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Synthesis, Structure, and Nonrigidity of Os7(CO)20(CNBut)

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Abstract

The cluster Os7(CO)20(CNBut) (1) has been prepared in ∼25% yield by the reaction of Os6(CO)18 with Me3NO and Os(CO)4(CNBut) at −78°C. The crystal structure of 1 reveals the expected capped octahedral arrangement of metal atoms with the noncarbonyl ligand attached to the capping Os atom. The OsOs lengths in the two independent molecules in the unit cell are in the range 2.823(1)–2.922(1) Å, with the longer bonds associated with the Os3 triangle farthest from the capping Os atom. The 13C NMR spectrum of 1 in solution at room temperature has a 3:3:1 pattern that is consistent with rotation of the individual Os(CO)2(L) (L=CO or CNBut) groups in the cluster. This in turn supports the idea that the capping Os(CO)2(CNBut) unit binds to the central Os6 via a centrally directed MO plus two tangential molecular orbitals.

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Correspondence to Roland K. Pomeroy.

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Wilcox, C.T., Jennings, M.C. & Pomeroy, R.K. Synthesis, Structure, and Nonrigidity of Os7(CO)20(CNBut). Journal of Cluster Science 15, 107–117 (2004). https://doi.org/10.1023/B:JOCL.0000027396.40533.6d

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