Ti2O(PO4)2·2H2O (1), a three-dimensional titanium oxophosphate, thermally transforms to Ti2O(PO4)2 (2), a fibrous novel compound. The crystal structure of 2 was solved ab initio using powder X-ray diffraction data (triclinic, P1[combining macron], a = 5.0843(1) Å, b = 8.6121(2) Å, c = 9.6766(2) Å, α = 74.501(2)°, β = 76.146(2)°, γ = 74.488(3)°, Z = 2). Compound 2, containing both 4- and 6-fold coordinated titanium atoms, shows measurable thermally activated nitrogen-adsorption. To our knowledge, the process described here constitutes the first example of nitrogen-fixation by an inorganic material at above-ambient temperature.