Natural Thioredoxin Reductase Inhibitors from Jatropha integerrima
yin, sheng; Zhu, Jian-Yong; Lou, Lan-Lan; Guo, Yan-Qiong; Li, Wei; Guo, Yan-Hong; Bao, Jing-Mei; Tang, Gui-Hua; Bu, Xianzhang; RSC Adv.  (2015) –; doi:10.1039/C5RA07274C

data_7220529
_publ_section_title
;
 Natural Thioredoxin Reductase Inhibitors from Jatropha integerrima
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07274C
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H28 O4'
_chemical_formula_sum            'C20 H28 O4'
_chemical_formula_weight         332.42
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_Hall           'P 31'
_space_group_name_H-M_alt        'P 31'
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-10-30 deposited with the CCDC.
2015-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.57764(10)
_cell_length_b                   14.57764(10)
_cell_length_c                   7.54977(6)
_cell_measurement_reflns_used    15320
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.6970
_cell_measurement_theta_min      3.4710
_cell_volume                     1389.437(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2417
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega -118.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2034  -38.0000 -120.0000 105

  2 omega -119.00  -73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2034 -125.0000 -120.0000 46

  3 omega -119.00  -73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2034 -125.0000   90.0000 46

  4 omega -126.00  -79.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.2034  -99.0000  -30.0000 47

  5 omega   15.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       42.2034   57.0000 -180.0000 100

  6 omega   71.00  175.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   39.0000  168.0000 104

  7 omega   72.00  174.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   45.0000  -60.0000 102

  8 omega   71.00  174.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   61.0000 -120.0000 103

  9 omega   71.00  174.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   61.0000  -90.0000 103

 10 omega   15.00  109.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -94.0000   90.0000 94

 11 omega   21.00  134.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -77.0000  -90.0000 113

 12 omega   21.00  134.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -77.0000   30.0000 113

 13 omega   26.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -45.0000  -90.0000 51

 14 omega   26.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -61.0000   30.0000 103

 15 omega   26.00  129.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -61.0000  -90.0000 103

 16 omega   24.00  122.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -125.0000   60.0000 98

 17 omega   23.00   69.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -30.0000  -60.0000 46

 18 omega   26.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -45.0000 -150.0000 51

 19 omega   66.00  167.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   77.0000 -120.0000 101

 20 omega   24.00   65.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -30.0000   60.0000 41

 21 omega   28.00   91.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000 -125.0000  150.0000 63

 22 omega   15.00   74.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -94.0000 -180.0000 59

 23 omega  115.00  141.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  125.0000  150.0000 26

 24 omega   26.00   76.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      100.0000  -45.0000   60.0000 50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0164338000
_diffrn_orient_matrix_UB_12      -0.0303518000
_diffrn_orient_matrix_UB_13      0.1879486000
_diffrn_orient_matrix_UB_21      -0.0243082000
_diffrn_orient_matrix_UB_22      -0.1094278000
_diffrn_orient_matrix_UB_23      -0.0684924000
_diffrn_orient_matrix_UB_31      0.1185066000
_diffrn_orient_matrix_UB_32      0.0446832000
_diffrn_orient_matrix_UB_33      -0.0400845000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17884
_diffrn_reflns_theta_full        71.76
_diffrn_reflns_theta_max         71.76
_diffrn_reflns_theta_min         3.50
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.154
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3593
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0262
_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^)+(0.0463P)^2^+0.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0696
_reflns_number_gt                3535
_reflns_number_total             3593
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra07274c2.cif
_cod_data_source_block           zjy_yjiz_9td_2_141022
_cod_original_cell_volume        1389.436(17)
_cod_database_code               7220529
_reflns_odcompleteness_completeness 98.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C17(H17)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C1A(H1AA,H1AB,
 H1AC), C1B(H1BA,H1BB,H1BC)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'