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The controversial space-group problem of spinel, MgAl2O4, whether it is Fd3m or F
3m, was studied by electron diffraction. It was confirmed that the appearance of 'forbidden reflections' such as {200} was caused by the double reflection process of reflections with high indices on the non-zero-order Laue zone. Consequently, the space group of spinel is Fd3m, and the assignment of the space group to F3m is ruled out. The change of space group from F3m to Fd3m associated with a phase transition, proposed by Mishra & Thomas [Acta Cryst. (1977), A33, 678], can also be explained by double diffraction: the magnitudes of primary reflections with high indices rapidly decrease due to the increase of the Debye-Waller factors at elevated temperatures.
3m, was studied by electron diffraction. It was confirmed that the appearance of 'forbidden reflections' such as {200} was caused by the double reflection process of reflections with high indices on the non-zero-order Laue zone. Consequently, the space group of spinel is Fd3m, and the assignment of the space group to F3m is ruled out. The change of space group from F3m to Fd3m associated with a phase transition, proposed by Mishra & Thomas [Acta Cryst. (1977), A33, 678], can also be explained by double diffraction: the magnitudes of primary reflections with high indices rapidly decrease due to the increase of the Debye-Waller factors at elevated temperatures.
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