The One Stage Synthesis and Crystal Structure of 5,5,5-Trifluoro-2-pentanone-4,4-diolato-triphenylantimony(V)

Abstract

5,5,5-Trifluoro-2-pentanone-4,4-diolato-triphenylantimony(V) (1) was obtained by the onestep oxidation reaction of triphenylantimony, tert-butylhydroperoxide, and trifluoroacetylacetone. The crystal structure of 1 has been determined by X-ray diffraction method (MoKα-radiation, graphite monochromator, θ/2θ-scan mode in the range 2° ≤ 2θ ≤ 54°, 3734 observed reflection with F > 6σ(F), R = (0.029, Rw = 0.031, S = 1.03). Crystal of 1 is monoclinic, at 20°C a = 9.369(5) Å, b = 16.891(6) Å, c = 13.934(5) Å, β = 102.04(2)°, V = 2157(3) ų, d(ca1cd) = 1.611 g cm⁻³, Z = 4, space group P2₁/n. It was shown that 1 is a six-coordinated antimony complex. The coordination mode of the Sb atom in 1 can be described as a significantly distorted octahedron. In crystal structure the molecules of 1 are associated into a centrosymmetrical dimer by a weak hydrogen O...H—bonds between adjacent molecules.