Homonuclear vanadium-51 dipolar couplings in inorganic solids obtained via hahn spin echo decay NMR spectroscopy.
Dipolar dephasing of the magnetization following a Hahn spin echo pulse sequence potentially provides a quantitative means for determining the dipolar second moment in solids. In this work, the possibility of employing Hahn spin echo decay spectroscopy to obtain quantitative 51V-51V dipolar second moments is explored. Theoretical spin echo response curves are compared to experimental ones for a collection of crystalline vanadium-containing compounds. This work suggests that 51V dipolar second moments can be obtained by selectively exciting the central m = 1/2 --> -1/2 by a Hahn echo sequence for vanadate compounds with line broadening no greater than approximately 220 ppm. For vanadates with greater broadening of the central transition due to chemical shift, second-order quadrupolar, and dipolar interactions, off-resonance effects lead to an oscillatory time dependence of the spin echo. Experimentally determined second moments of the normalized echo decay intensities lie within 10-33% of the calculated values if the second moments are extrapolated to zero evolution time due to the time scale dependence of spin exchange among neighboring vanadium nuclei. Alternatively, the second moments can be obtained to within 10-25% of the calculated values if the broadening of the central transition due to chemical shift and second-order quadrupolar effects can be estimated.
Gee
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Department of Chemistry and Biochemistry, Long Island University-Brooklyn Campus, New York 11201, USA.