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Abstract <p>Tris(2-methoxyphenyl)antimony bis[3,4-difluorobenzoate] (<b>1</b>) and tris(2-methoxyphenyl)antimony bis[benzenesulfonate] (<b>2</b>) were obtained by oxidative addition reaction from triarylantimony and 3,4-difluorobenzoic/benzenesulfonic acid in the presence of tertiary butyl hydroperoxide in ether. The structure of <b>1</b> and <b>2</b> was established using IR spectroscopy and X-ray diffraction analysis (XRD). Crystals <b>1</b> [C<sub>35</sub>H<sub>27</sub>O<sub>7</sub>F<sub>4</sub>Sb, <i>M</i> 757.32; triclinic system, symmetry group <i>P</i>-1; cell parameters: <i>a</i> = 9.219(4) Å, <i>b</i> = 9.507(6) Å, <i>c</i> = 20.240(11) Å; α = 99.43(3)°, β = 95.756(16)°, γ = 107.90(3)°; <i>V</i> = 1643.6(16) Å<sup>3</sup>; <i>Z</i> = 2; ρ<sub>calc</sub> = 1.530 g/cm<sup>3</sup>; 2θ 6.68°–54.98°; total reflections 31 858; independent reflections 7153; number of specified parameters 427; <i>R</i><sub>int</sub> = 0.0429; <i>GOOF</i> 1.051; <i>R</i><sub>1</sub> = 0.0265, <i>wR</i><sub>2</sub> = 0.0551; residual electron density (max/min); 0.30/–0.44 e/Å<sup>3</sup>], <b>2</b> [C<sub>33</sub>H<sub>31</sub>O<sub>9</sub>S<sub>2</sub>Sb, <i>M</i> 757.46; monoclinic system, symmetry group <i>C</i>2/<i>c</i>; cell parameters: <i>a</i> = 21.157(9) Å, <i>b</i> = 10.363(4) Å, <i>c</i> = 18.285(7) Å; β&#xa0;= 126.590(13)°, <i>V</i> = 3219(2) Å<sup>3</sup>, <i>Z</i> = 1; ρ<sub>calc</sub> = 1.563 g/cm<sup>3</sup>; 2θ 6.012°–54.234°; total reflections 32 454; independent reflections 3541; number of specified parameters 231; <i>R</i><sub>int</sub> = 0.0283; <i>GOOF</i> 1.161; <i>R</i><sub>1</sub> = 0.0283, <i>wR</i><sub>2</sub> = 0.0659; residual electron density (max/min); 0.74/–0.83 e/Å<sup>3</sup>] consist of trigonal bipyramidal molecules with electronegative ligands in axial positions. Sb–C bond lengths vary in the range 2.093(2)−2.125(3) Å, OSbO bond angles take values 176.63(6)° and 174.52(10)°, respectively. The Sb–O distances in <b>1</b> (2.1106(17) and 2.1149(17) Å) are shorter than in <b>2</b> (2.128(2) and 2.128(2) Å). Intramolecular Sb∙∙∙O contacts in <b>1</b> (3.162(2) and 3.257(2) Å) are significantly smaller than in <b>2</b> (3.617(2) and 3.617(2) Å) and do not exceed the sum of their van der Waals radii (3.7 Å). Complete tables of atomic coordinates, bond lengths and bond angles for structures have been deposited in the Cambridge Structural Data Bank (nos. 2123247 (<b>1</b>) and 2116583 (<b>2</b>), deposit@ccdc.cam.ac.uk; http://www.ccdc cam.ac.uk).</p>

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Synthesis and Structure of Tris(2-methoxyphenyl)antimony Bis[3,4-difluorobenzoate] [(2-MeO)C6H4]3Sb[OC(O)C6H3(F2-3,4)]2 and Tris(2-methoxyphenyl)antimony Bis[benzenesulfonate] [(2-MeO)C6H4]3Sb[OSO2C6H5]2

  • 期刊论文

  • 发表日期：

    2025年12月1日

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  • V. V. Sharutin,
  • M. O. Morodetsky

摘要

Abstract

Tris(2-methoxyphenyl)antimony bis[3,4-difluorobenzoate] (1) and tris(2-methoxyphenyl)antimony bis[benzenesulfonate] (2) were obtained by oxidative addition reaction from triarylantimony and 3,4-difluorobenzoic/benzenesulfonic acid in the presence of tertiary butyl hydroperoxide in ether. The structure of 1 and 2 was established using IR spectroscopy and X-ray diffraction analysis (XRD). Crystals 1 [C35H27O7F4Sb, M 757.32; triclinic system, symmetry group P-1; cell parameters: a = 9.219(4) Å, b = 9.507(6) Å, c = 20.240(11) Å; α = 99.43(3)°, β = 95.756(16)°, γ = 107.90(3)°; V = 1643.6(16) Å3; Z = 2; ρcalc = 1.530 g/cm3; 2θ 6.68°–54.98°; total reflections 31 858; independent reflections 7153; number of specified parameters 427; Rint = 0.0429; GOOF 1.051; R1 = 0.0265, wR2 = 0.0551; residual electron density (max/min); 0.30/–0.44 e/Å3], 2 [C33H31O9S2Sb, M 757.46; monoclinic system, symmetry group C2/c; cell parameters: a = 21.157(9) Å, b = 10.363(4) Å, c = 18.285(7) Å; β = 126.590(13)°, V = 3219(2) Å3, Z = 1; ρcalc = 1.563 g/cm3; 2θ 6.012°–54.234°; total reflections 32 454; independent reflections 3541; number of specified parameters 231; Rint = 0.0283; GOOF 1.161; R1 = 0.0283, wR2 = 0.0659; residual electron density (max/min); 0.74/–0.83 e/Å3] consist of trigonal bipyramidal molecules with electronegative ligands in axial positions. Sb–C bond lengths vary in the range 2.093(2)−2.125(3) Å, OSbO bond angles take values 176.63(6)° and 174.52(10)°, respectively. The Sb–O distances in 1 (2.1106(17) and 2.1149(17) Å) are shorter than in 2 (2.128(2) and 2.128(2) Å). Intramolecular Sb∙∙∙O contacts in 1 (3.162(2) and 3.257(2) Å) are significantly smaller than in 2 (3.617(2) and 3.617(2) Å) and do not exceed the sum of their van der Waals radii (3.7 Å). Complete tables of atomic coordinates, bond lengths and bond angles for structures have been deposited in the Cambridge Structural Data Bank (nos. 2123247 (1) and 2116583 (2), deposit@ccdc.cam.ac.uk; http://www.ccdc cam.ac.uk).