Layered manganese oxides containing Lithium and/or potassium have been synthesized by the electrochemical reduction of permanganate solutions. The synthesis provides products with manganese near an oxidation state of four. The products as shown by XRD have the rancieite-type structure and crystallite size on the order of 10 nm. In this paper, the synthesis and characterization will be presented along with the initial cycling of these materials as positive electrodes in Li-batteries.