2,2,4-Trimethyl-7-nitro-2,3-dihydro-1<i>H</i>-1,5-benzodiazepin-5-ium perchlorate
Mehdi, Sayed Hasan; Sulaiman, Othman; Ghalib, Raza Murad; Yeap, Chin Sing; Fun, Hoong-Kun; Acta Crystallographica Section E 66 (2010) o1845–; doi:10.1107/S1600536810024475

data_2226498
_publ_section_title
;
 2,2,4-Trimethyl-7-nitro-2,3-dihydro-1<i>H</i>-1,5-benzodiazepin-5-ium
 perchlorate
;
_journal_coeditor_code           HB5507
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1845
_journal_paper_doi               10.1107/S1600536810024475
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C12 H16 N3 O2 +, Cl O4 -'
_chemical_formula_moiety         'C12 H16 N3 O2 +, Cl O4 -'
_chemical_formula_sum            'C12 H16 Cl N3 O6'
_chemical_formula_weight         333.73
_chemical_name_systematic
;
2,2,4-Trimethyl-7-nitro-2,3-dihydro-1<i>H</i>-1,5-benzodiazepin-5-ium
perchlorate
;
_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                 132.176(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.046(7)
_cell_length_b                   11.818(3)
_cell_length_c                   15.636(6)
_cell_measurement_reflns_used    7331
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      2.16
_cell_volume                     2882.1(17)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII DUO 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  0.0657
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24582
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2009)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.688
_refine_diff_density_min         -0.685
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0714P)^2^+7.0069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1273
_refine_ls_wR_factor_ref         0.1379
_reflns_number_gt                2816
_reflns_number_total             3323
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5507.cif
_cod_data_source_block           I
_cod_original_cell_volume        2882.0(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2226498
_cod_database_fobs_code          2226498