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_1552596
_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 O12'
_chemical_formula_weight         616.64
_chemical_name_common            SY1
_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                   9.4820(13)
_cell_length_b                   13.0317(15)
_cell_length_c                   26.090(4)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    293.(2)
_cell_measurement_theta_max      74.80
_cell_measurement_theta_min      3.39
_cell_volume                     3223.9(8)
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 924)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON II'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_monochromator  mulilayer
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            30628
_diffrn_reflns_theta_full        75.12
_diffrn_reflns_theta_max         75.12
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'Ius 3.0'
_diffrn_source_type              microfocus
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_process_details
;
;
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.656
_exptl_crystal_size_mid          0.624
_exptl_crystal_size_min          0.564
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.228
_refine_ls_abs_structure_details
;

Flack x determined using 2533 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_coef       0.0093(8)
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0372
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                6176
_reflns_number_total             6597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            10.cif
_cod_data_source_block           HQJ53
_cod_original_cell_volume        3223.9(7)
_cod_database_code               1552596
_shelx_res_checksum              4770
_shelx_hkl_checksum              49255