This is NYSBC standard data set and pulse program for 1H-13C/15N cross polarization with rotor synchronized 13C/15N hahnecho followed by 13C/15N acquisition with 1H decoupling. The pulse program has power safety limitations specific for the particular probe. The pulse program CPECHO_15N_3.2EF750.nysbc and CPECHO_15N_3.2EF750.nysbc, ramp shape file tancn_100_SCALE and include file power_intro.incl are located in the dataset directory.

Sample heating

To minimized heating of conductive samples, we recommend using an Efree/lowE probe. However, a combination of frictional heating from spinning and RF heating on long pulses on both channel may cause substantial sample heating and temperature gradient across the sample even in an Efree probe. The heating may damage the sample. The heating and temperature gradient across the rotor may substantially compromise the precision of measurements and data fitting.

Citation

doi:10.1103/PhysRev.94.630. Carr, H. Y.; Purcell, E. M. (1954). "Effects of Diffusion on Free Precession in Nuclear Magnetic Resonance Experiments". Physical Review. 94 (3): 630–638.

[https://www.sciencedirect.com/science/article/abs/pii/0022236477902761]https://www.sciencedirect.com/science/article/abs/pii/0022236477902761)

https://www.ncbi.nlm.nih.gov/pubmed/10868566?dopt=Abstract Heating of samples induced by fast magic-angle spinning, Brus, J., Solid State Nucl. Magn. Reson. 16, 151–160 (2000).

https://onlinelibrary.wiley.com/doi/abs/10.1002/mrc.4450 Heating and temperature gradients of lipid bilayer samples induced by RF irradiation in MAS solid-state NMR experiments, Wang, J., Zhang, Z., Zhao, W., Wang, L. & Yang, J., Magn. Reson. Chem. 54, 753–759 (2016).

https://www.biorxiv.org/content/10.1101/566729v1.full TmDOTP : An NMR- based Thermometer for Magic Angle Spinning NMR Experiments Dongyu Zhang, Boris Itin, Ann E. McDermott; preprinted

Probe and power limitations

CP experiments require long simultaneous medium to high power pulses on 1H and X channels. Adjust the probe power length and safety limitations in the pulse sequence to follow your probe specifications. When in doubt, contact the manufacturer.

Protocol

Use the experiment to optimize 1H decoupling in protein samples

Samples

The experiments were performed with crystallized u-15N,13C-labeled-N-acetyl-valine and u-15N,13C membrane protein in hydrated lipids.

Processing and analysis

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Pulse Sequence and Parameter Set Pulse Sequence and Parameter Set