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Transitionmetal complexes with pyrazole-based ligands

Part 21. Thermal decomposition of copper and cobalt halide complexes with 3,5-dimethyl-1-thiocarboxamidepyrazole

Journal of Thermal Analysis and Calorimetry
Authors:
K. Mészáros Szécsényi
,
V. Leovac
,
A. Kovács
,
G. Pokol
, and
Ž. Jaćimović

Abstract  

The thermal decomposition of Cu2L2Cl4, Cu2L2Cl2, Cu2L2Br2 and Co2L2Cl4 complexes (L=3,5-dimethyl-1-thiocarboxamidepyrazole) is described. The influence of the central ion to ligand mole ratio on the course of complex formation is examined in reaction of L with copper(II) chloride. In Cu(II):L mole ratio of 1:1, in methanolic solution the reaction yields to yellow-green Cu2L2Cl4 crystals. In the filtrate a thermodynamically more stable orange Cu2L2Cl2 copper(I) complex is forming. With a Cu(II):L mole ratio of 1:2 only the latter compound is obtained. The composition and the structure of the compounds have been determined on the basis of customary methods. On the basis of FTIR spectrum of the intermediate which is forming during the thermal decomposition of Cu2L2Cl2 a decomposition mechanism is proposed.

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Abstract  

Manganese(II) chloride complexes with 3,4- and 3,5-lutidine have been prepared. The crystal symmetry and cell dimensions have been calculated on the basis of powder diffraction data. The compounds were characterised also by FT-IR spectrometry. The thermal decomposition of the complexes has been studied by thermogravimetry and DSC. By plotting densities vs. molar mass, the diagram obtained has correspondence to similar observations in other solid metal-lutidine complex systems.

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Abstract  

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, HL 1, [Zn(OAc)2(HL1)2], or 3-amino-5-phenylpyrazole, HL 2 [Zn(OAc)2(HL2)2], or 4-acetyl-3-amino-5-methylpyrazole, HL 3, [Zn(OAc)(L3)(HL3)]2, with isothiocyanate and HL 2 [Zn(SCN)2(HL2)2], or HL 3 [Zn(SCN)2(HL3)2], and with nitrate, isothiocyanate and 3,5-dimethyl-1-carboxamidinepyrazole, HL 4 [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.

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Abstract  

The synthesis of copper(II) chloride complexes with 3,5-dimethylpyrazole, 1-carboxamidine-3,5-dimethylpyrazole, 5-amino-4-carboxamide-1-phenylpyrazole and 4-acetyl-3-amino-5-methylpyrazole is described. The compounds are characterized by elemental analysis, FT-IR spectroscopy, thermal methods, magnetic moment and molar conductivity measurements. Thermal decomposition of the dichloro-(3,5-dimethylpyrazole)-copper(II) complex results in an unstable intermediate with a stochiometric composition. The decomposition of the other compounds is continuous.

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Abstract  

Complexes represented by the general formula [MCl2L2] (M(II)=Zn, Mn, Co) and complexes of [Cu3Cl6L4] and CuSO4L24H2O, CoSO4L23H2O, [ZnSO4L3] where L stands for 3-amino-5-methylpyrazole were prepared. The complexes were characterized by elemental analysis, FT-IR spectroscopy, thermal (TG, DTG, DSC and EGA) methods and molar conductivity measurements. Except for the Zn-complexes, the magnetic susceptibilities were also determined. Thermal decomposition of the sulphato complexes of copper(II) and cobalt(II) and the chloro complexes of cobalt(II) and manganese(II) resulted in well-defined intermediates. On the basis of the IR spectra and elemental analysis data of the intermediates a decomposition scheme is proposed.

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Journal of Radioanalytical and Nuclear Chemistry
Authors:
Z. Németh
,
Z. Homonnay
,
F. Árva
,
Z. Klencsár
,
E. Kuzmann
,
J. Hakl
,
K. Vad
,
S. Mészáros
,
K. Kellner
,
G. Gritzner
, and
A. Vértes

Abstract  

In this paper we present 57Co emission Mössbauer and AC magnetic susceptibility studies of La0.8Sr0.2CoO3-δ perovskite. The observed coexistence of paramagnetic and magnetic subspectra in the 57Co emission Mössbauer spectra, as well as the difference of their isomer shifts support the existence of electronic phase separation in this perovskite, in good agreement with the double exchange based cluster model.

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