Accurate Determination of 1 H-15 N Dipolar Couplings Using Inaccurate Settings of the Magic Angle in Solid-State NMR Spectroscopy.
Angew Chem Int Ed Engl
; 58(13): 4286-4290, 2019 03 22.
Article
em En
| MEDLINE
| ID: mdl-30694593
ABSTRACT
Magic-angle spinning (MAS) is an essential ingredient in a wide variety of solid-state NMR experiments. The standard procedures to adjust the rotor angle are not highly accurate, resulting in a slight misadjustment of the rotor from the magic angle ( θRL=tan-12 ) on the order of a few millidegrees. This small missetting has no significant impact on the overall spectral resolution, but is sufficient to reintroduce anisotropic interactions. Shown here is that site-specific 1 H-15 N dipolar couplings can be accurately measured in a heavily deuterated protein. This method can be applied at arbitrarily high MAS frequencies, since neither rotor synchronization nor particularly high radiofrequency field strengths are required. The off-MAS method allows the quantification of order parameters for very dynamic residues, which often escape an analysis using existing methods.
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Texto completo:
1
Coleções:
01-internacional
Base de dados:
MEDLINE
Assunto principal:
Isótopos de Carbono
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Espectroscopia de Ressonância Magnética
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Espectrina
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Domínios de Homologia de src
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Ressonância Magnética Nuclear Biomolecular
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Deutério
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Isótopos de Nitrogênio
Limite:
Animals
Idioma:
En
Ano de publicação:
2019
Tipo de documento:
Article