We investigated the structure of BDN(bis(4-diethylaminodithiobenzil) Nickel)-SOH(Stearyl alcohol) Langmuir-Blodgett films using small angle X-ray diffraction and polarized FTIR spectroscopy. The results show that the microcrystal domains formed on the surface of LB film resemble a well-laminated periodic structure with a molecular spacing of 2.56 nm. Meanwhile, the tilted angles of the molecules of SOH and BDN are about 30 degrees, referring to the normal direction of the sample surface, as determined by our XRD and FTIR studies.