Synthesis and Structure of Tris(3-Fluorophenyl)antimony Chloro(pentachlorophenoxide) (3-FC6H4)3SbCl(OC6Cl5)

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) ų; 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/ų]. 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).