具有五配位Zn中心的微孔金属有机双桥连配体化合物的溶热合成及表征

A new two dimensional zinc complex was reported. This compound was synthesized under solvothermal condition by using THF as solvent. The crystal structure was determined by using single crystal X-ray diffraction. Crystal data: Zr', (B DC)( D ABCO)( H 20)z, monoclinic, space group C 2/c,a =10.871(17),b=19.10 (3),c=7.15 5(川,a= 90,口二115.99(3),Y=90,Z 二8,V 二1335(4),Dr二2.085岁cm3,R二0.08 58. This compound has two-dimensional network structure. Each zinc metal center was coordinated by two DABCO, two BDC and one water molecule. DABCO and BDC ligands bridge to two zinc atoms, respectively. The extension of this〔。-ordination result in a two-dimensional network and form a 7.16 x 9.98A zporous structure. It was interesting to find that the 2-dimensional was an interpenetrated structure formed by two coordinate polymer networks. This kind of structure is very rare in the coordinate compounds. The m-m interaction between the phenyl group of BDC was believed to the key of the growth of this coordination network.     

FeY沸石的二次合成和表征

采用预处理法二次合成ＦｅＹ沸石，并用ＸＲＤ，ＩＲ，ＥＳＲ，ＭＢＳ等手段进行样品进行表征，结果表明，经（ＮＨ４）２ＳｉＦ６预处理的样品，有更多的Ｆｅ进入沸石骨架脱铝位，进入沸石骨架位的Ｆｅ以四面体或畸变四面体配位形式存在，且不易还原成低价Ｆｅ由于Ｆｅ进入沸石骨架，样品的晶胞参数增大，骨架红外反对称和对称伸缩振动率向低波数位移，而未经（ＮＨ４）２ＳｉＦ６预处理的样品，Ｆｅ只能有限地取代骨架位的铝，且骨     

一维链状硫酸铟的溶剂热合成与表征

在溶剂热条件下, 以三乙烯四胺(TETA)作为模板剂, 合成出具有一维链状结构的硫酸铟化合物(C6H22N4)0.5[In(OH)](SO4)2(1). 采用红外光谱、热重分析、ICP、元素分析、粉末X射线衍射及单晶X射线衍射等手段对其进行了表征. 结果表明, 化合物1属于单斜晶系, P2(1)/c空间群, a=1.05240(3) nm, b=1.36802(4) nm, c=0.75295(2) nm, β=101.558(2)°, V=1.06204(5) nm3, Z=4, R1=0.0368, wR2=0.0897, GOF=1.068. 其结构是由InO4(OH)2八面体和SO4四面体通过共顶点连接形成的一维阴离子Tancoite-type 链. 质子化的TETA阳离子通过与阴离子链中的O原子之间的氢键作用将一维链连接成为三维超分子结构.     

碳化硅单晶材料的溶剂热合成与表征

SiC single crystals have been prepared by the method of solvothermal synthesis with a system of SiCl4, CCl4 and metal K in an auto clave. X-ray diffraction (XRD), Raman spectra and transmission electron microscopy(TEM) were used to characterize the products. XRD reveals that the products are SiC crystals and TEM exhibits that SiC single crystal sofwires and platelets are obtained under different usages of metal K. The SiC wires have diameters of 10～20 nm and length up to 1.5μm; the platelets have lateral dimensions of 0.1～3 μm, exhibiting regular polygonal shapes and step-bunched side surface. Furthermore, the growth mechanism of the SiC single crystals is discussed and the effect of super saturation on the crystal growth and morphology is also investigated.     

用水热法和溶剂热法合成LiSrAlF6

用水热和溶剂热法（甲苯作溶剂）合成了LiSrAlF6单相多晶。研究了反应物摩尔比、反应温度和反应时间等对产物的影响。采用环境扫描电子显微镜观察到LiSrAlF6晶体的形貌特征为六角晶形,并聚集成花朵形。试探了LiCaAlF6多晶粉末的水热和溶剂热合成,但未能获得纯相产物。     

F-T合成沉淀铁催化剂中助剂Si作用的穆斯堡尔谱研究

采用穆斯堡尔谱方法研究了用于F-T合成的Fe-Cu-K-Si沉淀铁催化剂中助剂Si的作用。研究结果表明,Si明显起着分散和稳定铁晶粒的作用,此外,铁与高分散Si之间存在着相互作用,从而导致催化剂在灼烧,氢还原及合成气反应后铁的化学形态的变化。     

含过渡金属镉或汞的四元硫化物的溶剂热合成及性能

利用溶剂热法合成了2种四元硫化物Rb₂CdSbS₃（SH）（1）和Rb₂HgSb₄S₈（2）。单晶X射线衍射分析表明,化合物1为一维链状结构,由[CdSbS₃（SH）]^2-阴离子和Rb⁺阳离子组成。化合物2为二维层状结构,由[HgSb₄S₈]^2-阴离子和Rb⁺阳离子组成。固体紫外可见漫反射光谱分析结果表明,化合物1和2的带隙分别为2.06和2.15 eV。荧光分析结果表明化合物1和2均具有黄光发射特性。     

微孔[Me4N]2HgGe4S10的溶剂热合成与表征

用溶剂热方法合成了[Me₄N]₂HgGe₄S₁₀, 通过单晶X射线衍射, IR, DSC-TG手段对其进行了表征. 结果表明, 标题化合物属四方晶系, I-4空间群, 晶胞参数a＝0.92687(8) nm, c＝1.43739(12) nm, V＝1.23484(18) nm³, Z＝2, Mo Kα λ＝0.071073 nm, R₁＝0.0570, wR₂＝0.1374, 空旷骨架结构由超四面体Ge₄S₁₀与HgS₄四面体共用顶点连接而成, 有机模板离子在一维孔道中. 该化合物具有一定的热稳定性, 在320 ℃发生分解形成GeS₂.     

微孔[Me4N]2HgGe4S10的溶剂热合成与表征

用溶剂热方法合成了[Me₄N]₂HgGe₄S₁₀, 通过单晶X射线衍射, IR, DSC-TG手段对其进行了表征. 结果表明, 标题化合物属四方晶系, I-4空间群, 晶胞参数a＝0.92687(8) nm, c＝1.43739(12) nm, V＝1.23484(18) nm³, Z＝2, Mo Kα λ＝0.071073 nm, R₁＝0.0570, wR₂＝0.1374, 空旷骨架结构由超四面体Ge₄S₁₀与HgS₄四面体共用顶点连接而成, 有机模板离子在一维孔道中. 该化合物具有一定的热稳定性, 在320 ℃发生分解形成GeS₂.     

溶剂热法直接合成酞菁铜晶体

以喹啉为溶剂, 在反应釜中将1,3-二异吲哚、钼酸铵和二水乙酸铜在喹啉中反应, 降至室温后得到长10.5 mm针状的酞菁铜单晶, 最佳的反应条件: 以10 mL喹啉为溶剂, 于270 ℃反应8 h, 产率为51.3%.     

层状MAgTeS3 (M＝K, Rb)的溶剂热合成与表征

以硫醇为螯合剂, 在溶剂热条件下合成了两种层状硫代亚碲酸盐KAgTeS₃ (1)和RbAgTeS₃ (2). X射线单晶解析表明, 1和2是类质同晶化合物. 在晶体结构中, 银硫四面体通过共用顶点形成无限的平行链, 在相邻链中银硫四面体取向相反, 这些链与链由三角锥配位的碲互相连接形成阴离子层状结构, 阳离子在阴离子层间. 1的结晶学数据为: M_r＝370.75, P2₁/c, a＝0.73639(6) nm, b＝1.06468(8) nm, c＝0.85203(6) nm, β＝106.4640(10)°, V＝0.64062(8) nm³, Z＝4, R(F)＝4.44%, wR(F²)＝11.66%. 2的结晶学数据: M_r＝417.12, P2₁/c, a＝0.75531(12) nm, b＝1.07076(7) nm, c＝0.8583(2) nm, β＝106.497(6)°, V＝0.66558(19) nm³, Z＝4, R(F)＝6.00%, wR(F²)＝15.43%. DSC及紫外-可见漫反射光谱研究表明, 这两种化合物为半导体, 并具有很好的热稳定性.     

Hydrothermal Synthesis and Properties of Open-Framework Mixed-valence Iron Phosphates IIIII21.543FeFe(PO) with Three-dimensional Structure

Introduction The metal phosphates have attracted much attention because of their potential applications in catalysis, sorp-tion, and magnetic properties.1-5 A large number of metal phosphates6-10 with 1-D chain, 2-D layer and 3-D open-framework have been synthesized under mild hydrothermal conditions in the presence of organic amines. Chiral open-framework phosphates have been synthesized in the presence of chiral metal complexes and chiral structure-directing agents.11-15 In the past years,…     

Synthesis and Characterization of a New Metal-organic Framework with Nou Topology

A new compound, [H2N(CH3)2]2[Zn(btec)].H2O(1, H4 btec = 1,2,4,5-benzenetetracarboxylic acid) has been solvothermally synthesized and structurally characterized by singlecrystal X-ray diffraction. The crystal structure is of monoclinic, space group P21/c with a = 9.5741(3), b = 14.5044(4), c = 13.7329(5) , β = 100.582(4)°, V = 1874.61(10) 3, C14H20N2O9 Zn, Mr = 425.7, Z = 4, Dc = 1.387 g/cm3, μ = 1.349 mm-1, F(000) = 776, R = 0.0560 and w R = 0.1684 for 2834 observed reflections(I 2σ(I)). Compound 1 based on μ4-btec and tetrahedral building unit features a three-dimensional(3D) anionic framework with mixed connected nou topology. The luminescent property and thermogravimetric analysis of compound 1 are investigated.     

有机杂化硫代碲酸盐化合物（H2en）TeS3和[Ni（en）3]TeS3的溶剂热合成与表征

用低温溶剂热法合成了2种分立结构的有机杂化硫代碲（Ⅳ）酸盐化合物（H₂en）TeS₃（1）和[Ni（en）₃]TeS₃（2）（en=乙二胺）,通过X-射线单晶衍射,红外光谱,元素分析等手段对它们的结构进行了表征。晶体结构解析结果表明：2个化合物均属单斜晶系,空间群分别为P2₁和P2₁/c。化合物1和2具有孤立三角锥[TeS₃]^2-阴离子,化合物1的平衡阳离子为双质子化乙二胺[H₂en]²⁺,阴离子基团[TeS₃]^2-和阳离子基团[H₂en]²⁺之间通过N-H…S氢键连接。化合物2的阳离子基团为过渡金属Ni与乙二胺的配合物[Ni（en）₃]²⁺。另外,对该2种晶体进行了紫外-可见漫反射光谱测试和热重分析。     

有机杂化硫代碲酸盐化合物(H_2en)TeS_3和[Ni(en)_3]TeS_3的溶剂热合成与表征

用低温溶剂热法合成了2种分立结构的有机杂化硫代碲(Ⅳ)酸盐化合物(H2en)TeS3(1)和[Ni(en)3]TeS3(2)(en=乙二胺),通过X-射线单晶衍射,红外光谱,元素分析等手段对它们的结构进行了表征。晶体结构解析结果表明:2个化合物均属单斜晶系,空间群分别为P21和P21/c。化合物1和2具有孤立三角锥[TeS3]2-阴离子,化合物1的平衡阳离子为双质子化乙二胺[H2en]2+,阴离子基团[TeS3]2-和阳离子基团[H2en]2+之间通过N-H…S氢键连接。化合物2的阳离子基团为过渡金属Ni与乙二胺的配合物[Ni(en)3]2+。另外,对该2种晶体进行了紫外-可见漫反射光谱测试和热重分析。     

Hydrothermal Synthesis and Properties of Open-Framework Mixed-valence Iron Phosphates Fe2^111Fe1.5^11（PO4）3 with Three-dimensional Structure

The open‐framework iron phosphate Fe₂^lllFe_1.5^ll,(PO₄)₃ was hydrothermally synthesized and characterized by elemental analysis, IR, EPR, XPS and single crystal X‐ray diffraction analysis. The title compound crystallized in the triclinic, space group P1 with a=0.64724(4) nm, b=0.79651(6) nm, c=0.94229(5) nm, a= 104.447(2)°. β= 108.919(4)°. y= 101.741(4)°, V=0.42302(5) nm³, Z= 1 and R_I (wR₂)=0.0307 (0.0793). Crystal data were collected on a Rigaku R‐AXIS RAPID IP diffractometer with Mo Ka (γ=0.071073 nm) at 293(2) K in the range of 2.43°<Õ <27.46°. The structure of 1 consists of 19 non‐hydrogen atoms including three and a half crystallographically independent Fe and three P atoms. Fe(1) connects its symmetrical Fe(1A) through bridging oxygen forming a dimer and the dimers are connected by Fe(4) forming an infinite staircase‐like chain. Fe(2) and Fe(3) connect the infinite chains into a layer with bridging oxygen. Layers are interconnected via Fe(4) forming the six‐membered and eight‐membered channel systems.     

[C4N2H12]1.5[Zn2(PO4)(HPO4)2]·H2O晶体的合成与表征

由于在电学、磁学、光学、吸附、离子交换和催化等领域具有潜在的应用价值,具有开放骨架结构的金属磷酸盐的合成一直受到人们的广泛关注。在这些磷酸盐微孔化合物中,磷酸锌晶体是拓扑结构最为丰富的一种犤1犦。自从Stucky等犤2犦报道具有SOD、Li-ABW、FAU等已知结构磷酸锌的合成以来,已经有近百种具有0-D犤3,4犦,1-D犤5,6犦,2-D犤7～9犦,3-D犤10～13犦结构的磷酸锌被成功地合成出来。其中令人瞩目的是具有螺旋孔道的手性磷酸锌犤14犦以及具有二十四元环孔道的两种微孔磷酸锌化合物犤15,16犦的合成。这些化合物大多是采用水热技术以有…     

以有机溶剂热生长技术制备金属硫族化合物[Mn(en)_3]PdSe_2及其晶体结构分析

以有机溶剂热生长技术 (solvothermaltechnique) ,即在 180℃乙二胺 (en)溶液中 ,以MnCl3,PdCl2 ,K2 Se在密闭容器中反应 7d ,制备出新的硫族化合物 [Mn(en) 3]PdSe2 ,其阴离子基团为 [PdSe2 ]2 -,阳离子基团为过渡金属Mn与乙二胺 (en)的配合物 :[Mn(en) 3]2 +.以单晶X射线衍射技术解得该晶体结构属正交晶系 ,空间群为Pbcn ,[Mn(en) 3]·PdSe2 (Ⅰ )的晶胞数据 :a =1.1484( 2 ) ,b=1.5 0 5 7( 3 ) ,c =0 .93 62 2 ( 19)nm ,Z =4.