Oxovanadium(V) and Cobalt(III) Complexes of Dithiocarbazate-Based Schiff Base Ligands: Formation of a Thiadiazole Ring by Vanadium-Induced Cyclization of the Coordinated Ligand
Subodh Kanti Dutta; Satyabrata Samanta; Dipesh Ghosh; Ray J. Butcher; Muktimoy Chaudhury; Inorganic Chemistry 41 (2002) 5555–5560; doi:10.1021/ic0200895

data_4318662
_publ_section_title
;
 Oxovanadium(V) and Cobalt(III) Complexes of Dithiocarbazate-Based Schiff
 Base Ligands: Formation of a Thiadiazole Ring by Vanadium-Induced
 Cyclization of the Coordinated Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5555
_journal_page_last               5560
_journal_paper_doi               10.1021/ic0200895
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C18 H19 Co N4 O3 S4'
_chemical_formula_weight         526.54
_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                78.122(6)
_cell_angle_beta                 73.888(6)
_cell_angle_gamma                78.255(6)
_cell_formula_units_Z            4
_cell_length_a                   12.0842(8)
_cell_length_b                   13.5251(9)
_cell_length_c                   14.1960(10)
_cell_measurement_reflns_used    70
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      2.00
_cell_volume                     2154.7(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w 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  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10298
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.34
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.213
_exptl_absorpt_correction_T_max  0.8091
_exptl_absorpt_correction_T_min  0.6656
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.88
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9835
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.238
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.4174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                7615
_reflns_number_total             9835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0200895_1.cif
_cod_data_source_block           mc9
_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               4318662