Molecular dynamics as studied by static-powder and magic-angle spinning 2H NMR.
The 2H NMR magic-angle spinning (MAS) technique is compared to the static-powder quadrupole echo (QE) and Jeener-Brockaert (JB) pulse sequences for a quantitative investigation of molecular dynamics in solids. The linewidth of individual spinning sidebands of the one-dimensional MAS spectra are observed to be characteristic of the correlation time from approximately 10(-2) to approximately 10(-8) s so that the dynamic range is increased by approximately three orders of magnitude when compared to the QE experiment. As a consequence, MAS 2H NMR is found to be more sensitive to the presence of an inhomogeneous distribution of correlation times than the QE and JB experiments which rely upon lineshape distortions due to anisotropic T2 and T1Q relaxation, respectively. All these results are demonstrated experimentally and numerically using the two-site flip motion of dimethyl sulfone and of the nitrobenzene guest in the alpha-p-tert-butylcalix[4]arene-nitrobenzene inclusion compound.
Hologne
Maggy
M
Institut de Chimie, FRE 2446 CNRS, Université Louis Pasteur, BP 296, 67008 Strasbourg, Cedex, France.
Hirschinger
J Jérôme
JJ
D003198:Computer Simulation; D003461:Crystallography / Q000379:methods*; D003903:Deuterium; D004121:Dimethyl Sulfoxide; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008958:Models, Molecular; D009038:Motion; D009578:Nitrobenzenes / Q000737:chemistry*; D011208:Powders / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013113:Spin Labels; D013450:Sulfones / Q000737:chemistry*
D009578:Nitrobenzenes; D011208:Powders; D013113:Spin Labels; D013450:Sulfones; C025910:dimethyl sulfone; D003903:Deuterium; D004121:Dimethyl Sulfoxide