Ni(II)-salt catalyzed activation of primary amine-sp3Calpha-H and cyclization with 1,2-diketone to tetrasubstituted imidazoles
Srikanta Samanta; Dipanwita Roy; Saikat Khamarui; Dilip K. Maiti; Chem.Commun. 50 (2014) 2477–; doi:10.1039/c3cc48437h

data_7112027
_publ_section_title
;
 Ni(II)-salt catalyzed activation of primary amine-sp3Calpha-H and
 cyclization with 1,2-diketone to tetrasubstituted imidazoles
;
_journal_name_full               Chem.Commun.
_journal_page_first              2477
_journal_paper_doi               10.1039/c3cc48437h
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C28 H22 N2'
_chemical_formula_sum            'C28 H22 N2'
_chemical_formula_weight         387.48
_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                94.42(3)
_cell_angle_beta                 103.09(3)
_cell_angle_gamma                91.42(2)
_cell_formula_units_Z            4
_cell_length_a                   10.24(2)
_cell_length_b                   10.26(2)
_cell_length_c                   21.35(4)
_cell_measurement_temperature    296(2)
_cell_volume                     2176(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.994
_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  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0826
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6493
_diffrn_reflns_theta_full        20.73
_diffrn_reflns_theta_max         20.73
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9696
_exptl_absorpt_correction_T_min  0.9445
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.86
_exptl_crystal_size_mid          0.66
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         4198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.150
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1239P)^2^+2.8741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2588
_refine_ls_wR_factor_ref         0.2767
_reflns_number_gt                2938
_reflns_number_total             4198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc48437h.txt
_cod_data_source_block           ss39A_Om
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7112027