(<i>E</i>)-5-(2-Chlorophenyl)-7-ethyl-2-oxo-2,3-dihydro-1<i>H</i>-thieno[2,3-<i>e</i>][1,4]diazepin-4-ium 2,4,6-trinitrophenolate
Betz, Richard; Gerber, Thomas; Hosten, Eric; Dayananda, Alaloor S.; Yathirajan, Hemmige S.; Ramesha, A. R.; Acta Crystallographica Section E 68 (2012) o516–o517; doi:10.1107/S1600536812002607

data_2233587
_publ_section_title
;
 (<i>E</i>)-5-(2-Chlorophenyl)-7-ethyl-2-oxo-2,3-dihydro-1<i>H</i>-thieno[2,3-<i>e</i>][1,4]diazepin-4-ium
 2,4,6-trinitrophenolate
;
_journal_coeditor_code           PK2384
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o516
_journal_page_last               o517
_journal_paper_doi               10.1107/S1600536812002607
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C15 H14 Cl N2 O S +, C6 H2 N3 O7 -'
_chemical_formula_moiety         'C15 H14 Cl N2 O S +, C6 H2 N3 O7 -'
_chemical_formula_sum            'C21 H16 Cl N5 O8 S'
_chemical_formula_weight         533.90
_chemical_melting_point          518
_chemical_name_systematic
'(<i>E</i>)-5-(2-Chlorophenyl)-7-ethyl-2-oxo-2,3-dihydro-1<i>H</i>-thieno[2,3-<i>e</i>][1,4]diazepin-4-ium 2,4,6-trinitrophenolate'
_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                 110.6660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5704(2)
_cell_length_b                   20.0667(5)
_cell_length_c                   11.3741(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.89
_cell_volume                     2257.35(8)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997) and Mercury (Macrae <i>et al.</i>, 2008)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_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  0.0132
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21254
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.322
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008).
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1096
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5607
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0309
_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 w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+1.1718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0813
_reflns_number_gt                5073
_reflns_number_total             5607
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2384.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233587
_cod_database_fobs_code          2233587