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C19H22Cl3N2S4Sn (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, m(MoKa) = 1.394 mm-1, F(000) = 1400, S = 0.955, (D/s)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, m(MoKa) = 1.660 mm-1, F(000) = 1104, S = 1.010, (D/s)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 chlorodi- (p-chlorbenzyl)tin dithioethylcarbamate (C19H22Cl3N2S4Sn, Mr = 553.54) 2 have been synthesized by the reaction of di(p-chlorbenzyl)tin dichloride with sodium dithiocarbamate. The crystal structures were deter- mined by X-ray single-crystal diffraction. The crystal of compound 1 belongs to monoclinic, space group C2/c with a = 21.998(9), b = 6.469(3), c = 20.204(8) , ?= 94.444(6)o, Z = 4, V = 2866.3(19) 3, Dc = 1.609 g/cm3, (MoK) = 1.394 mm1, F(000) = 1400, S = 0.955, (?)max = 0.000, R = 0.0389 and wR = 0.0817. The crystal of compound 2 is of monoclinic, space group P2(1)/c with a = 13.088(10), b = 9.304(7), c = 19.593(14) , ?=107.158(10)o, Z = 4, V = 2280(3) 3, Dc = 1.613 g/cm3, ?MoK) = 1.660 mm1, F(000) = 1104, S = 1.010, (?)max = 0.001, 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 compound 2, the structure consists of discrete molecules containing five-coordinated tin atom in a seriously distorted trigonal bipyrami- dal configuration.
基金
国家自然科学基金(No. 20271025)
山东省自然科学基金 (No. L2003B01)
