Revision of the Absolute Configurations of Bethosides B and C and Their Aglycone
Victoria L. Challinor; Patricia Y. Hayes; Paul V. Bernhardt; William Kitching; Reginald P. Lehmann; James J. De Voss; Journal of Organic Chemistry 76 (2011) 7275–7280; doi:10.1021/jo2012797

data_4026565
_publ_section_title
;
 Revision of the Absolute Configurations of Bethosides B and C and Their
 Aglycone
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7275
_journal_page_last               7280
_journal_paper_doi               10.1021/jo2012797
_journal_volume                  76
_journal_year                    2011
_chemical_formula_moiety         'C27 H42 O4'
_chemical_formula_sum            'C27 H52 O7'
_chemical_formula_weight         488.69
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.756(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.6540(16)
_cell_length_b                   5.9858(12)
_cell_length_c                   19.445(2)
_cell_measurement_reflns_used    952
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.5881
_cell_measurement_theta_min      3.7901
_cell_volume                     1356.3(4)
_computing_cell_refinement
;
 ?
;
_computing_data_collection
;
 ?
;
_computing_data_reduction
;
 ?
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0595
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5446
_diffrn_reflns_theta_full        62.42
_diffrn_reflns_theta_max         62.42
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.50138
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.2(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3097
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1625P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2006
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                2573
_reflns_number_total             3097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2012797_si_002.cif
_cod_data_source_block           472vc2
_cod_original_cell_volume        1356.4(4)
_cod_database_code               4026565