Cluster chemistry : X. Preparation of 1,2-bis(diphenylphosphino)ethane derivatives of Ru 3(CO) 12: crystal and molecular structures of Ru 3(CO) 10(η-PH 2PCH 2CH 2PPh 2)

Abstract

The reactions of dppe with Ru 3(CO) 12 catalysed by Ph 2CO??? have been investigated. Under the appropriate conditions Ru 3(CO) 11(PPh 2CH 2CH 2PPh 2) (with only one P atom coordinated), [Ru 3(CO) 11] 2(η-dppe) (with one dppe ligand bridging two Ru 3(CO) 11 clusters), Ru 3(CO) 10(η-dppe) and Ru 3(CO) 8(η-dppe) 2(both with dppe bridging Ru-Ru bonds) can all be isolated in good yields. A full X-ray crystallographic analysis of Ru 3(CO) 10(η-dppe) shows that it crystallizes in the triclinic system, space group P 1 , a 10.615(2), b 11.769(6), c 16.584(4) Å, α 75.68(2), β 84.59(2), γ 69.64(2)°. The structure was refined to R = 0.030, R w = 0.034 using 3558 data with I ⩾ 2.5 σ I. The dppe ligand bridges a Ru-Ru bond (2.856(1) Å), occupying equatorial sites on adjacent Ru atoms. Other distances: non-bridged RuRu bonds are 2.855(1), 2.847(1); RuP, 2.330(2) Å.