Quassinoids with Inhibitory Activities against Plant Fungal Pathogens from <i>Picrasma javanica</i>.
Chen, Jian-Jun; Bai, Wei; Lu, Yu-Bo; Feng, Zi-Yun; Gao, Kun; Yue, Jian-Min; Journal of natural products  (2021) –; doi:10.1021/acs.jnatprod.1c00096

data_1563901
_publ_section_title
;
 Quassinoids with Inhibitory Activities against Plant Fungal Pathogens
 from <i>Picrasma javanica</i>.
;
_journal_name_full               'Journal of natural products'
_journal_paper_doi               10.1021/acs.jnatprod.1c00096
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C31 H36 O11'
_chemical_formula_sum            'C31 H36 O11'
_chemical_formula_weight         584.60
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-11-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8318(5)
_cell_length_b                   14.3813(6)
_cell_length_c                   16.3643(6)
_cell_measurement_reflns_used    5237
_cell_measurement_temperature    298.4(6)
_cell_measurement_theta_max      70.2610
_cell_measurement_theta_min      4.0840
_cell_volume                     2784.49(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      298.4(6)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -64.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 30

  2 omega  -17.00   11.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 28

  3 omega   27.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 44

  4 omega  -81.00  -47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   30.0000 34

  5 omega    7.00   33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000    0.0000 26

  6 omega   34.00   97.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -120.0000 63

  7 omega   46.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000  150.0000 78

  8 omega   28.00  123.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   38.0000  -30.0000 95

  9 omega   83.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  149.0000  -67.0000 43

 10 omega   43.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -180.0000 51

 11 omega   82.00  111.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  150.0000 29

 12 omega   46.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000  150.0000 25

 13 omega   49.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000  150.0000 45

 14 omega   40.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000  150.0000 32

 15 omega   79.00  105.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -124.0000   48.0000 26

 16 omega   55.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  -30.0000 26

 17 omega  109.00  134.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   90.0000 25

 18 omega  141.00  166.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  150.0000 25

 19 omega   39.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   60.0000 53

 20 omega  105.00  131.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  150.0000 26

 21 omega   53.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 50

 22 omega   53.00   79.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000   60.0000 26

 23 omega  100.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   63.0000  150.0000 74

 24 omega  122.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   38.0000  -30.0000 52

 25 omega   53.00  100.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000   60.0000 47

 26 omega  125.00  150.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -91.0000   60.0000 25

 27 omega  133.00  171.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 38

 28 omega   86.00  115.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000 -180.0000 29

 29 omega   45.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -35.0000  -90.0000 25

 30 omega   54.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000  150.0000 50

 31 omega   91.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   38.0000   90.0000 86

 32 omega  148.00  173.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   38.0000  -60.0000 25

 33 omega  102.00  128.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   38.0000  -60.0000 26
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0039062000
_diffrn_orient_matrix_UB_12      0.0984489000
_diffrn_orient_matrix_UB_13      -0.0369893000
_diffrn_orient_matrix_UB_21      -0.1298543000
_diffrn_orient_matrix_UB_22      -0.0002713000
_diffrn_orient_matrix_UB_23      0.0069186000
_diffrn_orient_matrix_UB_31      0.0084496000
_diffrn_orient_matrix_UB_32      0.0421939000
_diffrn_orient_matrix_UB_33      0.0863192000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14433
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.039
_diffrn_reflns_theta_min         4.092
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.884
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Flack x determined using 1828 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1352P)^2^+0.2161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2033
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4797
_reflns_number_total             5263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np1c00096_si_002.cif
_cod_data_source_block           chenjj0628
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_absolute_configuration' value 'AD' was changed
to 'ad' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2784.5(2)
_cod_database_code               1563901
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 93.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
2.a Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C11(H11), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B), C15(H15A,H15B), C29(H29A,H29B)
2.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C28(H28)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              97680
_shelx_hkl_checksum              54
_olex2_submission_special_instructions 'No special instructions were received'