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Probing Noncovalent Interactions by Fast Magic-Angle Spinning NMR at 100 kHz and More.
Chemphyschem
October 2024
Institute of Technical and Macromolecular Chemistry, RWTH Aachen University, Worringerweg 2, 52074, Aachen, Germany.
Noncovalent interactions are the basis for a large number of chemical and biological molecular-recognition processes, such as those occurring in supramolecular chemistry, catalysis, solid-state reactions in mechanochemistry, protein folding, protein-nucleic acid binding, and biomolecular phase separation processes. In this perspective article, some recent developments in probing noncovalent interactions by proton-detected solid-state Nuclear Magnetic Resonance (NMR) spectroscopy at Magic-Angle Spinning (MAS) frequencies of 100 kHz and more are reviewed. The development of MAS rotors with decreasing outer diameters, combined with the development of superconducting magnets operating at high static magnetic-field strengths up to 28.
View Article and Find Full Text PDFMagic-angle spinning NMR structure of Opa60 in lipid bilayers.
J Struct Biol X
June 2024
Department of NMR-based Structural Biology, Max-Planck-Institute for Multidisciplinary Sciences, Am Faßberg 11, 37077 Göttingen, Germany.
Here we report the structure of Opa60 in lipid bilayers using proton-detected magic-angle spinning nuclear magnetic resonance (MAS NMR). Preparations including near-native oligosaccharide lipids reveal a consistent picture of a stable transmembrane beta barrel with a minor increase in the structured region as compared with the previously reported detergent structure. The large variable loops known to interact with host proteins could not be detected, confirming their dynamic nature even in a lipid bilayer environment.
View Article and Find Full Text PDFSolid-state NMR backbone chemical shift assignments of α-synuclein amyloid fibrils at fast MAS regime.
Biomol NMR Assign
December 2024
Latvian Institute of Organic Synthesis, Aizkraukles 21, Riga, LV-1006, Latvia.
The α-synuclein (α-syn) amyloid fibrils are involved in various neurogenerative diseases. Solid-state NMR (ssNMR) has been showed as a powerful tool to study α-syn aggregates. Here, we report the H, C and N back-bone chemical shifts of a new α-syn polymorph obtained using proton-detected ssNMR spectroscopy under fast (95 kHz) magic-angle spinning conditions.
View Article and Find Full Text PDFSedimentation of large, soluble proteins up to 140 kDa for H-detected MAS NMR and C DNP NMR - practical aspects.
J Biomol NMR
September 2024
Leibniz-Forschungsinstitut für Molekulare Pharmakologie, Robert-Rössle-Str. 10, 13125, Berlin, Germany.
Solution NMR is typically applied to biological systems with molecular weights < 40 kDa whereas magic-angle-spinning (MAS) solid-state NMR traditionally targets very large, oligomeric proteins and complexes exceeding 500 kDa in mass, including fibrils and crystalline protein preparations. Here, we propose that the gap between these size regimes can be filled by the approach presented that enables investigation of large, soluble and fully protonated proteins in the range of 40-140 kDa. As a key step, ultracentrifugation produces a highly concentrated, gel-like state, resembling a dense phase in spontaneous liquid-liquid phase separation (LLPS).
View Article and Find Full Text PDFHigh-resolution heteronuclear correlations between spin-1/2 and half-integer quadrupolar nuclei under fast MAS solid-state NMR.
Biophys Chem
July 2024
JEOL Ltd., Musashino, Akishima, Tokyo 196-8558, Japan. Electronic address:
High isotropic resolution is essential for the structural elucidation of samples with multiple sites. In this study, utilizing the benefits of TRAPDOR-based heteronuclear multiple quantum coherence (T-HMQC) and a pair of one rotor period long cosine amplitude modulated low-power (cos-lp) pulse-based symmetric-split-t multiple-quantum magic angle spinning (MQMAS) methods, we have developed a proton-detected 2D Cl/H T-HMQC-MQMAS pulse sequence under fast MAS (70 kHz) to achieve high-resolution in the indirect dimension of the spin-3/2 (Cl) nuclei connected via protons. As T-HMQC polarizes not only single-quantum central transition (SQ) but also triple-quantum (TQ) coherences, the proposed 2D pulse sequence is implemented via selection of two coherence pathways (SQ→TQ →SQ and TQ → SQ→TQ) resulting in the Cl isotropic dimension and is superior to the existing double-quantum satellite-transition (DQ) T-HMQC in terms of resolution.
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