The synthesis of seven new complexes of mixed ligands and metals are reported. Their stoichiometries (metals:ligands) were found to be 1:3, 2:2 and 3:2 corresponding to FeL12L2H, M2L1L2 and M’M2L1L2, respectively (where M’ = Cu2+, M = Cu2+, Co2+ or Ni2+; HL1 = Methyl Red; H2L2 = Alizarin Yellow R). The complexes were characterized by elemental analysis, infrared and Nujol mull electronic spectra and magnetic moment measurements. The results of the electrical conductivity studies for the prepared complexes in the solid state (using compressed tablets) indicated reasonable semiconducting properties. The magnitude of these values, log sigma291 lay between -5.46 and -8.67, resulting from the structure and nature of the substituent of the two mixed ligands as well as the high metallic content of their complexes.