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_1513373
_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 unk
_chemical_formula_moiety         'H2 O, C11 H16 O5'
_chemical_formula_sum            'C11 H18 O6'
_chemical_formula_weight         246.25
_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             2012-06-27
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6087(5)
_cell_length_b                   6.6339(4)
_cell_length_c                   27.605(2)
_cell_measurement_reflns_used    1616
_cell_measurement_temperature    103.1
_cell_measurement_theta_max      29.3070
_cell_measurement_theta_min      3.1519
_cell_volume                     1210.24(15)
_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      103.1
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega   38.00   71.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       21.1393    0.0000  -90.0000 33

  2 omega  -52.00   65.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       21.1393    0.0000   30.0000 117

  3 omega  -52.00    5.00   1.0000    3.5000
omega____ theta____ kappa____ phi______ frames
    -       21.1393    0.0000  -90.0000 57
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0680666000
_diffrn_orient_matrix_UB_12      0.0081276000
_diffrn_orient_matrix_UB_13      -0.0198003000
_diffrn_orient_matrix_UB_21      -0.0607333000
_diffrn_orient_matrix_UB_22      -0.0773691000
_diffrn_orient_matrix_UB_23      0.0101139000
_diffrn_orient_matrix_UB_31      -0.0565544000
_diffrn_orient_matrix_UB_32      0.0732803000
_diffrn_orient_matrix_UB_33      0.0129011000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            4604
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86045
_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    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.202
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.350
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      0.348
_refine_ls_R_factor_all          0.1718
_refine_ls_R_factor_gt           0.1693
_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^)+(0.0001P)^2^+400.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4022
_refine_ls_wR_factor_ref         0.4033
_reflns_number_gt                2281
_reflns_number_total             2341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np4004799_si_003.cif
_cod_data_source_block           exp_686
_cod_original_cell_volume        1210.23(15)
_cod_database_code               1513373
_reflns_odcompleteness_completeness 97.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32