Spinel (MgAl2O4) single crystals which had been neutron irradiated at (nominally) 400 and 750°C to high doses (53-250 dpa) were examined using 27Al magic angle spinning (MAS) nuclear magnetic resonance (NMR). The sensitivity of this procedure to a specific cation (Al) residing in different crystallographic environments allowed us to determine the distribution of the Al between the tetrahedral and octahedral cation sites in the spinel structure. Our results indicate that the Al was distributed nearly equally over both cation sites in the spinel, resulting in a nearly inverse structure.