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_4112849
_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            'C16 H17 N O6'
_chemical_formula_weight         319.31
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_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.434(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.136(2)
_cell_length_b                   7.047(3)
_cell_length_c                   15.439(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70
_cell_measurement_theta_min      30
_cell_volume                     1537.9(8)
_computing_cell_refinement       Difrac
_computing_data_collection       Difrac
_computing_data_reduction        NRCVAX
_computing_molecular_graphics    Ortep-3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu Ka'
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2925
_diffrn_reflns_theta_full        69.92
_diffrn_reflns_theta_max         69.92
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       Needles
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0067(10)
_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   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1103P)^2^+1.3044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2172
_refine_ls_wR_factor_ref         0.2509
_reflns_number_gt                1572
_reflns_number_total             2925
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja046344xsi20040621_105636.cif
_cod_data_source_block           kdg155b
_cod_original_cell_volume        1537.8(7)
_cod_database_code               4112849