Trilobolide-6-<i>O</i>-isobutyrate, a eudesmanolide from <i>Wedelia trilobata</i>
Xue-Song Huang; Ren-Wang Jiang; Vincent Eng-Choon Ooi; Acta Crystallographica Section E 59 (2003) o771–o772; doi:10.1107/S1600536803009590

data_2202181
_publ_section_title
;
 Trilobolide-6-<i>O</i>-isobutyrate, a eudesmanolide from <i>Wedelia
 trilobata</i>
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o771
_journal_page_last               o772
_journal_paper_doi               10.1107/S1600536803009590
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C23 H32 O9'
_chemical_formula_moiety         'C23 H32 O9'
_chemical_formula_sum            'C23 H32 O9'
_chemical_formula_weight         452.49
_chemical_name_common            trilobolide-6-O-isobutyrate
_space_group_IT_number           170
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 65'
_symmetry_space_group_name_H-M   'P 65'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.8368(8)
_cell_length_b                   9.8368(8)
_cell_length_c                   42.455(5)
_cell_measurement_reflns_used    4824
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      2.44
_cell_volume                     3557.7(6)
_computing_cell_refinement       'SMART and SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SHELXS97 (Sheldrick, 1990)'
_computing_molecular_graphics    'XP (Bruker, 1998)'
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Siemens SMART/CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            19275
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.4
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.31
_refine_ls_abs_structure_Flack   unk
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2119
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.066
_refine_ls_R_factor_gt           0.051
_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^)+(0.105P)^2^+0.2647P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.141
_refine_ls_wR_factor_ref         0.153
_reflns_number_gt                3029
_reflns_number_total             4172
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            tk6094.cif
_cod_data_source_block           I
_cod_original_cell_volume        3557.6(6)
_cod_database_code               2202181
_cod_database_fobs_code          2202181