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Article type: Research Article
Authors: Gushchin, Aleksey V. | Usyatinsky, Rafail I. | Fukin, Georgy K. | Dodonov, Victor A. | Zakharov, Lev N.
Affiliations: Organic Chemistry Department, Nizhny Novgorod State University, Nizhny Novgorod, 603600, Russia | G. A. Razuvaev Institute of Organometallic Chemistry, Russian Academy of Sciences, Nizhny Novgorod, 603600, Russia
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) Å3, 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.
DOI: 10.1080/10241229812331341349
Journal: Main Group Chemistry, vol. 2, no. 3, pp. 187-190, 1998
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