Epivernadol diacetate
Koul, Jawahir L.; Koul, Surrinder; Taneja, Subbash C.; Schürmann, Markus; Preut, Hans; Spiteller, Michael; Acta Crystallographica Section E 61 (2005) o3349–o3350; doi:10.1107/S1600536805029387

data_2206880
_publ_section_title
;
 Epivernadol diacetate
;
_journal_coeditor_code           BT6736
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3349
_journal_page_last               o3350
_journal_paper_doi               10.1107/S1600536805029387
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C24 H28 O10'
_chemical_formula_moiety         'C24 H28 O10'
_chemical_formula_sum            'C24 H28 O10'
_chemical_formula_weight         476.46
_chemical_name_common            'Epivernadol diacetate'
_chemical_name_systematic
;
(4aR,5R,6S,7S,8aS)-methyl
8a-ethenyloctahydro-5-acetoxy-7-{[2-(acetoxymethyl)-1-oxo-2-propenyl]oxy}-
\a,4-bis(methylene)-3-oxo-1H-2-benzopyran-6-acetate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0887(2)
_cell_length_b                   12.8750(4)
_cell_length_c                   23.8205(8)
_cell_measurement_reflns_used    14723
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      2.97
_cell_volume                     2480.71(13)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2001)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
208 frames via \w-rotation (\D\w=1\%) and two times 60 s per frame
(two sets at different \k-angles)
;
_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  0.069
_diffrn_reflns_av_sigmaI/netI    0.0766
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            14723
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.144
_refine_ls_extinction_coef       0.0057(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         2589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0643P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1154
_reflns_number_gt                1373
_reflns_number_total             2589
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6736.cif
_cod_data_source_block           I
_cod_database_code               2206880
_cod_database_fobs_code          2206880