We report here the hydrothermal synthesis of a series of novel zinc vanadium oxides, using tetramethyl ammonium ion in order to stabilize the layered structure of vanadium oxide during electrochemical redox reactions with lithium. The compounds were synthesized by the reaction of zinc chloride, vanadium (V) oxide, and tetramethyl ammonium hydroxide at 165 degrees C for 60 hours. Four new zinc vanadium oxide compounds were discovered, only one of which contained the organic cation; another was found to have a layered structure with bridging V-O-V groups analogous to that of beta alumina. These compounds were characterized by Xray powder diffraction, and IR. Three of the compounds reacted readily with lithium, and their electrochemical behavior in lithium cells were determined.