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_1519613
_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         'C30 H48 O4'
_chemical_formula_sum            'C30 H48 O4'
_chemical_formula_weight         472.68
_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   mixed
_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                 103.188(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4572(3)
_cell_length_b                   7.77569(19)
_cell_length_c                   19.2277(5)
_cell_measurement_reflns_used    3374
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.3520
_cell_measurement_theta_min      4.8460
_cell_volume                     1376.64(7)
_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      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega    3.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 43

  2 omega  -81.00  -45.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -30.0000 36

  3 omega   45.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 28

  4 omega   23.00   68.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -180.0000 45

  5 omega   20.00   71.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000 -120.0000 51

  6 omega   89.00  116.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000 -125.0000 -180.0000 27

  7 omega   -9.00   57.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000  -57.0000  -30.0000 66

  8 omega   71.00  119.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000   90.0000 48

  9 omega   38.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   57.0000 -150.0000 87

 10 omega   44.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000    0.0000 49

 11 omega   37.00   89.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000  -60.0000 52

 12 omega   39.00   65.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -37.0000  -90.0000 26

 13 omega   36.00   93.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000   60.0000 57

 14 omega   35.00   72.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -25.0000 -120.0000 37

 15 omega   37.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -38.0000   90.0000 25

 16 omega   39.00   95.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000 -111.0000 -150.0000 56

 17 omega   75.00  107.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000    0.0000 32

 18 omega  121.00  147.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -60.0000 26

 19 omega   85.00  174.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   12.0000  150.0000 89

 20 omega  126.00  151.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  178.0000    0.0000 25

 21 omega   88.00  113.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   38.0000   60.0000 25

 22 omega  133.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   38.0000   60.0000 44

 23 omega   64.00   90.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   25.0000  120.0000 26

 24 omega   52.00  137.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -77.0000    0.0000 85
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1444126000
_diffrn_orient_matrix_UB_12      -0.0908425000
_diffrn_orient_matrix_UB_13      -0.0331258000
_diffrn_orient_matrix_UB_21      -0.0479886000
_diffrn_orient_matrix_UB_22      0.0201668000
_diffrn_orient_matrix_UB_23      0.0709451000
_diffrn_orient_matrix_UB_31      -0.0695261000
_diffrn_orient_matrix_UB_32      0.1748520000
_diffrn_orient_matrix_UB_33      -0.0254291000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5707
_diffrn_reflns_point_group_measured_fraction_full 0.758
_diffrn_reflns_point_group_measured_fraction_max 0.744
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.278
_diffrn_reflns_theta_min         4.724
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81496
_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    1.140
_exptl_crystal_description       needle
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.192
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Flack x determined using 1076 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.03(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3912
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0953P)^2^+0.0530P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1310
_reflns_Friedel_coverage         0.401
_reflns_Friedel_fraction_full    0.480
_reflns_Friedel_fraction_max     0.462
_reflns_number_gt                3783
_reflns_number_total             3912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np5010196_si_003.cif
_cod_data_source_block           jiangk0311
_cod_depositor_comments
'Adding full bibliography for 1519613--1519615.cif.'
_cod_original_cell_volume        1376.64(6)
_cod_database_code               1519613
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.51
_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, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8), C17(H17), C20(H20), C23(H23), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,
 H12B), C15(H15A,H15B), C16(H16A,H16B), C19(H19A,H19B), C21(H21A,H21B),
 C22(H22A,H22B)
2.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              76417
_shelx_hkl_checksum              68107
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'