Abstract An approach for conveniently implementing low-power CN n ν and RN n ν symmetry-based band-selective mixing sequences for generating homo- and heteronuclear chemical shift correlation NMR spectra of low γ nuclei in biological solids is demonstrated. Efficient magnetisation transfer characteristics are achieved by selecting appropriate symmetries requiring the application of basic RF elements of relatively long duration and numerically tailoring the RF field modulation profile of the basic element. The efficacy of the approach is experimentally shown by the acquisition of 15Nâ??13C dipolar and 13Câ??13C scalar and dipolar coupling mediated chemical shift correlation spectra at representative MAS frequencies.
Content Type Journal Article
Pages 1-8
DOI 10.1007/s10858-011-9516-2
Authors
Christian Herbst, Department of Physics; Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani, 34190 Thailand
Jirada Herbst, Department of Mathematics, Statistics and Computer, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani, 34190 Thailand
Jörg Leppert, Research group Biomolecular NMR spectroscopy, Leibniz Institute for Age Research, Fritz Lipmann Institute, 07745 Jena, Germany
Oliver Ohlenschläger, Research group Biomolecular NMR spectroscopy, Leibniz Institute for Age Research, Fritz Lipmann Institute, 07745 Jena, Germany
Matthias Görlach, Research group Biomolecular NMR spectroscopy, Leibniz Institute for Age Research, Fritz Lipmann Institute, 07745 Jena, Germany
Ramadurai Ramachandran, Research group Biomolecular NMR spectroscopy, Leibniz Institute for Age Research, Fritz Lipmann Institute, 07745 Jena, Germany
31P NMR correlation maps of 18O/16O chemical shift isotopic effects for phosphometabolite labeling studies
31P NMR correlation maps of 18O/16O chemical shift isotopic effects for phosphometabolite labeling studies
Abstract Intramolecular correlations among the 18O-labels of metabolic oligophosphates, mapped by J-decoupled 31P NMR 2D chemical shift correlation spectroscopy, impart stringent constraints to the 18O-isotope distributions over the whole oligophosphate moiety. The multiple deduced correlations of isotopic labels enable determination of site-specific fractional isotope enrichments and unravel the isotopologue statistics. This approach ensures accurate determination of 18O-labeling...
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06-06-2011 12:53 AM
Sensitive 13Câ??13C correlation spectra of amyloid fibrils at very high spinning frequencies and magnetic fields
Sensitive 13Câ??13C correlation spectra of amyloid fibrils at very high spinning frequencies and magnetic fields
Abstract Sensitive 2D solid-state 13Câ??13C correlation spectra of amyloid β fibrils have been recorded at very fast spinning frequencies and very high magnetic fields. It is demonstrated that PARIS-xy recoupling using moderate rf amplitudes can provide structural information by promoting efficient magnetization transfer even under such challenging experimental conditions. Furthermore, it has been shown both experimentally and by numerical simulations that the method is not...
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04-01-2011 09:23 AM
[NMR paper] Resonance assignment of proteins with high shift degeneracy based on 5D spectral info
Resonance assignment of proteins with high shift degeneracy based on 5D spectral information encoded in G2FT NMR experiments.
Related Articles Resonance assignment of proteins with high shift degeneracy based on 5D spectral information encoded in G2FT NMR experiments.
J Am Chem Soc. 2005 Apr 6;127(13):4554-5
Authors: Atreya HS, Eletsky A, Szyperski T
A suite of novel (5,3)D G2FT triple resonance NMR experiments encoding highly resolved 5D spectral information is presented for sequential resonance assignment of proteins exhibiting high chemical...
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11-25-2010 08:21 PM
[NMR paper] Histogram-based scoring schemes for protein NMR resonance assignment.
Histogram-based scoring schemes for protein NMR resonance assignment.
Related Articles Histogram-based scoring schemes for protein NMR resonance assignment.
J Bioinform Comput Biol. 2004 Dec;2(4):747-64
Authors: Wan X, Tegos T, Lin G
In NMR protein structure determination, after the resonance peaks have been identified and chemical shifts from peaks across multiple spectra have been grouped into spin systems, associating these spin systems to their host residues is the key toward the success of structural information extraction and thus the...
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11-24-2010 10:03 PM
[NMR paper] CAMRA: chemical shift based computer aided protein NMR assignments.
CAMRA: chemical shift based computer aided protein NMR assignments.
Related Articles CAMRA: chemical shift based computer aided protein NMR assignments.
J Biomol NMR. 1998 Oct;12(3):395-405
Authors: Gronwald W, Willard L, Jellard T, Boyko RF, Rajarathnam K, Wishart DS, Sönnichsen FD, Sykes BD
A suite of programs called CAMRA (Computer Aided Magnetic Resonance Assignment) has been developed for computer assisted residue-specific assignments of proteins. CAMRA consists of three units: ORB, CAPTURE and PROCESS. ORB predicts NMR chemical shifts...
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11-17-2010 11:15 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...
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08-14-2010 04:19 AM
Broadband homonuclear TOCSY with amplitude and phase-modulated RF mixing schemes
Broadband homonuclear TOCSY with amplitude and phase-modulated RF mixing schemes
Anika Kirschstein, Christian Herbst, Kerstin Riedel, Michela Carella, Jörg Leppert, Oliver Ohlenschläger, Matthias Görlach and Ramadurai Ramachandran
Journal of Biomolecular NMR; 2008; 40(4); pp 227-237
Abstract:
We have explored the design of broadband scalar coupling mediated 13C–13C and cross-relaxation suppressed 1H–1H TOCSY sequences employing phase/amplitude modulated inversion pulses. Considering a variety of supercycles, pulsewidths and a RF field strength of 10 kHz, the Fourier coefficients...
Mikey
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08-14-2008 12:42 AM
Four-dimensional heteronuclear correlation experiments for chemical shift assignment of solid proteins
Four-dimensional heteronuclear correlation experiments for chemical shift assignment of solid proteins
W. Trent Franks, Kathryn D. Kloepper, Benjamin J. Wylie and Chad M. Rienstra
Journal of Biomolecular NMR; 2007; 39(2); pp 107 - 131
Abstract:
Chemical shift assignment is the first step in all established protocols for structure determination of uniformly labeled proteins by NMR. The explosive growth in recent years of magic-angle spinning (MAS) solid-state NMR (SSNMR) applications is largely attributable to improved methods for backbone and side-chain chemical shift correlation...