Neuroprotective Dihydroagarofuran Sesquiterpene Derivatives from the Leaves of Tripterygium wilfordii
Chen, Fang-You; Li, Chuang-Jun; Ma, Jie; Zhou, Jian; Li, Li; Zhang, Zhao; Chen, Nai-Hong; Zhang, Dong-Ming; Journal of Natural Products  (2018) –; doi:10.1021/acs.jnatprod.7b00615

data_1548732
_publ_section_title
;
 Neuroprotective Dihydroagarofuran Sesquiterpene Derivatives from the
 Leaves of Tripterygium wilfordii
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.7b00615
_journal_year                    2018
_chemical_formula_moiety         'C33 H38 O12'
_chemical_formula_sum            'C33 H38 O12'
_chemical_formula_weight         626.63
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-18
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.952(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6865(2)
_cell_length_b                   11.9018(3)
_cell_length_c                   13.7460(4)
_cell_measurement_reflns_used    7101
_cell_measurement_temperature    103.2
_cell_measurement_theta_max      70.9419
_cell_measurement_theta_min      3.3251
_cell_volume                     1531.08(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      103.2
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega  -26.00   17.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   45.0000  -60.0000 43

  2 omega   35.00   60.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000   45.0000  -60.0000 25

  3 omega   -9.00   32.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036  -37.0000 -180.0000 41

  4 omega    9.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036   77.0000   60.0000 92

  5 omega   22.00   48.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036   56.0000  -67.0000 26

  6 omega   37.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036   56.0000 -150.0000 64

  7 omega   16.00   99.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036   37.0000   30.0000 83

  8 omega   46.00   97.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036   37.0000  -90.0000 51

  9 omega   30.00   95.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036   77.0000  120.0000 65

 10 omega  -24.00   34.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       34.8036  -68.0000  -81.0000 58

 11 omega   82.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 27

 12 omega   70.00  150.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 80

 13 omega  100.00  167.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 67

 14 omega   42.00   97.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 55

 15 omega   41.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 50

 16 omega   92.00  173.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 81

 17 omega   75.00  100.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -120.0000 25

 18 omega   41.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 57

 19 omega   45.00  122.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000    0.0000 77

 20 omega  126.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 48

 21 omega   81.00  106.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 25

 22 omega   81.00  107.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 26

 23 omega   92.00  117.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 25

 24 omega   92.00  118.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   56.0000 -150.0000 26

 25 omega   88.00  117.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   68.0000 -128.0000 29

 26 omega  127.00  163.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   68.0000 -128.0000 36

 27 omega   70.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 32

 28 omega   96.00  123.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -180.0000 27

 29 omega   72.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -150.0000 26

 30 omega   92.00  117.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 25

 31 omega  134.00  160.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 26

 32 omega  103.00  129.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000    0.0000 26

 33 omega   81.00  107.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -150.0000 26

 34 omega  121.00  170.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 49

 35 omega  143.00  169.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -120.0000 26

 36 omega  127.00  173.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 46

 37 omega   85.00  111.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 26
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0353631000
_diffrn_orient_matrix_UB_12      -0.0655429000
_diffrn_orient_matrix_UB_13      0.0871464000
_diffrn_orient_matrix_UB_21      0.1474034000
_diffrn_orient_matrix_UB_22      -0.0573304000
_diffrn_orient_matrix_UB_23      0.0224711000
_diffrn_orient_matrix_UB_31      0.0641712000
_diffrn_orient_matrix_UB_32      0.0957213000
_diffrn_orient_matrix_UB_33      0.0732708000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11802
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.096
_diffrn_reflns_theta_min         3.328
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2489 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         5749
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0570P)^2^+0.1885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                5585
_reflns_number_total             5749
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np7b00615_si_002.cif
_cod_data_source_block           exp_4149
_cod_original_cell_volume        1531.09(8)
_cod_database_code               1548732
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.757
_shelx_hkl_checksum              86119
_shelx_res_checksum              34207
_shelx_shelxl_version_number     2014/7