Highly regioselective nucleophilic/cycloaddition reactions of N-arylamino 1,3-diazabuta-1,3-dienes with α-nitrosostyrenes: synthesis of functionalised imidazoles and imidazole oxides
Sharma, Arun K.; Hundal, Geeta; Obrai, Sangeeta; Mahajan, Mohinder P.; Journal of the Chemical Society, Perkin Transactions 1  (1999) 615–; doi:10.1039/a808574i

data_7212978
_publ_section_title
;
 Highly regioselective nucleophilic/cycloaddition reactions of N-arylamino
 1,3-diazabuta-1,3-dienes with \a-nitrosostyrenes: synthesis of
 functionalised imidazoles and imidazole oxides
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              615
_journal_paper_doi               10.1039/a808574i
_journal_year                    1999
_chemical_formula_sum            'C32 H30 N4 O'
_chemical_formula_weight         486.60
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 95.20(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.056(2)
_cell_length_b                   20.437(5)
_cell_length_c                   21.335(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     2629.7(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            1853
_diffrn_reflns_theta_max         17.50
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.103
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         1491
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_obs          0.0512
_refine_ls_shift/esd_max         -0.092
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+1.6943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1792
_refine_ls_wR_factor_obs         0.1488
_reflns_number_observed          1192
_reflns_number_total             1600
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808574isup1.cif
_cod_data_source_block           imidazole3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+1.6943P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+1.6943P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7212978