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13C, 15N Resonance Assignment of Parts of the HET-s Prion Protein in its Amyloid Form

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Abstract

The partial 15N and 13C solid-state NMR resonance assignment of the HET-s prion protein fragment 218–289 in its amyloid form is presented. It is based on experiments measured at MAS frequencies in the range of 20–40 kHz using exclusively adiabatic polarization-transfer schemes. The resonance assignment within each residue is based on two-dimensional 13C––13C correlation spectra utilizing the DREAM mixing scheme. The sequential linking of the assigned residues used a set of two- and three-dimensional 15N––13C correlation experiments. Almost all cross peaks visible in the spectra are assigned, but only resonances from 43 of the 78 amino-acid residues could be detected. The missing residues are thought to be highly disordered and/or highly dynamic giving rise to broad resonance lines that escaped detection in the experiments applied. The line widths of the observed resonances are narrow and comparable to line widths observed in micro-crystalline samples. The 43 assigned residues are located in two fragments of about 20 residues.

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Abbreviations

2D:

two-dimensional

3D:

three-dimensional

APHH:

adiabatic-passage Hartmann-Hahn

CP:

cross polarization

CW:

continuous wave

DREAM:

dipolar recoupling enhanced by amplitude modulation

HORROR:

homonuclear rotary resonance

MAS:

magic angle spinning

NMR:

nuclear magnetic resonance

NOE:

nuclear overhauser effect

PDSD:

proton-driven spin diffusion

R2T:

rotational resonance tickling

RFDR:

radio-frequency driven spin diffusion

TPPI:

time-proportional phase increment

TRIS:

tris(hydroxymethyl)aminomethane

XiX:

X inverse X

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Authors and Affiliations

  1. Physical Chemistry, ETH Zurich, CH-8093, Zurich, Switzerland

    Ansgar B. Siemer, Matthias Ernst & Beat H. Meier

  2. Structural Biology Laboratory, The Salk Institute, La Jolla, CA, 92037, USA

    Christiane Ritter & Roland Riek

  3. Biomolecular Research, Structural Biology, Paul Scherrer Institut, CH-5232, Villigen, PSI, Switzerland

    Michel O. Steinmetz

Authors
  1. Ansgar B. Siemer
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  2. Christiane Ritter
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  3. Michel O. Steinmetz
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  4. Matthias Ernst
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  5. Roland Riek
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  6. Beat H. Meier
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Siemer, A.B., Ritter, C., Steinmetz, M.O. et al. 13C, 15N Resonance Assignment of Parts of the HET-s Prion Protein in its Amyloid Form. J Biomol NMR 34, 75–87 (2006). https://doi.org/10.1007/s10858-005-5582-7

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  • DOI: https://doi.org/10.1007/s10858-005-5582-7

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