Sustained release of matrine via salt formation with hesperetin
Zhu, Yujing; Shi, Xiaoju; Li, Duanxiu; Li, Shuang; Wang, Lin; Deng, Zongwu; Huang, Shaohua; Zhang, Hailu; CrystEngComm 26 (2024) 1090–1098; doi:10.1039/D3CE01129A

data_7248036
_publ_section_title
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 Sustained release of matrine via salt formation with hesperetin
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_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1090
_journal_page_last               1098
_journal_paper_doi               10.1039/D3CE01129A
_journal_volume                  26
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H24 N2 O, H2 O'
_chemical_formula_sum            'C15 H27.5 N2 O2.75'
_chemical_formula_weight         279.89
_chemical_name_systematic        matrine-h2o
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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_audit_update_record
;
2024-01-02 deposited with the CCDC.	2024-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.7266(6)
_cell_length_b                   11.7266(6)
_cell_length_c                   21.9372(16)
_cell_measurement_reflns_used    9884
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      56.65
_cell_measurement_theta_min      3.72
_cell_volume                     3016.7(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33397
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         56.909
_diffrn_reflns_theta_min         3.718
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1402 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.9073.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.119
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3084
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0339
_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^+0.4975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.677
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2731
_reflns_number_total             3084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01129a2.cif
_cod_data_source_block           mat-h2o
_cod_depositor_comments
'Adding full bibliography for 7248035--7248036.cif.'
_cod_original_cell_volume        3016.7(4)
_cod_original_formula_sum        'C15 H27.50 N2 O2.75'
_cod_database_code               7248036
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9(4)
 0.1(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 H2c-O2
 0.82 with sigma of 0.02
 H2d-O2
 0.82 with sigma of 0.02
4.a Riding coordinates:
 O2(H2c,H2d)
4.b Ternary CH refined with riding coordinates:
 C13(H13), C15(H15), C6(H6), C5(H5)
4.c Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C3(H3a,H3b), C4(H4a,H4b), C7(H7a,H7b), C2(H2a,H2b), C12(H12a,
 H12b), C8(H8a,H8b), C9(H9a,H9b), C11(H11a,H11b), C10(H10a,H10b)
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_smtbx_masks_special_details
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A solvent mask was calculated and 60 electrons were 
found in a volume of 284\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.75[H2O] per Asymmetric Unit 
which account for 60 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              91326
_shelx_fab_checksum              59412
_olex2_submission_special_instructions 'No special instructions were received'