Isolation, pharmacological activity and structure determination of physalin B and 5β,6β-epoxyphysalin B isolated from Congolese <i>Physalis angulata</i> L.
Mangwala Kimpende, Peter; Lusakibanza, Mariano; Mesia, Kahunu; Tona, Lutete; Tits, Monique; Angenot, Luc; Frédérich, Michel; Van Meervelt, Luc; Acta Crystallographica Section C 69 (2013) 1557–1562; doi:10.1107/S010827011303117X

data_2019294
_publ_section_title
;
 Isolation, pharmacological activity and structure determination of
 physalin B and 5\b,6\b-epoxyphysalin B isolated from Congolese
 <i>Physalis angulata</i> L.
;
_journal_coeditor_code           FG3314
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1557
_journal_page_last               1562
_journal_paper_doi               10.1107/S010827011303117X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '2C28 H30 O9, C3 H6 O, 0.22(H2 O)'
_chemical_formula_moiety         '2C28 H30 O9, C3 H6 O, 0.22H2 O'
_chemical_formula_sum            'C29.5 H33.22 O9.61'
_chemical_formula_weight         541.54
_chemical_name_common
;
Physalin B acetone hemisolvate 0.11-hydrate
;
_chemical_name_systematic
;(8<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>S</i>,14<i>R</i>,16<i>S</i>,17<i>R</i>,20<i>S</i>,22<i>R</i>,24<i>R</i>,25<i>S</i>)-16,24-Cyclo-13,14-secoergosta-2,5-diene-1,15-dioxo-14:17,14:27-diepoxy-13-hydroxy-18,26-dioic
acid 18:20,26:22-di-\g-lactone \d-lactone acetone hemisolvate 0.11-hydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.863(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5153(9)
_cell_length_b                   14.1333(11)
_cell_length_c                   14.6716(10)
_cell_measurement_temperature    100(2)
_cell_volume                     2576.6(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0824
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25302
_diffrn_reflns_theta_full        71.58
_diffrn_reflns_theta_max         71.58
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1148.4
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.204
_refine_ls_abs_structure_details 'Flack (1983), 4126 Friedel pairs'
_refine_ls_abs_structure_Flack   0.0(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         9227
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                7497
_reflns_number_total             9227
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fg3314.cif
_cod_data_source_block           X
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2019294