Crystal structures of 4,4'-(disulfane-1,2-diyl)bis(5-methyl-2<i>H</i>-1,3-dithiol-2-one) and 4,4'-(diselanane-1,2-diyl)bis(5-methyl-2<i>H</i>-1,3-dithiol-2-one)
Trentin, Ivan; Schindler, Claudia; Schulzke, Carola; Acta Crystallographica Section E 74 (2018) 840–845; doi:10.1107/S2056989018007454

data_2242506
_publ_section_title
;
 Crystal structures of
 4,4'-(disulfane-1,2-diyl)bis(5-methyl-2<i>H</i>-1,3-dithiol-2-one) and
 4,4'-(diselanane-1,2-diyl)bis(5-methyl-2<i>H</i>-1,3-dithiol-2-one)
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              840
_journal_page_last               845
_journal_paper_doi               10.1107/S2056989018007454
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C8 H6 O2 S6'
_chemical_formula_moiety         'C8 H6 O2 S6'
_chemical_formula_sum            'C8 H6 O2 S6'
_chemical_formula_weight         326.49
_chemical_name_systematic
;
4,4'-(Diselanane-1,2-diyl)bis(5-methyl-2<i>H</i>-1,3-dithiol-2-one)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.845(2)
_cell_length_b                   9.0387(18)
_cell_length_c                   13.370(3)
_cell_measurement_reflns_used    13753
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      58.5
_cell_measurement_theta_min      6.4
_cell_volume                     1239.6(5)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2010)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2010)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2010)
;
_computing_molecular_graphics
;
XP (Bruker, 1998), DIAMOND (Brandenburg, 2001),
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
<i>CIFTAB</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2016/6</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR-92 (Altomare <i>et al.</i>,  1994), <i>SHELXS2016/6</i> (Sheldrick,
2008)
;
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'STOE IPDS2T'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13324
_diffrn_reflns_theta_full        29.23
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.9421
_exptl_absorpt_correction_T_min  0.7709
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.001
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.344
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+0.2272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0597
_refine_ls_wR_factor_ref         0.0635
_reflns_number_gt                2636
_reflns_number_total             3344
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            wm5446sup1.cif
_cod_data_source_block           it14ii
_cod_original_cell_volume        1239.6(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2242506
_cod_database_fobs_code          2242506
_shelx_res_checksum              86525