New three-component reaction: novel formation of a seven-membered ring by the unexpected reaction at the gamma-position of the beta-keto ester.
Fujioka, Hiromichi; Murai, Kenichi; Kubo, Ozora; Ohba, Yusuke; Kita, Yasuyuki; Organic letters 9 (2007) 1687–1690; doi:10.1021/ol070402c

data_1505362
_publ_section_title
;
 New three-component reaction: novel formation of a seven-membered ring by
 the unexpected reaction at the gamma-position of the beta-keto ester.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              1687
_journal_page_last               1690
_journal_paper_doi               10.1021/ol070402c
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C15 H18 N2 O2 '
_chemical_formula_sum            'C15 H18 N2 O2'
_chemical_formula_weight         258.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 92.4184(11)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   6.34620(10)
_cell_length_b                   10.8112(2)
_cell_length_c                   19.3646(4)
_cell_measurement_reflns_used    12496
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      4.1
_cell_volume                     1327.42(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13427
_diffrn_reflns_theta_full        68.19
_diffrn_reflns_theta_max         68.19
_exptl_absorpt_coefficient_mu    0.699
_exptl_absorpt_correction_T_max  0.613
_exptl_absorpt_correction_T_min  0.529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             552.00
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.70
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2402
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[0.0019Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                1803
_reflns_number_total             2402
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol070402csi20070216_070902.cif
_cod_data_source_block           '_061017'
_cod_original_formula_sum        'C15 H18 N2 O2 '
_cod_database_code               1505362