Trinuclear Palladium II Acetate

Submitted by JOHN F. BERRY, F. ALBERT COTTON, SERGEY IBRAGIMOV, and CARLOS A. MURILLO Checked by DAREN J. TIMMONS and KYLE A. FRICKE  

One of the most versatile starting materials for the preparation of palladium(n) complexes is the trinuclear Pd3(OAc)g, which has the unusual but well-known D31, structure in which six acetate groups bridge three nearly square planar metal atoms.Recentiy, several syntheses have been reported for this compound, 

Laboratory for Molecular Structure and Bonding, Department of Chemistry, Texas A M University, College Station, TX 77842. 

There are various reports suggesting the hypothesis that various [Pd(OAc)2] aggregates also form in solution because the H NMR spectra usually showed a complex pattern in the acetate region where only a single peak would be expected from the highly symmetrical Dsh structure. Recently, we found that a complex pattern in the NMR spectrum in CeDe and CDCI3 may be attributed to hydrolysis or to the formation of a nitrite derivative that is formed following some of the recently reported preparations for Pd3(OAc)6.  

Here we report a reproducible and dependable two-step procedure for the synthesis of trinuclear Pd3(OAc)6 from PdCl2. The method proceeds in high yield to produce a crystalline material that is soluble in various organic solvents and that gives a H NMR spectrum with only one acetate resonance. 

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