Evidence of Desulfurization in the Oxidative Cyclization of Thiosemicarbazones. Conversion to 1,3,4-Oxadiazole Derivatives
Patricia Gómez-Saiz; Javier García-Tojal; Miguel A. Maestro; Francisco J. Arnaiz; Teófilo Rojo; Inorganic Chemistry 41 (2002) 1345–1347; doi:10.1021/ic015625s

data_4317755
_publ_section_title
;
 Evidence of Desulfurization in the Oxidative Cyclization of
 Thiosemicarbazones. Conversion to 1,3,4-Oxadiazole Derivatives
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1345
_journal_page_last               1347
_journal_paper_doi               10.1021/ic015625s
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C8 H14 N4 O4'
_chemical_formula_sum            'C8 H14 N4 O4'
_chemical_formula_weight         230.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.302(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.415(1)
_cell_length_b                   7.1097(8)
_cell_length_c                   12.763(1)
_cell_measurement_temperature    298(2)
_cell_volume                     1124.68(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6674
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        1.8
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9625
_exptl_absorpt_correction_T_min  0.9471
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+0.0400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                1812
_reflns_number_total             2280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015625s_3.cif
_cod_data_source_block           comp3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1124.7(2)
_cod_database_code               4317755