Suppressed hydration in metoclopramide hydrochloride by salt cocrystallisation
Nugraha, Yuda Prasetya; Uekusa, Hidehiro; CrystEngComm 20 (2018) 2653–; doi:10.1039/C8CE00129D

data_7230207
_publ_section_title
;
 Suppressed hydration in metoclopramide hydrochloride by salt
 cocrystallisation
;
_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2653
_journal_paper_doi               10.1039/C8CE00129D
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C14 H23 Cl N3 O2, Cl, H2 O'
_chemical_formula_sum            'C14 H25 Cl2 N3 O3'
_chemical_formula_weight         354.27
_chemical_name_common            'Metoclopramide HCl Monohydrate'
_chemical_name_systematic
'4-Amino-5-chloro-N-((2-diethylamino)-ethyl)-2-methoxybenzamide hydrochloride monohydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-12-12 deposited with the CCDC.
2018-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.605(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1124(17)
_cell_length_b                   8.5524(12)
_cell_length_c                   16.849(3)
_cell_measurement_reflns_used    17713
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.072
_cell_volume                     1725.7(5)
_computing_cell_refinement       'RIGAKU CrystalClear-SM Expert2.0 r4'
_computing_data_collection       'RIGAKU CrystalClear-SM Expert2.0 r4'
_computing_data_reduction        'RIGAKU CrystalClear-SM Expert2.0 r4'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'RIGAKU XtaLab'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17713
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'sealed tube with SHINE monochromator X-ray'
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'abscor, T. Higashi RIGAKU'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_description       block
_exptl_crystal_F_000             752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.395
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+0.6960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3386
_reflns_number_total             3954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00129d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7230206--7230208.cif.'
_cod_original_cell_volume        1725.7(4)
_cod_database_code               7230207
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.856
_shelx_estimated_absorpt_t_max   0.932
_shelx_res_checksum              70665