Analysis and elimination of artifacts in indirect covariance NMR spectra via unsymmetrical processing

Indirect covariance NMR offers an alternative method of extracting spin–spin connectivity information via the conversion of an indirect‐detection heteronuclear shift‐correlation data matrix to a homonuclear data matrix. Using an IDR (inverted direct response)‐HSQC‐TOCSY spectrum as a starting point...

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Veröffentlicht in:Magnetic resonance in chemistry 2005-12, Vol.43 (12), p.999-1007
Hauptverfasser: Blinov, Kirill A., Larin, Nicolay I., Kvasha, Mikhail P., Moser, Arvin, Williams, Antony J., Martin, Gary E.
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Sprache:eng
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Zusammenfassung:Indirect covariance NMR offers an alternative method of extracting spin–spin connectivity information via the conversion of an indirect‐detection heteronuclear shift‐correlation data matrix to a homonuclear data matrix. Using an IDR (inverted direct response)‐HSQC‐TOCSY spectrum as a starting point for the indirect covariance processing, a spectrum that can be described as a carbon–carbon COSY experiment is obtained. These data are analogous to the autocorrelated 13C–13C double quantum INADEQUATE experiment except that the indirect covariance NMR spectrum establishes carbon–carbon connectivities only between contiguous protonated carbons. Cyclopentafuranone and the complex polynuclear heteroaromatic naphtho[2′,1′:5,6]‐naphtho[2′,1′:4,5]thieno[2,3‐c]quinoline are used as model compounds. The former is a straightforward example because of its well‐resolved proton spectrum, while the latter, which has considerable resonance overlap in its congested proton spectrum, gives rise to two types of artifact responses that must be considered when using the indirect covariance NMR method. Copyright © 2005 John Wiley & Sons, Ltd.
ISSN:0749-1581
1097-458X
DOI:10.1002/mrc.1674