Ni(Ⅱ)-3,5-二氯水杨醛缩氨基甲磺酸席夫碱-邻菲咯林三元配合物的合成及晶体结构

采用Ni(Ⅱ)盐和氨基甲磺酸缩3,5-二氯水杨醛席夫碱(H2L)以及1,10-邻菲咯林(phen)在甲醇和水溶液中合成了三元配合物[Ni(Ⅱ)(C8H7O4NCl2S)(Phen)(H2O)]3(1),通过元素分析、红外光谱对配合物 1 进行了表征,并通过X射线衍射测定了其结构.结构解析表明,配合物 1 属三斜晶系,空间群P ī,晶胞参数为:a=1.5640(3)nm,b=1.5650(3)nm,c=1.5650(3)nm;α=94.84(3)°,β=94.73(3)°,γ=94.80(3)°,V=3.7881(13)nm3,Z=6,Dc=1.420 g· cm-3,F(000)=1602,μ=1.100 mm-1,最终偏差因子(对I>2σ(I)的衍射点),R1=0.0769,ωR2=0.1306,对全部衍射点R1=0.1323,ωR2=0.1468,ω-1=[σ2(Fo)2+(0.1977P)2],P=(Fo2+2Fc2)/3.配合物 1 通过卤卤作用(Cl-Cl 0.3574(8)nm)堆积成3D无限层状结构.     

双核Cu(Ⅱ)-5-溴水杨醛缩氨基甲磺酸席夫碱4,4′-联吡啶三元配合物的合成及晶体结构

采用Cu(Ⅱ)盐和氨基甲磺酸缩-5-溴水杨醛席夫碱(H2L)以及4,4′-联吡啶(bpy)在乙醇和水溶液中合成了三元配合物,通过元素分析、红外光谱对配合物进行了表征,并用X射线衍射测定了其结构。结构解析表明,该标题配合物属单斜晶系,空间群P21/c,晶胞参数为:a=0.9509(2)nm,b=1.8783(2)nm,c=1.0514(2)nm;β=98.48(1)°,V=1.8575(3)nm3,Z=2,Dc=1.812 g.cm-3,F(000)=1016,μ=3.473,最终偏差因子(对I>2σ(I)的衍射点)R1=0.0459,wR2=0.0739,对全部衍射点R1=0.1205,wR2=0.0887,ω-1=[σ2(Fo)2+0.0345P],P=(Fo2+2Fc2)/3。邻近配合物分子间存在着大量的氢键,席夫碱三元配合物通过氢键作用堆积成2D网状结构。     

双核Cu(II)-5-溴水杨醛缩氨基甲磺酸席夫碱4,4'-联吡啶三元配合物的合成及晶体结构

采用Cu(II)盐和氨基甲磺酸缩-5-溴水杨醛席夫碱(H2L)以及4,4'-联吡啶(bpy)在乙醇和水溶液中合成了三元配合物,通过元素分析、红外光谱对配合物进行了表征,并用X射线衍射测定了其结构.结构解析表明,该标题配合物属单斜晶系,空间群P21/c,晶胞参数为: a=0.9509(2) nm,b=1.8783(2) nm,c=1.0514(2) nm;β= 98.48 (1)°,V=1.8575(3) nm3, Z=2,Dc=1.812 g·cm-3, F(000)=1016, μ=3.473,最终偏差因子(对I＞2σ(I)的衍射点)R1=0.0459, wR2=0.0739,对全部衍射点R1=0.1205, wR2=0.0887, ω-1= [σ2(Fo)2+0.0345P],P=(Fo2+2Fc2)/3.邻近配合物分子间存在着大量的氢键, 席夫碱三元配合物通过氢键作用堆积成2D网状结构.     

一种新型Pb(Ⅱ)配位聚合物的合成、表征及性质研究

本文以吡啶-4-甲醛缩4-氨基安替比林和Pb(NO3)2为原料,溶剂热法成功合成出了一个新型Pb(Ⅱ)的配合物[Pb(L4)2(NO3)2](L4=吡啶-4-甲醛缩4-氨基安替比林),并通过红外光谱、元素分析、X-粉末衍射、单晶X射线衍射对配合物的单晶结构进行了表征.该配合物属于单斜晶系,空间群Cc,晶胞参数a=2.3842(3) nm,b=0.97378(11) nm,c=1.9611(2) nm,α=90°,β=128.836(9)°,y =90°,V=3.5466(7) nm3,Z=4,Dc=1.715 Mg/m3,F(000) =1808,μ=4.823 mm-1,R1=0.0476,ωR2=0.1158 [I＞2σ(I)].室温固态荧光测试显示,配合物在470nm(λmax)具有强的荧光吸收.     

Ni（II）-3，5-二氯水杨醛缩氨基甲磺酸席夫碱-邻菲咯林三元配合物的合成及晶体结构

采用Ni（II）盐和氨基甲磺酸缩3,5-二氯水杨醛席夫碱（H2L）以及1,10-邻菲咯林（phen）在甲醇和水溶液中合成了三元配合物[Ni（II）（C8H7O4NCl2S）（Phen）（H2O）],（1）,通过元素分析、红外光谱对配合物1进行了表征,并通过X射线衍射测定了其结构。结构解析表明,配合物1属三斜晶系,空间群Pi,晶胞参数为：a=1．5640（3）nm,b=1．5650（3）nm,c=1．5650（3）nm;α=94．84（3）°,β=94．73（3）°,γ=94．80（3）°,V=3．7881（13）nm^3,Z=6,Dc=1．420g·cm^3,F（000）=1602,μ=1．100mm^-4,最终偏差因子（对Ⅰ〉2σ（Ⅰ）的衍射点）,R1=0．0769,ωR2=0．1306,对全部衍射点R1=0．1323,ωR2=0．1468,ω^-1=[σ^2（F0）^2＋（0．1977P）^2],P=（F0^2＋2Fc^2）／3。配合物1通过卤卤作用（Cl-Cl0．3574（8）nm）堆积成3D无限层状结构。     

一种新型双核Cu(Ⅰ)配合物的合成、表征及性质研究

以吡啶-4-甲醛缩4-氨基安替比林和CuCl为原料,采用水热法成功合成出了一个新型双核铜(Ⅰ)的配合物[Cu(L)Cl](L=吡啶-4-甲醛缩4-氨基安替比林),并通过单晶X射线衍射、红外光谱、拉曼光谱、元素分析、热重分析和荧光分析等手段,对该配合物进行表征及性质研究.结果表明:该配合物晶体属于单斜晶系,空间群为P21/c,晶胞参数a =1.3616(4) nm,b =0.68631(19) nm,c =1.9132(5) nm,α=90°,β=106.260(4)°,γ=90°,V=1.7163(8) nm3,Z=4,Dc=1.514 Mg/m3,F(000)=800,μ=1.439 mm-1,R1 =0.0939,ωR2 =0.2363[I＞2σ(I)].     

一种环状双核钠配合物[Na(H2O)(μ2-Ans)(Phen)]2的合成、晶体结构及其表征

在热乙醇水溶液中,5-氨基萘磺酸(HAns)、邻菲啰啉(phen)和NaOH经回流反应合成了一种新的钠配合物[Na(H2O) (μ2-Ans)(Phen)]2(1),通过元素分析、红外光谱、紫外光谱和热重分析等进行了表征并采用X射线单晶衍射测定了配合物的分子结构.该配合物属单斜晶系,空间群P21/n,a=0.70346(13) nm,b=1.0959(2) nm,c=2.5854(5) nm,β=94.934(4)°,V=1.9858(6)nm3,R=0.0493,ωR=0.1755.结构分析表明,配合物由于磺基μ2模式的桥联配位作用而呈现分立的环状双核结构,并通过芳环堆积作用和分子间氢键扩展为三维超分子体系.此外测试了该配合物的荧光性质.     

配合物[Cu(pht)2(fa)2](H2O)2的合成、晶体结构及性质研究

用醋酸铜、苯妥英(即5,5-二苯基-2,2咪唑烷酮,简称Hpht)与糠胺(2-furfurylamine,简称fa)反应,得到一种新的配合物[Cu(pht)2 (fa)2] (H2O)2,通过红外光谱、元素分析以及Ⅹ-射线单晶衍射的方法,对配合物的结构进行了表征.该晶体属三斜晶系,Pt空间群,晶胞参数:a =0.9878(2) nm,b=1.0068(2) nm,c=1.0640(3) nm,α=78.664(3)°,β=75.490(2)°,γ=72.050(3)°,Z=1,Dc=1.368 mg·m-3,R1=0.0986,ωR2 =0.2191.每个标题配合物分子中Cu(Ⅱ)离子与2个Hphi配体、2个fa配体的4个氮原子形成四方形构型,同时利用琼脂扩散法测试了配合物、苯妥英和铜盐对大肠杆菌(Escherichia Coli),金黄色葡萄球菌(Staphylococcus Aureus),枯草芽孢杆菌(Bacillus Subtilis)的抑菌活性,结果表明,它们对3种致病细菌均有一定的抑制作用.     

一种新型双核Zn(Ⅱ)配合物的合成、表征及性质研究

选用溶剂热法,以邻羟基苯甲醛缩4-氨基安替比林和Zn(NO3)2·6H2O为原料,成功合成出了一种新型双核Zn(Ⅱ)配合物[Zn2(L-)2(NO3)2](HL为邻羟基苯甲醛缩4-氨基安替比林),并采用单晶X射线衍射、红外光谱、X-粉末衍射、元素分析、热重分析等对该配合物单晶结构进行表征.结果表明:该配合物晶体属于三斜晶系,空间群为P1,晶胞参数a=0.80724(11)nm,b=0.94547(13) nm,c=1.28831(18) nm,α =99.281 (2)°,β=103.814(2)°,y=107.373 (2)°,V=0.8821 (2) nm3,Z =2,Dc=1.633 Mg/m3,F(000) =444,μ=1.432 mm-1,R1=0.0449,wR2=0.1083[I＞2σ-(I)].室温下固态荧光测试显示,配合物具有强的荧光吸收在490 nm(λmax).     

4,4＇-联吡啶钴（Ⅱ）、铜（Ⅱ）配合物的合成及其晶体结构

本文用溶液法合成了未见报道的4,4'-联吡啶铜、钴二元配合物,并获得到了单晶.利用元素分析、X射线单晶仪对其结构进行了表征.结果表明两个晶体均属单斜晶系,空间群C2/c.铜配合物的晶体结构参数为a=1.8272(3)am,b=1.1149(2)am,c=2.4667(4)am,α=90°,β=91.518(2)°,γ=90°,V=5.0231(14)nm3,Z=4,F(000)=2236,Mr=1070.69,Dc=1.416g.cm3,μ=0.449 mm-1,R1=0.0951,ωR2=0.2301.钴配合物的结构参数为a=1.8016(6)am,b=1.1478(4)nm,c=2.4517(9)mm,α=90°,β=93.647(5)°,γ=90°,V=5.059(3)nm3,Z=4,F(000)=1940,Mr=927.91,Dc=1.218 g.cm3,μ=0.393 mm-1,R1=0.0852,ωR2=0.2118.     

Synthesis, structure and characterization of a new inorganic-organic hybrid complex (C3H5N2)2[Cd(C3H4N2)2Nb2O3F8]·2H2O

(C₃H₅N₂)₂[Cd(C₃H₄N₂)₂Nb₂O₃F₈]·2H₂O (C₃H₄N₂=imidazole) (1) was prepared from the hydrothermal reaction of Nb₂O₅, 3CdSO₄·8H₂O, C₃H₄N₂, HF and H₂O at 403 K, and characterized by single crystal X-ray diffraction and IR spectra. 1 crystallizes in the orthorhombic system, space group Pba2, with a=11.0192(9), b=16.8012(14), c=6.8717(6) ?, and Z=2. The crystal is made up of [Cd(C₃H₄N₂)₂Nb₂O₃F₈]²⁻ anions, [C₃H₅N₂]⁺ complex cations and H₂O molecules of crystallization. And the backbone of the compound is a one dimension coordination polymeric chain containing the anions. The complex cations and anions are linked through hydrogen bonding interactions. Co-crystallized water molecules fill in the pores and hydrogen bond to the host. Bond valence sums show that O1, O3 and F3 have much more negative charge, which are in agreement with the crystal structure that they act as bridging atoms.Supplementary material CCDC-606794 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge at http://www.ccdc.cam.ac.uk/ const/retrieving.html or from the Cambridge Data Centre (CCDC), 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033 or e-mail: deposit@ccdc.cam.ac.uk.     

Structure of a potent neuromuscular blocking agent: Caracurine-II dimethochloride octahydrate, [C40H44N4O2]2+·2CI−·8H2O

Crystals of this calabash curare alkaloid, space groupP2₁; havea=12.695(4), Å,b=7.424(2) Å,c=21.762(6) Å,=98.03(5)°,Z=2,F(000)=884. The structure was solved by direct methods and refined by least squares toR=0.10. The alkaloid cation, with two-fold molecular symmetry, has a highly fused ring system and is structurally rigid. This determination provides accurate stereochemical parameters for those atoms and groups (N⁺ centers, aromatic rings, and hydrogen bond acceptors) postulated by various theories as involved in binding to the acetylcholine receptor. In the crystal, layers of alkaloid cations parallel to thebc plane alternate with layers containing two Cl^– ions and eight water molecules distributed almost randomly over ten sites. Electrostatic attractions between N⁺ and Cl^– bind the alternating layers together. Each one of the ten sites is, on average, 4.60 Å from one or two N⁺, allowing the two Cl_– ions to be disordered. Binding interactions within the alkaloid layers are solely van der Waals attractions. Within each H²O/C1^– layer there is a complex hydrogen bond system, including four infinite spirals parallel to theb axis, with an average bonding distance of 2.94 Å. There are no hydrogen bonds between layers. The possible relevance to the activity of the alkaloid of its ability to organize large amounts of water is discussed.     

Synthesis and crystal structure of [Nd(H2O)2]2(C2O4)3

Some crystals of [Nd(H₂O)₂]₂(C₂O₄)₃ were synthesized hydrothermally by heating at 200°C for 8 days an aqueous suspension of neodymium oxalate decahydrate in presence of terephthallic acid and guanidinium carbonate. They crystallize in the orthorhombic system, space group P2₁2₁2₁, with a = 8.6702(7) Å, b = 9.558(2) Å, and c = 17.009(2) Å. The structure of this complex is built up by two independent neodymium atoms, three bischelating oxalate ligands, and four water molecules forming a rectangle building unit of 6-membered ring, [Ln(H₂O)₂(C₂O₄)]₆. The packing of these units leads to a layer parallel to the plane (001). However, the neodymium atoms of two neighbor layers share an edge of oxalato oxygen atoms thus giving a double-layer. The three dimensionality between these double-layers is insured by hydrogen bonds of water molecules which are bound to the neodymium atoms. There is no zeolitic water molecule. The two neodymium atoms are nine-coordinated. In both cases, the coordination polyhedron can be described as a distorted tricapped trigonal prism.     

Crystal and molecular structure of Dibromobis ([1,2,4]triazolo[1,5-a]pyrimidine-N3)zinc hemihydrate,C10H8N8Br2Zn·1/2 H2O

The structure of the title compound (C₁₀H₈N₈Br₂Zn·1/2H₂O), prepared from the ligand and zinc bromide in ethanol, was solved by X-rays analysis.M _r =465.18, monoclinic, space groupP2₁/n,a=21.2376(11),b=7.1339(6),c=20.0469(11) Å,=98.583(4)°,V _c =3003.2 ų,Z=8,D _x =2.057 Mg m^–3,(Cu K)=87 cm^–1,F(000)=1832,T=300 K. Final conventionalR-factor=0.034 andR _w =0.036 for 4255 unique reflections withI> 3(I) out of 5685 measurements. The structure was solved using automatic programsPatsys andDirdif. The two independent molecules are almost identical. The Zn atom is tetrahedrally coordinated by two Br atoms and two N(3) atoms of the triazolopyrimidine ligands. The planar triazolopyrimidine ligands make angles of 94.0 and 57.5° (moleculeA) with the ZnBr₂ plane (98.6 and 57.0° for moleculeB). The water molecule is involved in hydrogen bonds with bromine only.On leave from Chemistry Department, University of Benin, Benin-City, Nigeria.     

配位聚合物[Mn(bpda)(benzidine)]_n的晶体性能研究

根据文献合成了联苯二甲酸,并通过水热法制备了[Mn(bpda)(benzidine)]n暗棕色的针状晶体.通过X-射线衍射分析、元素分析、IR等方法对配合物进行了表征,并通过TG分析对该配合物的热稳定性及热分解机理做了初步探讨.结果表明,正是基于bpda分子四齿μ3-配位形式,使得该配体的热稳定性要明显高于另一配体联苯胺.