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

data_7230208
_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'
_chemical_formula_sum            'C14 H23 Cl2 N3 O2'
_chemical_formula_weight         336.25
_chemical_melting_point          460
_chemical_name_common            'Metoclopramide HCl anhydrate'
_chemical_name_systematic
'4-Amino-5-chloro-N-((2-diethylamino)-ethyl)-2-methoxybenzamide hydrochloride monohydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2017-11-14 deposited with the CCDC.
2018-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.6866(4)
_cell_length_b                   7.0245(2)
_cell_length_c                   33.0316(9)
_cell_measurement_reflns_used    36288
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.165
_cell_measurement_theta_min      4.028
_cell_volume                     3407.74(16)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 2009)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 2009)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 2009)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2008)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID2'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1327
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            36288
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.165
_diffrn_reflns_theta_min         4.028
_diffrn_source                   'rotating anode X-ray'
_exptl_absorpt_coefficient_mu    3.493
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'abscor, T. Higashi RIGAKU'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       needle
_exptl_crystal_F_000             1424
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.159
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1287P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1996
_refine_ls_wR_factor_ref         0.2502
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1526
_reflns_number_total             3100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00129d2.cif
_cod_data_source_block           shelx_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7230206--7230208.cif.'
_cod_database_code               7230208
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.607
_shelx_estimated_absorpt_t_max   0.902
_shelx_res_checksum              3617