The formation of a sequence of insoluble Pd(l1) compounds was demonstrated by heterometric titration. The species Pd, AADO (AADO = acetylacetone dioxime), Pd, AADO and PdAADO were detected and a further compound, Pd(AADO), was synthesized. The elemental analysis of Pd, AADO and Pd(AADOH), is reported. The visible spectrum of Pd/AADo mixtures in solution (at pH = 11) is reported and assigned. IR spectra of Pd, AADO, Pd(AADO), and AADO are recorded and compared, and the structure of the compounds is deduced.