Universität zu Köln

Heinrich, Frank, Kessler, Michael T., Dohmen, Stephan, Singh, Mrityunjay, Prechtl, Martin H. G. ORCID: 0000-0003-2155-8006 and Mathur, Sanjay (2012). Molecular Palladium Precursors for Pd0 Nanoparticle Preparation by Microwave Irradiation: Synthesis, Structural Characterization and Catalytic Activity. Eur. J. Inorg. Chem. (36). S. 6027 - 6034. WEINHEIM: WILEY-V C H VERLAG GMBH. ISSN 1099-0682

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Abstract

Two new palladium complexes [Pd(MEA)2Cl2] (1) and [Pd(MEA)2Br2] (2) [MEA = (2-methoxyethyl)amine] were synthesized by the reaction of 2 equiv. of MEA with PdCl2 or [(cod)PdBr2] (cod = cycloocta-1,5-diene), respectively. Single-crystal X-ray diffraction analysis of 1 and 2 revealed the formation of square-planar trans complexes with palladium coordinated by chloride/bromide ions and N-atoms of MEA bonded in a monodentate fashion. Given their molecular form and solubility, 1 and 2 act as intractable precursors to Pd nanoparticles by microwave-assisted synthesis. The influence of the reaction temperature, irradiation time and surfactant (PVP) concentration on the size (540 nm) of the resulting particles was studied by DLS (hydrodynamic diameter) and TEM analyses (particle size). The growth mechanism of the nanoparticles depended on the type of halide ligand. Powder X-ray diffractometry confirmed the formation of elemental Pd particles that were embedded in carbonized wood to examine their potential as a catalyst. The catalytic activity of these nanoscale particles was evaluated in carboncarbon cross-coupling reactions by using Heck, Suzuki and Sonogashira reactions as benchmark models. The investigations included recycling experiments that resulted in total turnover numbers of 4321 (Heck), 6173 (Sonogashira) and 8223 (Suzuki).

Item Type:	Journal Article
Creators:	Creators Email ORCID ORCID Put Code Heinrich, Frank UNSPECIFIED UNSPECIFIED UNSPECIFIED Kessler, Michael T. UNSPECIFIED UNSPECIFIED UNSPECIFIED Dohmen, Stephan UNSPECIFIED UNSPECIFIED UNSPECIFIED Singh, Mrityunjay UNSPECIFIED UNSPECIFIED UNSPECIFIED Prechtl, Martin H. G. UNSPECIFIED orcid.org/0000-0003-2155-8006 UNSPECIFIED Mathur, Sanjay UNSPECIFIED UNSPECIFIED UNSPECIFIED
URN:	urn:nbn:de:hbz:38-477174
DOI:	10.1002/ejic.201200380
Journal or Publication Title:	Eur. J. Inorg. Chem.
Number:	36
Page Range:	S. 6027 - 6034
Date:	2012
Publisher:	WILEY-V C H VERLAG GMBH
Place of Publication:	WEINHEIM
ISSN:	1099-0682
Language:	English
Faculty:	Unspecified
Divisions:	Unspecified
Subjects:	no entry
Uncontrolled Keywords:	Keywords Language LIGAND-FREE PALLADIUM; COUPLING REACTIONS; IONIC LIQUIDS; NOBLE-METAL; SUZUKI; HECK; NANOSTRUCTURES; MORPHOLOGY; NANOWIRES; COMPLEXES Multiple languages Chemistry, Inorganic & Nuclear Multiple languages
URI:	http://kups.ub.uni-koeln.de/id/eprint/47717