ? H52A O52 H52B 111(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 S3 Au1 S1 C1 -179.95(8) . . . . ? S2 Au1 S1 C1 1.59(8) . . . . ? S4 Au1 S2 C2 179.23(8) . . . . ? S1 Au1 S2 C2 -1.95(8) . . . . ? S4 Au1 S3 C3 3.85(8) . . . . ? S1 Au1 S3 C3 -174.97(8) . . . . ? S3 Au1 S4 C4 -3.01(9) . . . . ? S2 Au1 S4 C4 175.45(9) . . . . ? Au1 S1 C1 C2 -0.8(2) . . . . ? Au1 S1 C1 C5 179.15(19) . . . . ? C5 C1 C2 C6 -0.2(3) . . . . ? S1 C1 C2 C6 179.77(17) . . . . ? C5 C1 C2 S2 178.95(17) . . . . ? S1 C1 C2 S2 -1.1(3) . . . . ? Au1 S2 C2 C1 2.2(2) . . . . ? Au1 S2 C2 C6 -178.77(19) . . . . ? Au1 S3 C3 C4 -4.6(2) . . . . ? Au1 S3 C3 C7 175.89(19) . . . . ? C7 C3 C4 C8 0.8(3) . . . . ? S3 C3 C4 C8 -178.73(18) . . . . ? C7 C3 C4 S4 -177.86(18) . . . . ? S3 C3 C4 S4 2.6(3) . . . . ? Au1 S4 C4 C3 1.3(2) . . . . ? Au1 S4 C4 C8 -177.2(2) . . . . ? C2 C1 C5 O1 -179.7(3) . . . . ? S1 C1 C5 O1 0.3(4) . . . . ? C2 C1 C5 N1 -0.1(3) . . . . ? S1 C1 C5 N1 179.97(17) . . . . ? C1 C2 C6 O2 -179.7(2) . . . . ? S2 C2 C6 O2 1.1(4) . . . . ? C1 C2 C6 N1 0.4(3) . . . . ? S2 C2 C6 N1 -178.76(17) . . . . ? C4 C3 C7 O3 -179.4(3) . . . . ? S3 C3 C7 O3 0.1(4) . . . . ? C4 C3 C7 N2 0.5(3) . . . . ? S3 C3 C7 N2 -179.89(18) . . . . ? C3 C4 C8 O4 176.9(3) . . . . ? S4 C4 C8 O4 -4.5(4) . . . . ? C3 C4 C8 N2 -1.9(3) . . . . ? S4 C4 C8 N2 176.76(18) . . . . ? O2 C6 N1 C5 179.7(2) . . . . ? C2 C6 N1 C5 -0.4(3) . . . . ? O1 C5 N1 C6 180.0(2) . . . . ? C1 C5 N1 C6 0.3(3) . . . . ? O4 C8 N2 C7 -176.5(3) . . . . ? C4 C8 N2 C7 2.3(3) . . . . ? O3 C7 N2 C8 178.1(3) . . . . ? C3 C7 N2 C8 -1.8(3) . . . . ? C16 N11 C12 N12 -179.7(2) . . . . ? C16 N11 C12 N15 0.2(4) . . . . ? C16 N13 C14 N14 178.3(2) . . . . ? C16 N13 C14 N15 -1.3(3) . . . . ? N12 C12 N15 C14 179.6(2) . . . . ? N11 C12 N15 C14 -0.3(3) . . . . ? N14 C14 N15 C12 -178.7(2) . . . . ? N13 C14 N15 C12 0.9(3) . . . . ? C14 N13 C16 N16 -178.1(2) . . . . ? C14 N13 C16 N11 1.2(3) . . . . ? C12 N11 C16 N16 178.6(2) . . . . ? C12 N11 C16 N13 -0.7(4) . . . . ? C26 N21 C22 N22 178.6(2) . . . . ? C26 N21 C22 N23 -1.1(3) . . . . ? N22 C22 N23 C24 -179.1(2) . . . . ? N21 C22 N23 C24 0.7(3) . . . . ? C22 N23 C24 N24 -179.3(2) . . . . ? C22 N23 C24 N25 0.8(3) . . . . ? N24 C24 N25 C26 178.4(2) . . . . ? N23 C24 N25 C26 -1.7(3) . . . . ? C24 N25 C26 N26 -179.5(2) . . . . ? C24 N25 C26 N21 1.1(3) . . . . ? C22 N21 C26 N25 0.2(3) . . . . ? C22 N21 C26 N26 -179.2(2) . . . . ? O31 C31 N31 C32 -1.0(4) . . . . ? O31 C31 N31 C33 -178.5(3) . . . . ? O41 C41 N41 C42 -0.2(4) . . . . ? O41 C41 N41 C43 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.051 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.126