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1.
新型化合物[Ni(en)2V6O14]n的水热合成与晶体结构   总被引:1,自引:0,他引:1  
金属 -氧簇合物在催化吸附、医药临床、能量存储和材料科学等方面的应用越来越受到关注 [1~ 3 ] .钒 -氧簇合物的结构新颖 ,在材料领域中具有广泛的应用前景 .采用水热合成技术 ,以简单的无机、有机起始原料在相对低温下制备金属 -氧簇合物晶体是近年来刚刚兴起的研究工作 [4 ] ,并且已经合成出一维链状化合物 Cu(prn) 2 V2 O6[5]、层状结构 Ni(C10 H8N2 ) 2 V3 O8.5[6]及三维网状结构 (H2 en Me)[Ni(en) 2 V12 O2 8][7] .我们采用水热技术合成了由 { V V 2 O7} n 单元层与桥配体 [Ni(en) 2 ]2 +构建的三维无机 -有机化合物 [Ni(en…  相似文献   

2.
金属氧酸盐因其在医药临床、工业催化、功能材料等方面的广泛应用而引起人们的关注[1~6], 其中, 有关钒化学的研究一直很活跃, 钒具有与钼、钨明显不同的结构特性, 钒可以采取VO4, VO5和VO6方式配位, 同时, 钒的价态可以是+3, +4和+5价. 由于钒可采取多种配位方式及多种价态, 与钼酸盐和钨酸盐相比, 钒酸盐更具有结构柔顺性, 同时易形成低价或混合价态物种.在以往的文献中, 有关P-V-O体系多金属氧酸盐的水热合成的研究已有大量的报道[7], 在常规溶液合成中, 人们已对As-V-O体系进行了相对深入的研究, 而有关水热合成的研究报道却很少, 已见报道的砷钒化合物有K6*6H2O[8,9], 4-[10], 6-[11](X=SO2-3, SO2-4, H2O). 为了探究水热条件下As-V-O体系的反应特性, 我们开展了这方面的研究工作, 并取得了突破性进展. 本文采用中温水热技术合成了含有机基团的砷矾超分子化合物2**4H2O, 探讨这类化合物的非线性光学性质、催化性质及其它功能特性将是一个非常有意义的研究领域.  相似文献   

3.
利用水热合成方法制备了Keggin结构多金属氧酸盐[Mn(phen)3]2(H3O)·2H2O,用元素分析、红外光谱、热分析和X射线单晶衍射测试技术对其结构进行了表征. 结果表明,该化合物属于单斜晶系,C2/c空间群,a=2.728 5(3) nm,b=2.506 0(3) nm,c=1.633 6(18) nm,β=104.911(2)°,V=10.79 4(2) nm3,Z=4,R1=0.078 4,wR2=0.199 9. 化合物分子结构单元由1个Keggin结构多金属氧酸盐阴离子5-,2个配位阳离子[Mn(phen)3]2+,1个质子和2个结晶水分子构成. 化合物分子之间通过π-π堆积作用形成了三维超分子结构.  相似文献   

4.
采用水热法合成了一个钨-钒簇聚物[Cu(en)2]2[WⅥ4.5WⅤ2VⅤVⅣ9.5O4 4{Cu(en)2(H2O)}2]·3H2O(1,en=乙二胺),并通过X射线单晶衍射、元素分析、傅里叶变换红外光谱、X射线粉末衍射、热重分析、价键计算、X射线光电子能谱、电子顺磁共振和磁性分析对其结构和性能进行了表征.结果表明,化合物1是以双支撑的四帽Keggin结构[WⅥ4.5WⅤ2VⅣ9.5O4 0(VⅤO4){Cu(en)2(H2O)}2]4-钨-钒簇合物阴离子为基本结构单元,与4个[Cu(en)2]2+配合物阳离子以共价键和弱键相连接形成二维层状结构,相邻层又通过氢键连接成三维超分子网络.研究了化合物1的磁性及光催化降解罗丹明B的活性.  相似文献   

5.
利用水热技术合成了一种新型[Co(bim)x]配合物修饰的磷钼多金属氧酸盐超分子化合物[Co(bim)3] [Co(Hbim)2( H2 O) P2 Mo5 O23]·5H2O.通过元素分析、红外光谱、热重分析和X射线单晶衍射对化合物进行了表征.化合物属于单斜晶系,P2(1)空间群;晶胞参数:a=11.505 (2) nm,b=19.123 (3) nm,c=13.852(2) nm,α=90.00°,β=100.073(2)°,γ=90.00°,V=3 000.6(8)nm3,F(000)=1 756.0,Z=2.并测试了合成化合物的电化学性质.  相似文献   

6.
多金属氧酸盐 ( POMs)由于结构新奇 ,物理性能优异 ,在催化、医药、材料和光化学等领域有应用前景 ,而受到人们广泛关注 [1~ 8] .近年来 ,水热技术和有机指导剂的引入促进了 POMs的有机 -无机杂化材料如 [N( CH3) 4]5V18O4 6 [2 ]和 [V4 O10 ( phen) 2 ][3]等研究的迅速发展 .以上化合物多数仅以有机胺为抗衡离子或直接配位连接到无机骨架上 .而以过渡金属配合物为结构导向剂的合成策略 ,最近才引起人们的重视[9~ 11] .本文以钒酸盐 -过渡金属配合物作为研究体系 ,在水热条件下合成了一种未见文献报道的由新型过渡金属配合物连接的…  相似文献   

7.
采用水热法合成了一个钨-钒簇聚物[Cu(en)2]2[WⅥ4.5WV2 VVVⅣ9.5O44{Cu(en)2(H2O)}2]·3H2O(1, en=乙二胺),并通过X射线单晶衍射、元素分析、傅里叶变换红外光谱、X射线粉末衍射、热重分析、价键计算、X射线光电子能谱、电子顺磁共振和磁性分析对其结构和性能进行了表征.结果表明,化合物1是以双支撑的四帽Keggin结构[WⅥ4.5WV2 VⅣ9.5O40(VVO4){Cu(en)2(H2O)}2]4-钨-钒簇合物阴离子为基本结构单元,与4个[ Cu( en)2]2+配合物阳离子以共价键和弱键相连接形成二维层状结构,相邻层又通过氢键连接成三维超分子网络.研究了化合物1的磁性及光催化降解罗丹明B的活性.  相似文献   

8.
孙英华  杨美玲  郭庆芳  陈迪  姜小宇 《应用化学》2014,31(10):1210-1215
用水热方法合成了一个新型的钼钒多金属氧酸盐[PⅤMoⅥ7MoⅤVⅣ8O44][Ni(Phen)2OH]4·3H2O(1),用元素分析、红外光谱和X射线单晶衍射等技术手段对化合物的晶体结构进行了表征。结果表明,该化合物属于三斜晶系,P-1空间群,a=1.51300(11)nm,b=1.74813(15)nm,c=2.58896(18)nm,α=72.842(4)°,β=89.240(5)°,γ=72.627(5)°,V=6.2233(8)nm3,Z=1,R1=0.0962,wR2=0.2572。化合物是高还原态的四帽α-Keggin结构钼钒多金属氧簇,通过簇阴离子4个钒帽上的端氧分别支撑4个镍过渡金属配合物,形成一个中性的多金属氧酸盐。多金属氧簇上的端氧与结晶水分子之间的强烈氢键使化合物形成了三维超分子结构。  相似文献   

9.
多金属氧酸盐在催化、医药和材料等方面的应用越来越成为无机化学研究的热点[1~5].水热合成技术在合成多核金属氧酸盐中有独特的优点.在众多的钼钒酸盐中,只有几种双帽及四帽Keggin结构被合成出来[6~13].本文报道一种含有不同配位阳离子的四帽Keggin结构砷钼钒酸盐[Co(en)3]·[Co(en)2(H2O)2]2·[Mov4MoⅥ4VⅣ8O40(AsO4)]的合成与结构.该化合物的结构是由不同的阳离子--1个[Co(en)3]3+和2个[Co(en)2(H2O)2]2+及簇阴离子[Mov4MoⅥ4VⅣ8O40(AsO4)]5-构成的.[Mo8V8O40(AsO4)]5-簇阴离子具有四帽"Keggin"结构,两对V原子位于4个"双帽"位置,簇笼中央是1个{AsO4}四面体.  相似文献   

10.
多金属氧酸盐在催化、医药和材料等方面的应用越来越成为无机化学研究的热点[1~5].水热合成技术在合成多核金属氧酸盐中有独特的优点.在众多的钼钒酸盐中,只有几种双帽及四帽Keggin结构被合成出来[6~13].本文报道一种含有不同配位阳离子的四帽Keggin结构砷钼钒酸盐[Co(en)3]·[Co(en)2(H2O)2]2·[Mov4MoⅥ4VⅣ8O40(AsO4)]的合成与结构.该化合物的结构是由不同的阳离子--1个[Co(en)3]3+和2个[Co(en)2(H2O)2]2+及簇阴离子[Mov4MoⅥ4VⅣ8O40(AsO4)]5-构成的.[Mo8V8O40(AsO4)]5-簇阴离子具有四帽"Keggin"结构,两对V原子位于4个"双帽"位置,簇笼中央是1个{AsO4}四面体.  相似文献   

11.
Scandium magnesium gallide, Sc2MgGa2, and yttrium magnesium gallide, Y2MgGa2, were synthesized from the corresponding elements by heating under an argon atmosphere in an induction furnace. These intermetallic compounds crystallize in the tetragonal Mo2FeB2‐type structure. All three crystallographically unique atoms occupy special positions and the site symmetries of (Sc/Y, Ga) and Mg are m2m and 4/m, respectively. The coordinations around Sc/Y, Mg and Ga are pentagonal (Sc/Y), tetragonal (Mg) and triangular (Ga) prisms, with four (Mg) or three (Ga) additional capping atoms leading to the coordination numbers [10], [8+4] and [6+3], respectively. The crystal structure of Sc2MgGa2 was determined from single‐crystal diffraction intensities and the isostructural Y2MgGa2 was identified from powder diffraction data.  相似文献   

12.
13.
On Dialkali Metal Dichalcogenides β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 and Rb2Te2 The first presentation of pure samples of α- and β-Rb2S2, α- and β-K2Te2, and Rb2Te2 is described. Using single crystals of K2S2 and K2Se2, received by ammonothermal synthesis, the structure of the Na2O2 type and by using single crystals of β-Na2S2 and β-K2Te2 the Li2O2 type structure will be refined. By combined investigations with temperature-dependent Guinier-, neutron diffraction-, thermal analysis, and Raman-spectroscopy the nature of the monotropic phase transition from the Na2O2 type to the Li2O2 type will be explained by means of the examples α-/β-Na2S2 and α-/β-K2Te2. A further case of dimorphic condition as well as the monotropic phase transition of α- and β-Rb2S2 is presented. The existing areas of the structure fields of the dialkali metal dichalcogenides are limited by the model of the polar covalence.  相似文献   

14.
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16.
[(n‐Bu)2Sn(O2PPh2)2] ( 1 ), and [Ph2Sn(O2PPh2)2] ( 2 ) have been synthesized by the reactions of R2SnCl2 (R=n‐Bu, Ph) with HO2PPh2 in Methanol. From the reaction of Ph2SnCl2 with diphenylphosphinic acid a third product [PhClSn(O2PPh2)OMe]2 ( 3 ) could be isolated. X‐ray diffraction studies show 1 to crystallize in the monoclinic space group P21/c with a = 1303.7(1) pm, b = 2286.9(2) pm, c = 1063.1(1) pm, β = 94.383(6)°, and Z = 4. 2 crystallizes triclinic in the space group , the cell parameters being a = 1293.2(2) pm, b = 1478.5(4) pm, c = 1507.2(3) pm, α = 98.86(3)°, β = 109.63(2)°, γ = 114.88(2)°, and Z = 2. Both compounds form arrays of eight‐membered rings (SnOPO)2 linked at the tin atoms to form chains of infinite length. The dimer 3 consists of a like ring, in which the tin atoms are bridged by methoxo groups. It crystallizes triclinic in space group with a = 946.4(1) pm, b = 963.7(1) pm, c = 1174.2(1) pm, α = 82.495(6)°, β = 66.451(6)°, γ = 74.922(6)°, and Z = 1 for the dimer. The Raman spectra of 2 and 3 are given and discussed.  相似文献   

17.
The structures of the hypophosphites KH2PO2 (potassium hypophosphite), RbH2PO2 (rubidium hypophosphite) and CsH2PO2 (caesium hypophosphite) have been determined by single‐crystal X‐ray diffraction. The structures consist of layers of alkali cations and hypophosphite anions, with the latter bridging four cations within the same layer. The Rb and Cs hypophosphites are isomorphous.  相似文献   

18.
Summary The ability of [MoS4]2–, anions to be used as ligands for transition metal ions has been widely demonstrated, especially with Fe2+. The present study has been restricted to linear complexes such as (NEt4)2 [Cl2FeS2MoS2] and (NEt4)2[Cl2FeS2MoS2FeCl2]. Their electrochemical properties are described: upon electrochemical reduction, these compounds yield MoS2, as a black precipitate, and an iron complex in solution, assumed to be [SFeCl2]2–. The electrochemical reduction goes through two electron transfers, coupled with the breakdown of the molecular skeleton: a DISPl and an ECE mechanism. Depending on the solvent, the following equilibrium may be observed: [Cl4Fe2MoS4]2–[Cl2FeMoS4]2–+FeCl2. The equilibrium constant, KD, was evaluated by differential pulse polarography. KD is tightly related to the donor number of the solvent.  相似文献   

19.
TG and DTA studies on Me3SnO2PCl2, Me2Sn(O2PCl2)2 and Ph3SnO2PCl2 were carried out under dynamic argon atmosphere. The results show that the decomposition proceeds in different stages leading to the formation of Sn3(PO4)2 as a stable product. This compound was characterized by IR spectroscopy. Decomposition schemes involving reductive elimination reactions were proposed.  相似文献   

20.
Wu YT  Linden A  Siegel JS 《Organic letters》2005,7(20):4353-4355
[reaction: see text] Fluoranthene 2 and heptacycle 3 are easily accessible from the reaction of diyne 1 and norbornadiene (NBD) in the presence of the rhodium catalyst. The unusual [(2+2)+(2+2)] adduct 3 was confirmed by the X-ray crystal structure analysis.  相似文献   

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