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The distribution of In 3+  between tetrahedral and octahedral sites and coordinate of oxygen in In  x  Fe 3− x  O 4  ( x  = 0, 0.1, 0.2, and 0.3) spinels have been determined on powder samples by the Rietveld method. The weight function with a form  wYi  = l/ Y oi   2  ( Y oi   = the observed profile intensity at the  i th step) was incorporated in the present Rietveld refinement. Structures thus refined were satisfactory not only in their internal consistency but also in their conformity with single crystal data. These results corroborate earlier study, which indicated a preference of In 3+  for the tetrahedral site.  iv In–O distances in the present specimens [1.97(3) Å–2.00(5) Å] were close to the value calculated from a bond-valence scheme. In In  x  Fe 3− x  O 4 , calculated  vi Fe 2+ –O distances increased with increasing  x , and they were in between two  vi Fe 2+ –O distances in Fe 3 O 4  and  γ -Fe 2 SiO 4  (spinel structure). A change of semimetallic nature to semiconductive one by In-doping in Fe 3 O 4  would be responsible for the elongation of  vi Fe 2+ –O distance.

Crystal structure refinements of In x Fe 3− x O 4 ( x ≤ 0.3) spinels by the Rietveld method