Methanesulfonic acid salt forms of carbamazepine and 10,11-dihydrocarbamazepine
Eberlin, Alex R.; Eddleston, Mark D.; Frampton, Christopher S.; Acta Crystallographica Section C 69 (2013) 1260–1266; doi:10.1107/S010827011302859X

data_2019239
_publ_section_title
;
 Methanesulfonic acid salt forms of carbamazepine and
 10,11-dihydrocarbamazepine
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1260
_journal_page_last               1266
_journal_paper_doi               10.1107/S010827011302859X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C15 H12 N2 O1, C2 H1 F3 O2'
_chemical_formula_moiety         'C15 H12 N2 O1, C2 H1 F3 O2'
_chemical_formula_sum            'C17 H13 F3 N2 O3'
_chemical_formula_weight         350.29
_chemical_name_common
;
Carbamazepine-trifluoroacetic acid (1/1)
;
_chemical_name_systematic
;
Dibenzo[<i>b</i>,<i>f</i>]azepine-5-carboxamide--trifluoroacetic acid (1/1)
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.191(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9968(12)
_cell_length_b                   5.2660(3)
_cell_length_c                   20.1911(12)
_cell_measurement_reflns_used    3607
_cell_measurement_temperature    100.0(10)
_cell_measurement_theta_max      75.5552
_cell_measurement_theta_min      3.0122
_cell_volume                     1558.60(18)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(10)
_diffrn_detector_area_resol_mean 10.5598
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7053
_diffrn_reflns_theta_full        74.48
_diffrn_reflns_theta_max         74.48
_diffrn_reflns_theta_min         3.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2011)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Lath
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.288
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0945P)^2^+0.5500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1368
_reflns_number_gt                2937
_reflns_number_total             3189
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ky3042.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2019239