Catalytic intermolecular beta-C-H alkenylation of alpha-enamino-ketones with simple alkynes
Zhiqian Wang; Brandon J. Reinus; Guangbin Dong; Chem.Commun. 50 (2014) 5230–; doi:10.1039/C3CC47556E

data_7112627
_publ_section_title
;
 Catalytic intermolecular beta-C-H alkenylation of alpha-enamino-ketones
 with simple alkynes
;
_journal_name_full               Chem.Commun.
_journal_page_first              5230
_journal_paper_doi               10.1039/C3CC47556E
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C24 H18 N2 O'
_chemical_formula_weight         350.40
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.30
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.425
_cell_length_b                   14.739
_cell_length_c                   16.609
_cell_measurement_temperature    153(2)
_cell_volume                     4020.786
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2157
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9136
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    0.071
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1472
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9137
_refine_ls_number_restraints     338
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.2171
_refine_ls_R_factor_gt           0.1100
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1080P)^2^+2.5245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2471
_refine_ls_wR_factor_ref         0.3097
_reflns_number_gt                4167
_reflns_number_total             9137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47556e.txt
_cod_data_source_block           shelxl
_cod_depositor_comments
;

2018-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C96 H72 N8 O4'
_cod_original_formula_weight         1401.62
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4020.8
_cod_database_code               7112627