Synthesis and structure of tris(2-methoxy-5-clorophenyl)antimony difluoride

Tris (2-methoxy-5-chlorophenyl)antimony difluoride (1) has been obtained by the substitution reaction between tris (2-methoxy-5-chlorophenyl)antimony dibromide and sodium fluoride in an aqueous acetone solution, yielding 92%, after crystallization from a mixture of acetonitrile and octane. The compound has been identified by IR spectroscopy and X-ray diffraction analysis. According to the X-ray diffraction data, yellow-brown crystals 1 have a slightly distorted trigonal-bipyramidal coordination with axially arranged halogen atoms. According to a diffractometer D8 QUEST Bruker, the critical parameters of the unit cell of the compound are: space group P -1, a = 12.93(10), b = 14.84(18), c = 15.1(2) Å, α = 64.5(6)°, β = 65.6(4)°, γ = 65.1(3)°, V = 2269(46) Å3, ρ calc = 1.711 g/cm3, Z = 2. The Sb-C bond lengths are 2.09(4), 2.08(5), and 2.06(4) Å, the CSbC valence angles are 116.99(2), 122.05(2), 120.86(1)°. The Sb-F bond lengths are 1.995(3) and 1.936(3). The oxygen atoms of the methoxy groups are coordinated to the metal atom [the Sb∙∙∙OMe intramolecular distances equal 3.25(5), 3.04(3), and 3.11(5) Å]. The Sb∙∙∙O valence angles are equal to 108.2(9), 114.4(7), and 115.3 (9)°, respectively. The FSbF axial angle is 179.13(9)°, and the equator angles are 114.78(3), 116.01(2), and 113.45(2)°.