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Reduction and subsequent oxidation of Mo(CO)4(DAB) (DAB = 1,4-diazabutadiene = -diimine) yield complexes with the formula Mo2(CO)6(IAE) (IAE = q-(l-(isopropylamino)-2-(isopropylimino)ethane-A,Ar)). Several methods were developed for the preparation of Mo2(CO)6(IAE) of which one involves a cyclic process with respect to Mn2(CO)10 and one a pseudocatalytic process with Hg2+ as catalyst. All methods have in common the oxidative elimination of CO from (Mo(CO)4(DAB))l resulting in the generation of the coordinative unsaturated Mo(CO)3(DAB) intermediate for which a structure containing a , -coordinated DAB ligand has been proposed. Dimerization of these 16-electron species yield the Mo2(CO)6(IAE) complexes. The X-ray crystal structure for the isopropyl derivative showed the formation of a carbon-carbon bond between two DAB ligands (1.61 (2) Á) and the formation of a short Mo-Mo single bond (2.813 (3) Á). The crystal was orthorhombic with space group R22,21 and cell constants a = 8.190 (1) Á, b = 10.099 (2) Á, c = 16.844 (2) A, and Z = 2.