Synthesis and Crystal Structure of a Ca~Ⅱ Coordination Polymer of H_2Adefovir (H_2Adefovir={[2-(6-Amino-9H-purin-9-yl)ethoxy]methyl}phosphonic Acid)

A Ca II coordination polymer of H 2 Adefovir (H 2 Adefovir={[2-(6-amino-9H-purin-9-yl)ethoxy]methyl}phosphonic acid),[Ca(H 2 O)(Adefovir)] n (1),has been synthesized via the reaction of Ca(OH) 2 and H 2 Adefovir under hydrothermal conditions.Complex 1 crystallizes in the monoclinic system,space group P2 1 /c with a=22.344(5),b=6.8505(14),c=8.0101(17),β=90.356(4)o,V=1226.0(4)3,M r=329.28,D c=1.784 g/cm 3,μ=0.672 mm-1,F(000)=680,Z=4,the final R=0.0296 and wR=0.0916 for 2295 observed reflections with I > 2σ(I).In the structure,the Ca II center is coordinated to the phosphate group of Adefovir anion,forming a 2D coordination layer,and such layers are linked into a 3D framework by hydrogen-bonding interactions between the adenine groups of Adefovir anion.     

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.     

A Novel 3D Silver-triazolate Coordination Polymer with 6.102 Topology: Synthesis, Crystal Structure and Phosphorescence

A novel three-dimensional (3D) silver(I) coordination polymer, namely [Ag2(dmtrz)2]n (1) (Hdmtrz=3,5-dimethyl-1H,1,2,4-triazole), was synthesized through diffusion method. 1 was characterized by elemental analysis, FT-IR spectroscopy, thermogravimetric analysis (TGA) and single-crystal X-ray diffraction. 1 crystallizes in the orthorhombic system, space group Iba2 with a=12.5026(10), b=7.6026(6), c=18.8981(17), V=1796.3(3)3, Z=6, Mr=407.98, Dc=2.263 g·cm-3, μ=3.252 mm-1, F(000)=1176, the final R=0.0304 and wR=0.0634 for 1310 observed reflections (I > 2σ(I)). In the structure of 1, silver(I) centers are triconnected to dmtrz ligands, forming the (3,3)-connected 3D coordination polymer with a 6.102 topology. The luminescence property of 1 was also studied in solid state at room temperature.     

Synthesis, Structure and Topological Analysis of a New Zinc（Ⅱ） Complex [Zn2（bptc）（bpe）（H2O）]n

A novel zinc coordination polymer,[Zn 2 (bptc)(bpe)(H 2 O)] n (1,H 4 bptc=3,3,4,4-benzophenonetetracarboxylate,bpe=1,2-bis(4-pyridyl) ethane),has been prepared under hydrother-mal conditions.The crystal structure is of monoclinic,space group C/2c with a=27.50(2),b=6.207(4),c=16.233(11),β=107.522(14)°,V=2642 (3)3,C 29 H 22 N 2 O 11 Zn 2,M r=705.27,Z=4,D c=1.773 g/cm 3,F(000)=1432,μ=1.887 mm-1,R=0.0421 and wR=0.1049 for 2594 observed reflections (I > 2σ(I)).X-ray single-crystal diffraction analysis shows that 1 features two-dimensional [Zn 2 (bptc)(H 2 O)] layers,which are further linked by the bpe ligands to give rise to a three-dimensional pillar-layered structure.According to the topology analysis,this framework can be simplified into a (4,6)-connected (4 4 ·6 2)(4 4 ·6 10 ·8) network.     

Crossed Ladders in a 2-D Mixed-ligand Lanthanide Coordination Polymer:Synthesis,Crystal Structure and Photoluminescence

A new metal-organic coordination polymer,[Ce(L 1)(L 2)(H 2 O)]·2H 2 O (1,H 2 L 1=2,6-dimethylpyridine-3,5-dicarboxylic acid,H 2 L 2=(E)-2,6-dimethyl-4-styrylpyridine-3,5-dicer-boxylic acid),has been synthesized and characterized by elemental analysis,IR,and X-ray single-crystal diffraction.Compound 1 crystallizes in triclinic,space group P1 and displays a two-dimensional coordination network structure.In 1,the relatively rare crossed ladders cons-tructed by mixed ligands organize a 2-D grid with the topology of (4 2 6) 2 (4 8 6 6 8),and the layers further build up a 3-D supramolecular architecture via interlaminar hydrogen bonds.     

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.     

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 ℃).     

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 μ1,1,3 Formic Bridging 3D Microporous Ni(Ⅱ) Complex

A μ1,1,3 formic bridging Ni2 complex [Ni3(HCOO)6·H2O]]n 1 has been synthesi-zed under hydrothermal conditions. The single-crystal X-ray diffraction analysis shows that 1 exhibits a 3D open microporous tube formed by covalent and coordination bonds. Complex 1 crystallizes in the monoclinic system, space group P21/c with a = 11.1487(13), b = 9.7763(11), c =17.9685(17) A, β= 126.948(6)°, C6H6Ni3O13, Mr = 462.02, V = 1565.2(3) A3 Z = 4, Dc= 1.961 g/cm3, μ = 3.630 mm-1, F(000) = 917.7, Rint = 0.0234, the final R = 0.0234 and wR = 0.0734 for 3469 observed reflections (Ⅰ>2σ(Ⅰ)).     

Zigzag-Ladder Structure Coordination Polymer Containing Supramolecular Capsules of Dinuclear Lanthanide Ions by p-Sulfonatothiacalix[4]arene

Two isomorphous 2D zigzag-ladder structure coordination polymers containing coordination supramolecular capsules are reported,which are built by trivalent lanthanide ions,pyridine N-oxide(PNO) and p-sulfonatothiacalix[4]arene(H4TCAS4-):[Ln2(PNO)2(H2O)10?(H2TCAS)2].[Ln2(H2TCAS)2(H2O)6(MeOH)2].2MeOH.12H2O(Ln = La,1;Nd,2).Crystal data for complex 1:C31H51La2NO33S8,Mr = 1500.03,triclinic system,P 1 space group,with a = 11.732(2),b = 15.007(3),c = 15.262(3),α = 78.05(3),β = 80.77(3),γ = 83.89(3)°,Z = 2,V = 2587.3(9)3,Dc = 1.925 g/cm3,μ = 2.051 mm-1,F(000) = 1500,the final R = 0.0300 and wR = 0.0823;and those for complex 2:C31H51Nd2NO33S8,Mr = 1510.69,triclinic system,P1 space group,with a = 11.719(2),b = 14.941(3),c = 15.157(3),α = 78.03(3),β = 80.84(3),γ = 83.95(3)°,Z = 2,V = 2555.9(9)3,Dc = 1.963 g/cm3,μ = 2.436 mm-1,F(000) = 1512,the final R = 0.0493 and wR = 0.1267.There are two coordination environments of lanthanide ions.One is bridged by two PNO molecules forming a dimeric Ln ion in the O,O'-μ2 mode.The dinuclear ions are shrouded by two H2TCAS6-ions through coordination interactions and hydrogen bonds.The other coordination mode of Ln ions is a zigzag 1D chain linked by up-down H2TCAS6-ions.By the coordination capsules,the complexes form 2D zigzag-ladder structure coordination polymers.     

一维链状银(Ⅰ)配位聚合物的合成、表征及晶体测定

采用水热法合成了1个配位聚合物[Ag₂(L)(LH)]NO₃·1.5H₂O(1,LH=2-(4-methoxyphenyl)-1H-imidazo[4,5-f][1,10]phenanthro-line),并对其进行了元素分析、红外光谱、热重表征和Ｘ射线单晶衍射测定。配位聚合物1属于单斜晶系,空间群为C2/c,晶胞参数为：a=2.733 8(6),b=1.580 7(3),c=1.736 0(4) nm,β=107.73(3)°,V=7.146(2) nm³,Z=4,293(2) K。在晶体中,2个Ag(Ⅰ)原子与来自于不同LH和L配体上的3个氮原子分别形成三配位的畸变的三角形构型。     

Preparation,Crystal Structure,Thermal Decomposition and Explosive Properties of K2（tza）2（H2O） （tza=Tetrazole-1-acetic Acid）

A new energetic compound based on the tetrazole-1-acetic acid (tza) and potassium(I) salt, K2(tza)2(H2O), was synthesized and characterized by elemental analysis and FT-IR spectrum. Its crystal structure was determined by single-crystal X-ray diffraction analysis. The results show that the crystal belongs to the orthorhombic system, space group Pna21 with a = 1.11972(17) nm, b = 0.46647(7) nm, c = 2.5158(4) nm, V = 1.3140(3) nm3, K2C6H8N8O5, Mr = 350.40 g·mol-1, Dc = 1.771 g·cm-3, μ(MoKα) = 0.759 mm-1, F(000) = 712, Z = 4, R = 0.023 and wR = 0.0527 for 2961 observed reflections (I > 2σ(I)). The K(I) cation is six-coordinated with four O atoms from three carboxylate groups, one O atom from one H2O molecule and one N atom from tetrazolyl ring, in which each tza is coordinated in a tridentate chelating bridging coordination mode. The thermal decomposition mechanism of the title complex was studied by DSC and TG-DTG techniques. Under nitrogen atmosphere at a heating rate of 10 K·min-1, the thermal decomposition of the complex contains one main exothermic process between 191.7 and 243.8 ℃ in the DSC curve. Its combustion heat was mensurated by oxygen bomb calorimetry. The non-isothermal kinetics parameters were calculated by the Kissinger's method and Ozawa-Doyle's method, respectively. The sensitivity properties of K2(tza)2(H2O) were also determined with standard methods, which was very sensitive to flame.     

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 synthesi- zed by the reaction of mellitic acid and Cu(CH3COO)2·H2O in the presence of base. Crystallogra- phic data for 1: C12H80O16Cu3, Mr = 598.80, orthorhombic, Pbcn, a = 8.4378(6), b = 10.0396(7), c = 17.6799(12) A, V = 1497.70(18) A3, Z = 4, Dc = 2.656 g/cm3,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.     

Two-dimensional Lanthanide Coordination Polymers Constructed from Ce3＋/pr3＋ Cation, Imidazole-4,5- dicarboxylate and in situ Generated Oxalate Anions

Two new lanthanide coordination polymers [Ln(C 5 H 2 N 2 O 4)(H 2 O) 2 (C 2 O 4) 0.5 ] n nH 2 O (Ln=Ce III (1) or Pr III (2);C 5 H 2 N 2 O 4=imidazole-4,5-dicarboxylate anion;C 2 O 4=oxalate anion) have been synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analyses and IR spectrum.Both compounds crystallize in monoclinic,space group P2 1 /c with a=7.5225(3),b=17.2416(6),c=8.6089(3),β=110.9610(10)°,V=1042.68(7)3,Z=4,C 6 H 8 N 2 O 9 Ce,M r=392.26,D c=2.499 g/cm 3,μ(MoKα)=4.414 mm 1,F(000)=752,the final R=0.0167 and wR=0.0412 for 1;a=7.4973(3),b=17.2113(8),c=8.5729(4),β=110.9440(10)°,V=1033.14(8)3,Z=4,C 6 H 8 N 2 O 9 Pr,M r=393.05,D c=2.527 g/cm 3,μ(MoKα)=4.764 mm 1,F(000)=756,the final R=0.0192 and wR=0.0455 for 2.X-ray diffraction analyses reveal that the lanthanide cations in compound 1 or 2 are linked by imidazole-4,5-dicarboxylate and in situ generated oxalate anions via Ln-O and Ln-N covalent bonds to form two-dimensional layered networks.The successful synthesis of compound 1 or 2 also indicates a crystallographic confirmation for the decomposition of curcumin to form oxalate anion under solvothermal conditions.     

Facile Synthesis and Crystal Structure of a Novel Cyanopyridine

The title compound 2-amino-4-(4-hydroxy-3,5-dimethoxyphenyl)-5-methyl-6-phenyl nicotinonitrile,C 21 H 19 N 3 O 3,was synthesized via four-component reactions between propio-phenone,malononitrile,syringaldehyde and ammonium acetate in ethanol under reflux without catalyst and characterized by IR,1 H NMR,13 C NMR,MS,EA and single-crystal X-ray diffraction.Single-crystal X-ray diffraction analysis shows that the compound is of monoclinic system,space group P2 1 /n with a=8.4600(17),b=17.139(3),c=13.408(3),β=107.06(3)°,V=1858.6(6)3,Z=4,M r=361.39,F(000)=760,μ(MoKα)=0.088 mm-1,D c=1.292 g/cm 3,λ=0.71073,the final R=0.0751 and wR=0.0938 for 3333 observed reflections with I > 2σ(I).The crystal packing of the title compound is stabilized by intermolecular hydrogen bonds.     

Synthesis and Crystal Structure of Methyl 3-（5- Bromo-1-ethyl-1H-indole-3-carbonyl）aminopropionate

Methyl 3-(5-bromo-1-ethyl-1H-indole-3-carbonyl)aminopropionate has been syn-thesized by the acylation of 5-bromo-3-trichloroacetylindole with β-alanine methyl ester,followed by alkylation with ethyl iodide,in 82.6% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of monoclinic,space group P2 1 /c with a=11.7927(8),b=14.9342(8),c=9.0060(5),β=101.558(6)°,V=1553.93(16)3,Z=4,D c=1.510 g/cm 3,λ=0.71073,μ(MoKα)=2.656 mm-1,M r=353.22 and F(000)=720.The structure was refined to R=0.0401 and wR=0.0825 for 1704 observed reflections with I > 2σ(I).In the crystal structure,intermolecular N(2)-H(2)···O(1) hydrogen bond and weak intermolecular bonds (C(1)-H(1) O(1) and C(10)-H(10B) O(2)) are formed,and π-π stacking also exists.     

Synthesis, Crystal Structure and Antibacterial Activity of a New Ternary Copper（Ⅱ） Complex with 2,6-Pyridinedicarboxylic Acid and 1,10-Phenanthroline

A new ternary copper(II) complex,[C 43 H 27 Cu 2 N 7 O 5 ]·[C 14 H 6 CuN 2 O 8 ]·6.5H 2 O,has been synthesized by the reaction of copper sulfate,2,6-pyridinedicarboxylic acid and 1,10-phenanthroline (phen),and characterized by elemental analysis,IR,UV and X-ray single-crystal diffraction.It crystallizes in triclinic,space group P1,with a=14.379(5),b=15.510(5),c=15.835(6),α=78.567(6),β=63.594(6),γ=81.287(6)°,V=3092.1(19)3,C 57 H 46 Cu 3 N 9 O 19.5,M r=1359.54,Z=2,D c=1.446 Mg/m 3,λ(MoKα)=0.71073,μ=1.101 mm-1,F(000)=1362,S=1.071,the final R=0.0718 and wR=0.11960 for 10705 observer reflections (I > 2σ(I)).The structure unit of the title complex consists of a mononuclear part and a di-nuclear part,and the three copper ions show three coordination modes.Each 6-coordinated geometry of the Cu atom is a distorted octahedral coordination geometry.The 3D supramolecular system is formed by the hydrogen bond O-H···O and π-π stacking interaction between neighboring single cells.The antibacterial activity of the title complex is also studied.     

A lvt‐type Framework [Cu2(tza)4]·ClO4·4H2O Derived from 1H‐tetrazole‐1‐acetic Acid

The reaction of 1H‐tetrazole‐1‐acetic acid (Htza) and perchloric acid with cuprous chloride with slow evaporation at room temperature gave a novel 3D porous Cu^II coordination polymer, [Cu₂(tza)₄] · ClO₄ · 4H₂O ( 1 ), (tza = tetrazole‐1‐acetate). The structure exhibits an unusual 3D microporous coordination framework built up by four coordinated Cu^II nodes and bidentate bridging tza ligands with lvt‐type topology. Furthermore, the magnetic properties of complex 1 were also investigated.     

Synthesis and Crystal Structure of [{Cd(hmbdc)(H2O)3}·2H2O]n

A novel coordination polymer [{Cd(hmbdc)(H2O)3}·2H2O]n (hmbdc=5-hydroxy- isophthalic acid) has been synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c, with a=9.599(3), b=18.699(5), c=7.557(2) (A), β= 108.198(4)°, V=1288.6(6) (A)3, Z=4, Mr=382.60, Dc=1.972 g/cm3, F(000)=760, μ=1.740, the final R=0.0555 and wR=0.0995 for 1732 observed reflections with Ⅰ ＞ 2σ(Ⅰ). The structural analysis shows that the intermolecular hydrogen bonds and π-π interactions result in a three-dimensional supramolecular framework.     

Synthesis,Crystal Structure and Thermal Property of a 2D Brick Wall Framework Constructed from a New Mononuclear Complex

One new coordination polymer with the chemical formula [CoCu2L2·K2·1.5C2H5OH]n(H4L = 2-hydroxy-3-[(E)-({3-[(2-hydroxybenzoyl)amino]propyl}imino)methyl] benzoic acid) has been synthesized based on the slow diffusion method,and characterized by IR spectroscopy,thermalgravimetric and X-ray diffraction analysis.It crystallizes in the monoclinic system,space group P21/n with a = 11.98860(10),b = 24.4279(3),c = 14.9008(2) ,β = 104.7490(10)°,V = 4220.01(8) 3,Z = 2,Mr = 1009.94,Dc = 1.590 g/cm3,F(000) = 2056,μ(MoKα) = 1.649 mm-1,the final R = 0.0411 and wR = 0.1178 for 5920 observed reflections with I 2σ(I).The compound possesses a 2D brick wall structure constructed from trinuclear units.