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Broadband homonuclear chemical shift correlation at high MAS frequencies: a study of tanh/tan adiabatic RF pulse schemes without \({^{{\bf 1}}\hbox{{\bf H}}}\) decoupling during mixing

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Abstract

At high magic angle spinning (MAS) frequencies the potential of tanh/tan adiabatic RF pulse schemes for 13C chemical shift correlation without 1H decoupling during mixing has been evaluated. It is shown via numerical simulations that a continuous train of adiabatic 13C inversion pulses applied at high RF field strengths leads to efficient broadband heteronuclear decoupling. It is demonstrated that this can be exploited effectively for generating through-bond and through-space, including double-quantum, correlation spectra of biological systems at high magnetic fields and spinning speeds with no 1H decoupling applied during the mixing period. Experiments carried out on a polycrystalline sample of histidine clearly suggest that an improved signal to noise ratio can be realised by eliminating 1H decoupling during mixing.

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References

  • Bak M, Nielsen NC (1997) REPULSION, A novel approach to efficient powder averaging in solid-state NMR. J Magn Reson 125:132–139

    Article  Google Scholar 

  • Bak M, Rasmussen JT, Nielsen NC (2000) SIMPSON: a general simulation program for solid-state NMR spectroscopy. J Magn Reson 147:296–330

    Article  ADS  Google Scholar 

  • Baldus M (2002) Correlation experiments for assignment and structure elucidation of immobilized polypeptides under magic angle spinning. Prog Nucl Magn Reson Spectrosc 41:1–47

    Article  Google Scholar 

  • Bennett AE, Griffin RG, Vega S (1994) Recoupling of homo- and heteronuclear dipolar interactions in rotating solids. In: NMR basic principles and progress, vol 33. Springer, Berlin, pp 1–77

  • Bennett AE, Rienstra CM, Auger M, Lakshmi KV, Griffin RG (1995) Heteronuclear decoupling in rotating solids. J Chem Phys 103:6951–6958

    Article  ADS  Google Scholar 

  • Bennett AE, Rienstra CM, Griffiths JM, Zhen W, Lansbury PT, Griffin RG (1998) Homonuclear radio frequency-driven recoupling in rotating solids. J Chem Phys 108:9463–9479

    Article  ADS  Google Scholar 

  • Brinkmann A, Levitt MH (2001) Symmetry principles in the nuclear magnetic resonance of spinning solids: heteronuclear recoupling by generalized Hartmann-Hahn sequences. J Chem Phys 115:357–384

    Article  ADS  Google Scholar 

  • Brinkmann A, Schmedt auf der Günne J, Levitt MH (2002) Homonuclear zero-quantum recoupling in fast magic-angle spinning nuclear magnetic resonance. J Magn Reson 156:79–96

    Article  ADS  Google Scholar 

  • Carravetta M, Eden M, Zhao X, Brinkmann A, Levitt MH (2000) Symmetry principles for the design of radiofrequency pulse sequences in the nuclear magnetic resonance of rotating solids. Chem Phys Lett 321:205–215

    Article  Google Scholar 

  • De Paepe G, Bayro MJ, Lewandowski J, Griffin RG (2006) Broadband homonuclear correlation spectroscopy at high magnetic fields and MAS frequencies. J Am Chem Soc 128:1776–1777

    Article  Google Scholar 

  • Dusold S, Sebald A (2000) Dipolar recoupling under magic-angle spinning conditions. Annu Rep NMR Spectrosc 41:185–264

    Article  Google Scholar 

  • Griffin RG (1998) Dipolar recoupling in MAS spectra of biological solids. Nature Struct Biol 5:508–512

    Article  Google Scholar 

  • Hardy EH, Detken A, Meier BH (2003) Fast-MAS total through-bond correlation spectroscopy using adiabatic pulses. J Magn Reson 165:208–218

    Article  ADS  Google Scholar 

  • Heise B, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2002) Chemical shift correlation via RFDR: elimination of resonance offset effects. J Biomol NMR 24:237–243

    Article  Google Scholar 

  • Herbst C (2006a) Festkörper-NMR-Untersuchungen an isotopen-markierten biologischen Systemen, Diploma, Friedrich-Schiller-Universität Jena

  • Herbst C, Riedel K, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2006b) Solid state NMR at high magic angle spinning frequencies: dipolar chemical shift correlation with adiabatic inversion pulse based RF pulse schemes. J Biomol NMR 35:241–248

    Article  Google Scholar 

  • Hughes CE, Luca S, Baldus M (2004) Radio-frequency driven polarization transfer without heteronuclear decoupling in rotating solids. Chem Phys Lett 385:435–440

    Article  Google Scholar 

  • Hwang TL, van Zijl PCM, Garwood M (1998) Fast broadband inversion by adiabatic pulses. J Magn Reson 133:200–203

    Article  Google Scholar 

  • Leppert J, Heise B, Görlach M, Ramachandran R (2002) REDOR: an assessment of the efficacy of dipolar recoupling with adiabatic inversion pulses. J Biomol NMR 23:227–238

    Article  Google Scholar 

  • Leppert J, Heise B, Ohlenschläger O, Görlach M, Ramachandran R (2003) Broadband RFDR with adiabatic inversion pulses. J Biomol NMR 26:13–24

    Article  Google Scholar 

  • Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2004a) Adiabatic TOBSY in rotating solids. J Biomol NMR 29:167–173

    Article  Google Scholar 

  • Leppert J, Urbinati CR, Häfner S, Ohlenschläger O, Swanson MS, Görlach M, Ramachandran R (2004b) Identification of NH···N hydrogen bonds by magic angle spinning solid state NMR in a double-stranded RNA associated with myotonic dystrophy. Nucleic Acids Res 3:1177–1183

    Article  Google Scholar 

  • Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2004c) RFDR with adiabatic inversion pulses: application to internuclear distance measurements. J Biomol NMR 28:229–233

    Article  Google Scholar 

  • Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2004d) Adiabatic heteronuclear decoupling in rotating solids. J Biomol NMR 29:319–324

    Article  Google Scholar 

  • Levitt MH, Freeman R, Frenkiel T (1983) Broadband decoupling in high-resolution nuclear magnetic resonance spectroscopy. Adv Magn Reson 11:47–110

    Google Scholar 

  • Levitt MH (2002) Symmetry-based pulse sequences in magic-angle spinning solid-state NMR. In: Grant DM, Harris RK (eds) Encyclopedia of nuclear magnetic resonance, vol 9. John Wiley, Chichester, New York, p 165

  • Marin-Montesinos I, Brouwer DH, Antonioli G, Lai WC, Brinkmann A, Levitt MH (2005) Heteronuclear decoupling interference during symmetry-based homonuclear recoupling in solid-state NMR. J Magn Reson 177:307–317

    Article  ADS  Google Scholar 

  • McDermott AE (2004) Structural and dynamic studies of proteins by solid-state NMR spectroscopy: rapid movement forward. Curr Opin Struct Biol 14:554–561

    Article  Google Scholar 

  • Mou Y, Chao JCH, Chan JCC (2006) Efficient spin-spin scalar coupling mediated C-13 homonuclear polarization transfer in biological solids without proton decoupling. Solid State Nucl Magn Reson 29:278–282

    Article  Google Scholar 

  • Riedel K (2004) Festkörper-NMR untersuchungen von ribonukleinsäuren mittels adiabatischer symmetriebasierter pulssequenzen, Diploma, Friedrich-Schiller-Universität Jena

  • Riedel K, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2004a) Heteronuclear decoupling in rotating solids via symmetry-based adiabatic RF pulse schemes. Chem Phys Lett 395:356–361

    Article  Google Scholar 

  • Riedel K, Leppert J, Häfner S, Ohlenschläger O, Görlach M, Ramachandran R (2004b) Homonuclear chemical shift correlation in rotating solids via \({{{RN}_{n}}^\nu}\) symmetry-based adiabatic RF pulse schemes. J Biomol NMR 30:389–395

    Article  Google Scholar 

  • Riedel K, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2005) TEDOR with adiabatic inversion pulses: resonance assignments of 13C/15N labelled RNAs. J Biomol NMR 31:49–57

    Article  Google Scholar 

  • Riedel K, Herbst C, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2006a) Broadband homonuclear double-quantum NMR/filtering via zero-quantum dipolar recoupling in rotating solids. Chem Phys Lett 424:178–183

    Article  Google Scholar 

  • Riedel K, Herbst C, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2006b) Tailoring broadband inversion pulses for MAS solid state NMR. J Biomol NMR 35:275–283

    Article  Google Scholar 

  • Riedel K, Herbst C, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2006c) Heteronuclear decoupling in rotating solids: improving the efficacy of \({{{CN}_{n}}^\nu}\) symmetry-based tanh/tan adiabatic RF pulse schemes. Chem Phys Lett 429:590–594

    Article  Google Scholar 

  • States DJ, Haberkorn RA, Ruben DJ (1982) A two-dimensional nuclear overhauser experiment with pure absorption phase in four quadrants. J Magn Reson 48:286–292

    Google Scholar 

  • Thompson LK (2002) Solid-state NMR studies of the structure and mechanisms of proteins. Curr Opin Struct Biol 12:661–669

    Article  Google Scholar 

Download references

Acknowledgements

This study has been funded in part by a PhD fellowship to Kerstin Riedel from Stiftung Stipendien-Fonds des Verbandes der Chemischen Industrie e.V. The FLI is a member of the Science Association ‘Gottfried Wilhelm Leibniz’ (WGL) and is financially supported by the Federal Government of Germany and the State of Thuringia.

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Authors and Affiliations

  1. Research Group Molecular Biophysics/NMR Spectroscopy, Leibniz Institute for Age Research, Fritz Lipmann Institute, 07745, Jena, Germany

    Kerstin Riedel, Christian Herbst, Jörg Leppert, Oliver Ohlenschläger, Matthias Görlach & Ramadurai Ramachandran

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  1. Kerstin Riedel
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  2. Christian Herbst
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  3. Jörg Leppert
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  4. Oliver Ohlenschläger
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  5. Matthias Görlach
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  6. Ramadurai Ramachandran
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Correspondence to Ramadurai Ramachandran.

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Riedel, K., Herbst, C., Leppert, J. et al. Broadband homonuclear chemical shift correlation at high MAS frequencies: a study of tanh/tan adiabatic RF pulse schemes without \({^{{\bf 1}}\hbox{{\bf H}}}\) decoupling during mixing. J Biomol NMR 37, 277–286 (2007). https://doi.org/10.1007/s10858-006-9137-3

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  • DOI: https://doi.org/10.1007/s10858-006-9137-3

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