Reaction of [Au(DAPTA)(Cl)] with RaaiR' in CH(2)Cl(2) medium following ligand addition leads to [Au(DAPTA)(RaaiR')](Cl) [DAPTA = diacetyl-1,3,5-triaza-7-phosphaadamantane, RaaiR' = p-R-C(6)H(4)-N = NC(3)H(2)-NN-1-R ', (1-3), abbreviated as N,N '-chelator, where N(imidazole) and N(azo) represent N and N ', respectively; R = H (a), Me (b), Cl (c) and R '= Me (1), CHCH(3)(2), CH(2)Ph (3)]. The (1)H NMR spectral measurements D(2)O suggest methylene, CH(2), in RaaiEt gives a complex AB type multiplet while in RaaiCH(2)Ph it shows AB type quarters. (13)C NMR spectrum in DO suggest the molecular skeleton. The (1)H-(1)H COSY spectrum in D(2)O as well as contour peaks in the (1)H-(13)C HMQC spectrum in D(2)O assign the solution structure.