Crystal structure of 1,5-diethyl-1<i>H</i>-1,5-benzodiazepine-2,4(3<i>H</i>,5<i>H</i>)-dithione
Lamkaddem, Abderrahman; Harcharras, Mohamed; Shaim, Abdelillah; Zouihri, Hafid; Echchahed, Bousselham; Bi, Wenhua; Acta Crystallographica Section E 71 (2015) o83–; doi:10.1107/S205698901402790X

data_2240352
_publ_section_title
;
 Crystal structure of
 1,5-diethyl-1<i>H</i>-1,5-benzodiazepine-2,4(3<i>H</i>,5<i>H</i>)-dithione
;
_journal_coeditor_code           TK5353
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o83
_journal_paper_doi               10.1107/S205698901402790X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C13 H16 N2 S2'
_chemical_formula_moiety         'C13 H16 N2 S2'
_chemical_formula_sum            'C13 H16 N2 S2'
_chemical_formula_weight         264.40
_chemical_name_systematic
;
1,5-Diethyl-1<i>H</i>-1,5-benzodiazepine-2,4(3<i>H</i>,5<i>H</i>)-dithione
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 104.0870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.8896(2)
_cell_length_b                   8.87430(10)
_cell_length_c                   15.5361(2)
_cell_measurement_reflns_used    7669
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.5
_cell_volume                     2659.75(5)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2009)
;
_computing_data_collection
;
APEX2 (Bruker, 2009)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14634
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.380
_exptl_absorpt_correction_T_max  0.9060
_exptl_absorpt_correction_T_min  0.8802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.210
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0331
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+1.6941P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                2963
_reflns_number_total             3312
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk5353sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2240352
_cod_database_fobs_code          2240352