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Experimental and Theoretical Studies of 45Sc NMR Interactions in Solids
Journal of the American Chemical Society (2006)
  • Aaron J. Rossini, University of Windsor
  • Robert W. Schurko, University of Windsor
Solid-state 45Sc NMR spectroscopy, ab initio calculations, and X-ray crystallography are applied to examine the relationships between 45Sc NMR interactions and molecular structure and symmetry. Solid-state 45Sc (I = 7/2) magic-angle spinning (MAS) and static NMR spectra of powdered samples of Sc(acac)3, Sc(TMHD)3, Sc(NO3)3·5H2O, Sc(OAc)3, ScCl3·6H2O, ScCl3·3THF, and ScCp3 have been acquired. These systems provide a variety of scandium coordination environments yielding an array of distinct 45Sc chemical shielding (CS) and electric field gradient (EFG) tensor parameters. Acquisition of spectra at two distinct magnetic fields allows for the first observations of scandium chemical shielding anisotropy (CSA). 45Sc quadrupolar coupling constants (CQ) range from 3.9 to 13.1 MHz and correlate directly with the symmetry of the scandium coordination environment. Single-crystal X-ray structures were determined for Sc(TMHD)3, ScCl3·6H2O, and Sc(NO3)3·5H2O to establish the hitherto unknown scandium coordination environments. A comprehensive series of ab initio calculations of EFG and CS tensor parameters are in excellent agreement with the observed parameters. Theoretically determined orientations of the NMR interaction tensors allow for correlations between NMR tensor characteristics and scandium environments. Solid-state 45Sc, 13C, and 19F NMR experiments are also applied to characterize the structures of the microcrystalline Lewis acid catalyst Sc(OTf)3 (for which the crystal structure is unknown) and a noncrystalline, microencapsulated, polystyrene-supported form of the compound.
Publication Date
July 25, 2006
Publisher Statement
Reprinted (adapted) with permission from Journal of the American Chemical Society, 128(32); 10391-10402. Doi: 10.1021/ja060477w. Copyright 2006 American Chemical Society.
Citation Information
Aaron J. Rossini and Robert W. Schurko. "Experimental and Theoretical Studies of 45Sc NMR Interactions in Solids" Journal of the American Chemical Society Vol. 128 Iss. 32 (2006) p. 10391 - 10402
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