Comparative effects of conjugated and deconjugated isomeric enones on the transannular Diels-Alder reaction.
Caussanel, Franck; Deslongchamps, Pierre; Dory, Yves L.; Organic letters 5 (2003) 4799–4802; doi:10.1021/ol035791z

data_1507406
_publ_section_title
;
 Comparative effects of conjugated and deconjugated isomeric enones on the
 transannular Diels-Alder reaction.
;
_journal_issue                   25
_journal_name_full               'Organic letters'
_journal_page_first              4799
_journal_page_last               4802
_journal_paper_doi               10.1021/ol035791z
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C22 H28 O9'
_chemical_formula_weight         436.44
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.709(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5871(15)
_cell_length_b                   21.160(4)
_cell_length_c                   11.2517(16)
_cell_measurement_temperature    293(2)
_cell_volume                     2282.4(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.679
_diffrn_measured_fraction_theta_max 0.679
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2777
_diffrn_reflns_theta_full        64.88
_diffrn_reflns_theta_max         64.88
_diffrn_reflns_theta_min         4.18
_exptl_absorpt_coefficient_mu    0.829
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             928
_refine_diff_density_max         0.137
_refine_diff_density_min         -0.139
_refine_diff_density_rms         0.034
_refine_ls_extinction_coef       0.0053(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0489P)^2^+1.2364P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1202
_reflns_number_gt                2332
_reflns_number_total             2633
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol035791zsi20030916_052011.cif
_cod_data_source_block           fc535
_cod_original_cell_volume        2282.4(7)
_cod_database_code               1507406