Abstract—

Oxidation of tris(3-fluorophenyl)antimony with tert-butyl hydroperoxide in the presence of 2-methylcarboranylcarboxylic acid leads to the formation of tris(3-fluorophenyl)antimony bis(2-methylcarboranylcarboxylate) (1), whose structural features were established by X-ray diffraction analysis. According to X-ray diffraction analysis carried out at 293 K using a D8 Quest Bruker automatic four-circle diffractometer (two-coordinate CCD detector, MoK_α radiation, λ = 0.71073 Å, graphite monochromator), crystals are characterized as follows: C₂₆H₃₈B₂₀F₃O₄Sb, M 809.52; monoclinic syngony, symmetry group С2/c; cell parameters: a = 19.050(13) Å, b = 14.441(9) Å, c = 14.568(9) Å; α = 90°, β = 98.51(2)°, γ = 90°; V = 3964(4) ų ; Z = 4; crystal size 0.8 × 0.55 × 0.29 mm; reflection index intervals –25 ≤ h ≤ 25, –18 ≤ k ≤ 18, –18 ≤ l ≤ 19; total reflections 37 401; independent reflections 4709; R_int 0.0545; GOOF 1.108; R₁ = 0.0578, wR₂ = 0.1482; residual electron density –0.59/1.09 e /ų. According to the X-ray diffraction data, the antimony atoms in the molecules of compound 1 have a distorted trigonal-bipyramidal coordination with oxygen atoms of the carboxylate ligands in axial positions. The Sb–C bonds (2.104(4)–2.114(8) Å) are shorter than the Sb–O distances (2.113(3) Å), the OSbО axial angle is 178.48(15)°, the CSbC angles are 109.7(2)°, 118.4(2)°, and 131.8(3)°. The significant increase in one of the angles is associated with the cis-conformation of carboxylate ligands relative to the equatorial plane. There is a propeller conformation of aryl ligands with respect to the equatorial plane [C₃]. Structure 1 contains intramolecular Sb···O=C contacts between the antimony and oxygen atoms of the carbonyl groups of the carboxylate ligands, which are 3.089(3) Å. The formation of a spatial network in the crystal of compound 1 is due to the presence of weak hydrogen bonds carboxylate ligands and fluorine aryl ligands with the participation of boron atoms: B···H (3.19 Å) and F···B (3.45 Å). Complete tables of atomic coordinates, bond lengths, and bond angles have been deposited with the Cambridge Crystallographic Data Center (no. 2178731; deposit@ccdc.cam.ac.uk or http://www.ccdc.cam.ac.uk/data_request/cif).

中文翻译：

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三(3-氟苯基)二(2-甲基碳硼基羧酸)锑的合成及晶体结构

摘要-

在 2-甲基碳硼基羧酸存在下，用叔丁基过氧化氢氧化三（3-氟苯基）锑，形成三（3-氟苯基）锑双（2-甲基碳硼基羧酸）（1），其结构特征由下式确定： X射线衍射分析。根据使用 D8 Quest Bruker 自动四环衍射仪（二坐标 CCD 探测器，Mo K _α辐射，λ = 0.71073 Å，石墨单色仪）在 293 K 下进行的 X 射线衍射分析，晶体的特征如下：₂₆ H ₃₈ B ₂₀ F ₃ O ₄ Sb，M 809.52；单斜同构，对称群С2/ c ; 电池参数：a = 19.050(13) Å，b = 14.441(9) Å，c = 14.568(9) Å；α=90°，β=98.51(2)°，γ=90°；V = 3964(4) Å ³；Z = 4；晶体尺寸0.8×0.55×0.29毫米；反射指数区间 –25 ≤ h ≤ 25、–18 ≤ k ≤ 18、–18 ≤ l ≤ 19；全反射 37 401；独立思考4709；R_整数0.0545；愚蠢1.108；R ₁ = 0.0578，wR ₂ = 0.1482；残余电子密度 –0.59/1.09 e /Å ³。X射线衍射数据表明，化合物1分子中的锑原子与轴向位置的羧酸配体的氧原子形成扭曲的三方双锥配位。Sb-C键(2.104(4)–2.114(8) Å)比Sb-O键距离(2.113(3) Å)短，OSbО轴角为178.48(15)°，CSbC角为109.7( 2)°、118.4(2)°和131.8(3)°。其中一个角度的显着增加与羧酸配体相对于赤道面的顺式构象有关。芳基配体相对于赤道面[C ₃ ]具有螺旋桨构象。结构1含有羧酸配体羰基的锑和氧原子之间的分子内Sb…O=C接触，其尺寸为3.089(3) Å。化合物1晶体中空间网络的形成是由于弱氢键羧酸盐配体和氟芳基配体的存在以及硼原子的参与：B·H (3.19 Å)和F·B ( 3.45 埃）。完整的原子坐标、键长和键角表已保存在剑桥晶体学数据中心（编号 2178731；deposit@ccdc.cam.ac.uk 或 http://www.ccdc.cam.ac.uk/数据请求/CIF）。