Anti-inflammatory Terpenoids from the Leaves and Twigs of Dysoxylum gotadhora.
Jiang, Kan; Chen, Lu-Lin; Wang, Shu-Fang; Wang, Yi; Li, Ya; Gao, Kun; Journal of natural products 78 (2015) 1037–1044; doi:10.1021/np5010196

data_1519614
_publ_section_title
;
 Anti-inflammatory Terpenoids from the Leaves and Twigs of Dysoxylum
 gotadhora.
;
_journal_issue                   5
_journal_name_full               'Journal of natural products'
_journal_page_first              1037
_journal_page_last               1044
_journal_paper_doi               10.1021/np5010196
_journal_volume                  78
_journal_year                    2015
_chemical_absolute_configuration none
_chemical_formula_moiety         'C20 H28 O2'
_chemical_formula_sum            'C20 H28 O2'
_chemical_formula_weight         300.42
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.588(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.4345(4)
_cell_length_b                   6.06696(15)
_cell_length_c                   12.7077(4)
_cell_measurement_reflns_used    4197
_cell_measurement_temperature    249(30)
_cell_measurement_theta_max      70.7210
_cell_measurement_theta_min      3.8520
_cell_volume                     864.64(5)
_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, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      249(30)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -80.00  -45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -60.0000 35

  2 omega  -64.00  -37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 27

  3 omega  -34.00   24.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 58

  4 omega  -18.00   25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000  -60.0000 43

  5 omega   27.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000    0.0000 56

  6 omega   -6.00   62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  150.0000 68

  7 omega   42.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 82

  8 omega   38.00  101.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -99.0000   60.0000 63

  9 omega   -9.00   87.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -38.0000  -30.0000 96

 10 omega   27.00   61.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000  -60.0000 34

 11 omega   38.00   98.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -150.0000 60

 12 omega   50.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000   90.0000 42

 13 omega   66.00  116.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  120.0000 50

 14 omega   75.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000   90.0000 26

 15 omega   65.00   94.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000    0.0000 29

 16 omega   68.00  165.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  -90.0000 97

 17 omega   93.00  138.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000 -150.0000 45

 18 omega  152.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   90.0000 25

 19 omega  101.00  126.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   63.0000  150.0000 25

 20 omega  101.00  136.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000   90.0000 35

 21 omega   37.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000    0.0000  -90.0000 77

 22 omega   42.00   82.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -150.0000 40

 23 omega   94.00  134.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000   90.0000 40

 24 omega   66.00  105.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000  120.0000 39

 25 omega  114.00  148.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000  120.0000 34

 26 omega  137.00  176.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   63.0000 -150.0000 39

 27 omega   38.00  114.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000  -90.0000 76

 28 omega  123.00  148.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  120.0000 25

 29 omega   72.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000   60.0000 26

 30 omega  141.00  172.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000   90.0000 31

 31 omega   46.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -50.0000 -120.0000 25

 32 omega   40.00   81.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000    0.0000 41

 33 omega   68.00  135.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000  -60.0000 67

 34 omega   64.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -63.0000   90.0000 26

 35 omega   40.00  126.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000   90.0000 86

 36 omega   99.00  125.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000  120.0000 26

 37 omega   37.00   69.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   60.0000 32
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0136383000
_diffrn_orient_matrix_UB_12      -0.1613671000
_diffrn_orient_matrix_UB_13      0.0986182000
_diffrn_orient_matrix_UB_21      0.0631002000
_diffrn_orient_matrix_UB_22      -0.1659110000
_diffrn_orient_matrix_UB_23      -0.0462864000
_diffrn_orient_matrix_UB_31      0.1212156000
_diffrn_orient_matrix_UB_32      0.1044987000
_diffrn_orient_matrix_UB_33      0.0787618000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5827
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.641
_diffrn_reflns_theta_min         3.857
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.561
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86259
_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 black'
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_description       block
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1369 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.08(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3211
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0445
_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^)+(0.0852P)^2^+0.0797P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1240
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_reflns_Friedel_fraction_full    0.976
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                3142
_reflns_number_total             3211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np5010196_si_004.cif
_cod_data_source_block           jk_2_47
_cod_depositor_comments
'Adding full bibliography for 1519613--1519615.cif.'
_cod_original_cell_volume        864.63(5)
_cod_database_code               1519614
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C5(H5), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C11(H11A,H11B), C12(H12A,H12B)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15)
2.d X=CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              2178
_shelx_hkl_checksum              62982
_olex2_submission_special_instructions 'No special instructions were received'