Ethyl <i>ent</i>-15α-[(2-methoxybenzyloxy)methyl]-16-oxobeyeran-20-oate
Wu, Ya; Wang, Xia; Gong, Jian-hong; Wei, Chang-yong; Tao, Jing-chao; Acta Crystallographica Section E 68 (2012) o495–; doi:10.1107/S1600536812001833

data_2233486
_publ_section_title
;
 Ethyl <i>ent</i>-15\a-[(2-methoxybenzyloxy)methyl]-16-oxobeyeran-20-oate
;
_journal_coeditor_code           HB6600
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o495
_journal_paper_doi               10.1107/S1600536812001833
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C31 H44 O5'
_chemical_formula_moiety         'C31 H44 O5'
_chemical_formula_sum            'C31 H44 O5'
_chemical_formula_weight         496.66
_chemical_name_systematic
;
Ethyl <i>ent</i>-15\a-[(2-methoxybenzyloxy)methyl]-16-oxobeyeran-20-oate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7047(17)
_cell_length_b                   10.749(2)
_cell_length_c                   29.653(6)
_cell_measurement_reflns_used    398
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      2.0
_cell_volume                     2774.5(9)
_computing_cell_refinement       'RAXIS (Rigaku, 2004)'
_computing_data_collection       'RAXIS (Rigaku, 2004)'
_computing_data_reduction        'RAXIS (Rigaku, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Rgaku R-AXIS-IV'
_diffrn_measurement_method       'Oscillation  frames'
_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  0.1016
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_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            8377
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(RAXIS; Rigaku, 2004)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.209
_refine_diff_density_min         -0.193
_refine_ls_abs_structure_details none
_refine_ls_extinction_coef       0.023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         2876
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0652
_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^)+(0.0776P)^2^+0.8183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1613
_refine_ls_wR_factor_ref         0.1717
_reflns_number_gt                2419
_reflns_number_total             2876
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb6600.cif
_cod_data_source_block           I
_cod_database_code               2233486
_cod_database_fobs_code          2233486