Cryogenic NMR spectroscopy of endohedral hydrogen-fullerene complexes

Cryogenic NMR spectroscopy of endohedral hydrogen-fullerene complexes
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DOI:
10.1063/1.2174012
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发表时间:
2006-03-14
影响因子:
4.4
通讯作者:
Komatsu, K
Komatsu, K
中科院分区:
化学2区
文献类型:
--
作者:
Carravetta, M;Johannessen, OG;Komatsu, K

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在低温条件下,我们观察到了被困在改性富勒烯笼中的氢分子的H-1 NMR谱。静态样品上的实验在样品温度下进行到4.3 K,而魔角旋转(MAS)实验在温度下进行到20 K,旋转频率为15 kHz。这两种类型的NMR谱显示在低于50 K的温度下,分子内H-1-H-1偶极耦合的大幅增加,揭示了少量的空间旋转状态的热选择。静态和MAS光谱进行了比较,以估计在高速低温MAS-NMR实验样品加热的程度。低温MAS-NMR数据表明,魔角旋转NMR的位置分辨能力可以与低温操作的高信号强度相结合,低温现象可以用化学位置选择性来研究。
We have observed H-1 NMR spectra of hydrogen molecules trapped inside modified fullerene cages under cryogenic conditions. Experiments on static samples were performed at sample temperatures down to 4.3 K, while magic-angle-spinning (MAS) experiments were performed at temperatures down to 20 K at spinning frequencies of 15 kHz. Both types of NMR spectra show a large increase in the intramolecular H-1-H-1 dipolar coupling at temperatures below 50 K, revealing thermal selection of a small number of spatial rotational states. The static and MAS spectra were compared to estimate the degree of sample heating in high-speed cryogenic MAS-NMR experiments. The cryogenic MAS-NMR data show that the site resolution of magic-angle-spinning NMR may be combined with the high signal strength of cryogenic operation and that cryogenic phenomena may be studied with chemical site selectivity.