Layered perovskite manganites with a nominal chemsitry of Sm2-2xSr1+2x-2yCa2yMn2O7 (x=0.2, 0.3, 0.4, 0.5; y=0, 0.2, 0.3) were prepared using sol-gel method. The crystal structures of these compounds were studied by X-ray diffraction (XRD) and FTIR absorption spectra. The absorption peaks become weaker and move a little to higher frequency with increasing of Sm/Sr concentration. As the Sm doping increases to x=0.2 and x=0.3, the absorption peaks show a cubic structure character, reflecting that the samples suffer from a transition from tetragonal structure to cubic structure. This coincides with the X-ray diffraction results. The high temperature electrical properties were studied by conventional four-probe method. Although all samples exhibit the semiconductive behavior, lnρ-1 000/T curves are not linear and they obey the small polaron hopping mechanism. Moreover, the resistivity decreases with x reducing. This is due to that Sm doping increases the Jahn-Teller ion Mn3+ / Mn4+ ratio, and decreases the eg bandwidth. Layered perovskite manganites with a nominal chemsitry of Sm2-2xSr1 + 2x-2yCa2yMn2O7 (x = 0.2, 0.3, 0.4, 0.5; y = 0, 0.2, 0.3) were prepared using sol- gel method. The crystal structures of these compounds were studied The absorption peaks become weaker and move a little to higher frequency with increasing of Sm / Sr concentration. As the Sm doping increases to x = 0.2 and x = 0.3, the absorption peaks show a cubic structure character, reflecting that the samples suffer from a transition from tetragonal structure to cubic structure. The high temperature electrical properties were studied by conventional four-probe method. semiconductive behavior, lnρ-1 000 / T curves are not linear and they obey the small polaron hopping mechanism. Moreover, the resistivity decreases with x reducing. This is due to that Sm doping increases the Jahn-Teller ion Mn3 + / Mn4 + ratio, and decreases the eg bandwidth