新型4-氟水杨酸双核铜配合物的合成及其荧光性能

以4-氟水杨酸(H2foac)和2,2'-联吡啶(bipy)为原料,甲醇和水为溶剂,醋酸铜为离子源,采用溶剂热法合成了一个新型的双核铜配合物{[Cu2(foac)2(bipy)2]·3H2O(1)},其结构和荧光性能经IR,FL,元素分析和X-射线单晶衍射表征。1属三斜晶系,Pī空间群,晶胞参数a=8.198(2),b=9.986(3),c=11.814(4),α=91.45(3)°,β=105.78(2)°,γ=92.87(3)°,V=928.8(5)3,Z=1,Dc=1.433 g·cm-3,μ=1.210mm-1,F(000)=408。1中两个Cu(Ⅱ)分别与bipy的两个氮原子,foac2-的两个氧原子及另一个foac2-的桥联氧原子配位形成扭曲的四方锥配位环境。在375 nm激发波长激发下,1的发射峰位于390 nm。     

新型单核镍配合物的原位合成及其荧光性能

以3,5-二氯水杨醛和碳酰肼为原料,DMF和乙腈为溶剂,硝酸镍为离子源,采用溶剂热法原位合成了一个新型的单核席夫碱配合物Ni(L){1, H₃L=(3,5-二氯-2-羟基-苯亚甲基)［N′-(3,5-二氯-2-羟基-苯亚甲基)］-1-氨基-N-氨基甲酸},其结构经FT-IR,元素分析和X-射线单晶衍射表征。1(CCDC: 1 044 165)属单斜晶系,空间群P2₁/m,晶胞参数a=10.416 6(5) , b=6.516 2(3) , c=13.479 1(6) , β=109.330(5)°, V=863.34(7) ³, Z=2, Dc=1.834 g·cm^-3, μ=1.764 mm^-1, F(000)=474。 Ni(III)与L^3-中的两个氮原子和两个氧原子配位,形成一个平面的四配位结构。用荧光发射光谱研究了1的荧光性能。结果表明：在最大激发波长（435 nm）激发下,1的DMF溶液在500 nm附近显示出较强的荧光性能。     

铕(Ⅲ)-锌(Ⅱ)双核配合物的合成和表征

Two new Eu(Ⅲ)-Zn(Ⅱ) binuclear complexes Zn(Salen)EuL₃ have been synthesized, where Salen=Shiff base of bissalicylaldehyde with ethlenediamine and L=acetylacetone (for complex Ⅰ) or trifluoroacetylacetone (for compelx Ⅱ). Analytical experimetal such as IR, UV and elemental analysis suggest the possible component and structure, the fluorescence spectrum of the complex Ⅱ suggests the M^*→M fluorescence mechanism.     

硝酸铕与二甲基甲酰胺配合物的研究

一、配合物合成及溶解性 配合物按文献[1]的方法合成,为微红色粉末,易溶于水、DMF、DMSO、乙醚、甲醇、乙醇、丙酮、氯仿,不溶于甲苯、二甲苯、CCl_4。 二、分析方法及实验条件 分析方法和实验条件同文献[1];燃烧能的测定仪器、实验条件,量热计当量计算和热交换校正,燃烧焓的换算和生成热的计算同文献[2]。 结果与讨论 一、配合物的性质 1.组成分析 元素分析实验值(％):Eu27.26,C20.07,H3.76,N14.85;计算值(％):Eu27.27,C19.40,H3.80,N15.08。 2.熔点及X-射线粉末衍射分析 配合物熔点为102.0～102.5℃;配合物及硝酸铕水合物     

双酚大环配体硝酸铕三元配合物的合成、晶体结构与荧光性质

在硝酸铕模板下用丙二胺和2,6-二甲酰基-4-甲基苯酚通过[2＋2]缩合反应, 合成了一个新的双酚亚胺大环配体硝酸铕三元配合物[Eu(H2L)(NO3)3] (L表示大环配体), 并进行了系统的物理表征. 晶体结构研究表明: 配合物为中性分子, 由一个Eu3＋, 一个中性大环配体(H2L)和三个配位硝酸根组成. 晶体结构属单斜晶系, P21/c 空间群, 晶胞参数a＝1.57296(11) nm, b＝0.96957(7) nm, c＝1.91196(13) nm, β＝104.445(1)°, V＝2.8237(3) nm3, Z＝4, R＝0.0507, wR＝0.1168, Eu3＋为10配位, 呈扭曲的双冠四方反棱柱配位构型. 在低温下(77 K), 配合物在甲醇溶液中以紫外光激发产生了Eu3＋离子特征的荧光发射.     

新型β-二酮铕配合物的合成和性能研究

以肉桂酸和苯乙酮为原料合成了1,5-二苯基-4-烯-1,3-戊二酮（DPPD）配体,以DPPD为第一配体,1,10-邻菲罗啉为第二配体,合成了稀土铕配合物并通过红外光谱进行了表征,同时,研究了配合物的发光性能。     

稀土铕三元配合物-甲基丙烯酸甲酯共聚物的合成和荧光性能研究

在较温和的条件下,利用二苯甲酰甲烷为第一配体,甲基丙烯酸为第二配体与氯化铕在乙醇中反应,合成了一个新的稀土三元配合物Eu(DBM)2MA.2H2O[DBM:C6H5COCHCOC6H5,MA:CH2C(CH3)COO-]。然后将铕三元配合物与甲基丙烯酸甲酯(MMA)进行共聚反应,制备了一个新的键合型稀土高分子共聚物。通过元素分析、EDTA配位滴定分析、红外、紫外、荧光光谱分析测定了配合物及共聚物的组成、结构和发光性能;利用差热-热重分析测定了共聚物的热稳定性,用差示扫描量热法和凝胶色谱法测定了共聚物的玻璃化温度和平均分子量。研究结果表明,稀土三元配合物和相应的共聚物在612.94 nm处均能发出强的Eu3+特征荧光。     

芳香羧酸铕-含氮杂环配体三元配合物的合成及性质研究

分别以苯甲酸、苯乙酸、β-苯丙酸、苯丙烯酸为第一配体,1,10-邻菲口罗啉或2,2′-联吡啶为第二配体,合成了7种铕(Ⅲ)的三元配合物。通过元素分析、配位滴定分析,确定了各配合物的组成。通过红外光谱对配合物的结构进行了初步表征,在配合物中羧基氧原子和邻菲口罗啉及联吡啶中的氮原子均参与了配位。采用TG-DTG技术对7种配合物的热分解过程进行了研究,以phen为第二配体的4种铕(Ⅲ)的三元配合物具有良好的热稳定性。室温下测定了各配合物粉末的激发和发射光谱。结果表明:羧酸配体相同,以邻菲口罗啉为第二配体的配合物的荧光强度要大于以联吡啶为第二配体的配合物的相应荧光强度。7种铕(Ⅲ)的三元配合物中,最强发射峰强度顺序为:Eu(-βPPA)3phen>Eu(BA)3phen>Eu(PLA)3phen>Eu(BA)3bipy>Eu(PLA)3bipy>Eu(CA)3phen.H2O>Eu(CA)3bipy(其中BA为苯甲酸根、PLA为苯乙酸根、β-PPA为β-苯丙酸根、CA为苯丙烯酸根、phen为1,10-邻菲口罗啉、bipy为2,2′-联吡啶)。     

均苯三甲酸铕二元配合物的合成及其荧光性质

以1,3,5-苯三甲酸(H3BTC)为配体,采用溶液沉淀法合成了均苯三甲酸铕二元发光配合物Eu(BTC).2H2O(1),其结构经IR,元素分析和等离子体原子发射光谱(ICP)表征.荧光光谱分析结果表明,1在紫外光照射下,发出Eu3+的特征红光,其中电偶极跃迁(5D0→7F2,613 nm)的发射最强;同时1还具有相对...     

铕三元配合物-聚氨酯丙烯酸酯发光材料的合成与荧光性能研究

以1,10-邻菲啰啉和2,7-二羟基萘-3,6-二磺酸钠为配体,合成了铕-2,7-二羟基萘-3,6-二磺酸-邻菲啰啉三元配合物{[Eu(HL)(phen)(H2O)](H2O)3}∞;利用配合物中未参与配位的-OH作为活性基团,以二月桂酸二丁基锡为催化剂,与具有活性基团-NCO的异佛尔酮-二异氰酸酯反应制备铕三元配合物-聚氨酯丙烯酸酯发光材料。通过X射线单晶衍射、红外、热分析和荧光光谱分析,测定了配合物及发光材料的组成、结构、热稳定性和发光性能。结果表明,在496 nm波长激发下,配合物及发光材料在610 nm处能发出较强的特征荧光,且随着配合物含量的增加,荧光性能增强,同时在测试范围内没有发生荧光淬灭现象,是一种极具潜在应用的新型发光材料。     

A Novel Tripyridyldiamine Nickel Complex:Synthesis,Structure and Characterization

A novel nickel(II)complex[Ni(H2 tpda)(NCS)2(CH3 OH)]was synthesized by using tripyridyldiamine as ligand and Ni(NCS)2 as starting materials,and characterized by a variety of techniques including single-crystal X-ray diffraction,IR spectroscopy and TG-DSC.The single-crystal structure reveals that the complex exhibits as a neutral molecule and that the central atom Ni(II)is octahedrally coordinated by an H2 tpda,two NCS-ions and a ligand molecule CH3 OH.The 3 D supramolecular network is formed through hydrogen bonds andπ-πinteractions.The complex can catalyze the addition reaction of carbon dioxide and propylene oxide.     

Synthesis and Characterization of a Novel Coordination Complex Based on Fluorescein

A novel coordination complex,{[Cd)2(C_(20)H_(10)O_5)_2(H_2O)_4]·10H_2 O}_n,has been synthesized based on fluorescein(2-(6-hydroxy-3-oxo-3 H-xanthen-9-yl) benzoic acid) and systematically characterized by elemental analysis,infrared(IR) spectrum,thermo gravimetric analysis(TGA),powder X-ray diffraction(PXRD) and single-crystal X-ray diffraction.Compound 1 crystallizes in monoclinic,space group P2/n with a = 20.428(5),b = 8.084(2),c = 21.689(5) ?,β = 96.360(5)o,M_r = 993.46,V = 3559.7(15) ?~3,Z = 4,D_x = 1.845 g/cm~3,μ = 1.276 mm-1,F(000) = 1974,GOOF = 1.044,λ(Mo Kα) = 0.71073 ?,the final R = 0.0553 and wR = 0.1720 for 7245 observed reflections with I 2σ(I).     

新型富勒烯膦金属配合物的合成

用配体取代法合成了新型富勒烯膦金属配合物——C60.双(二苯基膦)戊烷合钯[C60Pd(dpppe),1],其结构经UV-Vis,IR,XPS及元素分析表征。在1的分子结构中,C60以σ-π配位方式与Pd配位,形成新型的η2-C60双齿膦金属配合物。     

In situ Ionothermal Synthesis and Characterization of a Novel Cuprous Halide Complex

A new compound [mpba][Cu_2Br_3](1, mpba = 4-(N-methylpyridin-4-yl)benzoic acid) has been ionothermally synthesized and characterized by single-crystal X-ray diffraction analysis, infrared spectrum, elemental analyses, fluorescence spectrum, and thermogravimetric analysis. In compound 1, the [mpba]+ cation is a new organic template, which is obtained firstly in this work by in situ alkylation reaction of N-heterocycles 4-(pyridin-4-yl)benzoic acid with [Emim]Br(Emim = 1-ethyl-3-methyl imidazolium). Hirshfeld surface analysis shows that weak interactions between the [mpba]+ cations and 1D inorganic [Cu_2Br_3]~– are mainly C–H···Br hydrogen bonds. In addition, a pairwise O–H···O interaction is observed between the adjacent [mpba]+cations. These different types of weak interactions make compound 1 stable up to 300 ℃. Fluorescence spectrum investigation shows 1 has a strong yellow emission at 555 nm. Theoretical calculation not only demonstrates compound 1 is a wild band semiconductor with a 3.3 e V band gap but also elucidates the fluorescence emission derives from the p-π* transition of electrons from [Cu_2Br_3]~– to [mpba]~+.     

A Novel Cobalt(III) Mixed-polypyridyl Complex: Synthesis, Characterization and DNA Binding

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Synthesis and Characterization of a Novel Lanthanide Complex with Photoluminescent and Semiconductive Properties

A novel lanthanide complex [La(2,5-PA)(2,5-HPA)(H₂O)₂]_n · nH₂O (I) (2,5-H₂PA = 2,5-pyridinedicarboxylic acid) was synthesized by a hydrothermal reaction and structurally characterized by singlecrystal X-ray diffraction (СIF file CCDC no. 1570808). Complex I is characteristic of a two-dimensional (2D) layered structure with the La₃+ ion coordinating with seven oxygen atoms and two nitrogen atoms to yield a slightly distorted monocapped square antiprism. The [La(2,5-PA)(2,5-HPA)(H₂O)₂]_n layers and lattice water molecules interlink together through hydrogen bonding interactions to give a three-dimensional (3D) supramolecular framework. Photoluminescence measurements under room temperature with solidstate samples show that it displays an emission in the green region of the light spectrum. Solid-state UV-Vis spectrum conducted with solid-state samples reveals the existence of a wide optical band gap of 3.57 eV.     

壳寡糖锌(Ⅱ)配合物的合成与结构表征

以壳寡糖(COS)为配位体,锌(Ⅱ)离子为配位离子,在均相反应条件下合成了壳寡糖锌(Ⅱ)配合物(COS-Zn),并优化了配合物的合成条件.利用红外光谱法(FT-IR)、差热分析法(DTA)和元素分析(EA)进行结构表征,并对配位机理进行了初步探讨.     

新型链状镍配合物的水热合成及其性质

采用水热法合成了一种新型的镍配合物{\[Ni(bipy)(H₂O)₄]·(H₂Dhbs)₂·(H₂O)₄}_n（H₂Dhbs=2,5-二羟基苯磺酸，bipy=4,4′-联吡啶），其结构和性能经FL， IR，元素分析，X-射线单晶衍射和TG表征。结果表明：bipy与镍离子配位，形成链状结构。H₂Dhbs-配体没有参与配位，仅起平衡结构电荷的作用。在结构单元中，\[Ni(bipy)(H₂O)₄]²⁺， H₂Dhbs^-和自由水分子之间通过氢键连接。与配体相比，配合物的荧光发射峰发生了红移，最大发射峰位于464 nm，荧光寿命为2.081 7 ms。     

Synthesis and Characterization of a Novel Phosph(V)azane-Tin(IV) Complex

Abstract

The reaction of bis(anilino)phosphine oxide (C₆H₅NH)₂P(O)H, 1 with Bu₂ ⁿSnCl₂ in the presence of an excess of triethylamine (TEA) in dry tetrahydrofurane (THF) yields the novel N,O-bonded tin complex Bu₂ ⁿSn[NPh(O)P(H)NPh(HNEt₃)]₂, 2. TEA is used as a base to deprotonate the phosphazane ligand and is separated as Et₃NH⁺Cl^?, whereas HTEA⁺ exists in the final product 2 and act as a charge balancing and H-bond structure–directing agent. This new compound has been fully characterized by means of IR, MS, and multinuclear (¹H, ³¹P, and ¹¹⁹Sn NMR) spectroscopy.