The distribution of cations in Ti
xV
1-xS
1.40 (0≤
x≤1), Ti
xV
1-xS
1.57 (0≤
x≤1) and Fe
xV
3-xS
4 (0≤
x≤2), which have metal-deficient NiAs-like structures, is investigated by magnetic susceptibility, NMR and Mössbauer experiments. It is made clear that these cations increase the preferential occupation of the sites in the metal-full layers of each structure in the order of Ti, V and Fe which coincides with that of the ionization tendency. The interaction between metal atoms neighbouring along the c axis plays an important role in the site preference and magnetic properties. [J. Cryst. Soc. Jpn. 26,
220 (1984) ] .
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