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

data_7230206
_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, 0.5(C2 H2 O4), Cl'
_chemical_formula_sum            'C15 H24 Cl2 N3 O4'
_chemical_formula_weight         381.27
_chemical_melting_point          416
_chemical_name_common            'Metoclopramide hydrochloride oxalic acid'
_chemical_name_systematic
'4-Amino-5-chloro-N-(2-(diethylamino)ethyl)-2-methoxybenzamide hydrochloride oxalic acid'
_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   mixed
_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                   7.5270(4)
_cell_length_b                   14.1483(9)
_cell_length_c                   34.3682(19)
_cell_measurement_reflns_used    32557
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.457
_cell_measurement_theta_min      3.114
_cell_volume                     3660.0(4)
_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      93(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID'
_diffrn_measurement_method       \wscan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            32551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.457
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'rotating anode X-ray'
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'abscor, T.Higashi RIGAKU'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_description       plate
_exptl_crystal_F_000             1608
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone'
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.212
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4170
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0490P)^2^+0.6278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3418
_reflns_number_total             4170
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00129d2.cif
_cod_data_source_block           shelx_a
_cod_depositor_comments
'Adding full bibliography for 7230206--7230208.cif.'
_cod_database_code               7230206
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.914
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              89995