1428546-10-4Relevant academic research and scientific papers
Synthesis, characterization and crystal structures of carboxy- functionalized diiron propanedithiolate complexes
Zhao, Pei-Hua,Liu, Ya-Qing,Zhao, Gui-Zhe
, p. 144 - 149 (2013)
Four new carboxy-functionalized diiron propanedithiolate complexes 1-4 have been successfully synthesized and fully characterized. The all-carboxyl complexes [(μ-SCH2)2CHCO2CH 2CH2Cl][Fe2(CO)6] (1) and [(μ-SCH2)2CHCO2C6H 4I-p][Fe2(CO)6] (2) were prepared by the condensation reaction of the known complex [(μ-SCH2) 2CHCO2H][Fe2(CO)6] (A) with ClCH2CH2OH and p-IC6H4OH in the presence of 4-dimethylaminopyridine (DMAP) and dicyclohexylcarbodiimide (DCC) in yields of 46% and 66%, whereas the phosphine-substituted complexes [(μ-SCH2)2CHCO2CH2CH 2Cl][Fe2(CO)5PPh3] (3) and [(μ-SCH2)2CHCO2CH2CH 2Cl][Fe2(CO)4(PPh3)2] (4) were further synthesized through the carbonyl substitution reaction of 1 with PPh3 using the decarbonylating agent Me3NO·2H 2O in yields of 44% and 41%. The new complexes 1-4 were characterized by combustion analysis, IR and 1H, 13C and 31P NMR spectroscopic techniques. The molecular structures of 1-4 were unequivocally determined by single crystal X-ray diffraction analysis, in which the carboxy-functionalized substituent attached to the bridgehead-C atom resides in an equatorial position of the six-membered rings in the solid state.
