The synthesis and characterization of intercalated compound of decansulfonate into hydrated nickel is presented. The compound shows a layered structure as determined by high temperature powder X-ray diffraction (HTXRD). The layer distance of the product is increased from 24.7 $AA$ to 30.5 $AA$ by increasing the temperature which is in turn accomplished by changing the structure of the intercalated nickel compound. From the X-ray diffraction data and the decanesulfonate size, the orientation of the decanesulfonate onto the nickel layer is determined. The molecular axis of the decanesulfonate with bilayer structure is tilted to the perpendicular of the nickel layer.