Abstract

Oxidation of triarylantimony Ar₃Sb by peroxide benzoyl in benzene yielded relevant dibenzoates Ar₃Sb[OC(O)Ph]₂ [Ar = 4-FC₆H₄ (1), (4-F₃C)C₆H₄ (2), (2-MeO)C₆H₄ (3), 4-BrC₆H₄ (4), 3‑MeC₆H₄ (5), 4-MeC₆H₄ (6), (4-Me₂N)C₆H₄ (7), (2-MeO)(5-Br)C₆H₃] (8) up to 94%. Compounds 1−8 were identified using the IR spectroscopy and elemental analysis, and compounds 1 and 2 using the XRD analysis as well. According to the XRD data, crystals 1 consist of two types of crystallographically independent molecules (A and B), the geometrical parameters of which differ slightly from each other. Antimony atoms in 1 and 2 have trigonal pyramid coordination with benzoate ligands in axial positions. The Sb–C bond lengths are 2.042(11), 2.081(11), 2.143(9) Å for 1A, 2.091(10), 2.146(11), 2.162(9) Å for 1B, and 2.134(5), 2.135(4), 2.142(4) Å for 2. The Sb–O distances are 2.117(7), 2.128(8) Å for 1А, 2.117(7), 2.128(8) Å for 1В and 2.127(3), 2.133(3) Å for 2; however, metal atoms are also coordinated by carbonyl bidentate oxygen atoms carboxylate ligands (the distances Sb∙∙∙O=C vary in the intervals 2.669(9) −2.876(9) Å). The equatorial angles of CSbC are unequal: the largest angle is observed on the side of intramolecular contacts [103.6(5), 109.0(4), 147.2(4)° for 1A, 105.0(4), 108.1(4), 146.6(4)° for 1B, and 104.39 (17), 105.33(17), 150.21(16)° for 2]. The OSbO axial angles are 175.3(4), 176.0(4), and 175.10(10)°, respectively.

中文翻译：

---

过氧化苯甲酰氧化三芳基锑

摘要

三芳基锑 Ar ₃ Sb 在苯中被过氧化物苯甲酰氧化，得到相应的二苯甲酸酯 Ar ₃ Sb[OC(O)Ph] ₂ [Ar = 4-FC ₆ H ₄ ( 1 ), (4-F ₃ C)C ₆ H ₄ ( 2 )、(2-MeO)C ₆ H ₄ ( 3 )、4-BrC ₆ H ₄ ( 4 )、3-MeC ₆ H ₄ ( 5 )、4-MeC ₆ H ₄ ( 6 )、(4-Me _2N ) C _6H4 ( 7 ), (2-MeO)(5-Br)C ₆ H ₃ ] ( 8 ) 高达 94%。使用红外光谱和元素分析鉴定了化合物1 – 8 ，也使用 XRD 分析鉴定了化合物1和2 。根据 XRD 数据，晶体1由两种晶体学上独立的分子（A 和 B）组成，其几何参数彼此略有不同。1和2中的锑原子与苯甲酸酯配体在轴向位置具有三角锥配位。1A的 Sb-C 键长为 2.042(11)、2.081(11)、2.143(9) Å， 1B为 2.091(10)、 2.146 (11)、2.162(9) Å，2 为2.134(5)、2.135(4)、2.142(4) Å 。Sb-O 距离为1А为 2.117(7)、2.128(8) Å， 1В为 2.117(7)、2.128(8) Å，2为2.127(3)、2.133(3) Å ；然而，金属原子也可以通过羰基二齿氧原子羧酸盐配体配位（距离Sb∙∙∙O=C在2.669(9) −2.876(9) Å范围内变化）。CSbC的赤道角不相等：在分子内接触一侧观察到最大角度[1A为103.6(5)、109.0(4)、147.2(4)°、105.0(4)、108.1(4)、146.6 ( 1B为 4)° ，2 为 104.39 (17)、105.33(17)、150.21(16) °]。OSbO 轴角分别为 175.3(4)、176.0(4) 和 175.10(10)°。