Mo¨ssbauer and crystallographic investigations were carried out on DyFe3−xNixcompounds crystallizing in the PuNi3type of structure. The hyperfine field observed at the iron sites shows a maximum atx=0.75. The 12‐line spectrum observed at room temperature corresponding to the two different kinds of iron in the structure collapsed into a single six‐line pattern at 4.2 K. Lattice parametercshows a rapid decrease whenxis increased beyond 2.0, but no such behavior was found in thealattice parameter. The results of the x‐ray and Mo¨ssbauer data are explained in terms of site preference and nonlocalized transition‐metal moments, respectively.