二(对氯苄基)锡双吗啉氨荒酸酯和二(对氯苄基)氯化锡N,N-二乙基氨荒酸酯的合成、表征及晶体结构  

Synthesis and Crystal Structure of Di(p-chlorbenzyl)tin Bis(dithiomorpholincarbamate)and Chlorodi(p-chlorbenzyl)tin Dithioethylcarbamate

作　　者：尹汉东[1] 王勇[1] 王传华[1] 

机构地区：[1]聊城大学化学系,聊城252059

出　　处：《Chinese Journal of Structural Chemistry》2004年第8期926-931,共6页结构化学（英文）

基　　金：国家自然科学基金(20271025);山东省自然科学基金 (Z2001B02)资助课题

摘　　要：利用二(对氯苄基)二氯化锡和吗啉氨荒酸钠、N,N-二乙基氨荒酸钠反应,合成了二(对氯苄基)锡双吗啉氨荒酸酯C24H28Cl2N2O2S4Sn (Mr = 694.31) 1和二(对氯苄基)氯化锡N,N-二乙基氨荒酸酯C19H22Cl3NS2Sn (Mr = 553.54) 2。用X-射线单晶衍射测定了这2个化合物的晶体结构,测试结果表明:化合物1的晶体为单斜晶系,空间群C2/c, a = 21.998(9), b = 6.469(3), c = 20.204(8) ,β= 94.444(6)o , Z = 4, V = 2866.3(19) 3, Dc = 1.609 g/cm3, μ(MoKα) = 1.394 mm-1, F(000) = 1400,S = 0.955, (?)max = 0.000,R = 0.0389, wR = 0.0817。化合物2的晶体为单斜晶系,空间群P21/c, a = 13.088(10), b = 9.304(7), c = 19.593(14) ,β = 107.158(10)o, Z = 4, V = 2280(3) 3, Dc = 1.613 g/cm3,μ(MoKα) = 1.660 mm-1, F(000) = 1104,S = 1.010, (?)max = 0.001,R = 0.0290, wR = 0.0651。在化合物1中,锡原子呈六配位畸变八面体构型, 化合物2的锡原子则是五配位畸变三角双锥构型。Di(p-chlorbenzyl)tin bis(dithiomorpholincarbamate) (C24H28Cl2N2O2S4Sn, Mr = 6694.31) 1 and chloro- di(p-chlorbenzyl)tin dithioethylcarbamate (C19H[(2)0(2)]Cl3NS2Sn, Mr = [(553.5)(4)]) 2 have been synthesized by reacting di(p-chlorbenzyl)tin dichloride with sodium dithiocarbamate. The crystal structures of 1 and 2 have been determined by X-ray single-crystal diffraction. Crystal data for 1: monoclinic, space group C2/c, a = 21.998(9), b = 6.469(3), c = 20.204(8) [(\305)-45.4(,)] ?= 94.444(6), Z = 4, V = 2866.3(19) 3, Dc = 1.609 g/cm3, ?MoK? = 1.394 mm-1, F(000) = 1400, S = 0.955, (/)max = 0.000, R = 0.0389 and wR = 0.[(08)(17)]; and those for 2: monoclinic, space group P2(1)/c, a = 13.088(10), b = 9.304(7), c = 19.593(14) [(\305)-45.4(,)] ?=107.158(10), Z = 4, V = 2280(3) 3, Dc = 1.613 g/cm3, ?MoK? = 1.660 mm-1, F(000) = 1104, S = 1.010, (/)max = [(0.00)(1)(, )]R = 0.0290 and wR = [(0.0651)(. )]In compound 1, the structure consists of discrete molecules containing six-coordinated tin atom in a distorted octahedral configuration; while in 2, the structure is made up of discrete molecules containing five-coordinated tin atom in a seriously distorted trigonal bipyramidal configuration.

关 键 词：二(对氯苄基)锡双吗啉氨荒酸酯 二(对氯苄基)氯化锡N N-二乙基氨荒酸酯 合成 晶体结构 红外光谱 

分 类 号：O627[理学—有机化学]