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Two‐Dimensional Double‐Quantum 2 H NMR Spectroscopy in the Solid State under OMAS Conditions: Correlating 2 H Chemical Shifts with Quasistatic Line Shapes
Author(s) -
Hoffmann Anke,
Schnell Ingo
Publication year - 2004
Publication title -
chemphyschem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.016
H-Index - 140
eISSN - 1439-7641
pISSN - 1439-4235
DOI - 10.1002/cphc.200301215
Subject(s) - spectroscopy , quasistatic process , chemistry , chemical shift , nuclear magnetic resonance spectroscopy , line (geometry) , analytical chemistry (journal) , atomic physics , solid state nuclear magnetic resonance , physics , nuclear magnetic resonance , thermodynamics , quantum mechanics , stereochemistry , mathematics , chromatography , geometry
Solid‐state 2 H NMR spectroscopy is a well‐established and versatile method to study molecular orientation and dynamics in selectively deuterated samples. Herein, we introduce a 2D 2 H double‐quantum (DQ) NMR experiment performed under fast magic‐angle spinning with a slight offset of the magic angle (OMAS). The experiment combines 2 H chemical‐shift resolution with DQ‐filtered quasistatic 2 H line shapes. In this way, it is possible to separate 2 H resonances and to independently determine 2 H quadrupole couplings at multiple sites. While 2 H chemical shifts are resolved in the 2 H DQ dimension, the quadrupole parameters can be obtained from characteristic line shapes which are reintroduced in the second dimension by the magic‐angle offset. The 2D 2 H DQ OMAS experiment is demonstrated on L ‐histidine which was deuterated at multiple sites by recrystallisation from D 2 O.