A new class of supermicroporous mixed oxides, with pore sizes in the 10-20 .ANG. range has been prepared utilizing basic metal acetates. The reactions are carried out in non-aqueous solvent media to which an excess of amine is added. Hydrolysis of the reagents is effected by addition of a water-propanol mixture and refluxing. The amine and solvent are removed by thorough washing and/or calcining at temperatures as low as 200.degree. C. Mixtures of transition metal oxides with either ZrO.sub.2, TiO.sub.2, La.sub.2O.sub.3, SiO.sub.2, Al.sub.2O.sub.3 or mixtures thereof were prepared. The surface area curves of the pure oxides are Type I with surface areas of 400-600 m.sup.2/g and up to 1100 m.sup.2/g for the mixed oxides.