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The system (1 - x)NiIn 2 S 4  - xNiIn 2 Se 4  has been investigated by X-ray powder methods. The subsolidus phase diagram is constructed in the temperature interval 600 -1000 °C. The spinel type NiIn2S4 exhibits a phase width up to the composition NiIn 2 S 2 Se 2  at 900 °C and NiIn 2 S 2.8 Se 1.2  at 600 °C. A new layered compound is formed for 0.7 ≥ x ≥ 0.5 at 600 °C and for x = 0.6 at 900 °C which crystallizes in the MgAl 2 S 4 -type with a = 392.4 and c = 3739.6 pm (x = 0.6) for the hexagonal cell.

A New Layered Chalcogenide in the System NiIn 2 S 4 -NiIn 2 Se 4