Comprehensive determination of the solid state stability of bethanechol chloride active pharmaceutical ingredient using combined analytical tools
Rotival, Romain; Corvis, Yohann; Cartigny, Yohann; Négrier, Philippe; Marchivie, Mathieu; Massip, Stéphane; Gana, Inès; Lemoine, Pascale; Espeau, Philippe; CrystEngComm 15 (2013) 7970–; doi:10.1039/c3ce40707a

data_7210827
_publ_section_title
;
 Comprehensive determination of the solid state stability of bethanechol
 chloride active pharmaceutical ingredient using combined analytical tools
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              7970
_journal_paper_doi               10.1039/c3ce40707a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C7 H17 Cl N2 O2'
_chemical_formula_weight         196.68
_space_group_IT_number           14
_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                 93.749(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0933(6)
_cell_length_b                   16.2066(11)
_cell_length_c                   8.8042(7)
_cell_measurement_reflns_used    1750
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.25
_cell_measurement_theta_min      5.46
_cell_volume                     1009.95(14)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rigaku RAXIS Rapid'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Rigaku VariMax mirror'
_diffrn_radiation_source         'micro-focus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.1413
_diffrn_reflns_av_sigmaI/netI    0.1050
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5976
_diffrn_reflns_theta_full        70.02
_diffrn_reflns_theta_max         70.02
_diffrn_reflns_theta_min         6.83
_exptl_absorpt_coefficient_mu    3.103
_exptl_absorpt_correction_T_max  0.9127
_exptl_absorpt_correction_T_min  0.7894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku/MSC Inc., 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1872
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0739
_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^)+(0.0645P)^2^+2.1966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1797
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                1714
_reflns_number_total             1872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40707a.txt
_cod_data_source_block           bethan
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7210827