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A synthetic method for the design of heterogeneous catalysts incorporating monodisperse platinum nanoparticles into ordered mesoporous oxide frameworks has been developed. Nanoparticles were synthesized in solution in the presence of surface templating polymer and encapsulated into mesoporous oxide matrices. After polymer removal by calcination, ethylene hydrogenation rates were consistent with previously reported results, while superior activity of low coordination atoms in small crystallites during ethane hydrogenolysis was demonstrated. Changes in reaction selectivity with particle size during the hydrogenation/dehydrogenation of cyclohexene were attributed to a hydrogen coverage effect influencing the hydrogenation pathway and the apparent structure sensitivity of the dehydrogenation pathway.