Accurate NMR determination of C-H or N-H distances for unlabeled molecules
PBN-AR
Instytucja
Centrum Badań Molekularnych i Makromolekularnych Polskiej Akademii Nauk
Informacje podstawowe
Główny język publikacji
angielski
Czasopismo
SOLID STATE NUCLEAR MAGNETIC RESONANCE
ISSN
0926-2040
EISSN
1527-3326
Wydawca
ACADEMIC PRESS INC ELSEVIER SCIENCE, 525 B ST, STE 1900, SAN DIEGO, CA 92101-4495 USA
DOI
URL
Rok publikacji
2016
Numer zeszytu
Strony od-do
15-21
Numer tomu
73
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+ 3
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Język
angielski
Treść
Cross-Polarization with Variable Contact-time (CP-VC) is very efficient at ultra-fast MAS (nu(R) >= 60 kHz) to measure accurately the dipolar interactions corresponding to C-H or N-H short distances, which are very useful for resonance assignment and for analysis of dynamics. Here, we demonstrate the CP-VC experiment with H-1 detection. In the case of C-H distances, we compare the CP-VC signals with direct (C-13) and indirect (H-1) detection and find that the latter allows a S/N gain of ca. 2.5, which means a gain of ca. 6 in experimental time. The main powerful characteristics of CP-VC methods are related to the ultra-fast spinning speed and to the fact that most of the time only the value of the dipolar peak separation has to be used to obtain the information. As a result, CP-VC methods are: (i) easy to set up and to use, and robust with respect to (ii) rf-inhomogeneity thus allowing the use of full rotor samples, (iii) rf mismatch, and (iv) offsets and chemical shift anisotropies. It must be noted that the CP-VC 2D method with indirect H-1 detection requires the proton resolution and is thus mainly applicable to small or perdeuterated molecules. We also show that an analysis of the dynamics can even be performed, with a reasonable experimental time, on unlabeled samples with C-13 or even N-15 natural abundance. (C) 2015 Elsevier Inc. All rights reserved.
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PX-56c5f26281062a841e96cad0
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