Synthesis,Crystal Structure and Photoluminescence of [Gd(C_6NO_2H_5)_3-(H_2O)_2]_(2n)·(nH_5O_2)(nHgCl_5)(2nHgCl_4)·(2nH_2O)

A heterometallic 4f-5d inorganic-organic metal-isonicotinato hybrid Gd(C6NO2H5)3-(H2O)22n·(nH5O2)(nHgCl5)(2nHgCl4)·(2nH2O) 1 has been synthesized via hydrothermal reaction and structurally characterized.Complex 1 crystallizes in the space group C2/c of monoclinic system with four formula units in a cell:a=24.234(8)=b=20.816(7)=c=15.333(3)=β=128.091(8)°=V=6088(3)3=C36H47Cl13Gd2Hg3N6O20=Mr=2260.92=Dc=2.467 g/cm3=S=0.896=μ(MoKα)=10.331 mm-1=F(000)=4216=R=0.0344 and wR=0.0629.The crystal structure analysis reveals that the title complex is characteristic of a one-dimensional chain-like structure.Photoluminescent investigation reveals that the title complex displays a broad and intense emission in the green region.     

Synthesis and Crystal Structure of an Unusual Dodecacoordinated Lanthanum Complex by Phenanthroline and Nitrate （phenH）_2[La（NO_3）_5（phen）]·CH_3OH

Lanthanum complex (phenH)2[La(NO3)5(phen)]·CH3OH (1, phen=phenanthroline) was synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a=20.3040(3), b=10.7091(1), c=19.0771(2), β=102.090(1)°, V=4056.07(8)3, Z=4, Dc=1.676 g/cm3, μ= 1.142 mm-1, F(000)=2056, the final R=0.0346 and wR=0.0793 for 9981 (Rint=0.0358) independent reflections. The mononuclear complex 1 consists of four parts: two phenH+ cations formed by the protonation of phen, one complex anion [La(NO3)5(phen)]2-, and one solvent methanol molecule. The complex anion contains one phen and five nitrate ligands which both chelate the center La(III) ion, adopting a distorted twelve-coordinated icosahedral geometry. The cations, anion and solvent molecule are linked together by hydrogen bonds. One of the protonated phenanthrolines (phenH+) acting as cation connects to the anion via N–H…O hydrogen bond directly, and the other one links to the anion through an intermediate solvent CH3OH via N–H…O and O–H…O hydrogen bonds. By the plentiful additional weak C–H…O intermolecular hydrogen bonds, the compound molecules construct a two-dimensional layer structure.     

Crystal Structure of Catena-poly-[2,2'-bisbenzimidazole Mn(Ⅱ)-μ-Benzene-1,3-dicarboxylato]

The title complex,[(BBI)Mn(BDC)]n 1(BBI = 2,2'-bisbenzimidazole(C14H10N4),BDC=benzene-1,3-dicarboxylate dianion(C8H10O4)),crystallizes in the monoclinic system,space group C2/c,with a=17.822(8),b=16.181(7),c=13.355(6),β=92.112(5)°,V=3848.67(304)3,Z=8,C22H14MnN4O4,Mr=453.31,Dc=1.565 g/cm3,F(000)=1848,μ=0.725 mm-1,S=1.000,the final R=0.0310 and wR=0.0589.1 contains hydrogen bonds and π-π stacking interactions between the neighboring aryl-ring of BBI's,which helps to form a three-dimensional crystal structure.     

Hydrothermal Synthesis,Crystal Structure and Antimicrobial Activity of a New Ni(Ⅱ) Complex

The title complex [NiL]·H2O(C20H24N2NiO5,L = paeonol-ehylenediamine) was synthesized by the hydrothermal method and characterized by IR,cyclic voltammetry and X-ray single-crystal diffraction.The complex belongs to the monoclinic system,space group P21/c with a=13.4361(13),b=7.3290(10),c=20.981(2),β=109.244°,V=1950.6(4)3,Z=4,F(000)=904,Dc=1.468 g/cm3,μ(MoKα)=1.029 mm-1,the final R=0.0588 and wR=0.1577.The complex exhibits antimicrobial activities(antimicrobial activities against Staphylococcus aureus and Escherichia codi) by agar diffusion measurement.     

Synthesis and Crystal Structure of Tetra（（8-quinolyl）-amido-N）ytterbium Bi（tetrahydrofuran-O）lithium

The treatment of the mixture of n-BuLi with 1 equiv.8-aminoquinoline in THF in situ,which reacted further with 1/3 equiv.of YbCl3 in THF,to give the homoleptic lanthanide amide ate complex Yb(NH-C9H6N)4Li(C4H8O)2(1).The crystal structure was determined by X-ray diffraction and the following crystallographic data were obtained:C44H44N8O2YbLi,Mr = 896.85,monoclinic,space group C2/c,a = 7.8384(16),b = 22.294(5),c = 22.668(5),β = 97.614(5)°,V = 3926.3(14)3,Z = 4,Dc = 1.517 g/cm3,F(000)= 1812,μ(MoKα)= 2.431 mm-1,R = 0.0542 and wR = 0.1523 for 3372 observed reflections with I > 2σ(I).The structure of molecule 1 consists of one ytterbium atom,one lithium atom,four 8-aminoquinoline ligands and two THF molecules.The ytterbium atom is coordinated by eight nitrogen atoms of four 8-aminoquinoline ligands,forming a distorted dodecahedral geometry.     

Synthesis and Crystal Structure of a New Complex （H3IDC）（Prz）0.5（H2O）

The compound （H3IDC）（Prz）0.5（H2O） （H3IDC = imidazole-4,5-dicarboxylate, Prz = piperazine） has been prepared from a hydrothermal approach and was characterized by IR analysis and X-ray diffraction. Its crystal structure consists of discrete 4,5-imidazole-dicarboxylate, H2O and piperazine molecules. The whole structural motif was assembled by three different non-covalent interactions of O-H…O, N-H…O and π-π stacking, which play an important role in packing the molecules. Interestingly, the connections between imidazole-4,5-dicarboxylate molecule and water molecule result in a helical polymeric chain. Crystal data for compound 1： monoclinic system, space group P21/c, a = 6.4600（13）, b = 19.910（4）, c = 6.9123（14） A^°, β = 94.26（3）°, V= 886.6（3） A^°^3, Z= 4, C7H10O5N3, Mr = 216.18.     

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 and Crystal Structure of a Zinc（Ⅱ）Complex with 2,2＇-Diphenic Acid and Benzimidazole Ligands

A new complex [Zn1.5(dpa)1.5(bim)]2n(dpa = 2,2-diphenic acid,bim = benzimida-zole)1 has been hydrothermally synthesized and structurally characterized by elemental analysis,IR,fluorescence spectrum and single-crystal X-ray diffraction.The complex crystallizes in monoclinic,space group C2/c with a = 18.773(8),b = 16.560(7),c = 16.417(9),β = 94.737(9)o,V = 5086(4)3,C56H36N4O12Zn3,Mr = 1153.00,Dc = 1.506 g/cm3,μ(MoKα)= 1.472 mm1,F(000)= 2344,Z = 4,the final R = 0.0573 and wR = 0.1164 for 2968 observed reflections(I > 2σ(I)).It exhibits a one-dimensional chain-like structure and shows luminescent property in the blue region.     

Synthesis and Crystal Structure of Diaquabis{2,4-dibromo-6-[(2-ethylaminoethylimino)methyl]-phenolato}nickel(Ⅱ) Dinitrate Diacetonitrile

The title mononuclear Schiff base nickel(Ⅱ) complex [Ni(C11H14Br2N2O)2(H2O)2]· 2NO3·2C2H3N was prepared and characterized by elemental analysis,IR spectrum,and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system,space group P21/n with a=15.534(2),b=7.647(1),c=16.435(2),β=103.252(2)o,V=1900.3(4)3,Z=2,Dc=1.750 g/cm3,Mr=1000.99,λ(MoKα)=0.71073,μ=4.776 mm-1,F(000)=996,the final R=0.0368 and wR=0.0724. A total of 3988 unique reflections were collected,of which 2764 with I > 2σ(I) were observed. The complex consists of a mononuclear [Ni(C11H14Br2N2O)2(H2O)2]2+ cation,two nitrate anions and two acetonitrile molecules. The Ni atom,lying on the inversion centre,is six-coordinated by two Schiff bases and two water molecules to assume an octahedral coordination geometry. The molecules in the crystal are linked through intermolecular hydrogen bonds of N–H…O,N–H…Br,O–H…O,O–H…N and C–H…O to form layers.     

Asymmetric Synthesis and Crystal Structure of （-）-N-[（3R）-3-Cyclohexyl]-3-phenylpropananoyl]bornane-10,2-sultam

The title compound (-)-N-[(3R)-3-cyclohexyl]-3-phenylpropananoyl]bornane-10,2sultam (C 25 H 35 NO 3 S,M r=429.60),a derivative of camphorsultam,crystallizes in the monoclinic space group P2 1 /c with a=10.3301(7),b=19.4040(13),c=11.8106(8),β=100.5580(10)°,V=2327.3(3) 3,Z=4,D c=1.226 g/cm 3,λ=0.71073,μ(MoKα)=0.165 mm-1 and F(000)=928.X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat form (Fig.1).The planes constructed by (C(4),C(5),C(6),C(7)) and (C(7),C(8),C(9),C(4)) form a dihedral angle of 69.5°.The C(1)-C(2)-C(3) plane forms dihedral angles to the aforementioned planes of 89.8(1) and 85.9(3)°,respectively.And molecules are linked via hydrogen bonding (C-H···N/O) interactions.     

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.     

Synthesis and Structural Characterization of a New 3D Lead Coordination Polymer with a Tetrazole-1-acetate Ligand

One new lead coordination polymer,[Pb(tza) 2 ] n (1,Htza=tetrazole-1-acetic acid) has been synthesized under hydrothermal conditions and characterized by elemental analysis,IR spectroscopy,thermogravimetric analysis (TGA),fluorescence spectra and single-crystal X-ray diffraction.Coordination polymer 1 is of monoclinic system,space group C2/c with a=15.4388(16),b=10.4039(11),c=8.3360(8),β=119.2070(10)°,V=1168.7(2)3,C 6 H 6 N 8 O 4 Pb,Z=4,M r=461.38,D c=2.622 g/cm 3,μ(MoKα)=14.463 mm-1,F(000)=848,the final R=0.0373 and wR=0.0904 for 2744 observed reflections with I > 2σ(I).1 is a 3D coordination framework built from Pb-carboxylate chains and the tetrazole nitrogen atoms of tza ligands.Furthermore,the luminescent property of 1 has also been investigated.     

Syntheses and Crystal Structures of Two Supramolecular Architectures:(H_2tfbdc)·(tfbdc)·(Hbipy)_2 and (tfbdc)·(H_2pz)(tfbdc=Tetrafluoroterephthalate,bipy=4,4'-Bipyridine,pz=Pyrazine)

Two new supramolecular compounds,2C 10 H 9 N 2 + ·C 8 HF 4 O 4 2-·C 8 H 2 F 4 O 4 /(H 2 tfbdc)· (tfbdc)·(Hbipy) 2 (1) and C 4 H 6 N 2 2+ ·C 8 HF 4 O 4 2-/(tfbdc)·(H 2 pz) (2),were synthesized and characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.Compound 1 crystallizes in the triclinic system,space group P1,with a=8.3453(12),b=10.1798(15),c=10.6626(16),α=87.591(2),β=74.047(2),γ=69.006(2)°,V=834.53(12) 3,D c=1.614 g/cm 3,F(000)=400,u=1.45 cm-1,Z=2,the final R=0.0353 and wR=0.1005 for 5882 observed reflections with I > 2σ(I);and compound 2 crystallizes in the monoclinic system,space group P2 1 /c,with a=10.471(4),b=5.4419(19),c=12.249(4),β=114.909(6)°,V=633(4)3,D c=1.669 g/cm 3,F(000)=320,u=1.63 cm-1,Z=2,the final R=0.0794 and wR=0.2923 for 3213 observed reflections with I > 2σ(I).Both compounds 1 and 2 crystallize as charge-transfer organic salts with the dianionic or neutral acid components lying at the inversion centers.Hbipy + cations and anionic acid in compound 1 are linked to form a chain by means of C-H···O hydrogen bonds.Adjacent chains are further extended into a two-dimensional layer network via N-H···O and O-H···N hydrogen bonds.In compound 2,the acid and base subunits are arranged alternately to generate a linear tape motif via N-H O hydrogen bonds;these tapes are further combined into a three-dimensional array with CdSO 4 topology via C-H O intermolecular hydrogen bonds.     

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.     

Synthesis,Structure,and Magnetic Property of One Novel Entangled Cobalt~Ⅱ-organic Compound

One novel entangled cobalt compound,{[Co 3 (nbta) 2 (4,4-bpy) 2 (H 2 O) 2 ](H 2 O) 2 } n (1,H 3 nbta=5-nitro-1,2,3-benzenetricarboxylic acid,4,4-bpy=4,4-bipyridyl),was prepared and characterized by X-ray diffraction,magnetism,elemental analysis,XPS,TGA and IR spectroscopy.The crystal of 1 crystallizes in monoclinic,space group Pc with a=13.0717(16),b=11.4167(14),c=15.9342(19),β=90.5190(10)o,V=2377.9(5)3,Z=2,C 48 H 36 Co 3 N 8 O 20,M r=1221.64,D c=1.706 g/cm 3,F(000)=1242 and μ(MoKα)=1.128 mm-1.The final R=0.0497 and wR=0.1461 for 4185 observed reflections with I > 2σ(I) and R=0.0721 and wR=0.1619 for all data.X-ray diffraction analyses revealed that Co(1) is linked by the nbta 3-ligands to form the ladder shape along the c axis,which is further extended into two-dimensional networks via the joint of Co(2) along the a axis.Moreover,these two dimensional motifs are interconnected by the 4,4-bpy bridges to form a complicated 3-D polymeric framework.Magnetic measurements revealed that compound 1 shows strong antiferromagnetic property.     

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.     

Two Polymorphs of the Inclusion Compound [（n-C4H9）4N] ＋（C13H9O3）-H2O

Two polymorphs of the inclusion compound [(n-C4H9)4N]+·(C13H9O3)-·H2O havebeen prepared and characterized by X-ray crystallography. Polymorph 1: triclinic P 1 , a =13.4982(2), b = 13.5743(2), c = 17.1996(2) , α = 67.045(1), β = 77.845(1), γ = 88.762(1)°, V =2830.43(7)3, Z = 4, R = 0.0491, wR = 0.1276; Polymorph 2: tetragonal P43, a = b = 13.53690(1) , c = 30.8491(8) , V = 5653.02(16)3, Z = 8, R = 0.0448, wR = 0.0984. In these two crystalstructures, the hydrogen-bonded ribbons built of 4,4 -dihydroxybenzophenone (DHBP, C13H10O3)anions and water molecules are orderly arranged to generate two-dimensional host layers, withtetrabutylammonium cations contained between the layers to form the sandwich-like inclusioncompounds. The structures of 1 and 2, which exist as two polymorphs, both display the similarpacking pattern and hydrogen-bond linking model.     

2-D Supramolecular Network and Photoluminescence of a Coupled 1,4-Dihydrylpyridine

A coupled 1,4-dihydrylpyridine compound(C40H48N2O10,1) has been synthesized.Its structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system,space group P21/c with a = 8.3300(2),b = 15.720(3),c = 14.480(3) ,β = 90.08(3)°,V = 1896.1(7) 3,Z = 2,Mr = 716.80,Dc = 1.255 g/cm3,and F(000) = 764.The structure was solved by direct methods and refined by full-matrix least-squares method to the final R = 0.0556 and wR = 0.1499(I > 2σ(I)).There exist several supramolecular motifs in the crystal structure.The compound exhibits strong photoluminescence in the solid state at room temperature.     

A Lanthanide-transition Metal Coordination Polymer：{[CuEu（Hbidc）_2（H_2O）_4]·H_2O}_n（H_3bidc=1H-benzimidazole-5,6-dicarboxylic Acid）

The title complex 1,{[CuEu(Hbidc)2(H2O)4]·H2O}n(H3bidc = 1H-benzimidazole-5,6-dicarboxylic acid),has been solvothermally synthesized and structurally characterized by single-crystal X-ray diffraction.Complex 1 crystallizes in triclinic,space group P1,with a = 7.791(2),b = 12.058(3),c = 12.109(3),α = 82.189(5),β = 72.407(5),γ = 89.184(4)°,V = 1073.7(5)3,C18H18CuEuN4O13,Mr = 713.86,Dc = 2.208 g/cm3,μ(MoKα) = 3.967 mm-1,F(000) = 700,GOOF = 0.950,Z = 2,the final R = 0.0531 and wR = 0.1068 for I > 2σ(I).Complex 1 possess a tape-like chain structure consisting of Eu2C8O4 and Cu2Eu2C18N4O4 metallic rings alternatively arranged and is the first 3d-4f heterometallic complex based on the 1H-ben-zimidazole-5,6-dicarboxylato ligand(Hbidc).Plenty of hydrogen-bonding and π...π stacking interactions connect the 1D chains to construct a 3D supramolecular architecture.