Publication date: August 2017 Source:Journal of Magnetic Resonance, Volume 281
Author(s): Navin Khaneja, Ashutosh Kumar
The paper describes a family of novel recoupling pulse sequences in magic angle spinning (MAS) solid state NMR, called two pulse recoupling. These pulse sequences can be employed for both homonuclear and heteronuclear recoupling experiments and are robust to dispersion in chemical shifts and rf-inhomogeneity. The homonuclear pulse sequence consists of a building block ( ? ) ? ( ? ) - ? where ? = ? 4 n , and n is number of blocks in a rotor period. The recoupling block is made robust to rf-inhomogeneity by extending it to ( ? ) ? ( ? ) - ? ( ? ) ? + ? ( ? ) ? - ? . The heteronuclear recoupling pulse sequence consists of a building block ( ? ) ? 1 ( ? ) - ? 1 and ( ? ) ? 2 ( ? ) - ? 2 on channel I and S, where ? 1 = 3 ? 8 n , ? 2 = ? 8 n and n is number of blocks in a rotor period. The recoupling block is made robust to rf-inhomogeneity by extending it to ( ? ) ? 1 ( ? ) - ? 1 ( ? ) ? + ? 1 ( ? ) ? - ? 1 and ( ? ) ? 2 ( ? ) - ? 2 ( ? ) ? + ? 2 ( ? ) ? - ? 2 on two channels respectively. The recoupling pulse sequences mix the z magnetization. Experimental quantification of this method is shown for 13C ? -13CO homonuclear recoupling in a sample of Glycine and 15N-13C ? heteronuclear recoupling in Alanine. Application of this method is demonstrated on a sample of tripeptide N-formyl-[U-13C,15N]-Met-Leu-Phe-OH (MLF). Compared to R-sequences (Levitt, 2002), these sequences are more robust to rf-inhomogeneity and give better sensitivity, as shown in Fig. 3. Graphical abstract
[NMR paper] MAS solid state NMR of proteins: simultaneous (15)N- (13)CA and (15)N- (13)CO dipolar recoupling via low-power symmetry-based RF pulse schemes.
MAS solid state NMR of proteins: simultaneous (15)N- (13)CA and (15)N- (13)CO dipolar recoupling via low-power symmetry-based RF pulse schemes.
MAS solid state NMR of proteins: simultaneous (15)N- (13)CA and (15)N- (13)CO dipolar recoupling via low-power symmetry-based RF pulse schemes.
J Biomol NMR. 2015 Feb 25;
Authors: Herbst C, Bellstedt P, Görlach M, Ramachandran R
Abstract
The generation of efficient RN n (?)s,(?)k symmetry-based low-power RF pulse schemes for simultaneous (15)N-(13)CA and (15)N-(13)CO dipolar recoupling...
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02-26-2015 11:11 PM
MAS solid state NMR of proteins: simultaneous 15 Nâ?? 13 CA and 15 Nâ?? 13 CO dipolar recoupling via low-power symmetry-based RF pulse schemes
MAS solid state NMR of proteins: simultaneous 15 Nâ?? 13 CA and 15 Nâ?? 13 CO dipolar recoupling via low-power symmetry-based RF pulse schemes
Abstract
The generation of efficient RN n νs,νk symmetry-based low-power RF pulse schemes for simultaneous 15Nâ??13CA and 15Nâ??13CO dipolar recoupling is demonstrated. The method involves mixing schemes employing phase and amplitude-modulated dual band-selective 180° pulses as basic â??Râ?? element and tailoring of the RF field-modulation...
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02-25-2015 05:56 PM
[NMR paper] Proton-Detected 2D Radio Frequency Driven Recoupling Solid-state NMR Studies on Micelle-associated Cytochrome-b5
Proton-Detected 2D Radio Frequency Driven Recoupling Solid-state NMR Studies on Micelle-associated Cytochrome-b5
Publication date: Available online 1 March 2014
Source:Journal of Magnetic Resonance</br>
Author(s): Manoj Kumar Pandey , Subramanian Vivekanandan , Kazutoshi Yamamoto , Sangchoul Im , Lucy Waskell , Ayyalusamy Ramamoorthy</br>
Solid-state NMR spectroscopy is increasingly used in the high-resolution structural studies of membrane-associated proteins and peptides. Most such studies necessitate isotopically labeled (13C, 15N and 2H) proteins/peptides,...
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03-02-2014 01:53 AM
[NMR paper] Designing Dipolar Recoupling and Decoupling Experiments for Biological Solid-State NMR Using Interleaved Continuous Wave and rf Pulse Irradiation.
Designing Dipolar Recoupling and Decoupling Experiments for Biological Solid-State NMR Using Interleaved Continuous Wave and rf Pulse Irradiation.
Designing Dipolar Recoupling and Decoupling Experiments for Biological Solid-State NMR Using Interleaved Continuous Wave and rf Pulse Irradiation.
Acc Chem Res. 2013 Apr 4;
Authors: Bjerring M, Jain S, Paaske B, Vinther JM, Nielsen NC
Abstract
Rapid developments in solid-state NMR methodologyhave boosted this technique into a highly versatile tool for structural biology. The invention of...
Radio frequency assisted homonuclear recoupling - A Floquet description of homonuclear recoupling via surrounding heteronuclei in fully protonated to fully deuterated systems
Radio frequency assisted homonuclear recoupling - A Floquet description of homonuclear recoupling via surrounding heteronuclei in fully protonated to fully deuterated systems
Publication year: 2011
Source: Journal of Magnetic Resonance, In Press, Accepted Manuscript, Available online 18 January 2011</br>
Michal, Leskes , Ümit, Akbey , Hartmut, Oschkinat , Barth-Jan, van Rossum , Shimon, Vega</br>
We present a Floquet theory approach for the analysis of homonuclear recoupling assisted by radio frequency (RF) irradiation of surrounding heteronuclear spins. This description covers a...
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01-19-2011 03:04 PM
Recoupling of native homonuclear dipolar couplings in magic-angle-spinning solid-stat
Recoupling of native homonuclear dipolar couplings in magic-angle-spinning solid-state NMR by the double-oscillating field technique.
Related Articles Recoupling of native homonuclear dipolar couplings in magic-angle-spinning solid-state NMR by the double-oscillating field technique.
J Chem Phys. 2010 Aug 14;133(6):064501
Authors: Straaso LA, Nielsen NC
A new solid-state NMR method, the double-oscillating field technique (DUO), that under magic-angle-spinning conditions produces an effective Hamiltonian proportional to the native high-field...
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08-17-2010 01:53 PM
Broadband 15Nâ??13C dipolar recoupling via symmetry-based RF pulse schemes at high MA
Abstract An approach for generating efficient
RNnnS, nk symmetry-based dual channel RF pulse schemes for γ-encoded broadband 15Nâ??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 â??Râ?? element so as to obtain heteronuclear double quantum dipolar recoupling sequences with satisfactory magnetisation transfer characteristics. The basic â??Râ?? element was implemented as a sandwich of a small number of short pulses of equal duration with each pulse characterised by...
Two pulse recoupling
Linear Mode
