A novel lithium iron phosphate has been synthesized by a solution route at moderate temperature. The structure was determined from powder by XRD, HRTEM and SAED experiments. LiFe2P3O10 tripolyphosphate crystallizes in the monoclinic system, space group P21/m, with lattice constants a = 4.597(7) Å, b = 8.566(4) Å, c = 9.051(4) Å, ˇ=97.47◦ and Z = 2. Internal and external vibrational modes (Raman and FTIR) show that the dominant spectral features come from the (P3O10)5− oxo-anions displaying internal and external modes along with the P–O–P bridging modes. Magnetic measurements are consistent with the high-spin configuration of Fe2+ cation with an effective magnetic moment 5.51B. A weak antiferromagnetic ordering is observed belowthe Néel temperature at TN = 19K. Electron paramagnetic resonance spectroscopy confirms this electronic configuration and provides evidence of the presence of a carbonaceous layer onto the particle surface. Electrochemical measurements were carried out in lithium cells with LiPF6–EC–DEC electrolyte at 25 ◦C. The material delivered a capacity 70 mAh/g in the voltage range 2.7–3.9 V, close to the theoretical value (72 mAh/g). The resulting cyclic voltammogram indicates a stable structure with a good reversibility with the redox peaks at 3.26 and 3.13V vs. Li0/Li+.