We report on the first synthesis of a new NASICON framework Li2Ni2(MoO4)(3) and on the investigation of its electrochemical behavior upon Li extraction coupled with structural analysis. Li2Ni2( MoO4)(3) was synthesized by a novel soft-combustion approach involving glycine as a combustion agent and the product was found to crystallize in an orthorhombic structure (space group Pmcn) with lattice parameters alpha = 10.424(4) Angstrom, b = 17.525(1) Angstrom, and c = 5.074(3) Angstrom. Reversible extraction and insertion of lithium from and into the framework structure delivered a reversible capacity of similar to115 mAh/g (4.9-1.5 V window) after the first charge/discharge cycle. (C) 2004 The Electrochemical Society.