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

data_2019436
_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          'C2 N4 O4 S3'
_chemical_formula_moiety         'C2 N4 O4 S3'
_chemical_formula_sum            'C2 N4 O4 S3'
_chemical_formula_weight         240.24
_chemical_melting_point          336
_chemical_name_systematic
;
6,7-Dinitro-1,3,5,2,4-trithiadiazepine
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.36(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.182(2)
_cell_length_b                   8.436(2)
_cell_length_c                   8.609(2)
_cell_measurement_reflns_used    11
_cell_measurement_temperature    293(2)
_cell_volume                     811.9(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            581
_diffrn_reflns_theta_full        56.97
_diffrn_reflns_theta_max         56.97
_diffrn_reflns_theta_min         6.57
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    8.375
_exptl_absorpt_correction_T_max  0.4700
_exptl_absorpt_correction_T_min  0.3800
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(SHELXS83; Sheldrick, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.158
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_matrix_type           full
_refine_ls_number_parameters     61
_refine_ls_number_reflns         543
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
   [\s^2^(Fo^2^)+0.0000+0.7454*P+(0.0347P)^2^+1.0000sin\q/\l]
 where P = 0.33333Fo^2^ + 0.66667Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                511
_reflns_number_total             543
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qs3029sup1.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2019436
_cod_database_fobs_code          2019436