# Copyright The Royal Society of Chemistry, 1998 data_tet _audit_creation_method SHELXL _chemical_name_systematic ; tetraethylammonium tetrakis(2-methylmercaptotetrazolato)aurate(III) ; _chemical_name_common ? _chemical_formula_moiety (NEt4)[Au(Smetetraz)4] _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H32 Au N17 S4' _chemical_formula_weight 787.79 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0181 .0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0311 .0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .3331 .5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x+1/2, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' '-x, -y, -z' '-y, x-1/2, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' _cell_length_a 15.2180(10) _cell_length_b 15.2180(10) _cell_length_c 6.5110(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1507.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 16.64 _cell_measurement_theta_max 25.16 _exptl_crystal_description cube _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.735 _exptl_crystal_density_method ? _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 12.094 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 233(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 0.7 _diffrn_reflns_number 1454 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 5.82 _diffrn_reflns_theta_max 59.96 _reflns_number_total 1058 _reflns_number_observed 1002 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'PLATON,HELENA (Spek, 1995)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL (Keller,1995), ZORTEP (Zsolnai,1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+( 0.0963P)^2^+6.6817P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1058 _refine_ls_number_parameters 87 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0650 _refine_ls_R_factor_obs 0.0614 _refine_ls_wR_factor_all 0.1789 _refine_ls_wR_factor_obs 0.1738 _refine_ls_goodness_of_fit_all 1.194 _refine_ls_goodness_of_fit_obs 1.195 _refine_ls_restrained_S_all 1.194 _refine_ls_restrained_S_obs 1.195 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au Au 0.2500 0.2500 0.11203(13) 0.0684(5) Uani 1 d S . S S 0.1064(2) 0.3071(2) 0.1236(5) 0.0885(10) Uani 1 d . . C1 C 0.1134(9) 0.4169(9) 0.0608(20) 0.077(3) Uani 1 d . . N2 N 0.1120(7) 0.4842(8) 0.1902(19) 0.087(3) Uani 1 d . . N3 N 0.1125(9) 0.5572(8) 0.0713(25) 0.098(3) Uani 1 d . . N4 N 0.1153(9) 0.5373(9) -0.1203(19) 0.098(4) Uani 1 d . . N5 N 0.1164(7) 0.4496(8) -0.1300(15) 0.081(3) Uani 1 d . . C6 C 0.1180(15) 0.4044(12) -0.3259(24) 0.121(6) Uani 1 d . . H6A H 0.1201(15) 0.4472(12) -0.4362(24) 0.181 Uiso 1 calc R . H6B H 0.0654(15) 0.3688(12) -0.3398(24) 0.181 Uiso 1 calc R . H6C H 0.1694(15) 0.3669(12) -0.3328(24) 0.181 Uiso 1 calc R . N10 N 0.7500 0.2500 0.5000 0.072(5) Uani 1 d S . C11 C 0.8251(11) 0.2719(12) 0.3615(23) 0.103(5) Uani 1 d . . H11A H 0.8091(11) 0.3224(12) 0.2760(23) 0.124 Uiso 1 calc R . H11B H 0.8363(11) 0.2220(12) 0.2700(23) 0.124 Uiso 1 calc R . C12 C 0.9108(9) 0.2939(11) 0.4827(32) 0.109(5) Uani 1 d . . H12A H 0.9576(9) 0.3076(11) 0.3867(32) 0.163 Uiso 1 calc R . H12B H 0.9277(9) 0.2436(11) 0.5654(32) 0.163 Uiso 1 calc R . H12C H 0.9004(9) 0.3440(11) 0.5714(32) 0.163 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 0.0711(6) 0.0711(6) 0.0630(7) 0.000 0.000 0.000 S 0.074(2) 0.082(2) 0.110(3) 0.011(2) 0.019(2) 0.002(2) C1 0.073(7) 0.084(8) 0.075(7) -0.006(6) 0.006(6) -0.018(6) N2 0.085(7) 0.086(7) 0.090(7) -0.003(6) -0.002(6) 0.006(5) N3 0.099(9) 0.073(7) 0.121(10) -0.003(7) -0.006(7) 0.012(6) N4 0.102(9) 0.083(8) 0.108(11) 0.017(6) -0.010(6) -0.007(6) N5 0.077(7) 0.083(8) 0.081(7) -0.001(5) -0.004(5) -0.014(5) C6 0.164(17) 0.123(13) 0.075(8) -0.005(9) -0.011(10) -0.011(11) N10 0.067(7) 0.067(7) 0.082(12) 0.000 0.000 0.000 C11 0.102(11) 0.088(10) 0.119(12) 0.004(8) 0.023(8) 0.000(8) C12 0.065(8) 0.110(11) 0.150(14) -0.006(11) 0.012(9) -0.005(7) _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 S 2.354(4) . ? Au S 2.354(4) 4 ? Au S 2.354(4) 2 ? Au S 2.354(4) 3 ? S C1 1.722(14) . ? C1 N2 1.33(2) . ? C1 N5 1.34(2) . ? N2 N3 1.35(2) . ? N3 N4 1.28(2) . ? N4 N5 1.34(2) . ? N5 C6 1.45(2) . ? N10 C11 1.494(15) . ? N10 C11 1.494(15) 3_655 ? N10 C11 1.494(15) 6_656 ? N10 C11 1.494(15) 8_666 ? C11 C12 1.56(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 S Au S 89.942(5) . 4 ? S Au S 89.941(6) . 2 ? S Au S 176.3(2) 4 2 ? S Au S 176.3(2) . 3 ? S Au S 89.941(6) 4 3 ? S Au S 89.941(6) 2 3 ? C1 S Au 107.0(5) . . ? N2 C1 N5 107.6(12) . . ? N2 C1 S 126.7(11) . . ? N5 C1 S 125.7(10) . . ? C1 N2 N3 105.7(12) . . ? N4 N3 N2 111.3(12) . . ? N3 N4 N5 106.3(11) . . ? N4 N5 C1 109.1(11) . . ? N4 N5 C6 121.1(12) . . ? C1 N5 C6 129.8(13) . . ? C11 N10 C11 105.7(13) . 3_655 ? C11 N10 C11 111.4(7) . 6_656 ? C11 N10 C11 111.4(7) 3_655 6_656 ? C11 N10 C11 111.4(7) . 8_666 ? C11 N10 C11 111.4(7) 3_655 8_666 ? C11 N10 C11 105.7(13) 6_656 8_666 ? N10 C11 C12 112.5(12) . . ? _refine_diff_density_max 1.331 _refine_diff_density_min -1.180 _refine_diff_density_rms .132 #=END data_spy _audit_creation_method SHELXL _chemical_name_systematic ; chloro{2-(N,N-dimethylammoniummethyl) phenyl}bis(2-mercaptopyridinium)gold(II) chlorid x H2O ; _chemical_name_common ? _chemical_formula_moiety '[Au(Hdamp-C1)(HSpy)2Cl]Cl2 x H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H23 Au Cl3 N3 O S2' _chemical_formula_weight 676.84 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2)1)/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 15.910(6) _cell_length_b 11.036(3) _cell_length_c 14.650(5) _cell_angle_alpha 90.00 _cell_angle_beta 71.22(2) _cell_angle_gamma 90.00 _cell_volume 2435.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.25 _cell_measurement_theta_max 12.03 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.846 _exptl_crystal_density_method ? _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 6.557 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 300 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% none _diffrn_reflns_number 5316 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4781 _reflns_number_observed 3460 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'SDP, HELENA' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL (Keller,1995), ZORTEP (Zsolnai,1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1939)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 26 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+( 0.0494P)^2^+16.9761P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except H(8), H(22), H32 -difmap' _refine_ls_hydrogen_treatment 'riding model, refined' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4755 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_obs 0.0558 _refine_ls_wR_factor_all 0.1383 _refine_ls_wR_factor_obs 0.1148 _refine_ls_goodness_of_fit_all 1.080 _refine_ls_goodness_of_fit_obs 1.077 _refine_ls_restrained_S_all 1.094 _refine_ls_restrained_S_obs 1.077 _refine_ls_shift/esd_max 0.046 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au Au 0.65724(3) 0.14090(4) 0.93785(3) 0.04448(15) Uani 1 d . . Cl1 Cl 0.6580(2) 0.2767(3) 1.0625(2) 0.0600(8) Uani 1 d . . Cl2 Cl 0.8740(2) 0.2723(3) 0.8434(2) 0.0662(8) Uani 1 d . . Cl3 Cl 0.8888(2) -0.2026(3) 0.5120(3) 0.0741(10) Uani 1 d . . C1 C 0.6382(6) 0.0170(10) 0.8409(8) 0.044(3) Uani 1 d . . C2 C 0.5523(8) -0.0102(12) 0.8513(9) 0.059(3) Uani 1 d . . H2 H 0.5069(8) 0.0284(12) 0.8988(9) 0.070 Uiso 1 calc R . C3 C 0.5316(8) -0.0942(13) 0.7924(9) 0.062(3) Uani 1 d . . H3 H 0.4727(8) -0.1145(13) 0.8021(9) 0.075 Uiso 1 calc R . C4 C 0.5974(8) -0.1477(12) 0.7200(10) 0.065(3) Uani 1 d . . H4 H 0.5838(8) -0.1990(12) 0.6763(10) 0.078 Uiso 1 calc R . C5 C 0.6834(10) -0.1249(14) 0.7126(12) 0.089(5) Uani 1 d . . H5 H 0.7285(10) -0.1668(14) 0.6672(12) 0.107 Uiso 1 calc R . C6 C 0.7054(8) -0.0401(11) 0.7717(10) 0.062(3) Uani 1 d . . C7 C 0.8038(9) -0.0286(15) 0.7664(12) 0.088(5) Uani 1 d . . H7A H 0.8097(9) 0.0392(15) 0.8061(12) 0.105 Uiso 1 calc R . H7B H 0.8211(9) -0.1014(15) 0.7930(12) 0.105 Uiso 1 calc R . N8 N 0.8634(7) -0.0109(11) 0.6701(8) 0.068(3) Uani 1 d . . H8 H 0.8684(88) -0.0814(129) 0.6288(99) 0.082 Uiso 1 d . . C9 C 0.9551(7) 0.0092(14) 0.6608(11) 0.083(5) Uani 1 d . . H9A H 0.9749(7) 0.0834(14) 0.6264(11) 0.125 Uiso 1 calc R . H9B H 0.9903(7) -0.0570(14) 0.6261(11) 0.125 Uiso 1 calc R . H9C H 0.9613(7) 0.0146(14) 0.7238(11) 0.125 Uiso 1 calc R . C10 C 0.8315(14) 0.1025(15) 0.6252(15) 0.115(7) Uani 1 d . . H10A H 0.7710(14) 0.0910(15) 0.6277(15) 0.172 Uiso 1 calc R . H10B H 0.8683(14) 0.1121(15) 0.5593(15) 0.172 Uiso 1 calc R . H10C H 0.8357(14) 0.1737(15) 0.6611(15) 0.172 Uiso 1 calc R . S20 S 0.6916(2) -0.0239(3) 1.0192(3) 0.0617(8) Uani 1 d . . C21 C 0.7781(7) 0.0168(10) 1.0610(8) 0.047(3) Uani 1 d . . N22 N 0.8389(6) 0.0990(9) 1.0165(8) 0.053(2) Uani 1 d . . H22 H 0.8304(50) 0.1365(76) 0.9701(61) 0.013(20) Uiso 1 d . . C23 C 0.9116(8) 0.1238(13) 1.0409(10) 0.066(4) Uani 1 d . . H23 H 0.9515(8) 0.1821(13) 1.0063(10) 0.079 Uiso 1 calc R . C24 C 0.9279(10) 0.0663(16) 1.1139(12) 0.080(4) Uani 1 d . . H24 H 0.9783(10) 0.0835(16) 1.1307(12) 0.096 Uiso 1 calc R . C25 C 0.8672(12) -0.0192(16) 1.1632(11) 0.089(5) Uani 1 d . . H25 H 0.8762(12) -0.0607(16) 1.2145(11) 0.106 Uiso 1 calc R . C26 C 0.7916(10) -0.0444(12) 1.1365(10) 0.072(4) Uani 1 d . . H26 H 0.7509(10) -0.1024(12) 1.1700(10) 0.086 Uiso 1 calc R . S30 S 0.6120(3) 0.2806(3) 0.8432(3) 0.0688(10) Uani 1 d . . C31 C 0.6348(9) 0.4254(10) 0.8761(9) 0.057(3) Uani 1 d . . N32 N 0.7134(8) 0.4486(10) 0.8892(8) 0.061(3) Uani 1 d . . H32 H 0.7466(95) 0.4030(128) 0.8767(110) 0.073 Uiso 1 d . . C33 C 0.7359(11) 0.5579(13) 0.9135(10) 0.073(4) Uani 1 d . . H33 H 0.7905(11) 0.5693(13) 0.9227(10) 0.088 Uiso 1 calc R . C34 C 0.6785(12) 0.6523(14) 0.9247(11) 0.087(5) Uani 1 d . . H34 H 0.6935(12) 0.7290(14) 0.9409(11) 0.105 Uiso 1 calc R . C35 C 0.5982(13) 0.6323(13) 0.9116(10) 0.083(5) Uani 1 d . . H35 H 0.5580(13) 0.6958(13) 0.9196(10) 0.100 Uiso 1 calc R . C36 C 0.5768(10) 0.5211(12) 0.8873(10) 0.071(4) Uani 1 d . . H36 H 0.5224(10) 0.5091(12) 0.8779(10) 0.086 Uiso 1 calc R . O O 0.9185(9) -0.2639(13) 0.7945(10) 0.131(5) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.0419(2) 0.0429(2) 0.0489(3) -0.0017(2) -0.0150(2) -0.0015(2) Cl1 0.072(2) 0.058(2) 0.051(2) -0.0041(15) -0.0210(15) -0.008(2) Cl2 0.059(2) 0.070(2) 0.067(2) 0.013(2) -0.017(2) -0.009(2) Cl3 0.072(2) 0.064(2) 0.070(2) 0.003(2) 0.001(2) 0.006(2) C1 0.038(5) 0.048(6) 0.040(6) -0.001(5) -0.004(4) -0.010(5) C2 0.049(6) 0.069(8) 0.057(8) -0.006(7) -0.015(6) -0.007(6) C3 0.057(7) 0.080(9) 0.046(7) -0.001(7) -0.012(6) -0.013(7) C4 0.063(7) 0.067(8) 0.070(8) -0.022(7) -0.028(6) -0.009(7) C5 0.065(8) 0.091(11) 0.104(12) -0.055(10) -0.017(8) 0.000(8) C6 0.046(6) 0.054(8) 0.082(9) -0.018(7) -0.015(6) -0.006(6) C7 0.068(9) 0.082(11) 0.103(13) -0.015(10) -0.014(8) -0.013(8) N8 0.047(6) 0.068(8) 0.071(8) -0.008(6) 0.008(5) -0.005(5) C9 0.036(6) 0.099(12) 0.095(11) 0.018(10) 0.007(6) -0.001(7) C10 0.151(18) 0.076(12) 0.138(17) 0.029(12) -0.076(15) 0.007(11) S20 0.066(2) 0.047(2) 0.076(2) 0.013(2) -0.029(2) -0.0112(15) C21 0.052(6) 0.041(6) 0.043(6) 0.002(5) -0.006(5) -0.001(5) N22 0.059(6) 0.057(6) 0.047(6) 0.002(5) -0.024(5) 0.007(5) C23 0.058(7) 0.079(10) 0.066(8) -0.007(8) -0.028(6) 0.005(7) C24 0.076(10) 0.094(12) 0.082(11) -0.015(10) -0.043(9) 0.012(9) C25 0.118(13) 0.108(14) 0.052(9) -0.010(9) -0.044(9) 0.040(11) C26 0.102(11) 0.053(8) 0.060(9) 0.005(7) -0.024(8) 0.014(8) S30 0.092(2) 0.050(2) 0.086(3) -0.002(2) -0.059(2) 0.005(2) C31 0.080(9) 0.036(6) 0.057(8) -0.006(6) -0.026(7) 0.004(6) N32 0.084(9) 0.046(7) 0.057(7) 0.011(5) -0.031(6) -0.001(5) C33 0.095(11) 0.057(9) 0.069(9) 0.013(7) -0.027(8) -0.024(8) C34 0.121(14) 0.046(9) 0.089(12) -0.010(8) -0.027(10) -0.016(9) C35 0.131(14) 0.045(8) 0.064(9) -0.006(7) -0.018(9) 0.021(9) C36 0.098(10) 0.054(8) 0.070(9) -0.007(7) -0.038(8) 0.015(8) O 0.137(11) 0.117(11) 0.134(11) 0.008(9) -0.036(9) -0.003(9) _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 C1 2.063(11) . ? Au S20 2.334(3) . ? Au S30 2.337(3) . ? Au Cl1 2.365(3) . ? C1 C2 1.359(14) . ? C1 C6 1.37(2) . ? C2 C3 1.38(2) . ? C3 C4 1.36(2) . ? C4 C5 1.36(2) . ? C5 C6 1.39(2) . ? C6 C7 1.55(2) . ? C7 N8 1.44(2) . ? N8 C9 1.44(2) . ? N8 C10 1.57(2) . ? S20 C21 1.735(12) . ? C21 N22 1.334(14) . ? C21 C26 1.37(2) . ? N22 C23 1.344(15) . ? C23 C24 1.34(2) . ? C24 C25 1.38(2) . ? C25 C26 1.41(2) . ? S30 C31 1.741(12) . ? C31 N32 1.35(2) . ? C31 C36 1.38(2) . ? N32 C33 1.34(2) . ? C33 C34 1.36(2) . ? C34 C35 1.37(2) . ? C35 C36 1.35(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 C1 Au S20 86.9(3) . . ? C1 Au S30 83.5(3) . . ? S20 Au S30 169.99(12) . . ? C1 Au Cl1 171.8(3) . . ? S20 Au Cl1 92.25(12) . . ? S30 Au Cl1 96.83(12) . . ? C2 C1 C6 119.9(11) . . ? C2 C1 Au 115.8(8) . . ? C6 C1 Au 124.3(8) . . ? C1 C2 C3 120.9(12) . . ? C4 C3 C2 120.1(12) . . ? C5 C4 C3 118.8(12) . . ? C4 C5 C6 121.5(13) . . ? C1 C6 C5 118.5(11) . . ? C1 C6 C7 122.4(11) . . ? C5 C6 C7 118.4(12) . . ? N8 C7 C6 113.4(13) . . ? C9 N8 C7 116.2(12) . . ? C9 N8 C10 107.0(12) . . ? C7 N8 C10 108.6(13) . . ? C21 S20 Au 108.7(4) . . ? N22 C21 C26 116.8(12) . . ? N22 C21 S20 122.5(9) . . ? C26 C21 S20 120.4(10) . . ? C21 N22 C23 124.1(11) . . ? C24 C23 N22 121.3(14) . . ? C23 C24 C25 117.4(14) . . ? C24 C25 C26 120.6(14) . . ? C21 C26 C25 119.8(14) . . ? C31 S30 Au 108.1(4) . . ? N32 C31 C36 117.0(12) . . ? N32 C31 S30 119.9(9) . . ? C36 C31 S30 123.1(11) . . ? C33 N32 C31 123.2(12) . . ? N32 C33 C34 119.7(14) . . ? C33 C34 C35 118.7(14) . . ? C36 C35 C34 120.6(15) . . ? C35 C36 C31 120.8(15) . . ? _refine_diff_density_max 1.331 _refine_diff_density_min -1.660 _refine_diff_density_rms .164 #=END data_tetra _audit_creation_method SHELXL _chemical_name_systematic ; tris{2-(N,N-dimethylammoniummethyl)phenyl} tris(2-mercaptomethyltetrazolato)gold(III) ; _chemical_name_common ? _chemical_formula_moiety [Au(Hdamp-C1)(Smetetraz)3] _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H22 Au N13 S3' _chemical_formula_weight 677.60 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 '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' 'S' 'S' .1246 .1234 '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 10.135(3) _cell_length_b 10.239(4) _cell_length_c 13.967(5) _cell_angle_alpha 73.65(3) _cell_angle_beta 71.99(3) _cell_angle_gamma 63.01(3) _cell_volume 1211.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.31 _cell_measurement_theta_max 15.44 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.858 _exptl_crystal_density_method ? _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 6.364 _exptl_absorpt_correction_type 'Psi scans' _exptl_absorpt_correction_T_min 0.7126 _exptl_absorpt_correction_T_max 0.9992 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 11.5 _diffrn_reflns_number 5054 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4266 _reflns_number_observed 3806 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'SDP, HELENA' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL (Keller,1995), ZORTEP (Zsolnai,1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 14 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+( 0.0628P)^2^+0.2511P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom (except of N(8) - difmap)' _refine_ls_hydrogen_treatment 'riding model / refined' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4252 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_obs 0.0371 _refine_ls_wR_factor_all 0.0970 _refine_ls_wR_factor_obs 0.0883 _refine_ls_goodness_of_fit_all 1.120 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.127 _refine_ls_restrained_S_obs 1.091 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au1 Au 0.16911(3) 0.05718(2) 0.35430(2) 0.03849(11) Uani 1 d . . C1 C 0.1007(7) 0.1099(6) 0.2197(5) 0.0384(13) Uani 1 d . . C2 C -0.0314(9) 0.0980(8) 0.2211(6) 0.056(2) Uani 1 d . . H2 H -0.0893(9) 0.0716(8) 0.2831(6) 0.067 Uiso 1 calc R . C3 C -0.0776(11) 0.1248(9) 0.1322(7) 0.069(2) Uani 1 d . . H3 H -0.1663(11) 0.1166(9) 0.1345(7) 0.083 Uiso 1 calc R . C4 C 0.0074(12) 0.1637(9) 0.0392(7) 0.070(2) Uani 1 d . . H4 H -0.0233(12) 0.1818(9) -0.0212(7) 0.084 Uiso 1 calc R . C5 C 0.1379(11) 0.1751(8) 0.0379(6) 0.063(2) Uani 1 d . . H5 H 0.1963(11) 0.1997(8) -0.0245(6) 0.076 Uiso 1 calc R . C6 C 0.1850(8) 0.1510(7) 0.1266(5) 0.047(2) Uani 1 d . . C7 C 0.3269(8) 0.1676(7) 0.1196(6) 0.051(2) Uani 1 d . . H7A H 0.3955(8) 0.1431(7) 0.0551(6) 0.061 Uiso 1 calc R . H7B H 0.3762(8) 0.0980(7) 0.1740(6) 0.061 Uiso 1 calc R . N8 N 0.2967(7) 0.3234(7) 0.1277(5) 0.0470(14) Uani 1 d . . H8 H 0.2303(72) 0.3419(68) 0.1658(47) 0.023(17) Uiso 1 d . . C9 C 0.2561(10) 0.4310(8) 0.0343(6) 0.058(2) Uani 1 d . . H9A H 0.1728(10) 0.4256(8) 0.0190(6) 0.087 Uiso 1 calc R . H9B H 0.3417(10) 0.4074(8) -0.0219(6) 0.087 Uiso 1 calc R . H9C H 0.2276(10) 0.5296(8) 0.0451(6) 0.087 Uiso 1 calc R . C10 C 0.4248(10) 0.3278(10) 0.1542(6) 0.063(2) Uani 1 d . . H10A H 0.4484(10) 0.2571(10) 0.2148(6) 0.094 Uiso 1 calc R . H10B H 0.3975(10) 0.4257(10) 0.1659(6) 0.094 Uiso 1 calc R . H10C H 0.5117(10) 0.3034(10) 0.0989(6) 0.094 Uiso 1 calc R . S1 S 0.2571(3) -0.0054(2) 0.50959(14) 0.0556(5) Uani 1 d . . C11 C 0.3015(8) 0.1445(8) 0.4926(5) 0.049(2) Uani 1 d . . N12 N 0.3316(9) 0.2317(9) 0.4066(5) 0.073(2) Uani 1 d . . N13 N 0.3539(10) 0.3348(9) 0.4345(8) 0.090(3) Uani 1 d . . N14 N 0.3437(9) 0.3138(8) 0.5298(8) 0.080(2) Uani 1 d . . N15 N 0.3081(8) 0.1936(7) 0.5704(5) 0.057(2) Uani 1 d . . C16 C 0.2943(12) 0.1295(12) 0.6773(7) 0.081(3) Uani 1 d . . H16A H 0.3040(12) 0.1903(12) 0.7139(7) 0.121 Uiso 1 calc R . H16B H 0.3726(12) 0.0313(12) 0.6854(7) 0.121 Uiso 1 calc R . H16C H 0.1970(12) 0.1244(12) 0.7039(7) 0.121 Uiso 1 calc R . S2 S 0.3685(2) -0.1655(2) 0.3147(2) 0.0560(5) Uani 1 d . . C21 C 0.3328(8) -0.2056(7) 0.2152(5) 0.048(2) Uani 1 d . . N22 N 0.3970(9) -0.1886(8) 0.1180(5) 0.069(2) Uani 1 d . . N23 N 0.3337(12) -0.2368(9) 0.0711(6) 0.087(3) Uani 1 d . . N24 N 0.2353(10) -0.2842(8) 0.1363(6) 0.075(2) Uani 1 d . . N25 N 0.2334(7) -0.2645(6) 0.2271(5) 0.0521(14) Uani 1 d . . C26 C 0.1347(11) -0.3054(10) 0.3186(7) 0.070(2) Uani 1 d . . H26A H 0.0772(11) -0.3449(10) 0.3011(7) 0.104 Uiso 1 calc R . H26B H 0.0670(11) -0.2193(10) 0.3498(7) 0.104 Uiso 1 calc R . H26C H 0.1947(11) -0.3793(10) 0.3655(7) 0.104 Uiso 1 calc R . S3 S -0.0322(2) 0.2605(2) 0.41877(13) 0.0572(5) Uani 1 d . . C31 C -0.0902(8) 0.3934(7) 0.3150(5) 0.0409(14) Uani 1 d . . N32 N -0.0102(8) 0.4567(7) 0.2398(5) 0.061(2) Uani 1 d . . N33 N -0.1060(9) 0.5546(7) 0.1789(5) 0.073(2) Uani 1 d . . N34 N -0.2384(9) 0.5556(7) 0.2131(5) 0.072(2) Uani 1 d . . N35 N -0.2309(7) 0.4544(6) 0.2996(4) 0.0479(13) Uani 1 d . . C36 C -0.3613(10) 0.4249(10) 0.3596(8) 0.080(3) Uani 1 d . . H36A H -0.4465(10) 0.4873(10) 0.3282(8) 0.121 Uiso 1 calc R . H36B H -0.3839(10) 0.4454(10) 0.4272(8) 0.121 Uiso 1 calc R . H36C H -0.3403(10) 0.3225(10) 0.3633(8) 0.121 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 0.0522(2) 0.03540(15) 0.03476(15) -0.00155(9) -0.01588(10) -0.02159(11) C1 0.049(4) 0.028(3) 0.041(3) -0.005(2) -0.018(3) -0.012(3) C2 0.071(5) 0.053(4) 0.055(4) 0.000(3) -0.022(4) -0.033(4) C3 0.086(6) 0.065(5) 0.083(6) -0.004(4) -0.053(5) -0.035(5) C4 0.102(7) 0.057(5) 0.066(5) -0.003(4) -0.049(5) -0.028(5) C5 0.098(7) 0.046(4) 0.041(4) -0.002(3) -0.024(4) -0.022(4) C6 0.062(4) 0.035(3) 0.039(3) -0.006(3) -0.013(3) -0.015(3) C7 0.057(4) 0.038(3) 0.050(4) -0.006(3) 0.000(3) -0.020(3) N8 0.047(4) 0.049(3) 0.040(3) -0.015(3) 0.007(3) -0.022(3) C9 0.074(5) 0.043(4) 0.055(4) -0.006(3) -0.012(4) -0.025(4) C10 0.071(5) 0.069(5) 0.054(4) -0.008(4) -0.013(4) -0.034(4) S1 0.0924(14) 0.0441(9) 0.0460(9) 0.0050(7) -0.0352(10) -0.0347(10) C11 0.057(4) 0.046(4) 0.051(4) -0.003(3) -0.021(3) -0.025(3) N12 0.092(5) 0.081(5) 0.063(4) 0.012(4) -0.026(4) -0.057(5) N13 0.097(6) 0.077(5) 0.115(7) 0.024(5) -0.047(6) -0.059(5) N14 0.083(5) 0.061(4) 0.118(7) -0.012(5) -0.035(5) -0.041(4) N15 0.066(4) 0.053(4) 0.070(4) -0.011(3) -0.027(3) -0.030(3) C16 0.105(7) 0.112(8) 0.061(5) -0.023(5) -0.024(5) -0.065(7) S2 0.0615(11) 0.0401(9) 0.0726(12) -0.0109(8) -0.0340(10) -0.0122(8) C21 0.052(4) 0.038(3) 0.052(4) -0.012(3) -0.012(3) -0.012(3) N22 0.076(5) 0.055(4) 0.055(4) -0.010(3) -0.001(4) -0.016(4) N23 0.121(7) 0.075(5) 0.052(4) -0.028(4) -0.016(5) -0.021(5) N24 0.108(6) 0.067(4) 0.064(5) -0.031(4) -0.033(4) -0.027(4) N25 0.066(4) 0.041(3) 0.048(3) -0.015(3) -0.017(3) -0.013(3) C26 0.083(6) 0.067(5) 0.073(6) -0.010(4) -0.014(5) -0.046(5) S3 0.0640(12) 0.0567(11) 0.0343(8) -0.0087(8) -0.0079(8) -0.0114(9) C31 0.054(4) 0.037(3) 0.036(3) -0.012(3) -0.007(3) -0.020(3) N32 0.063(4) 0.052(4) 0.060(4) -0.010(3) 0.001(3) -0.026(3) N33 0.081(5) 0.048(4) 0.051(4) 0.007(3) -0.002(4) -0.010(4) N34 0.072(5) 0.052(4) 0.063(4) 0.003(3) -0.021(4) -0.005(4) N35 0.048(3) 0.040(3) 0.052(3) -0.008(2) -0.013(3) -0.013(3) C36 0.053(5) 0.067(5) 0.114(8) -0.002(5) -0.014(5) -0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.050(6) . ? Au1 S3 2.318(2) . ? Au1 S2 2.329(2) . ? Au1 S1 2.409(2) . ? C1 C6 1.389(9) . ? C1 C2 1.392(10) . ? C2 C3 1.374(10) . ? C3 C4 1.384(13) . ? C4 C5 1.374(13) . ? C5 C6 1.382(10) . ? C6 C7 1.494(11) . ? C7 N8 1.512(9) . ? N8 C10 1.478(10) . ? N8 C9 1.482(9) . ? S1 C11 1.723(7) . ? C11 N12 1.322(9) . ? C11 N15 1.351(9) . ? N12 N13 1.350(11) . ? N13 N14 1.266(12) . ? N14 N15 1.360(9) . ? N15 C16 1.443(11) . ? S2 C21 1.732(7) . ? C21 N22 1.311(9) . ? C21 N25 1.340(10) . ? N22 N23 1.347(11) . ? N23 N24 1.300(12) . ? N24 N25 1.333(9) . ? N25 C26 1.448(10) . ? S3 C31 1.728(7) . ? C31 N32 1.322(9) . ? C31 N35 1.332(9) . ? N32 N33 1.349(10) . ? N33 N34 1.273(11) . ? N34 N35 1.349(8) . ? N35 C36 1.440(10) . ? 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 C1 Au1 S3 93.4(2) . . ? C1 Au1 S2 93.8(2) . . ? S3 Au1 S2 171.42(7) . . ? C1 Au1 S1 178.3(2) . . ? S3 Au1 S1 87.70(8) . . ? S2 Au1 S1 85.26(8) . . ? C6 C1 C2 118.9(6) . . ? C6 C1 Au1 122.2(5) . . ? C2 C1 Au1 118.9(5) . . ? C3 C2 C1 121.0(8) . . ? C2 C3 C4 120.3(8) . . ? C5 C4 C3 118.7(7) . . ? C4 C5 C6 121.9(8) . . ? C5 C6 C1 119.3(7) . . ? C5 C6 C7 119.0(7) . . ? C1 C6 C7 121.7(6) . . ? C6 C7 N8 112.3(6) . . ? C10 N8 C9 111.4(6) . . ? C10 N8 C7 111.7(6) . . ? C9 N8 C7 112.1(6) . . ? C11 S1 Au1 98.4(2) . . ? N12 C11 N15 108.2(7) . . ? N12 C11 S1 128.6(6) . . ? N15 C11 S1 123.2(6) . . ? C11 N12 N13 105.5(7) . . ? N14 N13 N12 112.3(7) . . ? N13 N14 N15 106.5(7) . . ? C11 N15 N14 107.5(7) . . ? C11 N15 C16 129.0(7) . . ? N14 N15 C16 123.3(7) . . ? C21 S2 Au1 106.1(2) . . ? N22 C21 N25 108.2(7) . . ? N22 C21 S2 127.7(7) . . ? N25 C21 S2 124.1(6) . . ? C21 N22 N23 105.9(8) . . ? N24 N23 N22 111.2(7) . . ? N23 N24 N25 105.7(7) . . ? N24 N25 C21 109.0(7) . . ? N24 N25 C26 120.9(7) . . ? C21 N25 C26 130.1(6) . . ? C31 S3 Au1 106.8(2) . . ? N32 C31 N35 107.5(6) . . ? N32 C31 S3 128.3(6) . . ? N35 C31 S3 124.2(5) . . ? C31 N32 N33 105.9(7) . . ? N34 N33 N32 111.6(6) . . ? N33 N34 N35 105.9(6) . . ? C31 N35 N34 109.0(6) . . ? C31 N35 C36 129.5(7) . . ? N34 N35 C36 121.5(7) . . ? _refine_diff_density_max 1.766 _refine_diff_density_min -2.337 _refine_diff_density_rms .151 #=END data_purin _audit_creation_method SHELXL _chemical_name_systematic ; Chloro{2(N,N-dimethylammoniummethyl)phenyl-C1} (6-mercaptopurinato)gold(III) chloride ; _chemical_name_common ? _chemical_formula_moiety [Au(Hdamp-C1)(Spurine)Cl]Cl _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H16 Au Cl2 N5 S' _chemical_formula_weight 554.24 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.599(3) _cell_length_b 9.762(2) _cell_length_c 17.452(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.710(10) _cell_angle_gamma 90.00 _cell_volume 1768.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.58 _cell_measurement_theta_max 15.25 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_method ? _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 8.745 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.376 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 3.5 _diffrn_reflns_number 4897 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.94 _reflns_number_total 4231 _reflns_number_observed 3051 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'PLATON, HELENA (Spek, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL (Keller,1995), ZORTEP (Zsolnai,1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+( 0.0622P)^2^+1.4953P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom, except of H(8) and H(29) - geom' _refine_ls_hydrogen_treatment 'riding model /refined' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4231 _refine_ls_number_parameters 216 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_obs 0.0412 _refine_ls_wR_factor_all 0.1152 _refine_ls_wR_factor_obs 0.0975 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.041 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.041 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au Au 0.11105(3) 0.07112(3) 0.20136(2) 0.03648(11) Uani 1 d . . Cl1 Cl 0.2687(2) 0.2366(2) 0.2243(2) 0.0596(6) Uani 1 d . . C1 C 0.0559(8) 0.1211(8) 0.3022(5) 0.043(2) Uani 1 d . . C2 C 0.1248(11) 0.0590(10) 0.3697(6) 0.063(3) Uani 1 d . . H2 H 0.1880(11) -0.0055(10) 0.3662(6) 0.075 Uiso 1 calc R . C3 C 0.0995(13) 0.0926(11) 0.4413(6) 0.074(3) Uani 1 d . . H3 H 0.1467(13) 0.0525(11) 0.4865(6) 0.088 Uiso 1 calc R . C4 C 0.0048(10) 0.1855(10) 0.4463(5) 0.059(3) Uani 1 d . . H4 H -0.0125(10) 0.2079(10) 0.4949(5) 0.071 Uiso 1 calc R . C5 C -0.0641(10) 0.2451(9) 0.3809(5) 0.053(2) Uani 1 d . . H5 H -0.1285(10) 0.3075(9) 0.3854(5) 0.063 Uiso 1 calc R . C6 C -0.0407(8) 0.2153(8) 0.3069(4) 0.040(2) Uani 1 d . . C7 C -0.1272(9) 0.2773(8) 0.2361(5) 0.050(2) Uani 1 d . . H7A H -0.1076(9) 0.2360(8) 0.1893(5) 0.060 Uiso 1 calc R . H7B H -0.2161(9) 0.2557(8) 0.2375(5) 0.060 Uiso 1 calc R . N8 N -0.1131(7) 0.4295(7) 0.2315(4) 0.0398(14) Uani 1 d . . H8 H -0.1158(62) 0.4613(72) 0.2783(44) 0.022(18) Uiso 1 d . . C9 C 0.0174(9) 0.4702(11) 0.2192(7) 0.061(3) Uani 1 d . . H9A H 0.0820(9) 0.4353(11) 0.2614(7) 0.092 Uiso 1 calc R . H9B H 0.0231(9) 0.5683(11) 0.2179(7) 0.092 Uiso 1 calc R . H9C H 0.0308(9) 0.4331(11) 0.1706(7) 0.092 Uiso 1 calc R . C10 C -0.2173(10) 0.4837(11) 0.1680(6) 0.066(3) Uani 1 d . . H10A H -0.2903(10) 0.5091(11) 0.1897(6) 0.099 Uiso 1 calc R . H10B H -0.2424(10) 0.4143(11) 0.1289(6) 0.099 Uiso 1 calc R . H10C H -0.1862(10) 0.5625(11) 0.1446(6) 0.099 Uiso 1 calc R . S20 S -0.0574(2) -0.0862(2) 0.17777(12) 0.0428(5) Uani 1 d . . N21 N -0.0846(7) -0.2615(7) 0.0537(4) 0.051(2) Uani 1 d . . C22 C -0.0411(10) -0.3043(9) -0.0102(5) 0.057(2) Uani 1 d . . H22 H -0.0917(10) -0.3711(9) -0.0396(5) 0.068 Uiso 1 calc R . N23 N 0.0621(7) -0.2667(7) -0.0379(4) 0.051(2) Uani 1 d . . C24 C 0.1244(8) -0.1640(8) 0.0045(4) 0.039(2) Uani 1 d . . C25 C 0.0890(7) -0.1093(7) 0.0686(4) 0.036(2) Uani 1 d . . C26 C -0.0183(8) -0.1587(8) 0.0941(4) 0.040(2) Uani 1 d . . N27 N 0.1702(6) -0.0068(7) 0.1006(4) 0.0389(15) Uani 1 d . . C28 C 0.2579(8) -0.0001(9) 0.0555(5) 0.043(2) Uani 1 d . . H28 H 0.3264(8) 0.0613(9) 0.0629(5) 0.051 Uiso 1 calc R . N29 N 0.2339(8) -0.0938(8) -0.0019(4) 0.046(2) Uani 1 d . . H29 H 0.2760(75) -0.0973(75) -0.0301(45) 0.025(21) Uiso 1 d . . Cl2 Cl 0.5949(2) 0.1172(2) 0.12483(12) 0.0481(5) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.0366(2) 0.0366(2) 0.0361(2) -0.00197(13) 0.00690(11) 0.00274(14) Cl1 0.0456(12) 0.0505(12) 0.083(2) -0.0131(12) 0.0126(11) -0.0105(10) C1 0.057(5) 0.035(4) 0.036(4) -0.005(3) 0.003(4) -0.002(4) C2 0.075(7) 0.063(6) 0.046(5) 0.005(5) 0.000(5) 0.015(5) C3 0.105(9) 0.073(7) 0.034(4) 0.014(5) -0.009(5) -0.009(6) C4 0.088(7) 0.051(5) 0.042(5) -0.013(4) 0.019(5) -0.017(5) C5 0.075(6) 0.046(5) 0.041(4) -0.016(4) 0.021(4) -0.007(4) C6 0.042(4) 0.036(4) 0.042(4) -0.007(3) 0.009(3) -0.006(4) C7 0.065(6) 0.033(4) 0.048(5) -0.010(4) 0.004(4) -0.007(4) N8 0.045(4) 0.040(3) 0.038(3) -0.006(3) 0.017(3) 0.004(3) C9 0.048(6) 0.060(6) 0.079(7) 0.003(5) 0.022(5) -0.007(5) C10 0.078(7) 0.056(6) 0.060(6) 0.010(5) 0.008(5) 0.022(5) S20 0.0423(11) 0.0498(12) 0.0395(10) -0.0030(9) 0.0156(8) -0.0044(9) N21 0.053(4) 0.054(4) 0.047(4) -0.005(3) 0.012(3) -0.008(3) C22 0.066(6) 0.052(6) 0.053(5) -0.015(4) 0.016(4) -0.013(5) N23 0.057(5) 0.052(4) 0.045(4) -0.010(3) 0.012(3) 0.002(4) C24 0.042(4) 0.042(4) 0.035(4) 0.009(3) 0.008(3) 0.009(4) C25 0.039(4) 0.032(4) 0.035(4) 0.004(3) 0.007(3) 0.002(3) C26 0.042(4) 0.043(4) 0.035(4) 0.002(3) 0.004(3) 0.001(4) N27 0.037(4) 0.037(3) 0.041(4) -0.003(3) 0.003(3) 0.001(3) C28 0.036(4) 0.045(5) 0.049(5) 0.004(4) 0.012(4) 0.001(4) N29 0.051(4) 0.053(5) 0.039(4) 0.002(3) 0.018(3) 0.008(4) Cl2 0.0497(12) 0.0543(12) 0.0427(10) 0.0123(9) 0.0151(9) 0.0011(10) _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 C1 2.024(8) . ? Au N27 2.124(7) . ? Au Cl1 2.300(2) . ? Au S20 2.328(2) . ? C1 C6 1.391(11) . ? C1 C2 1.393(12) . ? C2 C3 1.370(15) . ? C3 C4 1.369(15) . ? C4 C5 1.355(13) . ? C5 C6 1.393(11) . ? C6 C7 1.508(11) . ? C7 N8 1.497(10) . ? N8 C10 1.494(11) . ? N8 C9 1.495(11) . ? S20 C26 1.747(8) . ? N21 C26 1.340(10) . ? N21 C22 1.356(11) . ? C22 N23 1.334(11) . ? N23 C24 1.337(10) . ? C24 C25 1.359(11) . ? C24 N29 1.372(11) . ? C25 N27 1.364(10) . ? C25 C26 1.389(11) . ? N27 C28 1.335(10) . ? C28 N29 1.343(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au N27 172.9(3) . . ? C1 Au Cl1 90.4(2) . . ? N27 Au Cl1 94.0(2) . . ? C1 Au S20 88.1(2) . . ? N27 Au S20 87.8(2) . . ? Cl1 Au S20 176.65(8) . . ? C6 C1 C2 120.3(8) . . ? C6 C1 Au 123.8(6) . . ? C2 C1 Au 115.9(7) . . ? C3 C2 C1 120.1(10) . . ? C4 C3 C2 119.9(9) . . ? C5 C4 C3 120.5(9) . . ? C4 C5 C6 121.6(9) . . ? C1 C6 C5 117.7(8) . . ? C1 C6 C7 123.3(7) . . ? C5 C6 C7 118.8(8) . . ? N8 C7 C6 113.1(7) . . ? C10 N8 C9 111.5(7) . . ? C10 N8 C7 109.0(7) . . ? C9 N8 C7 112.2(7) . . ? C26 S20 Au 96.4(3) . . ? C26 N21 C22 115.7(8) . . ? N23 C22 N21 130.8(8) . . ? C22 N23 C24 110.8(7) . . ? N23 C24 C25 124.2(8) . . ? N23 C24 N29 131.3(8) . . ? C25 C24 N29 104.5(7) . . ? C24 C25 N27 111.7(7) . . ? C24 C25 C26 120.5(7) . . ? N27 C25 C26 127.8(7) . . ? N21 C26 C25 117.9(7) . . ? N21 C26 S20 123.7(6) . . ? C25 C26 S20 118.4(6) . . ? C28 N27 C25 104.6(7) . . ? C28 N27 Au 145.9(6) . . ? C25 N27 Au 109.5(5) . . ? N27 C28 N29 110.9(7) . . ? C28 N29 C24 108.3(7) . . ? _refine_diff_density_max 1.372 _refine_diff_density_min -1.279 _refine_diff_density_rms .192 #=END data_thiaz _audit_creation_method SHELXL _chemical_name_systematic ; Chloro{2-(N,N-dimethylammoniummethyl)phenyl-C1}bis (mercaptothiazolinium)gold(III) dichlorid ; _chemical_name_common ? _chemical_formula_moiety '[Au(Hdamp-C1)(HSthiaz)2Cl]Cl2 x acetone' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H29 Au Cl3 N3 O S4' _chemical_formula_weight 735.00 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 '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 10.257(11) _cell_length_b 10.508(13) _cell_length_c 13.785(18) _cell_angle_alpha 107.23(7) _cell_angle_beta 102.90(7) _cell_angle_gamma 97.84(7) _cell_volume 1350.1(28) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.97 _cell_measurement_theta_max 14.38 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max .4 _exptl_crystal_size_mid .35 _exptl_crystal_size_min .22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method ? _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 6.070 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.9093 _exptl_absorpt_correction_T_max 0.9996 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method CAD4 _diffrn_standards_number 3 _diffrn_standards_interval_count 400 _diffrn_standards_interval_time 3600 _diffrn_standards_decay_% 6.3 _diffrn_reflns_number 6203 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5291 _reflns_number_observed 4842 _reflns_observed_criterion >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction 'PLATON, HELENA (Spek, 1996)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SCHAKAL(Keller,1995), ZORTEP (Zsolnai, 1997)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 18 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+( 0.0379P)^2^+1.1163P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment 'fully refined' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5273 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_obs 0.0269 _refine_ls_wR_factor_all 0.0655 _refine_ls_wR_factor_obs 0.0617 _refine_ls_goodness_of_fit_all 1.106 _refine_ls_goodness_of_fit_obs 1.100 _refine_ls_restrained_S_all 1.113 _refine_ls_restrained_S_obs 1.100 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Au Au 0.13704(2) 0.47176(2) 0.636172(12) 0.02623(6) Uani 1 d . . Cl1 Cl -0.06233(12) 0.32222(11) 0.62851(10) 0.0412(3) Uani 1 d . . Cl2 Cl 0.78632(12) 0.59186(11) 0.12078(9) 0.0348(2) Uani 1 d . . Cl3 Cl 0.28524(12) 0.01342(11) 0.01042(11) 0.0466(3) Uani 1 d . . C1 C 0.3035(4) 0.6013(4) 0.6340(3) 0.0275(9) Uani 1 d . . C2 C 0.3225(5) 0.5884(5) 0.5359(4) 0.0354(10) Uani 1 d . . H2 H 0.2724(50) 0.5238(51) 0.4819(39) 0.031(13) Uiso 1 d . . C3 C 0.4329(6) 0.6706(6) 0.5261(4) 0.0444(12) Uani 1 d . . H3 H 0.4498(69) 0.6611(69) 0.4585(54) 0.078(21) Uiso 1 d . . C4 C 0.5224(6) 0.7677(6) 0.6151(4) 0.0460(12) Uani 1 d . . H4 H 0.5951(60) 0.8135(58) 0.6080(43) 0.048(15) Uiso 1 d . . C5 C 0.5032(5) 0.7831(5) 0.7129(4) 0.0380(11) Uani 1 d . . H5 H 0.5557(54) 0.8420(54) 0.7717(41) 0.040(14) Uiso 1 d . . C6 C 0.3936(4) 0.7005(4) 0.7251(3) 0.0281(9) Uani 1 d . . C7 C 0.3748(5) 0.7198(5) 0.8340(3) 0.0291(9) Uani 1 d . . H7A H 0.3087(42) 0.6513(43) 0.8297(30) 0.014(10) Uiso 1 d . . H7B H 0.3557(50) 0.8082(55) 0.8629(39) 0.038(13) Uiso 1 d . . N8 N 0.5018(4) 0.7187(4) 0.9124(3) 0.0304(8) Uani 1 d . . H8 H 0.5695(55) 0.8003(56) 0.9206(41) 0.046(15) Uiso 1 d . . C9 C 0.5560(6) 0.5945(5) 0.8753(4) 0.0402(11) Uani 1 d . . H9A H 0.6419(56) 0.6025(54) 0.9280(42) 0.045(14) Uiso 1 d . . H9B H 0.5840(54) 0.5992(55) 0.8153(44) 0.044(15) Uiso 1 d . . H9C H 0.4731(49) 0.5110(49) 0.8589(35) 0.032(12) Uiso 1 d . . C10 C 0.4742(6) 0.7341(6) 1.0163(4) 0.0395(11) Uani 1 d . . H10A H 0.5545(60) 0.7340(56) 1.0687(45) 0.049(15) Uiso 1 d . . H10B H 0.4437(54) 0.8062(59) 1.0365(41) 0.040(15) Uiso 1 d . . H10C H 0.4207(64) 0.6555(68) 1.0096(47) 0.059(18) Uiso 1 d . . S20 S 0.03259(12) 0.65744(11) 0.67182(10) 0.0356(3) Uani 1 d . . C21 C -0.0073(4) 0.6733(4) 0.7882(4) 0.0303(9) Uani 1 d . . S22 S -0.10223(13) 0.79304(12) 0.83008(11) 0.0413(3) Uani 1 d . . C23 C -0.0511(6) 0.7843(5) 0.9627(4) 0.0421(11) Uani 1 d . . H23A H -0.1225(57) 0.7995(54) 0.9935(41) 0.043(14) Uiso 1 d . . H23B H 0.0282(57) 0.8564(57) 1.0036(42) 0.045(15) Uiso 1 d . . C24 C -0.0243(6) 0.6425(5) 0.9465(4) 0.0383(11) Uani 1 d . . H24A H 0.0411(61) 0.6395(58) 1.0089(46) 0.054(16) Uiso 1 d . . H24B H -0.1085(67) 0.5673(67) 0.9329(49) 0.068(19) Uiso 1 d . . N25 N 0.0279(4) 0.6089(4) 0.8533(3) 0.0334(8) Uani 1 d . . H25 H 0.0825(64) 0.5433(66) 0.8442(48) 0.063(18) Uiso 1 d . . S30 S 0.25254(15) 0.30405(12) 0.57166(11) 0.0439(3) Uani 1 d . . C31 C 0.2087(5) 0.1642(4) 0.6068(4) 0.0338(10) Uani 1 d . . S32 S 0.2133(2) 0.00781(13) 0.52195(11) 0.0514(4) Uani 1 d . . C33 C 0.2010(9) -0.0692(6) 0.6217(6) 0.057(2) Uani 1 d . . H33A H 0.1462(61) -0.1473(67) 0.5877(46) 0.049(17) Uiso 1 d . . H33B H 0.2836(119) -0.0707(116) 0.6602(89) 0.163(49) Uiso 1 d . . C34 C 0.1402(7) 0.0229(5) 0.6973(5) 0.0468(13) Uani 1 d . . H34A H 0.1670(53) 0.0268(54) 0.7577(44) 0.038(15) Uiso 1 d . . H34B H 0.0384(66) -0.0044(61) 0.6740(47) 0.056(17) Uiso 1 d . . N35 N 0.1770(4) 0.1585(4) 0.6901(3) 0.0358(9) Uani 1 d . . H35 H 0.1767(56) 0.2196(58) 0.7350(44) 0.040(16) Uiso 1 d . . C50 C 0.2886(7) 0.7708(7) 0.2220(5) 0.059(2) Uani 1 d . . O51 O 0.2578(6) 0.6541(5) 0.1616(5) 0.092(2) Uani 1 d . . C52 C 0.1927(8) 0.8645(8) 0.2216(6) 0.061(2) Uani 1 d . . H52A H 0.2075(69) 0.9335(74) 0.2895(60) 0.078(22) Uiso 1 d . . H52B H 0.1118(66) 0.8186(64) 0.1949(47) 0.050(18) Uiso 1 d . . H52C H 0.2164(80) 0.9182(82) 0.1773(63) 0.097(26) Uiso 1 d . . C53 C 0.4264(11) 0.8304(12) 0.2945(10) 0.101(3) Uani 1 d . . H53A H 0.4488(83) 0.8968(88) 0.2559(64) 0.097(28) Uiso 1 d . . H53B H 0.4178(65) 0.8784(68) 0.3574(52) 0.054(19) Uiso 1 d . . H53C H 0.4831(98) 0.7541(102) 0.2749(73) 0.123(33) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au 0.02954(9) 0.01955(9) 0.03067(9) 0.01127(6) 0.00729(6) 0.00436(6) Cl1 0.0353(6) 0.0290(6) 0.0553(7) 0.0164(5) 0.0070(5) -0.0020(5) Cl2 0.0402(6) 0.0312(5) 0.0361(6) 0.0138(4) 0.0094(5) 0.0149(5) Cl3 0.0353(6) 0.0255(5) 0.0713(8) 0.0048(5) 0.0161(6) 0.0055(5) C1 0.029(2) 0.025(2) 0.034(2) 0.015(2) 0.010(2) 0.008(2) C2 0.045(3) 0.030(2) 0.033(2) 0.011(2) 0.014(2) 0.006(2) C3 0.054(3) 0.049(3) 0.042(3) 0.023(2) 0.025(2) 0.011(2) C4 0.042(3) 0.046(3) 0.059(3) 0.026(3) 0.024(3) 0.001(2) C5 0.038(3) 0.032(2) 0.041(3) 0.015(2) 0.006(2) 0.000(2) C6 0.026(2) 0.026(2) 0.037(2) 0.016(2) 0.009(2) 0.008(2) C7 0.029(2) 0.024(2) 0.035(2) 0.012(2) 0.006(2) 0.006(2) N8 0.031(2) 0.026(2) 0.032(2) 0.011(2) 0.0043(15) 0.004(2) C9 0.040(3) 0.040(3) 0.043(3) 0.016(2) 0.008(2) 0.017(2) C10 0.047(3) 0.037(3) 0.032(2) 0.012(2) 0.006(2) 0.009(2) S20 0.0385(6) 0.0299(6) 0.0486(7) 0.0234(5) 0.0147(5) 0.0136(5) C21 0.022(2) 0.022(2) 0.046(3) 0.012(2) 0.007(2) 0.005(2) S22 0.0389(6) 0.0330(6) 0.0589(8) 0.0192(6) 0.0149(6) 0.0201(5) C23 0.040(3) 0.033(3) 0.056(3) 0.012(2) 0.016(2) 0.016(2) C24 0.044(3) 0.031(2) 0.044(3) 0.014(2) 0.017(2) 0.013(2) N25 0.035(2) 0.026(2) 0.046(2) 0.017(2) 0.016(2) 0.011(2) S30 0.0658(8) 0.0280(6) 0.0577(8) 0.0230(5) 0.0385(7) 0.0199(6) C31 0.040(3) 0.023(2) 0.042(3) 0.012(2) 0.014(2) 0.011(2) S32 0.0899(11) 0.0259(6) 0.0485(7) 0.0133(5) 0.0344(7) 0.0188(6) C33 0.097(5) 0.032(3) 0.060(4) 0.025(3) 0.039(4) 0.024(3) C34 0.069(4) 0.031(3) 0.049(3) 0.020(2) 0.023(3) 0.012(3) N35 0.052(3) 0.023(2) 0.039(2) 0.012(2) 0.020(2) 0.013(2) C50 0.069(4) 0.056(4) 0.059(4) 0.021(3) 0.030(3) 0.008(3) O51 0.100(4) 0.046(3) 0.117(4) -0.002(3) 0.052(3) 0.010(3) C52 0.068(5) 0.056(4) 0.056(4) 0.016(3) 0.016(3) 0.015(3) C53 0.098(7) 0.087(7) 0.099(8) 0.024(6) -0.005(6) 0.027(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au C1 2.045(5) . ? Au S30 2.326(3) . ? Au S20 2.331(3) . ? Au Cl1 2.364(3) . ? C1 C2 1.380(6) . ? C1 C6 1.400(6) . ? C2 C3 1.384(7) . ? C3 C4 1.375(8) . ? C4 C5 1.370(7) . ? C5 C6 1.397(6) . ? C6 C7 1.514(6) . ? C7 N8 1.500(6) . ? N8 C9 1.484(6) . ? N8 C10 1.487(6) . ? S20 C21 1.709(5) . ? C21 N25 1.294(6) . ? C21 S22 1.738(5) . ? S22 C23 1.819(6) . ? C23 C24 1.513(7) . ? C24 N25 1.467(6) . ? S30 C31 1.714(5) . ? C31 N35 1.275(6) . ? C31 S32 1.726(5) . ? S32 C33 1.809(6) . ? C33 C34 1.506(8) . ? C34 N35 1.462(6) . ? C50 O51 1.212(8) . ? C50 C53 1.464(12) . ? C50 C52 1.484(10) . ? 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 C1 Au S30 83.6(2) . . ? C1 Au S20 87.8(2) . . ? S30 Au S20 167.29(4) . . ? C1 Au Cl1 176.53(12) . . ? S30 Au Cl1 96.72(11) . . ? S20 Au Cl1 91.29(10) . . ? C2 C1 C6 120.4(4) . . ? C2 C1 Au 116.2(3) . . ? C6 C1 Au 123.4(3) . . ? C1 C2 C3 120.6(5) . . ? C4 C3 C2 119.4(5) . . ? C5 C4 C3 120.5(5) . . ? C4 C5 C6 121.2(5) . . ? C5 C6 C1 117.8(4) . . ? C5 C6 C7 120.1(4) . . ? C1 C6 C7 122.0(4) . . ? N8 C7 C6 112.9(4) . . ? C9 N8 C10 111.1(4) . . ? C9 N8 C7 112.4(4) . . ? C10 N8 C7 109.7(4) . . ? C21 S20 Au 107.0(2) . . ? N25 C21 S20 128.0(4) . . ? N25 C21 S22 113.8(4) . . ? S20 C21 S22 118.2(3) . . ? C21 S22 C23 89.9(2) . . ? C24 C23 S22 104.7(4) . . ? N25 C24 C23 105.6(4) . . ? C21 N25 C24 115.6(4) . . ? C31 S30 Au 110.6(2) . . ? N35 C31 S30 129.1(4) . . ? N35 C31 S32 113.9(3) . . ? S30 C31 S32 116.9(3) . . ? C31 S32 C33 90.6(3) . . ? C34 C33 S32 106.1(4) . . ? N35 C34 C33 105.7(5) . . ? C31 N35 C34 117.0(4) . . ? O51 C50 C53 121.7(8) . . ? O51 C50 C52 122.1(7) . . ? C53 C50 C52 116.0(7) . . ? _refine_diff_density_max 1.458 _refine_diff_density_min -1.608 _refine_diff_density_rms .111