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Indirect detection of nitrogen-14 in solids via protons by nuclear magnetic resonance spectroscopy

机译:核磁共振波谱间接检测质子固体中的氮14

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This Communication describes the indirect detection of N-14 nuclei (spin I = 1) in solids by nuclear magnetic resonance (NMR) spectroscopy. The two-dimensional correlation method used here is closely related to the heteronuclear multiple quantum correlation (HMQC) experiment introduced in 1979 to study molecules in liquids, which has recently been used to study solids spinning at the magic angle. The difference is that the coherence transfer from neighboring H-1 nuclei to N-14 is achieved via a combination of J couplings and residual dipolar splittings (RDS). Projections of the two-dimensional correlation spectra onto the N-14 dimension yield powder patterns which reflect the N-14 quadrupolar interaction. In contrast to the indirect detection of N-14 via 13 C nuclei that was recently demonstrated [Gan, J. Am. Chem. Soc. 128 (2006) 6040; Cavadini et. al., J. Am. Chem. Soc., 128 (2006) 7706], this approach may benefit from enhanced sensitivity, and does not require isotopic enrichment in C-13, although the H-1 line-widths may have to be reduced upon selective deuteration. (c) 2006 Elsevier Inc. All rights reserved.
机译:该来文描述了通过核磁共振(NMR)光谱法间接检测固体中的N-14核(Spin I = 1)。此处使用的二维相关方法与1979年引入的异核多量子相关(HMQC)实验密切相关,该实验用于研究液体中的分子,最近已用于研究以魔角旋转的固体。区别在于,通过J耦合和残余偶极分裂(RDS)的结合,可以实现从相邻H-1原子核到N-14的相干转移。二维相关光谱在N-14维上的投影产生了反映N-14四极相互作用的粉末图案。与最近证明的通过13 C核间接检测N-14形成对比[Gan,J. Am。化学Soc。 128(2006)6040;卡瓦迪尼等等,J。Am。化学Soc。,128(2006)7706],这种方法可能受益于增强的灵敏度,并且不需要C-13中的同位素富集,尽管在选择性氘化后可能必须减小H-1线宽。 (c)2006 Elsevier Inc.保留所有权利。

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