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a b s t r a c tNickel titanium oxyphosphate Ni 0.5 TiOPO 4 (NTP), was prepared by co-precipitation route. Its structure was determined by single crystal X-ray diffraction. The compound crystallizes in the monoclinic system, S.G: P2 1 /c [a = 7.333(1)Å, b = 7.316(2)Å, c = 7.339(2)Å,ˇ= 119.62(3) • , Z = 4, R 1 = 0.0142, wR 2 = 0.0429]. The structure might be described as a {TiOPO 4 } framework made of corner-sharing [TiO 6 ] octahedra chains running parallel to [0 0 1] and cross linked by phosphate [PO 4 ] tetrahedral, where half of octahedral cavities created are occupied by Ni atoms, and the other half of octahedral sites are vacant. During the first discharge, the NTP electrode delivered a capacity of 530 mAh/g, upon cycling within 0.5-4 V. To understand the electrochemical reaction mechanism using different characterization techniques viz. in situ synchrotron diffraction. Reciprocal magnetic susceptibility ( −1 ) of NTP, between 4 and 300 K, shows an almost linear behavior and can be fitted by the simple Curie-Weiss law.