In the presented article, oxide forms of iron catalysts with the wustite structure and with a R = Fe2+/Fe3+ molar ratio in the range from 3.78 to 8.16 were investigated. The chemical composition of the tested catalyst precursors was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The X-ray diffraction (XRD) technique was used to determine the phase composition and location of reflections characteristic of the Fe1−xO phase. The molar ratio of iron ions R = Fe2+/Fe3+ was determined by manganometric titration. The distribution of promoters in the structure of iron catalyst precursors with different R = Fe2+/Fe3+ ratio was determined by a selective etching method. The dependence of the lattice parameter