The structural behaviour at high temperature of the oxidized nickelates R 2NiO 4+δ(R=La, Pr and Nd) has been studied by means of neutron diffraction measurements. In the case of La 2NiO 4+δ the structure has tetragonal symmetry for the full measured temperature range. The temperature dependence of a and b cell-parameters shows the existence of a first order structural transformation, from an orthorhombic symmetry at room temperature, to a tetragonal symmetry at higher temperatures for Pr and Nd compounds. The value of this transformation temperature is about 690 K in the case of Pr 2NiO 4+δ and 790 K for Nd 2NiO 4+ δ. In the latter case, keeping the sample under vacuum (∼10 −6 Torr) at a temperature around 1100 K, the structure becomes again orthorhombic, but different from the previous one. This effect is due to the loss of interstitial oxygen from the system at constant high temperature with the time.