MAS dependent sensitivity of different isotopomers in selectively methyl protonated protein samples in solid state NMR.
J. Biomol. NMR 73, 625-631 (2019)
Sensitivity and resolution together determine the quality of NMR spectra in biological solids. For high-resolution structure determination with solid-state NMR, proton-detection emerged as an attractive strategy in the last few years. Recent progress in probe technology has extended the range of available MAS frequencies up to above 100 kHz, enabling the detection of resolved resonances from sidechain protons, which are important reporters of structure. Here we characterise the interplay between MAS frequency in the newly available range of 70-110 kHz and proton content on the spectral quality obtainable on a 1 GHz spectrometer for methyl resonances. Variable degrees of proton densities are tested on microcrystalline samples of the alpha-spectrin SH3 domain with selectively protonated methyl isotopomers (CH3, CH2D, CHD2) in a perdeuterated matrix. The experimental results are supported by simulations that allow the prediction of the sensitivity outside this experimental frequency window. Our results facilitate the selection of the appropriate labelling scheme at a given MAS rotation frequency.
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Publikationstyp
Artikel: Journalartikel
Dokumenttyp
Wissenschaftlicher Artikel
Typ der Hochschulschrift
Herausgeber
Schlagwörter
Solid State Nmr ; Magic Angle Spinning (mas) ; Selective Deuteration ; Ch3 Labelling ; Methyl Isotopomers ; Microcrystalline Proteins; High-resolution; 100 Khz; Perdeuterated Proteins; Resonance Assignment; Spectroscopy; Spectra; Enhancement
Keywords plus
Sprache
englisch
Veröffentlichungsjahr
2019
Prepublished im Jahr
HGF-Berichtsjahr
2019
ISSN (print) / ISBN
0925-2738
e-ISSN
1573-5001
ISBN
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Konferenztitel
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Konferenzort
Konferenzband
Quellenangaben
Band: 73,
Heft: 10-11,
Seiten: 625-631
Artikelnummer: ,
Supplement: ,
Reihe
Verlag
Springer
Verlagsort
Van Godewijckstraat 30, 3311 Gz Dordrecht, Netherlands
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0000-00-00
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Prüfer
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0000-00-00
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0000-00-00
Anmelder/Inhaber
weitere Inhaber
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Priorität
Begutachtungsstatus
Peer reviewed
POF Topic(s)
30203 - Molecular Targets and Therapies
Forschungsfeld(er)
Enabling and Novel Technologies
PSP-Element(e)
G-503090-001
Förderungen
Copyright
Erfassungsdatum
2019-09-26