Vanadium-induced formation of thiadiazole and thiazoline compounds. Mononuclear and dinuclear oxovanadium(v) complexes with open-chain and cyclized thiosemicarbazone ligands
Rubčić, Mirta; Milić, Dalibor; Horvat, Gordan; Đilović, Ivica; Galić, Nives; Tomišić, Vladislav; Cindrić, Marina; Dalton Transactions  (2009) 9914–9923; doi:10.1039/b913653c

data_7002747
_publ_section_title
;
 Vanadium-induced formation of thiadiazole and thiazoline compounds.
 Mononuclear and dinuclear oxovanadium(v) complexes with open-chain and
 cyclized thiosemicarbazone ligands
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              9914
_journal_page_last               9923
_journal_paper_doi               10.1039/b913653c
_journal_year                    2009
_chemical_formula_moiety         'C32 H30 N6 O7 S2 V2, 0.5(C2 H6 O)'
_chemical_formula_sum            'C33 H33 N6 O7.5 S2 V2'
_chemical_formula_weight         799.65
_chemical_name_systematic
'diethoxo-\m-oxo-dioxobis[2-(5-phenylamino-[1,3,4]thiadiazol-2-yl)-phenolato]divanadium(V) ethanol hemisolvate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.441(3)
_cell_angle_beta                 84.791(3)
_cell_angle_gamma                62.827(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6448(4)
_cell_length_b                   12.1611(4)
_cell_length_c                   14.4691(5)
_cell_measurement_reflns_used    8271
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      28.3658
_cell_measurement_theta_min      3.7802
_cell_volume                     1745.41(12)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(1)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15723
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.409
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         7536
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0913
_reflns_number_gt                5391
_reflns_number_total             7536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b913653c.txt
_cod_data_source_block           3b_x_0.5_EtOH
_cod_original_formula_sum        'C33 H33 N6 O7.50 S2 V2'
_cod_database_code               7002747