Synthesis, Crystal Structure, and Luminescent Properties of a Cadmium(II) Coordination Polymer Based on Glutaric Acid and Triazole

A new coordination polymer, [Cd₇(μ ₃-O)₂(glut)₂(Hglut)₂(trz)₄]_n (1) (H₂glut = glutaric acid and Htrz = 1,2,4-triazole), has been synthesized under hydrothermal conditions, and further characterized by elemental analysis, IR, thermogravimetric analysis and single-crystal X-ray diffraction. Complex 1 features a fairly complicated three-dimensional (3D) (3,3,6,10)-connected framework constructed from two-dimensional (2D) infinite [Cd₇(μ ₃-O)₂(glut)₄(Hglut)₂]_n layers and [Cd(trz)₄]^2? units. Moreover, the thermal stability and photoluminescent properties of 1 were also investigated.     

One Pillared Layered Zn(Ⅱ) Coordination Compound Based on 2,6-Naphthalenedicarboxylic Acid: Synthesis,Structure and Luminescent Property

One new pillared layered zinc hydroxide {Zn_4(OH)_6(ndc)·2(H_2 O)}_n,(H_2 ndc =2,6-na-phthalenedicarboxylic acid) has been achieved under hydrothermal conditions by using2,6-na-phthalenedicarboxylic acid, 2,4-diami-6-phenyl-1,3,5-triazine as well as Zn(OAc)_2·2 H_2 O,and structurally characterized by X-ray single-crystal diffraction, IR spectra, elemental analysis,powder X-ray diffraction(PXRD) and thermogravimetric analysis(TGA). The X-ray single-crystal diffraction proves that the title compound is in monoclinic system, space group P2_1/c with a =16.362(8), b = 9.324(5), c = 5.364(3) ?, β = 99.081(9)°, V = 808.1(7) ?~3, D_c = 2.522 g/cm~3, M_r =613.73, Z = 2, F(000) = 608, μ = 5.935 mm~(-1), GOOF = 1.050, R = 0.0469 and wR(Ⅰ 2σ(Ⅰ)) =0.1291. In the title compound, the tetrahedral and octahedral zinc atoms are connected by μ_3-OH groups to form zinc hydroxide inorganic layers extending parallel to the bc-plane. The adjacent layers are pillared by the connection of Zn2 atoms with ndc~(2-)ligands to construct a three-dimensional(3D) structure; meanwhile, the interactions of five hydrogen bonds make the 3D network structure more stable. Furthermore, the title compound exhibits luminescent property at solid state.     

A Luminescent Three-Dimensional Coordination Polymer Based on Cu(I) Halide Clusters Showing Dia Topology with 8-Fold Interpenetration

One interesting copper(I) halide-based coordination polymer with a formula of [Cu₄(Br)₄(bib)₂]_n (1) (bib = 1,4-bis(imidazol-2-methyl)butane) has been prepared by solvothermal method, and characterized by X-ray single crystal diffraction, elemental analyses, IR and TGA. Structure analyses reveal that the compound is constructed of copper(I) halide clusters and flexible bib ligands, which features a 8-fold interpenetrated 3D framework with 4-connected extended dia topology. Furthermore, the compound exhibits high thermal stability and intense fluorescent emission, and can be explored for potential red luminescent materials.     

Synthesis and Characterization of a Novel 3D Coordination Polymer Based on Cu（II） Cations and Mellitic Acid

A new mellitate complex [Cu3（μ2-mellitate）（μ2-H2O）（H2O）2·H2O]n 1 has been synthesized by the reaction of mellitic acid and Cu（CH3COO）2·H2O in the presence of base. Crystallographic data for 1： C12H8O16Cu3, Mr = 598.80, orthorhombic, Pbcn, a = 8.4378（6）, b = 10.0396（7）, c = 17.6799（12）A, V = 1497.70（18）A^3, Z = 4, De = 2.656 g/cm^3, μ = 4.327 mm^-1, F（000） = 1180, R = 0.0431 and wR = 0.0964 for 1075 observed reflections （I 〉 2σ（I））. X-ray crystal structural analysis revealed that the mellitate anions behave as the bridging ligands and link eight copper atoms repeatedly to form a novel three-dimensional metal-organic coordination polymer with two different rhombic tunnels in the solid-state structure.     

Synthesis,Structure and Luminescent Property of an Europium(Ⅲ) Coordination Polymer

A novel europium(Ⅲ) coordination polymer, [Eu3(pydc)3(SO4)(H2O)5(ox)0.5]·3H2O(1, H2 ox = oxalic acid, H2 pydc = pyridine-2,6-dicarboxylic acid), has been synthesized hydrothermally from the self-assembly of lanthanide ions(Eu3+) with the flexible oxalic acid and the rigid pyridine-2,6-dicarboxylic acid ligands, respectively. It crystallizes in the triclinic system, space group P1 with a = 11.225(4), b = 12.390(5), c = 13.752(5)A, α = 89.228(7), β = 71.142(6), γ = 75.552(6)°, Dc = 2.317 g/cm3, μ = 5.480 mm-1, F(000) = 1150, Z = 2, the final R = 0.0351 and w R = 0.0949 for 8782 observed reflections with I 2σ(I). Structural analysis reveals that complex 1 exhibits a three-dimensional metal-organic framework via π-π stacking interactions. In addition, complex 1 displays a red fluorescence emission in the solid state at room temperature, which corresponds to the 5D0 → 7F2 transition of Eu3+ ions.     

三聚氰酸钴配合物的合成、晶体结构及荧光性质

本文合成了一个新的配合物Co(H2CA)2(H2O)2(H3CA=三聚氰酸),并通过元素分析、红外、荧光和单晶X-Ray射线进行了表征。标题化合物属于三斜晶系,P1空间群,a=0.503 83(7)nm,b=0.699 82(10)nm,c=0.911 08(13)nm,α=90.107(2)°,β=98.032(2)°,γ=110.788(2)°,V=0.296 92(7)nm3,Z=1,R=0.038 2。在配合物中,Co(Ⅱ)离子与三聚氰酸配体上的N原子,配位水的O原子配位,形成规则的平面正方形配位构型。相邻的2个Co(Ⅱ)平面四边形单元通过配体三聚氰酸上的氢键形成三维网状结构。室温荧光光谱测定表明该化合物在420 nm处有强的荧光发射。     

苯基多羧酸及含氮配体构筑的三维框架结构锌配位聚合物的合成、晶体结构和荧光性质

以醋酸锌、5-溴-1,2,4-苯基三羧酸(BTCAH₃)和4,4'-联吡啶(4,4'-bipy)为原料,在水热条件下合成了1个三维框架结构化合物[Zn₃(BTCA)₂(4,4'-bipy)₃](1),利用红外光谱、元素分析、热重、X-粉末衍射以及X-单晶衍射对该化合物进行了表征。化合物1是单斜晶系,C2/c空间群。在化合物1中,锌离子通过BTCA^3-配体的羧酸氧原子形成一个具有3-节点、4-连接的三维框架结构。4,4'-联吡啶配体在框架结构中连接锌离子。另外,研究了该化合物的热稳定性和固体荧光性质。     

两个基于2,3,5,6-四氟-二（1,2,4-三氮唑-1-甲基）苯和1,4-萘二甲酸混合配体的配位聚合物的合成、结构及其荧光性能

采用水热法成功合成了两个基于2,3,5,6-四氟-二(1,2,4-三氮唑-1-甲基)苯（Fbtx）及1,4-萘二甲酸（H2NDC）混合配体的配位聚合物,分子式分别为{[Co(NDC)(Fbtx)(H2O)2]·0.5H2NDC}n(1, CCDC: 1978985)和{[Cu(NDC)(Fbtx)(H2O)]·1.5H...     

X-Ray Absorption Spectroscopy of Strontium(II) Coordination

Detailed analyses of crystalline, hydrated, and precipitated strontium compounds and an aqueous strontium solution by synchrotron extended X-ray absorption fine structure (EXAFS) were used to quantify local thermal and static disorder and to characterize strontium coordination in a variety of oxygen-ligated bonding environments. Analysis of anharmonic vibrational disorder (i.e., significant contribution from a third cumulant term (C(3)) in the EXAFS phase-shift function) in compounds with low and high static disorder around strontium showed that first-shell anharmonic contributions were generally not significant above experimental error in the EXAFS fits (R+/-0.02 ? with and without C(3)). The only case in which a significant apparent decrease in Sr-O distance was observed with increasing temperature, and for which a third cumulant term was significant, was for dilute strontium in aqueous solution. Empirical parameterization of Debye-Waller factor (sigma(2)) for strontium compounds as a function of backscatterer atomic number (Z), interatomic Sr-Z distance, and temperature of spectral data collection showed systematic increases in sigma(2) as a function of increasing temperature and Sr-Z bond length. At values of sigma(2) greater than approximately 0.025 ?(2) (for N<12 and R(Sr)-Z>3 ?), backscattering was generally not significant above noise levels in spectra of compounds of known crystal structure. Comparison of the EXAFS spectra of freshly precipitated SrCO(3) (spectra collected wet) to that of dry, powdered strontianite (SrCO(3)(s)) indicated no significant differences in the local atomic structure around strontium. Analysis of partially hydrated strontium in natural Ca-zeolite (heulandite) showed that strontium is substituted only in the calcium (Ca2) site. Backscattering from aluminum and silicon atoms in the zeolite framework were apparent in the EXAFS spectra at low and room temperature at distances from central strontium of <4.2 ?. Comparison of strontium structural coordination determined in this and previous studies suggests that previous EXAFS determinations of hydrated strontium may have underestimated first-shell interatomic distances and coordination numbers because minor contributions to the EXAFS phase-shift and amplitude functions were not accounted for, either theoretically or empirically. Copyright 2000 Academic Press.     

One Trinuclear Copper(II) Polymer Based on Pyridine-2,4,6-Tricarboxylic Acid: Synthesis,Structure, and Magnetic Analysis

The reaction of CuCl₂ · 2H₂O with pyridine-2,4,6-tricarboxylic acid (H₃Pyta) in ethanol and water under hydrothermal synthesis conditions leads to the formation of a trinuclear copper polymer {[Cu₃(Pyta^3–)₂(H₂O)₈] · 4H₂O}n (I) (C₁₆H₂₈N₂O₂₄Cu₃, Mr = 823.05, ρ_calcd = 1.955 g cm^–3). The polymer was characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffraction (СIF file CCDC no. 1525203). The result showed that I belongs to the monoclinic system, P2₁/c space group. TGA curve shows that polymer I first removes water molecules, and then the ligand split for polymer I, and the remained residue is CuO. The magnetic measurement reveals the pyridine-2,4,6-tricarboxylic acid as bridge ligand can mediate the antiferromagnetic coupling interaction between magnetic centers.     

Synthesis and Structure of a New Coordination Polymer Based on Indium and 1,4-Benzenedicarboxylate

A new coordination polymer {[In(bdc)(OH)]·4H2O}n(H2bdc=1,4-benzenedi-carboxylic acid) has been synthesized through hydrothermal conditions,and was characterized by X-ray single-crystal diffraction and other measurements.The complex crystallizes in the orthorhombic system,space group Imma with a=18.3621(13),b=7.1932(5),c=11.8278(8),V=1562.24(19)3,Z=4.Dc=1.565g/cm3,Mr=368.00,F(000)=728,μ(MoKα)=1.542 mm-1,S=1.019,R=0.0468 and wR=0.1326 for 884 observed reflections(2σ(Ⅰ)).The title compound represents a 3-D framework containing four kinds of tunnels in different shapes and sizes.     

苯基多羧酸及含氮配体构筑的三维框架结构锌配位聚合物的合成、晶体结构和荧光性质

以醋酸锌、5-溴-1,2,4-苯基三羧酸(BTCAH₃)和4,4’-联吡啶(4,4’-bipy)为原料,在水热条件下合成了1个三维框架结构化合物[Zn₃(BTCA)₂(4,4’-bipy)₂](1),利用红外光谱、元素分析、热重、X-粉末衍射以及X-单晶衍射对该化合物进行了表征。化合物1是单斜晶系,C2/c空间群。在化合物1中,锌离子通过BTCA^3-配体的羧酸氧原子形成一个具有3-节点、4-连接的三维框架结构。4,4’-联吡啶配体在框架结构中连接锌离子。另外,研究了该化合物的热稳定性和固体荧光性质。     

A New One-dimensional Coordination Polymer Based on 3,5-Dinitro-salicylic Acid:Synthesis,Crystal Structure,Luminescent Property and Theoretical Calculation

A new one-dimensional Mg(Ⅱ) coordination polymer, [Mg(L)(phen)(H_2O)](1), has been hydrothermally synthesized by using 3,5-dinitro-salicylic acid(H2L) and 1,10-phenanthroline(phen). It crystallizes in monoclinic, space group C2/c with a = 33.038(7), b = 6.6481(13), c = 22.750(5) ?, β = 126.99(3)o, V = 3991.1(14) ?3, Z = 8, C19H12 MgN_4O_8, Mr = 448.64, Dc = 1.493 g/cm3, F(000) = 1840, μ(Mo Ka) = 0.146 mm-1, R = 0.0559 and w R = 0.0975. In 1, each L anion bridges two Mg(Ⅱ) atoms to give one-dimensional zigzag chains with the Mg···Mg separation of 5.34 ?, which are extended by π-π stacking interactions between 1,10-phenanthroline ligands into a two-dimensional supramolecular layer. Moreover, the O–H···O hydrogen-bonding interactions further stabilize the layer structure of 1. The luminescent property was also studied for 1 in solid state at room temperature. In addition, natural bond orbital(NBO) analysis was performed by the B3LYP/LANL2 DZ method in Gaussian 09 Program. The calculation results show obvious covalent interaction between the coordinated atoms and Mg(Ⅱ) ion.     

三维1,4-二-(4-羧基吡啶基)丁烷合铜(Ⅱ)、银(I)配合物的合成及晶体结构表征

利用1,4-二-(4-羧基吡啶基)丁烷(L)合成了铜(Ⅱ)、银(I)的配合物[[CuL(H2O)3]·2(H2O)·2(NO3)}n(1)、{[AgL]·(H2O)·     

Ionothermal Synthesis,Crystal Structure and Photocatalytic Property of a New Cobalt Coordination Polymer

The reaction of flexible bis(imidazole) ligand and 1,2-bis(imidazol-1'-yl)methane(bimm) with Co(Ⅱ) salt under ionothermal method resulted in the formation of a new coordination polymer {[Co(bimm)3]·(PF6)2}n(1). X-ray single-crystal diffraction determination reveals that 1 crystallizes in the triclinic P1 space group, with a = 8.647(6), b = 12.092(9), c = 14.967(11) , α = 88.912(8), β = 81.199(8), γ = 89.395(8)°, V = 1546(2)3, Z = 2, Mr = 793.39, Dc = 1.704 Mg/m3, μ = 0.768 mm-1, F(000) = 798, the final R = 0.0626 and w R = 0.1634 for 4319 observed reflections with Ⅰ 2δ(Ⅰ). In compound 1, the Co(Ⅱ) ion is connected to another Co(Ⅱ) by two bimm ligands to form 1D double chains which are further linked by bimm ligands to form a 2D wavelike layer. Topologically, the structure of 1 represents a uninodal 2D 4-connected sql/Shubnikov tetragonal plane net. Moreover, thermogravimetric analyses and photocatalytic property for 1 have also been investigated.     

A Luminescent Cd(Ⅱ) Coordination Polymer Constructed from Isophthalic Acid and 1,3-Bis-(4-pyridyl)propane

A new coordination complex [Cd2(ip)2(bpp)]n(1, H2 ip = isophthalic acid, bpp = 1,3-bis-(4-pyridyl) propane) has been synthesized and structurally characterized. Crystal data for the title complex are as follows: triclinic system, space group P1 with a = 9.6724(6), b = 10.2243(6), c = 14.8205(9) ?, α = 88.927(5), β = 71.664(6), γ = 75.767(5)°, V = 1345.79(14) ?3, Mr = 751.29, Z = 2, F(000) = 740, Dc = 1.854 g/cm3, μ(Mo Kα) = 1.636 mm-1, R = 0.0259 and w R = 0.0623 for 4754 observed reflections with I 2σ(I). X-ray structure analysis reveals that complex 1 holds a 3D architecture based on α-Po primitive cubic units with the [Cd4(COO)8] units treated as 6-connected nodes. Solid-state properties for 1, such as infrared spectroscopy, elemental analyses, thermal stability and luminescent property, have also been investigated.     

异烟酸与Ag(Ⅰ)及硅钨酸配位聚合物的合成与晶体结构

水热条件下,合成得到了异烟酸与Ag(Ⅰ)及硅钨酸所形成的配位聚合物[Ag12(L)8(H2O)5](SiW12O40).6H2O(1)(L=isonicotinate,异烟酸)。通过元素分析和红外光谱、紫外光谱、X-射线单晶衍射对其组成和结构进行了表征。晶体结构分析结果表明:该配合物属于单斜晶系,C2/m空间群;晶胞参数分别为a=1.259 5(2)nm,b=2.429 7(3)nm,c=1.825 7(3)nm,β=103.794(2)°,V=5.425 9(13)nm3,Z=2;异烟酸与Ag髣及硅钨酸形成具有微孔的三维结构配位聚合物,即硅钨酸离子通过静电作用连接异烟酸离子与Ag髣所形成的二维波浪式网格而形成三维结构。     

Synthesis and Crystal Structure of a Novel 1D Magnesium(II) Coordination Polymer Constructed by L-Cysteic Acid

A novel coordination polymer [Mg(L)(H2O)2]·H2O] (LH2 = L-cysteic acid) has been synthesized and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal crystallizes in orthorhombic system, space group P212121, with a = 5.962(3), b = 11.224(6), c = 13.664(7) , V = 914.3(8) 3, Z = 4, Mr = 245.50, Dc = 1.783 g/cm3, μ = 0.445 mm–1, flack parameter = 0.32(16), F(000) = 512, the final R = 0.0458 and wR = 0.1172 for 1578 observed reflections with I > 2σ(I). The Mg(II) atom shows an octahedral geometry defined by two carboxyl O atoms from two different L-cysteic acid ligands, one carboxyl O atom and one amino N atom from the adjacent ligand, and two aqua ligands. The Mg(II) atoms are bridged by L-cysteic acid ligands, leading to a 1D infinite zigzag chain. In the structure there are extensive hydrogen bonds, through which the complex completes its 3D framework structure.