Antonijevic Sasa, Halpern-Manners Nicholas
Department of Chemistry, University of California, Berkeley, 1 Cyclotron Road Building 11-D64, Berkeley, CA 94720, USA.
Solid State Nucl Magn Reson. 2008 May;33(4):82-7. doi: 10.1016/j.ssnmr.2008.04.006. Epub 2008 Apr 20.
A novel two-dimensional nuclear magnetic resonance (NMR) experiment is proposed for indirect observation of 14N nuclei in various types of nitrogen-containing solids. In a method somewhat similar to the heteronuclear single-quantum correlation (HSQC) experiment widely used for protein structure determination in solutions, this technique correlates spin S=1/2 nuclei, e.g., 1H, 13C, with the 14N spin I=1 nucleus in solids. The present experiment, however, transfers coherence from neighboring 1H or 13C nuclei to 14N via a combination of J-couplings and residual dipolar splittings (RDS). Projections of the two-dimensional NMR spectra onto the 14N dimension yield powder patterns that reflect the 14N quadrupolar interaction, which can be used to study molecular structure and dynamics. Indirect detection of amide nitrogen-14 via 1H and 13C is shown experimentally on a model compound of N-acetyl-glycine.
提出了一种新型二维核磁共振(NMR)实验,用于间接观测各类含氮固体中的¹⁴N核。在一种与广泛用于溶液中蛋白质结构测定的异核单量子相关(HSQC)实验有些类似的方法中,该技术将自旋S = 1/2核(如¹H、¹³C)与固体中的¹⁴N自旋I = 1核相关联。然而,本实验通过J耦合和残余偶极分裂(RDS)的组合,将相干性从相邻的¹H或¹³C核转移到¹⁴N。二维NMR谱在¹⁴N维度上的投影产生反映¹⁴N四极相互作用的粉末图谱,可用于研究分子结构和动力学。在N - 乙酰甘氨酸的模型化合物上通过实验展示了经由¹H和¹³C对酰胺氮 - 14的间接检测。
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