Inter- and Intramolecular [4 + 1]-Cycloadditions Between Electron-Poor Dienes and Electron-Rich Carbenes
Claude Spino; Hadi Rezaei; Kristina Dupont-Gaudet; Francis Bélanger; Journal of the American Chemical Society 126 (2004) 9926–9927; doi:10.1021/ja046344x

data_4112848
_publ_section_title
;
 Inter- and Intramolecular [4 + 1]-Cycloadditions Between Electron-Poor
 Dienes and Electron-Rich Carbenes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9926
_journal_page_last               9927
_journal_paper_doi               10.1021/ja046344x
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C17 H19 N O6'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.99(5)
_cell_angle_beta                 73.01(7)
_cell_angle_gamma                77.47(6)
_cell_formula_units_Z            2
_cell_length_a                   7.843(7)
_cell_length_b                   10.205(5)
_cell_length_c                   10.691(8)
_cell_measurement_temperature    293(2)
_cell_volume                     798.1(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2829
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_correction_T_min  0.9490
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Colorless
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_exptl_crystal_description       Plates
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.50
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_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1068P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046344xsi20040621_105612.cif
_cod_data_source_block           hr2-179
_cod_original_cell_volume        798.1(10)
_cod_database_code               4112848