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_4317753
_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         'C16 H18 Cu2 N10 O6 S2'
_chemical_formula_sum            'C16 H18 Cu2 N10 O6 S2'
_chemical_formula_weight         637.60
_chemical_name_systematic
; 
 ? 
;
_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                72.734(1)
_cell_angle_beta                 86.646(1)
_cell_angle_gamma                70.362(1)
_cell_formula_units_Z            1
_cell_length_a                   7.5259(5)
_cell_length_b                   8.7096(6)
_cell_length_c                   9.9215(6)
_cell_measurement_temperature    298(2)
_cell_volume                     584.29(7)
_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 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0204
_diffrn_reflns_av_sigmaI/netI    0.0179
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4140
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    2.056
_exptl_absorpt_correction_T_max  0.4581
_exptl_absorpt_correction_T_min  0.4263
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.812
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.832
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0727P)^2^+0.1717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                2612
_reflns_number_total             2820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic015625s_1.cif
_cod_data_source_block           comp1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4317753