The photochemical reaction of Mo(CO) 6 with the diethylgermane Et 2 GeH 2 leads to the formation of several new complexes, which were detected by IR and 1 H and 13 C NMR spectroscopy. From the mixture of compounds, a binuclear complex, [{Mo(μ-η 2 -H-GeEt 2 )(CO) 4 } 2 ], was isolated in crystalline form, and its molecular structure was established by single-crystal X-ray diffraction studies. The agostic hydride ligand of the Mo( μ-η 2 -H-GeEt 2 ) group was located in the structure at a chemically reasonable position between the Mo and Ge atoms of the Mo-Ge bond of the bridging germyl ligand, and its presence was confirmed by 1 H NMR spectroscopy due to a proton resonance at δ = -7.86. Two dihydride complexes were identified by 1 H and 13 C NMR spectroscopy, due to their differing thermal behavior. A DFT study of the structural properties of possible reaction products was performed.
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