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Reactions between K[BHBus3] and [Ru3(CO)10(µ-EPh2CH2EPh2)](E = P or As) afford solutions of the dephenylated anions, [Ru3(µ3-EPhCH2EPh2)(CO)9]–, which can be reversibly protonated to give [Ru3(µ-H)(µ3-EPhCH2EPh2)(CO)9]. The latter complexes may also be obtained directly from [Ru3(CO)10(µ-EPh2CH2EPh2)] and H2(20 atm, 80 °C, 2h) in cyclohexane (yields 65–75%). Similar complexes were obtained in poor yield from [Ru3(CO)10(µ-PPh2CH2CH2PPh2)]. The group 1 B metal-containing clusters [MRu3(µ3-EPhCH2EPh2)(CO)9(PPh3)](E = P, M = Cu, Ag, or Au; E = As, M = Au) were prepared from [Ru3(µ3-EPhCH2EPh2)(CO)9]– and sources of [M(PPh3)]+; the analogous [AuRu3(µ3-PPhCH2CH2PPh2)(CO)9(PPh3)] was also obtained. Single-crystal X-ray studies on the first three, title complexes showed that they are isostructural, the M(PPh3) fragment bridging the same Ru–Ru bond as that bridged by the PPh group of the face-capping phosphidophosphine ligand. Detailed examination of bond parameters in the Ru2MP moiety suggests that the three M(PPh3) fragments are not strictly isolobal, although it is the Ag(PPh3) fragment which interacts least strongly with the Ru3 core. The structures were refined by least-squares methods to residuals of 0.039, 0.044, and 0.041 for 4 560, 4 917, and 9 275 independent ‘observed’ reflections, respectively.
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Journal of the Chemical Society, Dalton Transactions
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