HRMAS: TOCSY-HSQC with DIPSI2

Citation

A.G. Palmer III, J. Cavanagh, P.E. Wright & M. Rance, J. Magn. Reson. 93, 151-170 (1991) https://www.sciencedirect.com/science/article/pii/002223649190036S L.E. Kay, P. Keifer & T. Saarinen, J. Am. Chem. Soc. 114, 10663-5 (1992) (https://pubs.acs.org/doi/abs/10.1021/ja00052a088](https://pubs.acs.org/doi/abs/10.1021/ja00052a088) J. Schleucher, M. Schwendinger, M. Sattler, P. Schmidt, O. Schedletzky, S.J. Glaser, O.W. Sorensen & C. Griesinger, J. Biomol. NMR 4, 301-306 (1994) [https://www.ncbi.nlm.nih.gov/pubmed/8019138]https://www.ncbi.nlm.nih.gov/pubmed/8019138)

Protocol

to improve amide signal - use fractionally 2H (at Calpha) Kcsa at pH 3.5 8 resolved resonance at pH 6.5 and 40 resolved resonance at pH 3.5

DIPSI length: 12ms - no crosspeaks 50ms - a couple of crosspeaks 75ms - more crosspeaks.

DIPSI should be rotor synchronized (N x spinning frequency, N=1,2)

Samples

The experiments were performed with a precipitated fractionally deuterated U-13C/15N KcsA, LPR =1, 9:1 DOPE-DOPS D2O citrate buffer pH 3.5

Processing and analysis

Pulse Sequence and Parameter Set