Comparative analysis of NMR spectral parameters and molecular dynamics of 1:6‐anhydro‐3:4‐thia‐2‐ O ‐tosyl‐β‐ D ‐allopyranose and 1,6:3,4‐dianhydro‐2‐ O ‐tosyl‐β‐ D ‐galactopyranose in the solid phase

A search of x‐ray data for 1:6‐anhydro‐3:4‐thia‐2‐ O ‐tosyl‐β‐ D ‐allopyranose ( 1 ) and 1:6,3:4‐dianhydro‐2‐ O ‐tosyl‐β‐ D ‐galactopyranose ( 2 ) revealed two CH·O intermolecular contacts for both compounds and one CH·S interaction for 1 . Inspection of hydrogen bonding showed that these interactions are stronger for 2 . The 13 C relaxation times in the rotating frame, 13 C T * 1ρ , measured at B 1 =36.7 kHz showed apparent differences in internal molecular motion on the kilohertz scale for both samples. A PASS‐2D experiment recorded at a spinning rate of 1 kHz was performed to establish the values of principal elements of chemical shift tensors 13 C δ ii . DFT GIAO calculations of shielding parameters were carried out and the orientations of 13 C δ ii were assigned. An attempt to correlate 13 C NMR spectral parameters and molecular dynamics in the solid state with structure, internal motion and intermolecular interactions is presented. Copyright © 2005 John Wiley & Sons, Ltd.