二维网状锌(Ⅱ)配位聚合物[Zn(HIDC)(bib)_(0.5)]_n的合成、晶体结构和荧光性质

<正>金属-有机配位聚合物(Metal-Organic Coordination Polymers,MOCPs)材料因其多变的结构拓扑以及其在离子交换、气体储存、分离、催化和荧光传感等方面的潜在应用已引起了科学家的广泛关注。氮杂环多元羧酸配体由于其骨架比较稳定,氮原子     

二维网状锌(Ⅱ)配位聚合物[Zn(HIDC)(bib)0.5]n的合成、晶体结构和荧光性质

A new 2D Zn(Ⅱ) coordination polymer [Zn(HIDC)(bib)_0.5]_n(1) was obtained by the hydrothermal reaction of ZnCl₂, imidazole-4,5-dicarboxylic acid (H₃IDC), and 1,4-bis(imidazol-1-yl)-butane (bib) with 2∶2∶1 mole ratio. X-ray diffraction crystal structural analysis reveals its crystallizes in monoclinic, space group P2₁/n with a=0.943 38(16), b=1.022 48(18), c=1.393 8(2) nm, β=109.434(3)°, V=1.267 9(4) nm³,Z=4, D_c=1.648 Mg·m^-3, F(000)=636, the final R₁=0.044 1, and wR₂=0.100 3 for 1 742 observed reflections with I≥2σ(I). In 1, each Zn(Ⅱ) ion is five-coordinated with a distorted trigonal bipyramidal coordination geometry, and each μ₂-HIDC² acts as a bridge to bond two neighboring Zn(Ⅱ) ions, leading to an 1D zigzag chain architecture. The adjacent chains are further linked by bib to form an infinite 2D network structure. The fluorescence spectrum of 1 exhibits intense emission at 436 nm when excited at 380 nm in solid state at room temperature. CCDC: 748259.     

由咪唑-4,5-二羧酸和1,4-对苯二甲酸构筑的一个三维镉(Ⅱ)配位聚合物的合成、结构及荧光性质

以CdCl₂、咪唑-4,5-二羧酸(H₃IDC)和1,4-对苯二甲酸(H₂BDC)为原料,在水热条件下合成得到了一个新的三维镉(Ⅱ)配位聚合物[Cd₂(HIDC)(BDC)(H₂O)]_n(1),通过元素分析、红外光谱、粉末X-射线衍射、热重分析和单晶X-射线衍射法等对其组成和结构进行了表征。单晶X-射线结构分析表明,在配合物1的晶体结构中含有沿a轴方向的一维无限的{[Cd₂(CO₂)]₂(CO₂)₂}_n配位聚合链。此聚合链再通过桥连HIDC²与BDC^2-配体的连接,最终形成一复杂的三维金属-有机框架结构。配合物1的固体室温荧光测试结果表明,在波长为350nm的光激发下于456nm处出现强烈的荧光发射。     

树枝状聚酯多元醇的烯丙基末端改性

在三乙胺作催化剂的情况下,树枝状聚酯多元醇与丁二酸杆作用生成树枝状聚酯多元醇丁二酸单酯;后者在相转移催化下,与氯丙烯在弱碱条件下进行成酯反应,合成了未见文献报道的对枝状聚酯多元醇丁二酸烯丙基酯化产物,羟基酯化率为80％。     

配合物(n-Bu)_2Sn(C_(10)H_8N_2O_4)(C_2H_5OH)的合成和晶体结构

以2-羰基丙酸水杨酰腙作为配体与二正丁基氧化锡(Ⅳ)在苯/乙醇混合溶剂中反应, 合成了新型配合物(n-Bu)2Sn(C10H8N2O4)(C2H5OH)(C10H8N2O42为2-羰基丙酸水杨酰腙负二价离子)。用单晶X-射线衍射分析法测定了该配合物的晶体结构。晶体属四方晶系, I41/a空间群, 晶胞参数a = 2.5113(7), b = 2.5113(7), c = 1.5062(6) nm, V = 9.499(5) nm3, Z = 16, Dc = 1.396 g/cm3, m(MoKa) = 1.105 mm1, F (000) = 4096。对于2499 (I >2s(I))个可观测点, 最终可靠因子R = 0.0349, wR = 0.0793。在该配合物的分子结构中, 中心锡原子与3个O原子、1个N原子和2个C原子形成扭曲的八面体几何构型, 其中3个O原子和1个N原子为赤道配位原子, 而CSnC为配合物的轴。相邻配合物分子间因Sn…O的弱相互作用和分子间氢键的作用而以二聚体的结构形式存在。     

配合物Ni(C14H10N2O3)(C5H5N)的合成和晶体结构

A novel nickel(Ⅱ) complex with 2,4-dihydroxybenzalidene benzoylhydrazone and pyridine ligands, Ni(C₁₄H₁₀N₂O₃)(C₅H₅N), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex has been determined by single crystal X-ray diffraction techniques. The crystal belongs to orthorhombic, space group Pbca. The cell parameters are: a=1.580 20(19) nm, b=1.362 18(16) nm, c=1.616 50(19) nm, and V=3.479 5(7) nm³, Z=8, D_c=1.497 Mg·m^-3, μ(MoKα)=1.139 mm^-1, F(000)=1 616, R=0.032 9 and wR=0.077 0 for 2 772 observed reflections (I>2σ(I)) out of 3810 unique ones. The nickel(Ⅱ) ion lies in a distorted square-planar environment composed of two oxygen atoms, one nitrogen atom of tridentate acyhydrazone schiff base ligand and one nitrogen atom of the pyridine ligand. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 244668.     

三元混合配合物Cu(C10H8N2O3)·(C5H5N)·(H2O)的合成和晶体结构

The novel copper(Ⅱ) complex with 2-oxo-propionic acid benzoyl hydrazone and pyridine ligands, Cu(C₁₀H₈N₂O₃)·(C₅H₅N)·(H₂O) (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionicacid benzoyl hydrazone), has been synthesized and characterized by elemental analysis and IR. The crystal structure of the title complex was determined by single crystal X-ray diffraction technique. Complex crystallized in the triclinic space group P1 with a = 0.729 08(10) nm, b= 1.020 01(14) nm, c= 1.126 28(15) nm, α = 71.644(2) °, β = 80.437(2) °, γ = 89.160(2)°, V= 0.78328(18) nm³, Z= 2, D_c= 1.547 Mg·m^-3, μ(MoKα) = 1.417 mm^-1, F(000) = 374. The final R₁ = 0.030 6, wR₂= 0.084 2 for 2 992 observed reflections [I≥2σ(I)] out of 3357 unique reflections. In this complex, copper(Ⅱ) ion is square-pyramidally coordinated by two oxygen atoms and one nitrogen atom of tridentate C₁₀H₈N₂O₃^2- ligand, one nitrogen atom of the pyridine ligand, and one oxygen atom of water molecule with the oxygen atom of water molecule locating at the apical position. The analysis of the crystal structure indicates that the complex has a one-dimensional chain structure, which is formed by intermolecular hydrogen bonds. CCDC: 222656.     

Synthesis and Crystal Structure of a Copper(II) Complex with 2,4-Dihydroxybenzylidene Benzoylhydrazone Ligand

1 INTRODUCTION The chemical properties of acylhydrazones Schiff bases and their complexes with some transition metal ions have been intensively investigated in several re- search areas because of their chelating capability and pharmacological applications[1～10]. Intriguingly, the copper(II) complexes are shown to be signifycantly more potent than the metal free chelate, suggesting that the metal complex is the biologically active species. Owing to the biological interest in these types …     

二聚体配合物[(n-Bu)2Sn(C10H8N2O3)(C2H5OH)]2的合成和晶体结构

The novel seven-coordinate complex [(n-Bu)₂Sn(C₁₀H₈N₂O₃)(C₂H₅OH)]₂ (C₁₀H₈N₂O₃^2- is the dinegative ion of 2-oxo-propionic acid benzoyl hydrazone) was synthesized by the reaction of (n-Bu)₂SnO with 2-oxo-propionic acid benzoyl hydrazone in 1∶1 molar ratio in benzene-ethanol (V/V, 3/1), and its structure was characterized by X-ray single crystal diffraction. The crystal belongs to a tetragonal system with space group I4₁/a, a=2.4890(2)nm, b=2.4890(2)nm, c=1.5170(3)nm, V=9.398(2)nm³, Z=8, F(000)=3968, D_c=1.366g·cm^-3, and the structure was refined to final R₁=0.0530, wR₂=0.0971. The structure of the title complex is described as a dimer through weak interactions of Sn…O bonding and hydrogen bond. The tin atoms rendered sev-en-coordination in a distorted pentagonal bipyramid geometry structure, four oxygen atoms [O1, O2, O2^#1 and O4] and one nitrogen atom N2 formed the equatorial plane and C11-Sn1-C15 is the axis. CCDC: 212696.     

由MCl2(M=Zn，Cd)与咪唑-4，5-二羧酸和1，4-双(咪唑-1-基)丁烷构筑的两个二重穿插二维配位聚合物的合成、结构和性质

以2∶1∶4物质的量比的咪唑-4,5-二羧酸(H3IDC),1,4-双(咪唑-1-基)丁烷(bib)和ZnCl2或CdCl2为反应物,在水热条件下分别得到了1个二重穿插的二维锌(Ⅱ)配位聚合物{[Zn2(IDC)(bib)Cl].H2O}n(1)和1个二重穿插的二维镉(Ⅱ)配位聚合物[Cd2(HIDC)(bib)1.5Cl2]n(2)。用元素分析、红外光谱以及单晶X-射线衍射结构分析对它们的组成和结构进行了表征,并对它们的热稳定性和荧光性质进行了初步的研究。