(14)N overtone transition in double rotation solid-state NMR.

(14)N overtone transition in double rotation solid-state NMR.
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(14)双旋转固态NMR中的N泛音跃迁。

DOI:
10.1039/c5cp03266k
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发表时间:
2015
期刊:
PCCP
影响因子:
--
通讯作者:
Haies IM
Haies IM
中科院分区:
--
文献类型:
--
作者:
Haies IM

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涉及自旋-1 14 N核的外能级的固态NMR跃迁是免疫的,在微扰理论中的一阶,由核四极相互作用引起的加宽。当与魔角样品旋转结合获取时,相应的泛音光谱会产生仅几kHz宽的谱线,从而可以直接检测氮化合物,而无需标记。尽管这种技术取得了成功,但由于大的四极相互作用产生的间接的二阶效应,“泛音”共振仍然被加宽。在这里,我们证明了另一个数量级的光谱分辨率可以通过使用双旋转。这使得14 N固态NMR谱线的宽度更接近通常与15 N的高分辨率固态NMR光谱学相关的区域,并证明了通过开发脉冲方法来抑制这些二阶效应可能实现的分辨率的改善。
Solid-state NMR transitions involving outer energy levels of the spin-1 14N nucleus are immune, to first order in perturbation theory, to the broadening caused by the nuclear quadrupole interaction. The corresponding overtone spectra, when acquired in conjunction with magic-angle sample spinning, result in lines, which are just a few kHz wide, permitting the direct detection of nitrogen compounds without the need for labeling. Despite the success of this technique, “overtone” resonances are still broadened due to indirect, second order effects arising from the large quadrupolar interaction. Here we demonstrate that another order of magnitude in spectral resolution may be gained by using double rotation. This brings the width of the 14N solid-state NMR lines much closer to the region commonly associated with high-resolution solid-state NMR spectroscopy of 15N and demonstrates the improvements in resolution that may be possible through the development of pulsed methodologies to suppress these second order effects.
固体 14N 泛音 NMR 光谱中的交叉偏振
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