 
data_97src112
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C6 H10 Br2 Hg N2 S4' 
_chemical_formula_weight          598.81 
_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'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'S'  'S'   0.1246   0.1234 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Hg'  'Hg'  -2.3894   9.2266 
 '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                    7.6230(10) 
_cell_length_b                    8.9510(10) 
_cell_length_c                    10.914(2) 
_cell_angle_alpha                 82.760(10) 
_cell_angle_beta                  73.330(6) 
_cell_angle_gamma                 80.54(2) 
_cell_volume                      701.2(2) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     2553
_cell_measurement_theta_min       1.95
_cell_measurement_theta_max       25.01
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.08
_exptl_crystal_size_min           0.08
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     2.836 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              548 
_exptl_absorpt_coefficient_mu     17.239 
_exptl_absorpt_correction_type    refdelf
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71069 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'Nonius FR571 rotating anode' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device        'Nonius FAST TV area detector'
_diffrn_measurement_method        'Φ & ω scans'
_diffrn_standards_number          9.091
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             2553 
_diffrn_reflns_av_R_equivalents   0.0541 
_diffrn_reflns_av_sigmaI/netI     0.0487 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        6 
_diffrn_reflns_limit_k_min        -10 
_diffrn_reflns_limit_k_max        8 
_diffrn_reflns_limit_l_min        -12 
_diffrn_reflns_limit_l_max        12 
_diffrn_reflns_theta_min          1.95 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              1907 
_reflns_number_observed           1734 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        
'MADNESS (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        
'MADNESS (Pflugrath & Messerschmidt, 1989)'
_computing_data_reduction         
'MADNESS (Pflugrath & Messerschmidt, 1989)'
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-92 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F² for ALL reflections except for 0 with very negative F² 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses of fit S are based on F², conventional R-factors R 
 are based on F, with F set to zero for negative F². The observed criterion 
 of F² > 2sigma(F²) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1907 
_refine_ls_number_parameters      136 
_refine_ls_number_restraints      6 
_refine_ls_R_factor_all           0.0396 
_refine_ls_R_factor_obs           0.0372 
_refine_ls_wR_factor_all          0.1008 
_refine_ls_wR_factor_obs          0.1001 
_refine_ls_goodness_of_fit_all    1.035 
_refine_ls_goodness_of_fit_obs    1.081 
_refine_ls_restrained_S_all       1.034 
_refine_ls_restrained_S_obs       1.080 
_refine_ls_shift/esd_max          -0.003 
_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 
Hg1 Hg 0.09467(6) 0.28390(4) 0.26865(4) 0.0162(2) Uani 1 d . . 
Br1 Br 0.26929(14) 0.19519(11) 0.03627(10) 0.0154(3) Uani 1 d . . 
Br2 Br 0.35075(14) 0.29181(11) 0.38605(10) 0.0165(3) Uani 1 d . . 
S1 S -0.1002(4) 0.0780(3) 0.3647(3) 0.0160(6) Uani 1 d . . 
S2 S -0.2478(4) 0.3347(3) 0.5375(3) 0.0199(7) Uani 1 d . . 
S3 S -0.0389(4) 0.5612(3) 0.2551(3) 0.0186(6) Uani 1 d . . 
S4 S 0.1364(4) 0.8267(3) 0.1095(3) 0.0165(6) Uani 1 d . . 
N1 N -0.3714(12) 0.0813(10) 0.5813(8) 0.014(2) Uani 1 d . . 
H1 H -0.3849(12) -0.0093(10) 0.5709(8) 0.017 Uiso 1 calc R . 
N2 N 0.1857(12) 0.5739(9) 0.0136(8) 0.014(2) Uani 1 d . . 
H2 H 0.1704(12) 0.4836(9) 0.0035(8) 0.017 Uiso 1 calc R . 
C1 C -0.2459(15) 0.1554(11) 0.4957(11) 0.015(2) Uani 1 d . . 
C2 C -0.4831(17) 0.1563(13) 0.6911(11) 0.024(3) Uani 1 d . . 
H2A H -0.4465(17) 0.1112(13) 0.7671(11) 0.029 Uiso 1 calc R . 
H2B H -0.6120(17) 0.1459(13) 0.7041(11) 0.029 Uiso 1 calc R . 
C3 C -0.4571(16) 0.3236(12) 0.6680(11) 0.022(3) Uani 1 d . . 
H3A H -0.4442(16) 0.3600(12) 0.7446(11) 0.027 Uiso 1 calc R . 
H3B H -0.5620(16) 0.3844(12) 0.6445(11) 0.027 Uiso 1 calc R . 
C4 C 0.0984(14) 0.6394(11) 0.1192(10) 0.013(2) Uani 1 d . . 
C5 C 0.3101(15) 0.6609(11) -0.0860(11) 0.017(2) Uani 1 d . . 
H5A H 0.3017(15) 0.6444(11) -0.1702(11) 0.020 Uiso 1 calc R . 
H5B H 0.4368(15) 0.6303(11) -0.0826(11) 0.020 Uiso 1 calc R . 
C6 C 0.2500(15) 0.8252(11) -0.0603(10) 0.016(2) Uani 1 d U . 
H6A H 0.1656(15) 0.8725(11) -0.1100(10) 0.020 Uiso 1 calc R . 
H6B H 0.3561(15) 0.8801(11) -0.0829(10) 0.020 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 
Hg1 0.0171(3) 0.0145(3) 0.0160(3) 0.0011(2) -0.0030(2) -0.0042(2) 
Br1 0.0192(6) 0.0105(6) 0.0160(6) -0.0037(4) -0.0030(5) -0.0019(4) 
Br2 0.0206(6) 0.0101(6) 0.0214(6) -0.0003(5) -0.0097(5) -0.0037(4) 
S1 0.022(2) 0.012(2) 0.0139(14) -0.0020(11) -0.0016(12) -0.0050(11) 
S2 0.026(2) 0.011(2) 0.020(2) -0.0055(12) 0.0036(12) -0.0095(12) 
S3 0.0199(15) 0.014(2) 0.017(2) 0.0020(12) 0.0012(12) -0.0010(11) 
S4 0.024(2) 0.008(2) 0.019(2) -0.0032(12) -0.0065(12) -0.0033(11) 
N1 0.017(5) 0.009(5) 0.015(5) 0.001(4) -0.004(4) -0.006(4) 
N2 0.021(5) 0.008(5) 0.009(5) -0.006(4) 0.007(4) -0.005(4) 
C1 0.022(6) 0.006(6) 0.022(6) 0.001(5) -0.016(5) -0.003(4) 
C2 0.027(7) 0.031(8) 0.015(6) -0.000(5) 0.003(5) -0.019(6) 
C3 0.026(7) 0.010(7) 0.027(7) -0.002(5) -0.000(5) -0.007(5) 
C4 0.012(6) 0.012(6) 0.016(6) -0.002(5) -0.006(5) -0.000(4) 
C5 0.015(6) 0.014(7) 0.020(6) -0.006(5) 0.001(5) -0.002(4) 
C6 0.015(4) 0.013(4) 0.021(4) 0.003(3) -0.006(3) -0.004(3) 
 
_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 
Hg1 S1 2.494(3) . ? 
Hg1 S3 2.526(3) . ? 
Hg1 Br2 2.6384(11) . ? 
Hg1 Br1 2.6567(12) . ? 
S1 C1 1.686(12) . ? 
S2 C1 1.720(10) . ? 
S2 C3 1.815(12) . ? 
S3 C4 1.695(11) . ? 
S4 C4 1.733(10) . ? 
S4 C6 1.808(11) . ? 
N1 C1 1.330(14) . ? 
N1 C2 1.428(14) . ? 
N2 C4 1.311(13) . ? 
N2 C5 1.458(13) . ? 
C2 C3 1.523(15) . ? 
C5 C6 1.504(14) . ? 
 
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 Hg1 S3 122.60(9) . . ? 
S1 Hg1 Br2 112.73(7) . . ? 
S3 Hg1 Br2 101.03(7) . . ? 
S1 Hg1 Br1 102.34(7) . . ? 
S3 Hg1 Br1 110.67(7) . . ? 
Br2 Hg1 Br1 106.82(4) . . ? 
C1 S1 Hg1 101.7(4) . . ? 
C1 S2 C3 92.9(5) . . ? 
C4 S3 Hg1 105.1(4) . . ? 
C4 S4 C6 91.7(5) . . ? 
C1 N1 C2 118.2(8) . . ? 
C4 N2 C5 117.0(8) . . ? 
N1 C1 S1 123.1(8) . . ? 
N1 C1 S2 111.9(8) . . ? 
S1 C1 S2 125.0(7) . . ? 
N1 C2 C3 108.2(9) . . ? 
C2 C3 S2 105.8(8) . . ? 
N2 C4 S3 127.4(8) . . ? 
N2 C4 S4 112.4(8) . . ? 
S3 C4 S4 120.2(6) . . ? 
N2 C5 C6 106.5(8) . . ? 
C5 C6 S4 106.2(7) . . ? 
 
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 Hg1 S1 C1 -42.3(4) . . . . ? 
 Br2 Hg1 S1 C1 78.7(4) . . . . ? 
 Br1 Hg1 S1 C1 -166.9(4) . . . . ? 
 S1 Hg1 S3 C4 -147.9(4) . . . . ? 
 Br2 Hg1 S3 C4 85.9(4) . . . . ? 
 Br1 Hg1 S3 C4 -27.0(4) . . . . ? 
 C2 N1 C1 S1 177.8(8) . . . . ? 
 C2 N1 C1 S2 -0.6(12) . . . . ? 
 Hg1 S1 C1 N1 -176.5(8) . . . . ? 
 Hg1 S1 C1 S2 1.7(7) . . . . ? 
 C3 S2 C1 N1 -9.0(8) . . . . ? 
 C3 S2 C1 S1 172.7(8) . . . . ? 
 C1 N1 C2 C3 12.3(14) . . . . ? 
 N1 C2 C3 S2 -17.1(11) . . . . ? 
 C1 S2 C3 C2 14.9(8) . . . . ? 
 C5 N2 C4 S3 -174.3(8) . . . . ? 
 C5 N2 C4 S4 5.7(12) . . . . ? 
 Hg1 S3 C4 N2 31.9(10) . . . . ? 
 Hg1 S3 C4 S4 -148.1(5) . . . . ? 
 C6 S4 C4 N2 9.3(8) . . . . ? 
 C6 S4 C4 S3 -170.7(7) . . . . ? 
 C4 N2 C5 C6 -21.2(13) . . . . ? 
 N2 C5 C6 S4 25.6(10) . . . . ? 
 C4 S4 C6 C5 -20.3(8) . . . . ? 
 
_refine_diff_density_max    1.704 
_refine_diff_density_min   -1.261 
_refine_diff_density_rms    0.302 
