Improving solubility and avoiding hygroscopicity of tetrahydroberberine by forming hydrochloride salts by introducing solvents: [HTHB]Cl, [HTHB]Cl·CH3OH and [HTHB]Cl·CH3COOH
Zhang, Yunan; Zhang, Dajun; Zhang, Yu; Liu, Lixin; Zhang, Xuesong; Zhang, Lei; Zhang, Yunjie; Chang, Liang; Fan, Qiushuang; Zhang, Yongbiao; Xi, Jiaming; Zhang, Qiang; New Journal of Chemistry 41 (2017) 13268–; doi:10.1039/C7NJ02423A

data_7059118
_publ_section_title
;
 Improving solubility and avoiding hygroscopicity of tetrahydroberberine
 by forming hydrochloride salts by introducing solvents: [HTHB]Cl,
 [HTHB]Cl&#x00B7;CH3OH and [HTHB]Cl&#x00B7;CH3COOH
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13268
_journal_paper_doi               10.1039/C7NJ02423A
_journal_volume                  41
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C20 H22 N O4, Cl'
_chemical_formula_sum            'C20 H22 Cl N O4'
_chemical_formula_weight         375.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-05-01 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.5563(3)
_cell_length_b                   9.6115(5)
_cell_length_c                   23.9913(11)
_cell_measurement_reflns_used    2103
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8800
_cell_measurement_theta_min      3.1798
_cell_volume                     1742.43(14)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            5216
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.746
_diffrn_reflns_theta_min         3.186
_exptl_absorpt_coefficient_mu    0.246
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             792.0
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 948 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0419P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.658
_reflns_Friedel_fraction_full    0.922
_reflns_Friedel_fraction_max     0.912
_reflns_number_gt                2781
_reflns_number_total             3326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj02423a2.cif
_cod_data_source_block           shelx
_cod_database_code               7059118
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.952
_shelx_res_checksum              57347