Antiviral Triterpenes from the Twigs and Leaves of Lyonia ovalifolia
Lv, Xiao-Jing; Li, Yong; Ma, Shuang-Gang; Qu, Jing; Liu, Yun-Bao; Li, Yu-Huan; Zhang, Dan; Li, Li; Yu, Shi-Shan; Journal of Natural Products  (2016) –; doi:10.1021/acs.jnatprod.6b00585

data_1544415
_publ_section_title
;
 Antiviral Triterpenes from the Twigs and Leaves of Lyonia ovalifolia
;
_journal_name_full               'Journal of Natural Products'
_journal_paper_doi               10.1021/acs.jnatprod.6b00585
_journal_year                    2016
_chemical_formula_moiety         'C30 H48 O5'
_chemical_formula_sum            'C30 H48 O5'
_chemical_formula_weight         488.68
_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   geom
_audit_creation_date             2015-12-01
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.036(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.3157(4)
_cell_length_b                   38.8550(13)
_cell_length_c                   13.6376(6)
_cell_measurement_reflns_used    16099
_cell_measurement_temperature    104.7
_cell_measurement_theta_max      71.1168
_cell_measurement_theta_min      3.5206
_cell_volume                     5517.9(4)
_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)'
_diffrn_ambient_temperature      104.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -11.00   15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  111.0000 -120.0000 26

  2 omega  -50.00  -16.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  111.0000 -120.0000 34

  3 omega  -31.00   15.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  111.0000   30.0000 46

  4 omega  -32.00   32.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000   30.0000 64

  5 omega   -6.00   52.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -77.0000   90.0000 58

  6 omega  -32.00    9.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000  -60.0000 41

  7 omega   12.00   55.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000  -60.0000 43

  8 omega   22.00   80.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   37.0000  -30.0000 58

  9 omega   15.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   77.0000 -150.0000 81

 10 omega   32.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   77.0000   60.0000 71

 11 omega   18.00   44.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919  -37.0000 -150.0000 26

 12 omega   24.00  103.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       36.7919   37.0000 -180.0000 79

 13 omega   71.00  127.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 56

 14 omega  147.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 26

 15 omega   84.00  110.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -122.0000   32.0000 26

 16 omega   39.00   76.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -122.0000   32.0000 37

 17 omega   75.00  115.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -60.0000 40

 18 omega  101.00  166.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -60.0000 65

 19 omega   94.00  132.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 38

 20 omega  137.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 38

 21 omega   93.00  124.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 31

 22 omega  146.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 30

 23 omega   91.00  120.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 29

 24 omega  148.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 27

 25 omega   93.00  125.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 32

 26 omega  109.00  144.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  150.0000 35

 27 omega   82.00  163.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   60.0000 81

 28 omega   91.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 30

 29 omega   45.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 53

 30 omega  129.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 44

 31 omega   56.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 35

 32 omega   81.00  107.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 26

 33 omega   50.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 47

 34 omega  146.00  173.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 27

 35 omega   54.00   82.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000    0.0000 -150.0000 28

 36 omega   41.00   74.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 33

 37 omega   57.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -106.0000   96.0000 55
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1419984000
_diffrn_orient_matrix_UB_12      -0.0060223000
_diffrn_orient_matrix_UB_13      -0.0731296000
_diffrn_orient_matrix_UB_21      -0.0010906000
_diffrn_orient_matrix_UB_22      0.0338121000
_diffrn_orient_matrix_UB_23      -0.0592951000
_diffrn_orient_matrix_UB_31      0.0418147000
_diffrn_orient_matrix_UB_32      -0.0198032000
_diffrn_orient_matrix_UB_33      -0.0788858000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40576
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.251
_diffrn_reflns_theta_min         3.522
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93500
_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_colour            colorless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.400
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 8922 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1297
_refine_ls_number_reflns         20912
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0506
_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^)+(0.0784P)^2^+2.1230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1340
_reflns_Friedel_coverage         0.944
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                19962
_reflns_number_total             20912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np6b00585_si_001.cif
_cod_data_source_block           exp_3709
_cod_database_code               1544415
_shelx_estimated_absorpt_t_max   0.791
_shelx_estimated_absorpt_t_min   0.769
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_shelx_res_checksum              28787
_shelx_hkl_checksum              91370
_shelx_shelxl_version_number     2014/7