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Observation of H-1-C-13 and H-1-H-1 proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS

文献类型：期刊论文

作者Li, Shenhui1; Trebosc, Julien2; Lafon, Olivier2; Zhou, Lei1; Shen, Ming2,3,4; Pourpoint, Frederique2; Amoureux, Jean-Paul2,3,4; Deng, Feng1
刊名JOURNAL OF MAGNETIC RESONANCE
出版日期2015-02-01
卷号251页码:36-42
关键词Solid state NMR Paramagnetic solid 2D correlation spectra Chemical shift assignment
英文摘要The assignment of NMR signals in paramagnetic solids is often challenging since: (i) the large paramagnetic shifts often mask the diamagnetic shifts specific to the local chemical environment, and (ii) the hyperfine interactions with unpaired electrons broaden the NMR spectra and decrease the coherence lifetime, thus reducing the efficiency of usual homo- and hetero-nuclear NMR correlation experiments. Here we show that the assignment of H-1 and C-13 signals in isotopically unmodified paramagnetic compounds with moderate hyperfine interactions can be facilitated by the use of two two-dimensional (2D) experiments: (i) H-1-C-13 correlations with H-1 detection and (ii) H-1-H-1 double-quantum <-> single-quantum correlations. These methods are experimentally demonstrated on isotopically unmodified copper (II) complex of L-alanine at high magnetic field (18.8 T) and ultra-fast Magic Angle Spinning (MAS) frequency of 62.5 kHz. Compared to C-13 detection, we show that H-1 detection leads to a 3-fold enhancement in sensitivity for H-1-C-13 2D correlation experiments. By combining H-1-C-13 and H-1-H-1 2D correlation experiments with the analysis of C-13 longitudinal relaxation times, we have been able to assign the H-1 and C-13 signals of each L-alanine ligand. (C) 2014 Elsevier Inc. All rights reserved.
WOS标题词Science & Technology ; Life Sciences & Biomedicine ; Physical Sciences ; Technology
类目[WOS]Biochemical Research Methods ; Physics, Atomic, Molecular & Chemical ; Spectroscopy
研究领域[WOS]Biochemistry & Molecular Biology ; Physics ; Spectroscopy
关键词[WOS]ANGLE-SPINNING NMR ; STATE C-13 NMR ; SENSITIVITY ENHANCEMENT ; STRUCTURAL RESTRAINTS ; CRYSTAL-STRUCTURE ; SPECTROSCOPY ; COMPLEXES ; PROTEINS ; ASSIGNMENT ; METALLOPROTEINS
收录类别SCI
语种英语
WOS记录号WOS:000351252700006
公开日期2015-07-14
源URL[http://ir.wipm.ac.cn/handle/112942/1041]  
专题武汉物理与数学研究所_磁共振应用研究部
作者单位1.Chinese Acad Sci, Wuhan Inst Phys & Math, Natl Ctr Magnet Resonance Wuhan, State Key Lab Magnet Resonance & Atom & Mol Phys, Wuhan 430071, Peoples R China
2.Univ Lille 1, Univ Lille North France, Unit Catalysis & Chem Solids, CNRS UMR 8181,ENSCL, F-59652 Villeneuve Dascq, France
3.E China Normal Univ, Dept Phys, Shanghai 200062, Peoples R China
4.E China Normal Univ, Shanghai Key Lab Magnet Resonance, Shanghai 200062, Peoples R China
推荐引用方式
GB/T 7714		 Li, Shenhui,Trebosc, Julien,Lafon, Olivier,et al. Observation of H-1-C-13 and H-1-H-1 proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS[J]. JOURNAL OF MAGNETIC RESONANCE,2015,251:36-42.
APA Li, Shenhui.,Trebosc, Julien.,Lafon, Olivier.,Zhou, Lei.,Shen, Ming.,...&Deng, Feng.(2015).Observation of H-1-C-13 and H-1-H-1 proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS.JOURNAL OF MAGNETIC RESONANCE,251,36-42.
MLA Li, Shenhui,et al."Observation of H-1-C-13 and H-1-H-1 proximities in a paramagnetic solid by NMR at high magnetic field under ultra-fast MAS".JOURNAL OF MAGNETIC RESONANCE 251(2015):36-42.

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来源：武汉物理与数学研究所

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