Collect. Czech. Chem. Commun. 1992, 57, 2005-2011

Long-Range 2D INADEQUATE in Structure Determination

Jan Schramla, Vratislav Blechtaa and Eduard Krahéb

a Institute of Chemical Process Fundamentals, Czechoslovak Academy of Sciences, 165 02 Prague 6-Suchdol, Czechoslovakia
b Fachhochschule Münster, D-4430, Steinfurt, Germany


It is demonstrated that the 2D INADEQUATE experiment utilizing long-range 13C-13C spin-spin couplings is feasible and that it can solve structural assignment problems when one-bond connectivities do not provide sufficient clue for structure determination. In such cases, the long-range 2D INADEQUATE can be used instead of the standard 2D INADEQUATE since it also yields the one-bond connectivities in addition to the connectivities over more bonds. The two types of connectivities are easily distinguished according to satellite separations. Because of similar magnitudes of various long-range 13C-13C couplings, the method of J-resolved INADEQUATE suggested earlier for such purpose is unlikely to provide unambiguous results. The proposed method is utilized for complete assignment of 13C and 1H NMR spectra of dicyclohexylphenylphosphine.