E- or Z-Selective Knoevenagel Condensation of Acetoacetic Derivatives: Effect of Acylated Substituent, that is, TEMPO and Amines, as an Auxiliary, and New Accesses to Trisubstituted E- and Z-2-Alkenals and Furans
Tsutomu Inokuchi; Hiroyuki Kawafuchi; Journal of Organic Chemistry 71 (2006) 947–953; doi:10.1021/jo051952w

data_4021430
_publ_section_title
;
 E- or Z-Selective Knoevenagel Condensation of Acetoacetic
 Derivatives: Effect of Acylated Substituent, that is, TEMPO
 and Amines, as an Auxiliary, and New Accesses to Trisubstituted
 E- and Z-2-Alkenals and Furans
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              947
_journal_page_last               953
_journal_paper_doi               10.1021/jo051952w
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C36 H50 N2 O8'
_chemical_formula_weight         638.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Jun 28 23:31:16 2005'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                89.994(4)
_cell_angle_beta                 99.071(5)
_cell_angle_gamma                90.032(2)
_cell_formula_units_Z            2
_cell_length_a                   8.268(1)
_cell_length_b                   22.444(3)
_cell_length_c                   9.7559(6)
_cell_measurement_reflns_used    6749
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      0.9
_cell_volume                     1787.7(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.8719
_diffrn_measured_fraction_theta_max 0.8719
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12815
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.790
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.500
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.18
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   4.331
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     565
_refine_ls_number_reflns         7136
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          2.8414
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2663
_reflns_number_gt                6337
_reflns_number_total             7136
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            jo051952wsi20050928_123853.cif
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C36 H50 N2 O8 '
_cod_database_code               4021430