A novel procedure for determining H-1,H-1 NMR dipolar couplings in a dilute liquid crystalline medium based on H-1,H-1 COSY spectroscopy and a J-doubling procedure is presented. Subsequent conformational analysis of the central region of a partially deuterated decasaccharide employing H-1,H-1 and H-1,C-13 dipolar couplings, H-1.H-1 nuclear Overhauser effect spectroscopy, and computer modeling is described. In particular, the use of H-1,H-1 dipolar couplings is of paramount importance in deriving a three-dimensional structure of the decasaccharide.