Abstract: Some novel manganese(III) complexes with the ligand 2,3-dimethyl-1-phenyl-4-(3-methoxy-2-phenyl azo)5-pyrazolone, GAAP, guaiacol azoantipyrine, L, having the formulae [Mn(L)2(X)3], [Mn(L)2(Y)2Cl], where X = Cl-/ NO3-/ClO4-; Y = NCS- were synthesized and characterized by elemental analysis, molar conductance and magnetic susceptibility measurements and spectral ( IR, UV- Visible, FAB- mass) studies. The ligand was characterized by elemental analysis and spectral (IR, UV- Visible, 1HNMR,) studies. The X-ray diffraction study of the complex [Mn(L)2(Cl)3] indicated that it is not perfectly crystalline. The electrochemical properties of the complex [Mn(L)2(Cl)3] was investigated by cyclic voltammetry. Based on elemental analyses, thermo gravimetric and FAB- mass studies of the complexes a seven coordinate structure is tentatively proposed for the complexes.