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.
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