Cu(TFA)2-Catalyzed Oxidative Tandem Cyclization/1,2-Alkyl Migration of Enamino Amides for Synthesis of Pyrrolin-4-ones
Zhang, Zhi-Jing; Ren, Zhi-Hui; Wang, Yao-Yu; Guan, Zheng-Hui; Organic Letters 15 (2013) 4822–; doi:10.1021/ol4022222

data_1512345
_publ_section_title
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 Cu(TFA)2-Catalyzed Oxidative Tandem Cyclization/1,2-Alkyl Migration of
 Enamino Amides for Synthesis of Pyrrolin-4-ones
;
_journal_issue                   18
_journal_name_full               'Organic Letters'
_journal_page_first              4822
_journal_paper_doi               10.1021/ol4022222
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C20 H19 N3 O3'
_chemical_formula_weight         349.38
_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                76.232(11)
_cell_angle_beta                 86.614(12)
_cell_angle_gamma                78.203(12)
_cell_formula_units_Z            2
_cell_length_a                   8.050(5)
_cell_length_b                   9.761(7)
_cell_length_c                   11.482(7)
_cell_measurement_reflns_used    658
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.19
_cell_measurement_theta_min      2.51
_cell_volume                     857.7(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4379
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9869
_exptl_absorpt_correction_T_min  0.9690
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.180
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1014
_refine_ls_R_factor_gt           0.0593
_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^)+(0.0872P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1814
_reflns_number_gt                1849
_reflns_number_total             3033
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4022222_si_002.cif
_cod_data_source_block           xb6523_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512345