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 6Pa3 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 PCoCoP 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 CoCo bond length is 2.66(1) Å. The other bond lengths and angles in the structure have their expected values.
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