The reaction of aqueous solutions of SnCl4[dot]5H2O and K4Fe(CN)6 in a 2/1 Sn/Fe atomic ratio results in a hydrogelled polymeric material, characterized by bridging cyanides between the central metals of the adducts. Materials of this type have previously been noted uponreaction of PdCl42- with cyanometalates in aqueous solution and have been referred to as cyanogels. Dehydration of Sn/Fe cyanogels results in xerogels that maintain the initial polymeric structure of the hydrogel. Thermal processing of such gels under an air atmosphere at 900[degree]C produces a solid homogeneous mixture of microcrystalline SnO2 and Fe2O3.