Publication date: Available online 20 December 2017 Source:Journal of Magnetic Resonance
Author(s): Johannes Hellwagner, Nino Wili, Luis Fábregas Ibáñez, Johannes J. Wittmann, Beat H. Meier, Matthias Ernst
Dipolar recoupling techniques that use isolated rotor-synchronized ? pulses are commonly used in solid-state NMR spectroscopy to gain insight into the structure of biological molecules. These sequences excel through their simplicity, stability towards radio-frequency (rf) inhomogeneity, and low rf requirements. For a theoretical understanding of such sequences, we present a Floquet treatment based on an interaction-frame transformation including the chemical-shift offset dependence. This approach is applied to the homonuclear dipolar-recoupling sequence Radio–Frequency Driven Recoupling (RFDR) and the heteronuclear recoupling sequence Rotational Echo Double Resonance (REDOR). Based on the Floquet approach, we show the influence of effective fields caused by pulse transients and discuss the advantages of pulse-transient compensation. We demonstrate experimentally that the transfer efficiency for homonuclear recoupling can be doubled in some cases in model compounds as well as in simple peptides if pulse-transient compensation is applied to the ? pulses. Additionally, we discuss the influence of various phase cycles on the recoupling efficiency in order to reduce the magnitude of effective fields. Based on the findings from RFDR, we are able to explain why the REDOR sequence does not suffer in the recoupling efficiency despite the presence of effective fields. Graphical abstract
[NMR paper] A suite of pulse sequences based on multiple sequential acquisitions at one and two radiofrequency channels for solid-state magic-angle spinning NMR studies of proteins.
A suite of pulse sequences based on multiple sequential acquisitions at one and two radiofrequency channels for solid-state magic-angle spinning NMR studies of proteins.
A suite of pulse sequences based on multiple sequential acquisitions at one and two radiofrequency channels for solid-state magic-angle spinning NMR studies of proteins.
J Biomol NMR. 2016 Jun 30;
Authors: Sharma K, Madhu PK, Mote KR
Abstract
One of the fundamental challenges in the application of solid-state NMR is its limited sensitivity, yet a majority of...
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07-02-2016 07:23 PM
A suite of pulse sequences based on multiple sequential acquisitions at one and two radiofrequency channels for solid-state magic-angle spinning NMR studies of proteins
A suite of pulse sequences based on multiple sequential acquisitions at one and two radiofrequency channels for solid-state magic-angle spinning NMR studies of proteins
Abstract
One of the fundamental challenges in the application of solid-state NMR is its limited sensitivity, yet a majority of experiments do not make efficient use of the limited polarization available. The loss in polarization in a single acquisition experiment is mandated by the need to select out a single coherence pathway. In contrast, sequential acquisition strategies can encode...
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07-01-2016 03:06 AM
[NMR paper] Weak and Transient Protein Interactions Determined by Solid-State NMR.
Weak and Transient Protein Interactions Determined by Solid-State NMR.
Related Articles Weak and Transient Protein Interactions Determined by Solid-State NMR.
Angew Chem Int Ed Engl. 2016 Apr 21;
Authors: Dannatt HR, Felletti M, Jehle S, Wang Y, Emsley L, Dixon NE, Lesage A, Pintacuda G
Abstract
Despite their roles in controlling many cellular processes, weak and transient interactions between large structured macromolecules and disordered protein segments cannot currently be characterized at atomic resolution by X-ray...
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04-22-2016 08:45 PM
[Question from NMRWiki Q&A forum] Software to simulate pulse sequences
Software to simulate pulse sequences
Hi,I'm interested in software for windows or linux that simulate the effect of pulses, delay AND gradients using the product operator formalism.Do you have suggestions?ThanksMarco
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06-18-2014 04:23 AM
[NMR paper] Motion-adapted pulse sequences for oriented sample (OS) solid-state NMR of biopolymers.
Motion-adapted pulse sequences for oriented sample (OS) solid-state NMR of biopolymers.
Motion-adapted pulse sequences for oriented sample (OS) solid-state NMR of biopolymers.
J Chem Phys. 2013 Aug 28;139(8):084203
Authors: Lu GJ, Opella SJ
Abstract
One of the main applications of solid-state NMR is to study the structure and dynamics of biopolymers, such as membrane proteins, under physiological conditions where the polypeptides undergo global motions as they do in biological membranes. The effects of NMR radiofrequency irradiations on...
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09-07-2013 09:54 PM
Challenges in numerical simulations of solid-state NMR experiments: Spin exchange pulse sequences.
Challenges in numerical simulations of solid-state NMR experiments: Spin exchange pulse sequences.
Challenges in numerical simulations of solid-state NMR experiments: Spin exchange pulse sequences.
Solid State Nucl Magn Reson. 2011 Feb 1;
Authors: Vosegaard T
While simulations are essential for interpretation of solid-state NMR experiments, large spin systems involved in e.g. spin-diffusion experiments and/or dynamic effects like chemical exchange pose great challenges for the numerical simulations, where we typically want to include effects of...
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02-19-2011 06:02 PM
[NMR paper] Improved pulse sequences for pure exchange solid-state NMR spectroscopy.
Improved pulse sequences for pure exchange solid-state NMR spectroscopy.
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Magn Reson Chem. 2004 Feb;42(2):285-90
Authors: Vosegaard T, Nielsen NC
Spin-exchange experiments are useful for improving the resolution and establishment of sequential assignments in solid-state NMR spectra of uniformly (15)N-labeled proteins oriented macroscopically in phospholipid bilayers. To exploit this advantage fully, it is crucial that the diagonal peaks in the...
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11-24-2010 09:25 PM
BMRB library of Bruker pulse sequences
The following Bruker pulse sequences can be found on BMRB website.
Shift correlation:
Homonuclear
Three-dimensional TOCSY-HSQC 3D experiment
NOESY-HSQC 3D experiment
Heteronuclear
Transient effects in ?–pulse sequences in MAS solid-state NMR
Linear Mode
