Synthesis and 83Kr NMR spectroscopy of Kr@C60†
George R.
Bacanu, 
a
Elizabeth S.
Marsden,
a
Mark C.
Walkey,
a
Mohamed
Sabba,
a
Sally
Bloodworth,
a
Graham J.
Tizzard,
a
Malcolm H.
Levitt
a
and
Richard J.
Whitby
*a
a
Elizabeth S.
Marsden,
a
Mark C.
Walkey,
a
Mohamed
Sabba,
a
Sally
Bloodworth,
a
Graham J.
Tizzard,
a
Malcolm H.
Levitt
a
and
Richard J.
Whitby
*a
Abstract
Synthesis of Kr@C60 is achieved by quantitative high-pressure encapsulation of the noble gas into an open-fullerene, and subsequent cage closure. Krypton is the largest noble gas entrapped in C60 using ‘molecular surgery’ and Kr@C60 is prepared with >99.4% incorporation of the endohedral atom, in ca. 4% yield from C60. Encapsulation in C60 causes a shift of the 83Kr resonance by −39.5 ppm with respect to free 83Kr in solution. The 83Kr spin-lattice relaxation time T1 is approximately 36 times longer for Kr encapsulated in C60 than for free Kr in solution. This is the first characterisation of a stable Kr compound by 83Kr NMR.
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