Spin Diffusion Driven by R-Symmetry Sequences: Applications to Homonuclear Correlation Spectroscopy in MAS NMR of Biological and Organic Solids.
J Am Chem Soc. 2011 Mar 1;
Authors: Hou G, Yan S, Sun S, Han Y, Byeon IJ, Ahn J, Concel J, Samoson A, Gronenborn AM, Polenova T
We present a family of homonuclear (13)C-(13)Cmagic angle spinning spin diffusion experiments, based on R2(n)(v) (n = 1 and 2, v = 1 and 2) symmetry sequences. These experiments are well suited for (13)C-(13)C correlation spectroscopy in biological and organic systems and are especially advantageous at very fast MAS conditions, where conventional PDSD and DARR experiments fail. At very fast MAS frequencies the R2(1)(1), R2(2)(1), and R2(2)(2) sequences result in excellent quality correlation spectra both in model compounds and in proteins. Under these conditions, individual R2(n)(v) display different polarization transfer efficiency dependencies on isotropic chemical shift differences: R2(2)(1) recouples efficiently both small and large chemical shift differences (in proteins these correspond to aliphatic-to-aliphatic and carbonyl-to-aliphatic correlations, respectively), while R2(1)(1) and R2(2)(2) exhibit the maximum recoupling efficiency for the aliphatic-to-aliphatic or carbonyl-to-aliphatic correlations, respectively. At moderate MAS frequencies (10-20 kHz), all R2(n)(v) sequences introduced in this work display similar transfer efficiencies, and their performance is very similar to that of PDSD and DARR. Polarization transfer dynamics and chemical shift dependencies of these R2-driven spin diffusion (RDSD) schemes are experimentally evaluated and investigated by numerical simulations for [U-(13)C,(15)N]-alanine and the [U-(13)C,(15)N] N-formyl-Met-Leu-Phe (MLF) tripeptide. Further applications of this approach are illustrated for several proteins: spherical assemblies of HIV-1 U-(13)C,(15)N CA protein, U-(13)C,(15)N-enriched dynein light chain DLC8, and sparsely (13)C/uniformly (15)N enriched CAP-Gly domain of dynactin. Due to the excellent performance and ease of implementation, the presented R2(n)(v) symmetry sequences are expected to be of wide applicability in studies of proteins and protein assemblies as well as other organic solids by MAS NMR spectroscopy.
PMID: 21361320 [PubMed - as supplied by publisher]
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Gang Wu, Zhehong Gan, Irene C. M. Kwan, James C. Fettinger and Jeffery T. Davis
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja2052446/aop/images/medium/ja-2011-052446_0001.gif
Journal of the American Chemical Society
DOI: 10.1021/ja2052446
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Chemical shift correlation at high MAS frequencies employing low-power symmetry-based mixing schemes
Chemical shift correlation at high MAS frequencies employing low-power symmetry-based mixing schemes
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...
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NMR studies of alkali metal ions in organic and biological solids
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Publication year: 2011
Source: Progress in Nuclear Magnetic Resonance Spectroscopy, In Press, Accepted Manuscript, Available online 13 June 2011</br>
Gang, Wu , Jianfeng, Zhu</br>
*Highlights:*? Comprehensive review of NMR of alkali metal ions in organic/biological solids ? Experimental solid-state NMR techniques and computational methods ? Survey of experimental alkali metal NMR data for organic/biological solids</br></br>
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06-14-2011 02:30 AM
Spin Diffusion Driven by R-Symmetry Sequences: Applications to Homonuclear Correlation Spectroscopy in MAS NMR of Biological and Organic Solids
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Guangjin Hou, Si Yan, Shangjin Sun, Yun Han, In-Ja L. Byeon, Jinwoo Ahn, Jason Concel, Ago Samoson, Angela M. Gronenborn and Tatyana Polenova
http://pubs.acs.org/appl/literatum/publisher/achs/journals/content/jacsat/0/jacsat.ahead-of-print/ja108650x/aop/images/medium/ja-2010-08650x_0001.gif
Journal of the American Chemical Society
DOI: 10.1021/ja108650x
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03-02-2011 02:01 AM
Homonuclear Mixing Sequences for Perdeuterated Proteins
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Publication year: 2010
Source: Journal of Magnetic Resonance, In Press, Accepted Manuscript, Available online 26 October 2010</br>
Kuo-Ying, Huang , Ansgar B., Siemer , Ann E., McDermott</br>
We test the performance of several 13C homonuclear mixing sequences on perdeuterated microcrystalline ubiquitin. All sequences were applied without 1H decoupling and at relatively low MAS frequencies. We found that RFDR gave the highest overall transfer efficiency and that DREAM performs surprisingly well under these conditions being twice...
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10-27-2010 08:51 AM
On the Performance of Spin Diffusion NMR Techniques in Oriented Solids: Prospects for
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Authors: Traaseth NJ, Gopinath T, Veglia G
NMR spin diffusion experiments have the potential to provide both resonance assignment and internuclear...
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10-13-2010 02:18 PM
NMR Spectroscopy Explained: Simplified Theory, Applications and Examples for Organic Chemistry and Structural Biology - Thomas L. James (2007)
NMR Spectroscopy Explained: Simplified Theory, Applications and Examples for Organic Chemistry and Structural Biology
Edited by Neil E. Jacobsen (2007)
Amazon book description
NMR Spectroscopy Explained : Simplified Theory, Applications and Examples for Organic Chemistry and Structural Biology provides a fresh, practical guide to NMR for both students and practitioners, in a clearly written and non-mathematical format. It gives the reader an intermediate level theoretical basis for understanding laboratory applications, developing concepts gradually within the context of examples and...
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Double quantum filtering homonuclear MAS NMR correlation spectra: a tool for membrane protein studies
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Jakob J. Lopez, Christoph Kaiser, Sarika Shastri and Clemens Glaubitz
Journal of Biomolecular NMR; 2008; 41(2) pp 97 - 104
Abstract:
13C homonuclear correlation spectra based on proton driven spin diffusion (PDSD) are becoming increasingly important for obtaining distance constraints from multiply labeled biomolecules by MAS NMR. One particular challenging situation arises when such constraints are to be obtained from spectra with a large natural abundance signal background which...