We present two sequences which combine ((1)H,(15)N) and ((15)N,(13)C) selective cross-polarization steps with an efficient variant of the J-based homonuclear transfer scheme, in which a spin-state-selective (S(3)E) block is incorporated to improve both resolution and sensitivity in the direct (13)C dimension. We propose these two sequences as a part of a suite of four N-C correlation experiments allowing for the assignment of protein backbone resonances in the solid state. We illustrate these experiments under ultra-fast magic angle spinning conditions on two samples of microcrystalline dimeric human superoxide dismutase (SOD, 153×2 amino acids), in its diamagnetic ("empty", Zn(II)) and paramagnetic (Cu(II), Zn(II)) states.

13C-Detected Through-Bond Correlation Experiments for Protein Resonance Assignment by Ultra-Fast MAS Solid-State NMR / Emeline Barbet-Massin;Andrew J. Pell;Michael J. Knight;Amy L. Webber;Isabella C. Felli;Roberta Pierattelli;Lyndon Emsley;Anne Lesage;Guido Pintacuda. - In: CHEMPHYSCHEM. - ISSN 1439-4235. - STAMPA. - 14:(2013), pp. 331-337. [10.1002/cphc.201201097]

13C-Detected Through-Bond Correlation Experiments for Protein Resonance Assignment by Ultra-Fast MAS Solid-State NMR

FELLI, ISABELLA CATERINA;PIERATTELLI, ROBERTA;
2013

Abstract

We present two sequences which combine ((1)H,(15)N) and ((15)N,(13)C) selective cross-polarization steps with an efficient variant of the J-based homonuclear transfer scheme, in which a spin-state-selective (S(3)E) block is incorporated to improve both resolution and sensitivity in the direct (13)C dimension. We propose these two sequences as a part of a suite of four N-C correlation experiments allowing for the assignment of protein backbone resonances in the solid state. We illustrate these experiments under ultra-fast magic angle spinning conditions on two samples of microcrystalline dimeric human superoxide dismutase (SOD, 153×2 amino acids), in its diamagnetic ("empty", Zn(II)) and paramagnetic (Cu(II), Zn(II)) states.
14
331
337
Emeline Barbet-Massin;Andrew J. Pell;Michael J. Knight;Amy L. Webber;Isabella C. Felli;Roberta Pierattelli;Lyndon Emsley;Anne Lesage;Guido Pintacuda
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/2158/817121
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