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1.
在水乙醇混合溶剂中,首次得到了2-羰基丙酸水杨酰腙、1,10-菲啰啉与硝酸钆形成的配合物[Gd(C10H9N2O4)(C10H8N2O4)(H2O)3]2·phen·4H2O,并测试了其单晶结构。该配合物属三斜晶系,空间群为P-1。每个配合物分子中有两个九配位的钆的结构单元,每个钆离子与两个三齿配体2-羰基丙酸水杨酰腙(分别以负一价和负二价形式)和三个水分子配位。每个钆单元在空间呈扭曲的单帽四方反棱柱。同时还有一个游离的1,10-菲啰啉存在于晶格中,通过氢键与配位水作用。生物活性试验表明该配合物对三种病原菌有一定的抑菌活性。  相似文献   

2.
在水-乙醇混合体系中, 以2-羰基丙酸水杨酰腙(C10H10N2O4)、2,2-联吡啶(C10H8N2, 简写bipy)与Eu(NO3)3•4H2O反应, 首次培养出黄色单晶[Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]•0.5bipy•3H2O. 该晶体属三斜晶系, 空间群为P-1, 晶胞参数a=0.93392(16) nm, b=1.3100(2) nm, c=1.3895(2) nm, α=97.205(3)°, β=105.411(2)°, γ=106.364(2)°, V=15.35(2) nm3, Z=2, μ=2.118 mm-1, Dc=1.686 Mg/m3, F(000)=786, R=0.0116, wR=0.0507, GOF=0.995. 晶体测试结果表明, 该单晶结构为铕的9配位配合物, 两个2-羰基丙酸水杨酰腙分别以负一价和负二价酮式和三个水分子同时参与配位; 每个2-羰基丙酸水杨酰腙中的羧基氧、酰胺基中的羰基氧和C=N中的氮与Eu3+配位, 形成两个共边的稳定五元环, 另三个配位原子则分别来自三个水分子中的氧原子, 该配合物在空间呈扭曲的单帽四方反棱柱, 而在不对称单位中还有游离的一个2,2-联吡啶分子和三个水分子, 这些游离分子与配位分子之间存在大量分子内和分子间氢键, 整个分子在空间呈三维网状结构. 发光性能测试表明该配合物具有很好的荧光性质.  相似文献   

3.
武望婷  胡怀明  王尧宇  史启祯 《化学学报》2005,63(22):2032-2036
在水-乙醇混合体系中, 以2-羰基丙酸水杨酰腙(C10H10N2O4)、2,2-联吡啶(C10H8N2, 简写bipy)与Eu(NO3)3•4H2O反应, 首次培养出黄色单晶[Eu(C10H9N2O4)(C10H8N2O4)(H2O)3]•0.5bipy•3H2O. 该晶体属三斜晶系, 空间群为P-1, 晶胞参数a=0.93392(16) nm, b=1.3100(2) nm, c=1.3895(2) nm, α=97.205(3)°, β=105.411(2)°, γ=106.364(2)°, V=15.35(2) nm3, Z=2, μ=2.118 mm-1, Dc=1.686 Mg/m3, F(000)=786, R=0.0116, wR=0.0507, GOF=0.995. 晶体测试结果表明, 该单晶结构为铕的9配位配合物, 两个2-羰基丙酸水杨酰腙分别以负一价和负二价酮式和三个水分子同时参与配位; 每个2-羰基丙酸水杨酰腙中的羧基氧、酰胺基中的羰基氧和C=N中的氮与Eu3+配位, 形成两个共边的稳定五元环, 另三个配位原子则分别来自三个水分子中的氧原子, 该配合物在空间呈扭曲的单帽四方反棱柱, 而在不对称单位中还有游离的一个2,2-联吡啶分子和三个水分子, 这些游离分子与配位分子之间存在大量分子内和分子间氢键, 整个分子在空间呈三维网状结构. 发光性能测试表明该配合物具有很好的荧光性质.  相似文献   

4.
合成了高氯酸镨和咪唑(C3H4N2), DL-α-丙氨酸(C3H7NO2)混配配合物晶体. 经傅立叶变换红外光谱、化学分析和元素分析确定其组成为[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3. 使用具有恒温环境的溶解-反应量热计, 以2.0 mol•L-1 HCl为量热溶剂, 在T=(298.150±0.001) K时测定出化学反应PrCl3•6H2O(s)+2C3H7NO2(s)+C3H4N2(s)+3NaClO4(s)=[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s)+3NaCl(s)+5H2O(1)的标准摩尔反应焓为ΔrHmө=(39.26±0.11) kJ•mol-1. 根据盖斯定律, 计算出配合物的标准摩尔生成焓为ΔfHmө{[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s), 298.150 K}=(-2424.2±3.3) kJ•mol-1. 采用TG-DTG技术研究了配合物在流动高纯氮气(99.99%)气氛中的非等温热分解动力学, 运用微分法(Achar-Brindley-sharp和Kissinger法)和积分法(Satava-Sestak和Coats-Redfern法)对非等温动力学数据进行分析, 求得分解反应的表观活化能E=108.9 kJ•mol-1, 动力学方程式为dα/dt=2(5.90×108/3)(1-α)[-ln(1-α)]-1exp(-108.9×103/RT).  相似文献   

5.
An organic-inorganic hybrid complex, [H2(PW12O40){Zn(C10H8N2)2(H2O)}]·1.5[Zn(C10H8N2)3]·1.75H2O has been synthesized hydrothermally and structurally characterized by X-ray crystallography. The crystal belongs to monoclinic, space grounp C2/c, with a=4.709 4(2) nm, b=1.431 77(7) nm, c=2.621 07(1) nm, β=90.125(4)°, V=17.673 4(2) nm3, Z=8, Dc=3.087 Mg·m-3, F(000)=14 884, μ(Mo Kα)=16.327 mm-1. The structure was refined to R1=0.068 7 and wR2=0.158 0 for 20 128 observed reflections with I>2σ(I). Single crystal structure shows that the title compound is constructed from [PW12O40]3- cluster anion and [Zn(C10H8N2)2(H2O)]2+ metal-organic complex cation, in which metal Zn(Ⅱ) cation are coordinately bonded to the terminal oxygen of Keggin polyanions. The title compound exhibits good catalytic activity for oxidation of benzaldehyde to benzoic acid. CCDC: 624772.  相似文献   

6.
合成了高氯酸镨和咪唑(C3H4N2), DL-α-丙氨酸(C3H7NO2)混配配合物晶体. 经傅立叶变换红外光谱、化学分析和元素分析确定其组成为[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3. 使用具有恒温环境的溶解-反应量热计, 以2.0 mol•L-1 HCl为量热溶剂, 在T=(298.150±0.001) K时测定出化学反应PrCl3•6H2O(s)+2C3H7NO2(s)+C3H4N2(s)+3NaClO4(s)=[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s)+3NaCl(s)+5H2O(1)的标准摩尔反应焓为ΔrHmө=(39.26±0.11) kJ•mol-1. 根据盖斯定律, 计算出配合物的标准摩尔生成焓为ΔfHmө{[Pr(C3H7NO2)2(C3H4N2)(H2O)](ClO4)3(s), 298.150 K}=(-2424.2±3.3) kJ•mol-1. 采用TG-DTG技术研究了配合物在流动高纯氮气(99.99%)气氛中的非等温热分解动力学, 运用微分法(Achar-Brindley-sharp和Kissinger法)和积分法(Satava-Sestak和Coats-Redfern法)对非等温动力学数据进行分析, 求得分解反应的表观活化能E=108.9 kJ•mol-1, 动力学方程式为dα/dt=2(5.90×108/3)(1-α)[-ln(1-α)]-1exp(-108.9×103/RT).  相似文献   

7.
本文采用邻菲罗啉和方酸为配体,在水热条件下通过自组装合成了具有二维网状结构的配位聚合物[Cd(C4O4)(C12N2H8)(H2O)]n,并应用X-光衍射技术测定了其单晶结构。结果表明:Cd原子与2个邻菲罗啉氮原子、3个方酸氧和1个水分子配位,生成了六配位扭曲八面体。方酸以少见的μ-1,2,3配位模式桥联3个中心金属离子,并进一步组装成二维网状配位聚合物。对配位聚合物的光学性能及热稳定性做了进一步的研究,实验结果表明:配位聚合物是具有良好热稳定性的强荧光材料,具有潜在的应用前景。  相似文献   

8.
在pH≈7.5的水溶液中,Na2WO4·2H2O,SbCl3·6H2O, 咪唑与 NiCl2·6H2O (或MnSO4·H2O,Co(NO3)2·6H2O, ZnSO4·7H2O)反应得到了四种咪唑配位的夹心型锑钨多氧酸盐Na9[{Na(H2O)2}3{M(C3H4N2)}3(SbW9O33)2]·xH2O(M=NiII, x = 32, CoII, x = 32,ZnII, x = 33, MnII, x = 34)。用X射线单晶衍射法确定了Na9[{Na(H2O)2}3{Ni(C3H4N2)}3(SbW9O33)2]·32H2O的结构,聚阴离子{Na(H2O)2}3{Ni(C3H4N2)}3(SbW9O33)2]9-具有近似C3v对称性,3个咪唑环垂直于中心带上六个金属离子(Na-Ni-Na-Ni-Na-Ni)所形成的平面。晶体结构中相邻的阴离子间存在着π-π相互作用,相邻咪唑的二面角为60º。用IR, UV-vis, TG 和DSC,对这些化合物的性质进行了表征,推测了它们的热分解过程。  相似文献   

9.
The novel seven-coordinate complex [(n-Bu)2Sn(C10H8N2O3)(C2H5OH)]2 (C10H8N2O32- is the dinegative ion of 2-oxo-propionic acid benzoyl hydrazone) was synthesized by the reaction of (n-Bu)2SnO with 2-oxo-propionic acid benzoyl hydrazone in 1∶1 molar ratio in benzene-ethanol (V/V, 3/1), and its structure was characterized by X-ray single crystal diffraction. The crystal belongs to a tetragonal system with space group I41/a, a=2.4890(2)nm, b=2.4890(2)nm, c=1.5170(3)nm, V=9.398(2)nm3, Z=8, F(000)=3968, Dc=1.366g·cm-3, and the structure was refined to final R1=0.0530, wR2=0.0971. The structure of the title complex is described as a dimer through weak interactions of Sn…O bonding and hydrogen bond. The tin atoms rendered sev-en-coordination in a distorted pentagonal bipyramid geometry structure, four oxygen atoms [O1, O2, O2#1 and O4] and one nitrogen atom N2 formed the equatorial plane and C11-Sn1-C15 is the axis. CCDC: 212696.  相似文献   

10.
The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C10H8N2O3)·(C5H5N)·(H2O) (C10H8N2O32- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm3, Z= 2, Dc= 1.547 Mg·m-3, μ(Mo) = 1.417 mm-1, F(000) = 374. The final R1 = 0.030 6, wR2= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C10H8N2O32- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.  相似文献   

11.
合成了2个新的希土冠醚配合物Ln(NO3)3·C26H38N2O4(Ln=La、Ce; C26H38N2O4=1, 7, 10, 16-四氧-4,13-二氮杂-N,N′-二苄基环十八烷)。通过元素分析,红外光谱,拉曼光谱及其 1H核磁共振谱进行表征。用四圆衍射仪测定了La(NO3)3·C26H38N2O4·CH3CN的晶体结构。晶体属三斜晶系,P1空间群,晶胞参数:a=1.2869(4) nm, b=1.5868(6) nm, c=0.9147(2) nm; α=101.89(2)°, β=105.38(2)°, γ=71.96(3)°; Z=2。dcald.=1.58 g·cm-3, μ(Mo)=13.25 cm-1。中心镧离子与冠醚配体中的4个氧原子和2个氮原子配位,3个硝酸根中的6个氧原子也与La3+配位,形成配位数为12的配合物。  相似文献   

12.
In the title compound, [Pb2(C8H4O4)2(C19H12N4O)2]n·3.5nH2O(1), has been synthesized by the hydrothermal assembly of 1,4-benzenedicarboxylate and 4-(1H-1,3,7,8-tetraazacyclopenta[l]-phenanthren-2-yl)phenol(TCPP) with lead acetate. Elemental analysis, X-ray crystal structure analysis, IR spectrum, thermogravimetric analysis and luminescence property were carried out for the structural determination and characterization of the title compound. Compound 1 crystallizes in triclinic, space group P1 with a=1.013 54(10) nm, b=1.104 84(11) nm, c=1.210 05(12) nm, α=76.812 0(10)°, β=74.814 0(10)°, γ=86.030 0(10)°, V=1.273 1(2) nm3, Pb2C54H39N8O13.5, Mr=1 430.31, Z=1, Dc=1.866 g·cm-3, μ=6.680 mm-1, F(000)=691, R=0.027 3 and wR=0.068 7 for 4 042 observed reflections (I>2σ(I)). The compound 1 exhibits two-dimensional network structures, which are further stacked through π-π interactions and hydrogen bonds to form three-dimensional supramolecular polymer. Solid-state luminescent spectrum of the compound 1 indicates intense fluorescent emission. CCDC: 748883.  相似文献   

13.
(Zn1-xMnx)C2O4·2H2O在空气中的热分解动力学研究   总被引:1,自引:0,他引:1  
用热分析(TG-DTG/DTA)、X射线衍射(XRD)技术和透射电镜(TEM)研究了固态物质Zn1-xMnxC2O4•2H2O在空气中热分解的过程。热分析结果表明,Zn1-xMnxC2O4•2H2O在空气中分两步分解,其失重率与理论计算失重率相吻合。 XRD和TEM结果表明,Zn1-xMnxC2O4•2H2O分解的最终产物为Zn1-xMnxO,其颗粒大小约为10-13 nm。在非等温条件下对Zn1-xMnxC2O4•2H2O的热分解动力学进行了分析。用Friedman法和Flynn-Wall-Ozawa(FWO)法求取了分解过程的活化能E,并用多元线性回归给出了可能的机理函数。Zn1-xMnxC2O4•2H2O两步热分解的活化能分别为155.7513 kJ/mol 和215.9397 kJ/mol。  相似文献   

14.
该文报道了N,N′-(2-苯并咪唑基甲基)亚氨基甲基膦酸{bbimpH2,[(C7H5N2)CH2]2NCH2PO3H2}的2个镍化合物Ni2(bbimp)2(4,4′-bipy)(H2O)2·2H2O (1)和[Ni2(bbimp)2(H2O)2][Ni(bbimp)(H2O)2]2·4H2O (2)。化合物1是4,4′-联吡啶作为桥连配体的中性双核结构。化合物2含有1个中性的[Ni2(bbimp)2(H2O)2]双核分子与2个中性的[Ni(bbimp)(H2O)2]单核分子。双核分子单元中的2个Ni(Ⅱ)离子被2个膦酸氧桥连。在化合物2中,膦酸氧桥连的2个Ni(Ⅱ)离子之间存在铁磁性相互作用。  相似文献   

15.
The novel copper(Ⅱ) coordination polymer with 2-oxo-propionic acid benzoyl hydrazone and hexamethylenetetramine ligands, {Cu(μ2-C10H8N2O3)( μ2-C6H12N4)1/2}n (C10H8N2O32- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR spectroscopy. The crystal structure was determined by single crystal X-ray diffraction analysis. The results show that the crystal of the title coordination polymer belongs to monoclinic space group C2/c, the cell parameters are as follows: a=1.787 5(2) nm, b=0.730 93(9) nm, c=2.038 2(2) nm, β=92.890(2)°, and V=2.659 6(5) nm3, Z=8, Dc=1.687 Mg·m-3, μ(Mo )=1.659 mm-1, F(000)=1 384, R=0.031 1, wR=0.079 0 for 2 454 observed reflections (I>2σ(I)) out of 2887 unique reflections. In this copper(Ⅱ) coordination polymer, each copper(Ⅱ) ion is five-coordinated with a geometry of distorted square-pyramid. Two oxygen atoms of the carboxyl of each C10H8N2O32- acts as a bridge to bond two neighboring copper(Ⅱ) ions, leading to an infinite one-dimensional chainlike coordination polymer. Each chain is linked by coordinated hexamethylenetetramines with its neighbors to form an infinite two-dimensional network structure. CCDC: 255347.  相似文献   

16.
郭鸿旭  王庆华  陈晨  梁敏  陈铃 《中国化学》2008,26(4):640-644
水热合成并通过红外、热重、单晶X-射线衍射表征了一个新颖镍配位阳离子修饰的还原型钼磷酸盐,Ni[Mo6O12(OH)3(PO4)(HPO4)3]2][Ni(H2O)2][Ni(H2O)(bipy)2]4·5H2O。单晶X-射线衍射研究表明,两个{Mo6P4}簇单元通过一个镍离子连接形成一个Ni[Mo6P4]2二聚结构单元,其进一步和其他的镍配位阳离子连接成钼磷酸盐一维链状结构。在H2O2存在下的液-固体系中,使用该化合物催化氧化苯甲醛的探针反应结果表明,该化合物具有较高的催化氧化活性。  相似文献   

17.
在pH≈10的乙醇-水溶液中以硫酸铜、酒石酸和邻菲咯啉反应合成了分子式为[Cu2(C4H2O6)(Phen)2(H2O)]·8H2O的配合物单晶。用X-射线单晶衍射测定了晶体结构,并研究了配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌的抗菌活性。晶体属单斜晶系,空间群P21。标题化合物为双核铜配合物,2个铜原子配位数不同。Cu(1)是五配位的,具有扭曲的四方锥结构,5个配位原子分别是酒石酸的去质子的羟基氧和羧基氧、邻菲咯啉的2个氮原子及1个水分子的氧原子。Cu(2)为四配位的,配位原子分别是酒石酸的去质子的羟基氧和羧基氧和邻菲咯啉的2个氮原子。分子中Cu(1)…Cu(2)间的距离为0.354 8 nm。存在分子内邻菲咯啉-邻菲咯啉的面—面π-π相互作用,面间距为0.381 3 nm。配合物对大肠杆菌、金黄色葡萄球菌、枯草杆菌具有较强的抗菌活性。  相似文献   

18.
在pH=7.5的水溶液中, Na2WO4•2H2O, NaAsO2, CoCl2•6H2O与对氨基吡啶反应, 得到了一种新的夹心型杂多钨酸盐Na6(C5H7N2){[Na(H2O)2]3Co(H2O)5[Co(H2O)]3(AsW9O33)2}•27H2O单晶, 用X射线单晶衍射法及元素分析确定了其结构, 晶体属三斜晶系, P 空间群, 其晶胞参数为: a=1.3276(8) nm, b=1.7581(10) nm, c=2.4381(14) nm, α=70.954(9)°, β=86.663(9)°, γ=72.885(9)°, V=5.136(5) nm3, Z=2, R1=0.0608, wR2=0.0848 [I>2σ(I)]. 在{[Na(H2O)2]3Co(H2O)5[Co(H2O)]3(AsW9O33)2}7-阴离子中, 一个Co2+与聚阴离子{[Na(H2O)2]3[Co(H2O)]3(AsW9O33)2}9-的一个端基氧共价连接, Co2+呈现出5和6两种配位数, 质子化的氨基吡啶正离子作为抗衡离子存在于晶体之中. 对标题化合物进行了IR, UV-Vis, TG-DSC表征. 对该化合物、Na2WO4•2H2O及CoCl2•6H2O催化H2O2氧化乙醛的活性进行了比较研究, 该化合物的催化活性远优于简单化合物Na2WO4•2H2O和CoCl2•6H2O.  相似文献   

19.
溶剂热法合成了1个新配位聚合物{[Ni(C18H18N4O5)(DMF)]·(DMF)}n。通过元素分析、红外光谱、热重以及X-射线单晶洐射对其进行了表征。该晶体为正交晶系,Pna21空间群。该化合物中,C18H18N4O5配体通过5个配位原子以及相邻的溶剂分子DMF上的1个配位原子与Ni(Ⅱ)原子配位,形成了1个扭曲的八面体配位构型。热重分析表明该化合物在140 ℃开始发生分解。  相似文献   

20.
The title coordination compound with N-substituted-salicyl Schiff ligand, Cu(C15H12N2O3)(C5H5N), has been synthesized. The coordination compound crystallizes in orthorhombic system, space group Pbca with a=2.037 62(7) nm, b=0.698 45(2)nm, c=2.508 76(9)nm, V=3.570 4(2) nm3, Z=8, F(000)=1 688, Dc=1.529 g·cm-3, Mr=410.91, μ=1.250 mm-1, R=0.031 3 and wR=0.077 0. In the coordination compound, one phenolate oxygen, one carbonyl oxygen and one hydrazine nitrogen atom from the dianionic ligand N-salicylaldehyde-N′-(4-methoxybenzoyl) hydrazone and one pyridine nitrogen atom coordinate to Cu(Ⅱ) ion, forming a distorted square plane. CCDC: 218182.  相似文献   

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