The distribution of iron cations in the crystal lattice of the Fe3-vO4 (v = 0.153) cation-deficient spinel produced by mechanical dispersion of α-Fe2O3 hematite in water is investigated using x-ray diffraction and Mössbauer spectroscopy. Analysis of the Mössbauer data shows that the Fe2.847O4 magnetite prepared by mechanochemical synthesis is a chemically heterogeneous compound. The crystal structure of Fe2.847O4 is characterized by local environments of the (Fe2.5+)0 cations at v0 < 0.1, v1 ≅ 0.12, v2 ≅ 0.18, and v3 ≅ 0.26, which are responsible for a broad distribution of magnetic hyperfine fields with, the P(H) probability maxima near 37.0, 36.0, 34.0, and 30.0 MA m-1. © 2002 MAIK "Nauka/Interperiodica".