The first experimental observation of diffraction from a thin surface layer at a 90 Bragg reflection is reported. A thin (< 1 mm) InGaAs film deposited on a GaAs(800) substrate was studied near the 90 Bragg position. Slight, less than 0.1%, difference in the lattice spacing between the layer and the substrate, has allowed, for the first time, a direct and exclusive observation of the diffraction profile from a thin layer as if it was a ªfree-standingº thin crystal.