Single crystals of sodium metaperrhenate, NaReO4, have been obtained by oxidation of rhenium metal with sodium nitrate under high pressure- high temperature conditions (modified Belttype apparatus, 4 kbar, 400 °C, Au-capsules). The crystals are tetragonal, space group I41/a, with a = 5.3654(4), c = 11.732(2) Å and Z = 4. The structure was refined to R - 0.026, Rw = 0.013 for 382 unique, absorption-corrected reflections. The scheelite-type structure for NaReO4, proposed by Beintema in 1937, could be confirmed. It consists of isolated ReO4 tetrahedra (Re-O= 1.728(2) Å ), connected by NaOs dodecahedra (<Na- O > = 2.582(2) Å).