New Facile Tandem Route to Oxo- and Thioxo[1,2,4]triazolo[1,5-a]pyridinium Salts
Roberta Palkó; Zsuzsanna Riedl; Orsolya Egyed; László Fábián; György Hajós; Journal of Organic Chemistry 71 (2006) 7805–7812; doi:10.1021/jo061361l

data_4021995
_publ_section_title
;
 New Facile Tandem Route to Oxo- and
 Thioxo[1,2,4]triazolo[1,5-a]pyridinium Salts
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7805
_journal_page_last               7812
_journal_paper_doi               10.1021/jo061361l
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C36 H31 N5 O7'
_chemical_formula_sum            'C36 H31 N5 O7'
_chemical_formula_weight         645.66
_chemical_name_systematic
;
  (E)-5-((E)-3-(1,4-bis(4-methoxyphenyl)-5-oxo-4,5-dihydro-1H-1,2,4-triazol-
  3-yl)allylidene)-1,3-bis(4-methoxyphenyl)imidazolidine-2,4-dione
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                72.45(1)
_cell_angle_beta                 70.51(1)
_cell_angle_gamma                70.07(1)
_cell_formula_units_Z            2
_cell_length_a                   10.517(1)
_cell_length_b                   12.589(1)
_cell_length_c                   13.854(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.74
_cell_measurement_theta_min      29.99
_cell_volume                     1588.7(3)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express'
_computing_data_reduction        'XCAD4 (Harms 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'CU k\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14065
_diffrn_reflns_theta_full        75.57
_diffrn_reflns_theta_max         75.57
_diffrn_reflns_theta_min         3.46
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.9046
_exptl_absorpt_correction_T_min  0.6944
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'DATCOR (Riebenspies, 1989)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         6603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1055P)^2^+0.1676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1802
_reflns_number_gt                4966
_reflns_number_total             6603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061361lsi20060707_121014.cif
_cod_database_code               4021995