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GaMo 4 Se 8  ( I ) and AlMo 4 S 8  ( II ) transform at  T  1  = 45(2) K and 24(2) K, respectively, from a cubic high-temperature modification with ordered defect spinel structure (space group  F [unk]3 m ,  a  = 10.1747(2) Å ( I ), 9.7289(2) Å ( II ) at 300 K) to a rhombohedrally distorted low-temperature modification ( R 3 m ,  a  rh  = 7.1537(3) Å, 6.8500(3) Å ( II ),  α  rh  = 60.572(5)°, 60.374(5)° ( II ) at 10 K). Structure parameters for both modifications are refined by the Rietveld method from X-ray powder data recorded at  T  = 300 K ( I, II ), 60 K ( I ), 50 K ( II ) and 10 K ( I, II ) on a Guinier diffractometer. In the cubic modification the tetrahedral Mo 4  clusters have [unk]3 m  symmetry and intracluster bond lengths of [Mo – Mo] = 2.881(2) Å ( I ), 2.829(2) Å ( II ). During the phase transition their symmetry is reduced to 3 m  as they expand each by about 0.05 Å at one of their triangular bases.

Structural phase transition in GaMo 4 Se 8 and AlMo 4 S 8 by X-ray powder diffraction