Magic-angle spinning structure determination

The use of cross-polarization/magic angle spinning NMR may well become the most powerful method to determine the structure of conjugated acid and bases in the solid state. 

R. C. Anderson, J. P. Stokes and M. J. Shapiro, Structure determination in combinatorial chemistry Utilization of magic angle spinning HMQC and TOCSY NMR spectra in the structure determination of Wang-bound lysine, Tet. Lett., 1995, 36, 5311-5314. 

J. Chin, B. Fell, M. J. Shapiro, J. Tomesch, J. R. Wareing and A. M. Bray, Magic angle spinning NMR for reaction monitoring and structure determination of molecules attached to multipin crowns, J. Org. Chem., 1997, 62, 538-539. 

The 2,2,6,6-tetramethylpiperidinoxyl radical (TEMPO) was first prepared in 1960 by Lebedev and Kazarnovskii by oxidation of its piperidine precursor.18 The steric hindrance of the NO bond in TEMPO makes it a highly stable radical species, resistant to air and moisture. Paramagnetic TEMPO radicals can be employed as powerful spin probes for elucidating the structure and dynamics of both synthetic and biopolymers (e.g., proteins and DNA) by ESR spectroscopy.19 Unlike solid-phase 1H-NMR where magic angle spinning is required in order to reduce the anisotropic effects in the solid-phase environment, solid-phase ESR spectroscopy can be conducted without specialized equipment. Thus, we conducted comparative ESR studies of various polymers with persistent radical labels, and we also determined rotational correlation times as a function of... 

Abstract Membrane proteins represent an important and challenging frontier in structural biology they mediate fundamental and medically important processes but are challenging targets for structure/ function studies. Magic angle spinning solid-state NMR methods for structure determination of proteins have developed rapidly in... 

---