3D DCP DARR

This is NYSBC standard data set and pulse program for DCP DARR 3D The pulse program has power safety limitations specific for the particular probe. The pulse program dbcpDARR3D_3.2EF750.nysbc, ramp shape file tancn_100_SCALE and include file power_intro.incl are located in the dataset directory.

Citation

Cross Polarization in the tilted frame: assignment and spectral simplification in heteronuclear spin systems, Marc Baldus, Aneta Petkova, Judith Herzfeld, Robert Griffin, Journal of Molecular Physics, 1998, 95 (6) p.1197-1207 https://www.tandfonline.com/doi/abs/10.1080/00268979809483251

13C-1H dipolar assisted rotary resonance in magic angle spinning NMR, Takegoshi, K, Nakamura S and Terao, T Chem Phys Lett 2001 (344) pp 631-637 [https://www.sciencedirect.com/science/article/abs/pii/S0009261401007916[(https://www.sciencedirect.com/science/article/abs/pii/S0009261401007916)

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

Use DARR and DCP experiments to set up DCPDARR. Set up magnet field drift compensation. Choose acquisition times in the indirect dimensions for the best resolution/sensitivity compromise.

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