3D 15N-13C-13C chemical shift correlation spectroscopy in rotating solids

B. Q. Sun, C. M. Rienstra, P. R. Costa, J. R. Williamson, R. G. Griffin

Research output: Contribution to journalArticle

Abstract

We describe 3D solid state MAS NMR experiments which separate chemical shifts in one 15N and two 13C dimensions. The polarization transfer from 1H to 15N and subsequently to 13C, is accomplished with recently developed techniques which overcome the shortcomings of constant amplitude Hartmann-Hahn cross polarization. Homonuclear (13C-13C) recoupling is performed with the MELODRAMA sequence. In the 2D 13C-13C spectra of adenosine monophosphate (AMP), successive MELODRAMA transfers propagate 13C magnetization around the five 13C's of the ribose ring, and the cross-peaks from successive transfer steps exhibit the negative/positive/negative... pattern expected from the double quantum polarization transfer process. The 3D 15N-13C-13C spectrum of unifonnly-15N,13C-labeled histidine consists of 13C-13C planes separated by 15N chemical shifts. The 2D planes are asymmetric since in many cases the polarization giving rise to each cross-peak originates on only one nuclear spin of the coupled pair. 3D 15N-13C-13C spectra of this type should be useful for dispersing overlapping spectra of peptides, proteins, and nucleic acids.

Original languageEnglish (US)
Pages (from-to)8540-8546
Number of pages7
JournalJournal of the American Chemical Society
Volume119
Issue number36
DOIs
StatePublished - Sep 10 1997
Externally publishedYes

Fingerprint

Chemical shift
polarization
spectroscopy
Spectroscopy
Polarization
MAS
Ribose
Nucleic acids
nucleic acid
Adenosine Monophosphate
Histidine
magnetization
peptide
Nucleic Acids
Peptides
nuclear magnetic resonance
Magnetization
Nuclear magnetic resonance
Proteins
protein

ASJC Scopus subject areas

  • Catalysis
  • Chemistry(all)
  • Biochemistry
  • Colloid and Surface Chemistry

Cite this

3D 15N-13C-13C chemical shift correlation spectroscopy in rotating solids. / Sun, B. Q.; Rienstra, C. M.; Costa, P. R.; Williamson, J. R.; Griffin, R. G.

In: Journal of the American Chemical Society, Vol. 119, No. 36, 10.09.1997, p. 8540-8546.

Research output: Contribution to journalArticle

Sun, B. Q. ; Rienstra, C. M. ; Costa, P. R. ; Williamson, J. R. ; Griffin, R. G. / 3D 15N-13C-13C chemical shift correlation spectroscopy in rotating solids. In: Journal of the American Chemical Society. 1997 ; Vol. 119, No. 36. pp. 8540-8546.
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