# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 440/104

data_tssnau 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum             'C13.50 H20 Au2 Cl3 N O2 S3' 
_chemical_formula_weight          824.77 
 
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' 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 
_symmetry_cell_setting            triclinic 
_symmetry_space_group_name_H-M    P-1
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                     7.977(1) 
_cell_length_b                    11.053(1) 
_cell_length_c                    12.455(1) 
_cell_angle_alpha                 107.37(1) 
_cell_angle_beta                  95.23(1) 
_cell_angle_gamma                 90.33(1) 
_cell_volume                      1043.1(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     203(2) 
_cell_measurement_reflns_used     2000
_cell_measurement_theta_min       5
_cell_measurement_theta_max       30
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.10 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     2.626 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              762 
_exptl_absorpt_coefficient_mu     14.741 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       203(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   'Stoe IPDS'
_diffrn_measurement_method        'image plate'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          'not applicable'
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             9778 
_diffrn_reflns_av_R_equivalents   0.048
_diffrn_reflns_av_sigmaI/netI     0.049 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          1.72 
_diffrn_reflns_theta_max          30.02 
_reflns_number_total              5240 
_reflns_number_gt                 4837 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'Stoe IPDS software'
_computing_cell_refinement        'Stoe IPDS software' 
_computing_data_reduction         'Stoe IPDS software'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F^2^ are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.054P)^2^+2.52P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'heavy atom'
_atom_sites_solution_secondary    'difference Fourier' 
_atom_sites_solution_hydrogens
'at calculated positions, except for methyl group (located from delta-F)'
_refine_ls_hydrogen_treatment     'riding model and rigid group respectively'
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0031(3) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_number_reflns          5240 
_refine_ls_number_parameters      226 
_refine_ls_number_restraints      9 
_refine_ls_R_factor_all           0.0388 
_refine_ls_R_factor_gt            0.0361 
_refine_ls_wR_factor_ref          0.0987 
_refine_ls_wR_factor_gt           0.0959 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.052 
_refine_ls_shift/su_max           0.003 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Au1 Au 0.87109(3) -0.262282(18) -0.181563(17) 0.02858(9) Uani 1 d . . . 
Au2 Au 0.66245(2) -0.14707(2) 0.022356(16) 0.02751(9) Uani 1 d . . . 
Cl2 Cl 0.40482(18) -0.19200(16) -0.07814(13) 0.0390(3) Uani 1 d . . . 
Cl1 Cl 0.9728(2) -0.40548(15) -0.09675(14) 0.0418(3) Uani 1 d . . . 
S1 S 0.78119(17) -0.14042(13) -0.29061(11) 0.0281(3) Uani 1 d . . . 
C2 C 0.9713(7) -0.0826(6) -0.3335(5) 0.0294(11) Uani 1 d . . . 
H2A H 1.0096 -0.1515 -0.3952 0.035 Uiso 1 calc R . . 
H2B H 0.9393 -0.0137 -0.3649 0.035 Uiso 1 calc R . . 
C3 C 1.1205(7) -0.0348(6) -0.2465(5) 0.0327(11) Uani 1 d . . . 
H3A H 1.2116 -0.0097 -0.2839 0.039 Uiso 1 calc R . . 
H3B H 1.1600 -0.1052 -0.2193 0.039 Uiso 1 calc R . . 
S4 S 1.08238(16) 0.09842(13) -0.12450(11) 0.0271(3) Uani 1 d . . . 
C5 C 1.0377(7) 0.2297(5) -0.1818(5) 0.0296(11) Uani 1 d . . . 
H5A H 1.0956 0.3069 -0.1312 0.036 Uiso 1 calc R . . 
H5B H 1.0828 0.2116 -0.2554 0.036 Uiso 1 calc R . . 
C6 C 0.8495(7) 0.2534(5) -0.1964(4) 0.0267(10) Uani 1 d . . . 
H6A H 0.7999 0.2543 -0.1270 0.032 Uiso 1 calc R . . 
H6B H 0.8355 0.3373 -0.2069 0.032 Uiso 1 calc R . . 
N7 N 0.7560(5) 0.1570(4) -0.2936(4) 0.0229(8) Uani 1 d . . . 
C8 C 0.6151(6) 0.0864(5) -0.2689(5) 0.0280(10) Uani 1 d . . . 
H8A H 0.5512 0.0383 -0.3400 0.034 Uiso 1 calc R . . 
H8B H 0.5393 0.1464 -0.2243 0.034 Uiso 1 calc R . . 
C9 C 0.6754(7) -0.0033(5) -0.2049(5) 0.0261(10) Uani 1 d . . . 
H9A H 0.5788 -0.0336 -0.1756 0.031 Uiso 1 calc R . . 
H9B H 0.7536 0.0429 -0.1400 0.031 Uiso 1 calc R . . 
S S 0.73637(14) 0.19336(12) -0.41325(9) 0.0226(2) Uani 1 d . . . 
O1 O 0.6770(5) 0.0796(4) -0.4997(3) 0.0329(8) Uani 1 d . . . 
O2 O 0.8952(5) 0.2506(4) -0.4203(3) 0.0308(8) Uani 1 d . . . 
C1P C 0.5811(6) 0.3076(4) -0.4017(3) 0.0240(9) Uani 1 d D . . 
C2P C 0.4126(6) 0.2679(5) -0.4246(3) 0.0277(10) Uani 1 d D . . 
H2P H 0.3813 0.1811 -0.4486 0.033 Uiso 1 calc R . . 
C3P C 0.2920(6) 0.3594(5) -0.4112(4) 0.0325(12) Uani 1 d D . . 
H3P H 0.1775 0.3337 -0.4261 0.039 Uiso 1 calc R . . 
C4P C 0.3353(6) 0.4883(5) -0.3763(4) 0.0304(11) Uani 1 d D . . 
C5P C 0.5053(7) 0.5238(5) -0.3538(4) 0.0316(11) Uani 1 d D . . 
H5P H 0.5371 0.6104 -0.3296 0.038 Uiso 1 calc R . . 
C6P C 0.6289(6) 0.4350(5) -0.3659(4) 0.0294(11) Uani 1 d D . . 
H6P H 0.7433 0.4607 -0.3502 0.035 Uiso 1 calc R . . 
C4M C 0.2028(9) 0.5884(7) -0.3612(5) 0.0440(16) Uani 1 d D . . 
H4M1 H 0.2501 0.6648 -0.3715 0.066 Uiso 1 calc R . . 
H4M2 H 0.1667 0.6075 -0.2858 0.066 Uiso 1 calc R . . 
H4M3 H 0.1069 0.5569 -0.4167 0.066 Uiso 1 calc R . . 
Cl1S Cl 0.5565(4) -0.4159(3) 0.1146(2) 0.0747(6) Uani 1 d . A -1 
C1S C 0.594(2) -0.5117(17) -0.0083(15) 0.056(4) Uiso 0.50 d PG A -1 
H1S1 H 0.6739 -0.5043 -0.0592 0.068 Uiso 0.50 d PG A -1 
H1S2 H 0.6086 -0.5933 0.0030 0.068 Uiso 0.50 d PG A -1 
 
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 0.03363(13) 0.02231(12) 0.02906(13) 0.00586(9) 0.00547(9) 0.00216(8) 
Au2 0.02401(12) 0.03380(14) 0.02419(12) 0.00844(9) 0.00052(8) 0.00251(8) 
Cl2 0.0290(6) 0.0454(8) 0.0397(7) 0.0119(6) -0.0075(5) -0.0022(6) 
Cl1 0.0540(9) 0.0324(7) 0.0428(8) 0.0163(6) 0.0071(7) 0.0058(6) 
S1 0.0312(6) 0.0242(6) 0.0261(6) 0.0035(5) 0.0017(5) 0.0007(5) 
C2 0.031(3) 0.031(3) 0.024(2) 0.003(2) 0.009(2) 0.007(2) 
C3 0.026(2) 0.035(3) 0.037(3) 0.009(2) 0.009(2) 0.003(2) 
S4 0.0234(6) 0.0303(6) 0.0251(6) 0.0052(5) 0.0001(4) 0.0016(5) 
C5 0.029(2) 0.029(3) 0.031(3) 0.011(2) -0.002(2) 0.001(2) 
C6 0.027(2) 0.024(2) 0.025(2) 0.0008(19) 0.0005(19) 0.0039(19) 
N7 0.0210(18) 0.023(2) 0.0234(19) 0.0062(16) -0.0006(15) 0.0007(15) 
C8 0.018(2) 0.032(3) 0.035(3) 0.011(2) 0.0066(19) 0.0025(19) 
C9 0.025(2) 0.029(3) 0.029(2) 0.015(2) 0.0066(19) 0.003(2) 
S 0.0203(5) 0.0250(6) 0.0209(5) 0.0041(5) 0.0031(4) 0.0004(4) 
O1 0.037(2) 0.030(2) 0.0268(18) 0.0021(16) 0.0035(16) 0.0031(17) 
O2 0.0206(16) 0.041(2) 0.0316(19) 0.0108(17) 0.0071(14) 0.0006(16) 
C1P 0.023(2) 0.025(2) 0.023(2) 0.0057(18) 0.0018(18) 0.0016(18) 
C2P 0.021(2) 0.030(3) 0.029(2) 0.005(2) -0.0003(18) -0.0027(19) 
C3P 0.019(2) 0.040(3) 0.036(3) 0.009(2) -0.001(2) -0.003(2) 
C4P 0.026(2) 0.038(3) 0.026(2) 0.009(2) 0.0001(19) 0.005(2) 
C5P 0.031(3) 0.025(3) 0.037(3) 0.008(2) 0.001(2) 0.000(2) 
C6P 0.023(2) 0.027(3) 0.040(3) 0.013(2) 0.005(2) -0.0028(19) 
C4M 0.039(3) 0.048(4) 0.049(4) 0.018(3) 0.010(3) 0.021(3) 
Cl1S 0.0974(18) 0.0739(15) 0.0490(11) 0.0163(11) -0.0042(11) -0.0054(13) 
 
_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 Au2 3.1155(5) .      Yes
Au1 S1 2.2581(14) .      Yes
Au2 S4 2.2711(13) 2_755  Yes
Au1 Cl1 2.2664(15) .     Yes
Au2 Cl1 2.2770(14) .     Yes
S1 C2 1.826(6) . ?
S1 C9 1.833(5) . ? 
C2 C3 1.511(8) . ? 
C3 S4 1.823(6) . ? 
S4 C5 1.822(6) . ? 
C5 C6 1.529(7) . ? 
C6 N7 1.488(6) . ? 
N7 C8 1.471(6) . ? 
N7 S 1.650(4) . ? 
C8 C9 1.502(7) . ? 
S O1 1.434(4) . ? 
S O2 1.435(4) . ? 
S C1P 1.759(5) . ? 
C1P C6P 1.384(6) . ? 
C1P C2P 1.389(6) . ? 
C2P C3P 1.385(6) . ? 
C3P C4P 1.391(6) . ? 
C4P C5P 1.390(6) . ? 
C4P C4M 1.517(8) . ? 
C5P C6P 1.380(6) . ? 
Cl1S C1S 1.634(18) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
S1 Au1 Cl1 171.27(5) . .     Yes 
S1 Au1 Au2 98.73(3) . .      Yes 
Cl1 Au1 Au2 89.47(4) . .     Yes 
S4 Au2 Cl1 178.86(5) 2_755 . Yes 
S4 Au2 Au1 84.72(3) 2_755 .  Yes 
Cl1 Au2 Au1 96.13(4) . .     Yes 
C2 S1 C9 108.1(2) . . ? 
C2 S1 Au1 105.7(2) . . ? 
C9 S1 Au1 109.17(17) . . ? 
C3 C2 S1 119.0(4) . . ? 
C2 C3 S4 115.9(4) . . ? 
C5 S4 C3 104.8(3) . . ? 
C5 S4 Au2 105.89(19) . 2_755 ? 
C3 S4 Au2 104.56(19) . 2_755 ? 
C6 C5 S4 113.0(4) . . ? 
N7 C6 C5 113.6(4) . . ? 
C8 N7 C6 117.2(4) . . ? 
C8 N7 S 117.7(3) . . ? 
C6 N7 S 115.2(4) . . ? 
N7 C8 C9 111.8(4) . . ? 
C8 C9 S1 113.4(4) . . ? 
O1 S O2 119.1(2) . . ? 
O1 S N7 106.3(2) . . ? 
O2 S N7 105.8(2) . . ? 
O1 S C1P 108.9(2) . . ? 
O2 S C1P 108.7(2) . . ? 
N7 S C1P 107.4(2) . . ? 
C6P C1P C2P 121.5(5) . . ? 
C6P C1P S 119.4(3) . . ? 
C2P C1P S 119.1(4) . . ? 
C3P C2P C1P 118.2(5) . . ? 
C2P C3P C4P 121.9(5) . . ? 
C5P C4P C3P 117.9(5) . . ? 
C5P C4P C4M 120.3(5) . . ? 
C3P C4P C4M 121.8(5) . . ? 
C6P C5P C4P 121.7(5) . . ? 
C5P C6P C1P 118.8(5) . . ? 
 
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 
S1 Au1 Au2 S4 -119.78(5) . . . 2_755 ? 
Cl1 Au1 Au2 S4 63.25(6) . . . 2_755 ? 
S1 Au1 Au2 Cl1 59.46(6) . . . . ? 
Cl1 Au1 Au2 Cl1 -117.51(6) . . . . ? 
C9 S1 C2 C3 73.0(5) . . . . ? 
S1 C2 C3 S4 -59.5(6) . . . . ? 
C2 C3 S4 C5 -65.5(5) . . . . ? 
C3 S4 C5 C6 100.8(4) . . . . ? 
S4 C5 C6 N7 -74.1(5) . . . . ? 
C5 C6 N7 C8 121.8(5) . . . . ? 
C5 C6 N7 S -93.2(5) . . . . ? 
C6 N7 C8 C9 -69.5(6) . . . . ? 
S N7 C8 C9 146.3(4) . . . . ? 
N7 C8 C9 S1 -71.2(5) . . . . ? 
C2 S1 C9 C8 63.7(4) . . . . ? 
C8 N7 S O1 -47.4(4) . . . . ? 
C6 N7 S O1 167.8(3) . . . . ? 
C8 N7 S O2 -174.9(4) . . . . ? 
C6 N7 S O2 40.3(4) . . . . ? 
C8 N7 S C1P 69.1(4) . . . . ? 
C6 N7 S C1P -75.7(4) . . . . ? 
O1 S C1P C6P -151.1(3) . . . . ? 
O2 S C1P C6P -20.0(4) . . . . ? 
N7 S C1P C6P 94.1(3) . . . . ? 
O1 S C1P C2P 31.4(3) . . . . ? 
O2 S C1P C2P 162.5(3) . . . . ? 
N7 S C1P C2P -83.4(3) . . . . ? 
C6P C1P C2P C3P 0.3(2) . . . . ? 
S C1P C2P C3P 177.7(3) . . . . ? 
C1P C2P C3P C4P 0.3(2) . . . . ? 
C2P C3P C4P C5P -0.6(5) . . . . ? 
C2P C3P C4P C4M -179.8(3) . . . . ? 
C3P C4P C5P C6P 0.4(6) . . . . ? 
C4M C4P C5P C6P 179.6(4) . . . . ? 
C4P C5P C6P C1P 0.1(6) . . . . ? 
C2P C1P C6P C5P -0.5(5) . . . . ? 
S C1P C6P C5P -177.9(3) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.859 
_diffrn_reflns_theta_full              30.02 
_diffrn_measured_fraction_theta_full   0.859 
_refine_diff_density_max    2.08 
_refine_diff_density_min   -2.59 
_refine_diff_density_rms    0.23