Two-dimensional double-quantum 2H NMR spectroscopy in the solid state under OMAS conditions:: Correlating 2H chemical shifts with quasistatic line shapes

Solid-state H-2 NMR spectroscopy is a well-established and versatile method to study molecular orientation and dynamics in selectively deuterated samples. Herein, we introduce a 2D H-2 double-quantum (DQ) NMR experiment performed under fast magic-angle spinning with a slight offset of the magic angle (OMAS). The experiment combines H-2 chemical-shift resolution with DQ-filtered H-2 line shapes. In this way, it is possible to seperate H-2 resonances and to independantly determine H-2 quadrupole couplings at multiple sites. While H-2 chemical shifts are resolved in the H-2 DQ dimension, the quadrupole parameters can be obtained in the second dimension by the magic angle offset. The 2D H-2 DQ OMAS experiment is demonstrated on L-hisitidine which was deuterated at multiple sites by recrystallization from D2O.