新型硅钨酸盐的水热法合成、结构表征和磁性

用水热方法合成了新型的硅钨杂多氧酸盐(C2H10N2)3(SiW12O40)·3H2O,用元素分析、IR和单晶X射线衍射分析技术对化合物的分子和晶体结构进行了表征。 结果表明,该化合物的晶体属于三斜晶系,P1空间群,a=1.3193(3) nm,b=1.3198(3) nm,c=1.3193(3) nm,α=76.05(3)°,β=76.13(3)°,γ=76.05(3)°,V=2.1231(7) nm3,Z=1,R1=0.0518,wR2=0.1355。 化合物分子由一个α-Keggin结构的硅钨多金属簇阴离子、3个乙二胺分子作为平衡阳离子和3个结晶水分子组成,簇阴离子的端氧与乙二胺阴离子及结晶水分子之间的多种类型的氢键连接形成三维超分子结构。 化合物磁性测量表明,其分子内存在反铁磁性相互作用。     

一种新的二帽Keggin多金属氧酸盐的合成、表征及磁性

在水热条件下合成了一种新的二帽二支撑的Keggin型钼钒多金属氧酸盐[Cu(2,2'-bpy)₃]{[Cu(2,2'-bpy)₂]₂HP^ⅤMo8VIV6IVO₄₂]}·2H₂O(1,bpy=联吡啶),利用元素分析、红外光谱、X射线光电子能谱,粉末和X射线单晶衍射等分析技术对化合物的晶体结构进行了表征。 结果表明,该化合物属于单斜晶系,C2/c空间群,a=2.8734(3) nm,b=1.47333(12) nm,c=2.31023(16) nm,β=112.509(5)°,V=9.0351(12) nm³,Z=1,R₁=0.0489,wR₂=0.1286。 化合物的阴离子是二帽α-Keggin结构P/Mo/V多金属氧簇,通过簇阴离子两个钒帽上的端氧分别支撑两个铜过渡金属配合物,化合物簇阴离子,水分子和2,2'-联吡啶分子之间通过π-π和氢键作用形成了三维超分子结构。     

新奇的双帽 pseudo-Keggin 结构磷钼钒酸盐的水热合成、晶体结构、性质及其量子化学计算

报道了一种新奇的磷钒酸盐[NH₄]₄H[PMo₈V₄^ⅣV₂^ⅤO₄₂]·24H₂O的合成方法,用元素分析、EPR、IR、UV谱和TG等手段进行了表征,并用X射线衍射法测定了晶体结构.结果表明,该杂多酸盐属于四方晶系,空间群P4/mnc,a=b=1.2592(2)nm,c=1.7565(4)nm,V=2.7848(8)nm³,Z=2.杂多阴离子具有双帽pseudoKeggin结构,不仅其中的8个金属位置被V和Mo无序占有,而且整个磷钼钒酸盐杂多阴离子的取向也是无序的.还应用EHMO方法研究了簇阴离子的电子结构.     

一种新型钼钒多酸化合物的合成、结构与荧光性能

采用水热技术,合成了一种新型四帽Keggin结构多酸化合物[H₃Mo₈^ⅥV₈^ⅣO₄₀(AsO₄)](en)₂(4,4-bipy)₇·9H₂O(en:乙二胺;bipy:联吡啶)(1),并对化合物进行了元素分析、红外光谱、X射线光电子能谱和X射线单晶结构分析。 晶体结构分析表明, 化合物属三斜晶系,P1空间群,晶胞参数a=1.47395(5) nm,b=1.48172(6) nm,c=1.62881(7) nm,α=66.16(3)°,β=87.15(2)°,γ=63.42(1)°,V=2.8723(2) nm³,Z=1,R₁=0.0728,wR₂=0.2014。 化合物由四帽Keggin多酸阴离子、4,4'-联吡啶、乙二胺和结晶水分子构成,化合物分子间存在大量的氢键,使化合物1形成3-D超分子结构。 荧光测试表明,化合物1能发出较强的荧光,有可能成为潜在的光活性材料。     

夹心型钼磷酸盐的水热合成与晶体结构

采用水热法合成了首例含过渡金属铬的夹心型钼磷酸盐〔Ｈ３Ｎ（ＣＨ２）６ＮＨ３〕２Ｈ３｛Ｃｒ〔Ｍｏ６Ｏ１５（ＨＰＯ４）（Ｈ２ＰＯ４）３〕２｝·４Ｈ２Ｏ超分子化合物,用单晶Ｘ－射线测定其晶体结构,该晶体属三斜晶系,空间群Ｐ１。晶胞参数ａ＝１２．１５６（２）,ｂ＝１２．８０９（３）,ｃ＝１３．５３０（３）,α＝１０２．４６（３）°,β＝９３．６７（３）°,γ＝９３．４６（３）°．Ｖ＝２０４６．９（７）３,Ｚ＝１,Ｍｒ＝２７６８．６９,Ｄｃ＝２．２４６ｇ／ｃｍ３,Ｆ（０００）＝１３３７,μ＝２．１６２ｍｍ－１,全矩阵最小二乘法修正至Ｒ＝０．０６６６,ｗＲ＝０．１７４５,独立可观测点数为７１４２。化合物是分别由质子化的１,６－己二胺、水和｛Ｃｒ〔Ｍｏ６Ｏ１５（ＨＰＯ４）（Ｈ２ＰＯ４）３〕２｝７－阴离子构成,而｛Ｃｒ〔Ｍｏ６Ｏ１５（ＨＰＯ４）（Ｈ２ＰＯ４）３〕２｝７－是由２个〔Ｍｏ６Ｐ４〕与Ｃｒ３＋形成了６配位的夹心型阴离子     

一种新型三维配位聚合物的合成以及表征和磁性测定(英文)

通过水热法合成了三维(3D)网状金属有机框架物[Pr(NTA)(H2O)]n(NTA=nitrilotriacetic acid);利用元素分析、红外光谱分析、X射线单晶衍射等表征了产物的结构,利用热重分析和示差热重分析评价了其热稳定性,并测定了其磁性能.结果表明,目标配合物的Pr(Ⅲ)采取九配位模式(N1O8)形成三帽三角棱柱几何构型,配位聚合物通过O-C-O链组装成高度有序的3D结构.此外,合成的配合物具有较高的热稳定性,并因(O2C-C-C-CO2)2桥联而显示反铁磁性.     

新型笼状钼磷超分子化合物的水热合成与晶体结构

用水热法首次合成了含有２ 种有机胺的新型笼状钼磷超分子化合物〔ＮＨ３（ＣＨ２）６ＮＨ３〕７〔ＮＨ３（ＣＨ２）２ＮＨ３〕２（Ｈ３Ｏ）６〔Ｐ２ Ｍｏ５Ｏ２３〕４·１１Ｈ２Ｏ,并通过元素分析、红外和Ｘ－ 射线单晶衍射法进行了结构表征．晶体属三斜晶系,空间群ｐ１杂多阴离子中的每个〔Ｐ２Ｍｏ５Ｏ２３〕６－ 是由５ 个ＭｏＯ６ 八面体和两个ＰＯ４ 四面体键合而成,其中Ｍｏ,Ｐ原子成一个畸变五角双锥构型．     

磷钼钒酸盐的电子结构与催化性质的研究

本文通过CNDO/2量子化学方法对Keggin型磷钼钒酸盐的电子结构和催化性质的理论研究,导出了该类杂多化合物的价成键轨道结构普适规则,并推广到其他同多杂多化合物。本文根据对前线分子轨道和化学键性质的分析,探讨了随杂阴离子中钒原子数目的变化,磷钼钒酸盐的氧化性质和氧化催化性质变化的规律。     

一种钴-取代型有机-无机杂化三维超分子多酸:合成、结构与表征

在水热条件下,成功合成了一例过渡金属钴修饰的有机-无机杂化Dawson型三维超分子多金属磷钨酸簇合物[Co(dap)_3]_2[H_2P_2W_(18)O_(62)]·11H_2O (1)(dap=1,2-丙二胺),采用X射线单晶衍射、元素分析、红外光谱及热重分析对化合物进行了结构分析和基本表征.化合物1属于正交晶系,Pnma空间群,单胞参数为a=2.688 92(7) nm,b=2.176 67(6) nm,c=1.480 93(5) nm,α=β=γ=90°.从超分子化学的角度来看,化合物1中的饱和Dawson型簇阴离子和金属-有机复合物之间通过广泛的氢键作用,进而形成有趣的4,8-连接的三维超分子网络结构.     

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（H2O2]2·[Mo4^ⅤMo4^ⅥV8^ⅣO40（AsO4）]的合成与结构

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.     

Hydrothermal Synthesis,Crystal Structure and Magnetic Properties of a Cobalt(II) Coordination Polymer Assembled by 4-Sulfophthalate and 4,4'-Bipyridine

1 INTRUDUCTION The rational design and synthesis of metal-direc- ted supramolecular framework have received much attention in coordination chemistry because of their potential applications in catalysis, molecular selec- tion, non-linear optics, ion exchange and microelec- tronics[1～4]. During the lastdecade, many high-di- mensional coordination complexes have been de- signed and prepared through molecular self-as- sembly process[5～10]. The construction of open metal organic framework, s…     

Hydrothermal Synthesis,Structure and Magnetic Property of a Novel Hexa-Ni~Ⅱ Substituted Polyoxometalate

A novel hexa-NiⅡ substituted trilacunary Keggin polyoxometalate [{Ni6（μ3- OH）3（en）3（H2O）6}（B-α-PW9O34）]-6H2O 1 （en = ethylenediamine） has been hydrothermally synthesized and characterized by IR spectra, elemental analysis, thermogravimetric analysis （TGA）, single-crystal X-ray diffraction and magnetic property. Compound 1 crystallizes in the hexagonal space R3c with a = 20.4124（5）, c = 21.4427（4）A, γ = 120.000°, V = 7737.5（3）A3, Z = 6, GOF = 1.083, R （wR） = 0.0317 （0.0610）. Single-crystal X-ray diffraction indicates that 1 contains a hexa-Nin substituted trivacant Keggin [{Ni6（μ3-OH）3（en）3（H2O）6}（B-α-PW9O34）] unit. The magnetic study shows the presence of ferromagnetic coupling interactions within hexa-Nin clusters with J1 = 0.69 cm-1 and J2 = 0.92 cm^-1 for 1.     

Synthesis, Crystal Structure and Luminescent Property of a One-dimensional Europium Citrate Complex

A new compound, [Eu(Hcit)(H2O)2]·H2O]n (1, Hcit3-= C(OH)(COO-)(CH2COO-)2), has been synthesized under hydrothermal reactions of europium oxide, MnCl2·4H2O and citric acid at 120 ℃ for three days. The compound was characterized by single-crystal X-ray diffraction analyses, IR and TGA. Complex 1 crystallizes in monoclinic, space group P21/n with a = 6.179(1), b = 9.688(2), c = 16.990(3) , β = 91.98(3)°, Z = 4, V = 1016.4(3) 3, C6H11EuO10, Mr = 395.11, Dc = 2.582 g/cm3, μ = 6.218 mm-1, F(000) = 760, R = 0.0183 and wR = 0.0411. Single-crystal X-ray analysis reveals that complex 1 displays 1D ladder chains along the a axis, with dinuclear Eu2O2 units serving as "steps" and carboxylate groups as "uprights", which are connected by hydrogen bonds. The solid-state luminescent property of complex 1 was investigated at room temperature. Upon excitation at 394 nm, compound 1 exhibits interesting luminescent properties with several intense bands in the visible region and the most intense and sharp emission being in the red region at 615 nm. The TGA and XRD results prove that complex 1 undergoes facile thermal decomposition to form Eu2O3 at about 870 ℃.     

不同形态的α-Fe2O3纳米粉体的水热合成、表征及其磁性研究

Four different hematite (α-Fe₂O₃) nanopowders with various morphologies have been synthesized in the presence of surfactant (HPC) via hydrothermal route at 180 ℃, using four kinds of iron salts, Fe₂(SO₄)₃, FeC₂O₄, FeSO₄ and (NH₄)₃Fe(C₂O₄)₃, as precursor materials. The products were characterized by means of X-ray diffraction (XRD), transmission electron micrograph (TEM), Fourier transform infrared spectroscopy (FTIR) and magnetization measurements. The hysteresis measurements show that the products exhibit weak ferromagnetic property at room temperature. It is concluded that the different precursor materials and the presence of the surfactant are important factors that exert significant effects on the morphologies and magnetic properties of the products.     

Hydrothermal Synthesis and Characterization of Carbohydrate Microspheres Coated with Magnetic Nanoparticles

Carbohydrate microspheres coated with magnetic nanoparticles were prepared by hydrothermal synthesis where a species of carbohydrate, such as vitamin C, glucose, and soluble starch, were used to obtain microsphere templates as the core of the composite microspheres. The dimension of the carbohydrate microspheres could be well controlled by adjusting the concentration of the starting material, the temperature, and the reaction time. The morphology of the magnetic composite microspheres was characterized by field‐emission scanning electron microscopy (FE‐SEM). The composition, as well as the structure of the composite microspheres, was confirmed by Fourier transform infrared spectroscopy (FTIR) and x‐ray diffraction (XRD).     

Synthesis, Crystal Structure and Magnetic Properties of a New 3D Cobalt Vanadate

A new cobalt vanadate compound 1 [Co^Ⅱ(H2O)2V2^VO6] has been hydrothermally synthesized and characterized by the elemental analyses and the single crystal X-ray diffraction analysis. Compound 1 crystallizes in the orthorhombic system, space group Pinna, with a=0.55646, b=1.06900, c=1.18452 nm, and Z=4. The magnetic susceptibility of the cobalt vanadate has been measured and indicates possible antiferromagnetic coupling between adjacent cobalt (Ⅱ) (0.5432—0.5697 nm) through bond or space.