Practical guides for 1H detected solid-state NMR under fast MAS for small molecules

被引:12
作者
Nishiyama, Yusuke [1 ,2 ]
Duong, Nghia Tuan [1 ,3 ]
机构
[1] RIKEN, RIKEN JEOL Collaborat Ctr, Nanocrystallog Unit, Yokohama, Kanagawa 2300045, Japan
[2] JEOL RESONANCE Inc, Akishima, Tokyo 1968558, Japan
[3] Aix Marseille Univ, CNRS, ICR, F-13397 Marseille, France
来源
JOURNAL OF MAGNETIC RESONANCE OPEN | 2022年 / 10-11卷
关键词
Fast MAS; 1H detection; Solid-state NMR; Heteronuclear correlation; Homonuclear correlation; ANGLE-SPINNING NMR; 100 KHZ MAS; MAGIC-ANGLE; CORRELATION SPECTROSCOPY; CROSS-POLARIZATION; SENSITIVITY ENHANCEMENT; DISTANCE MEASUREMENTS; INVERSE DETECTION; H DISTANCES; C-13; NMR;
D O I
10.1016/j.jmro.2022.100062
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
This primer article introduces a practical guide for setting up 1H detection solid-state NMR experiments under fast MAS conditions for small molecules. Sample independent adjustment/calibration including magic angle adjustment, shimming, radio-frequency field calibration, Hartmann-Hahn matching adjustments, and 1H heter-onuclear decoupling are demonstrated. Experimental setups which depend on samples are also shown for 1H NMR, 1H -1H homonuclear correlation measurements, and 1H-X heteronuclear correlation/distance measure-ments. Information obtained from each experiment is also highlighted.
引用
收藏
页数:23
相关论文
共 133 条
[71]   Satellite and central transitions selective 1H/{27Al} D-HMQC experiments at very fast MAS for quadrupolar couplings determination [J].
Nghia Tuan Duong ;
Nishiyama, Yusuke .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2017, 84 :83-88
[72]   Analysis of large-anisotropy-spin recoupling pulses for distance measurement under magic-angle spinning NMR shows the superiority and robustness of a phase modulated saturation pulse [J].
Nimerovsky, E. ;
Makrinich, M. ;
Goldbourt, A. .
JOURNAL OF CHEMICAL PHYSICS, 2017, 146 (12)
[73]   Phase-modulated LA-REDOR: A robust, accurate and efficient solid-state NMR technique for distance measurements between a spin-1/2 and a quadrupole spin [J].
Nimerovsky, Evgeny ;
Gupta, Rupal ;
Yehl, Jenna ;
Li, Mingyue ;
Polenova, Tatyana ;
Goldbourt, Amir .
JOURNAL OF MAGNETIC RESONANCE, 2014, 244 :107-113
[74]   Supplemental Shimming for HR-μMAS NMR Spectroscopy [J].
Nishiyama, Masahide ;
Lucas-Torres, Covadonga ;
Piao, Renzhong ;
Yanagisawa, Yoshinori ;
Nishiyama, Yusuke ;
Wong, Alan .
APPLIED MAGNETIC RESONANCE, 2019, 50 (11) :1305-1313
[75]   Accurate NMR determination of C-H or N-H distances for unlabeled molecules [J].
Nishiyama, Y. ;
Malon, M. ;
Potrzebowski, M. J. ;
Paluch, P. ;
Amoureux, J. P. .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2016, 73 :15-21
[76]  
Nishiyama Y., 2017, Solid-State NMR under Ultrafast MAS Rate of 40-120 KHz, DOI [10.1007/978-981-10-5966-7_6, DOI 10.1007/978-981-10-5966-7_6]
[77]   Efficient symmetry-based γ-encoded DQ recoupling sequences for suppression of t1-noise in solid-state NMR spectroscopy at fast MAS [J].
Nishiyama, Yusuke ;
Agarwal, Vipin ;
Zhang, Rongchun .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2021, 114
[78]   t1-Noise Suppression by γ-Free Recoupling Sequences in Solid-State NMR for Structural Characterization of Fully Protonated Molecules at Fast MAS [J].
Nishiyama, Yusuke ;
Agarwal, Vipin ;
Zhang, Rongchun .
JOURNAL OF PHYSICAL CHEMISTRY C, 2020, 124 (48) :26332-26343
[79]  
Nishiyama Y, 2019, NEW DEV NMR, V20, P506
[80]   Fast magic-angle sample spinning solid-state NMR at 60-100 kHz for natural abundance samples [J].
Nishiyama, Yusuke .
SOLID STATE NUCLEAR MAGNETIC RESONANCE, 2016, 78 :24-36