Stable-isotope-assisted NMR studies on 13C-enriched sialyl Lewisx in solution and bound to E-selectin
Stable-isotope-assisted NMR studies on 13C-enriched sialyl Lewisx in solution and bound to E-selectin
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DOI：
10.1021/ja983423y
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发表时间：
1999-03-24
影响因子：
15
通讯作者：
Homans, SW
中科院分区：
文献类型：
--
作者：
Harris, R;Kiddle, GR;Homans, SW
我们报道了C-1 - 3富集的Neu 5Ac α 2-3Gal β 1 - 4（Fuc α 1-3）GlcNAc（sialyl刘易斯（x））的溶液结构和动力学的测定，以及其与E-选择素的结合态构象。C-13富集材料的可用性使得能够测量作为四糖中的构象探针的反式糖苷C-13-C-13耦合常数，以及应用三维核Overhauser效应C-13-H-1异源单量子相关实验测量表征配体的结合态构象的分子内转移核Overhauser效应（TRNOE）。由第三（C-13）维提供的额外分散允许直接识别和定量这些TRNOE，并确定了几个TRNOE，以前没有报道。的配体的结合态构象，确定通过使用一个异向全弛豫矩阵分析的TRNOE数据，显着不同，从以前的研究报告。
We report the determination of the solution structure and dynamics of C-13-enriched Neu5Ac alpha 2-3Gal beta 1 -4(Fuc alpha 1-3)GlcNAc (sialyl Lewis(x)), together with its bound-state conformation in association with E-selectin. The availability of C-13-enriched material enabled both the measurement of trans-glycosidic C-13-C-13 coupling constants as conformational probes in the tetrasaccharide and the application of three-dimensional nuclear Overhauser effect C-13-H-1 heteronuclear single-quantum correlation experiments for the measurement of intramolecular transferred nuclear Overhauser effects (TRNOEs) characterizing the bound-state conformation of the ligand. The additional dispersion afforded by the third (C-13) dimension permitted straightforward identification and quantitation of these TRNOEs, and several TRNOEs were identified that had not previously been reported. The bound-state conformation of the ligand, determined by use of a heteronuclear full-relaxation matrix analysis of the TRNOE data, differs significantly from that reported in previous studies.