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In this article, six new Fe 3 S 2  cluster complexes Fe 3 (µ 3 S) 2 (CO) 7 [(Ph 2 P) 2 NR] ( 1 - 6 ) (R = (CH 2 ) 2 CH 3 , CH(CH 3 ) 2 , (CH 2 ) 3 CH 3 , CH 2 CH(CH 3 ) 2 ,  p -C 6 H 4 CCH and  m -C 6 H 4 CCH) were successfully synthesized by reactions of Fe 3 S 2 (CO) 9  and the corresponding aminodiphosphines under refluxing toluene. Meanwhile, treatment of Fe 3 S 2 (CO) 9  and (Ph 2 P) 2 NCH(CH 3 )Ph afforded two new Fe 3 S 2  cluster complexes Fe 3 (µ 3 -S) 2 (CO) 7 [(Ph 2 P) 2 NCH(CH 3 )Ph] ( 7 ) and Fe 3 (µ 3 -S) 2 (CO) 7 [(κ 2 -Ph 2 P) 2 NCH(CH 3 )(Ph)] ( 8 ). Complexes  1–8  were characterized by elemental analysis, FT-IR, NMR spectroscopy, and especially X-ray crystallography. The elctrochemical properties were investigated by cyclic voltammetry, showing that they all have electrocatalytic ability for the reduction of protons to H 2 .

Fe 3 S 2 cluster complexes containing aminodiphosphine ligand: synthesis, characterization, crystal structures and electrochemical properties