K2NiF4-type organic-based perovskites of the (C4H9NH3)2FexPb1-xCl4 (x=0.00, 0.25, 0.50, and 0.75) system have been synthesized using a low-temperatu re solution method under a flowing argon gas. When stoichiometric butylamine, iron chloride, and lead chloride are mixed, a yellow solution are obtained from slow cooling of 90 to -10 $^{circ}C.$ The final product is a plate-like yellow crystal. The X-ray crystallographic analysis has been carried out using XRD in the range of $5^{circ}{leq}$ 2${ heta}$ ${leq}80^{circ}.$ The local symmetry around the absorbing Pb atom of the samples has been determined by the EXAFS spectroscopic study. The crystals assign to orthorhombic system by the XRD analysis. The FT-IR spectra are analyzed in the range of 600 to 3300 cm-1 . DSC and TGA are measured to detect thermal stability between 30 and 300 $^{circ}C.$ Two endothermic peaks are detected in all samples. The electrical conductivity has been measured using the four-probes technique for the (C4H9NH3)2FexPb1-xCl4 system in 300-460 K. Photoluminescence phenomenon was also investigated at room-temperature.