Energetic materials composed of coordination polymers: {[Zn(μ-atrz)3](ClO4)2·2H2O}n and {[Cu(μ-atrz)3](NO3)2·2H2O}n

An improved synthetic pathway for trans-4,4′-azo-1,2,4-triazole (atrz) was discovered. Pure atrz was obtained directly without any other separation step in an environment friendly process. Treatment of atrz with zinc perchlorate and cupric nitrate led to the isolation of {[Zn(μ-atrz)₃](ClO₄)₂·2H₂O}_n and {[Cu(μ-atrz)₃](NO₃)₂·2H₂O}_n, which were well characterized. Their structures were determined by X-ray crystallographic analysis. The calculation results of the formation of {[Zn(μ-atrz)₃](ClO₄)₂ 2H₂O}_n and {[Cu(μ-atrz)₃](NO₃)₂ 2H₂O}_n indicates that the perfect crystal structures in spite of much resistance. A fundamental understanding of the structure and thermal properties involves factors, such as conjugated system, crystal structure, and inorganic metallic compounds that affect their thermal behavior. The high energy of the coordination compounds consists of chemical, electronic, and potential energy. The potential for the improvement of the coordination polymer opens up a new world for research of energetic materials.     

新型一维配位聚合物{[Cu(H2L)(HL)](ClO4)·3H2O}n的合成及其晶体结构

Cu(ClO4)2·6H2O与H2L{L=[2,3-f]-吡嗪[1,10]邻菲咯啉-2,3-二甲酸}反应合成了新型一维配位聚合物{ [Cu(H2L) (HL)] (C1O4)· 3H2O}n(1),其结构经UV,IR,XRD和元素分析表征. 1属单斜晶系,空间群C2/c,晶胞参数a=3.575 9(13) nm,b=0.962 7(3)nm,c=2.127 5(10)nm,β=116.106(8)°,V=6.577(5) nm3,Z=8,Dc=1.730 g·cm-3,Mr=856.56,F(000)=3 480,μ=0.837nm-1,R=0.082 6,wR=0.248.Cu2+分别与1个H2L的两个氮原子,2个不同μ2-HL的两个氮原子和一个羧酸氧原子配位,形成畸变四方锥的五配位构型.Cu(Ⅱ)通过HL桥联形成一维链,相邻一维链的芳环π-π堆积和分子间氢键作用使1构筑成三维超分子结构.     

{[Ag(ATO)2]ClO4}n的合成、结构表征和热分解机理

A new supermolecule coordination compound of perchlorate di(4- amino- 1,2,4- tri azole- 5- one)silver(I) was synthesized. It was characterized by element analysis, FT- IR, X- ray crystallogram and single crystal diffraction. The titled complex was also studied by means of TG- DTG and DSC under conditions of linear temperature increase. The thermal decomposition remainders were determined by infrared spectroscopic analysis. Thermal decomposition mechanism of the title coordination compound was suggested.     

{[Ag(ATO)2]ClO4}n的合成、结构表征和热分解机理

A new supermolecule coordination compound of perchlorate di(4-amino-1,2,4-triazole-5-one) silver(I) was synthesized.It was characterized by element analysis,FT-IR,X-ray crystallogram and single crystal diffraction.The titled complex was also studied by means of TG-DTG and DSC under conditions of linear trmperature increase.The thermal decomposition remainders were determined by infrared spectroscopic analysis.Thermal decomposition mechanism of the title coordination compound was suggested.     

Synthesis and crystal structure of a coordination polymer {[Cu2(L)2(Phen)2] · 8H2O} n

A novel metal coordination polymer, {[Cu₂(L)₂(Phen)₂] · 8H₂O} _n (I), has been synthesized by the reaction of Cu(NO₃)₂ with 2,2′-bipyridyl-4,4′-dicarboxylic acid (L) and 1,10-phenanthroline (Phen) at room temperature. The polymer was characterized by IR, elemental analyses and X-ray diffraction. Single-crystal structural analysis reveals that the center Cu²⁺ ions have two coordinated types. The Cu(1) atom has the five-coordinate mode, and Cu(2) forms an is octahedron of the six-coordinate mode. Two Cu²⁺ ions are connected by the O atom of carboxylate group bridges. Complex I contains eight molecules of water clusters and constructed a 1D tape structure.     

Synthesis and Crystal Structure of a 1-D Coordination Polymer {[Cu(NIT4py)2(ip)]·6H2O}n

A new complex {[Cu(NIT4py)2(ip)]·6H2O}n (NIT4py=2-(4'-pyridinyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide and ip = isophthalate dianion) has been synthesized and structurally characterized by X-ray diffraction. It crystallizes in orthorhombic, space group Cmcm with a = 25.161(3), b =10.045(1), c = 15.450(2)(A), C32H48N6O14Cu, Mr = 804.30, V = 3904.8(8)(A)3, Z = 4, Dc = 1.368 g/cm3,μ(MoKα) = 0.630 mm-1, F(000) = 1692, the final R = 0.0326 and wR = 0.0787 for 1843 independent reflections with Rint = 0.0372. Each Cu(II) ion is four-coordinated by two carboxylate oxygen atoms and two pyridyl-N atoms from NIT4py radicals to furnish a rhombus geometry. The central Cu(II) ion is located at an inversion center and a crystallographic two-fold axis. Each isophthalate dianion binds two Cu(II) ions in bis-monodentate mode, leading to a 1-D chain, and these 1-D chains are further linked into a 2-D network via hydrogen-bonding interactions.     

一维梯状配合物{[Cu2(4,4''-bpy)3(p-Ab)2(H2O)2]·(NO3)2·4H2O}n的晶体结构

合成了一维分子梯状配合物{[Cu2(4,4'-bpy)3(p-Ab)2(H2O)2]·(NO3) 2·4H2O}n(4,4'-bpy=4,4'-联吡啶,p-Ab-=对氨基苯甲酸根离子),该配合物晶体属单斜晶系,P2(1)/c空间群,晶胞参数:a=1.110 7(5) nm,b=1.550 4(3) nm,c=1.450 9(3) nm,β=104.81(3)°,V=2.415 5(12) nm3,Z=2.铜离子周围有3个氧原子和3个氮原子与之配位,其中2个氧原子由对氨基苯甲酸的螯合氧原子提供,另一个氧原子由配位水提供,3个氮原子分别由三个4,4'-联吡啶提供.这六个原子在铜离子周围形成一个畸变的八面体配位环境.配体对氨基苯甲酸只有一种配位形式--双齿螯合,第二配体4,4'-联吡啶的两个氮原子均参与配位,将配合物组装成一维分子梯结构.     

Crystal structure and magnetic properties of a nitronyl nitroxide complex {[Co2(NIT4Py)4(fum)2(H2O)4] · (H2O)2} n

The title compound {[Co₂(NIT4Py)₄(fum)₂(H₂O)₄] · (H₂O)₂} _n , where NIT4Py = 2-(4′-pyridinyl)-4,4,5,5-tetra-methylimidazoline-1-oxyl-3-oxide and fum = fumarate, was prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P 1 with a = 9.8853(9) Å, b = 13.2167(13) Å, c = 13.8481(12) Å, α = 68.5400(10)°, β = 73.467(2)°, γ = 74.596(2)°, V = 1587.6(3) ų, Z = 1, and R ₁ [I > 2σ(I)] = 0.0662. The complex consists of two kinds of neutral infinite 1-D chains, in which [Co(NIT4Py)₂(H₂O)₂] moieties are connected by fumarate anions in a bis-monodentate mode. These 1-D chains are further connected by hydrogen bonds, generating a 2-D network. The variable temperature magnetic susceptibility measurement reveals that the magnetic couplings between Co(II) and NIT4Py are weak antiferromagnetic interactions.     

Hydrothermal synthesis, crystal structure of two new coordination polymer {[Ni2(Imazameth)2(4,4′-Bipy)] · (ClO4) · CH2OH · H2O} n and [Cu2(PDA)1.5(2,2-Bipy)2](H2O)5(NO3)

Two new metal-organic coordination polymers framework formulated as [Cu₂(PDA)_1.5(2,2′-Bipy)₂](H₂O)₅(NO₃) (I) and {[Ni₂(Imazameth)₂(4,4′-Bipy)] · (ClO₄) · CH₂OH · H₂O _n (II), where H₂PDA = 1,4-phenylenediacetic acid, 2,2′-Bipy = 2,2′-bipyridine, Imazameth = (+/?)2-(4,5-dihydro-4-methyl-4-(1-methylethyl)-5-oxo-1H-imidazol-2-yl)-5-methyl-3-pyridinecarboxylic acid, 4,4′-Bipy = 4,4′-bipyridine, have been prepared and characterized by spectral method (IR), elemental analysis and single crystal X-ray diffraction techniques. Complex I consists of one-dimensional ladder-like chains featuring binuclear unit in which the two Cu²⁺ ions have different coordination geometry: one is five-coordinated, the other is six-coordinated. Complex II is a new two-dimensional copper complex with the peculiarity of having the 4,4′-Bipy ligand and Imazameth ligand acting as bridge to form planar network polymer. Both I and II exist abundant hydrogen bonds. It is result in the formation of a supermolecular crystal, in which they seem to be effective in the stabilization of the structure.     

新型一维链状配位聚合物{[Cu2(dhbd)(bipy)2]·10H2O}n的研究

采用水热法合成了标题配位聚合物{[Cu2(dhbd)(bipy)2]·10H2O}n(H4dhbd=2,3-二羟基丁二酸,bipy=2,2'-联吡啶),通过元素分析、红外光谱、热分析、X射线单晶衍射等技术对其进行了表征.配合物属单斜晶系,空间群C2/c,a=2.1965(4)nm,b=1.0671(2)nm,c=1.3662(3)nm,β=93.50(3)°,Z=4,R=0.0388.晶体的基本构建基元包含10个结晶H2O分子和由两个Cu(Ⅱ)原子、一个采用双二齿螯合配位的2,3-二羟基丁二酸根、两个2,2'-联吡啶形成具有C2旋转轴的U形双核单元,相邻的两个方向相反的U形双核单元通过双羧基O桥联形成沿c轴延伸的一维链;链间籍C-H…O和O-H…O氢键扩展为三维结构.配合物中呈现了一种2,3-二羟基丁二酸与过渡金属配位的新方式.     

{[Sr(CHZ)2(H2O)]·(NTO)2·3.5H2O}n的制备和晶体结构

将SrCO3与3-硝基-1, 2, 4-三唑-5-酮(NTO)分散于蒸馏水中,加热搅拌制备出NTO锶溶液,再与碳酰肼(CHZ)水溶液反应合成了新型配合物:{[Sr(CHZ)2(H2O)]?NTO)2?.5H2O}n。 其化学式为 C6H23N16O12.5Sr,Mr=606.97),并对其进行了元素分析和红外表征,利用单晶分析测定了晶体结构。晶体属于单斜晶系,空间群为C2/c,晶体学数据如下:a=24.587(5), b=12.689(2), c=16.481(4) ? =121.15(1)埃琕=4400.4(2) ?,Z=8,Dc=1.833 g/cm3,?= 0.255 cm-1, F(000) = 2472,R=0.0989,wR=0.0750。     

配位聚合物{[Co(4,4''''-bpy)(H2O)4](Fum)·4H2O}n的合成和晶体结构

0引言近年来,利用晶体工程方法设计、裁剪和组装具有一维、二维和三维有序超分子结构的配位聚合物引起了人们极大的兴趣,并成为材料科学和化学学科中最活跃的研究领域之一[1~3]。在超分子结构设计方面,利用过渡金属借助配体配位作用引导的自组装已成为一个热点。其中多联吡啶类     

{[Cu2Br3]n[Cu(H-Leof)2]·2H2O}(Leof是左氟沙星)

C om m ent Levofloxacin (S-(-)9-fluoro-2,3-dihydro-3-m ethyl- 10-(4-m ethyl-1-piperazinyl)-7-oxo-7H -pyrido[1,2,3-de]- 1,4-benzoxaxin-6-carboxilic acid)(Leof),is a synthetic fluorinated quinolone derivative, having activity a- gainstboth Gram ( )and Gram …     

Synthesis and Characterization of a One-dimensional Chain Polymer{[Cu(4-CPOA)(3-PyOH)_2(H_2O)_2]·H_2O}_n

1 INTRODUCTION Molecular self-assembly of coordination architec- tures is a rapidly developing research area of supra- molecular chemistry in recent years[1～6]. 4-Carboxy- phenoxyacetic acid (4-CPOAH2) is a multidentate flexible and rigid ligand, which is capable of coor- dinating to metal centers in versatile binding fashi- ons and can also form regular hydrogen bonds as both hydrogen-bond donors and acceptors. To date, only Na(I), Ni(II), Mn(II) and Co(II) complexes con- taining…     

Synthesis and Crystal Structure of a 1-D Coordination Polymer {[Cu(NIT4py)_2(ip)]·6H_2O}_n

1 INTRODUCTION Pyridyl-substituted nitroxide radicals have at- tracted considerable attention in recent years due to the ability to coordinate with metal ions and act as magnetic couplers, giving rise to new functional ma- terials with particular magnetic and optical prope- rties as well as a variety of structural topologies[1~3]. Considerable efforts have been made in designing and preparing multi-dimensional materials with app- ropriate bridges, such as pseudohalide, dicyanide, dicyanoa…     

配位聚合物{[Co(H2O)6][Co(H2O)4(pmts)]·4H2O}n的合成及晶体结构

以均苯四甲酸(pmts)和CoCl2·6H2O为原料,在碱件水溶液中通过水热法合成了配位聚合物{[Co(H2O)6][Co(H2O)4(pmts)]·4H2O}n,并对其进行了红外、紫外-可见吸收光谱和单品X-射线衍射结构测定.结果表明,Co2+分别与桥配体pmts的1,4位羧基氧及端配体水分子中的氧以轻度畸变的八血体...     

Unique seven-node rare-earth octacyanomolybdate(IV) three-dimensional molecular frameworks: {[Er(H2O)5(Er(H2O)4)3][Mo(CN)8]3·11H2O}n and {[Eu(H2O)5(Eu(H2O)4)3][Mo(CN)8]3·11H2O}n

The crystal structure analyses of {[Er(H₂O)₅(Er(H₂O)₄)₃][Mo(CN)₈]₃·11H₂O}_n (1) and {[Eu(H₂O)₅(Eu(H₂O)₄)₃][Mo(CN)₈]₃·11H₂O}_n (2), show that they are not only new neutral three-dimensional rare-earth octacyanomolybdate(IV) molecular frameworks, but that they also belong to an unknown structure type having seven different nodes. To the best of our knowledge this is different to any other known molybdenum(IV) octacyanide complexes published to date. Both compounds crystallize in the triclinic system, space group P-1, and are isostructural and isotypic. The coordination polyhedra of the molybdenum atoms in the three different [Mo(CN)₈]⁴⁻ anions are trigonal prisms, with two additional atoms. A new bridging mode for octacyanometallates is also observed with five of the eight cyanide groups involved in bridging either three or four rare-earth atoms, while the three remaining cyanide groups are terminal and are involved in hydrogen bonding. The four rare-earth atoms in 1 and 2 have different coordination polyhedra in the form of trigonal prisms with two additional atoms. The three-dimensional structures are made up of infinite two-dimensional slabs linked by one of the rare-earth metal atoms. In both compounds, apart from the 17 coordinated water molecules, there are 11 lattice water molecules of crystallization present in the cavities of the three-dimensional frameworks. The 28 water molecules and the terminal CN⁻ groups are involved in an extensive O–H⋯O and O–H⋯N hydrogen bonding network.     

Synthesis and crystal structure of a three-dimensional 3d-4f heterometallic coordination polymer {[Sm2Ni(Pdc)2(SO4)2(H2O)6] · H2O} n

A new 3d-4f coordination polymer {[Sm₂Ni(Pdc)₂(SO₄)₂(H₂O)₆] · H₂O} _n (H₂Pdc = pyridine-3,5-dicarboxylic acid) has been synthesized under hydrothermal conditions and structurally determined by X-ray diffraction method. The X-ray diffraction analysis reveals the compound crystallizes in the triclinic system, space group $P\bar 1$ , with a = 10.062(4), b = 10.249(4), c = 12.744(5) Å, α = 93.548(4)°, β = 102.601(4)°, γ = 94.022(3)°, V = 1275.4(8) ų, F(000) = 972, M _r = 1077.85, Z = 2, ρ _c = 2.624 g cm^?3, μ = 5.55 mm^?1, final R = 0.0299, wR = 0.0805 for 4716 independent reflections with R _int = 0.0204. According to the structure determination the complex is a three-dimensional (3D) network structure in which infinite lanthanide-carboxylate chains are linked by [Ni(SO₄)₂]^2? metalloligands to form a mixed-metal coordination network.     

Synthesis and Crystal Structure of a Nitronyl Nitroxide Complex {[Zn(NIT4Py)(fum)(H2O)2]·H2}n

The title compound {[Zn(NIT4Py)(fum)(H2O)2]·H2O}n, where N1T4Py=2-(4'-pyridinyl)-4,4,5,5-tetra-methylimidazoline-l-oxyl-3-oxide and rum=fumarate, has been prepared and structurally characterized by X-ray diffraction. It crystallizes in triclinic, space group P1 with a =6.9533(9), b=9.805(1), c=15.248(2)A, a=94.608(2), β=92.328(2),γ=105.840(2)°,C16H24N3O9Zn, Mr=467.75, V=994.8(2) A3, Z=2, Dc=1.562 g/cm3,μ(MoKa)=1.289 mm-1,F(000)=486, the final R=0.0243 and wR=0.0622 for 3505 independent reflections with Rint=0.0125. The Zn(Ⅱ) adopts a distorted five-coordinate triangle bipyramidal geometry. The basic framework structure of the complex is a 1-D chain. The intrachain hydrogen bonds are helpful to stabilize the 1-D chain structure. Furthermore, the chains are connected by O-H…O hydrogen bonds to give a 2-D double-layer network.