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_2243871
_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 H38 O7, C H Cl3'
_chemical_formula_moiety         'C28 H38 O7, C H Cl3'
_chemical_formula_sum            'C29 H39 Cl3 O7'
_chemical_formula_weight         605.95
_chemical_melting_point          553(2)
_chemical_name_common
;
Physangulide B chloroform solvate
;
_chemical_name_systematic
'(17<i>S</i>,20<i>R</i>,22<i>R</i>,24<i>R</i>,25<i>S</i>)-5\b,6\b:20,24-Diepoxy-4\b,25-dihydroxy-1-oxowith-2-en-26,22-olide chloroform solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/8
_cell_angle_alpha                90
_cell_angle_beta                 94.14(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.3633(15)
_cell_length_b                   15.952(3)
_cell_length_c                   12.657(3)
_cell_measurement_reflns_used    7825
_cell_measurement_temperature    290.0(10)
_cell_measurement_theta_max      75.9680
_cell_measurement_theta_min      5.5270
_cell_volume                     1482.8(5)
_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)
;
_diffrn_ambient_temperature      290.0(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2576
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13820
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.902
_diffrn_reflns_theta_min         3.501
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.167
_exptl_absorpt_correction_T_max  0.37548
_exptl_absorpt_correction_T_min  0.31586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prizmatic
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.338
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2401 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons  <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5743
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0643P)^2^+0.4392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                5622
_reflns_number_total             5743
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            dj2029sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1482.9(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2243871
_shelx_hkl_checksum              57300
_shelx_res_checksum              34990
_cod_database_fobs_code 2243871