Electrochemical reduction of cationic Li+@C60 to neutral Li+@C60˙−: isolation and characterisation of endohedral [60]fulleride

Hiroshi Ueno; Shinobu Aoyagi; Yu Yamazaki; Kei Ohkubo; Naohiko Ikuma; Hiroshi Okada; Tatsuhisa Kato; Yutaka Matsuo; Shunichi Fukuzumi; Ken Kokubo

doi:10.1039/C6SC01209D

Electrochemical reduction of cationic Li⁺@C₆₀ to neutral Li⁺@C₆₀˙⁻: isolation and characterisation of endohedral [60]fulleride†

Hiroshi Ueno,‡^a Shinobu Aoyagi,^b Yu Yamazaki,^a Kei Ohkubo,^cd Naohiko Ikuma,

^a Hiroshi Okada,^e Tatsuhisa Kato,^f Yutaka Matsuo,^eg Shunichi Fukuzumi^dh and Ken Kokubo

*^a

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* Corresponding authors

^a Division of Applied Chemistry, Graduate School of Engineering, Osaka University, Suita, Osaka 565-0871, Japan
E-mail: kokubo@chem.eng.osaka-u.ac.jp

^b Department of Information and Basic Science, Nagoya City University, Mizuho-ku, Nagoya 467-8501, Japan

^c Department of Material and Life Science, Graduate School of Engineering, Osaka University, ALCA and SENTAN, Japan Science and Technology (JST), Suita, Osaka 565-0871, Japan

^d Department of Chemistry and Nano Science, Ewha Womans University, Seoul 120-750, Korea

^e Department of Mechanical Engineering, School of Engineering, The University of Tokyo, Bunkyo-ku, Tokyo 113-8656, Japan

^f Department of Interdisciplinary Environment, Graduate School of Human and Environmental Studies, Kyoto University, Sakyo-ku, Kyoto 606-8501, Japan

^g Hefei National Laboratory for Physical Sciences at Microscale, University of Science and Technology of China, Hefei, Anhui 230026, China

^h Faculty of Science and Engineering, Meijo University, ALCA and SENTAN, Japan Science and Technology Agency (JST), Nagoya, Aichi 468-0073, Japan

Abstract

Lithium-encapsulated [60]fullerene Li@C₆₀, namely, lithium-ion-encapsulated [60]fullerene radical anion Li⁺@C₆₀˙⁻, was synthesised by electrochemical reduction of lithium-ion-encapsulated [60]fullerene trifluoromethanesulfonylimide salt [Li⁺@C₆₀](TFSI⁻). The product was fully characterised by UV-vis-NIR absorption and ESR spectroscopy as well as single-crystal X-ray analysis for the co-crystal with nickel octaethylporphyrin. In solution Li@C₆₀ exists as a monomer form dominantly, while in the crystal state it forms a dimer (Li@C₆₀–Li@C₆₀) through coupling of the C₆₀ radical anion cage. These structural features were supported by DFT calculations at the M06-2X/6-31G(d) level of theory.

Chemical Science

Electrochemical reduction of cationic Li⁺@C₆₀ to neutral Li⁺@C₆₀˙⁻: isolation and characterisation of endohedral [60]fulleride†

Abstract

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Electrochemical reduction of cationic Li⁺@C₆₀ to neutral Li⁺@C₆₀˙⁻: isolation and characterisation of endohedral [60]fulleride

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