Mesoporous Li3Fe2(PO4)(3) battery electrode materials (see Figure) with a discharge capacity of 140 mAh g(-1) at 20 mA g(-1) self-assemble under aqueous conditions using a cationic surfactant as the template. Mossbauer spectroscopy results are characteristic of Fe3+ ions in oxides, while the interaction of lithium with Fe and O in mesoporous Li3Fe2(PO4)(3) is verified by Li-7 NMR. This synthetic strategy may be applied to the production of other multi-metal phosphate ordered mesoporous structures.