Two new Fe 3S 3 cluster compounds, compound 5 〔Et 4N〕 3〔Fe 3( p ClPhS) 3Cl 6〕 and compound 6 〔Et 4N〕 3〔Fe 3(Cl 5PhS) 3Cl 6〕 have been successfully synthesized with one step reaction. Combination of compounds 5,6 and compounds 1~4 which were synthesized earlier, their UV,IR and CV spectra have been studied systematically, deeply to understand molecular electronic characteristics. There is a blueshift within 260nm and a redshift over 260nm in the UV spectra of compounds, it has been shown that Fe-S cluster needs more energy in transition of electric charge (CT), but needs less energy in d d transition area. In the IR spectra, the most interesting bands appearing in the regions of 422~386cm -1 and 492~474cm -1 are attributed to S-Fe-S (Fe 3S 3 unit) and FeS (Ph-S) stretching vibration respectively. The bands in the region 330~285cm -1 and 245~183cm -1 can be assigned to Fe-Cl and Fe-Br stretching vibration respectively. Their CV spectra show that this is a quasi reversible redox process. In this process, an Fe 2+ loses an electron and is oxidized to Fe 3+ , then gets an electron and is reduced to Fe 2+ . The redox electrical potentials of compounds 1, 3~6 are +0.07V / -0.60V, +0.24V / -0.80V, +0.40V / -0.80V, +0.43V / -1 20V, +0.54V/-1.00V, respectively. Two new Fe 3 S 3 cluster compounds, compound 5 [Et 4 N] 3 [Fe 3 (p ClPhS) 3Cl 6] and compound 6 [Et 4N] 3 [Fe 3 (Cl 5PhS) 3Cl 6] have been successfully synthesized with one step reaction. Combination of compounds 5,6 and compounds 1 ~ 4 which were synthesized earlier, their UV, IR and CV spectra have been studied systematically, deeply to understand molecular electronic characteristics. There is a blueshift within 260nm and a red shift over 260nm in the UV spectra of compounds, it has been shown that Fe-S cluster needs more energy in transition of electric charge (CT), but needs less energy in dd transition area. In the IR spectra, the most interesting bands appearing in the regions of 422 ~ 386 cm -1 and 492~474 cm -1 are attributed to S-Fe-S (Fe 3 S 3 unit) and FeS (Ph-S) stretching vibration respectively. The bands in the region 330-285 cm -1 and 245-183 cm -1, 1 can be assigned to Fe-Cl and Fe-Br stretching vibration respectively. Their CV spectra show that this is a quasi reversible redox process. In this process, an Fe 2+ loses an electron and is oxidized to Fe 3+, then gets an electron and is reduced to Fe 2+. The redox electrical potentials of compounds 1, 3 to 6 are + 0.07V / -0.60V, + 0.24V / -0.80V, + 0.40V / -0.80V, + 0.43V / -1 20V, + 0.54V / -1.00V, respectively.