Thermal Behavior and Spectroscopic Study of Neutral and Cationic Mononuclear Cyclopalladated Compounds

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2003-11-25

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The reactions of the precursor [Pd(N,C-dmba)(MeCN)2](NO 3) (1) (dmba = N,N-dimethylbenzylamine), with the proligands 3,5-dimethylpyrazole (Hdmpz), 2-quinolinethiol (qnSH) and 1,1′- bis(diphenylphosphine)ferrocene (dppf) afforded the compounds [Pd(N,C-dmba)(Hdmpz)(ONO2)]0.5CH2Cl2 (2), [Pd(N,C-dmba)(qnSH)(ONO2)] 0.5CH2Cl2 (3) and [Pd(N,C-dmba)(dppf)](NO3) (4), respectively. The mononuclear species 2,3 and 4 were characterized by elemental analysis, infrared spectroscopy, NMR and thermogravimetric analysis. The IR spectra show bands which are consistent with terminal monodentate nitrate group for 2-3 and ionic nitrate for 4. The 1H and 13C NMR data confirm that coordination of the organic ligands has occurred and the 31P{1H} NMR data for 4 clearly evidences the occurrence in solution of three cyclopalladated species with the dppf acting as a bridging ligand in two cases and as a chelate in one. The thermal behavior of compounds 1-4 suggests that complex 2 is the most stable. The X-ray diffractometry results show the formation of PdO from 1 and 2, Pd2OSO4 from 3, and of a mixture of PdO and Fe 2(PO4)3 from 4, as final decomposition products.

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Cyclopalladated species, IR and NMR spectroscopy, Thermogravimetric analysis, 1,1' bis(diphenylphosphine)ferrocene, 3,5 dimethylpyrazole, cation, ferrocene derivative, ligand, nitric acid derivative, palladium complex, pyrazole derivative, quinolinethiol, thiol derivative, unclassified drug, carbon nuclear magnetic resonance, chemical analysis, chemical structure, infrared spectroscopy, nuclear magnetic resonance, precursor, proton nuclear magnetic resonance, reaction analysis, spectroscopy, structure analysis, thermal analysis, thermogravimetry, X ray diffraction

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Journal of the Brazilian Chemical Society, v. 14, n. 5, p. 764-770, 2003.