Get 20M+ Full-Text Papers For Less Than $1.50/day. Start a 7-Day Trial for You or Your Team.

Learn More →

13C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or residual dipolar coupling constants

13C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or... The sensitivity of cryoprobes, which are rapidly becoming available, means that the measurement of coupling constants involving 13C, 13C pairs at the natural abundance of 13C can now, in principle, be done by using tens rather then hundreds of milligrams of compounds. However, a robust method that would yield reliable values of small long‐range carbon‐‐carbon coupling constants is still missing. In this Communication, we describe a novel 13C–detected incredible natural‐abundance double‐quantum transfer experiment (INADEQUATE) experiment for simultaneous correlation of one‐bond and long‐range 13C13C pairs and the measurement of both types of coupling constants in 13C natural abundance samples. This method yields accurate values of one‐bond and long‐range coupling constants by manipulation of pure phase in‐phase (IP) and antiphase (AP) doublets, and is referred to as 13C‐detected IPAP‐INADEQUATE. It is illustrated by the measurement of interglycosidic 3JCCOC coupling constants in a disaccharide molecule providing important information about the conformation of the glycosidic linkage. Owing to the simplicity of INADEQUATE spectra the carbon–carbon coupling constants are particularly suitable for studies of partially oriented molecules through the measurement of carbon–carbon residual dipolar couplings (RDCs). An example of this approach is presented. We expect the method to find a variety of applications in the conformational analysis of small molecules, determination of diastereoisomers and enantiomers, and studies of molecules in aligned media. Copyright © 2007 John Wiley & Sons, Ltd. http://www.deepdyve.com/assets/images/DeepDyve-Logo-lg.png Magnetic Resonance in Chemistry Wiley

13C‐detected IPAP‐INADEQUATE for simultaneous measurement of one‐bond and long‐range scalar or residual dipolar coupling constants

Jin, Lan; Uhrín, Dušan
Magnetic Resonance in Chemistry , Volume 45 (8) – Jan 1, 2007
Download PDF
6 pages

Loading next page...
 
/lp/wiley/13c-detected-ipap-inadequate-for-simultaneous-measurement-of-one-bond-ZmdSDS6GCO

References (36)

Publisher
Wiley
Copyright
Copyright © 2007 Wiley Subscription Services
ISSN
0749-1581
eISSN
1097-458X
DOI
10.1002/mrc.2031
pmid
17559162
Publisher site
See Article on Publisher Site

Abstract

The sensitivity of cryoprobes, which are rapidly becoming available, means that the measurement of coupling constants involving 13C, 13C pairs at the natural abundance of 13C can now, in principle, be done by using tens rather then hundreds of milligrams of compounds. However, a robust method that would yield reliable values of small long‐range carbon‐‐carbon coupling constants is still missing. In this Communication, we describe a novel 13C–detected incredible natural‐abundance double‐quantum transfer experiment (INADEQUATE) experiment for simultaneous correlation of one‐bond and long‐range 13C13C pairs and the measurement of both types of coupling constants in 13C natural abundance samples. This method yields accurate values of one‐bond and long‐range coupling constants by manipulation of pure phase in‐phase (IP) and antiphase (AP) doublets, and is referred to as 13C‐detected IPAP‐INADEQUATE. It is illustrated by the measurement of interglycosidic 3JCCOC coupling constants in a disaccharide molecule providing important information about the conformation of the glycosidic linkage. Owing to the simplicity of INADEQUATE spectra the carbon–carbon coupling constants are particularly suitable for studies of partially oriented molecules through the measurement of carbon–carbon residual dipolar couplings (RDCs). An example of this approach is presented. We expect the method to find a variety of applications in the conformational analysis of small molecules, determination of diastereoisomers and enantiomers, and studies of molecules in aligned media. Copyright © 2007 John Wiley & Sons, Ltd.

Journal

Magnetic Resonance in Chemistry – Wiley

Published: Jan 1, 2007

Keywords: ; ; ; ; ; ; ; ;

There are no references for this article.