 
data_shelx
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety 'C15 H12 N2 S7, C8 Au N4 S4'
_chemical_formula_sum     'C23 H12 Au N6 S11'
_chemical_formula_weight          922.01
 
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'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Au'  'Au'  -2.0133   8.8022
 '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'
 
_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                    7.25300(10)
_cell_length_b                    8.38770(10)
_cell_length_c                    26.2705(4)
_cell_angle_alpha                 86.2350(10)
_cell_angle_beta                  86.1760(10)
_cell_angle_gamma                 71.7200(10)
_cell_volume                      1512.47(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used    9820
_cell_measurement_theta_min        2.64
_cell_measurement_theta_max       27.25

_exptl_crystal_description       'plate'
_exptl_crystal_colour            'yellow'
_exptl_crystal_size_max           0.40
_exptl_crystal_size_mid           0.10
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.025
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              894
_exptl_absorpt_coefficient_mu     5.652
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.2108
_exptl_absorpt_correction_T_max   0.8055
_exptl_absorpt_process_details    sadabs
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       150(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 APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             25691
_diffrn_reflns_av_R_equivalents   0.0262
_diffrn_reflns_av_sigmaI/netI     0.0200
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -10
_diffrn_reflns_limit_k_max        10
_diffrn_reflns_limit_l_min        -32
_diffrn_reflns_limit_l_max        32
_diffrn_reflns_theta_min          2.56
_diffrn_reflns_theta_max          26.37
_reflns_number_total              6102
_reflns_number_gt                 6057
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection      'Bruker APEX2'
_computing_cell_refinement      'Bruker SAINT'
_computing_data_reduction       'Bruker SAINT' 
_computing_structure_solution   'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0000P)²+2.2448P] where P=(Fo²+2Fc²)/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          6102
_refine_ls_number_parameters      390
_refine_ls_number_restraints      12
_refine_ls_R_factor_all           0.0175
_refine_ls_R_factor_gt            0.0173
_refine_ls_wR_factor_ref          0.0421
_refine_ls_wR_factor_gt           0.0420
_refine_ls_goodness_of_fit_ref    1.253
_refine_ls_restrained_S_all       1.252
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Au1 Au 0.186082(13) 0.119884(11) 0.308248(4) 0.01273(3) Uani 1 1 d . . .
S1 S -0.14267(10) 0.22331(8) 0.32721(3) 0.01852(14) Uani 1 1 d . . .
S2 S 0.22676(10) -0.05776(8) 0.38058(3) 0.01960(14) Uani 1 1 d . . .
S3 S 0.13144(9) 0.30331(8) 0.23745(3) 0.01660(13) Uani 1 1 d . . .
S4 S 0.51614(9) 0.02442(8) 0.28644(3) 0.01719(13) Uani 1 1 d . . .
S5 S 0.00711(9) 0.75040(8) 0.28292(2) 0.01590(13) Uani 1 1 d . A .
S6 S 0.33582(9) 0.50141(8) 0.33239(2) 0.01557(13) Uani 1 1 d . A .
S8 S 0.28345(9) 0.83446(8) 0.19649(2) 0.01404(12) Uani 1 1 d . . .
S9 S 0.62247(9) 0.57867(8) 0.23637(2) 0.01407(12) Uani 1 1 d . . .
S10 S 0.51851(9) 0.94655(8) 0.10988(2) 0.01494(13) Uani 1 1 d . . .
S11 S 0.89535(9) 0.64336(8) 0.15188(2) 0.01549(13) Uani 1 1 d . . .
N1 N -0.5117(4) 0.2081(4) 0.42438(11) 0.0354(7) Uani 1 1 d . . .
N2 N -0.0548(5) -0.1802(4) 0.48776(11) 0.0401(7) Uani 1 1 d . . .
N3 N 0.3888(3) 0.4531(3) 0.13081(10) 0.0238(5) Uani 1 1 d . . .
N4 N 0.8574(3) 0.0907(3) 0.18151(10) 0.0235(5) Uani 1 1 d . . .
N5 N 0.3867(5) 0.8137(4) -0.01747(11) 0.0371(7) Uani 1 1 d . . .
N6 N 0.9038(4) 0.7310(3) 0.00641(10) 0.0268(6) Uani 1 1 d . . .
C1 C -0.1636(4) 0.1114(3) 0.38432(10) 0.0174(5) Uani 1 1 d . . .
C2 C -0.0117(4) -0.0072(3) 0.40575(10) 0.0181(5) Uani 1 1 d . . .
C3 C -0.3559(4) 0.1587(4) 0.40766(11) 0.0226(6) Uani 1 1 d . . .
C4 C -0.0385(5) -0.1015(4) 0.45173(11) 0.0248(6) Uani 1 1 d . . .
C5 C 0.3666(4) 0.2638(3) 0.21082(10) 0.0153(5) Uani 1 1 d . . .
C6 C 0.5253(4) 0.1471(3) 0.23072(10) 0.0156(5) Uani 1 1 d . . .
C7 C 0.3836(4) 0.3656(3) 0.16592(10) 0.0160(5) Uani 1 1 d . . .
C8 C 0.7113(4) 0.1162(3) 0.20411(10) 0.0176(5) Uani 1 1 d . . .
C9 C -0.0440(4) 0.6543(3) 0.33952(10) 0.0154(5) Uani 1 1 d . . .
C10 C 0.1090(4) 0.5370(3) 0.36280(10) 0.0161(5) Uani 1 1 d . A .
C12 C -0.1716(4) 0.5530(4) 0.41647(11) 0.0206(6) Uani 1 1 d . . .
C13 C -0.3062(5) 0.5316(5) 0.46030(13) 0.0394(9) Uani 1 1 d . A .
H13A H -0.2466 0.4253 0.4793 0.059 Uiso 1 1 calc R . .
H13B H -0.4293 0.5305 0.4473 0.059 Uiso 1 1 calc R . .
H13C H -0.3309 0.6251 0.4830 0.059 Uiso 1 1 calc R . .
C14 C 0.2540(4) 0.6443(3) 0.28216(9) 0.0130(5) Uani 1 1 d . . .
C15 C 0.3767(4) 0.6783(3) 0.24282(9) 0.0124(5) Uani 1 1 d . A .
C16 C 0.5029(4) 0.8116(3) 0.16223(9) 0.0123(5) Uani 1 1 d . . .
C17 C 0.6605(4) 0.6904(3) 0.18025(9) 0.0130(5) Uani 1 1 d . . .
C18 C 0.2676(4) 1.0366(3) 0.09318(10) 0.0191(6) Uani 1 1 d . . .
H18A H 0.1866 1.0727 0.1247 0.023 Uiso 1 1 calc R . .
H18B H 0.2560 1.1382 0.0706 0.023 Uiso 1 1 calc R . .
C19 C 0.8961(4) 0.4721(3) 0.11254(10) 0.0193(6) Uani 1 1 d . . .
H19A H 1.0315 0.4146 0.1004 0.023 Uiso 1 1 calc R . .
H19B H 0.8497 0.3895 0.1340 0.023 Uiso 1 1 calc R . .
C20 C 0.1857(4) 0.9188(4) 0.06639(11) 0.0245(6) Uani 1 1 d . . .
H20A H 0.1868 0.8211 0.0898 0.029 Uiso 1 1 calc R . .
H20B H 0.0490 0.9788 0.0585 0.029 Uiso 1 1 calc R . .
C21 C 0.7705(4) 0.5280(4) 0.06655(11) 0.0210(6) Uani 1 1 d . . .
H21A H 0.7731 0.4283 0.0480 0.025 Uiso 1 1 calc R . .
H21B H 0.6343 0.5847 0.0783 0.025 Uiso 1 1 calc R . .
C22 C 0.2976(5) 0.8588(4) 0.01892(12) 0.0258(6) Uani 1 1 d . . .
C23 C 0.8414(4) 0.6442(3) 0.03186(10) 0.0195(6) Uani 1 1 d . . .
S7 S -0.2689(4) 0.6910(3) 0.37020(7) 0.0167(4) Uani 0.551(4) 1 d P A 1
C11 C 0.0333(14) 0.4734(11) 0.4087(4) 0.022(3) Uani 0.551(4) 1 d PU A 1
H11 H 0.1096 0.3888 0.4313 0.026 Uiso 0.551(4) 1 calc PR A 1
C11A C -0.2118(16) 0.6651(14) 0.3710(4) 0.023(3) Uani 0.449(4) 1 d PU A 2
H11A H -0.3376 0.7377 0.3635 0.028 Uiso 0.449(4) 1 calc PR A 2
S7A S 0.0584(4) 0.4413(4) 0.41922(10) 0.0154(5) Uani 0.449(4) 1 d P A 2
 
 
_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 S1 2.2994(7) . ?
Au1 S3 2.3072(6) . ?
Au1 S2 2.3120(7) . ?
Au1 S4 2.3184(6) . ?
S1 C1 1.740(3) . ?
S2 C2 1.741(3) . ?
S3 C5 1.739(3) . ?
S4 C6 1.743(3) . ?
S5 C9 1.719(3) . ?
S5 C14 1.731(3) . ?
S6 C14 1.726(3) . ?
S6 C10 1.726(3) . ?
S8 C15 1.732(3) . ?
S8 C16 1.738(2) . ?
S9 C15 1.717(3) . ?
S9 C17 1.748(2) . ?
S10 C16 1.744(2) . ?
S10 C18 1.810(3) . ?
S11 C17 1.750(2) . ?
S11 C19 1.822(3) . ?
N1 C3 1.143(4) . ?
N2 C4 1.140(4) . ?
N3 C7 1.146(4) . ?
N4 C8 1.145(4) . ?
N5 C22 1.134(4) . ?
N6 C23 1.134(4) . ?
C1 C2 1.358(4) . ?
C1 C3 1.431(4) . ?
C2 C4 1.436(4) . ?
C5 C6 1.365(4) . ?
C5 C7 1.432(4) . ?
C6 C8 1.433(4) . ?
C9 C10 1.379(4) . ?
C9 C11A 1.407(11) . ?
C9 S7 1.717(3) . ?
C10 C11 1.433(10) . ?
C10 S7A 1.712(4) . ?
C12 C11 1.432(10) . ?
C12 C11A 1.457(12) . ?
C12 C13 1.498(4) . ?
C12 S7A 1.641(4) . ?
C12 S7 1.653(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.392(3) . ?
C16 C17 1.358(4) . ?
C18 C20 1.529(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C21 1.521(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C22 1.469(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C23 1.476(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C11 H11 0.9500 . ?
C11A H11A 0.9500 . ?
 
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 S3 86.53(2) . . ?
S1 Au1 S2 90.94(2) . . ?
S3 Au1 S2 177.42(2) . . ?
S1 Au1 S4 177.59(2) . . ?
S3 Au1 S4 91.10(2) . . ?
S2 Au1 S4 91.43(2) . . ?
C1 S1 Au1 101.06(10) . . ?
C2 S2 Au1 100.64(9) . . ?
C5 S3 Au1 100.86(9) . . ?
C6 S4 Au1 100.43(9) . . ?
C9 S5 C14 94.50(12) . . ?
C14 S6 C10 94.70(12) . . ?
C15 S8 C16 95.95(12) . . ?
C15 S9 C17 95.77(12) . . ?
C16 S10 C18 102.74(12) . . ?
C17 S11 C19 100.06(12) . . ?
C2 C1 C3 122.6(3) . . ?
C2 C1 S1 123.5(2) . . ?
C3 C1 S1 113.9(2) . . ?
C1 C2 C4 121.3(3) . . ?
C1 C2 S2 123.8(2) . . ?
C4 C2 S2 114.9(2) . . ?
N1 C3 C1 174.7(3) . . ?
N2 C4 C2 177.9(4) . . ?
C6 C5 C7 121.5(2) . . ?
C6 C5 S3 123.7(2) . . ?
C7 C5 S3 114.76(19) . . ?
C5 C6 C8 119.5(2) . . ?
C5 C6 S4 123.9(2) . . ?
C8 C6 S4 116.6(2) . . ?
N3 C7 C5 176.5(3) . . ?
N4 C8 C6 177.9(3) . . ?
C10 C9 C11A 106.9(5) . . ?
C10 C9 S7 116.5(2) . . ?
C11A C9 S7 9.6(5) . . ?
C10 C9 S5 117.42(19) . . ?
C11A C9 S5 135.6(5) . . ?
S7 C9 S5 126.08(18) . . ?
C9 C10 C11 107.8(4) . . ?
C9 C10 S7A 117.5(2) . . ?
C11 C10 S7A 9.7(4) . . ?
C9 C10 S6 116.62(19) . . ?
C11 C10 S6 135.6(4) . . ?
S7A C10 S6 125.89(19) . . ?
C11 C12 C11A 100.9(5) . . ?
C11 C12 C13 129.5(4) . . ?
C11A C12 C13 129.5(5) . . ?
C11 C12 S7A 12.1(4) . . ?
C11A C12 S7A 113.0(5) . . ?
C13 C12 S7A 117.5(3) . . ?
C11 C12 S7 113.9(4) . . ?
C11A C12 S7 13.1(4) . . ?
C13 C12 S7 116.5(3) . . ?
S7A C12 S7 126.01(19) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 S6 123.18(19) . . ?
C15 C14 S5 120.06(19) . . ?
S6 C14 S5 116.75(14) . . ?
C14 C15 S9 124.94(19) . . ?
C14 C15 S8 119.78(19) . . ?
S9 C15 S8 115.27(14) . . ?
C17 C16 S8 116.34(18) . . ?
C17 C16 S10 122.65(19) . . ?
S8 C16 S10 120.91(14) . . ?
C16 C17 S9 116.64(18) . . ?
C16 C17 S11 124.47(19) . . ?
S9 C17 S11 118.88(14) . . ?
C20 C18 S10 114.85(19) . . ?
C20 C18 H18A 108.6 . . ?
S10 C18 H18A 108.6 . . ?
C20 C18 H18B 108.6 . . ?
S10 C18 H18B 108.6 . . ?
H18A C18 H18B 107.5 . . ?
C21 C19 S11 113.98(19) . . ?
C21 C19 H19A 108.8 . . ?
S11 C19 H19A 108.8 . . ?
C21 C19 H19B 108.8 . . ?
S11 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C22 C20 C18 112.2(2) . . ?
C22 C20 H20A 109.2 . . ?
C18 C20 H20A 109.2 . . ?
C22 C20 H20B 109.2 . . ?
C18 C20 H20B 109.2 . . ?
H20A C20 H20B 107.9 . . ?
C23 C21 C19 110.7(2) . . ?
C23 C21 H21A 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C23 C21 H21B 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
N5 C22 C20 178.7(3) . . ?
N6 C23 C21 176.7(3) . . ?
C12 S7 C9 90.04(18) . . ?
C12 C11 C10 111.7(6) . . ?
C12 C11 H11 124.1 . . ?
C10 C11 H11 124.1 . . ?
C9 C11A C12 112.7(7) . . ?
C9 C11A H11A 123.7 . . ?
C12 C11A H11A 123.7 . . ?
C12 S7A C10 89.9(2) . . ?
 
_diffrn_measured_fraction_theta_max    0.987
_diffrn_reflns_theta_full              26.37
_diffrn_measured_fraction_theta_full   0.987
_refine_diff_density_max    0.807
_refine_diff_density_min   -1.232
_refine_diff_density_rms    0.077
