Low temperature solid-state NMR experiments of half-integer quadrupolar nuclides: caveats and data analysis.
Solid-state NMR spectroscopy of half-integer quadrupolar nuclides has received a lot of interest recently with the advent of new methodologies and higher magnetic fields. We present here the extension of our previous low temperature method to an 18.8T system. This new probe entailed a total redesign including a cross coil and variable capacitors that are operational at cryogenic temperatures. The limitations to sensitivity are also discussed; including a new diode network, the utilization of a cryogenic band pass filter, and the consequences of the RF profiles of the coil. Further, details of the spectroscopy of quadrupolar nuclei in a protein are discussed, such as the observation of the outer transitions and how to distinguish them from the desired +/-1/2 transition.
Lipton
Andrew S
AS
Macromolecular Structure and Dynamics Directorate, WR Wiley Environmental Molecular Sciences Laboratory, Pacific Northwest National Laboratory, Richland, WA 99352, USA.
Heck
Robert W
RW
Sears
Jesse A
JA
Ellis
Paul D
PD