Withanolides from <i>Physalis angulata</i> L.
Okmanov, R. Ya.; Makhmudova, M. M.; Bobaev, I. D.; Tashkhodjaev, B.; Acta Crystallographica Section E 77 (2021) 804–808; doi:10.1107/S205698902100709X

data_2243872
_publ_section_title
;
 Withanolides from <i>Physalis angulata</i> L.
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              804
_journal_page_last               808
_journal_paper_doi               10.1107/S205698902100709X
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C28 H40 O7'
_chemical_formula_moiety         'C28 H40 O7'
_chemical_formula_sum            'C28 H40 O7'
_chemical_formula_weight         488.60
_chemical_melting_point          528(3)
_chemical_name_common
;
14a-hydroxyixocarpanolide
;
_chemical_name_systematic
(20<i>R</i>,22<i>R</i>)-5\a,14\a,20-Trihydroxy-1-oxo-6\a,7\a-epoxywitha-2-enolide
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/8
_cell_angle_alpha                112.81(3)
_cell_angle_beta                 96.49(3)
_cell_angle_gamma                93.13(3)
_cell_formula_units_Z            1
_cell_length_a                   6.2374(12)
_cell_length_b                   9.5938(19)
_cell_length_c                   11.351(2)
_cell_measurement_reflns_used    1941
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      75.4630
_cell_measurement_theta_min      4.2650
_cell_volume                     618.5(3)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2018)
;
_computing_molecular_graphics
;
XP    (Sheldrick, 1998)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008), PLATON (Spek, 2020) and publCIF
(Westrip, 2010)'
;
_computing_structure_refinement
;
<i>SHELXL2014/8</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS7    (Sheldrick, 2008)
;
_diffrn_ambient_temperature      290.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4169
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.647
_diffrn_reflns_theta_min         4.271
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.85279
_exptl_absorpt_correction_T_min  0.77644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       prizmatic
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.193
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         2812
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0647P)^2^+0.0383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                2545
_reflns_number_total             2812
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2029sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        618.5(2)
_cod_database_code               2243872
_shelx_hkl_checksum              22691
_shelx_res_checksum              77263
_cod_database_fobs_code 2243872