三维聚合物双(三丁基锡)戊二酸酯的合成及晶体结构研究

用三丁基氯化锡与戊二羧酸二钠以2:1摩尔比反应,合成了双（三丁基锡）戊二羧酸酯,并用元素分析、红外光谱、核磁共振氢谱及X-射线单晶衍射进行了表征和结构测定。X-射线单晶衍射法测定表明,化合物属单斜晶系,空间群为Cc,晶胞参数:a=13.984（3）,b=16.164（3）,c=16.894（3）A,β=107.457（3）°,V=3642.9（11）A3,Z=4,C29H60O4Sn2,Dc=1.251g/cm3,μ=1.394 mm-1,R=0.0500,wR=0.0874,F（000）=1416。晶体结构中存在2种化学环境不同的三角双锥构型的锡原子,由于配体中2个羧基在不同方向的交联作用,使化合物呈现三维立体骨架结构,并且在骨架结构中存在沿a、b、c轴3个方向伸展的规则的大环直孔道。

Synthesis and Crystal Structure of Bis(tributyltin) Ester of Glutaric Acid with Three-dimensional Network

Bis(tributyltin) esters of glutaric acid were synthesized by the reaction of disodium dicarboxylates with the tributyltin chloride in 1:2 molar ratio and characterized by elemental analysis, IR and 1H NMR. Its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group Cc with a = 13.984(3) , b = 16.164(3), c = 16.894(3) A,β = 107.457(3)°, V= 3643(1) A3, Z = 4, Dc= 1.251 g/cm3,μ =1.394 mm-1, R= 0.0500, wR= 0.0874 and F(000) = 1416. The tin atom is five-coordinated in a distorted trigonal bipyramidal configuration. By two bridging carboxylate groups in different directions, the resulting structure is a three-dimensional framework polymer containing two different tin atoms. The framework structure contains regular large ring direct channels along the a, b and c axises.