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A unique polyurethane (PU) elastomer containing inorganic polyhedral oligomeric silsesquioxane (POSS) molecules as molecular reinforcements in the hard segment was investigated by means of wide-angle X-ray diffraction (WAXD), small-angle X-ray scattering (SAXS) and transmission electron microscopy (TEM) techniques. The mechanical properties of POSS modified polyurethane (POSS-PU) were also compared to those of polyurethane without POSS. The crystal structures of two different POSS molecules were first determined by X-ray powder diffraction analysis, yielding a rhombohedral cell with a=11.57Å, α=95.5° for octacyclohexyl-POSS (1,3,5,7,9,11,13,15-octacyclohexylpentacyclo[9.5.1.13,9.15,15.17,13] octasiloxane) and a=11.53Å, α=95.3° for hydrido-POSS (1-[hydridodimethylsiloxy]-3,5,7,9,11,13,15-heptacyclohexylpentacyclo [9.5.1.13,9.15,15.17,13] octasiloxane). WAXD results showed that …