The deposition of multilayers of yttrium arachidate by the Langmuir-Blodgett technique on a silicon/copper-coated glass substrate was investigated. The films were characterized by X-ray diffraction and photoelectron spectroscopy. The c parameter was determined to be 53.92 ± 0.05 Å. The compositions of the films as determined by photoelectron spectroscopic techniques showed them to be of good quality. The electron attenuation length in these films has been determined. The characteristic “odd-even” oscillations of the 00l X-ray diffraction peaks have been discussed in terms of a new model for the coordination of the carboxylate groups around the metal ions.