Investigations on Macrocyclic Complexes Containing [Fe 2 S 2 ] Clusters: Synthesis and Characterization

Two macrocyclic complexes containing [Fe 2 S 2 ] clusters [(μ‐SCH 2 ) 2 Fe 2 (CO) 5 ] 2 (NCH 2 CH 2 N)(Ph 2 PCH 2 CH 2 CH 2 PPh 2 ) ( 1 ) and [(μ‐SCH 2 ) 2 Fe 2 (CO) 5 ] 2 (NCH 2 CH 2 N)(Ph 2 PCH 2 CH 2 CH 2 CH 2 PPh 2 ) ( 2 ) were prepared from reactions of [(μ‐SCH 2 ) 2 Fe 2 (CO) 6 ] 2 (NCH 2 CH 2 N) with Ph 2 PCH 2 CH 2 CH 2 PPh 2 (dppp) or Ph 2 PCH 2 CH 2 CH 2 CH 2 PPh 2 (dppb) in the presence of the CO‐removing agent Me 3 NO·2H 2 O. Complexes 1 and 2 were characterized by elemental analysis and IR and NMR spectroscopy. In addition, the X‐ray structure of 2 showed the molecule to contain a 16 atom macrocycle, which is joined together by an ethylene group and a bidentate ligand dppb.