Issue 10, 2002

Structural characterisation of solution species implicated in the palladium-catalysed Heck reaction by Pd K-edge X-ray absorption spectroscopy: palladium acetate as a catalyst precursor

Abstract

Energy dispersive EXAFS (EDE), Quick EXAFS (QEXAFS), 13C NMR and X-ray crystallography have been used to probe the co-ordination sphere of palladium in the course of the phosphine free Heck reaction. [Pd2I6][NBu3H]2 has been isolated from the precatalytic solution and its crystal structure determined. EDE and QEXAFS spectra of the complexes Pd(OAc)2, Pd(PPh3)4 and [Pd2I6][NEt3H]2 illustrated the value of the technique in structure elucidation. EXAFS of the precatalytic solution detects [Pd2I6]2− and no co-ordinated carbon. EXAFS of the catalytic solution shows a first co-ordination sphere of 2 carbon atoms and a second of 2–2.5 iodines. A scheme involving an equilibrium between the oxidative addition product and the olefin co-ordination species, has been proposed to explain these results.

Graphical abstract: Structural characterisation of solution species implicated in the palladium-catalysed Heck reaction by Pd K-edge X-ray absorption spectroscopy: palladium acetate as a catalyst precursor

Supplementary files

Article information

Article type
Paper
Submitted
17 Jan 2002
Accepted
12 Mar 2002
First published
17 Apr 2002

J. Chem. Soc., Dalton Trans., 2002, 2207-2212

Structural characterisation of solution species implicated in the palladium-catalysed Heck reaction by Pd K-edge X-ray absorption spectroscopy: palladium acetate as a catalyst precursor

J. Evans, L. O'Neill, V. L. Kambhampati, G. Rayner, S. Turin, A. Genge, A. J. Dent and T. Neisius, J. Chem. Soc., Dalton Trans., 2002, 2207 DOI: 10.1039/B200617K

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