Crystal structure of dibenzo[<i>c</i>,<i>e</i>]thiepine-5(7<i>H</i>)-thione
Brown, Loren C.; Ghiassi, Kamran B.; Fulton, Ashley C.; Thum, Matthew; Acta Crystallographica Section E 78 (2022) –; doi:10.1107/S2056989022010532

data_2244218
_publ_section_title
;
 Crystal structure of
 dibenzo[<i>c</i>,<i>e</i>]thiepine-5(7<i>H</i>)-thione
;
_journal_coeditor_code           YK2177
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989022010532
_journal_volume                  78
_journal_year                    2022
_chemical_formula_iupac          'C14 H10 S2'
_chemical_formula_moiety         'C14 H10 S2'
_chemical_formula_sum            'C14 H10 S2'
_chemical_formula_weight         242.34
_chemical_name_systematic
;
Dibenzo[<i>c</i>,<i>e</i>]thiepine-5(7<i>H</i>)-thione
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.84(7)
_cell_length_b                   16.0(2)
_cell_length_c                   18.51(12)
_cell_measurement_reflns_used    6808
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.78
_cell_volume                     2322(4)
_computing_cell_refinement
;
SAINT (Bruker, 2017)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2017)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71076
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30500
_diffrn_reflns_theta_full        25.243
_diffrn_reflns_theta_max         27.584
_diffrn_reflns_theta_min         2.554
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Krause <i>et al.</i>, 2015)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.280
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         2664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0379P)^2^+1.9590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                2154
_reflns_number_total             2664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yk2177sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        232E1(4)
_cod_database_code               2244218
_shelx_estimated_absorpt_t_min   0.931
_shelx_estimated_absorpt_t_max   0.963
_shelx_hkl_checksum              354
_shelx_res_checksum              45900
_cod_database_fobs_code 2244218