4,5-Propylenedithio-1,3-dithiole-2-thione and 4,5-propylenedithio-1,3-dithiol-2-one
Xue, Gang; Fang, Qi; Yu, Wentao; Acta Crystallographica Section C 59 (2003) o653–o655; doi:10.1107/S0108270103022662

data_2013573
_publ_section_title
;
 4,5-Propylenedithio-1,3-dithiole-2-thione and
 4,5-propylenedithio-1,3-dithiol-2-one
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o653
_journal_page_last               o655
_journal_paper_doi               10.1107/S0108270103022662
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C6 H6 O S4'
_chemical_formula_moiety         'C6 H6 O S4'
_chemical_formula_sum            'C6 H6 O S4'
_chemical_formula_weight         222.35
_chemical_melting_point          393.5
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 108.736(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.358(4)
_cell_length_b                   4.5009(11)
_cell_length_c                   13.066(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.1575
_cell_measurement_theta_min      8.939
_cell_volume                     911.0(4)
_computing_cell_refinement       Xscans
_computing_data_collection       'Xscans (Bruker, 1996)'
_computing_data_reduction        Xscans
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_sigmaI/netI    0.0451
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            1439
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.63
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_T_max  0.9818
_exptl_absorpt_correction_T_min  0.6646
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Xscans (Bruker, 1996)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.392
_refine_ls_abs_structure_details
;  The Flack parameter was refined (Flack, 1983), but did not
    give a clear result.  This structure does not involve an absolute
    configuration question, and the absolute structure determination
    does not influence the interpretation of the chemical structure.
;
_refine_ls_abs_structure_Flack   0.3(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1150
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                925
_reflns_number_total             1150
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa1033.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2013573