含硫、氮配位的二正丁基锡二(二苯基卡巴腙)合成及晶体结构研究

Synthesis and Crystal Structure of Di-n-butyltin Bis(diphenylthiocarbazone)

以乙醇钠作碱 ,用二正丁基二氯化锡或三正丁基氯化锡与二苯基硫代卡巴腙反应 ,合成了二正丁基锡二 (二苯基硫代卡巴腙 ) [(n Bu) 2 Sn(SN4C13 H11) 2 ] .通过元素分析、红外光谱、紫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该化合物的晶体结构 .化合物为单斜晶系 ,空间群P2 1/c ,a =2 .0 2 15 ( 7)nm ,b =1.3 10 3 ( 5 )nm ,c =2 .8171( 10 )nm ,β =95 .472 ( 7)° ,Z =8,V =7.42 8( 5 )nm3 ,Dc=1.3 3 0g/cm3 ,μ =0 .83 4mm-1,F ( 0 0 0 ) =3 0 5 6,R1=0 .0 5 75 ,wR2 =0 .0 95 9.化合物中 ,中心锡原子为六配位畸变八面体构型 .

The compound (n-Bu)(2)Sn(SN4C13H11)(2) was prepared by the reaction of di-n-butyltin dichloride or tri-n-butyltin chloride with diphenylthiocarbazone in the presence of the sodium alcoholic. Its structure was determined with IR, H-1 NMR, UV spectra and X-ray crystallography analysis. It crystallizes in the monoclinic, space group P2(1)/c, a =2.0215(7) nm, b=1.3103(5) nm, c=2.8171(10) nm, beta=95.472(7)degrees, Z=8, V=7.428(5) nm(3), D-c = 1. 330 g/cm(3), mu = 0.834 mm(-1).