Dioxatricyclic and Oxabicyclic Polyketides from Trichocladium opacum.
Chen, Shenxi; Ren, Fengxia; Niu, Shubin; Liu, Xingzhong; Che, Yongsheng; Journal of natural products 77 (2014) 9–14; doi:10.1021/np4004799

data_1513371
_publ_section_title
;
 Dioxatricyclic and Oxabicyclic Polyketides from Trichocladium opacum.
;
_journal_issue                   1
_journal_name_full               'Journal of natural products'
_journal_page_first              9
_journal_page_last               14
_journal_paper_doi               10.1021/np4004799
_journal_volume                  77
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C11 H16 O5'
_chemical_formula_sum            'C11 H16 O5'
_chemical_formula_weight         228.24
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-25
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 103.612(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9972(8)
_cell_length_b                   7.3788(3)
_cell_length_c                   15.5846(10)
_cell_measurement_reflns_used    2014
_cell_measurement_temperature    102.7
_cell_measurement_theta_max      71.5620
_cell_measurement_theta_min      4.5492
_cell_volume                     1117.34(13)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution
'A short history of SHELX (Sheldrick, 2007)/Bruker'
_diffrn_ambient_temperature      102.7
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
  1 omega   21.00   65.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -120.0000 44

  2 omega  -71.00  -43.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000    0.0000 -120.0000 28

  3 omega  -92.00    3.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  125.0000    0.0000 95

  4 omega -112.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 87

  5 omega   35.00  123.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       56.0000   77.0000  120.0000 88

  6 omega  108.00  134.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  -30.0000 26

  7 omega   42.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -81.0000  -46.0000 30

  8 omega  139.00  165.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   90.0000 26

  9 omega   42.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000   60.0000 48

 10 omega   44.00   77.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -45.0000 -120.0000 33

 11 omega   99.00  174.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000   77.0000   30.0000 75

 12 omega  114.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  111.0000  120.0000 63

 13 omega   88.00  134.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      112.0000  -81.0000  -46.0000 46
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0144259000
_diffrn_orient_matrix_UB_12      -0.1743948000
_diffrn_orient_matrix_UB_13      0.0558849000
_diffrn_orient_matrix_UB_21      0.1520358000
_diffrn_orient_matrix_UB_22      0.0459999000
_diffrn_orient_matrix_UB_23      0.0408908000
_diffrn_orient_matrix_UB_31      -0.0428285000
_diffrn_orient_matrix_UB_32      0.1051478000
_diffrn_orient_matrix_UB_33      0.0746547000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3839
_diffrn_reflns_theta_full        71.65
_diffrn_reflns_theta_max         71.65
_diffrn_reflns_theta_min         2.92
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80909
_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_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(12)
_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     297
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+0.2366P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                3792
_reflns_number_total             3839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np4004799_si_002.cif
_cod_data_source_block           exp_918
_cod_original_cell_volume        1117.33(13)
_cod_database_code               1513371
_reflns_odcompleteness_completeness 89.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97