Fullerene complexes Raman spectroscopy

To make the reactive fulleride compound KeCeo in the Fe-Ceo synthesis, fullerenes and a slight excess of potassium were sealed in a glass tube under vacuum and heated for approximately four days at 250 °C. Both solid-state NMR and Raman spectroscopy were employed to determine that the KeCeo compound was in fact synthesized. The KeCeo product was then reacted in an inert atmosphere with cyclopentadienyl-iron-dicarbonyl-iodide (CpFe(CO)2l) in tetrahydrofuran (THF) to form the complex. The recovered product was dried in an inert atmosphere. Manipulations of air-sensitive materials were carried out in a glove box or using standard Schlenk techniques. THF was distilled just prior to use from sodium benzophenone ketyl. Ceo was obtained from Aldrich, and CpFeCCOjol was obtained from Strew. 

Recently [78b], the solid-state stracture of the CeoZ/ -Bu -calixlSlarene complex has been studied through characterization techniques such as SEM, TEM, AFM, XRD, and Raman spectroscopy. Interestingly, these studies evidenced the existence of a layered tetragonal array of fullerenes encapsulated by calixarenes [78b],... 

The complex, C9H7)Ir(CO)(// -C6o), in 0.1 M TBABF4/CH2CI2 shows two reversible reductions followed by an irreversible reduction and has an irreversible oxidation [116]. Infrared [116], Raman [117] and UV/visible [116] spectroscopies indicate that the reversible reductions are localized on the fullerene. Furthermore, infrared spectra indicated that the irreversible oxidation was followed by a chemical reaction at the Ir center with the loss of CO (dichloromethane did not have a large enough oxidation window to see the Ceo irreversible wave) and the irreversible reduction also resulted in a decomposition of the complex. The small shift in the reduction potential (—80 mV) indicates a weak interaction between Ir and C6o-... 

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