13C-detected 1H–2H separated local field NMR spectroscopy

We present a new NMR method for measuring 1H–2H dipolar couplings in macroscopically oriented media. To overcome the lack of dipolar resolution in 1D 1H and 2H spectra of deuterated molecules, we use a 2D heteronuclear correlation experiment where 1H chemical shifts and 1H–2H dipolar interactions in the first dimension are correlated with 13C chemical shifts and 2H–13C dipolar interactions in the second dimension. The technique is demonstrated on a columnar liquid-crystalline phase.