DBU-catalyzed tandem additions of electron-deficient 1,3-conjugated enynes with 2-aminomalonates: a facile access to highly substituted 2-pyrrolines
Xiuzhao Yu; Guanghua Zhou; Junliang Zhang; Chemical Communications 48 (2012) 4002–4004; doi:10.1039/c2cc30840a

data_7107583
_publ_section_title
;
 DBU-catalyzed tandem additions of electron-deficient 1,3-conjugated
 enynes with 2-aminomalonates: a facile access to highly substituted
 2-pyrrolines
;
_journal_issue                   33
_journal_name_full               'Chemical Communications'
_journal_page_first              4002
_journal_page_last               4004
_journal_paper_doi               10.1039/c2cc30840a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C28 H31 N O8'
_chemical_formula_weight         509.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.978(2)
_cell_angle_beta                 83.172(2)
_cell_angle_gamma                72.281(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0165(7)
_cell_length_b                   9.2153(7)
_cell_length_c                   16.4934(12)
_cell_measurement_temperature    296(2)
_cell_volume                     1296.16(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14351
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.573073
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.459
_exptl_crystal_size_min          0.305
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4523
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0528
_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^)+(0.0692P)^2^+0.8505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1675
_reflns_number_gt                3288
_reflns_number_total             4523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc30840a.txt
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107583