Layered $K_2NiF_4$type ($C_nH_{2n+1}NH_3)_2PbCl_4$(n=6, 8 and 10) system, or alkylammonium tetrachloroplumbate compound, has been synthesized from $PbCl_2$ and $C_nH_{2n+1}NH_3Cl$ solutions under argon ambient pressure for 12hrs at $90^{circ}C$. The crystal structure of the compound has been analyzed using X-ray powder diffaction in the range of $5^{circ}{leq}2{ heta}{leq}55^{circ}$, and all samples assigned to an orthorhombic system. Local distances of the Pb-Cl bond have been determined by Pb $L_{III}$-edge extended X-ray absorption fine structure (EXAFS) spectroscopy. The vibration modes of alkylammonium chains and the absorpton peaks of an excition have been examined by FT-IR and UV-Vis. reflectance spectra, respectively. The phase transition temperatures of the compounds have been studied by using DSC. According to the thermal analysis, two phase transition temperatures have been observed in the compositons of n=8 and 10.