Capturing a new hydrate polymorph of amodiaquine dihydrochloride dihydrate via heterogeneous crystallisation
Putra, Okky Dwichandra; Pettersen, Anna; Nilsson Lill, Sten O.; Umeda, Daiki; Yonemochi, Etsuo; Nugraha, Yuda Prasetya; Uekusa, Hidehiro; CrystEngComm 21 (2019) 2053–; doi:10.1039/C8CE01720D

data_7231887
_publ_section_title
;
 Capturing a new hydrate polymorph of amodiaquine dihydrochloride
 dihydrate via heterogeneous crystallisation
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2053
_journal_paper_doi               10.1039/C8CE01720D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C20 H24 Cl N3 O, 2(Cl), 2(H2 O)'
_chemical_formula_sum            'C20 H28 Cl3 N3 O3'
_chemical_formula_weight         464.80
_chemical_name_common            'Amodiaquine Dihydrochloride Dihydrate'
_chemical_name_systematic
'4-[(7-chloro-4-quinolyl)amino]-        2-[(diethylamino)methyl] phenol dihydrochloride dihydrate.'
_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-2016/6
_audit_update_record
;
2018-09-14 deposited with the CCDC.
2018-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1341(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.69610(14)
_cell_length_b                   10.9153(2)
_cell_length_c                   27.2368(5)
_cell_measurement_reflns_used    19441
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      68.237
_cell_measurement_theta_min      5.838
_cell_volume                     2274.93(7)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       RAPID-AUTO
_computing_data_reduction        RAPID-AUTO
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR-2014 (M.C. Burla 2011)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.739
_diffrn_measurement_device_type  RAPID-AUTO
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0624
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.739
_diffrn_reflns_Laue_measured_fraction_max 0.739
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19441
_diffrn_reflns_point_group_measured_fraction_full 0.739
_diffrn_reflns_point_group_measured_fraction_max 0.739
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         68.237
_diffrn_reflns_theta_min         5.838
_diffrn_source                   'rotating anode X-ray'
_exptl_absorpt_coefficient_mu    3.863
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'abscor, T.Higashi RIGAKU'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.406
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         3083
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0645P)^2^+0.6638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1135
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2665
_reflns_number_total             3083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01720d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7231887.cif.'
_cod_database_code               7231887
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.303
_shelx_estimated_absorpt_t_max   0.824
_shelx_res_checksum              88131