In this paper, we present examples of the use of photochemical metal organic deposition to form nanostructured metal oxide films. In the first example, we use two reactions with very different reaction rates to control the nanostructuring, utilizing tantalum (V) tetraethoxide acetylacetonate (as a thermally reactive source of tantalum oxide) and manganese (II) 2-ethylhexanoate (as a photochemically reactive source of manganese oxide). We prepare homogeneous precursor films of tantalum (V) tetraethoxide acetylacetonate and manganese (II) 2-ethylhexanoate and in the dark allow the tantalum complex to react forming tantalum oxide regions. The film is then exposed and the manganese complex is converted to a matrix surrounding the tantalum regions. The resultant structures are characterized by electron microscopy, energy dispersive X-ray spectroscopy and Auger spectroscopy. In the second example, we use two immiscible precursors, zirconium (IV) 2-ethylhexanoate and yttrium nitrate hexahydrate to form nanostructured precursor films. The nanostructuring of these films is apparent from SEM studies. Exposure of these films results in the formation of nanostructured films consisting of a zirconium oxide matrix with encapsulated yttrium oxide.