Polycrystalline samples of isostructural MSb 2 O 4 (M=Co, Ni) have been prepared by solid state synthesis and lithium-storage is investigated as possible anode materials for lithium-ion batteries. The reaction mechanism of lithium with MSb 2 O 4 (M=Co, Ni) is explored by galvanostatic cycling, cyclic voltammogram and ex situ studies. Both CoSb 2 O 4 and NiSb 2 O 4 exhibit similar electrochemical behavior and show reversible capacity of 490 and 412mAhg −1 respectively in the first cycle. Reversible alloying de-alloying of Li x Sb takes place in an amorphous matrix of M (Co, Ni) and Li 2 O during electrochemical cycling.