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鉬(鎢)硫簇化合物及硫代巴比妥酸衍生物的合成及結(jié)構(gòu)研究

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  本文選題:硫代巴比妥酸衍生物 + 鉬(鎢)硫簇化合物。 參考:《東華大學(xué)》2017年碩士論文


【摘要】:2-巰基吡啶(py2tH)、2-硫代巴比妥酸(H2TBA)及其衍生物1,3-二乙基-2-硫代巴比妥酸(HDETBA)是具有較強(qiáng)配位能力的含氮雜環(huán)化合物。研究表明,py2tH、H2TBA及HDETBA是具有O,S,N等配位點(diǎn)的多齒配體,通常具有豐富的生理活性、光學(xué)特征、化學(xué)和多樣的結(jié)構(gòu),使得人們對(duì)它們的研究興趣日益增長(zhǎng)。本文以py2t H為有機(jī)配體,與[NH4]2[MOn S4-n](M1=W,n1=0;M2=Mo,n2=2),過渡金屬CuX(X1=I,X2=Cl),采用液相擴(kuò)散法、固相合成法合成了簇合物(Bu4N)3[WS4Cu3I4](1)和配合物[Cu6(C5H4NS)6](2)兩種產(chǎn)物。以H2TBA、HDETBA為有機(jī)配體,通過液相擴(kuò)散法分別與稀土金屬鑭、鉺、鈥的高氯酸鹽反應(yīng)得到三種配位聚合物:{[La(H2TBA)4(DMF)4·S][La(H2TBAS-SH2TBA)2(DMF)4]}n(3),{[Er(HDETBA)3(DMF)3(CH3OH)(H2O)]·2DMF}n(4),[Ho(HDETBA)3(DMF)3(CH3OH)(H2O)]n(5)。并利用紅外光譜分析、元素分析以及X-射線單晶衍射等測(cè)試方法全面系統(tǒng)地對(duì)五種產(chǎn)物的結(jié)構(gòu)作了深入的研究。結(jié)果表明簇合物1的結(jié)構(gòu)單元由一個(gè)陰離子[WS4Cu3I4]3-和三個(gè)陽(yáng)離子[Bu4N]+組成類立方烷結(jié)構(gòu)構(gòu)型。配合物2由六個(gè)銅原子與六個(gè)2-巰基吡啶配體配位形成扭曲的八面體構(gòu)型。配位聚合物3由兩種不同的結(jié)構(gòu)單元組成,且兩單元之間通過氫鍵作用相互連接形成三維網(wǎng)狀結(jié)構(gòu),配位聚合物4和5是一維鏈狀結(jié)構(gòu)。
[Abstract]:2-mercaptopyridine py2t H2TBA) and its derivative 1 ~ (3) -diethyl-2-thiobarbituric acid (HDETBA) are nitrogen-containing heterocyclic compounds with strong coordination ability. It has been shown that py2tH2TBA and HDETBA are polydentate ligands with coordination sites such as OTX N, which usually have rich physiological activity, optical properties, chemistry and various structures, which make people have more and more interest in the study of these ligands. In this paper, using py2t H as organic ligand and [NH _ 4] _ 2 [MON S _ 4-n] M _ 1C _ 1 WN _ (1) O _ (2) M _ (2) M _ (2) O _ (2) Mo _ (2) O _ (2), transition metal CuX _ (1) X _ (1) ~ (1), a cluster complex Bu4N _ 3 [WS4Cu _ (3i _ 4)] ~ (1) and its complex [Cu6C _ (5H _ 4NS6)] ~ (2) were synthesized by liquid phase diffusion method. Using H _ 2TBA HDETBA as organic ligand, three kinds of coordination polymers were obtained by liquid phase diffusion reaction with rare earth metal lanthanum, erbium, holmium perchlorate: {[LaH2TBA4DMF4S] [LaH2TBAS-SH2TBA2TBA2DMF4]} n3n, {[ErHDETBA3OOHH] 2DMF} nni4U, [HoHDETBA3OOHHH]. The structures of the five products were studied thoroughly and systematically by means of infrared spectroscopy, elemental analysis and X-ray single crystal diffraction. The results show that the structural unit of cluster 1 is composed of one anion [WS4Cu3I4] 3- and three cations [Bu4N]. Complex 2 is composed of six copper atoms and six 2-mercaptopyridine ligands to form a distorted octahedral configuration. The coordination polymer 3 is composed of two different structural units, and the two units are connected to each other by hydrogen bonding to form a three-dimensional network structure. The coordination polymers 4 and 5 are one-dimensional chain structures.
【學(xué)位授予單位】:東華大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2017
【分類號(hào)】:O641.4

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