The need for a water-soluble vic-dioxime as an analytical reagent for nickel(II) and palladium(II) ions has long been evident. Thus, a preparation and investigation of some alicyclic vic-dioximes as possible watersoluble reagents was undertaken. Secondly, in order to obtain a better understanding of the structure of the inner-complex compounds that the vic-dioximes form with certain ions, an infrared spectroscopic study of the nature of the hydrogen bonds in these inner-complex compounds was made.