Окисление три-орто-толилсурьмы в присутствии пероксида, кислорода воздуха и 2,5-диметилбензолсульфоновой кислоты. Строение сульфо-(μ3-оксо)-трис-(μ2-оксо)-окта-орто-толилсурьмы

V. V. Sharutin; V. S. Senchurin

Authors

V. V. Sharutin South Ural State University, Chelyabinsk, Russian Federation
V. S. Senchurin South Ural State University, Chelyabinsk, Russian Federation

Keywords:

tri-ortho-tolylantimony, 2, 5-dimethylbenzenesulfonic acid, synthesis, structure, X-ray analysis

Abstract

The interaction of tri-ortho-tolylantimony with 2,5-dimethylbenzenesulfonic acid in diethyl ether in air in the presence of tert-butyl hydroperoxide (3:2:3 mol.) synthesized sulfo-(μ₃-oxo)-tris-(μ₂-oxo)-octa-ortho-tolylantimony (1), the yield of which after recrystallization from toluene:octane mixtures (5:1 vol.) was 63 %. The X-ray diffraction pattern of crystal 1 was obtained at 293 K on an automatic diffractometer D8 Quest Bruker (MoK_α-radiation, λ = 0.71073 Å, graphite monochromator), [C₄₂H₄₂O₈SSb₃, M 1072.07, the monoclinic syngony, the symmetry group P2₁/c; cell parameters: a 11.434(5), b 21.609(11), c 18.737(8) Å, α = 90.00 degrees,
β = 104.778(14) degrees, γ = 90.00 degrees; V = 4476(4) Å³; the crystal size is 1.05×0.65×0.11 mm; intervals of reflection indexes are –17 ≤ h ≤ 17, –33 ≤ k ≤ 33, –28 ≤ l ≤ 28; total reflections 125015; independent reflections 17125; R_int 0.0579; GOOF 1.044; R₁ = 0.0734, wR₂ = 0.1886; residual electron density 2.75/-1.12 e/Å³] in the trinuclear complex, two atoms of antimony are hexacoordinated (CSbO 159.4(2)–165.4(3)°; OSbO 164.9(2) and 167.4(2)°), the third atom of antimony is in strongly distorted trigonal-bipyramidal coordination (axial angle OSbC 161.9(3)°, equatorial angles OSbC and OSbO vary in the interval 110.5(2)–120.8(4)°). The Sb–С, μ₂-O–Sb and μ₃-O–Sb bond lengths are 2.095(9)–2.136 (7) Å, 1.904(5)–2.165 (5) Å, and 2.008 (4)–2.387 (5) Å, respectively. The bridge bidentate sulfate ligand is bound to antimony atoms, the Sb–O_sulf. distances are 2.100(5) and 2.108(5) Å. Complete tables of coordinates of atoms, bond lengths and valence angles are deposited at the Cambridge Structural Data (No. 1866027; deposit@ccdc.cam.ac.uk; http: //www.ccdc cam.ac.uk.).

Author Biographies

V. V. Sharutin, South Ural State University, Chelyabinsk, Russian Federation

доктор химических наук, профессор, главный научный сотрудник Управления научной и инновационной деятельности

V. S. Senchurin, South Ural State University, Chelyabinsk, Russian Federation

кандидат химических наук, доцент кафедры теоретической и прикладной химии

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