Crystal Structure of Vanadyl Bisacetylacetonate. Geometry of Vanadium in Fivefold Coordination

The structure of vanadyl bisacetylacetonate has been determined from three-dimensional x-ray diffraction data. The crystals are triclinic, space group P1̄, with a=7.53±0.02 A, b=8.23±0.03 A, c=11.24±0.04 A, α=73.0°, β=71.3°, γ=66.6°, Z=2. The structure consists of discrete molecules of VO(C5H7O2)2. Each vanadium atom has five oxygen neighbors at the corners of a rectangular (nearly square) pyramid, with vanadium near its center of gravity. The vanadium-oxygen distances are 1.56 A to the apex atom (vanadyl oxygen) and 1.96, 1.96, 1.97, and 1.98 A to the others. Other bond distances average 1.28 A for C–O, 1.40 A for C–C (ring), and 1.52 A for C–C (methyl). Standard deviations are 0.01 A for V–O bonds and 0.02 A for C–O and C–C bonds. Each acetylacetone skeleton is planar, and this plane makes an angle of 163° with the plane of the other acetylacetone skeleton of the same molecule.