A new iron titanyl oxyphosphate Fe 0.50 TiO(PO 4 ) was synthesized by both solid-state reaction and Cu 2+ -Fe 2+ ion exchange method. The material was then characterized by X-ray diffraction, Mo¨ssbauer spectroscopy, magnetic susceptibility measurements and Raman spectroscopy. The crystal structure of the compound was refined, using X-ray powder diffraction data, by Rietveld profile method; it crytallizes in the monoclinic system, space group P2 1 /c (No.14), with a ¼ 7:4039ð3Þ Å, b ¼ 7:3838ð3Þ Å, c ¼ 7:4083ð3Þ Å, b ¼ 120:361ð1Þ, V ¼ 349:44ð2Þ Å3 and Z ¼ 4. The volume of the title compound is comparable to those of the M 0.50 II TiO(PO 4 ) series, where M II ¼ Mg, Co, Ni and Zn. The framework is built up from [TiO 6 ] octahedra and [PO 4 ] tetrahedra. [TiO 6 ] octahedra are linked together by corners and form infinite chains along the c-axis. Ti atoms are displaced from the center of octahedral units showing an alternating short distance (1.73 A ˚) and a long one (2.22 A ˚). These chains are linked together by [PO 4 ] tetrahedra. Fe 2+ cations occupy a triangle-based antiprism sharing two faces with two [TiO 6 ] octahedra. Mo¨ssbauer and magnetic measurements show the existence of iron only in divalent state, located exclusively in octahedral sites with high spin configuration (t 2g 4 e g 2 ). Raman study confirms the existence of Ti-O-Ti chains.