Single crystals of Ag2FeSn3S8 have been obtained by heating pure metals and sulphur in evacuated silica tubes at 750 degreesC. Structural analysis of Ag2FeSn3S8 by single crystal X-ray diffraction analysis shows that it crystallizes in the Fd (3) over barm space group with a = 10.5723 (4) Angstrom. The room temperature resistivity for the above thiospinel is found to be 3.3 x 104 Omega cm. The usefulness of this material as cathode in rechargeable lithium batteries is indicated by a discharge capacity of = 107.7 A h/kg in 0. 1 M LiClO4 in THF when coupled with a lithium anode for several cycles. (C) 2003 Elsevier B.V. All rights reserved.