3D accordion spectroscopy for measuring 15N and 13CO relaxation rates in poorly resolved NMR spectra.
An experimental approach for the measurement of nuclear magnetic spin relaxation rate constants that combines triple-resonance techniques and accordion spectroscopy is described. Pulse sequences are discussed for the measurement of backbone 15N and 13CO R1 relaxation rate constants. The three-dimensional HNCO triple-resonance technique is employed to gain improved spectral resolution over conventional two-dimensional methods by frequency labeling both the 15N and 13CO spins. Accordion spectroscopy is used to reduce the dimensionality of the relaxation experiment. The "negative-time accordion" approach (A. M. Mandel and A. G. Palmer (1994), J. Magn. Reson. A 110, 62-72) is used for extracting rate constants from the t1 interferograms. The experiments are demonstrated using a 13C/15N isotopically enriched sample of the third fibronectin type III domain of human tenascin.
Carr
P A
PA
Department of Biochemistry and Molecular Biophysics, Columbia University, New York, New York 10032, USA.
Fearing
D A
DA
Palmer
A G
AG
D000465:Algorithms; D000596:Amino Acids / Q000032:analysis; D002244:Carbon / Q000032:analysis*; D002247:Carbon Isotopes; D002248:Carbon Monoxide / Q000032:analysis*; D004578:Electron Spin Resonance Spectroscopy; D005353:Fibronectins / Q000032:analysis*; D006801:Humans; D007368:Interferometry; D009682:Magnetic Resonance Spectroscopy; D009584:Nitrogen / Q000032:analysis*; D009587:Nitrogen Isotopes; D013057:Spectrum Analysis / Q000379:methods; D019063:Tenascin / Q000032:analysis*
D000596:Amino Acids; D002247:Carbon Isotopes; D005353:Fibronectins; D009587:Nitrogen Isotopes; D019063:Tenascin; D002244:Carbon; D002248:Carbon Monoxide; D009584:Nitrogen