氢氧化氯化四苯基二锡氧烷二聚体的合成、结构与性质  

The Synthesis,Crystal Structure and Character of Chloro-hydroxyltetraphenyl-distannoxane Drimer

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作  者:郑晓凤[1] 毛武涛[1] 尹玲[1] 张然[1] 刘西成[1] 田来进[1] 

机构地区:[1]曲阜师范大学化学科学学院,山东省曲阜市273165

出  处:《曲阜师范大学学报(自然科学版)》2007年第3期89-93,共5页Journal of Qufu Normal University(Natural Science)

基  金:山东省自然科学基金(Z2002F01);晶体材料国家重点实验室开放课题(2005B103);曲阜师大科研基金

摘  要:二苯基二氯化锡在三乙胺的三氯甲烷溶液中部分水解生成标题化合物氢氧化氯化四苯基二锡氧烷二聚体[Ph2(Cl)SnOSnPh2(OH)]2,通过元素分析,红外光谱和X-射线单晶衍射法分析表明,该化合物属于三斜晶系,P-1空间群,a=1.0366(17)nm,b=1.0780(18)nm,c=1.1799(19)nm,α=77.635(2)°,β=66.227(2)°,γ=75.215(2)°,υ=1.1574(3)nm3,Z=1,Dc=1.763 g.cm3,μ=2.290 mm1,R1=0.0525,wR2=0.1121.整个分子是以Sn2O2四元环为中心的对称二聚体结构,两个锡原子为五配位的三角双锥构型.该化合物能较好地催化乙酰乙酸乙酯和醇的酯交换反应.The compound tetraorganodistannoxane, [Ph2 (Cl) SnOSnPh2 (OH)]2, is synthesized in the solvent CHCl3 by hydrolyzing Ph2 SnCl2 partly and the colorless crystals suitable for X-ray analysis are obtained from the mother solution by slow evaporation at 298 K. The compound is characterized by elemental analysis and IR, and it is determined by X-ray single crystal diffraction. The compound is in centro-symmetric dimmer structure mode belonging to the triclinic space group P-1, a= 1. 0366 (17) nm,b= 1. 0780 (18) nm,c= 1. 1799(19) nm,α=77. 635(2)°,β=66. 227(2°) ,γ=75. 215(2)°,v= 1. 1574(3) nm^3 ,Z= 1 ,Dr = 1. 763 Mg /m^3 ,μ=2. 290 mm^1 ,R1 =0. 0525,wR2 =0. 1121. In the compound there is a four-member central cyclic Sn2O2 unit in which the bridging oxygen atoms are tri-coordinated. The tin atoms are five-coordinated with geometry of distorted trigonal bipyramid. The experiment of testing the catalytic activity manifests that the compound could catalize the esterification reaction of acetylacetic ether successfully.

关 键 词:晶体结构 氢氧化氯化四苯基二锡氧烷 催化活性 酯交换反应 

分 类 号:O641.4[理学—物理化学]

 

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