稀土元素1：12系列钨锗杂多配合物的合成及性质研究

本文首次合成出八种Ｋｅｇｇｉｎ结构的稀土元素钨锗杂多配合物ＬｎＨＧｅＷ１２Ｏ４０．ｘＨ２Ｏ。用ＩＣＰ，＾１８３ＷＮＭＲ，Ｘ射线粉末衍射，ＩＲ，ＵＶ，循环伏安和ＴＧ－ＤＴＡ热分析等手段，这些杂多配合物进行了表征和性质研究。讨论了结构和性质的关系，为此类配合物的催化应用提供了有效信息。     

K10H5[Ln（PMo7W2VO39）2]五元杂多配合物的合成与表征

合成了通式为K10H5[Ln(PMo7W2VO39)2].nH2O(Ln-La^3 ,Ce^3 ,Pr^3 ,Nd^3 ,Sm^3 ,Eu^3 ,Gd^3 ,Dy^3 ,Yb^3)的9种五元新型杂多配合物,并用元素化学分析,TG,ICP,IR,UV,31^1P,51V-NMR,ESR,XPS,XRD进行了表征,结果表明新配合物仍保持Keggin结构,稀土元素处于配合物的内界。借助TG－DTA,不同温度下的IR,XRD的水溶性实验考察了新配合物的热解性质,得出了热稳定的温度范围为400℃-500℃,为催化研究提供了依据。     

稀土元素1∶12系列钨锗杂多配合物的合成及性质研究

本文首次合成出八种Ｋｅｇｇｉｎ结构的稀土元素钨锗杂多配合物ＬｎＨＧｅＷ１２Ｏ４０·ｘＨ２Ｏ（简写为ＬｎＨＧｅＷ１２，Ｌｎ＝Ｌａ，Ｃｅ，Ｐｒ，Ｎｄ，Ｓｍ，Ｅｕ，Ｇｄ，Ｙｂ；ｘ＝１８～２８）。用ＩＣＰ，１８３ＷＮＭＲ，Ｘ射线粉末衍射，ＩＫ，ＵＶ，循环伏安和ＴＧ－ＤＴＡ热分析等手段，对这些杂多配合物进行了表征和性质研究，讨论了结构和性质的关系，为此类配合物的催化应用提供了有益信息。     

稀土锗钨钒酸根多元杂多配合物的合成和性质

合成了通式为Ｋ１３Ｈ２「Ｌｎ（ＧｅＷ１０ＶＯ３９）２」．ｎＨ２Ｏ（Ｌｎ＝Ｌａ,Ｃｅ,Ｐｒ,Ｎｄ,Ｓｍ,Ｅｕ,Ｇｄ,Ｔｂ,Ｄｙ,Ｙｂ）的１０种杂多配合物。利用ＩＲ,ＵＶ,ＥＳＲ,ＸＰＳ,Ｘ射线粉末衍射和磁化率对其结构进行了表征：循环伏安和极谱法研究了配合物的氧化还原性质,得出配合物经历了３步还原,第一步为钒的双电子可逆还原,第二步和第三步均为钨的不可逆还原;借助认温ＩＲ、变温ＸＲＤ和ＴＧ－ＤＴＡ研究     

稀土元素1∶12系列钨硅杂多配合物的合成及性质

用复分解法合成了七种稀土元素Keggin结构钨硅杂多配合物:LnHSiW_(12)O_(40)·xH_2O。用ICP、~(29)SiNMR、XPS、XRD、IR.UV、极谱、CV和TG—DTA对它们进行了系统研究,并讨论了其结构和性质的关系。     

Keggin结构过氧铌钨磷杂多配合物的合成、表征及催化性能

钼钨的杂多化合物（HPC）在催化、电催化、分子材料、药物等诸多领域中已显示出独特的功能。含过氧金属离子取代的杂多阴离子在催化以过氧化氢为氧化剂的烯烃环氧化反应中具有很高的活性和选择性。近年来,含铌的杂多配合物由于良好的催化活性和抗病毒性,引起了人们的重视。本文合成了8种Keggin结构过氧铌钨磷杂多配合物,并用红外、紫外吸收光谱、极谱-循环伏安、及^183W NMR谱等测试手段对其结构和性质进行了确定和比较,考察了它们对烯烃环氧化反应的催化活性。     

新型杂多配合物K3H2[GeW8Mo3VO40].4H2O的合成与晶体结构

用分步酸化、分步加料法合成出新型杂多配合物Ｋ３Ｈ２「ＧｅＷ８Ｍｏ３ＶＯ４０「．４Ｈ２Ｏ，并用Ｘ射线单晶衍射法测定基晶体结构。     

镧系元素钨硅杂多配合物异构体的合成及性质

合成了通式为K_(13)[Ln(β_i-SiW_(11)O_(39))_2]·xH_2O(Ln=La,Ce,Pr,Nd,Sm,Gd,Er;β_i=β_1,β_3)的两个系列的β-异构体。通过元素分析、极谱、循环伏安法,UV和VIS光谱、磁化率以及热分析等手段研究了异构体的组成和性质。     

镧系元素2：18系列钨磷杂多配合物的合成及性质

本文首次合成了11种镧系元素Dawson结构钨磷杂多配合物:Ln_2[P_2W_(18)O_(62)]·xH_2O(Ln=La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Yb),对它们进行了红外光谱、紫外光谱、极谱、X射线粉末衍射和X光电子能谱研究,并对其结构进行了讨论。     

镧系元素钨钒杂多配合物的合成与表征

报道了镧系元素钨钒杂多配合物的合成方法。元素分析和热重分析确定其通式为：Ｋ７Ｈ６「Ｌｎ（ＶＷ１０ＶＯ３９）２」．ｘＨ２Ｏ（Ｌｎ＝Ｌａ＾３＋、Ｃｅ＾３＋、Ｐｒ＾３＋、Ｎｄ＾３＋、Ｓｍ＾３＋、Ｅｕ＾３＋、Ｇｄ＾３＋、ｄＹ＾３＋、Ｙｂ＾３＋）。利用红外，喇曼，电子自旋共振，紫外和Ｘ射线衍射谱对其进行了表征。配合物的热解性质研究表明，其分解温度范围为４００－４５０℃，还研究了的氧化还原性质。     

A Novel 3D Extended Network Cobalt Paradodecatungstate:Synthesis,Characterization and Crystal Structure of [Co(H_2O)_5]_2[Co(H_2O)_4]_3[H_2W_(12)O_(42)]·11H_2O

1 INTRODUCTION Polyoxometalates are the unique metal-oxygen clusters composed of transition metals in groups V and VI (Mo, W, V, Nb, Ta) in a high oxidation state showing a large structural varieties as well as inte- resting physical and chemical properties in diverse fields including catalysis, analytical chemistry, nanotechnology, chemical sensing, biochemical and geochemical processes, medicine and materials science[1～5]. Recently, there has been increasing interest in the synthesis…     

Keggin型配合物（C12H9N2）3[PMo12O40]的水热合成及晶体结构

采用水热反应合成了有机-无机杂化的Keggin型配合物（C12H9N2）3[PMo12O40],并通过X-射线单晶衍射对其结构进行了分析。该配合物为正交晶系P212121空间群,晶胞参数为a=1.20800（1）nm,b=2.10108（4）nm,c=2.24234（5）nm。配合物包含了孤立的Keggin型[PMo1...     

Synthesis and Crystal Structure of[(CH_3)_4N]_4,H_2[ZnW_(11)SnO_(39)]·9H_2O

1INTRODUCTIONThepseudoliquidcharacterofheteropolycompoundsascatalystisdeterminedbytheircrystallographicproperties"3.Thedeterminationofthecrystalstructureofhet-eropolycompoundhasbecomeanimportantmethodtocharacterizeandidentifythesecompounds,atthesametimeitalsoprovidesinterestinginformationtoenrichhet-eropolyacidandcatalyticchemistry.Inthispaper,wereportthesynthesisandcrys-talstructureof[(CH,).Nj.H,[ZnW,,SnO,,j.gH,O.2EXPERIMENTAL2.1SynthesisNa,WO..ZH,O(18.2g,55mmol)wasdissolvedin…     

Synthesis,Structure and Properties of α Keggin type of K6H3[ZnW11 O40 Al]·9.5H2O

A new heteropolycomplex, K₆H₃[ZnW₁₁ O₄₀ Al]·9.5H₂O was prepared and characterized by means of elemental analysis, IR, UV spectroscopy, ²⁷Al NMR , electrochemistry and X ray crystallography. The crystal of K₆H₃[ZnW₁₁ O₄₀ Al]·9.5H₂O is cubic, space group Fm-3m , with lattice constants a=b=c =2.144 8(2) nm, V =9.866(2) nm³, Mo radiation, R =0.057 8 for 497 independent data with [ I>2δ(I) ]. The anion is of α type Keggin structure with C_s symmetry.     

基于[As_2W_(19)O_(67)(H_2O)]~(14-)构筑的含镧砷钨酸盐的合成和结构表征

通过水热法合成了一例[As_2W_(19)O_(67)(H_2O)]~(14-)({As_2W_(19)})构型保持的稀土衍生物K_(14)H_8[La(H_2O)_3As_2W_(19)O_(67)(H_2O)]_2·53H_2O(1),并测定了其晶体结构.同时,通过红外光谱、粉末衍射(XRPD)以及热分析对其进行了表征.X射线单晶结构分析表明,化合物1属于三斜晶系,P-1空间群,晶胞参数为a=1.239 5(10)nm,b=1.847 8(16)nm,c=2.268 5(19)nm,α=68.366(12)°,β=78.215(13)°,γ=78.406(12)°,Z=1,Mr=11 351.63,V=4.683(7)nm3,μ=24.794mm-1,R1=0.056 4,wR2=0.150 8[I2σ(I)].化合物1是二聚结构,其中LaIII离子采用九配位畸变的单加冠四方反棱柱配位构型.     

A kinetic study of the electron-transfer in the reaction of tribenzylchlorotin with[CoW_(12)O_(40)]~(5-)

A kinetic study of the electron-transfer in the reaction of tribenzylchlorotin with potassium 12-tungsto cobalt(Ⅲ) ate ion, K_5[CoW_(12)O_(40)],abbreviated as Co(Ⅲ)W,has been performed in different solvents.The studies were carried out in methanol, ethanol,acetonitrile and acetic acid/water.The rate constants,reaction rates and activation parameters were calculated. Our findings show that the rate of disappearance of the Co(Ⅲ) is pseudo-first order.The kinetic data is strongly affected by used solvents.T...     

STRUCTURE OF TRISUBSTITUTED TUNGSTOSILICATE ANION [A-β-SiW_9Al_3(H_2O)_2O_36(μ_3-O2/2)]_2~14-

<正> Crystal of H14C[A-β-SiW9Al3(H2O)2O36(μ3-O2/2)]2 ·8H2O belongs to monoclinic system, space group P2/m. with a= 1 7. 525(6), b=14.348(3). c= 21. 669(8) A , β=113. 12(8)°, V = 5011 (3) A3,Z = 2. Dc = 3. 254 g. cm-3, A (MoKα) = 0. 70169 A , μ=223. 21 cm-1, F(000) = 4614, T = 298K. R=0. 066 for 3010 unique reflections [I≥5σ(I) ]. The crystal consists of water molecules, protons (or H3O+ ) and dimeric anions [A-β-SiW9Al3 (H2O)2O36(μ3-O2/2)D214.the half of which has a SiO1 tetrahedron in the center, a W3O13 group, two W2Al(H2O) O12 groups and a W2AlO13 group around the SiO4.     

1-D链状簇合物[Ni(enMe)_2]_2[Ni(enMe)_2{HMoo_4~(VI)Mo_4~V_8~(VI)VO_(40)(V~VO_4)}]·4H_2O的水热合成和晶体结构

水热合成了一种新的1-D链状四帽pseudo-Keggin 结构钼钒簇合物[Ni(enMe)2]2- [Ni(enMe)2{H MoVI4MoV4VIV8O40(VVO4)}]4H2O 1,X-射线单晶结构分析表明,该晶体属单斜晶系,C2/c空间群。晶体学参数为a = 26.3006(6), b = 13.6195(3), c = 19.7122(5) ,b = 105.8330(10), V = 6793.0(3) ?, Z = 4, Dc = 2.566 g/cm3, Mr = 2623.96, m = 3.507 mm-1, F(000) =5088, R = 0.0700, wR = 0.1529, S = 1.019。该簇合物是由金属配位桥Ni(enMe)2桥联四帽pseudo-Keggin 结构{HMoVI4MoV4VIV8O40(VVO4)}簇构成一维链状结构,链与链间通过与另外一个配位阳离子[Ni(enMe)2]2+的氢键相互作用构成超分子网状结构。     

Synthesis and Luminescent Properties of Eu~(3 )-Doped Na_(24)P_2W_(22)O_(83)

TheheteropolytungstateisoneofthemostchallengingprojectsininorganicchemistryduetoitsaPPlicationonsolidstatechemistly,catalysis,biochemistry,separationandanalysis,etcl-4.Inthispaper,thepreparationmethodandluminescencepropertiesofEu' -dopedNanPZW22O83wereinvestigated.Therelationshipbetweentheluminescentpropertiesandcrystalstructurewasdiscussed.ExperimentalThesampleswerepreparedbysolidstatereactionfrommixturesofN'PZO7'10HZO,WOe,NaZWO"ZHzOandEuZO3.Thestoichiometricalmixtureswerecalcined…     

金属有机盐[CpFe(C6H6)]2·[Ni(mnt)2]的合成及晶体结构

通过[CpFe(C6H6)]PF6与Na2[Ni(mnt)2]复分解反应合成了金属有机盐[CpFe(C6H6)]2·[Ni(mnt)2],用元素分析、红外光谱和1H NMR进行了鉴定,并用X射线测定了晶体结构.结构分析表明,该化合物属于三斜晶系,空间群P1.晶胞参数:α=0.838(2)nm,b=1.084(6)nm,c=1.816(7)nm,α=83.41(4)°β=89.30(3)°,γ=80.22(3)°Z=2.晶体中混式夹心的阳离子处于几乎互相垂直的取向.配阴离子平面也存在两种取向,它们形成75.4°的二面角.测试表明,化合物表现半导体属性,其粉末压片室温电导率为4.1×10-S·cm-1.