Abstract
An approach for generating efficient \( {\rm{RN}}_{n}^{\nu_{\rm{S}}, {\nu_{\rm{k}}}} \) symmetry-based dual channel RF pulse schemes for γ-encoded broadband 15N–13C dipolar recoupling at high magic angle spinning frequencies is presented. The method involves the numerical optimisation of the RF phase-modulation profile of the basic “R” element so as to obtain heteronuclear double quantum dipolar recoupling sequences with satisfactory magnetisation transfer characteristics. The basic “R” element was implemented as a sandwich of a small number of short pulses of equal duration with each pulse characterised by a RF phase and amplitude values. The performance characteristics of the sequences were evaluated via numerical simulations and 15N–13C chemical shift correlation experiments. Employing such 13C–15N double-quantum recoupling sequences and the multiple receiver capabilities available in the current generation of NMR spectrometers, the possibility to simultaneously acquire 3D NCC and CNH chemical shift correlation spectra is also demonstrated.
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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
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
Bennett AE, Griffin RG, Vega S (1994) Recoupling of homo- and heteronuclear dipolar interactions in rotating solids. NMR basic principles and progress, vol 33. Springer, Berlin, pp 1–77
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
Brinkmann A, Levitt M (2001) Symmetry principles in the nuclear magnetic resonance of spinning solids: heteronuclear recoupling by generalized Hartmann-Hahn sequences. J Chem Phys 115:357–384
Castellani F, van Rossum BJ, Diehl A, Rehbein K, Oschkinat H (2003) Determination of solid-state NMR structures of proteins by means of three-dimensional 15N–13C-13C dipolar correlation spectroscopy and chemical shift analysis. Biochemistry 42:11476–11483
Cheng VB, Suzukawa HH, Wolfsberg M (1973) Investigations of a nonrandom numerical method for multidimensional integration. J Chem Phys 59:3992–3999
De Paepe G, Lesage A, Emsley L (2003) The performance of phase modulated heteronuclear dipolar decoupling schemes in fast magic-angle-spinning nuclear magnetic resonance experiments. J Chem Phys 119:4833–4841
Detken A, Hardy EH, Ernst M, Kainosho M, Kawakami T, Aimoto S, Meier BH (2001) Methods for sequential resonance assignment in solid, uniformly 13C, 15N labelled peptides: quantification and application to antamanide. J Biomol NMR 20:203–221
Dusold S, Sebald A (2000) Dipolar recoupling under magic-angle spinning conditions. Annu Rep NMR Spectrosc 41:185–264
Forrest S (1993) Genetic algorithms—principles of natural-selection applied to computation. Science 261:872–878
Freeman R, Wu XL (1987) Design of magnetic resonance experiments by genetic evolution. J Magn Reson 75:184–189
Frericks HL, Zhou DH, Yap LL, Gennis RB, Rienstra CM (2006) Magic-angle spinning solid-state NMR of a 144 kDa membrane protein complex: E. coli cytochrome bo3 oxidase. J Biomol NMR 36:55–71
Fung BM, Khitrin AK, Ermolaev K (2000) An improved broadband decoupling sequence for liquid crystals and solids. J Magn Reson 142:97–101
Goldberg DE (1989) Genetic algorithms in search, optimization and machine learning. Addison-Wesley, Massachusetts
Griffin RG (1998) Dipolar recoupling in MAS spectra of biological solids. Nature Struct Biol 5:508–512
Hansen JO, Kehlet C, Bjerring M, Vosegaard T, Glaser SJ, Khaneja N, Nielsen NC (2007) Optimal control based design of composite dipolar recoupling experiments by analogy to single-spin inversion pulses. Chem Phys Lett 447:154–161
Haupt RL, Haupt SE (2004) Practical genetic algorithms. Wiley, Hoboken
Herbst C, Riedel K, Ihle Y, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2008) MAS solid state NMR of RNAs with multiple receivers. J Biomol NMR 41:121–125
Herbst C, Herbst J, Kirschstein A, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2009a) Design of high-power, broadband 180° pulses and mixing sequences for fast MAS solid state chemical shift correlation NMR spectroscopy. J Biomol NMR 43:51–61
Herbst C, Herbst J, Kirschstein A, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2009b) Recoupling and decoupling of nuclear spin interactions at high MAS frequencies: numerical design of CN νn symmetry-based RF pulse schemes. J Biomol NMR 44:175–184
Herbst C, Herbst J, Leppert J, Ohlenschläger O, Görlach M, Ramachandran R (2009c) Numerical design of RN νn symmetry-based RF pulse schemes for recoupling and decoupling of nuclear spin interactions at high MAS frequencies. J Biomol NMR 44:235–244
Hong M (1999) Resonance assignment of 13C/15N labeled solid proteins by two- and three-dimensional magic-angle-spinning NMR. J Biomol NMR 15:1–14
Judson R (1997) Genetic algorithms and their use in chemistry. In: Lipkowitz KB, Boyd DB (eds) Reviews in computational chemistry, vol 10. VCH, New York, pp 1–73
Kehlet C, Bjerring M, Sivertsen AC, Kristensen T, Enghild JJ, Glaser SJ, Khaneja N, Nielsen NC (2007) Optimal control based NCO and NCA experiments for spectral assignment in biological solid-state NMR spectroscopy. J Magn Reson 188:216
Kupce E, Freeman R (2004) Projection-reconstruction technique for speeding up multidimensional NMR spectroscopy. J Am Chem Soc 126:6429–6440
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. Wiley, Chichester
Nielsen AB, Bjerring M, Nielsen JT, Nielsen NC (2009) Symmetry-based dipolar recoupling by optimal control: band-selective experiments for assignment of solid-state NMR spectra of proteins. J Chem Phys 131:025101
Pauli J, Baldus M, van Rossum B, de Groot H, Oschkinat H (2001) Backbone and side-chain 13C and 15N signal assignments of the α-spectrin SH3 domain by magic angle spinning solid-state NMR at 17.6 Tesla. ChemBioChem 2:272–281
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
Rienstra CM, Hohwy M, Hong M, Griffin R (2000) 2D and 3D 15N–13C-13C chemical shift correlation spectroscopy of solids: assignment of MAS spectra of peptides. J Am Chem Soc 122:10979–10990
Siemer AB, Ritter C, Steinmetz MO, Ernst M, Riek R, Meier BH (2006) 13C, 15N resonance assignment of parts of the HET-s prion protein in its amyloid form. J Biomol NMR 34:75–87
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
Sun BQ, Rienstra CM, Costa PR, Williamson JR, Griffin RG (1997) 3D 15N–13C–13C chemical shift correlation spectroscopy in rotating solids. J Am Chem Soc 119:8540–8546
van Rossum BJ, Castellani F, Pauli J, Rehbein K, Hollander J, de Groot HJM, Oschkinat H (2003) Assignment of amide proton signals by combined evaluation of HN, NN and HNCA MAS-NMR correlation spectra. J Biomol NMR 25:217–223
Veshtort M, Griffin RG (2006) SPINEVOLUTION: a powerful tool for the simulation of solid and liquid state NMR experiments. J Magn Reson 178:248–282
Wall M (1996) GAlib: A C++ Library of genetic algorithm components, version 2.4.7. http://lancet.mit.edu/ga/
Wu XL, Freeman R (1989) Darwin’s ideas applied to magnetic resonance. The marriage broker. J Magn Reson 85:414–420
Xu P, Wu XL, Freeman R (1992) User-friendly selective pulses. J Magn Reson 99:308–322
Zhou DH, Shah G, Cormos M, Franks WT, Mullen C, Sandoz D, Rienstra CM (2007a) Proton-detected solid-state NMR spectroscopy of fully protonated proteins at 40 kHz magic-angle spinning. J Am Chem Soc 129:11791–11801
Zhou DH, Shea JJ, Nieuwkoop AJ, Franks WT, Wylie BJ, Mullen C, Sandoz D, Rienstra CM (2007b) Solid-state protein-structure determination with proton-detected triple-resonance 3D magic-angle-spinning NMR spectroscopy. Angew Chem Int Ed 46:8380–8383
Acknowledgments
This study has been funded in part by a grant from the Deutsche Forschungsgemeinschaft (GO474/6-1). 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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Herbst, C., Herbst, J., Carella, M. et al. Broadband 15N–13C dipolar recoupling via symmetry-based RF pulse schemes at high MAS frequencies. J Biomol NMR 47, 7–17 (2010). https://doi.org/10.1007/s10858-010-9406-z
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DOI: https://doi.org/10.1007/s10858-010-9406-z