Crystal structures and properties of derivatives of the alkaloid matrine: salts and hydrate forms.
Liu, Jiyong; Shi, Dier; Yu, Kaxi; Liu, Shuna; Chen, Linshen; Hu, Xiurong; Acta crystallographica. Section C, Structural chemistry 80 (2024) –; doi:10.1107/S2053229624008064

data_2312618
_publ_section_title
;
 Crystal structures and properties of derivatives of the alkaloid matrine:
 salts and hydrate forms.
;
_journal_coeditor_code           OP3032
_journal_issue                   10
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624008064
_journal_volume                  80
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_iupac          'C15 H25 N2 O +, C9 H7 O4 -, 1.5H2 O'
_chemical_formula_moiety         'C15 H25 N2 O +, C9 H7 O4 -, 1.5(H2 O)'
_chemical_formula_sum            'C24 H35 N2 O6.5'
_chemical_formula_weight         455.54
_chemical_name_common
;
Matrine caffeinate sesquihydrate
;
_chemical_name_systematic
;(1<i>R</i>,2<i>R</i>,9<i>S</i>,17<i>S</i>)-6-Oxo-7,13-diazatetracyclo[7.7.1.0^2,7^.0^13,17^]heptadecan-13-ium
(2<i>E</i>)-3-(3,4-dihydroxyphenyl)prop-2-enoate sesquihydrate
;
_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
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1508(4)
_cell_length_b                   11.0066(5)
_cell_length_c                   25.7084(12)
_cell_measurement_reflns_used    9998
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.535
_cell_measurement_theta_min      3.800
_cell_volume                     2306.37(19)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009),
DIAMOND (Brandenburg & Putz, 1999) and
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2019 (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
SHELXT2018 (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43143
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.741
_diffrn_reflns_theta_min         3.801
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.173
_refine_diff_density_min         -0.260
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1970 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.07(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5269
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0585P)^2^+0.1825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0968
_reflns_number_gt                4863
_reflns_number_total             5269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op3032sup1.cif
_cod_data_source_block           matrine-ca
_cod_original_formula_sum        'C24 H35 N2 O6.50'
_cod_database_code               2312618
_shelx_estimated_absorpt_t_min   0.976
_shelx_estimated_absorpt_t_max   0.985
_cod_database_fobs_code 2312618