Department of Chemistry, University of Calicut, Kerala-619 635 Manuscript received 24 September 1987, accepted 13 January 1988 COUPLING of diazonium salts with \(\beta\)-ketonitriles have been studied extensively because the products have found use as yellow dyes and pigments1-3. Transition metal complexes of these azo dyes are reported to have excellent fastness properties1. However, there appears no systematic investigation on the structural aspects of these azo compounds and their metal complexes. The present communication reports the syntheses and characterisation of 2-(phenylazo)- 2- cyanoethylethanoate (phenylazoethylcyanoacetate) and its copper(II), nickel(II) and cobalt(II) complexes.