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Liquid-liquid interfacial reactions between FeSO4(aq.) and benzenehexathiol (BHT) in chloroform at room temperature and at 45 °C give bis(dithiolato)iron nanosheets 1-RTand 1-H, respectively. Nanosheets were characterized by IR, UV-Vis, SEM-EDS, TEM, XPS and PXRD. 1-His remarkably more crystalline than 1-RTand its chemical structure resembles not the porous nickel-BHT nanosheet ([Ni3(C6S6)2]n, “Type 1”) but the non-porous copper-BHT nanosheet ([Cu3(C6S6)]n, “Type 2”), evidenced by PXRD data. Electrical conductivity of 1-His 0.68 S cm−1with Ea= 270 meV.Liquid-liquid interfacial reaction between FeSO4(aq.) and benzenehexathiol (BHT) in chloroform at 45 °C gives bis(dithiolato)iron nanosheet 1-H, whose chemical structure resembles the non-porous copper-BHT nanosheet [Cu3(C6S6)]n. 1-Hwas characterized by various spectroscopic methods. Compared to 1-RTsynthesized at room temperature, 1-Hshows improved crystallinity and higher electrical conductivity of 0.68 S cm−1with Ea= 270 meV.