Photolysis of Mo(CO) 6 in n-heptane solution creates a coordinatiVely unsaturated d 6 species, which interacts with the Si-H bond of Et 2 SiH 2 and leads to the formation of Mo-H and Mo-Si bonds. The formation of a Mo-H bond was corroborated by 1 H NMR spectroscopy due to the detection of a high-field resonance at δ ) -8.33 flanked by 29 Si satellites. The formation of Mo-Si bonds was confirmed by the detection of two sets of 29 Si satellites on the hydride signal, which proVided J Si-H ) 57 and 33 Hz, and by the 29 Si{ 1 H} NMR spectrum, which reVealed a resonance at δ ) 207.7. The latter signal in the 29 Si NMR spectrum was obserVed as a doublet of quintets with 1 J Si-H ) 58 Hz and 2 J Si-H ) 41 Hz. The 95 Mo NMR spectrum showed at high field a resonance at δ ) -3785, characteristic for seVen-coordinate molybdenum compounds. The molecular structure of a noVel bis{(µ-η 2 -hydridodiethylsilyl)tetracarbonylmolybdenum(I)} complex, [{Mo(µ-η 2 -H-SiEt 2 )(CO) 4 } 2 ], was established by single-crystal X-ray diffraction studies. The molybdenum hydride obserVed in the 1 H NMR spectrum was located in the structure at a chemically reasonable position between the Mo and Si atoms of the Mo-Si bonds of the bridging silyl ligand with a Si-H bond length of 1.615(3) Å and that of the Mo-H bond amounting to 1.786(5) Å.
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