A hydrogen sulfate salt of chlordiazepoxide
Diesen, Veronica; Lousada, Cláudio; Fischer, Andreas; Acta Crystallographica Section E 68 (2012) o2091–o2092; doi:10.1107/S1600536812024920

data_2235443
_publ_section_title
;
 A hydrogen sulfate salt of chlordiazepoxide
;
_journal_coeditor_code           HB6784
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2091
_journal_page_last               o2092
_journal_paper_doi               10.1107/S1600536812024920
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C16 H15 Cl N3 O +, H S O4 -'
_chemical_formula_moiety         'C16 H15 Cl N3 O +, H O4 S -'
_chemical_formula_sum            'C16 H16 Cl N3 O5 S'
_chemical_formula_weight         397.837
_chemical_name_systematic
;
7-chloro-<i>N</i>-methyl-5-phenyl-2,3-dihydro-1<i>H</i>-
1,4-benzodiazepin-2-iminium 4-oxide hydrogen sulfate
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.657(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9899(6)
_cell_length_b                   8.7579(10)
_cell_length_c                   13.9084(6)
_cell_measurement_reflns_used    84
_cell_measurement_temperature    173
_cell_measurement_theta_max      20.7
_cell_measurement_theta_min      4.2
_cell_volume                     1679.9(2)
_computing_cell_refinement       'DIRAX (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2007)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23827
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         4.53
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    13
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3835
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0365P)^2^+1.1198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                2802
_reflns_number_total             3835
_reflns_threshold_expression     I>2\s(I)
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_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2235443
_cod_database_fobs_code          2235443