2D 13C-13C SARCOSY 16

This is NYSBC standard data set and pulse program for 13C-13C 2D SARCOSY with 16 step phase cycle The pulse program has power safety limitations specific for the particular probe. The pulse program DARR_3.2EF750.nysbc, ramp shape file tancn_100_SCALE and include file power_intro.incl are located in the dataset directory.

Citation

https://pubs.rsc.org/en/content/articlelanding/2009/CP/b818867j#!divAbstract Sensitivity absorptive scalar correlation NMR spectroscopy in solids, D. Lee, J. Struppe, D.W. Elliott, L.J. Mueller, J.J. Titman, JCCP 11, 2009, 3547-3553

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

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

Protocol

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