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The high-temperature behaviour of LiSrAlF 6 and LiCaAlF 6 , both P31c and Z = 2, was studied with high-resolution synchrotron angle-dispersive x-ray powder diffraction in the temperature ranges 150-823 and 298-723 K, respectively. No phase transitions were detected. The temperature dependencies of structural parameters and octahedral distortions are obtained with the Rietveld method. Both materials have highly anisotropic thermal expansion, with the c parameter in LiSrAlF 6 decreasing withdoi:10.1088/0953-8984/16/32/013 fatcat:mz36dufjzzef3pidxibdmug3hy