Efficient catalytic cyclizations of three and two imine assemblies: direct access to tetrahydroimidazo[1,5-c]imidazol-7-ones and imidazoles
Yasmin Saima; Saikat Khamarui; Krishnanka S. Gayen; Palash Pandit; Dilip K. Maiti; Chem.Commun. 48 (2012) 6601–; doi:10.1039/c2cc32760k

data_7107943
_publ_section_title
;
 Efficient catalytic cyclizations of three and two imine assemblies:
 direct access to tetrahydroimidazo[1,5-c]imidazol-7-ones and imidazoles
;
_journal_name_full               Chem.Commun.
_journal_page_first              6601
_journal_paper_doi               10.1039/c2cc32760k
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C31 H30 Cl3 N3 O5'
_chemical_formula_weight         630.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 95.619(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   65.41(2)
_cell_length_b                   11.699(4)
_cell_length_c                   25.152(8)
_cell_measurement_reflns_used    6450
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.81
_cell_measurement_theta_min      2.38
_cell_volume                     19155(11)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker Kappa Apex 2'
_diffrn_measurement_method       FastFourierTransform
_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  0.0469
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       70
_diffrn_reflns_limit_h_min       -69
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34111
_diffrn_reflns_theta_full        22.41
_diffrn_reflns_theta_max         22.41
_diffrn_reflns_theta_min         0.63
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.984
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1141
_refine_ls_number_reflns         11978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1195
_refine_ls_R_factor_gt           0.0742
_refine_ls_shift/su_max          1.256
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2811
_reflns_number_gt                7118
_reflns_number_total             11978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32760k.txt
_cod_data_source_block           YS37_0m
_cod_original_cell_volume        19154(11)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7107943