Pleurospiroketals A-E, Perhydrobenzannulated 5,5-Spiroketal Sesquiterpenes from the Edible Mushroom Pleurotus cornucopiae.
Wang, Shao-Juan; Bao, Li; Han, Jun-Jie; Wang, Quan-Xin; Yang, Xiao-Li; Wen, Hua-An; Guo, Liang-Dong; Li, Shao-Jie; Zhao, Feng; Liu, Hong-Wei; Journal of natural products 76 (2013) 45–50; doi:10.1021/np3006524

data_1508839
_publ_section_title
;
 Pleurospiroketals A-E, Perhydrobenzannulated 5,5-Spiroketal
 Sesquiterpenes from the Edible Mushroom Pleurotus cornucopiae.
;
_journal_issue                   1
_journal_name_full               'Journal of natural products'
_journal_page_first              45
_journal_page_last               50
_journal_paper_doi               10.1021/np3006524
_journal_volume                  76
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H22 O5'
_chemical_formula_sum            'C15 H22 O5'
_chemical_formula_weight         282.33
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-02-22
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.89040(10)
_cell_length_b                   10.02150(10)
_cell_length_c                   15.2050(2)
_cell_measurement_reflns_used    8751
_cell_measurement_temperature    155.0
_cell_measurement_theta_max      62.7091
_cell_measurement_theta_min      2.9038
_cell_volume                     1507.07(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_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, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      155.0
_diffrn_detector_area_resol_mean 16.0288
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -58.00  -16.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184  112.0000 -171.0000 42

  2 omega  -58.00   -8.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184  112.0000   84.0000 50

  3 omega   10.00  104.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000  -90.0000 94

  4 omega   38.00   71.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184 -112.0000  -84.0000 33

  5 omega   23.00   76.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000   90.0000 53

  6 omega   43.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000  -90.0000 28

  7 omega   20.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -77.0000  -60.0000 71

  8 omega   19.00   86.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000 -112.0000   95.0000 67

  9 omega   98.00  154.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000  120.0000 56

 10 omega  109.00  154.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000   90.0000 45

 11 omega   63.00   89.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000 -120.0000 26

 12 omega  100.00  153.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000 -120.0000 53

 13 omega   73.00   99.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -77.0000  120.0000 26

 14 omega   75.00  118.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000   30.0000 43

 15 omega   86.00  150.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  150.0000 64

 16 omega   70.00   95.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000   90.0000 25

 17 omega   33.00   59.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000    0.0000 26

 18 omega    8.00  106.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   38.0000    0.0000 98

 19 omega    3.00  103.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   77.0000   60.0000 100

 20 omega    3.00  103.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       33.1184   77.0000  150.0000 100

 21 omega   67.00  162.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000   60.0000 95

 22 omega   20.00  121.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -77.0000  -90.0000 101

 23 omega   68.00  158.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   63.0000 -152.0000 90

 24 omega   67.00  162.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   45.0000  -30.0000 95

 25 omega   60.00  161.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  150.0000 101

 26 omega   60.00  161.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  -90.0000 101

 27 omega   60.00  161.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000   77.0000  -30.0000 101

 28 omega   19.00  128.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -91.0000  124.0000 109

 29 omega   19.00   77.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.5000  -45.0000 -180.0000 58

 30 omega  -59.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184   38.0000  -60.0000 80

 31 omega  -82.00   -8.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -33.1184  112.0000    8.0000 74
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0496591000
_diffrn_orient_matrix_UB_12      -0.0844834000
_diffrn_orient_matrix_UB_13      0.0782820000
_diffrn_orient_matrix_UB_21      0.0985219000
_diffrn_orient_matrix_UB_22      0.0743712000
_diffrn_orient_matrix_UB_23      0.0612841000
_diffrn_orient_matrix_UB_31      -0.1099310000
_diffrn_orient_matrix_UB_32      0.1047071000
_diffrn_orient_matrix_UB_33      0.0195858000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14791
_diffrn_reflns_theta_full        62.80
_diffrn_reflns_theta_max         62.80
_diffrn_reflns_theta_min         5.29
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             608
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0419P)^2^+0.4419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                2340
_reflns_number_total             2416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np3006524_si_002.cif
_cod_data_source_block           gh_l194_3_4_5_1_3
_cod_database_code               1508839
_reflns_odcompleteness_completeness 97.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.60