Anti-inflammatory 12,20-Epoxypregnane and 11,12-seco-Pregnane Glycosides from the Stems of Hoya kerrii.
Seeka, Chonticha; Prabpai, Samran; Kongsaeree, Palangpon; Tewtrakul, Supinya; Lhinhatrakool, Thitima; Sutthivaiyakit, Somyote; Journal of natural products 80 (2017) 1714–1724; doi:10.1021/acs.jnatprod.6b00730

data_1546460
_publ_section_title
;
 Anti-inflammatory 12,20-Epoxypregnane and 11,12-seco-Pregnane Glycosides
 from the Stems of Hoya kerrii.
;
_journal_issue                   6
_journal_name_full               'Journal of natural products'
_journal_page_first              1714
_journal_page_last               1724
_journal_paper_doi               10.1021/acs.jnatprod.6b00730
_journal_volume                  80
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_compound_source        'Hoya kerrii'
_chemical_formula_moiety         'C31 H46 O10'
_chemical_formula_sum            'C31 H46 O10'
_chemical_formula_weight         578.68
_chemical_name_common
'kerriipregnane B 3-O-\^I^2^-D-diginopyranoside acetate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      18
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.0000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6220(4)
_cell_length_b                   19.96800(10)
_cell_length_c                   5.6990(5)
_cell_measurement_reflns_used    4571
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.967
_cell_measurement_theta_min      0.998
_cell_volume                     3143.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'platon and mercury 3.5'
_computing_publication_material  'J Nat Proc'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 14
_diffrn_measured_fraction_theta_full 0.840
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Kappa CCD2000'
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5050
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.786
_diffrn_reflns_theta_min         2.950
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.066(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0885P)^2^+0.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1424
_reflns_Friedel_coverage         0.684
_reflns_Friedel_fraction_full    0.790
_reflns_Friedel_fraction_max     0.939
_reflns_number_gt                4200
_reflns_number_total             4650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00730_si_004.cif
_cod_data_source_block           cmpd8a
_cod_database_code               1546460
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.978
_shelxl_version_number           2013-4
_shelx_res_checksum              66522
_shelx_hkl_checksum              40046