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_2021831
_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 -, 2H2 O'
_chemical_formula_moiety         'C20 H18 N O4 +, C14 H10 Cl2 N O2 -, 2(H2 O)'
_chemical_formula_sum            'C34 H32 Cl2 N2 O8'
_chemical_formula_weight         667.51
_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 dihydrate'
_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'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.8602(3)
_cell_length_b                   8.76477(12)
_cell_length_c                   34.5299(7)
_cell_measurement_reflns_used    8118
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.8020
_cell_measurement_theta_min      4.2180
_cell_volume                     6313.27(18)
_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
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_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -35
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_diffrn_source                   'fine-focus sealed X-ray tube'
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_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2017)
;
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       needle
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.433
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5569
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0548P)^2^+2.9645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                4442
_reflns_number_total             5569
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3076sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        6313.29(18)
_cod_database_code               2021831
_cod_database_fobs_code          2021831
_shelx_estimated_absorpt_t_min   0.641
_shelx_estimated_absorpt_t_max   0.801