Studies towards the total synthesis of solanoeclepin A: synthesis of the 7-oxabicyclo[2.2.1]heptane moiety and attempted seven-membered ring formation
Benningshof, Jorg C. J.; Blaauw, Richard H.; van Ginkel, Angeline E.; van Maarseveen, Jan H.; Rutjes, Floris P. J. T.; Hiemstra, Henk; Journal of the Chemical Society, Perkin Transactions 1  (2002) 1693–; doi:10.1039/b201987f

data_7204380
_publ_section_title
;
 Studies towards the total synthesis of solanoeclepin A: synthesis of
 the 7-oxabicyclo[2.2.1]heptane moiety and attempted seven-membered
 ring formation
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              1693
_journal_paper_doi               10.1039/b201987f
_journal_year                    2002
_chemical_formula_sum            'C19 H24 O6'
_chemical_formula_weight         348.4
_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'
_audit_creation_date             01-11-07
_audit_creation_method           Xtal3.7.1
_cell_angle_alpha                90.00000
_cell_angle_beta                 103.395(9)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            2
_cell_length_a                   8.5854(7)
_cell_length_b                   8.3775(7)
_cell_length_c                   12.4280(10)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    253
_cell_measurement_theta_max      44.53
_cell_measurement_theta_min      40.06
_cell_volume                     869.56(13)
_computing_cell_refinement       'local program'
_computing_data_collection       'CAD4 software'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  .02
_diffrn_reflns_av_sigmaI/netI    .026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2401
_diffrn_reflns_reduction_process 'perpendicular monochr Lp'
_diffrn_reflns_theta_max         74.63
_diffrn_reflns_theta_min         3.66
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.82
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         .401
_refine_diff_density_min         -.274
_refine_ls_abs_structure_details 'Flack xabs refined'
_refine_ls_abs_structure_Flack   -.7(3)
_refine_ls_extinction_coef       670(93)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   .989
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     228
_refine_ls_number_reflns         1651.5
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .066
_refine_ls_R_factor_gt           .06
_refine_ls_shift/su_max          .02
_refine_ls_shift/su_mean         .005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w=1/(1.0 + 0.01*(\s(Fobs)^2^) + 0.01/(\s(Fobs)))'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .07
_refine_ls_wR_factor_ref         .068
_reflns_d_resolution_high        .799
_reflns_d_resolution_low         12.061
_reflns_limit_h_max              10
_reflns_limit_h_min              0
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                2051
_reflns_number_total             1907
_reflns_threshold_expression     'Iobs > 2.50 sig(Iobs)'
_cod_data_source_file            b201987f.txt
_cod_data_source_block           p17jor
_cod_original_sg_symbol_Hall     p_2yb
_cod_original_sg_symbol_H-M      p_1_21_1
_cod_database_code               7204380