Синтез и строение хлоро(пентахлорфеноксида) трис(3-фторфенил)сурьмы  (3-FC6H4)3SbCl(OC6Cl5)

A. N. Efremov

Authors

A. N. Efremov South Ural State University, Chelyabinsk, Russian Federation

Keywords:

tris(3-fluorophenyl)antimony dichloride, tris(3-fluorophenyl)antimony bis(2, 3, 4, 5, 6-pentachlorophenoxide), tris(3-fluorophenyl)antimony chloro(pentachlorophenoxide), ligand redistribution reaction, X-ray diffraction analysis

Abstract

Tris(3-fluorophenyl)antimony chloro(pentachlorophenoxide) (1) has been synthesized by the interaction of tris(3-fluorophenyl)antimony dichloride with tris(3-fluorophenyl)antimony bis(2,3,4,5,6-pentachlorophenoxide) (1:1 mol.) in benzene. The compound has been identified by IR spectroscopy and X-ray diffraction analysis. The absorption band of the stretching vibrations of the SbC₃ fragment at 432 cm^–1 is observed in the IR spectrum of compound 1. There is also an intensive absorption band at 1267 cm^-1, which characterizes stretching vibrations of the C-O bond. According to the X-ray diffraction analysis the coordination of the antimony atom is trigonal-bipyramidal with the chlorine and oxygen atoms in the axial positions [C₂₄H₁₂OCl₆SbF₃,
M = 707.79; the triclinic system, space group P ; a 9.486(6), b 11.548(7); c 12.382(11) Å;
α 73.61(2), β 87.03(3), γ 84.221(19) degrees; V 1294.2(17) Å³; Z 2; µ 1.724 mm^–1; F(000) 668.0; crystal size 0.26´0.22´0.11 mm; 2θ for data collection 5.7–62.22 degrees; index ranges −13 ≤ h ≤ 13, −16 ≤ k ≤ 16, −17 ≤ l ≤ 17; total reflections 79173; independent reflections 8254; R_int 0.0560; variables 317, GOOF 1.021; R₁ = 0.0482; wR₂ = 0.1167; residual electron density 1.91/–0.56 e/Å³]. The OSbCl axial angle in the molecule of compound 1 is 179.14(8)°. The sum of the CSbC angles in the equatorial plane is 360°, while the values of the individual angles vary in the interval 113.49 (15)°–126.16 (15)°. The Sb–O axial bond length is shorter than the Sb–C equatorial bond lengths and equals 2.092 (3) Å. This pattern is characteristic of most triarylantimony diaroxides. The formation of the compound 1 crystal structure is due to the formation of weak intermolecular contacts C–H×××Cl 2.89 Å and F×××Cl 3.08, 3.11 Å. Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data Bank (No. 1849662; deposit@ccdc.cam.ac.uk; http://www.ccdc. cam.ac.uk).

Author Biography

A. N. Efremov, South Ural State University, Chelyabinsk, Russian Federation

аспирант кафедры теоретической и прикладной химии

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