We describe the direct single potential electrodeposition of crystalline CU2Sb, a promising anode material for lithium-ion batteries, from aqueous solutions at room temperature. The use of citric acid as a complexing agent increases the solubility of antimony salts and shifts the reduction potentials of copper and antimony toward each other, enabling the direct deposition of the intermetallic compound at pH 6. Electrodeposition Of CU2Sb directly onto conducting substrates represents a facile synthetic method for the synthesis of high quality samples with excellent electrical contact to a substrate, which is critical for further battery testing.