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Reaction of [Ru(p-cymene)Cl2]2 with K(η5-C5HPh4) in refluxing diglyme yields (η5-C5Ph4)2Ru in ca 50% yield. The complex was not susceptible to oxidation or reduction. (C5HPH4)2Ru crystallizes in the triclinic P1 space group with a = 8.549(4), b = 10.793(4), c = 12.842(5) Å, α = 65.98(3), β = 73.10(3), γ = 83.49(3)° and Z = 1. The least-squares data refined to R(F) = 3.53% and R(wF = 3.82% for the 3952 independent observed reflections with Fo ≥ 5σ(Fo). The metal-centroid distance is 1.832(2) Å and all other bond lengths and angles are similar to other octaphenylmetallocenes. 1H NMR analysis employing 2D J-resolved, COSY and low temperature techniques allowed assignment of all protons in the molecule. The motional processes of the phenyl groups are discussed.


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