One of the biggest and critical problems researchers attempt to solve in lithium-ion batteries is the dendrite formation that develops after repeated charges, causing batteries to short-circuit and sometimes explode. To approach this, Li3VO4 with working voltage between 0.5∼0.8 V (vs Li+/Li) is being considered as an option to avoid lithium dendrite growth. In this study, highly crystalline nanosized Li3VO4 has been synthesized from novel bimetallic complexes containing both vanadium and lithium with molecular formula [LiV(OtBu)4LiN[Si(CH3)3] (1) and [V8 Li2 O2(OMe)26] (2) (where Me = methyl and Bu = tert butyl). The chemical identity of the synthesized complexes was established by single-crystal X-ray diffraction studies, cyclovoltammetry, and spectrometric studies. The crystal structure and phase purity of the synthesized Li3VO4 were examined by powder X-ray diffraction while Transmission electron microscopy and X-ray photoelectron spectroscopy data confirmed the morphology and chemical composition respectively. The electrochemical properties of the anode made of lithium vanadate nanomaterials will be studied and discussed.