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A crystallographic study of the system Ni2+1−2xNi3+xLi+xO has been carried out. The crystal structure of the material in the range 0≤x≤0.4 at room temperature and up to 1000°C has been studied. The principal coefficients of thermal expansion and the phase diagram are given. The structural rhombohedral → face-centred cubic transition temperature of NiO has been determined.