Five solvates of a multicomponent pharmaceutical salt formed by berberine and diclofenac
Sun, Wei; Zuo, Limin; Zhao, Ting; Zhu, Zhiling; Shan, Guangzhi; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619015432

data_2021833
_publ_section_title
;
 Five solvates of a multicomponent pharmaceutical salt formed by berberine
 and diclofenac
;
_journal_coeditor_code           FP3076
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619015432
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C20 H18 N O4 +, C14 H10 Cl2 N O2 -, C2 H6 O'
_chemical_formula_moiety         'C20 H18 N O4 +, C14 H10 Cl2 N O2 -, C2 H6 O'
_chemical_formula_sum            'C36 H34 Cl2 N2 O7'
_chemical_formula_weight         677.55
_chemical_name_systematic
'5,6-Dihydro-9,10-dimethoxybenzo[<i>g</i>][1,3]benzodioxolo[5,6-<i>a</i>]quinolizinium 2-[2-(2,6-dichloroanilino)phenyl]acetate ethanol monosolvate'
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9667(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.15748(18)
_cell_length_b                   15.9353(3)
_cell_length_c                   25.4325(5)
_cell_measurement_reflns_used    8049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.4640
_cell_measurement_theta_min      4.4230
_cell_volume                     3298.10(12)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2017)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009),
PLATON (Spek, 2009),
Mercury (Macrae <i>et al.</i>,  2008) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4674
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur Atlas Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
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_diffrn_reflns_theta_full        66.546
_diffrn_reflns_theta_max         66.546
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       needle
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.473
_refine_ls_extinction_coef       0.00143(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0663P)^2^+1.0854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                4598
_reflns_number_total             5818
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3076sup1.cif
_cod_data_source_block           III
_cod_database_code               2021833
_cod_database_fobs_code          2021833
_shelx_estimated_absorpt_t_min   0.631
_shelx_estimated_absorpt_t_max   0.793