二正丁基锡二2-(2-甲酰基苯氧基)乙酸酯的合成、晶体结构及杀菌活性

Synthesis,Crystal Structure and Antibacterial Activity of Di-nbutyltin di-2-(2-formylphenoxy)acetic Ester

在苯溶液中,将2-(2-甲酰基苯氧基)乙酸与二正丁基氧化锡进行脱水反应,获得二正丁基锡二2-(2-甲酰基苯氧基)乙酸酯(1),并经过元素分析、1H NMR和IR及晶体结构测试技术进行了结构表征。结果表明,晶体属于C2/c空间群,晶胞参数:a=3.324 6(7)nm,b=0.484 54(10)nm,c=2.214 7(5)nm,β=131.373(2)°,V=2.677 3(9)nm3,Z=4,F(000)=1 208,Dc=1.467 g/cm3,μ=0.999 mm-1,R1=0.048 8,wR2=0.104 8。结构单元内包含1个独立分子,形成以六配位锡为中心的斜梯形双棱锥构型;分子间的Sn O(0.346 8 nm)配位作用,中心锡原子为八配位,构成以锡为中心的扭曲的六方双锥构型的一维链状桥环化合物。杀菌活性顺序为:化合物1>二丁基氧化锡>2-(2-甲酰基苯氧基)乙酸。

Di-n-butyhin di-2-（2-formylphenoxy）acetic ester（1 ） was synthesized by the reaction of di-n-butyl tin oxide with 2-（2-formylphenoxy）acetic acid and azeotropic removal of water with benzene. The compound was characterized by elemental analysis, ^1H NMR, FT-IR, and single crystal X-ray diffraction analysis. The crystal belongs to space group C2/c, and the cell parameter are ： a = 3.324 6 （7） nm, b = 0. 484 54 （10） nm, c =2. 214 7（5） nm,β = 131. 373（2） °, V=2. 677 3（9） m^3, Z =4, F（000） = 1 208 ,Dc = 1. 467 g/cm^4, μ =0. 999 nm^-1, R1 =0. 048 and wR2 =0. 104 8. There is one molecule in the unit cell, which adopts a skew-trapezoidal bipyramidal arrangement around the tin atom with hexa-coordination; in addition, there are weak bridging intermolecular Sn…O （0. 346 8 nm） interactions, and the endocyclic Sn atom is octa-coordinated and exists in distorted hexagonal bipyramidal geometry in a one-dimensional chain. The complex （1） exhibits good antibacterial properties, while the antibacterial activity decreased in the order of compound （1） 〉 di-n-butyhin oxide 〉 2 - （ 2 -formylphenoxy ）acetic acid.