Abstract

The red compound, catalytically active in the hydroformylation of olefins, which is isolated from the reaction of Co 2(CO) 8 with Bu 3P at elevated temperatures under CO and H 2 pressure is shown, on the basis of a three-dimensional X-ray study, to be bis[(tri-n-butylphosphine)tricarbonylcobalt], [Co(CO) 3Bu 3P] 2. The compound crystallizes with four molecules in space group T h 6Pa3 of the cubic system in a cell with edge 16.79(5) Å. The observed density of 1.05(5) g/cm 3 agrees t olerably with the calculated value of 0.97 g/cm 3. The structure has been solved by standard methods and refined by least-squares techniques to a conventional R factor of 0.13 for the 382 visually observed reflections. The overall molecular symmetry is D 3d with a linear PCoCoP bonding arrangement coincident with athreefold crystallographic axis and with a center of symmetry between the cobalt atoms. Each cobalt is situated near the center of a trigonal bipyramid, the cobalt being bound to one phosphorus atom, three carbonyl groups, and the other cobalt atom. The CoCo bond length is 2.66(1) Å. The other bond lengths and angles in the structure have their expected values.

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