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The clustering of nickel has been studied in a single crystal of lithium fluoride with about 2 × 10-3 Ni2+ ions per mole. The divalent ions cluster even at room temperature in samples quenched from dissolution temperature. The size of clusters is about 15 Å and their structure is not well defined. With annealing the clusters grow in size quickly, and their structure becomes that of spinel Li(LiNi)F4 at 250°C.