2,5-Bis(1,3-dithiol-2-ylidene)-1,3-dithiolane-4-thione
Ueda, Kazumasa; Suzuki, Kenta; Kunimoto, Kei; Yoza, Kenji; Acta Crystallographica Section E 68 (2012) o52–; doi:10.1107/S1600536811051518

data_2233144
_publ_section_title
;
 2,5-Bis(1,3-dithiol-2-ylidene)-1,3-dithiolane-4-thione
;
_journal_coeditor_code           FY2030
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o52
_journal_paper_doi               10.1107/S1600536811051518
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C9 H4 S7'
_chemical_formula_moiety         'C9 H4 S7'
_chemical_formula_sum            'C9 H4 S7'
_chemical_formula_weight         336.54
_chemical_name_common
;
2,5-Bis(1,3-dithiol-2-ylidene)-1,3-dithiolane-4-thione
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.177(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.669(5)
_cell_length_b                   3.9110(11)
_cell_length_c                   18.380(5)
_cell_measurement_reflns_used    794
_cell_measurement_temperature    93
_cell_measurement_theta_max      23.92
_cell_measurement_theta_min      2.33
_cell_volume                     1206.7(6)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'XCIF (Bruker, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.1356
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            6965
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    1.270
_exptl_absorpt_correction_T_max  0.9751
_exptl_absorpt_correction_T_min  0.8943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Sheldrick, 1996)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.520
_refine_ls_abs_structure_details 'Flack (1983), 1849 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.18(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4975
_refine_ls_number_restraints     421
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                3396
_reflns_number_total             4975
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fy2030.cif
_cod_data_source_block           I
_cod_original_cell_volume        1206.8(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2233144
_cod_database_fobs_code          2233144