Cyclopentadienyl-Ruthenium and -Osmium Chemistry. XXX. Synthesis and X-Ray Structure of [Ru(dppm-P)(dppm-P,P')(η-C₅H₅)][PF₆]_0.5[PO₂F₂]_0.5

Abstract

An improved, one-pot synthesis is reported for the [Ru (dppm -P)(dppm -P, P′)(η-C₅H₅)]⁺ cation as its BF₄^- salt. The crystal structure of [Ru ( dppm - P)( dppm -P,P′)(η-C₅H₅)]⁺, obtained as the mixed PF₆^-/PO₂F₂^- salt, has also been determined. There are few differences in dimensions between the mono- and bi-dentate dppm ligands; chelation sharply reduces the P-CH₂-P angle, and one phenyl group on each phosphorus is bent away from the metal. Crystals are monoclinic, space group C2/c with unit cell dimensions a 21.743(3), b 23.594(3), c 21.352(3)Ǻ, β 110.17(1) and Z 8. The structure was refined by a full-matrix least-squares procedure to final R 0.078 and Rw 0.087 for 4490 reflections with I > 2.5σ(I).