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Carbonylation of the hafnocene dinitrogen complex, [Me2Si(η5-C5Me4)(η5-C5H3-tBu)Hf]2(μ2, η2, η2-N2), yields the corresponding hafnocene oxamidide compound, arising from N2 cleavage with concomitant C–C and C–N bond formation. Monitoring the addition of 4 atm of CO by NMR spectroscopy allowed observation of an intermediate hafnocene complex with terminal and bridging isocyanates and a terminal carbonyl. 13C labeling studies revealed that the carbonyl is the most substitutionally labile ligand in the intermediate and that N–C bond formation in the bridging isocyanate is reversible. No exchange was observed with the terminal isocyanate. Kinetic data established that the conversion of the intermediate to the hafnocene oxamidide was not appreciably inhibited by carbon monoxide and support a pathway involving rate-determining C–C coupling of the isocyanate ligands. Addition of methyl iodide to the intermediate hafnocene resulted in additional carbon–carbon bond formation arising from CO homologation following n...
| Authors: | Donald J. Knobloch; Scott P. Semproni; Emil Lobkovsky; Paul J. Chirik | |
| Journal: | Journal of the American Chemical Society | |
| Year: | 2012 | |
| DOI: | 10.1021/ja208562d | |
| Publication date: | 10-02-2012 |
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