Synthesis and structure of tris(2-methoxyphenyl)antimony bis(4-methylbenzenesulfonate) solvate with benzene

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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, ρ calc = 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).

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4-methylbenzenesulfonic acid, tris(2-methoxyphenyl)antimony, tert-butyl hydroperoxide, oxidative addition reaction, synthesis, structure, x-ray diffraction analysis

Короткий адрес: https://sciup.org/147238618

IDR: 147238618   |   DOI: 10.14529/chem220302

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