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Stable-Isotope-Assisted NMR Studies on 13C-Enriched Sialyl Lewisx in Solution and Bound to E-Selectin

Lookup NU author(s): Professor Steve Homans

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Abstract

We report the determination of the solution structure and dynamics of ¹³C-enriched Neu5Acα2−3Galβ1−4(Fucα1−3)GlcNAc (sialyl Lewis^x), together with its bound-state conformation in association with E-selectin. The availability of ¹³C-enriched material enabled both the measurement of trans-glycosidic ¹³C−¹³C coupling constants as conformational probes in the tetrasaccharide and the application of three-dimensional nuclear Overhauser effect ¹³C−¹H 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 (¹³C) 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.

Publication metadata

Author(s): Harris R, Kiddle GR, Field RA, Milton MJ, Ernst B, Magnani JL, Homans SW

Publication type: Article

Publication status: Published

Journal: Journal of the American Chemical Society

Year: 1999

Volume: 121

Issue: 11

Pages: 2546-2551

Print publication date: 05/03/1999

ISSN (print): 0002-7863

ISSN (electronic): 1520-5126

Publisher: American Chemical Society

URL: http://dx.doi.org/10.1021/ja983423y

DOI: 10.1021/ja983423y

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