TY - JOUR
T1 - On the measurement of 15N-{1H} nuclear Overhauser effects. 2. Effects of the saturation scheme and water signal suppression
AU - Ferrage, Fabien
AU - Reichel, Amy
AU - Battacharya, Shibani
AU - Cowburn, David
AU - Ghose, Ranajeet
N1 - Funding Information:
We thank Geoffrey Bodenhausen for his careful reading of and critical comments on this manuscript. This work has been partially supported by a Grant MCB0843141 from the National Science Foundation . A grant from the NIH 5G12 RR03060 is acknowledged for partial support of the core facilities at CCNY. FF, SB, DC and RG are members of the New York Structural Biology Center, a STAR center supported by the New York State Office for Science, Technology and Academic Research.
PY - 2010/12
Y1 - 2010/12
N2 - Measurement of steady-state 15N-{1H} nuclear Overhauser effects forms a cornerstone of most methods to determine protein backbone dynamics from spin-relaxation data, since it is the most reliable probe of very fast motions on the ps-ns timescale. We have, in two previous publications (J. Magn. Reson. 192 (2008) 302-313; J. Am. Chem. Soc. 131 (2009) 6048-6049) reevaluated spin-dynamics during steady-state (or "saturated") and reference experiments, both of which are required to determine the NOE ratio. Here we assess the performance of several windowed and windowless sequences to achieve effective saturation of protons in steady-state experiments. We also evaluate the influence of the residual water signal due to radiation damping on the NOE ratio. We suggest a recipe that allows one to determine steady-state 15N-{1H} NOE's without artifacts and with the highest possible accuracy.
AB - Measurement of steady-state 15N-{1H} nuclear Overhauser effects forms a cornerstone of most methods to determine protein backbone dynamics from spin-relaxation data, since it is the most reliable probe of very fast motions on the ps-ns timescale. We have, in two previous publications (J. Magn. Reson. 192 (2008) 302-313; J. Am. Chem. Soc. 131 (2009) 6048-6049) reevaluated spin-dynamics during steady-state (or "saturated") and reference experiments, both of which are required to determine the NOE ratio. Here we assess the performance of several windowed and windowless sequences to achieve effective saturation of protons in steady-state experiments. We also evaluate the influence of the residual water signal due to radiation damping on the NOE ratio. We suggest a recipe that allows one to determine steady-state 15N-{1H} NOE's without artifacts and with the highest possible accuracy.
KW - Composite-pulse decoupling
KW - Homogeneous master equation
KW - Nuclear Overhauser effect
KW - Protein dynamics
KW - Radiation damping
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U2 - 10.1016/j.jmr.2010.09.014
DO - 10.1016/j.jmr.2010.09.014
M3 - Article
C2 - 20951618
AN - SCOPUS:78649444679
SN - 1090-7807
VL - 207
SP - 294
EP - 303
JO - Journal of Magnetic Resonance
JF - Journal of Magnetic Resonance
IS - 2
ER -