Tripterfordins A-O, Dihydro-β-agarofuran Sesquiterpenoids from the Leaves of <i>Tripterygium wilfordii</i>.
Zhou, Le; He, Qing-Jun; Lu, Li-Wei; Zhao, Feng; Zhang, Yan; Huang, Xiao-Xiao; Lin, Bin; Song, Shao-Jiang; Journal of natural products 82 (2019) 2696–2706; doi:10.1021/acs.jnatprod.9b00089

data_1552594
_publ_section_title
;
 Tripterfordins A-O, Dihydro-\b-agarofuran Sesquiterpenoids from the
 Leaves of <i>Tripterygium wilfordii</i>.
;
_journal_issue                   10
_journal_name_full               'Journal of natural products'
_journal_page_first              2696
_journal_page_last               2706
_journal_paper_doi               10.1021/acs.jnatprod.9b00089
_journal_volume                  82
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_sum            'C32 H40 O13'
_chemical_formula_weight         632.64
_chemical_name_common            HQT58
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8834(3)
_cell_length_b                   14.4364(4)
_cell_length_c                   16.8811(5)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    170.(2)
_cell_measurement_theta_max      68.26
_cell_measurement_theta_min      3.43
_cell_volume                     3139.71(15)
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTRUE PHOTON II'
_diffrn_radiation_monochromator  multi-layer
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22258
_diffrn_reflns_theta_full        68.31
_diffrn_reflns_theta_max         68.31
_diffrn_reflns_theta_min         4.03
_diffrn_source                   'Incoatec Ius 3.0'
_diffrn_source_type              Microfocus
_exptl_absorpt_coefficient_mu    0.873
_exptl_absorpt_process_details
;
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.166
_refine_ls_abs_structure_details
;

Flack x determined using 2424 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.0038(2)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0370P)^2^+0.5366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                5651
_reflns_number_total             5736
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1.cif
_cod_data_source_block           HQJ58
_cod_database_code               1552594
_shelx_res_checksum              23802
_shelx_hkl_checksum              3240