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Thermal behavior and spectroscopic study of neutral and cationic mononuclear cyclopalladated compounds

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Author(s): Ananias Sandra R. | Mauro Antonio E.

Journal: Journal of the Brazilian Chemical Society
ISSN 0103-5053

Volume: 14;
Issue: 5;
Start page: 764;
Date: 2003;
Original page

Keywords: cyclopalladated species | IR and NMR spectroscopy | thermogravimetric analysis

ABSTRACT
The reactions of the precursor [Pd(N,C-dmba)(MeCN)2](NO3) (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)]0.5CH2 Cl2 (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 Fe2(PO4)3 from 4, as final decomposition products.
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