Synthesis and Structure of tris(2-methoxyphenyl)antimony Bis(4-methylbenzenesulfonate) Solvate with Benzene

Abstract

The interaction of tris(2-methoxyphenyl)antimony with 4-methylbenzenesulfonic acid, in the presence of tert-butyl hydroperoxide (1:2:1 mol.) in ether at ambient temperature has given tris(2-methoxyphenyl)antimony disulfonate, which has been structurally characterized: tris(2-methoxyphenyl)antimony bis(4-methylbenzenesulfonate) solvate with benzene (2-MeOC6H4)3Sb[OSO2C6H4Me-4]2 ∙ 2 PhH (1). According to the X-ray diffraction data obtained on a Bruker D8 QUEST diffractometer, compound 1 has the following crystallographic parameters of the unit cell: space group C2/c, а = 26.683(12), b = 8.745(4), c = 35.463(17) Å,
α = 90.00°, β = 103.252(18)°, γ = 90.00°, V = 8055(6) Å3, ρcalc = 1.424 g/сm3, Z = 8. The antimony atom has a distorted trigonal-bipyramidal coordination with the oxygen atoms in axial positions. The OsulfSbOsulf axial angle is 175.49(9)°. The Sb−C bond lengths are in the range of values 2.093(3)–2.098(3) Å. The formation of the crystal structure in compound 1 is due to the presence of weak intermolecular hydrogen bonds S=O∙∙∙H–C 2.61–2.7 Å. The antimony atom departs from the equatorial plane [C3] by 0.076 Å. Complete tables of atom coordinates, bond lengths, and valence angles are deposited at the Cambridge Crystallographic Data Center (No. 2141659; deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk/data_request/cif).