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_2242505
_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_coeditor_code           WM5446
_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 S4 Se2'
_chemical_formula_moiety         'C8 H6 O2 S4 Se2'
_chemical_formula_sum            'C8 H6 O2 S4 Se2'
_chemical_formula_weight         420.29
_chemical_name_systematic
;
4,4'-(Disulfane-1,2-diyl)bis(5-methyl-2<i>H</i>-1,3-dithiol-2-one)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 108.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.960(2)
_cell_length_b                   9.1348(18)
_cell_length_c                   13.495(3)
_cell_measurement_reflns_used    11124
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      53.8
_cell_measurement_theta_min      3.2
_cell_volume                     1282.8(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
;
<i>XP</i> (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 0.999
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Stoe IPDS2T'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.862
_diffrn_reflns_theta_min         1.957
_exptl_absorpt_coefficient_mu    6.395
_exptl_absorpt_correction_T_max  0.7860
_exptl_absorpt_correction_T_min  0.3926
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.176
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.429
_exptl_crystal_size_min          0.408
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.513
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0513
_refine_ls_wR_factor_ref         0.0577
_reflns_number_gt                2009
_reflns_number_total             2733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5446sup1.cif
_cod_data_source_block           CSV72a12
_cod_database_code               2242505
_cod_database_fobs_code          2242505
_shelx_estimated_absorpt_t_min   0.150
_shelx_estimated_absorpt_t_max   0.180
_shelx_hkl_checksum              36981
_shelx_res_checksum              76098