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Mono- and dinuclear palladium(II) compounds containing N,S donor ligands

Synthesis, characterization and thermal behavior

Journal of Thermal Analysis and Calorimetry
Authors: A. Moro, A. Mauro, S. Ananias, A. Stevanato, and A. Legendre

Abstract  

Synthesis, spectroscopic characterization and thermal analysis of the compounds [Pd2(dmba)2(μ-NCO)(μ-2-qnS)] (1), [Pd2(dmba)2(μ-NCO)(μ-8-qnS)] (2), [Pd(2-qnS)2] (3) and [Pd(8-qnS)2] (4) (dmba=N,N-dimethylbenzylamine; 2-qnS=2-quinolinethiolate; 8-qnS=8-quinolinethiolate) are described. The thermal decomposition of these compounds occurs in four consecutive steps and the final decomposition products were identified as Pd(0) by X-ray powder diffraction. The thermal stability order of the complexes is 4>3>1>2.

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Abstract  

Synthesis, characterization and thermal behavior of four compounds that have the general formula [Cu{Pd(CN)4}(L)x]n, in which en=1,2-diaminoethane and pn=1,3-diaminopropane (L=en, x=1 (I); L=pn, x=1 (II); L=en, x=2 (III); L=pn, x=2 (IV)) were described in this work. The complexes were studied by elemental analysis, infrared spectroscopy (IR), differential thermal analysis (DTA) and thermogravimetry (TG) and the residues of the thermal decomposition were characterized by X-ray powder diffraction and found as a mixture of CuO and PdO. The stoichiometry of the compounds was established via thermogravimetric and elemental analyses and their structures were proposed as coordination polymers based on their infrared spectra. The following thermal stability sequence was found: IV<I=II<III.

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Abstract  

This work describes the synthesis, IR and UV-Vis spectroscopic characterization as well the thermal behavior of the [NiCl2(HIPz)4]⋅C3H6O (1), [Ni(H2O)2(HIPz)4](NO3)2 (2), [Ni(NCS)2(HIPz)4] (3) and [Ni(N3)2(HIPz)4] (4) (HIPz=4-iodopyrazole) pyrazolyl complexes. TG experiments reveal that the compounds 14 undergo thermal decomposition in three or four mass loss steps yielding NiO as final residue, which was identified by X-ray powder diffraction.

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Mono and dinuclear Pd(II) complexes with pyrazole and imidazole-type ligands

Synthesis, characterization and thermal behaviour

Journal of Thermal Analysis and Calorimetry
Authors: V. Lucca Neto, A. Mauro, A. Netto, A. Moro, and V. Nogueira

Abstract  

The cyanate-bridged cyclopalladated compound [Pd(C2,N-dmba)(μ-NCO)]2 (dmba=N,N-dimethylbenzylamine) reacts in acetone with pyrazole (pz), 3,5-dimethylpyrazole (dmpz), imidazole (imz) and 2-methylimidazole (mimz) to give [Pd2(C2,N-dmba)2(μ-NCO)(μ-pz)] (1), [Pd2(C2,N-dmba)2(μ-NCO)(μ-dmpz)] (2), [Pd(C2,N-dmba)(NCO)(imz)] (3) and [Pd(C2,N-dmba)(NCO)(mimz)] (4), respectively. The compounds were characterized by elemental analysis, IR spectroscopy and TG. The thermal decomposition of the compounds occurs in three consecutive steps and the final decomposition products were identified as Pd(0) by X-ray powder diffraction. The thermal stability order of the complexes is 2>3>1>4.

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Thermal study of cyclopalladated complexes of the type [Pd2(dmba)2X2(bpe)]

(X=NO- 3, Cl-, N- 3, NCO-, NCS-; bpe=trans-1,2-bis(4-pyridyl)ethylene)

Journal of Thermal Analysis and Calorimetry
Authors: E. T. de Almeida, A. M. Santana, A. V. G. Netto, Claudia Torres, and A. E. Mauro

The synthesis, characterization and thermal analysis of the novel cyclometallated compounds [Pd2(dmba)2Cl2(μ-bpe)] (1), [Pd2(dmba)2(N3)2(μ-bpe)] (2), [Pd2(dmba)2(NCO)2(μ-bpe)] (3), [Pd2(dmba)2(SCN)2(μ-bpe)] (4), [Pd2(dmba)2(NO3)2(μ-bpe)] (5) (bpe=trans-1,2-bis(4-pyridyl)ethylene; dmba=N,N-dimethylbenzylamine) are described. The thermal stability of [Pd2(dmba)2X2(μ-bpe)] complexes varies in the sequence 1>4>3>2>5. The final residues of the thermal decompositions were characterized as metallic palladium by X-ray powder diffraction.

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Abstract  

This work describes the synthesis, IR and 13C CPMAS NMR spectroscopic as well the thermal characterization of the new dicarboxylate complexes [Pd2(ox)2(4,4′-bipy)]n (1), [Pd2(ox)2(bpe)]n (2) and [Pd2(ox)2(pz)]n (3) {ox = oxalate, bipy = 4,4′-bipyridine, bpe = 1,2-bis(4-pyridyl)ethane, pz = pyrazine}. TG experiments reveal that compounds 13 undergo thermal decomposition in three steps. Metal palladium was the final product of the thermal decompositions, which was identified by X-ray powder diffraction.

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Abstract  

The synthesis and thermal behavior of the new [Pd(fum)(bipy)]n·2nH2O (1), [Pd(fum)(bpe)]n·nH2O (2) and [Pd(fum)(pz)]n·3nH2O (3) {bipy = 4,4′-bipyridine, bpe = 1,2-bis(4-pyridyl)ethene and pz = pyrazine} fumarate complexes are described in this work as well their characterization by IR and 13C CPMAS NMR spectroscopies. TG curves showed that the compounds released organic ligands and lattice water molecules in the temperature range of 46–491 °C. In all the cases, metallic palladium was identified as the final residue.

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Journal of Thermal Analysis and Calorimetry
Authors: V. Sargentelli, A. Mauro, A. de Godoy Netto, M. Mattioli, V. Nogueira, and V. De Lucca Neto

Abstract  

Pseudohalide complexes of copper(II) with aliphatic bidentate amines, [Cu(N3)2(N,N-diEten)]2 1, [Cu(NCO)2(N,N-diEten)]2 2, [Cu(NCO)2(N,N-diMeen)]2 3, [Cu(N3)(NCS)(N,N'-diMeen)]2 4 and [Cu(N3)(NCO)(N,N-diMeen)]2 5 (N,N-diEten=N,N-diethylethylenediamine; N,N-diMeen=N,N- dimethyl-ethylenediamine and N,N'-diMeen = N,N'-dimethylethylenediamine), were prepared, characterized and their thermal behavior was investigated by TG curves. According to thermal analysis and X-ray diffraction patterns all compounds decomposed giving copper(II) oxide as final product. The mechanisms of decomposition were proposed and an order of thermal stability was established.

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