In this study a series of Fe-Mo/Al/sub 2/O/sub 3/ catalysts with different atomic ratios, R = Mo/Mo + Fe, of 0.05, 0.25, 0.50, 0.75, 0.90, and 0.95 were prepared and characterized by x-ray diffraction and Moessbauer and Auger spectroscopic techniques. The percentage conversions of coal liquids soluble in tetrahydrofuran (THF), ethyl acetate, and pentane as a function of R values were also determined. Evidence of the interaction between the support and the active components of the catalysts was observed. Additional evidence of the variation in the amount of different species in the catalyst with the change in the concentration of iron atoms was also found. The activity of the Mo/Al/sub 2/O/sub 3/ catalyst was highly influenced by the presence of Fe atoms in the samples.