The intercalated compounds of alkylsulfonates into hydrated zinc were synthesized. From the high temperature powder X-ray diffraction (HTXRD), FT-IR, and molecular size, the temperature dependence of orientation for the intercalated alkylsulfonates were determined. In the temperatures range 1, alkylsulfonates were intercalated into hexa aqua zinc layer with the bilayer structure of $32.9^{circ}$angle for ${Zn(H_2O_4]^{2+}[C_nH_{2n+1}SO_3]_2;^-$. In the temperatures range 2, alkylsulfonates were intercalated into tetra aqua zinc layer with the bilayer structure of $55.2^{circ}$angle for ${Zn(C_nH_{2n+1}SO_3)_2$. In the temperatures range 3, alkylsulfonates were directly bonded to zinc ion with the bilayer structure of $76.5^{circ}$angle for ${Zn(C_nH_{2n+1}SO_3)_2$.