Synthesis and Crystal Structure of a Novel Ca(Ⅱ) Coordination Polymer Containing Dipyridine Dicarboxylic Ligand

The novel alkaline metal complex Ca(BPDCH)2(1, BPDCH2 = 2,2'-bipyridine-5,5'-dicarboxylic acid) has been synthesized by the hydrothermal reaction of Ca(NO3)2·4H2O with 2,2'-bipyridine-5,5'-dicarboxylic acid. The molecular and crystal structures of complex 1 have firstly been characterized by FTIR, elemental analysis, and X-ray single-crystal diffraction. The 3D MOF structure of complex 1 was interpreted by the versatile binding modes-the intermolecular hydrogen bonds and π-π stacking interactions of 2,2'-bipyridine-5,5'-dicarboxylic acid ligand. The analysis results show complex 1 belongs to a coordination polymer with 3D MOF structure. The results of thermogravimetric analysis and solubility demonstrate complex 1 is a thermostable compound and does not dissolve in water and traditional organic solvents.     

Synthesis,Crystal Structure,Thermal Behavior and Photoluminescence of a Novel Two-dimensional Cd(Ⅱ) Coordination Polymer

A new coordination polymer, [Cd2(bptc)(L)2(H2O)2]·5H2O(1, L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and H4 bptc = 3,3',4,4'-biphenyltetracarboxylic acid), has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 18.868(4), b = 7.2111(14), c = 19.464(4), β = 95.75(3)°, C54H31Cd2Cl2F2N8O15, Mr = 1365.57, V = 2635.0(9)3, Z = 2, Dc = 1.721 g/cm3, S = 1.034, μ(MoKα) = 0.995 mm–1, F(000) = 1358, R = 0.0501 and wR = 0.1076. In 1, each bptc anion bridges four Cd(II) atoms to form 2D layer structures, which are further extended by π-π stacking interactions into a 3D supramolecular architecture. The thermal behavior and luminescent properties of the compound have also been studied.     

Synthesis and Crystal Structure of a Novel Cobalt（Ⅱ） Coordination Polymer with 1,2,4,5-Benzenetetracarboxylate

A novel cobalt（II） coordination polymer,[Co（BTEC）1/2]n 1,has been synthesized with Co（NO3）2·6H2O and 1,2,4,5-benzenetetracarboxylic acid （H4BTEC） by the hydrothermal method,and characterized by elemental analysis,IR and single-crystal X-ray diffraction. Crystallographic data for 1： C5HO4Co,Mr = 183.99,monoclinic,space group C2/c,a = 16.619（6）,b = 7.416（3）,c = 8.040（3）A,β = 90.612（4）°,V = 990.8（6） A^3,Z = 8,Dc = 2.467 g/cm^3,μ = 3.390 mm^-1,F（000） = 720,R = 0.0307 and wR = 0.0847 for 912 observed reflections （I 〉 2σ（I））. X-ray crystal structural analysis revealed that each Co（II） adopts a tetrahedral coordination mode to link four separate BTEC ligands via uniform monodentate carboxylate groups and each BTEC ligand possesses an 8-connected geometry to connect eight Co（II） ions. Complex 1 exhibits a rare （4,8）-connected net with （45.6）2（410.614.84） topology.     

Synthesis and Crystal Structure of a New(6,3)-Connected Ni(Ⅱ) Coordination Polymer

The coordination polymer [Ni(dpa)(bpp)]n(H2dpa = 2,4'-biphenyl-dicarboxylic acid,bpp = 1,3-di(4-pyridyl)propane) was hydrothermally prepared and characterized by single-crystal X-ray diffraction,FTIR spectra,elemental analysis and thermal analysis.The crystal is of triclinic system,space group P1 with a = 12.516(5),b = 12.943(5),c = 15.130(5) ,α = 94.331(5),β = 91.827(5),γ = 108.382(5)°,C54H44N4Ni2O8,Mr = 497.18,V = 2315.3(15) 3,Dc = 1.426 g/cm3,F(000) = 1032,μ = 0.875 cm-1,Z = 2,the final R = 0.0496 and wR = 0.1100 for 5365 reflections with Ⅰ 2σ(Ⅰ).X-ray diffraction analysis reveals that the carboxylate group of 2,4'-diphenic acids acting as bridging ligands adopts two coordination modes:bis-mondentate and bidentate chelating.The compound exhibits a two-dimensional(6,3)-connected architecture.     

A Novel 3D Cu(Ⅱ) Coordination Polymer Containing Mixed Ligands: Synthesis,Crystal Structure and Properties

A novel compound, {[Cu2(nbdc)2(4,4'-bpy)2(H2O)2]·2H2O}n(H2nbdc = 4-nitrobenzene-1,2-dicarboxylic acid, 4,4'-bpy = 4,4'-bipyridine), was hydrothermally synthesized and characterized by elemental analysis, IR spectroscopy, thermogravimetric analysis(TGA), and single-crystal X-ray diffraction. The complex is of orthorhombic system, space group Pbcn with a = 32.222(7), b = 7.8503(16), c = 28.389(6), V = 7181(3)3, Dc = 1.720 g/cm3, Mr = 929.74, Z = 8, F(000) = 3792, μ = 1.273 mm-1, the final R = 0.0591 and wR = 0.1378 for 4548 observed reflections with I 2σ(I). The compound exhibits a 3D self-penetrating framework with bcu net topology, in which the(46·48)-networks are joined by the H2nbdc and 4,4'-bpy linkers.     

Urothermal Synthesis and Crystal Structure of a Zn（Ⅱ） Coordination Polymer with a 3-D Supramolecular Structure

A new metal-organic coordination polymer [Zn(hfipbb)(e-urea)]n(1,H2hfipbb = 4,4'-(hexafluoroisopropylidene)bis(benzoic acid),e-urea = ethylene urea) has been urothermally synthesized and characterized by elemental analysis and single-crystal X-ray diffraction.The title complex crystallizes in monoclinic,space group P21/c with a = 13.302(4),b = 10.981(3),c = 13.804(4) ,β = 93.587(5)°,V = 2012.3(10) 3,C20H14N2O5F6Zn,Mr = 541.72,Z = 4,Dc = 0.447 g/cm3, = 0.328 mm-1,F(000) = 272,R = 0.0340 and wR = 0.1107 for 4528 observed reflections(I >2σ(I)).In the structure of compound 1,two Zn(Ⅱ) ions are bridged by two carboxylate groups from two hfipbb ligands to form a dinuclear unit,and each dinuclear Zn(Ⅱ) unit is linked with its two adjacent dinuclear units through four hfipbb ligands into an infinite one-dimensional double-chain.The interesting structural feature of compound 1 is that the one-D double-chains are self-interconnected into a three-D supramolecular structure through hydrogen bonds between the coordinated e-urea molecules and carboxylate oxygen atoms(N1 and O2,N2 and O4).     

Three-dimensional 3d-4d Heterometallic Coordination Polymer——Synthesis,Structure,Magnetic and Luminescent Properties

A new three-dimensional 3d-4d heterometallic coordination polymer,[Cd2Mn(H2O)4(BTC)2]·2H2O(BTC=1,3,5-benzenetricarboxylate) was prepared under hydrothermal conditions and characterized by single crystal X-ray diffraction.This compound crystallized in the monoclinic space group C2/c,with cell parameters a=1.9452(4) nm,b=0.7094(2) nm,c=1.8064(4) nm,β=118.02(3)°,V=2.2004(8) nm3 and Z=4.Its structure contains trinuclear mixed metal clusters,which are further connected by BTC to form a three-dimensional framework.The compound exhibits intense photoluminescence at room temperature.Magnetic studies of the compound show a dominant antiferromagnetic exchange between the Mn(Ⅱ) ions.     

Hydrothermal Synthesis and Crystal Structure of One 3D Coordination Polymer of Nickle （II） Achieved from 5-Iodo-isophthalic Acid Ligand

A new coordination polymer [Ni（L）（m-bix）（H2O）]n （1, H2L = 5-iodo-isophthalic acid, m-bix=1,3-bis（imidazol-1-ylmethyl）-benzene） has been synthesized by the hydrothermal method and characterized by IR, elemental analysis, powder XRD and single-crystal X-ray analysis. The crystal is of triclinic, space group Pī with a = 9.1638（3）, b = 10.2319（3）, c = 13.2463（4） ？, α = 80.1710（10）, β = 83.671（2）, γ = 70.3790（10）o,C22H19NiIN4O5, Mr = 605.02, V = 1150.85（6） ？3, Dc = 1.746 g/cm3, F（000） = 600, μ = 2.225 mm-1, S = 1.045 and Z = 2. The final R = 0.0388 and wR = 0.1257 for 5089 observed reflections with I 〉 2σ（I）. In the title complex, the M and P layers are arranged alternately to give a double-layer structure by the symmetry related hydrogen bonds, and these double-layers are further joined together to achieve a 2D supramolecular architecture through I···π interaction involving iodine atoms and imidazole rings. The thermal stability of the title complex was studied by thermal gravimetric （TG） and differential thermal analysis （DTA）.     

Synthesis,Crystal Structure and Properties of a New Coordination Polymer Constructed with 3-（4-hydroxypyridinium-1-yl）phthalic Acid

A new nickel coordination polymer {[Ni(dpa)(bpe)(H2O)]2}n(1) has been hydro-thermally synthesized, and structurally characterized by UV spectroscopy, elemental analyses and single-crystal X-ray diffraction(H2dpa=3-(4-hydroxypyridinium-1-yl) phthalic acid, bpe=μ-1,2-di(4-pyridyl) ethylene). It crystallizes in the triclinic system, space group P1 with a=8.779(2), b=10.909(3), c=12.739(3), α=72.45(2), β=75.13(2), γ=86.47(2)°, V=1124.1(5) 3, Z=2, Mr=516.14, Dc=1.525 g/cm3, μ=0.912 mm-1, Rint=0.0532, F(000)=532, the final R=0.0523 and wR=0.1089 for 3949 observed reflections(I2σ(I)). The coordination around the Ni center is a distorted octahedron coordination geometry involving two protonated H2dpa ligands, two bpe ligands, and one coordinated H2O molecule. The dpa2- anion, as a bridging ligand, connects two Ni centers to form binuclear units, which are linked together by the bpe ligands to form two-dimensional layers, and the interlayer hydrogen bonding further extends the 2D sheet into a 3D supramolecular framework.     

Synthesis,Crystal Structure and Characterization of a Cobalt Coordination Polymer： [Co（bib）（L）]-0.5H2O

The title coordination polymer, [Co（bib）（L）].0.5H2O 1 （bib = 1,1＇-（1,4-butanediyl）bis（imidazole） and L = 4,4＇-oxy（bisbenzoate） has been hydrothermally synthesized and characterized by IR and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group Cc with a = 8.8568（5）, b = 19.936（1）, c = 26.209（2） γ, y = 97.510（1）°, V= 4587.8（5） A3, Z = 8, CoC24H23N4O5.5, Mr = 514.39, Dc = 1.489 g/cm3, F（000） = 2128, μ（MoKa） = 0.795 mm^-1, R = 0.0419 and wR = 0.1002. Compound 1 exhibits a rare two-fold interpenetrating CdSO4 type topology. The O-H...O hydrogen bonds stabilize the structure of 1.     

Hydrothermal Synthesis and Crystal Structure of a New Three-dimensional Co（II） Coordination Polymer Based on 2,3-Thiophenedicarboxylic Acid

A new Co（ll） polymer [Co（tdc）（l,4-bimb）]n 1 （H2tdc = thiophene-2,3-dicarboxy- lic acid, 1,4-bimb -- 1,4-bis（imidazol-1 ＇-yl）butane） was synthesized under hydrothermal conditions The compound crystallizes in the monoclinic system, space group C2/c with a = 15.643（9）, b = 8.839（5）, c=12.952（7） A, β = 105.964（6）°, V= 1721.8（16） A3, Z = 4, Mr = 419.32, Dc= 1.618 Mg/m3,μ = 1.149 mm-1, F（000） = 860, the final R = 0.0243 and wR =0.0613 for 1460 observed reflections with I 〉 2σ（I）. The compound presents a three-dimensional （3D） network extended by both tdc2- anions and 1,4-bimb ligands in which the tdc2- anions employ a chelating coordination mode. From the topology point of view, the structure could be described as a 3D 4-connected 65.8 CdSO4-type net. Infrared spectroscopy, elemental analyses, thermogravimetric analysis and powder X-ray diffraction properties of 1 are also investigated.     

A New Terbium（III） Coordination Compound with 2-Thiophenecarboxylic Ligand： Synthesis and Crystal Structure①

A new coordination compound with formula [Tb（2-TC）3（DMF）]n （1, 2-TC = 2-thio- phenecarboxylic ligand and DMF = dimethylformamide） was synthesized by solvothermal method. The structure of compound 1 was determined by single-crystal X-ray diffraction analyses, and characterized by elemental analyses, IR and powder X-ray diffraction. Structure analysis reveals compound 1, exhibiting a one-dimensional chain structure, crystallizes in triclinic space group P21/c, with a = 9.2751（19）, b = 16.490（3）, c = 15.865（5） A, β = 118.98（2）°, V= 2122.7（9）A3, D,. = 1.916 g/cm3, Mr= 612.45 （C18H15NO7S3Tb）, F（000） = 1196,μ（MoKa） = 3.67 mm-1, Z = 4, R = 0.0616 and wR = 0.0962 for 3865 observed reflections （I 〉 2o（I））, and R = 0.1092 for all data. Meanwhile, the photoluminescent properties of compound 1 were also investigated in the solid state at room temperature.     

Synthesis,Crystal Structure and Fluorescent Properties of a 4-Fold Interpenetrating Zn(Ⅱ) Polymer

A new coordination polymer [Zn(isop)(bps)]n 1(H2isop=benzene-1,3-dicer-boxylic acid,bps=4,4'-dipyridyl sulfide) has been prepared and structurally characterized by X-ray diffraction method.It crystallizes in monoclinic,space group P21/n with a=12.1936(11),b=10.7720(9),c=13.0685(11),V=1709.0(3)3,C18H12N2O4SZn,Mr=417.76,Z=4,Dc=1.624g/cm3,S=1.046,F(000)=848,the final R=0.0305 and wR=0.0858 for 3085 independent reflections with Rint=0.0147.Single-crystal X-ray diffraction analyses reveal that 1 is a 4-fold interpenetrating diamondoid network.The zinc(Ⅱ) atom is coordinated by two nitrogen atoms of two bps and two carboxylate oxygen atoms of isop ligands,resulting in a tetrahedral geometry.     

Crystal Structure and Luminescent Properties of a Zn(Ⅱ) Coordination Polymer Assembled by Mixed-ligand

A Zn(Ⅱ) coordination polymer [Zn(NIP)(3,3'-bpt)]·H2O(1, NIP = 5-nitroisophthalate, 3,3'-bpt = 1H-3,5-bis(3-pyridyl)-1,2,4-triazolate) has been synthesized by the hydrothermal reaction at 140 ℃ and structurally characterized by IR spectroscopy, X-ray diffraction, thermal analysis, single-crystal X-ray diffraction and luminescent properties. In complex 1, the zinc atom is five-coordinated with three carboxylate oxygen atoms from three H2 NIP and two nitrogen atoms from two 3,3'-bpt, respectively, forming a distorted trigonal bipyramidal geometry and showing a 1D chain structure, which is further bridged by NIP to form a 3D supramolecular network via self-assembly of hydrogen bonds.     

Hydrothermal Synthesis and Crystal Structure of a New 2D Zinc（Ⅱ） Coordination Polymer with 2-Aminoethanesulfonic Acid

A new 2D Zn(Ⅱ) coordination polymer [Zn(TAU)2]n (1, HTAU=2-aminoethane- sulfonic acid) constructed by 2-aminoethanesulfonic acid ligand has been hydrothermally synthesized by the reaction of Zn(CH3COO)2 and 2-aminoethanesulfonic acid with a 1:2 mole ratio and characterized by single-crystal X-ray diffraction, elemental analysis, infrared spectroscopy and thermogravimetric analysis. Crystal structural analysis reveals it crystallizes in monoclinic, space group P21/c with a=8.672(4), b=6.523(3), c=9.134(5) , β=115.441(5)°, V=466.6(4) 3, Mr=313.65, Z=2, Dc=2.232 Mg·m-3, F(000) =320, μ(MoKα)=3.091 mm-1, the final R=0.0358 and wR=0.0919 for 2026 observed reflections with Ⅰ > 2σ(Ⅰ). In the structure, each zinc(Ⅱ) ion is coordinated in a slightly distorted octahedron, and each μ3-TAU– acts as a bridge to bond three neighboring Zn(Ⅱ) ions to form an infinite 2D network structure.     

Synthesis,Structure and Magnetic Property of One Ni~Ⅱ Based Coordination Polymer

One new coordination polymer, [Ni(m-bix)(m-BDC)](1, m-bix = 1,3-bis(imidazol-1-ylmethyl)benzene, m-BDC = 1,3-benzenedicarboxylic acids), has been hydrothermally synthesized and structurally characterized by elemental analysis, IR, TGA and X-ray single-crystal diffraction. The green block crystal of complex 1(C22H18N4Ni O4) belongs to monoclinic system, space group P21/c with a = 10.0418(3), b = 23.8651(6), c = 8.7872(2) A, β = 112.333(3)o, V = 1947.88(9)A3, Z = 4, Dc = 1.572 g/cm3, Mr = 461.11, F(000) = 952, R = 0.0335 and w R = 0.0683 for 2827 observed reflections(I 2σ(I)). Complex 1 exhibits a novel 6-connected 3D sxd type topological framework. The magnetic characterization of complex 1 shows antiferromagnetic coupling exchange.     

Synthesis,Crystal Structure and Thermal Behavior of a New 2D Barium（Ⅱ） Coordination Polymer with 1H-benzimi-dazole-5,6-dicarboxylate as the Single Ligand

The self-assembly of 1H-benzimidazole-5,6-dicarboxylic acid with barium chloride under hydrothermal conditions afforded a new 2D coordination polymer,[Ba2(L)(HL)Cl]n(1,L = 1H-benzimidazole-5,6-dicarboxylate),which was characterized by elemental analysis,infrared spectroscopy,thermogravimetric analysis,and single-crystal X-ray diffraction.Compound 1 is of monoclinic system,space group P21/c with a = 10.0145(6),b=25.6854(15),c=7.3116(4) ?,β = 99.4980(10)°,V = 1854.95(19)3,C18H9Ba2ClN4O8,Z = 4,Mr=719.42,Dc = 2.576 g/cm3,μ(MoKα) = 4.427 mm-1,F(000) = 1352,the final R = 0.0202 and wR=0.0465 for 3051 observed reflections with I > 2σ(I).It exhibits an interesting two-dimensional network structure and high thermal stability(up to 420 ℃).     

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc（Ⅱ） Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound,[Zn(5-hydroxynicotinate) 2 2H 2 O] n,has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions,and its structure was determined by X-ray crystallography with the following data:monoclinic,space group C2/c,C 12 H 12 N 2 O 8 Zn,M r=377.61,a=10.223(3),b=10.319(3),c=13.613(4),β=105.922(6)°,Z=4,V=1380.9(8)3,F(000)=768,D c=1.816 g/cm 3,μ(MoKα)=1.826 mm-1,the final R=0.0401 and wR=0.1380 for 1157 observed reflections (I > 2σ(I)).In the structure of the title compound,the Zn II ion located in an inversion center lies in a distorted tetrahedral environment at a N 2 O 2 coordination mode,and the 5-hydroxynicotinic acid ligand links symmetry-related Zn II ions at a μ 2-N,O bridging way forming a two-dimensional covalent structure.In the crystal,solvent water molecules form intermolecular O-H O hydrogen bonds and pyridine rings of adjacent layers form π-π stacking (3.346),which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.     

Hydrothermal Synthesis and Crystal Structure of a Znic(Ⅱ) Coordination Polymer Assembled by 4-Sulfophthalate and 4,4'-Bipyridine

A new organometallic coordinate polymer {[Zn2(4-sphth)2(4,4'-bpy)4(H2O)4][Zn(4,4'-bpy)2(H2O)4]}n·n[(4,4'-bpy)(H2O)4](4-sphth=4-sulfophthalic acid,4,4'-bpy = 4,4'-bipyridine) 1 has been hydrothermally synthesized and characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction.The complex crystallizes in monoclinic,space group C2/c with a=18.8659(13),b=23.0861(13),c=22.5449(14),β=107.4120(10)o,V=9369.3(10)3,Mr=1981.86,Dc=1.405 g/cm3,μ(MoKα)=0.891 mm-1,F(000)=4100,Z=4,the final R=0.0644 and wR=0.1615 for 5984 observed reflections(I 2σ(I)).Furthermore,compound 1 shows blue photoluminescent property at room temperature.