A tetraethylammonium (TEA) salt of TeO 4 (2-) was synthesized by reacting Te(OH) 6 with tetraethylammonium hydroxide. X-ray structural analysis of (TEA) 2TeO 4.2H 2O confirmed that this new compound consists of discrete TeO 4 (2-) anions of distorted tetrahedral structure together with TEA cations and water molecules of crystallization [ a = 8.0820(9) A, b = 13.7730(12) A, c = 20.1590(18) A, V = 2244.0(4) A (3), Z = 4, and space group Pccb]. The (125)Te NMR spectrum indicated that water reacts with the TeO 4 (2-) anion to regenerate octahedral tellurate species in solution.