Improved resolution in 13C solid-state spectra through spin-state-selection

Journal of Magnetic Resonance

Volumn 184, Issue 2, 2007, Pages 322-329

  Verel, René ^a   Manolikas, Theofanis ^a   Siemer, Ansgar B ^a   Meier, Beat H ^a  

^a ETH ZURICH   (Switzerland)

Author keywords

High resolution; Solid state NMR; Spin state selection

Indexed keywords

NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; OPTICAL BEAM SPLITTERS; OPTICAL RESOLVING POWER; QUANTUM THEORY;

SPECTRAL RESOLUTION; SPIN-STATE-SELECTION;

SOLID STATE PHYSICS;

CARBON;

ALGORITHM; ARTICLE; CHEMICAL MODEL; CHEMISTRY; COMPUTER SIMULATION; EVALUATION; METHODOLOGY; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; SENSITIVITY AND SPECIFICITY; SPIN LABELING;

ALGORITHMS; CARBON ISOTOPES; COMPUTER SIMULATION; MAGNETIC RESONANCE SPECTROSCOPY; MODELS, CHEMICAL; SENSITIVITY AND SPECIFICITY; SPIN LABELS;

EID: 33846581838     PISSN: 10907807     EISSN: 10960856     Source Type: Journal    
DOI: 10.1016/j.jmr.2006.09.024     Document Type: Article

References (40)

1. Bennett A.E., Rienstra C.M., Auger M., Lakshmi K.V., and Griffin R.G. Heteronuclear decoupling in rotating solids. J. Chem. Phys. 103 (1995) 6951-6958
2. Fung B.M., Khitrin A.K., and Ermolaev K. An improved broadband decoupling sequence for liquid crystals and solids. J. Magn. Reson. 142 (2000) 97-101
3. Detken A., Hardy E.H., Ernst M., and Meier B.H. Simple and efficient decoupling in magic-angle spinning solid-state NMR: the XiX scheme. Chem. Phys. Lett. 356 (2002) 298-304
4. DePaepe G., Lesage A., and Emsley L. The performance of phase modulated heteronuclear dipolar decoupling schemes in fast magic-angle-spinning nuclear magnetic resonance experiments. J. Chem. Phys. 119 (2003) 4833-4841
5. Elena B., de Paepe G., and Emsley L. Direct spectral optimisation of proton-proton homonuclear dipolar decoupling in solid-state NMR. Chem. Phys. Lett. 398 (2004) 532-538
6. Pauli J., van Rossum B., Forster H., de Groot H.J., and Oschkinat M.H. Sample optimization and identification of signal patterns of amino acid side chains in 2D RFDR spectra of the alpha-spectrin SH3. J. Magn. Reson. 143 (2000) 411-416
7. Martin R.W., and Zilm K.W. Preparation of protein nanocrystals and their characterization by solid state NMR. J. Magn. Reson. 165 (2003) 162-174
8. Bermel W., Bertini I., Felli I.C., Piccioli M., and Pierattelli R. 13C-detected protonless NMR spectroscopy of proteins in solution. Prog. Nucl. Magn. Reson. Spectrosc. 48 (2006) 25-45
9. Straus S.K., Bremi T., and Ernst R.R. Resolution enhancement by homonuclear J decoupling in solid-state MAS NMR. Chem. Phys. Lett. 262 (1996) 709-715
10. 13C-enriched amino acids and proteins. J. Magn. Reson. 164 (2003) 270-285
11. β decoupling. J. Magn. Reson. Ser. B 113 (1996) 91-96
12. β decoupling. J. Magn. Reson. Ser. B 113 (1996) 190-194
13. 13C direct detection experiments on the paramagnetic oxidized monomeric copper, zinc superoxide dismutase. J. Am. Chem. Soc. 125 (2003) 16423-16429
14. 13C homonuclear scalar decoupling during acquisition. J. Magn. Reson. 172 (2005) 56-62
15. 13C-detected experiments with proteins and oligonucleotides. J. Biomol. NMR 31 (2005) 1-9
16. Meissner A., Schulte-Herbrüggen T., Briand J., and Sørensen O.W. Double spin-state-selective coherence transfer. Application for twodimensional selection of multiplet components with long transverse relaxation times. Mol. Phys. 95 (1998) 1137-1142
17. Nielsen N.C., Thogersen H., and Sørensen O.W. A systematic strategy for design of optimum coherent experiments applied to efficient interconversion of double- and single-quantum coherences in nuclear magnetic resonance. J. Chem. Phys. 105 (1996) 3962-3968
18. Sørensen M.D., Meissner A., and Sørensen O.W. Spin-state-selective coherence transfer via intermediate states of two-spin coherence in IS spin systems: Application to E.COSY-type measurement of J coupling constants. J. Biomol. NMR 10 (1997) 181-186
19. Verel R., van Beek J.D., and Meier B.H. INADEQUATE-CR experiments in the solid state. J. Magn. Reson. 140 (1999) 300-303
20. Ottiger M., Delaglio F., Marquardt J.L., Tjandra N., and Bax A. Measurement of dipolar couplings for methylene and methyl sites in weakly oriented macromolecules and their use in structure determination. J. Magn. Reson. 134 (1998) 365-369
21. Andersson P., Weigelt J., and Otting G. Spin-state selection filters for the measurement of heteronuclear one-bond coupling constants. J. Biomol. NMR 12 (1998) 435-441
22. Duma L., Hediger S., Lesage A., and Emsley L. Spin-state selection in solid-state NMR. J. Magn. Reson. 164 (2003) 187-195
23. Duma L., Hediger S., Brutscher B., Bockmann A., and Emsley L. Resolution enhancement in multidimensional solid-state NMR spectroscopy of proteins using spin-state selection. J. Am. Chem. Soc. 125 (2003) 11816-11817
24. Igumenova T.I., McDermott A.E., Zilm K.W., Martin R.W., Paulson E.K., and Wand A.J. Assignments of carbon NMR resonances for microcrystalline ubiquitin. J. Am. Chem. Soc. 126 (2004) 6720-6727
25. Ritter C., Maddelein M.L., Siemer A.B., Luhrs T., Ernst M., Meier B.H., Saupe S.J., and Riek R. Correlation of structural elements and infectivity of the HET-s prion. Nature 435 (2005) 844-848
26. Sørensen O.W., Eich G.W., Levitt M.H., Bodenhausen G., and Ernst R.R. Product operator formalism for the description of NMR pulse experiments. Prog. Nucl. Magn. Reson. Spectrosc. 16 (1984) 163-192
27. Hediger S., Meier B.H., and Ernst R.R. Adiabatic passage Hartmann-Hahn cross polarization in NMR under magic angle sample spinning. Chem. Phys. Lett. 240 (1995) 449
28. Lesage A., Auger C., Caldarelli S., and Emsley L. Determination of through-bond carbon-carbon connectivities in solid-state NMR using the INADEQUATE experiment. J. Am. Chem. Soc. 119 (1997) 7867-7868
29. Bax A., Freeman R., and Frenkiel T.A. An NMR technique for tracing out the carbon skeleton of an organic-molecule. J. Am. Chem. Soc. 103 (1981) 2102-2104
30. 13C coupling observed via double-quantum coherence. J. Am. Chem. Soc. 102 (1980) 4849-4851
31. Ernst R.R., Bodenhausen G., and Wokaun A. Principles of nuclear magnetic resonance in one and two dimensions (1987), Clarendon Press, Oxford
32. Brinkmann A., Eden M., and Levitt M.H. Synchronous helical pulse sequences in magic-angle spinning nuclear magnetic resonance: double quantum recoupling of multiple-spin systems. J. Chem. Phys. 112 (2000) 8539-8554
33. Levitt M.H. Symmetry-based pulse sequences in magic-angle spinning solid-state NMR, encyclopedia of NMR (2002), John Wiley & Sons, Ltd, Chichester
34. Igumenova T.I., Wand A.J., and McDermott A.E. Assignment of the backbone resonances for microcrystalline ubiquitin. J. Am. Chem. Soc. 126 (2004) 5323-5331
35. 13C labeled ubiquitin: spectral simplification and stereospecific assignment of isopropyl groups. J. Biomol. NMR 35 (2006) 167-173
36. Siemer A.B., Ritter C., Ernst M., Riek R., and Meier B.H. High-resolution solid-state NMR spectroscopy of the prion protein HET-s in its amyloid conformation. Angew. Chem. Int. Ed. 44 (2005) 2441-2444
37. A.B. Siemer, A.A. Arnold, C. Ritter, T. Westfeld, M. Ernst, R. Riek, B.H. Meier, Observation of highly flexible residues in amyloid fibrils of the HET-s Prion. J. Am. Chem. Soc. (2006) (early publication on the web).
38. 15N resonance assignment of parts of the HET-s prion protein in its amyloid form. J. Biomol. NMR 34 (2006) 75-87
39. Emsley L., and Bodenhausen G. Self-refocusing effect of 270° Gaussian pulses. Applications to selective two-dimensional exchange spectroscopy. J. Magn. Reson. 82 (1989) 211-221
40. MatNMR is a toolbox for processing NMR/EPR data under Matlab and can be freely downloaded at http://matnmr.sourceforge.net.