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1.
在水热条件下,Cu(Ⅱ)-H2biim配合物与Dawson型钨磷酸盐构筑了1个无机-有机杂化化合物[Cu(H2biim)2(H2O)][{Cu(H2biim)2}2(P2W18O62)]·11H2O(1)(H2biim=2,2'-联咪唑)。 通过单晶X射线衍射、红外光谱(IR)、X射线粉末衍射(XRD)、元素分析、电化学分析等技术手段对其进行了表征。 结构分析表明,在化合物1分子中,[P2W18O62]6-单元作为双齿配体与2个Cu2+离子配位形成双支撑的杂多阴离子[{Cu(H2biim)2}2(P2W18O62)]2-,在其外部有1个游离的[Cu(H2biim)2(H2O)]2+ 和11个H2O分子。 H2biim分子与杂多阴离子/H2O分子间存在
氢键,通过氢键、静电和π-π堆积作用,进一步构成具有3D结构的晶体材料。 该晶体化合物对H2O2和NaNO2的还原具有良好的电催化作用;同时,作为酸催化剂用于合成环己酮乙二醇缩酮反应,催化活性高,可重复使用。 相似文献
2.
通过水热法成功合成了两个新的基于(β-Mo8O26)4-构型的无机-有机杂化材料,分子式分别为{[Ni(β-Mo8O26)(H2O)4](H2Fbix) 2H2O}n(1)和{[Co(β-Mo8O26)(H2O)4](H2Fbix) 2H2O}n(2)(Fbix=2,3,5,6-四氟-二(1,4-咪唑-1-甲基)苯)。利用X-射线单晶衍射、X-射线粉末衍射、红外光谱、热重分析和元素分析等对该化合物的结构和性能进行了表征。晶体结构分析表明:化合物1和2为同构化合物。在化合物1中,扭曲八面体构型的NiII与两个β-[Mo8O26]4-单... 相似文献
3.
水合铵硼氧酸盐及其饱和溶液的FTIR和Raman光谱研究 总被引:1,自引:0,他引:1
研究了NH4B5O8·4H2O和(NH4)2B8O13·6H2O及其饱和溶液于20℃的FTIR和Raman光谱,对振动频率进行了归属.根据振动光谱特征,预测(NH4)2B8O13·6H2O中所含基本结构单元为[B7O 11(OH)·B(OH)3]2-.首次将Raman光谱中516cm-1处的强散射峰归属为这一多聚硼氧配阴离子的对称脉冲振动峰,并对以上2种铵硼氧酸盐饱和溶液中硼氧配阴离子的存在形式{B(OH)3,[B3O3(OH)4]-和[B5O6(OH)4]-}和相互作用机理进行了探讨. 相似文献
4.
采用水热合成方法制备了2个基于Keggin型杂多酸的无机-有机杂化物, 化学式分别为{[Cu2(4,4′- bipy)4(H2O)4](SiMo12O40)·18H2O}n(1)和{[Cu2(4,4′-bipy)4(H2O)4](PMo6W6O40)·18H2O}n(2)(bipy=bipyridine). 结构分析 表明2个化合物同构, Cu2+是六配位, 分别与4个4,4′-bipy上的N原子和2个水分子上的O原子结合, 形成 [Cu(4,4′-bipy)2(H2O)2]n2n+二维层状结构. 杂多阴离子通过静电与配位阳离子[Cu(4,4′-bipy)2(H2O)2]n2n+作用交叉排列在层间. 通过红外光谱、 粉末X射线衍射和固体紫外-可见漫反射光谱等对化合物的性质进行了表征. 研究了所合成化合物对水溶性染料亚甲基蓝的降解活性, 发现2种化合物对于亚甲基蓝均表现出显著的光降解活性, 并对它们的催化机理进行了讨论. 相似文献
5.
通过水热方法合成了2个由多铌酸盐和过渡金属配合物形成的有机-无机杂化配合物[Cu(TETA)]4[VNb12(VO)4O40][OH]·10H2O(1)和[Cu(TETA)]4[VNb12(VO)6O40][OH]5·5H2O(2)(TETA=三亚乙基四胺). 化合物1和2的多阴离子分别是由4个{VO5}帽和6个{VO5}帽加盖在Keggin型多铌酸盐的方形缺口上形成的, 它们通过多酸阴离子中Nb-Ot (Ot =端氧)与[Cu(TETA)]2+配合物的金属中心配位构筑形成三维结构. 价键计算结果表明, Keggin中心的钒为+5价, 帽位的钒为+4价, X射线光电子能谱分析(XPS)结果也证实了这一结论. 通过单晶X射线衍射分析、红外光谱(IR)、粉末X射线衍射(PXRD)、热重(TG)分析和元素分析对这2个化合物的结构和性质进行了表征. 相似文献
6.
利用水热法和直接沉淀法, 设计合成了5例由过渡金属(TM)-联咪唑配阳离子与Dawson型钨磷酸阴离子构成的多金属氧酸盐(POM)基有机-无机杂化化合物[Ni(H2biim)3]4[Ni(H2biim)2(P2W18O62)2]·2H2O(1), [CoIII(H2biim)3]2[P2W18O62]·8H2O(2), [Cu(H2biim)2]3[P2W18O62]·4H2O(3), [CoII(H2biim)3]2H2[P2W18O62]·9H2O(4)和 [Ni(H2biim)3]3[P2W18O62]·2H2O(5); 并利用X射线单晶衍射分析(SC-XRD)、 红外光谱(IR)和热重-差热分析 (TG-DTA)等对其进行了表征. 化合物1~5作为载体用于固定辣根过氧化物酶(HRP)时, 显示出了较高的酶固定化能力. 另外, 利用圆二色光谱(CD)和激光扫描共聚焦显微镜(LSCM)等方法评价了固定化酶HRP/1~HRP/5的重复使用性、 储存稳定性和检测过氧化氢(H2O2)的性能. 由于该类POMs与HRP间存在强的相互作用, 利用简单的物理吸附法即可实现POMs对HRP的固载. POMs对酶的固定不但提高了HRP对使用及储存环境的耐受性, 同时也拓展了POMs在酶固定化领域的应用. 相似文献
7.
通过扩散法合成了一个新的配位聚合物{[Cu2(OH)(btre)1.5(1,2,4-btc)]·13H2O}n(1·13H2O)(btre=1,2-二(4H-1,2,4-三唑)乙烷,1,2,4-btc=1,2,4-苯三甲酸根)。测试了1·13H2O的晶体结构,并用红外光谱、元素分析、粉末X射线衍射对其进行表征。单晶X射线衍射表明1是基于四核铜簇[Cu4(μ2-OH)2N12]构筑的10-连接的3D框架,其拓扑符号为312·428·55。研究了1·13H2O的热稳定性以及对甲基橙的催化降解作用。 相似文献
8.
采用水热法合成了一种新型多酸基无机-有机杂化材料{[Co(btp)(Hbtp)(H2O)3](PW12O40)·3H2O}n(1),并对化合物1进行了结构测定。X射线单晶衍射结果显示,Co(Ⅱ)离子通过btp配体连接形成一维链,[PW12O40]3-游离于相邻一维链相互交叉形成的孔隙中,从而扩展成三维结构。热重分析表明化合物1具有良好的热稳定性。此外,还对化合物1的质子导电性能进行了研究。结果表明,化合物1在358 K和98%RH条件下的质子电导率为6×10-5 S·cm-1。 相似文献
9.
制备了K3[Fe(C2H5P2O7)2]·4.5H2O和K3[Fe(C2H6P2O7)2(OH)2]·3H2O两种固体配合物,用化学分析、穆斯堡尔谱、红外光谱、差热热重分析和电导测定等研究了它们的性质,推测了配合物的结构。 相似文献
10.
氢氧化钠与己二胺四甲叉膦酸(H8L)在水溶液中反应合成了一个新型的配合物[Na3(H6L)2(H2O)8][Na(H2O)6]·8H2O(1),其结构经IR和X-射线单晶衍射表征。结果表明1属P-1空间群,晶胞参数a=7.705 9(1) , b=11.655 6(2) , c=18.119 7(3) ,α=97.247(1)°,β=94.797(1)°, γ=101.827(1)°。 1中部分钠离子通过与四膦酸配体中的氧原子配位,形成一维链状结构{[Na3(H6L)2(H2O)8]-}∞,该阴离子链的电荷被孤立离子团[Na(H2O)6]+平衡。在未配位的膦酸基团、氨基、配位水分子、结晶水分子之间的氢键相互作用下,化合物堆积形成一个结构致密的三维超分子结构。 相似文献
11.
Q. Wu P. T. Ma Y. P. Song J. P. Wang J. Y. Niu 《Russian Journal of Coordination Chemistry》2011,37(5):399-403
A unique hybrid borotungstate, [Cu(En)(Phen)(H2O)]4[α-BW12O40]{[Cu(En)(Phen)]2[Cu(En)2 · (H2O)]2[Cu(En)(Phen)(H2O)]2[α-BW12O40]3]} sd 10H2O (I) (Phen = 1,10-phenanthroline, En = ethylenediamine), has been hydrothermally synthesized and characterized by elemental analyses,
IR, and UV spectra, powder X-ray diffraction, thermogravimetric analysis, X-ray photoelectron spectroscopy, and singlecrystal
X-ray diffraction analysis. X-ray crystallography shows that I contains a discrete saturated Keggin-type [BW12O40]5− polyoxoanion and a rare trimeric saturated Keggin-type polyoxoanion {[Cu(En)(Phen)]2[Cu(En)2(H2O)]2[Cu(En)(Phen)(H2O)]2[α-BW12O40]3]}3−. It is noteworthy that I represents the first example of borotungstate containing four saturated Keggin-type units in one molecule. 相似文献
12.
《Journal of Coordination Chemistry》2012,65(13):2238-2248
Two new organic–inorganic polyoxometalates [Cu(dien)(H2O)]2{[Cu2(dien)2(OH)]2[Cu4(B-α-XW9O33)2]}·4H2O (X?=?Sb, 1; X?=?As, 2) (dien?=?diethylenetriamine) were hydrothermally synthesized and characterized by elemental analysis, IR spectra, thermogravimetric (TG) analyses, and single-crystal X-ray diffraction. Both compounds are constructed from one four-coordinate [Cu(dien)(H2O)]2+, one {[Cu2(dien)2(OH)]2[Cu4(B-α-XW9O33)2]} building unit, and four water molecules of crystallization. Structural analysis shows that the sandwich-like polyoxotungstate cluster anions [Cu4(B-α-XW9O33)2]10? are linked by six adjacent dimeric cations [Cu2(dien)2(OH)]3+ into a 2-D architecture with a (6,3)-connected topology. Magnetic measurements of 1 and 2 exhibit the presence of antiferromagnetic interactions within the tetranuclear-CuII cluster. 相似文献
13.
Xuemei Han Wansheng You Limei Dai Lijun Qi Yong Fang Weiwei Li 《Journal of Cluster Science》2009,20(4):707-716
Two coordination polymers based on vanadium-substituted Keggin polyoxotungstophosphates as bridging ligands, {[Ni(4,4′-bipy)1.5(OH)(H2O)]2[H3PW10V2O40]}·4H2O (4,4′-bpy = 4,4′-bipyridine) 1 and {[Ni(dpa)2][Ni(dpa)(H2O)3]2[PW9V3O40]}·4H2O (dpa = 2,2′-dipyridylamine) 2, have been obtained by hydrothermal reactions and characterized by elemental analysis, IR, XRD, TGA and single-crystal X-ray
Diffraction analysis. Compound 1 is a 2D layered structure built from 1D infinite zigzag {Ni2(4,4′-bipy)3(OH)2(H2O)2}n2+ chains bridged via [H3PW10V2O40]2− anions. Compound 2 exhibits a one-dimensional chain-like structure constructed from [Ni(dpa)2]2+ fragments bridged via bis-supported Keggin polyoxoanions [Ni(dpa)(H2O)3]2[PW9V3O40]2−. The two examples demonstrate that vanadium-substituted Keggin polyoxometalates have greater coordination capability. 相似文献
14.
Rui-Ge Cao Ying Liu Qun Tang Liang Wang Lin-Hua Xie Zhong-Min Su 《Journal of solid state chemistry》2009,182(1):49-3394
Four organic-inorganic hybrid compounds based on Anderson-type polyoxoanions, namely, {[Cu(2,2′-bpy)(H2O)3]2[Cr(OH)6Mo6O18]}{[Cu(2,2′-bpy)(H2O)Cl][Cu(2,2′-bpy)(H2O)(NO3)][Cr(OH)6Mo6O18]}·18H2O (1), [Cu(2,2′-bpy)(H2O)2Cl]{[Cu(2,2′-bpy)(H2O)2][Cr(OH)6Mo6O18]}·4H2O (2), (H3O){[Cu(2,2′-bpy)(H2O)2]2[Cu(2,2′-bpy)(H2O)]2}[Cr(OH)6Mo6O18]3·36H2O (3), and (H3O){[Cu(2,2′-bpy)(H2O)2]2[Cu(2,2′-bpy)(H2O)]2}[Al(OH)6Mo6O18]3·33H2O (4), were isolated by conventional solution method, and crystal structures have been determined by single-crystal X-ray diffraction. Among them, compound 1 displays a discrete supramolecular structure, compound 2 shows a chainlike structure with chloro-copper complexes as counteranions, and compounds 3 and 4 are isomorphic and exhibit unique 3D open frameworks with lattice water molecules residing in the channels. The compounds 3 and 4 represent the first example of 3D organic-inorganic hybrid compounds in the TMs/2,2′-bpy/POMs system. Investigation of the reaction conditions reveals that the geometry and size of the anions together with its coordinating abilities to the metal centers have a decisive influence on both the composition and the dimensionality of the final compounds. 相似文献
15.
《Journal of Coordination Chemistry》2012,65(3):259-270
A number of ternary complexes of Cu2+ with thiosemicarbazide (TSC) including [Cu(bpy)(TSC)2]Cl2, [Cu(o-phen)(TSC)2]Cl2 and [Cu(bpy)(TSC)2][CuCl4] [Cu(o-phen)(TSC)2] [CuCl4] have been synthesised and characterized. Their reactivities in aqueous and DMF solutions were studied. It was observed that while on coordination to Cu2+ thiosemicarbazide is converted to thiocyanate in aqueous solution, in DMF solution the thiocyanate is further aerially oxidised to sulfate. In the presence of hydrogen peroxide, oxidation to sulfate is rapid and from the mother liquor we could isolate [(bpy)2Cu2(C2O4)Cl2]·H2O whose structure was determined by X-ray crystallography. X-ray crystal structure of [Cu(bpy)(H2O)2SO4] is also discussed.* 相似文献
16.
Two new heteropolyoxovanadoborates (H2dap)2H6{(VO)12O6[B3O6(OH)]6(H2O)}·13H2O (1, dap = 1,2-diaminopropane) and {[Zn(dien)]2[Zn(dien)(H2O)]4(VO)12O6[B3O6(OH)]6(H2O)}2·15H2O (2, dien = diethylenetriamine) have been hydrothermally synthesized and structurally characterized. Both 1 and 2 contain {(VO)12O6[B3O6(OH)]6(H2O)} cluster (denoted on V12B18), which is constructed by a puckered B18O36(OH)6 ring sandwiched between two triangles of six alternating cis and trans edge-sharing vanadium atoms, and a central water molecule. 1 consists of discrete [V12B18]10− cluster anions with H2dap2+ as counterions, while 2 consists of discrete neutral {[Zn(dien)]2[Zn(dien)(H2O)]4[V12B18]} clusters, which are built from two types of zinc(II) complex fragments connecting with V12B18 cluster through two Zn-(μ
3-O)-B bonds. Interestingly, 2 is the only example of the V12B18 cluster decorated by two types of zinc(II) complex fragments. 相似文献
17.
《Journal of Coordination Chemistry》2012,65(3):522-532
Three supramolecular compounds based on [P2Mo5O23]6? and Ni(II)–bim, [Ni(bim)3]3[P2Mo5O23]·2H2O (1), [Ni(Hbim)(bim)2]4[P2Mo5O23]2·3H2O (2), and [Ni(bim)(Hbim)(phen)]2[P2Mo5O23]·7H2O (3) (bim?=?2,2′-biimidazole, phen?=?1,10-phenanthroline), have been synthesized under hydrothermal conditions and characterized by elemental analysis, single-crystal X-ray diffraction, IR, and TG. All the compounds show 3-D supramolecular networks constructed from weak interactions among free Ni(II) complex, water, and oxygens of [P2Mo5O23]6?. Compound 3 represents the first supramolecular example integrating {Ni(bim)(Hbim)(phen)} with Strandberg-type phosphomolybdate. The compounds display good electrocatalytic activity to reduce hydrogen peroxide and intense fluorescence properties in solution at room temperature. 相似文献
18.
Two new hybrid compounds, [Cu(1)(phen)(H2O)][Cu(2)(phen)(H2O)]([Cu(3)]0.25(H2O)][P2Mo5O23]·3.75H2O (1) and [Cu(en)2]1.5[P2Mo5O23]2·(enH2)3·2H2O (2) (phen = 1,10-phenanthroline, en = ethylenediamine), have been hydrothermally synthesized and characterized by IR, UV–Vis spectroscopy, X-ray photoelectron spectroscopy (XPS), powder XRD analyses, TG analyses, cyclic voltammogram analyses, elemental analyses, and single crystal X-ray diffraction analyses. Single crystal X-ray diffraction analyses reveal that the two compounds have a 1-D chain structure formed by Strandberg-type POMs and TMCs with –A–B–C–B–A–B–C–B– linking mode, then further extend into a 2-D layer structure through π?π or hydrogen bond interactions. 相似文献
19.
Gerasko O. A. Virovets A. V. Sokolov M. N. Dybtsev D. N. Gerasimenko A. V. Fenske D. Fedin V. P. 《Russian Chemical Bulletin》2002,51(10):1800-1805
The supramolecular compounds {[W3Se4Cl3(H2O)6]2[PyHC36H36N24O12]}Cl3·18H2O (1) and {[Cl3SnMo3Se4Cl3(H2O)6][Cl3SnMo3Se4Cl2(H2O)7](C36H36N24O12)}Cl·26H2O (2) were isolated from solutions of the selenium-containing tungsten and molybdenum clusters [W3Se4(H2O)9]4+ and [Cl3SnMo3Se4(H2O)9]3+, respectively, and organic cavitand cucurbituril. X-ray diffraction analysis demonstrated that the macrocylcic cucurbituril molecule is coordinated on both sides by the cluster cations through the formation of complementary hydrogen bonds. Compound 1 has a chain structure stabilized by Se...Se interactions between the adjacent cluster cores. In compound 2, the bridging 2-selenium atoms of the cluster fragment Mo3Se4 are coordinated to the tin atom of the SnCl3
– ligand, thus losing the ability to be involved in Se...Se interactions. 相似文献
20.
The new complexes [Mn(Hpchce)2(o-phen)], {2[Mn(pchcm)(o-phen)2]}·7H2O and [Ni(Hpchcm)(o-phen)2]Cl·CH3OH with [N′-(pyridine-4-carbonyl)-hydrazine]-carbodithioic acid ethyl ester (H2pchce) and [N′-(pyridine-4-carbonyl)-hydrazine]-carbodithioic acid methyl ester (H2pchcm) have been synthesized, containing o-phenanthroline (o-phen) as a coligand. These ligands and their complexes have been characterized by elemental analyses, IR, magnetic susceptibility and single crystal X-ray data. H2pchce (2), [Mn(Hpchce)2(o-phen)] (3) {2[Mn(pchcm)(o-phen)2]}·7H2O (4) and [Ni(Hpchcm)(o-phen)2]Cl·CH3OH (5) crystallized in the monoclinic system, space group Pc, C2/c, P21/n and P21/n, respectively. The (N, O) donor sites of the bidentate ligands chelate the Mn(II) and Ni(II) centers forming a five-membered CN2OM ring. The resulting complexes are paramagnetic and have a distorted octahedral geometry. 相似文献