Solid-State NMR Structure Determination from Diagonal-Compensated, Sparsely Nonuniform-Sampled 4D Proton–Proton Restraints
Identifieur interne : 001B86 ( Ncbi/Checkpoint ); précédent : 001B85; suivant : 001B87Solid-State NMR Structure Determination from Diagonal-Compensated, Sparsely Nonuniform-Sampled 4D Proton–Proton Restraints
Auteurs : Rasmus Linser [Allemagne, États-Unis, Australie] ; Benjamin Bardiaux [France] ; Loren X0a B. Andreas [France] ; Sven G. Hyberts [États-Unis] ; Vanessa K. Morris [Australie] ; Guido Pintacuda [France] ; Margaret Sunde [Australie] ; Ann H. Kwan [Australie] ; Gerhard Wagner [États-Unis]Source :
- Journal of the American Chemical Society [ 0002-7863 ] ; 2014.
Abstract
We report acquisition of diagonal-compensated protein structural restraints from four-dimensional solid-state NMR spectra on extensively deuterated and 1H back-exchanged proteins. To achieve this, we use homonuclear 1H–1H correlations with diagonal suppression and nonuniform sampling (NUS). Suppression of the diagonal allows the accurate identification of cross-peaks which are otherwise obscured by the strong autocorrelation or whose intensity is biased due to partial overlap with the diagonal. The approach results in unambiguous spectral interpretation and relatively few but reliable restraints for structure calculation. In addition, the diagonal suppression produces a spectrum with low dynamic range for which ultrasparse NUS data sets can be readily reconstructed, allowing straightforward application of NUS with only 2% sampling density with the advantage of more heavily sampling time-domain regions of high signal intensity. The method is demonstrated here for two proteins, α-spectrin SH3 microcrystals and hydrophobin functional amyloids. For the case of SH3, suppression of the diagonal results in facilitated identification of unambiguous restraints and improvement of the quality of the calculated structural ensemble compared to nondiagonal-suppressed 4D spectra. For the only partly assigned hydrophobin rodlets, the structure is yet unknown. Applied to this protein of biological significance with large inhomogeneous broadening, the method allows identification of unambiguous crosspeaks that are otherwise obscured by the diagonal.
Url:
DOI: 10.1021/ja504603g
PubMed: 24988008
PubMed Central: 4132958
Affiliations:
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Sparsely Nonuniform-Sampled 4D Proton–Proton Restraints</title>
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<sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Solid-State
NMR Structure Determination from Diagonal-Compensated,
Sparsely Nonuniform-Sampled 4D Proton–Proton Restraints</title>
<author><name sortKey="Linser, Rasmus" sort="Linser, Rasmus" uniqKey="Linser R" first="Rasmus" last="Linser">Rasmus Linser</name>
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<affiliation wicri:level="1"><nlm:aff id="aff1">Department of Biological Chemistry and Molecular Pharmacology,<institution>Harvard Medical School</institution>
, Boston, Massachusetts 02115,<country>United States</country>
</nlm:aff>
<country xml:lang="fr">États-Unis</country>
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<affiliation wicri:level="1"><nlm:aff id="aff2">School of Chemistry,<institution>University of New South Wales</institution>
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<country xml:lang="fr">Australie</country>
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<author><name sortKey="Bardiaux, Benjamin" sort="Bardiaux, Benjamin" uniqKey="Bardiaux B" first="Benjamin" last="Bardiaux">Benjamin Bardiaux</name>
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, Paris CEDEX 15,<country>France</country>
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<country xml:lang="fr">France</country>
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<author><name sortKey="Andreas, Loren X0a B" sort="Andreas, Loren X0a B" uniqKey="Andreas L" first="Loren X0a B." last="Andreas">Loren X0a B. Andreas</name>
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<author><name sortKey="Hyberts, Sven G" sort="Hyberts, Sven G" uniqKey="Hyberts S" first="Sven G." last="Hyberts">Sven G. Hyberts</name>
<affiliation wicri:level="1"><nlm:aff id="aff1">Department of Biological Chemistry and Molecular Pharmacology,<institution>Harvard Medical School</institution>
, Boston, Massachusetts 02115,<country>United States</country>
</nlm:aff>
<country xml:lang="fr">États-Unis</country>
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<author><name sortKey="Morris, Vanessa K" sort="Morris, Vanessa K" uniqKey="Morris V" first="Vanessa K." last="Morris">Vanessa K. Morris</name>
<affiliation wicri:level="1"><nlm:aff id="aff5">School of Medical Sciences and School of Molecular Bioscience,<institution>University of Sydney</institution>
, Sydney NSW 2006,<country>Australia</country>
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<country xml:lang="fr">Australie</country>
<wicri:regionArea># see nlm:aff country strict</wicri:regionArea>
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<author><name sortKey="Pintacuda, Guido" sort="Pintacuda, Guido" uniqKey="Pintacuda G" first="Guido" last="Pintacuda">Guido Pintacuda</name>
<affiliation wicri:level="1"><nlm:aff id="aff4"><institution>Institut des Sciences Analytiques, UMR 5280 CNRS/Ecole Normale Supérieure de Lyon/Université de Lyon 1</institution>
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</nlm:aff>
<country xml:lang="fr">France</country>
<wicri:regionArea># see nlm:aff country strict</wicri:regionArea>
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<author><name sortKey="Sunde, Margaret" sort="Sunde, Margaret" uniqKey="Sunde M" first="Margaret" last="Sunde">Margaret Sunde</name>
<affiliation wicri:level="1"><nlm:aff id="aff5">School of Medical Sciences and School of Molecular Bioscience,<institution>University of Sydney</institution>
, Sydney NSW 2006,<country>Australia</country>
</nlm:aff>
<country xml:lang="fr">Australie</country>
<wicri:regionArea># see nlm:aff country strict</wicri:regionArea>
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<author><name sortKey="Kwan, Ann H" sort="Kwan, Ann H" uniqKey="Kwan A" first="Ann H." last="Kwan">Ann H. Kwan</name>
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, Sydney NSW 2006,<country>Australia</country>
</nlm:aff>
<country xml:lang="fr">Australie</country>
<wicri:regionArea># see nlm:aff country strict</wicri:regionArea>
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<author><name sortKey="Wagner, Gerhard" sort="Wagner, Gerhard" uniqKey="Wagner G" first="Gerhard" last="Wagner">Gerhard Wagner</name>
<affiliation wicri:level="1"><nlm:aff id="aff1">Department of Biological Chemistry and Molecular Pharmacology,<institution>Harvard Medical School</institution>
, Boston, Massachusetts 02115,<country>United States</country>
</nlm:aff>
<country xml:lang="fr">États-Unis</country>
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<series><title level="j">Journal of the American Chemical Society</title>
<idno type="ISSN">0002-7863</idno>
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<imprint><date when="2014">2014</date>
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<front><div type="abstract" xml:lang="en"><p content-type="toc-graphic"><graphic xlink:href="ja-2014-04603g_0006" id="ab-tgr1"></graphic>
</p>
<p>We report acquisition of diagonal-compensated
protein structural
restraints from four-dimensional solid-state NMR spectra on extensively
deuterated and <sup>1</sup>
H back-exchanged proteins. To achieve this,
we use homonuclear <sup>1</sup>
H–<sup>1</sup>
H correlations
with diagonal suppression and nonuniform sampling (NUS). Suppression
of the diagonal allows the accurate identification of cross-peaks
which are otherwise obscured by the strong autocorrelation or whose
intensity is biased due to partial overlap with the diagonal. The
approach results in unambiguous spectral interpretation and relatively
few but reliable restraints for structure calculation. In addition,
the diagonal suppression produces a spectrum with low dynamic range
for which ultrasparse NUS data sets can be readily reconstructed,
allowing straightforward application of NUS with only 2% sampling
density with the advantage of more heavily sampling time-domain regions
of high signal intensity. The method is demonstrated here for two
proteins, α-spectrin SH3 microcrystals and hydrophobin functional
amyloids. For the case of SH3, suppression of the diagonal results
in facilitated identification of unambiguous restraints and improvement
of the quality of the calculated structural ensemble compared to nondiagonal-suppressed
4D spectra. For the only partly assigned hydrophobin rodlets, the
structure is yet unknown. Applied to this protein of biological significance
with large inhomogeneous broadening, the method allows identification
of unambiguous crosspeaks that are otherwise obscured by the diagonal.</p>
</div>
</front>
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<affiliations><list><country><li>Allemagne</li>
<li>Australie</li>
<li>France</li>
<li>États-Unis</li>
</country>
</list>
<tree><country name="Allemagne"><noRegion><name sortKey="Linser, Rasmus" sort="Linser, Rasmus" uniqKey="Linser R" first="Rasmus" last="Linser">Rasmus Linser</name>
</noRegion>
</country>
<country name="États-Unis"><noRegion><name sortKey="Linser, Rasmus" sort="Linser, Rasmus" uniqKey="Linser R" first="Rasmus" last="Linser">Rasmus Linser</name>
</noRegion>
<name sortKey="Hyberts, Sven G" sort="Hyberts, Sven G" uniqKey="Hyberts S" first="Sven G." last="Hyberts">Sven G. Hyberts</name>
<name sortKey="Wagner, Gerhard" sort="Wagner, Gerhard" uniqKey="Wagner G" first="Gerhard" last="Wagner">Gerhard Wagner</name>
</country>
<country name="Australie"><noRegion><name sortKey="Linser, Rasmus" sort="Linser, Rasmus" uniqKey="Linser R" first="Rasmus" last="Linser">Rasmus Linser</name>
</noRegion>
<name sortKey="Kwan, Ann H" sort="Kwan, Ann H" uniqKey="Kwan A" first="Ann H." last="Kwan">Ann H. Kwan</name>
<name sortKey="Morris, Vanessa K" sort="Morris, Vanessa K" uniqKey="Morris V" first="Vanessa K." last="Morris">Vanessa K. Morris</name>
<name sortKey="Sunde, Margaret" sort="Sunde, Margaret" uniqKey="Sunde M" first="Margaret" last="Sunde">Margaret Sunde</name>
</country>
<country name="France"><noRegion><name sortKey="Bardiaux, Benjamin" sort="Bardiaux, Benjamin" uniqKey="Bardiaux B" first="Benjamin" last="Bardiaux">Benjamin Bardiaux</name>
</noRegion>
<name sortKey="Andreas, Loren X0a B" sort="Andreas, Loren X0a B" uniqKey="Andreas L" first="Loren X0a B." last="Andreas">Loren X0a B. Andreas</name>
<name sortKey="Pintacuda, Guido" sort="Pintacuda, Guido" uniqKey="Pintacuda G" first="Guido" last="Pintacuda">Guido Pintacuda</name>
</country>
</tree>
</affiliations>
</record>
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