Three trithiadiazepines and a trithiatriazepine
Jones, Ray; Acta Crystallographica Section C 70 (2014) 60–66; doi:10.1107/S2053229613033287

data_2019438
_publ_section_title
;
 Three trithiadiazepines and a trithiatriazepine
;
_journal_coeditor_code           QS3029
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              60
_journal_page_last               66
_journal_paper_doi               10.1107/S2053229613033287
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C3 H3 N3 O S3'
_chemical_formula_moiety         'C3 H3 N3 O S3'
_chemical_formula_sum            'C3 H3 N3 O S3'
_chemical_formula_weight         193.26
_chemical_melting_point          325
_chemical_name_systematic
;
7-Acetyl-1,3,5,2,4,6-trithiatriazene
;
_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                 102.21(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.647(3)
_cell_length_b                   5.8620(10)
_cell_length_c                   14.674(4)
_cell_measurement_reflns_used    12
_cell_measurement_temperature    293(2)
_cell_volume                     727.0(4)
_computing_cell_refinement       'Nicolet R3m software'
_computing_data_collection       'Nicolet R3m software'
_computing_data_reduction        'Nicolet R3m software'
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009) and
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), OLEX2 (Dolomanov <i>et al.</i>,
2009) and
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS83 (Sheldrick, 1983)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nicolet R3m'
_diffrn_measurement_method       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1074
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            812
_diffrn_reflns_theta_full        49.99
_diffrn_reflns_theta_max         49.99
_diffrn_reflns_theta_min         5.23
_diffrn_standards_decay_%        7
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.806
_exptl_absorpt_correction_T_max  0.3400
_exptl_absorpt_correction_T_min  0.1700
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(SHELXS83; Sheldrick, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.424
_refine_ls_extinction_coef       0.074(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0697P)^2^+0.6145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                743
_reflns_number_total             756
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3029sup1.cif
_cod_data_source_block           IV
_cod_original_cell_volume        727.0(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019438
_cod_database_fobs_code          2019438