A H anisotropic-isotropic chemical shift correlation experiment which employs symmetry-based recoupling sequences to reintroduce the chemical shift anisotropy in ν and ultrafast MAS to resolve H sites in ν is described. This experiment is used to measure H shift parameters for L-ascorbic acid, a compound with a relatively complex hydrogen-bonding network in the solid. The H CSAs of hydrogen-bonded sites with resolved isotropic shifts can be extracted directly from the recoupled lineshapes. In combination with DFT calculations, hydrogen positions in crystal structures obtained from X-ray and neutron diffraction are refined by comparison with simulations of the full two-dimensional NMR spectrum. The improved resolution afforded by the second dimension allows even unresolved hydrogen-bonded sites H to be assigned and their shift parameters to be obtained.
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