Heterobimetallic nickel and molybdenum complexes of the composition [Ni(L)MoO2(A)(4)]center dot nH(2)O (A = H2O (1), py (2), 2-pic (3), 3-pic (4), and 4-pic (5); n = 0,2) and [Ni(L)(MoO2)(BB)(2)](BB = bpy (6) and (phen (7)) have been synthesized from the multidentate ligand disalicylaldehyde oxaloyldihydrazone (H4L) in methanol. The composition of the complexes has been established based on data obtained from elemental analyses, thermoanalytical, mass spectral and molecular weight studies. The probable structures of the complexes have been discussed in the light of molar conductance, magnetic moment data and electronic. EPR and infrared spectral studies. In all of the complexes, the dihydrazone is present in enol form and coordinates to the metal centre as a tetrabasic hexadentate ligand. All of the complexes are normal paramagnetic to the extent of two unpaired electrons per nickel atom. The mu(eff) values for the complexes lying in the region 2.87-3.07 B.M. are consistent with the octahedral stereochernistry of nickel(II) in the heterobimetallic complexes. The EPR and electronic spectral data also support the distorted octahedral stereochemistry of the nickel(II) centre. Both nickel and molybdenum have octahedral geometry in the complexes. (C) 2011 Elsevier B.V. All rights reserved.