As part of an ongoing research program to synthesize novel pillared layered materials, nickel and cobalt hydroxyacetates were inserted between the layers of amine intercalates of alpha-zirconium phosphate. The structure of the resultant nickel composite, derived from x-ray powder data, was found to consist of a three-tiered layer of nickel atoms bridged by hydroxo and acetato groups. Heating to 420 degrees C converted the hydroxyacetate layers to oxide and imparted ordered magnetic domains to the composite. The phosphate layers appear to act as a template directing the growth of the inserted layers in this class of composite materials.