17β<i>H</i>-Periplogenin, a cardiac aglycone from the root bark of <i>Periploca sepium</i> Bunge
Zhang, Yu-Wei; Bao, Yong-Li; Wu, Yin; Yu, Chun-Lei; Li, Yu-Xin; Acta Crystallographica Section E 68 (2012) o1582–o1583; doi:10.1107/S1600536812018521

data_2235289
_publ_section_title
;
 17\b<i>H</i>-Periplogenin, a cardiac aglycone from the root bark of
 <i>Periploca sepium</i> Bunge
;
_journal_coeditor_code           WN2470
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1582
_journal_page_last               o1583
_journal_paper_doi               10.1107/S1600536812018521
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C23 H34 O5'
_chemical_formula_moiety         'C23 H34 O5'
_chemical_formula_sum            'C23 H34 O5'
_chemical_formula_weight         390.50
_chemical_name_common            17<i>\b</i>H-periplogenin
_chemical_name_systematic
;4-[(3<i>S</i>,5<i>S</i>,8<i>R</i>,9<i>S</i>,10<i>R</i>,13<i>R</i>,14<i>S</i>,17<i>S</i>)-3,5,14-trihydroxy-10,13-dimethyl-hexadecahydro-1<i>H</i>-
cyclopenta[<i>a</i>]phenanthren-17-yl]furan-2(5<i>H</i>)-one
;
_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                 103.118(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.434(3)
_cell_length_b                   10.554(4)
_cell_length_c                   13.537(5)
_cell_measurement_reflns_used    5262
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.54
_cell_volume                     1034.4(7)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5262
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9983
_exptl_absorpt_correction_T_min  0.9778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.171
_refine_diff_density_min         -0.181
_refine_ls_extinction_coef       0.013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         1927
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0536P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                1097
_reflns_number_total             1927
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wn2470.cif
_cod_data_source_block           I
_cod_original_cell_volume        1034.4(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2235289
_cod_database_fobs_code          2235289