Acetate groups of anhydrous nickel(II) acetate have been substituted with some higher carboxylic acids and hydroxycarboxylic acids in toluene under reflux and the products Ni(OOCR)(OOCR'), Ni(OOCR)(OOCR ") and Ni(OOCR)(OOCR''') [where R=C13H27, C17H35 or C21H43 and R'=C6H4OH, R " =C6H5CH(OH) and R'''=(C6H5)(2)C(OH)] obtained have been characterized by elemental analyses, electronic and IR spectra and conductivity measurements. An octahedral environment around nickel(II) ion is suggested and the molecular weight determinations confirm the dinuclear nature of these complexes.