In this paper the synthesis and structural characterisation of two new K2NiF4-type phases, Ba2In0.5Sb0.5O4 and Sr2In0.5Sb0.5O4, are reported. These are the first examples of K2NiF4 compounds of general formula A2MIII0.5M’V0.5O4 with both 3+ and 5+ cations in the octahedral sites. Ba2In0.5Sb0.5O4 is shown to have a tetragonal cell [space group I4/mmm, a
= 4.1651(1), c
= 13.299(1)
Å] with an essentially disordered arrangement of In and Sb. In the case of Sr2In0.5Sb0.5O4, however, ordering of In and Sb is observed leading to an expanded unit cell [Pmcb, a
= 5.7592(1), b
= 5.7740(1), c
= 12.543(1)
Å]. The results therefore show that varying the size of the alkaline earth cation has a pronounced effect on the ordering of In and Sb within the structure.
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