Hydrothermal Synthesis,Crystal Structure,Thermal Stability and Photophysical Property of a Novel Zinc Complex with Mixed Ligands

A novel metal-organic coordination complex [Zn(CHIP)(AIC)]n(1, CHIP = 2-(4-chlorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline, AIC = 5-amino-isophthalic acid) has been synthesized by hydrothermal reactions and characterized by elemental analysis, thermogravimetric(TG) analysis, infrared spectrum(IR) and single-crystal X-ray diffraction. Complex 1 crystallizes in monoclinic, space group C2/c with a = 18.259(5), b = 17.191(4), c = 16.371(4) A, V = 4717(2) A3,C27H-116 ClN 5O4Zn, Mr = 575.29, Dc = 1.620 g/cm3, μ(Mo Kα) = 1.202 mm, F(000) = 2335, Z = 8, the final R = 0.032 and w R = 0.074 for 4723 observed reflections(I 2σ(I)). Single-crystal X-ray diffraction reveals that 1 exhibits one-dimensional(1D) double chains, which are linked by H-bond intersections into a 2D structure. TG analysis shows clear weight loss due to the decomposition of different ligands. The luminescent properties for the ligand and complex 1 were also studied.     

Synthesis,Structure and Properties of a Zinc(II) Complex with the Lapacholate Anion and Ethanol as Ligands

The reaction of lapachol, 2-hydroxy-3-(3-methyl-2-butenyl)-1,4-naphtoquinone, C₁₅H₁₄O₃, with zinc acetate, in ethanol, produces a chelate formula Zn(C₁₅H₁₃O₃)₂(C₂H₆O)₂, whose structure has been determined by single crystal X-ray diffraction. It pertains to the triclinic system, space group P I (No. 2), a = 8.2380(3) Å, b = 9.4900(2) Å, c = 11.0110(4) Å, α = 112.536(2)°, β = 91.204(2)°, γ = 92.664(2)°, Z = 1. Some spectroscopic and chemical properties of the complex are also reported.     

Cd(Ⅱ)双苯吡唑基吡啶-草酸混配合物的合成、结构与性质

合成了Cd(Ⅱ)与类蝎型吡唑衍生物和草酸的混合配体的配合物[Cd2(HL)2(ox)]·1.5H2O(H2L=2,6-二(5-苯基-吡唑-3-基)吡啶,H2ox=草酸)。 通过元素分析、红外光谱、紫外光谱、X射线粉末衍射(PXRD)和X射线单晶结构分析确定了配合物的结构。 配合物晶体属于三斜晶系、P-1空间群,Cd(Ⅱ)是六配位,由一个ox2-基中的2个O原子和来自2个HL-中的4个N原子配位,构成变形八面体配位构型,而相邻Cd(Ⅱ)原子间均通过HL-上的N原子和草酸根分别连接形成2条互不相交的一维无限链状结构。 性质测试结果表明,该配合物具有良好的热稳定性和荧光特性,对环己烷氧化反应也具有一定的催化活性。     

二维半导体合金的制备、结构和性质

原子层厚度的二维半导体材料因具有特殊的低维效应而被广泛研究. 面向光电器件应用, 需要可控调节二维半导体材料的能带结构, 包括带隙、价带/导带位置等. 合金方法是一种调控半导体能带的通用方法. 本综述介绍了近几年来二维半导体合金材料的研究进展, 包括材料的热力学稳定性、可控制备、结构表征和性质研究. 介绍的材料体系是过渡金属二硫族化物的单层合金材料, 金属元素主要是第六副族的Mo和W, 硫族元素主要是S和Se.     

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。     

混合配体的铜(Ⅱ)配合［Cu(C2H4O2N)(C12H8N2)(H2O)］.ClO4.2.5H2O的合成、性质及晶体结构

本文对甘氨酸、1,10-邻菲咯啉铜(Ⅱ)固体配合物进行了合成和表征,并利用X射线分析研究了其晶体结构。     

Synthesis,Crystal Structure and Luminescent Properties of a Novel Zinc(II) Complex of N-Acetyl-L-glutamic Acid and Imidazole Ligands

1 INTRODUCTION As is well known, some transition metal ions play an important role in controlling the behavior of many biological macromolecules and produce pro- found effects on their biological actions, medicine and people’s health[1～3]. Zinc is an essential com- ponent of many proteins. In the active sites of zinc enzymes, zinc is bound to the nitrogen of imidazole groups and oxygen of carboxylate groups of amino acids[4～6]. Additional interest in these proteins lies in the fact th…     

Synthesis,Crystal Structure and Luminescent Property of Ladder-shaped Zinc Coordination Polymer with Mixed Polyfunctional Ligands

One new Zn(Ⅱ) complex [Zn_2(cptpy)_2(tzba)(H_2O)]·H_2O(1, Hcptpy = 4-(4-carboxyphenyl)-2,2?:4?,4??-terpyridine(Hcptpy), H_2tzba = 4-(tetrazol-5-yl)benzenecarboxylic acid) has been synthesized and characterized by elemental analysis and single-crystal X-ray diffraction techniques. It is formulated as C52H36O8N10Zn2, crystallizes in monoclinic system, space group P21/c with α = 15.1599(13), b = 28.083(2), c = 10.9039(9) ?, b = 97.517(8)o. V = 4602.3(6) ?3, Z = 4, Mr = 1059.68, Dc = 1.529 g/cm~3, F(000) = 2168 and μ = 1.112 mm-1. The final R = 0.0831 and w R = 0.2143 for 8458 observed reflections with I 2s(I). The assembly of polyfunctional organic ligands Hcptpy and H_2tzba with Zn(II) atoms resulting in a rare example of double-edge ladders, which is further extended into a 3D supramolecular network via O–H···O/N hydrogen bonds. In addition, thermal gravimetric analysis(TGA) and PXRD patterns for 1 were studied. Photo luminescent property of 1 was also investigated.     

Template Synthesis and Structure of Dinuclear Zinc Complex with Three Kinds of Pyrazole Ligands

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Synthesis,Crystal Structure,and Magnetic Properties of a Co Metal-organic Framework with Mixed Dicarboxylate and Tricarboxylate Ligands

One new mixed-ligand coordination polymer,namely[Co_2(btc)(bpdc)_(0.5)(py)_3]_n(1),was hydrothermally synthesized using biphenyl-2,4,4'-tricarboxylic acid(H_3btc) as a main building block,along with two auxiliary ligands(H_2bpdc = 2,2'-bipyridine-5,5'-dicarboxylic acid and py =pyridine).The product 1 was characterized by IR spectroscopy,elemental,thermogravimetric,and single-crystal X-ray diffraction analyses.Single-crystal X-ray diffraction studies show that compound 1 possesses an intricate 3D metal-organic framework based on tetracobalt(Ⅱ) units.Magnetic susceptibility measurement indicates that compound 1 shows an antiferromagnetic coupling between the Co(Ⅱ) ions.     

具有五配位Zn中心的微孔金属有机双桥连配体化合物的溶热合成及表征

A new two dimensional zinc complex was reported. This compound was synthesized under solvothermal condition by using THF as solvent. The crystal structure was determined by using single crystal X-ray diffraction. Crystal data: Zr', (B DC)( D ABCO)( H 20)z, monoclinic, space group C 2/c,a =10.871(17),b=19.10 (3),c=7.15 5(川,a= 90,口二115.99(3),Y=90,Z 二8,V 二1335(4),Dr二2.085岁cm3,R二0.08 58. This compound has two-dimensional network structure. Each zinc metal center was coordinated by two DABCO, two BDC and one water molecule. DABCO and BDC ligands bridge to two zinc atoms, respectively. The extension of this〔。-ordination result in a two-dimensional network and form a 7.16 x 9.98A zporous structure. It was interesting to find that the 2-dimensional was an interpenetrated structure formed by two coordinate polymer networks. This kind of structure is very rare in the coordinate compounds. The m-m interaction between the phenyl group of BDC was believed to the key of the growth of this coordination network.     

六硫基·二(2-甲基吡啶)合锌的结构表征

标题化合物采用锌粉、硫粉及 2 甲基吡啶直接反应 ,最后得到金黄色晶体 ,其结构由X 射线结晶学分析得到晶体数据。晶体属单斜晶系 ,空间群Cc,Z =4,Mr=,a =7.5 10 (2 ) ,b =17.2 95 (5 ) ,c=13.6 85 (1) ,β =94.6 0 (1)° ,V =1771.7 3,Dc=1.6 6 g/cm3,μ(MoKα) =2 0 .9cm- 1,F(0 0 0 ) =90 4。利用 2 389个独立观察点修正到R =0 .0 5 1,Rw =0 .0 6 1。标题化合物是 1个中性分子 ,分子中有 1个扭曲ZnS2 N2 四面体核心。     

一个含苯甲酸配体的Mn-Ce混合金属簇合物的合成、晶体结构与磁性研究

本文使用(NH₄)₂Ce(NO₃)₆氧化Mn2+法合成了1个结构新颖的Mn-Ce混合金属簇合物[Mn₃Ce₂(O)₅(O₂CPh)₉(CH₃OH)₃]·2CH₃CN(1·2CH₃CN, HO₂CPh代表苯甲酸), 并对其进行元素分析、红外光谱、单晶X-射线结构分析、磁性等表征。结构分析表明, 化合物1·2CH₃CN属于三斜晶系P1空间群, 结构中2个Mn⁴⁺离子、2个Ce⁴⁺离子和4个桥连μ₃-O原子组成1个不规则的立方烷, 然后通过另1个桥连μ₃-O原子与另1个Mn³⁺离子相连。晶胞内分子间没有氢键作用, 但存在较强的π-π堆积作用。磁性研究表明, 簇合物内Mn离子之间存在铁磁性耦合作用, 基态自旋值S=5和磁各向异性参数D=-0.31 cm^-1, 交流磁化率没有频率依赖现象。     

一种混合价态钌配合物的合成、晶体结构和电化学性质

[Ru6(μ-O2CCH3)12(CH3OH)2(HCOO)2][Ru2(μ-O2CCH3)4(H2O)2](PF6)2.2H2O(Ru2(Ⅱ,Ⅲ)混合价)是通过二步反应合成的。首先Ru2(O2CCH3)4Cl在加热条件下与甲醇反应得到红棕色中间物,然后将该中间物在甲醇水(体积比7∶1)溶液中用Ag2SO4和NH4PF6进行脱氯配位反应得到此化合物。用元素分析、红外光谱、热重分析、循环伏安、X-衍射单晶结构分析等对其进行了表征。晶体结构表明,标题化合物的晶体属单斜晶系,空间群为P21/n,晶胞参数:a=0.85362(14)nm,b=1.19589(19)nm,c=3.6642(6)nm,β=92.316(3)°,Z=2,每个结构基元包含2个不同的配离子,其中[Ru2(μ-O2CCH3)4(H2O)2]+是1个双核钌配离子,[Ru6(μ-O2CCH3)12(CH3OH)2(HCOO)2]+是由另1个由甲醇配位、甲酸根桥连的六核钌配离子。2个独立的结构单元通过氢键形成三维超分子网络结构。采用循环伏安法对其电化学性质进行了表征,结果为一对准可逆的氧化还原峰,表明该配合物的中心金属二价钌原子Ru(Ⅱ)与三价钌原子Ru(Ⅲ)之间存在电子转移。     

一个含苯甲酸配体的Mn-Ce混合金属簇合物的合成、晶体结构与磁性研究

本文使用(NH4)2Ce(NO3)6氧化Mn2+法合成了1个结构新颖的Mn-Ce混合金属簇合物[Mn3Ce2(O)5(O2CPh)9(CH3OH)3]·2CH3CN(1.2CH3CN,HO2CPh代表苯甲酸),并对其进行元素分析、红外光谱、单晶X-射线结构分析、磁性等表征。结构分析表明,化合物1.2CH3CN属于三斜晶系P1空间群,结构中2个Mn4+离子、2个Ce4+离子和4个桥连μ3-O原子组成1个不规则的立方烷,然后通过另1个桥连μ3-O原子与另1个Mn3+离子相连。晶胞内分子间没有氢键作用,但存在较强的π-π堆积作用。磁性研究表明,簇合物内Mn离子之间存在铁磁性耦合作用,基态自旋值S=5和磁各向异性参数D=-0.31 cm-1,交流磁化率没有频率依赖现象。     

由邻苯二甲酸和Medpq配体构筑的锌的配合物的水热合成及晶体测定

A metal-organic coordination polymer [Zn(Pht)(Medpq)]_n (Pht=phthalic acid, Medpq=2-methyldipyrido[3,2-f:2′,3′-h]quinoxaline) (1) has been hydrothermally synthesized and structurally characterized by elemental analysis, IR spectrum, TG and X-ray single-crystal structure analysis. Title complex crystallizes in the monoclinic system, space group Cc, with a=1.027 4(4) nm, b=2.955 7(11) nm, c=0.685 2(3) nm, β=112.941°, V=1.916 3(13) nm³, C₂₃H₁₄N₄O₄Zn, M_r=475.75, D_c=1.649 g·cm^-3, μ(Mo Kα)=1.324 mm^-1, F(000)=968, Z=4, the final R=0.038 8 and wR=0.071 7 for 2 697 observed reflections (I>2σ(I)). In the crystal structure, the Zinc atom is six-coordinated with four carboxylate oxygen atoms from two different carboxylate groups and two nitrogen atoms from Medpq ligand, showing a slightly distorted octahedral geometry. Furthermore, it exhibits a one-dimensional structure with Pht-Zn-Medpq as building units. CCDC: 716600.     

漆酚缩甲醛镧配合物的制备、结构及性能

利用漆酚缩甲醛(PUF)和三氯化镧在非水热溶剂中反应制得漆酚缩甲醛镧配合物(PUFLa)，IR、XPS和TG表征结果表明：三氯化镧中La^3 与漆酚缩甲醛中酚羟基上的氧形成了配位键；在La^3 的作用下，PUF上的侧链进一步交联聚合。PUFLa在亚硫酸钠水溶液中能引发催化甲基丙烯酸甲酯聚合。通过正交实验设计考察了PUFLa用量、反应温度、反应时间、单体甲基丙烯酸甲酯用量和亚硫酸钠浓度对单体转化率的影响。结果表明。反应温度和反应时间是影响单体转化率的主要因素。PUFLa还具有良好的耐热性和抗溶剂性。     

Synthesis and Crystal Structure of a New Mononuclear Cobalt(Ⅲ) Complex with 2,2''-Dipyridylamine and Glycine as Ligands

A new mononuclear cobalt(Ⅲ) complex [Co(dpa)2(Gly)](ClO4)2·4H2O was synthesized by the reaction of Co2 , glycine (gly) and 2,2'-dipyridylamine (dpa) in a methanol-water solution, and its structure was characterized by IR, EA, ES-MS and X-ray structure analysis. The compound crystallizes in the monoclinic system, space group P21/n with a = 12.8795(2), b =13.2904(2), c = 19.1104(2) (A),β= 109.378(1)°, V= 3085.89(8) (A)3, Z = 4, Mr = 746.36, Dc = 1.606g/cm3,μ= 0.808 mm-1, F(000) = 1536, the final R = 0.0543 and wR = 0.1306 for 5393 independent reflections. The magnetic measurement of the compound at room temperature shows that it is diamagnetic and the cobalt ion is in low spin 3 oxidation state. ES-MS experiments show that the [Co(dpa)2(Gly)]2 cation is very stable in the methanol solution.     

混合配体镍配合物[Ni（NCS）2（phen）2]的合成、晶体结构及荧光性质

合成了含异硫氰酸根和邻菲咯啉（phen）混合配体的镍配合物[Ni（NCS）2（phen）2],通过红外光谱、紫外光谱和X射线单晶衍射等手段对其结构进行了表征.研究了配合物的固体荧光光谱.单晶结构解析结果表明,标题化合物属于正交晶系,Pbcn空间群,晶胞参数为：a=1.296 2（2）nm,b=1.019 0（1）nm,c=1.759 5（2）nm,V=2.323 9（4）nm3,Z=4,Dc=1.530 g/cm3,μ=1.043 mm-1,F（000）=1 096,R1=0.042 1,wR2=0.108 1.配合物中镍离子采用6配位的八面体配位构型,晶体堆积中通过π-π作用形成一维超分子结构.