Studies of β-Diketone Complexes of Rhenium. VI. The Crystal and Molecular Structure of cis-Dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III)

Abstract

A compound, obtained in large yields from the reaction of acetylacetone and oxodichloroethoxobis(triphenylphosphine)rhenium(V) in benzene, has been shown by single crystal X-ray diffraction to be cis-dichloropentane-2,4-dionato-trans-bis(triphenylphosphine)rhenium(III). The crystals are monoclinic with a = 13.06(1), b = 18.30(1), c = 16.55(1) Å, and β = 112.7(2)°. The space group is P21/c and there are four molecules per unit cell. A total of 3841 independent reflections, of which 2686 were observed, were examined by film methods, the intensities being measured with a microdensitometer. The structure was refined by full matrix least-squares analysis to an R2 value of 0.068. The ligands are arranged around the rhenium atom in the manner described by the compound name to give a rough octahedron of nearest neighbours and the Re—Cl (2.369 Å av.), Re—O (2.02 Å av.), and Re—P (2.474 Å av.) distances are as expected.