Enhanced spectral resolution in immobilized peptides and proteins by combining chemical shift sum and difference spectroscopy

Journal of Magnetic Resonance

Volumn 159, Issue 2, 2002, Pages 243-249

  Luca, Sorin ^a   Baldus, Marc ^a  

^a MAX PLANCK INSTITUTE FOR BIOPHYSICAL CHEMISTRY   (Germany)

Author keywords

Chemical shifts; Correlation spectroscopy; Magic angle spinning; Protein backbone structure; Spectral resolution

Indexed keywords

PEPTIDE; PROTEIN; UBIQUITIN;

ARTICLE; CHEMISTRY; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE; PROTEIN SECONDARY STRUCTURE;

NUCLEAR MAGNETIC RESONANCE, BIOMOLECULAR; PEPTIDES; PROTEIN STRUCTURE, SECONDARY; PROTEINS; UBIQUITIN;

EID: 0036923765     PISSN: 10907807     EISSN: None     Source Type: Journal    
DOI: 10.1016/S1090-7807(02)00019-8     Document Type: Article

References (44)

1. H. Sternlicht, D. Wilson, Magnetic resonance studies of macromolecules. I aromatic-methyl interactions and helical structure effects in lysozyme, Biochemistry 6 (1967) 2881-2892.
2. J.L. Markley, D.H. Meadows, O. Jardetzky, Nuclear magnetic resonance studies of helix-coil transitions in polyamino acids, J. Mol. Biol. 27 (1967) 25-40.
3. K.H. Gross, H.R. Kalbitzer, Distribution of chemical-shifts in H-1 nuclear magnetic-resonance spectra of proteins, J. Magn. Reson. 76 (1988) 87-99.
4. S. Spera, A. Bax, Empirical correlation between protein backbone conformation and C-Alpha and C-Beta C-13 nuclear-magnetic-resonance chemical-shifts, J. Am. Chem. Soc. 113 (1991) 5490-5492.
5. H. Saito, Conformation-dependent C-13 chemical-shifts a new means of conformational characterization as obtained by high-resolution solid-state C-13 NMR, Magn. Reson. Chem. 24 (1986) 835-852.
6. H. Saito, S. Tuzi, A. Naito, Empirical versus nonempirical evaluation of secondary structure of fibrous and membrane proteins by solid-state NMR: A practical approach, Annu. Rep. NMR Spectrosc. 36 (1998) 79-121.
7. S. Luca, D.V. Filippov, J.H. van Boom, H. Oschkinat, H.J.M. de Groot, M. Baldus, Secondary chemical shifts in immobilized peptides and proteins: A qualitative basis for structure refinement under magic angle spinning, J. Biomol. NMR 20 (2001) 325-331.
8. E.R. Andrew, A. Bradbury, R.G. Eades, Nuclear magnetic resonance spectra from a crystal rotated at high speed, Nature 182 (1958) 1659.
9. S.K. Straus, T. Bremi, R.R. Ernst, Experiments and strategies for the assignment of fully C-13/N- 15-labelled polypeptides by solid state NMR, J. Biomol. NMR 12 (1998) 39-50.
10. M. Hong, Resonance assignment of C-13/N-15 labeled solid proteins by two- and three-dimensional magic-angle-spinning NMR, J. Biomol. NMR 15 (1999) 1-14.
11. A. McDermott, T. Polenova, A. Bockmann, K.W. Zilm, E.K. Paulsen, R.W. Martin, G.T. Montelione, Partial NMR assignments for uniformly (C-13, N-15)-enriched BPTI in the solid state, J. Biomol. NMR 16 (2000) 209-219.
12. J. Pauli, M. Baldus, B. van Rossum, H. de Groot, H. Oschkinat, Backbone and side-chain C-13 and N-15 signal assignments of the alpha-spectrin SH3 domain by magic angle spinning solid-state NMR at 17.6 tesla, Chembiochem 2 (2001) 272-281.
13. T.A. Egorova-Zachernyuk, J. Hollander, N. Fraser, P. Gast, A.J. Hoff, R. Cogdell, H.J.M. de Groot, M. Baldus, Heteronuclear 2D-correlations in a uniformly [C-13, N-15] labeled membrane-protein complex at ultra-high magnetic fields, J. Biomol. NMR 19 (2001) 243-253.
14. D.S. Wishart, B.D. Sykes, Chemical-shifts as a tool for structure determination, Methods Enzymol. 239 (1994) 363-392.
15. A.C. de Dios, J.G. Pearson, E. Oldfield, Secondary and tertiary structural effects on protein nmr chemical-shifts an abinitio approach, Science 260 (1993) 1491-1496.
16. D.S. Wishart, D.A. Case, Use of chemical shifts in macromolecular structure determination, Methods Enzymol. 338 (2001) 3-34.
17. G. Kozlov, I. Ekiel, N. Beglova, A. Yee, A. Dharamsi, A. Engel, N. Siddiqui, A. Nong, K. Gehring, Rapid fold and structure determination of the archaeal translation elongation factor 1 beta from Methanobacterium thermoautotrophicum, J. Biomol. NMR 17 (2000) 187-194.
18. A. Bax, R. Freeman, S.P. Kempsell, Natural abundance C-13-C-13 coupling observed via double- quantum coherence, J. Am. Chem. Soc. 102 (1980) 4849-4851.
19. E.M. Menger, S. Vega, R.G. Griffin, Observation of carbon carbon connectivities in rotating solids, J. Am. Chem. Soc. 108 (1986) 2215-2218.
20. M. Iwadate, T. Asakura, M.P. Williamson, C-alpha and C-beta carbon-13 chemical shifts in proteins from an empirical database, J. Biomol. NMR 13 (1999) 199-211.
21. L. Müller, Mapping of spin-spin coupling via zero-quantum coherence, J. Magn. Reson. 59 (1984) 326-331.
22. J.M. Koons, G.E. Pavlovskaya, A.A. Jones, P.T. Inglefield, Determination of interatomic distances by zero-quantum correlation spectroscopy under rotational-resonance conditions, J. Magn. Reson. 124 (1997) 499-502.
23. T.P. Spaniol, A. Kubo, T. Terao, Resolution enhancement of magic-angle spinning NMR spectra for paramagnetic solids by zero-quantum NMR, Mol. Phys. 96 (1999) 827-834.
24. R.R. Ernst, G. Bodenhausen, A. Wokaun, in: Principles of Nuclear Magnetic Resonance in One and Two Dimensions, Clarendon Press, Oxford, 1987.
25. G. Bodenhausen, R.L. Vold, R.R. Vold, Multiple quantum spin-echo spectroscopy, J. Magn. Reson. 37 (1980) 93-106.
26. M. Baldus, B.H. Meier, Total correlation spectroscopy in the solid state. The use of scalar couplings to determine the through-bond connectivity, J. Magn. Reson. Ser. A 121 (1996) 65-69.
27. M. Baldus, Correlation experiments for assignment and structure elucidation of immobilized polypeptides under magic angle spinning, Prog. Nucl. Magn. Reson. Spectrosc. 41 (2002) 1-47.
28. R. Verel, M. Baldus, M. Nijman, J.W.M. van Os, B.H. Meier, Adiabatic homonuclear polarization transfer in magic-angle-spinning solid-state NMR, Chem. Phys. Lett. 280 (1997) 31-39.
29. R. Verel, M. Baldus, M. Ernst, B.H. Meier, A homonuclear spin-pair filter for solid-state NMR based on adiabatic-passage techniques, Chem. Phys. Lett. 287 (1998) 421-428.
30. N. Bloembergen, On the interaction of Nuclear Spins in a crystalline lattice, Physica 15 (1949) 386-426.
31. T. Szyperski, G. Wider, J.H. Bushweller, K. Wüthrich, Reduced dimensionality in triple-resonance NMR experiments, J. Am. Chem. Soc. 115 (1993) 9307-9308.
32. T. Szyperski, B. Banecki, D. Braun, R.W. Glaser, Sequential resonance assignment of medium-sized N-15/C-13- labeled proteins with projected 4D triple resonance NMR experiments, J. Biomol. NMR 11 (1998) 387-405.
33. N.S. Astrof, C.E. Lyon, R.G. Griffin, Triple resonance solid state NMR experiments with reduced dimensionality evolution periods, J. Magn. Reson. 152 (2001) 303-307.
34. M. Hong, Solid-state NMR determination of C-13 alpha chemical shift anisotropies for the identification of protein secondary structure, J. Am. Chem. Soc. 122 (2000) 3762-3770.
35. S. Vijaykumar, C.E. Bugg, W.J. Cook, Structure of ubiquitin refined at 1.8 Å resolution, J. Mol. Biol. 194 (1987) 531-544.
36. G. Cornilescu, J.L. Marquardt, M. Ottiger, A. Bax, Validation of protein structure from anisotropic carbonyl chemical shifts in a dilute liquid crystalline phase, J. Am. Chem. Soc. 120 (1998) 6836-6837.
37. K. Schmidt-Rohr, Complete dipolar decoupling of 13C and its use in two-dimensional double-quantum solid-state NMR for determining polymer conformations, J. Magn. Reson. Ser. 131 (1998) 209-217.
38. F.M. Marassi, A simple approach to membrane protein secondary structure and topology based on NMR spectroscopy, Biophys. J. 80 (2001) 994-1003.
39. A. Lange, S. Luca, M. Baldus, Structural constraints from proton-mediated rare-spin correlation spectroscopy, J. Am. Chem. Soc. 124 (2002) 9704-9705.
40. G. Metz, X.L. Wu, S.O. Smith, Ramped-amplitude cross-polarization in magic-angle-spinning NMR, J. Magn. Reson. Ser. A 110 (1994) 219-227.
41. S. Hediger, B.H. Meier, N.D. Kurur, G. Bodenhausen, R.R. Ernst, NMR cross-polarization by adiabatic passage through the Hartmann-Hahn condition (APHH), Chem. Phys. Lett. 223 (1994) 283-288.
42. S.R. Hartmann, E.L. Hahn, Nuclear double resonance in rotating frame, Physical Review 128 (1962) 2042-2053.
43. A. Pines, M.G. Gibby, J.S. Waugh, Proton-enhanced NMR of dilute spins in solids, J. Chem. Phys. 59 (1973) 569-590.
44. A.E. Bennett, C.M. Rienstra, M. Auger, K.V. Lakshmi, R.G. Griffin, Heteronuclear decoupling in rotating solids, J. Chem. Phys. 103 (1995) 6951-6958.