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_2312620
_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 H24 N2 O, 1.75H2 O'
_chemical_formula_moiety         'C15 H24 N2 O, 1.75(H2 O)'
_chemical_formula_sum            'C15 H27.5 N2 O2.75'
_chemical_formula_weight         279.89
_chemical_name_common
;
Matrine 1.75-hydrate
;
_chemical_name_systematic
'(1<i>R</i>,2<i>R</i>,9<i>S</i>,17<i>S</i>)-7,13-Diazatetracyclo[7.7.1.0^{2,7}.0^{13,17}]heptadecan-6-one 1.75-hydrate'
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   mixed
_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            8
_cell_length_a                   11.7364(3)
_cell_length_b                   11.7364(3)
_cell_length_c                   21.9295(9)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      60.516
_cell_measurement_theta_min      3.716
_cell_volume                     3020.64(17)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49632
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.760
_diffrn_reflns_theta_min         3.716
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.6983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2016)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.234
_refine_ls_abs_structure_details
;
 Flack x determined using 1323 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0507P)^2^+0.5768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                3335
_reflns_number_total             3473
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            op3032sup1.cif
_cod_data_source_block           matrine-h
_cod_original_cell_volume        3020.6(2)
_cod_original_formula_sum        'C15 H27.50 N2 O2.75'
_cod_database_code               2312620
_shelx_estimated_absorpt_t_min   0.962
_shelx_estimated_absorpt_t_max   0.975
_cod_database_fobs_code 2312620