LiNi 1/3 Co 1/3 Mn 1/3 O 2 (LNMCO) powders were formed by a two-step synthesis including preparation of an oxalate precursor by "chimie douce" followed by a solidstate reaction with lithium hydroxide. The product was characterized by TG-DTA, X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR), Raman spectroscopy, electron spin resonance (ESR), and SQUID magnetometry. XRD data revealed well-crystallized layered LNMCO with α-NaFeO 2 -type structure (R-3 m space group). Morphology studied by SEM and TEM shows submicronic particles of 400-800 nm with a tendency to agglomerate. The local structure investigated by vibrational spectroscopy (FTIR, Raman), ESR, and SQUID measurements confirms the well-crystallized lattice with a cation disorder of 2.6% Ni 2+ ions in Li(3b) sites. Electrochemical tests were carried out in the potential range 2.5-4.5 V vs. lithium metal on samples heated at 900°C for 12 h. Initial discharge capacity is 154 mAh/g at C/5, while a capacity of 82 mAh/g is still delivered at 10