Cationic Copper Hydride Clusters Arising from Oxidation of (Ph₃P)₆Cu₆H₆

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Abstract

Transfer of the first electron from (Ph₃P)₆Cu₆H₆ to Cp*₂Fe+ is fast (k > 106 L·mol-1·s-1). Transfer of a second electron to the same oxidant has a much lower thermodynamic driving force and is considerably slower, with k = 9.29(4) × 103 L·mol-1·s-1. The second oxidation leads to the formation of [(Ph₃P)₆Cu₆H₅]+. The structure of [(Ph₃P)₆Cu₆H₅]+ has been confirmed by its conversion back to (Ph₃P)₆Cu₆H₆ and by microanalysis; X-ray diffraction shows that the complex is a bitetrahedron in the solid state. [(Ph₃P)₆Cu₆H₅]+ can also be prepared by treating (Ph₃P)₆Cu₆H₆ with MeOTf. With less than 1 equiv of Cp*₂Fe+ as oxidant, (Ph₃P)₆Cu₆H₆ gives [(Ph₃P)₇Cu₇H₆]+ as the major product; X-ray diffraction shows a Cu₆ octahedron with one face capped by an additional Cu. [(Ph₃P)₇Cu₇H₆]+ can also be prepared by treating (Ph₃P)₆Cu₆H₆ with [Cu(CH₃CN)₄]+ (along with 1 equiv of Ph₃P), and can be converted back to (Ph₃P)₆Cu₆H₆ with base/H₂.

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