Three-dimensional structure determination of a uniformly labeled molecule by frequency-selective dipolar recoupling under magic-angle spinning

被引：35

作者：

Nomura, K

Takegoshi, K ^{[1
]}

Terao, T

Uchida, K

Kainosho, M

机构：

[1] Kyoto Univ, Grad Sch Sci, Dept Chem, Kyoto 6068502, Japan

[2] Teikyo Univ, Sch Sci & Engn, Dept Biosci, Utsunomiya, Tochigi 3208551, Japan

[3] Tokyo Metropolitan Univ, Grad Sch Sci, Dept Chem, Tokyo 1920397, Japan

来源：

JOURNAL OF BIOMOLECULAR NMR | 2000年 / 17卷 / 02期

基金：

日本学术振兴会;

关键词：

MAS; R2TR; selective dipolar recoupling; solid state NMR; three-dimensional structure determination; uniformly labeled powder sample;

D O I：

10.1023/A:1008398906753

中图分类号：

Q5 [生物化学]; Q7 [分子生物学];

学科分类号：

071010 ; 081704 ;

摘要：

The complete three-dimensional (3D) structure of a glycylisoleucine (Gly-Ile) molecule was determined by individually measuring six dihedral angles with a frequency-selective homonuclear dipolar recoupling method, R2TR (rotational resonance in the tilted rotating frame), using a powder sample of diluted uniformly 13,15-labeled Gly-Ile. Each dihedral angle was obtained by recoupling a dipolar interaction between three or four bonds distant spins concerned or observing a dipolar correlation 2D powder pattern. The 3D structure of a Gly-Ile molecule was also determined by X-ray crystallography, and a good agreement with the NMR result was obtained. The results demonstrate that the R2TR method in a uniformly labeled powder sample can provide the 3D structure without the need to prepare a lot of selectively labeled samples.

引用

页码：111 / 123

页数：13

共 36 条

[1] NUCLEAR CROSS-RELAXATION INDUCED BY SPECIMEN ROTATION [J].