Salt forms of the pharmaceutical amide dihydrocarbamazepine
Buist, Amanda R.; Kennedy, Alan R.; Acta Crystallographica Section C 72 (2016) 155–160; doi:10.1107/S2053229616001133

data_2020409
_publ_section_title
;
 Salt forms of the pharmaceutical amide dihydrocarbamazepine
;
_journal_coeditor_code           YF3097
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              155
_journal_page_last               160
_journal_paper_doi               10.1107/S2053229616001133
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C15 H15 N2 O +, Br -, H2 O'
_chemical_formula_moiety         'C15 H15 N2 O +, Br -, H2 O'
_chemical_formula_sum            'C15 H17 Br N2 O2'
_chemical_formula_weight         337.22
_chemical_name_systematic
'(10,11-Dihydro-5<i>H</i>-dibenzo[<i>b</i>,<i>f</i>]azepin-5-yl)(hydroxy)methylidene]azanium bromide monohydrate'
_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                 96.931(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.4857(2)
_cell_length_b                   24.5526(9)
_cell_length_c                   10.9796(4)
_cell_measurement_reflns_used    2990
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.2320
_cell_measurement_theta_min      3.1064
_cell_volume                     1468.02(9)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare et al., 1994)
;
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur E'
_diffrn_measurement_method       'omega 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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0510
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6786
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.670
_refine_diff_density_min         -0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3324
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.7435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                2687
_reflns_number_total             3324
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            yf3097sup1.cif
_cod_data_source_block           III
_cod_depositor_comments
'Adding full bibliography for 2020407--2020409.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2020409
_cod_database_fobs_code          2020409