Abstract

The reactions of tris(para-tolyl)antimony (4-МеС₆H₄)₃Sb with chloroacetic acid and of triphenylantimony Ph₃Sb with 3,4,5-trifluorobenzoic and 2,3-difluorobenzoic acids in the presence of tert-butyl hydroperoxide afford triarylantimony dicarboxylates Ar₃Sb[OC(O)R]₂, where Ar = p-Tol, R = CH₂Cl (I), Ar = Ph, C₆H₂F₃-3,4,5 (II), and C₆H₃F₂-2,3 (III). According to the X-ray diffraction data (CIF files CCDC nos. 1883320 (I), 1979844 (II), and 1980334 (III)), the Sb atoms in compounds I−III have the coordination of a trigonal bipyramid. The OSbO axial angles are 174.47(6)° (I), 173.98(7)° (II), and 175.98(6)° (III). The Sb−O and Sb−С bond lengths are 2.145(2), 2.143(2), and 2.104(2)–2.109(2) Å in compound I; 2.121(2), 2.121(2) and 2.098(2)–2.112(3) Å in compound II; and 2.1302(18), 2.1132(18), and 2.109(3)–2.117(3) Å in compound III. The intramolecular Sb⋅⋅⋅O distances with the carbonyl oxygen atom (3.054(3) and 3.080(3) Å (I), 3.033 Å (II), and 2.959(3) and 3.054(2) Å (III)) are less than the sum of the van der Waals radii of Sb and O. The structural organization of the compounds is due to hydrogen bonds of the О⋅⋅⋅H and F⋅⋅⋅H types, СН⋅⋅⋅π and F⋅⋅⋅π interactions, and stacking effect.

中文翻译：

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三苯基和三（对甲苯基）锑二羧酸盐：合成和结构

摘要

三（对甲苯基）锑 (4-МеС ₆ H ₄ ) ₃ Sb 与氯乙酸的反应以及三苯基锑Ph ₃ Sb 与 3,4,5-三氟苯甲酸和 2,3-二氟苯甲酸在叔存在下的反应丁基氢过氧化物提供三芳基锑二羧酸盐 Ar ₃ Sb[OC(O)R] ₂，其中 Ar = p -Tol, R = CH ₂ Cl ( I ), Ar = Ph, C ₆ H ₂ F ₃ -3,4,5 ( II ), 和 C ₆ H ₃ F ₂ -2,3 ( III）。根据 X 射线衍射数据（CIF 文件 CCDC 编号 1883320（I）、1979844（II）和 1980334（III）），化合物I - III 中的 Sb 原子具有三角双锥的配位。OSbO 轴角为 174.47(6)° ( I )、173.98(7)° ( II ) 和 175.98(6)° ( III )。化合物I 中的 Sb-O 和 Sb-С 键长分别为 2.145(2)、2.143(2) 和 2.104(2)–2.109(2) Å ；化合物II 中的2.121(2)、2.121(2) 和 2.098(2)–2.112(3) Å ；和 2.1302(18)、2.1132(18) 和 2.109(3)–2.117(3) Å 在化合物III 中. 与羰基氧原子的分子内 Sb⋅⋅⋅O 距离（3.054(3) 和 3.080(3) Å ( I )、3.033 Å ( II ) 和 2.959(3) 和 3.054(2) Å ( III )）为小于 Sb 和 O 的范德华半径之和。 化合物的结构组织是由于 О⋅⋅⋅H 和 F⋅⋅⋅H 类型的氢键，СН⋅⋅⋅π 和 F⋅⋅ ⋅π 相互作用和堆叠效应。