data_05src0055
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C12 H10 S6'
_chemical_formula_sum
 'C12 H10 S6'
_chemical_formula_weight          346.56
 
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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    Pbca
_symmetry_space_group_name_hall   '-P 2ac 2ab'
 
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    14.1438(15)
_cell_length_b                    12.9258(12)
_cell_length_c                    14.7767(8)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      2701.5(4)
_cell_formula_units_Z             8
_cell_measurement_temperature     120(2)
_cell_measurement_reflns_used     3480
_cell_measurement_theta_min       2.91
_cell_measurement_theta_max       27.48
 
_exptl_crystal_description        block
_exptl_crystal_colour             colourles
_exptl_crystal_size_max           0.38
_exptl_crystal_size_mid           0.25
_exptl_crystal_size_min           0.15
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.704
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1424
_exptl_absorpt_coefficient_mu     0.988
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.7052
_exptl_absorpt_correction_T_max   0.8659
_exptl_absorpt_process_details    'SADABS V2.10 (Sheldrick, G.M., 2003)'
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       120(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker-Nonius KappaCCD Area Detector'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  9.091
_diffrn_standards_number          none
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         negligible
_diffrn_reflns_number             27114
_diffrn_reflns_av_R_equivalents   0.0345
_diffrn_reflns_av_sigmaI/netI     0.0213
_diffrn_reflns_limit_h_min        -18
_diffrn_reflns_limit_h_max        18
_diffrn_reflns_limit_k_min        -16
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -17
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          3.15
_diffrn_reflns_theta_max          27.49
_reflns_number_total              3096
_reflns_number_gt                 2684
_reflns_threshold_expression      >2sigma(I)
 
_computing_data_collection        ?
_computing_cell_refinement        'DENZO, COLLECT'
_computing_data_reduction         'DENZO, COLLECT'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'PLATON (Spek, 1990)'
_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)+(0.0269P)²+3.0483P] 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          3096
_refine_ls_number_parameters      163
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0340
_refine_ls_R_factor_gt            0.0266
_refine_ls_wR_factor_ref          0.0660
_refine_ls_wR_factor_gt           0.0618
_refine_ls_goodness_of_fit_ref    1.020
_refine_ls_restrained_S_all       1.020
_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
C1 C 0.13566(12) 0.62251(13) 0.46299(11) 0.0141(3) Uani 1 1 d . . .
C2 C 0.15478(12) 0.69688(14) 0.53250(11) 0.0156(3) Uani 1 1 d . . .
C3 C 0.11257(13) 0.55210(15) 0.65563(12) 0.0212(4) Uani 1 1 d . . .
H3A H 0.1143 0.5289 0.7195 0.025 Uiso 1 1 calc R . .
H3B H 0.0468 0.5730 0.6416 0.025 Uiso 1 1 calc R . .
C4 C 0.13987(15) 0.46240(15) 0.59503(12) 0.0229(4) Uani 1 1 d . . .
H4A H 0.0934 0.4061 0.6045 0.028 Uiso 1 1 calc R . .
H4B H 0.2022 0.4363 0.6152 0.028 Uiso 1 1 calc R . .
C5 C 0.10966(11) 0.66835(13) 0.38248(11) 0.0131(3) Uani 1 1 d . . .
C6 C 0.14398(12) 0.79626(14) 0.50349(12) 0.0170(4) Uani 1 1 d . . .
H6 H 0.1531 0.8553 0.5408 0.020 Uiso 1 1 calc R . .
C7 C 0.08498(11) 0.61923(13) 0.29685(11) 0.0123(3) Uani 1 1 d . . .
C8 C 0.08038(12) 0.50273(13) 0.16349(11) 0.0152(3) Uani 1 1 d . . .
H8 H 0.0892 0.4513 0.1183 0.018 Uiso 1 1 calc R . .
C9 C 0.01358(12) 0.64395(13) 0.23721(11) 0.0132(3) Uani 1 1 d . . .
C10 C 0.01040(12) 0.57530(13) 0.16105(11) 0.0139(3) Uani 1 1 d . . .
C11 C -0.11657(14) 0.70555(15) 0.08049(13) 0.0218(4) Uani 1 1 d . . .
H11A H -0.0635 0.7515 0.0635 0.026 Uiso 1 1 calc R . .
H11B H -0.1677 0.7155 0.0356 0.026 Uiso 1 1 calc R . .
C12 C -0.15235(13) 0.73567(15) 0.17326(13) 0.0217(4) Uani 1 1 d . . .
H12A H -0.1964 0.6816 0.1950 0.026 Uiso 1 1 calc R . .
H12B H -0.1883 0.8012 0.1682 0.026 Uiso 1 1 calc R . .
S1 S 0.18953(3) 0.66321(4) 0.64270(3) 0.02063(11) Uani 1 1 d . . .
S2 S 0.14683(5) 0.48809(4) 0.47500(3) 0.03699(16) Uani 1 1 d . . .
S5 S -0.07722(3) 0.57289(4) 0.07694(3) 0.02042(11) Uani 1 1 d . . .
S6 S -0.05914(3) 0.75219(3) 0.25565(3) 0.01843(11) Uani 1 1 d . . .
S3 S 0.11205(3) 0.80229(3) 0.39204(3) 0.01703(10) Uani 1 1 d . . .
S4 S 0.15030(3) 0.51492(3) 0.25719(3) 0.01483(10) Uani 1 1 d . . .
 
 
_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
C1 C5 1.379(2) . ?
C1 C2 1.433(2) . ?
C1 S2 1.7536(18) . ?
C2 C6 1.363(3) . ?
C2 S1 1.7557(18) . ?
C3 C4 1.515(3) . ?
C3 S1 1.8122(19) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 S2 1.8071(19) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C7 1.458(2) . ?
C5 S3 1.7375(17) . ?
C6 S3 1.7096(18) . ?
C6 H6 0.9500 . ?
C7 C9 1.378(2) . ?
C7 S4 1.7363(17) . ?
C8 C10 1.364(2) . ?
C8 S4 1.7087(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.434(2) . ?
C9 S6 1.7577(17) . ?
C10 S5 1.7554(17) . ?
C11 C12 1.512(3) . ?
C11 S5 1.8035(19) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 S6 1.8071(19) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
 
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
C5 C1 C2 112.37(15) . . ?
C5 C1 S2 122.48(13) . . ?
C2 C1 S2 125.12(13) . . ?
C6 C2 C1 112.70(16) . . ?
C6 C2 S1 123.83(14) . . ?
C1 C2 S1 123.46(14) . . ?
C4 C3 S1 113.02(13) . . ?
C4 C3 H3A 109.0 . . ?
S1 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
S1 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 S2 116.96(14) . . ?
C3 C4 H4A 108.1 . . ?
S2 C4 H4A 108.1 . . ?
C3 C4 H4B 108.1 . . ?
S2 C4 H4B 108.1 . . ?
H4A C4 H4B 107.3 . . ?
C1 C5 C7 128.72(15) . . ?
C1 C5 S3 110.66(13) . . ?
C7 C5 S3 120.61(12) . . ?
C2 C6 S3 112.06(13) . . ?
C2 C6 H6 124.0 . . ?
S3 C6 H6 124.0 . . ?
C9 C7 C5 129.01(15) . . ?
C9 C7 S4 110.75(12) . . ?
C5 C7 S4 120.24(12) . . ?
C10 C8 S4 112.21(13) . . ?
C10 C8 H8 123.9 . . ?
S4 C8 H8 123.9 . . ?
C7 C9 C10 112.42(15) . . ?
C7 C9 S6 120.95(13) . . ?
C10 C9 S6 126.58(13) . . ?
C8 C10 C9 112.46(15) . . ?
C8 C10 S5 121.25(13) . . ?
C9 C10 S5 126.07(13) . . ?
C12 C11 S5 111.98(13) . . ?
C12 C11 H11A 109.2 . . ?
S5 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
S5 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 S6 113.39(13) . . ?
C11 C12 H12A 108.9 . . ?
S6 C12 H12A 108.9 . . ?
C11 C12 H12B 108.9 . . ?
S6 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C2 S1 C3 97.25(9) . . ?
C1 S2 C4 106.05(9) . . ?
C10 S5 C11 100.40(8) . . ?
C9 S6 C12 103.20(8) . . ?
C6 S3 C5 92.18(9) . . ?
C8 S4 C7 92.13(8) . . ?
 
_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              27.49
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.811
_refine_diff_density_min   -0.775
_refine_diff_density_rms    0.066
