Crystal structure of the high-temperature phase of lithium ionic conductor, Li3PS4, was determined using high-temperature synchrotron X-ray diffraction data. Li3PS4 belongs to the thio-LISICON (LIthium Super Ionic CONductor) family and shows high ionic conductivity above 500 K. The high-temperature α phase with space group, Pbcn(60), has an orthorhombic cell parameter, a = 8.6125(2) Å, b = 9.0211(2) Å, and c = 8.42621(2) Å at 906 K. The PS4 tetrahedra are isolated with each other and form an alternating T+ row and T- row, where T+ and T- indicate that the apex of the tetrahedra is up and down, respectively. These PS4 arrangements are different from those of the medium temperature β-phase and the low-temperature γ-phase.
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