摘要
利用三苯基氯化锡和对苯二甲酸二钠、哌嗪荒酸二钠在甲醇中反应 ,合成了双核有机锡 (Ⅳ )配合物 [Ph3 Sn (CH3 OH)O2 CC6H4 CO2 (CH3 OH)SnPh3 ]·2CH3 OH (1)和 [Ph3 SnS2 CN(CH2 CH2 ) 2 NCS2 SnPh3 ]·2CH3 OH (2 ) .通过元素分析、红外光谱和核磁共振氢谱对其结构进行了表征 .用X射线单晶衍射测定了这两个化合物的晶体结构 .化合物 1为单斜晶系 ,空间群P2 1/n ,a =1.5 199(5 )nm ,b =0 .90 0 0 (3)nm ,c =1.82 0 6 (6 )nm ,β =113.970 (5 )° ,Z =2 ,V =2 .2 75 5(13)nm3 ,Dc=1.413g/cm3 ,μ =1.146mm-1,F(0 0 0 ) =980 ,R1=0 .0 35 3,wR2 =0 .0 6 0 6 .化合物 2为单斜晶系 ,空间群P2 1/c,a =1.5 0 6 6 (5 )nm ,b =1.0 875 (4 )nm ,c =1.35 42 (5 )nm ,β =91.6 14(5 )°,Z =2 ,V =2 .2 178(14)nm3 ,Dc=1.498g/cm3 ,μ =1.35 1mm-1,F(0 0 0 ) =10 0 8,R1=0 .0 40 1,wR2 =0 .1148.在 1和 2的晶体中 ,锡原子呈五配位畸变三角双锥构型 .配合物
Binuclear organotin(Ⅳ) complexes [Ph 3Sn(CH 3OH)O 2CC 6H 4CO 2(CH 3OH)SnPh 3]·2CH 3OH (1) and [Ph 3SnS 2CN(CH 2CH 2) 2NCS 2SnPh 3]·2CH 3OH (2) were synthesized by the reaction of Ph 3SnCl with terephthalate or piperazinylbisdithiocarbamate in 2∶1 molar ratio in methanol solution. Their structure were characterized by elementary analysis,IR and 1 H NMR and the crystal structures were determined by X-ray single crystal diffraction. The crystal 1 belongs to monoclinic with space group P2 1/n, a=1.5199(5) nm, b= 0.9000(3) nm, c=1.8206(6) nm, β=113.970(5)°, Z=2, V=2.2755(13) nm 3, D c=1.413 g/cm 3, μ=1.146 mm -1, F(000)=980, R 1=0.0353, wR 2=0.0606. The crystal 2 belongs to monoclinic with space group P2 1/c, a=1.5066(5) nm, b=1.0875(4) nm, c=1.3542(5) nm, β=91.614(5)°, Z=2, V=2.2178(14) nm 3, D c=1.498 g/cm 3, μ=1.351 mm -1, F(000)=1008, R 1=0.0401, wR 2= 0.1148. In the crystals of complexes 1 and 2, the tin atoms rendered five-coordinate in a distorted trigonal bipyramidal configurations. The complex 1 is formed 2-D network structure by packing along the a-axis through hydrogen bonding.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2002年第5期897-903,共7页
Acta Chimica Sinica
基金
教育部骨干教师基金
山东省自然科学基金 (No .Y2 0 0 0B0 8)资助项目
