Hydrothermal Synthesis and Structure of a New Two- dimensional Zincophosphite:Zn2(HPO3)3(H2DACH (DACH = 1,2-diaminocyclohexane)

A new open-framework zincophosphite, Zn2(HPO3)3(H2DACH 1, was hydrothermally synthesized in the presence of 1,2-diaminocyclohexane (DACH) as structure-directing agent. Its structure was determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction and thermogravimetric analysis. Crystal data for 1: Mr = 486.88, monoclinic, space group P21/c with a = 10.2287(11), b = 9.7624(11), c = 16.1686(18) A,β = 92.573(2), V = 1612.9(3) A3, Z = 4, Dc = 2.005 g/cm3, F(000) = 984, μ = 3.314 mm-1 and S = 1.152. The final R = 0.0473 and wR = 0.1121 for 2456 observed reflections with I > 2σ(I). The inorganic layer consisting of four- and eight-membered rings is constructed of alternating ZnO4 tetrahedra and HPO3 pseudo pyramids by sharing vertices. The organic template molecules reside in the interlayer region and interact with the inorganic network through H-bonds.     

A New 3-D Supramolecular Framework Built by Co_4-Substituted Sandwiched Phosphotungstates,Organoamines and Co-Complexes: Synthesis,Structure, and Property

A neoteric organic-inorganic hybrid Co-substituted phosphotungstate H6{[Co(en)2(OAc)2]2[Co4(H2 O)2(PW9 O34)2]}?2 H2 en?36 H2 O(1, en = enthylenediamine) has been made under hydrothermal conditions and characterized by IR spectrum, thermogravimetric analysis, diffuse-reflectance spectroscopy, powder X-ray diffraction, single-crystal X-ray diffraction and cyclic voltammetry, respectively. Crystal data for 1: monoclinic, P21/c, a = 18.2234(12), b = 15.3696(9), c = 20.1706(17) ?, β = 106.563(8)°, V = 5415.1(7) ?3, Z = 2, Mr = 6072.30, Dc = 3.724 g/cm3, μ = 20.087 mm-1, F(000) = 5540, R = 0.0585, w R = 0.1543 and S = 1.024. Single-crystal X-ray structure analysis reveals that compound 1 exhibits a 3-D supramolecular framework via H-bonding interactions, in which the discrete Co-complex is modified by two types of organic ligands, en and acetate. In addition, the adsorption experiments demonstrate compound 1 possesses a remarkable capability for scavenging of methylene blue.     

Hydrothermal Synthesis and Structure of One New Polyoxotungsate [Ni(trien)]_4[Ni_4(H_2O)_2(HPW_9O_(34))_2]·4H_2O

One new sandwich-type tetra-nickel substituted polyoxotungsate,[Ni(trien)]4-[Ni4(H2O)2(HPW9O34)2]·4H2O(1,trien=triethylenetetramine),has been hydrothermally synthesized and characterized by IR,elemental analysis,TGA,and single-crystal X-ray diffraction analysis.Crystal data for 1:triclinic,space group P with a=13.279(3),b=13.816(3),c=14.494(4),α=95.403(1),β=113.173(4),γ=93.809(3)o,V=2418.0(10)3,Z=1 and Dc=3.861 g/cm3.X-ray crystallographic study shows that compound 1 is a relatively rare inorganic-organic hybrid polyoxo tungstate constructed from sandwich Ni-substituted polyoxo-anions and nickel complexes.     

含有两个簇阴离子[As_8V_(14)O_(42)(SO_4)]~(6-)的金属-氧簇合物(H_2en)_6[As_8V_(14)O_(42)(SO_4)]_28H_2O的水热合成与晶体结构

合成了一种新的砷-钒-氧簇合物(H2en)6[As8V14O42(SO4)]28H2O(en为乙二胺),用元素分析、IR和TG-DTA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, 该晶体属单斜晶系,P21/c空间群,晶胞参数a = 20.9235(4),b = 11.9382(2),c = 43.5783(6) 牛琤 = 102.13,V = 10642.1(3) ?,Z = 4,Mr = 4678.01,Dc = 2.920 g/cm3,F(000) = 8944,m = 7.437 mm-1,R = 0.0735,wR = 0.1361。结构测定表明,结构中2个簇阴离子{[As8V14O42(SO4)]6-}与有机铵阳离子[H2en]2+之间靠静电作用相结合,同时与H2O通过氢键构成无限的三维骨架结构。     

几种卟啉及其配合物合成方法的改进

本文首先改进了meso位有强推电子基团的四-[4-(N,N-二甲基)苯胺基]卟啉(TDMAPPH~2)的合成方法.在此基础上, 改进了最近报道的一种新型水溶性卟啉四-[4-(N,N,N-二甲基, 丙磺酸基)苯胺基]卟啉(TDMAPPTPSH~2)的合成, 进而合成了系列水溶性金属卟啉(M'TDMAPPTPS, M'=Co,Cu,Zn,Mg,Mn,Ni).并由IR,UV-vis光谱法和元素分析得到确证.     

具有四帽假Keggin结构"簇阴离子对"的多金属氧簇[Co(2,2-bipy)3]4[MoⅤ5MoⅥ5VⅣ6O40(PO4)]2·4H2O的水热合成与晶体结构

金属氧簇合物在催化、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[1～4]. 在众多的金属氧簇合物中, 只有几种双帽及四帽Keggin结构被合成出来[5 ～12], 而含有四帽假Keggin结构的钼钒氧簇合物尚未见报道.     

一种二帽pseudo-Keggin结构簇合物[HN(C2H5)3]3[N(C2H5)3]2[MoⅣ8MoⅤ4VⅣ2O38(PO4)]的水热合成、结构和性质研究

The novel polyoxometalate, [HN(C₂H₅)₃]₃[N(C₂H₅)₃]₂[Mo^Ⅳ₈Mo^Ⅴ₄V^Ⅳ₂O₃₈(PO₄)], was synthesized and characterized by elementary analysis, EPR, IR spectra and X-ray diffraction. The compound crystallizes in triclinic system, space group P1 with a= 1.41999(2)nm, b=1.43467(2)nm, c=1.694610(10)nm, α=95.7250(10)°, β=92.2110(10)°, γ=92.6060(10)°, V=3.42829(7)nm³, Z=2, D_c=2.388g·cm^-3, M_r=2465.10g·mol^-1, μ=2.489mm^-1, F(000)=2388, R₁=0.0584, wR₂=0.1461, S=1.164. The het-eropolyanion is a bi-capped pseudo-Keggin complex. CCDC： 186645.     

[Cu(enMe)_2]_4[H_5V_(18)~(IV)O_(42)(Cl)]·8H_2O:由金属-氧簇和金属配合物构筑的微孔材料的合成和结构

合成了标题化合物[Cu(enMe)2]4[H5VIV18O42(Cl)]8H2O 1,晶体属于四方晶系,P4/nnc空间群,晶胞参数a = 15.0034(3), c = 18.8149(3) ? V = 4235.27(14) ?, Z = 2, Dc = 2.055 g/cm3, Mr = 2620.74, m = 2.988 mm-1, F(000) = 2608, R = 0.0766, wR = 0.2118, S = 1.193, (Δr)max = 0.969×103 , (Δr)min = 0.454×103 e/3。化合物1的阴离子[VIV18O42(Cl)]8-通过金属配合物阳离子[Cu(enMe)2]2+连接形成3-D骨架结构。     

两种基于B5On(n=11, 12)簇构筑的具有深紫外吸收的硼酸盐

以碱金属和碱土金属为模板, 在溶剂热条件下合成了两种具有深紫外吸收特性的硼酸盐Na₂Ba· [B₅O₈(OH)]₂·2H₂O(1)和KSr[B₅O₈(OH)₂](2), 并利用单晶X射线衍射(SCXRD)、 粉末X射线衍射(PXRD)、 傅里叶变换红外(FTIR)光谱、 紫外-可见吸收光谱(UV-Vis)和热重分析(TG)等手段对化合物的结构和性能进行了研究. 结果表明, 化合物1可归属于单斜晶系P2/c空间群, 结构中四连接的B₅O₁₀(OH)簇单元通过共氧连接形成含有两种9-元环窗口的二维层; 化合物2结晶于单斜晶系C2/c空间群, 结构中四连接的B₅O₁₀(OH)₂簇单元则通过共氧交替连接构筑了罕见的含有8-/12-元环孔道的二维褶皱层. 两种基于B₅O_n(n=11, 12)簇单元构筑的化合物均具有低于200 nm的深紫外吸收边, 在紫外/深紫外区具有潜在的应用价值.