The reaction of dialkyl alkylphosphonates with trivalent metal chlorides has recently been reported (1,2). The typical products of these reactions is a solid which is insoluble in most organic solvents and water. A monomeric structure was postulated for the iron phosphonates(1), while polynuclear structure was proposed for titanium, vanadium, and chromium phosphonates(2). Infrared(1) and Mossbauer-effect(3) studies were unable to differentiate between the monomeric or polynuclear structure for the iron phosphonates, In an attempt to further characterize the iron phosphonates, an x-ray diffration study was undertaken. The results of these studies are reported herein.