The synthesis and characterization of mononuclear iron complexes containing mono-thiocarbonate ligands are described. The new compounds of general formula CpFe(CO) 2 SCO 2 R [R=Et (1), iso-Bu (2), Ph (3), 4-C 6 H 4 NO 2 (4), Me (5)] were prepared by reacting the iron sulfides (μ-S x )[CpFe(CO) 2 ] 2 (x=2, 3) with the corresponding chloroformates (ROCOCl). These new complexes have been characterized by elemental analyses and spectroscopic methods. The crystal structure of CpFe(CO) 2 SCO 2 Et, 1, has been determined by single crystal X-ray diffraction analysis.