Proton-nitrogen-14 overtone two-dimensional correlation NMR spectroscopy of solid-sample at very fast magic angle sample spinning

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• 作者：Yusuke Nishiyama^a ; ^{yunishiy@jeol.co.jp} ; Michal Malon^a ; Zhehong Gan^b ; Yuki Endo^a ; Takahiro Nemoto^a
• 关键词：Solid-state NMR ; 14N overtone ; Very fast MAS ; HMQC ; 0.75  ; mm MAS
• 刊名：Journal of Magnetic Resonance
• 出版年：2013
• 出版时间：May, 2013
• 年：2013
• 卷：230
• 期：Complete
• 页码：160-164
• 全文大小：626 K

文摘

¹H-¹⁴N overtone (OT) heteronuclear multiple quantum coherence (HMQC) experiment at very fast magic angle spinning (MAS) is reported. The ¹⁴N OT coherence is excited and reconverted by ¹⁴N OT pulses at twice the ¹⁴N Larmor frequency. The OT coherence is free from the first order quadrupolar broadening. MAS further removes the broadening due to chemical shift anisotropy (CSA). With a small 0.75 mm MAS rotor and coil system, very fast MAS up to 90 kHz and very strong rf field are achieved, enhancing the sensitivity of indirect ¹⁴N OT observation via protons. In comparison with ¹H-¹⁴N double-quantum HMQC, an enhancement factor of 1.8 is obtained for glycine with the ¹⁴N OT irradiation. The bandwidth in the ¹⁴N OT dimension is limited due to long ¹⁴N OT pulses.