Adiabatic homonuclear polarization transfer in magic-angle-spinning solid-state NMR1Presented in part at the 38th ENC conference, March 23–27, 1997, Orlando, Florida, USA.1

Verel, René; Baldus, Marc; Nijman, Marcel J.; Os, J. W. M. van; Meier, Beat H.

doi:10.1016/s0009-2614(97)01093-2

Cited by 58 publications

(16 citation statements)

References 21 publications

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“…Notably, such measurements also revealed intermolecular contacts in our tetrameric [ 1 H/ 2 H, 13 C, 15 N] ion channel for which the combined application of dedicated ssNMR schemes and mixed labelling approaches that previously allowed detecting such constraints (see, e.g., Etzkorn et al 2004; Wasmer et al 2008; Etzkorn et al 2010) is precluded. It seems likely that fractional deuteration will also facilitate the determination of longer internuclear distances using rotational-resonance recoupling (Spencer et al 1991; Costa et al 1997) or rotating-frame (Nomura et al 1999; Sonnenberg et al 2004) and MAS-modulated variants (Verel et al 1997; Ramachandran et al 2003) thereof. In addition, coherent transfer schemes that mediate ( 13 C, 15 N) transfer via proton spins such as CHC (Seidel et al 2005), PAR (Paepe et al 2008) or PAIN-CP (De Paepe et al 2011) experiments may be readily combined with fractional deuteration to suppress chemical-shift offset affects or to enhance transfer efficiencies.…”

Section: Discussionmentioning

confidence: 99%

Fractional deuteration applied to biomolecular solid-state NMR spectroscopy

et al. 2011

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Solid-state Nuclear Magnetic Resonance can provide detailed insight into structural and dynamical aspects of complex biomolecules. With increasing molecular size, advanced approaches for spectral simplification and the detection of medium to long-range contacts become of critical relevance. We have analyzed the protonation pattern of a membrane-embedded ion channel that was obtained from bacterial expression using protonated precursors and D2O medium. We find an overall reduction of 50% in protein protonation. High levels of deuteration at Hα and Hβ positions reduce spectral congestion in (1H,13C,15N) correlation experiments and generate a transfer profile in longitudinal mixing schemes that can be tuned to specific resonance frequencies. At the same time, residual protons are predominantly found at amino-acid side-chain positions enhancing the prospects for obtaining side-chain resonance assignments and for detecting medium to long-range contacts. Fractional deuteration thus provides a powerful means to aid the structural analysis of complex biomolecules by solid-state NMR.Electronic supplementary materialThe online version of this article (doi:10.1007/s10858-011-9585-2) contains supplementary material, which is available to authorized users.

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Section: Discussionmentioning

confidence: 99%

Fractional deuteration applied to biomolecular solid-state NMR spectroscopy

et al. 2011

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“…Finally, we note that the efficiency of the transfer can be optimized further by adiabatically [42] establishing the CP transfer. This technique can be characterized by a slow modulation of one of the R F amplitudes through the CP matching condition [20], and has been demonstrated previously to yield more efficient (broadband) polariza- tion transfer also among I3C,l5N systems [16] and homonuclear spin pairs [43,44]. Preliminary results indicate that generally the efficiency of the SPECIFIC transfer can be increased without losing selectivity.…”

Section: (18)mentioning

confidence: 99%

Cross polarization in the tilted frame: assignment and spectral simplification in heteronuclear spin systems

Baldus¹,

Petkova²,

Herzfeld³

et al. 1998

Molecular Physics

524

508

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A frequency selective heteronuclear polarization transfer technique is introduced for rotating solids. In this method, radiofrequency fields comparable with the frequency offsets are applied to establish Hartmann-Hahn cross polarization that therefore depends explicitly on the resonance offset of the nuclei involved. Under these conditions, spectrally induced filtering in combination with cross polarization (SPECIFIC CP) can be achieved and is demonstrated to be useful for spectral simplification or assignment in heteronuclear spin pairs. The design principles are outlined and demonstrated experimentally on I3C, "N labelled amino acids.

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“…For polarization transfer at higher spinning frequencies, experiments have been developed in which the ratio of recoupling nutation frequency to MAS frequency is low [14,15]. In addition, dipolar recoupling using an adiabatic modulation of the system Hamiltonian has been demonstrated using no [16] or small [17] r.f. fields on the recoupling channel.…”

Section: Introductionmentioning

confidence: 99%

Radio-frequency driven polarization transfer without heteronuclear decoupling in rotating solids

Hughes

Luca

Baldus

2004

Chemical Physics Letters

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This Letter reports significant excitation of 13 C homonuclear double-quantum coherence in a solid-state magic-angle-spinning NMR experiment, acquired without heteronuclear decoupling of abundant 1 H spins. The heteronuclear decoupling efficiency of a group of existing homonuclear polarization transfer sequences are investigated and optimal schemes are identified. Since the approach permits the application of fast MAS and significantly reduces the total radio-frequency power used, it is particularly well suited to biomolecular applications at ultra-high magnetic fields.

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Adiabatic homonuclear polarization transfer in magic-angle-spinning solid-state NMR1Presented in part at the 38th ENC conference, March 23–27, 1997, Orlando, Florida, USA.1

Cited by 58 publications

References 21 publications

Fractional deuteration applied to biomolecular solid-state NMR spectroscopy

Fractional deuteration applied to biomolecular solid-state NMR spectroscopy

Cross polarization in the tilted frame: assignment and spectral simplification in heteronuclear spin systems

Radio-frequency driven polarization transfer without heteronuclear decoupling in rotating solids

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