Divergent synthesis from reactions of 2-trifluoromethyl-1,3-conjugated enynes with N-acetylated 2-aminomalonates.
Yang, Jieru; Zhou, Xiaofan; Zeng, Yu; Huang, Chaoqian; Xiao, Yuanjing; Zhang, Junliang; Organic & biomolecular chemistry 15 (2017) 2253–2258; doi:10.1039/c6ob02749k

data_7155551
_publ_section_title
;
 Divergent synthesis from reactions of 2-trifluoromethyl-1,3-conjugated
 enynes with N-acetylated 2-aminomalonates.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2253
_journal_page_last               2258
_journal_paper_doi               10.1039/c6ob02749k
_journal_volume                  15
_journal_year                    2017
_chemical_formula_sum            'C20 H22 F3 N O5'
_chemical_formula_weight         413.39
_chemical_name_systematic
'(Z)-diethyl 1-acetyl-5-benzylidene-4-(trifluoromethyl)pyrrolidine-2,2-dicarboxylate'
_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
_audit_update_record
;
2016-03-13 deposited with the CCDC.
2017-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                103.635(2)
_cell_angle_beta                 97.925(2)
_cell_angle_gamma                91.114(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8343(4)
_cell_length_b                   10.9242(5)
_cell_length_c                   10.9439(5)
_cell_measurement_temperature    296(2)
_cell_volume                     1015.12(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11891
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9842
_exptl_absorpt_correction_T_min  0.9665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0677P)^2^+0.4206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1270
_refine_ls_wR_factor_ref         0.1526
_reflns_number_gt                2564
_reflns_number_total             3536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ob02749k2.cif
_cod_data_source_block           z
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7155551
_solvent_exptl_crystal_recrystallization_method DCM/Hexane