Authors:A. Petrović, D. Petrović, V. Leovac, and M. Budimir
The paper describes the results of differential thermal analysis of the octahedral Fe(III) complexes of the general formula [Fe(HLn)2]Cl and Fe(HL3)L3, as well as of the corresponding ligands H2Ln (H2Ln — tridentate salicylaldehyde semi thiosemi- and S-methylisothiosemi-carabazones with n=1, 2 and 3 respectively). The decomposition of the complexes involving sulphur-containing ligands (H2L2 and H2L3) starts with sulphur elimination. In case of the complexes [Fe(HL2)]Cl and [Fe(HL3)]Cl sulphur evolves independently, whereas with Fe(HL3)L3 it is eliminated within the SCH3 group. In the former case, sulphur elimination takes place at the same temperature for both complexes. The change in the coordination mode, being a consequence of the replacement of O by S, has no essential effect on thermal stability of the coordination polyhedron. The complexes involving ONN coordination, realized with the H2L3 ligand, exhibit a comparatively highest thermal stability of the coordination polyhedron.
Authors:Ž. Jaćimović, V. Leovac, G. Giester, Z. Tomić, and Katalin Szécsényi
Molecular and crystal structure of diaqua-sulphato(pyridoxal semicarbazone-ONO)iron(II) and dichloroaqua(pyridoxal semicarbazone-ONO)iron(III)
complexes with tridentate ONO pyridoxal semicarbazone ligand, PLSC, of formula [FeII(PLSC)(H2O)2SO4] and [FeIII(PLSC)(H2O)Cl2]Cl is reported. Thermal decomposition of the compounds was followed in argon and air gas carriers. The dequation mechanism
is discussed in the view of the crystal structure, emphasizing the complexity of the related parameters and processes.
Authors:V. Leovac, R. Petković, A. Kovács, G. Pokol, and Katalin Szécsényi
Factors determining the complex formation reaction of copper(II), nickel(II) and cobalt(II) chloride and copper(II) bromide
with 3,5-dimethyl-1-(hydroxymethyl)-pyrazole (HL) has been studied. Depending on experimental conditions, complexes with different
composition were obtained: [CuCl2(dmp)]2 (I), [CuCl2(dmp)2]2 (II), [CoCl2(dmp)2] (III) (dmp=3,5-dimethylpyrazole), [CuBr(L)]2 (IV), [CoCl(L)(EtOH)]4 (V) and [NiCl(L)(EtOH)]4 (VI). The compounds were characterized by FTIR spectroscopy, solution conductivity and magnetic measurements. The crystal structure
of [CoCl(L)(EtOH)]4 has been determined by single crystal X-ray diffraction. The thermal decomposition of the compounds was studied and found
to be continuous for all of the compounds. The desolvation mechanism of [MCl(L)(EtOH)]4 (M=Co(II), Ni(II)) is explained on the basis of the route of complex formation of CoCl2 with HL.
Authors:D. Petrovic, A. Petrovic, V. Leovac, and S. Lukic
The thermal decomposition of copper(II) complexes with salicylaldehyde S-methylthiosemicarbazone of general formula Cu(HL)X·nH2O (X=Py+NO3, NCS, 0.5SO4) and [Cu(L)NH3]·H2O was investigated in air atmosphere in the interval from room temperature to 1000°C. Decomposition of the complexes occurred
in several successive endothermic and exothermic processes, and the residue was in all cases CuO.
Authors:K. Mészáros Szécsényi, V. Leovac, Ž. Jaćimović, V. Češljević, A. Kovács, G. Pokol, and S. Gál
We report the synthesis and the characterization (elemental analysis, FT-IR spectroscopy, thermal methods and molar conductivity
measurements) of the mixed complexes of zinc with acetate and 3-amino-5-methylpyrazole, HL1, [Zn(OAc)2(HL1)2], or 3-amino-5-phenylpyrazole, HL2 [Zn(OAc)2(HL2)2], or 4-acetyl-3-amino-5-methylpyrazole, HL3, [Zn(OAc)(L3)(HL3)]2, with isothiocyanate and HL2 [Zn(SCN)2(HL2)2], or HL3 [Zn(SCN)2(HL3)2], and with nitrate, isothiocyanate and 3,5-dimethyl-1-carboxamidinepyrazole, HL4 [Zn(NO3)(NCS)(HL4)2].
The thermal decomposition of the complexes is generally continuous resulting zinc oxide as end product,except [Zn(OAc)(L3)(HL3)]2 in which case a well-defined intermediate was observed between 570–620 K. On the basis of the IR spectra and elemental analysis
data of the intermediate a decomposition scheme is proposed.