Cyclic voltammetry of 5 showed three irreversible reduction events (Figure ). An attempt to reference the reduction potentials to a ferrocene internal standard was unsuccessful due to reactivity with Fc and Fc + . The lack of electrochemical reversibility may be due to large structural changes occurring different oxidation states. Undeterred, we proceeded to stoichiometrically reduce 5 with 1 equiv of KC8 per iron at -78 °C in THF, which resulted in a deep purple solution. Crystallization from diethyl ether at -40 °C give iron(II) complex 6 in 46% yield. Its X-ray crystal structure, shown in Figure , shows a tetrameric assembly in the solid state, with K + bridging S atoms and Dipp groups. There are six (SCS)Fe units in each asymmetric unit, and the average Fe-C and Fe-SPincer bond lengths are 1.947(4) Å and 2.23(9) Å, respectively. The average distance between S and K in the central bridge is 3.19(1) Å. As in 5-Solv, the Fe-S bond lengths are ~0.05 Å longer on the side of the pincer where the S is bridging two iron centers.