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2 H QUOSY 2D‐NMR Experiments in Weakly Aligning Systems: From the Conventional to the Ultrafast Approach
Author(s) -
Gouilleux Boris,
Meddour Abdelkrim,
Lesot Philippe
Publication year - 2020
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.202000336
Subject(s) - homonuclear molecule , chemistry , deuterium , nuclear magnetic resonance spectroscopy , anisotropy , pulse sequence , spectroscopy , two dimensional nuclear magnetic resonance spectroscopy , analytical chemistry (journal) , nmr spectra database , ultrashort pulse , chemical shift , spectral line , deuterium nmr , nuclear magnetic resonance , crystallography , stereochemistry , atomic physics , physics , molecule , laser , optics , organic chemistry , quantum mechanics , astronomy
We describe three anisotropic ultrafast (UF) QUadrupolar Ordered SpectroscopY (QUOSY) 2D‐NMR experiments (referred to as ADUF 2D NMR spectroscopy) designed for recording the 2 H homonuclear 2D spectra of weakly aligned (deuterated) solutes in sub‐second experiment times. These new ADUF 2D experiments derive from the Q ‐COSY, Q ‐resolved and Q ‐DQ 2D pulse sequences ( J. Am. Chem. Soc . 1999 , 121 , 5249) and allow the correlation between the two components of each quadrupolar doublet, and then their assignment on the basis of 2 H chemical shifts. The UF 2D pulse sequences are analyzed by using the Cartesian spin‐operator formalism for spin I =1 nuclei with a small quadrupolar moment. The optimal experimental/practical conditions as well as the resolution, sensitivity and quantification issues of these ADUF 2D experiments are discussed on comparison to their conventional 2D counterparts and their analytical potentialities. Illustrative ADUF 2D experiments using deuterated achiral/prochiral/chiral solutes in poly‐γ‐benzyl ‐L ‐glutamate based chiral liquid crystals are presented, as well as the first examples of natural abundance deuterium (ANADUF) 2D spectrum using 14.1 T magnetic field and a basic gradient unit (53 G.cm −1 ) in oriented solvents.