Recent advances in solid-state NMR spectroscopy of quadrupolar nuclei

被引:107
作者
Ashbrook, Sharon E. [1 ,2 ]
机构
[1] Univ St Andrews, Sch Chem, St Andrews KY16 9ST, Fife, Scotland
[2] Univ St Andrews, EaStCHEM, St Andrews KY16 9ST, Fife, Scotland
基金
英国工程与自然科学研究理事会;
关键词
HYPERBOLIC SECANT PULSES; MAGNETIC-RESONANCE-SPECTROSCOPY; DOUBLE-ROTATION NMR; ANGLE-SPINNING NMR; TRANSITION MAS NMR; LOW-GAMMA NUCLEI; SENSITIVITY ENHANCEMENT; MULTIPLE-QUANTUM; MQMAS NMR; 1ST-PRINCIPLES CALCULATIONS;
D O I
10.1039/b907183k
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
Nuclear magnetic resonance (NMR) spectroscopy of quadrupolar nuclei (i. e., those with a spin quantum number I > 1/2) has always been viewed as "difficult'' owing to the presence of an anisotropic broadening arising from the interaction of the nuclear electric quadrupole moment with the electric field gradient. This quadrupolar interaction can be considerable, resulting in broadening of the spectral resonances often over many MHz. Furthermore, magic-angle spinning (MAS), a conventional approach for increasing the resolution in solid-state NMR, is often unable to remove the broadening completely and high-resolution spectra are generally not obtained. Despite the vast amount of information contained in the anisotropic linewidths and lineshapes, the resolution and sensitivity challenges have, until recently, somewhat limited the application of solid-state NMR for quadrupolar nuclei. In general, structural information, such as that obtained through recoupling techniques or from two-dimensional correlation spectroscopy, is much more difficult to extract easily and accurately. However, recent advances in magnet design, probe hardware and pulse sequence development have significantly improved the ease with which quadrupolar spins can be studied and high-resolution spectra can be obtained, and recent applications are beginning to exploit the wealth of information available. In this discussion, we highlight just a few of the recent developments in this area, including new state-of-the art correlation experiments, the expanding study of nuclei with low gyromagnetic ratio, g, the increasing application of first-principles calculations in the solid state, and methods which exploit the quadrupolar broadening to provide information on dynamics. Whilst not a complete review, it is hoped that this brief overview of some of the more exciting recent developments can provide insight into the challenges, and the rewards, involved in the NMR study of quadrupolar nuclei.
引用
收藏
页码:6892 / 6905
页数:14
相关论文
共 50 条
  • [21] Spectral editing in, solid-state MAS NMR of quadrupolar nuclei using selective satellite inversion
    Dey, Krishna K.
    Prasad, S.
    Ash, Jason T.
    Deschamps, Michael
    Grandinetti, Philip J.
    JOURNAL OF MAGNETIC RESONANCE, 2007, 185 (02) : 326 - 330
  • [22] Solid-state NMR spectroscopy
    Reif, Bernd
    Ashbrook, Sharon E.
    Emsley, Lyndon
    Hong, Mei
    NATURE REVIEWS METHODS PRIMERS, 2021, 1 (01):
  • [23] Structural information from quadrupolar nuclei in solid state NMR
    Ashbrook, Sharon E.
    Duer, Melinda J.
    CONCEPTS IN MAGNETIC RESONANCE PART A, 2006, 28A (03) : 183 - 248
  • [24] Nuances of multi-quantum excitation in solid state NMR of quadrupolar nuclei
    Srivastava, Deepansh
    Ramachandran, Ramesh
    RSC ADVANCES, 2013, 3 (47) : 25231 - 25236
  • [25] Signal enhancement of J-HMQC experiments in solid-state NMR involving half-integer quadrupolar nuclei
    Wang, Qiang
    Trebosc, Julien
    Li, Yixuan
    Xu, Jun
    Hu, Bingwen
    Feng, Ningdong
    Chen, Qun
    Lafon, Oliver
    Amoureux, Jean-Paul
    Deng, Feng
    CHEMICAL COMMUNICATIONS, 2013, 49 (59) : 6653 - 6655
  • [26] Solid-State NMR Spectroscopy of Proteins
    Mueller, Henrik
    Etzkorn, Manuel
    Heise, Henrike
    MODERN NMR METHODOLOGY, 2013, 335 : 121 - 156
  • [27] I-STMAS, a new high-resolution solid-state NMR method for half-integer quadrupolar nuclei
    Amoureux, JP
    Morais, C
    Trebosc, J
    Rocha, J
    Fernandez, C
    SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2003, 23 (04) : 213 - 223
  • [28] On the applicability of cosine-modulated pulses for high-resolution solid-state NMR of quadrupolar nuclei with spin > 3/2
    Sasaki, Akiko
    Trebosc, Julien
    Nagashima, Hiroki
    Amoureux, Jean -Paul
    SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2023, 125
  • [29] Protons as Versatile Reporters in Solid-State NMR Spectroscopy
    Vasa, Suresh K.
    Rovo, Petra
    Linser, Rasmus
    ACCOUNTS OF CHEMICAL RESEARCH, 2018, 51 (06) : 1386 - 1395
  • [30] Correlation NMR spectroscopy involving quadrupolar nuclei
    Amoureux, J. P.
    Trebosc, J.
    Delevoye, L.
    Lafon, O.
    Hu, B.
    Wang, Q.
    SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2009, 35 (01) : 12 - 18