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.     

Syntheses and Crystal Structures of Two Novel Spiro Compounds Containing 1,5-Dioxaspiro[5.5]undecane-2,4-dione

Two novel spiro compounds,3-benzylidene-1,5-dioxaspiro[5.5]undecane-2,4-dione 1 and 3-(2-fluorobenzylidene)-1,5-dioxaspiro[5.5]undecane-2,4-dione 2,have been synthesized and characterized by X-ray single-crystal diffraction,IR and elemental analysis.Compound 1 belongs to the monoclinic system,space group P21/n with a=12.326(3),b=5.6420(11),c=20.089(4),β= 101.79(3)o,C16H16O4,Mr= 272.29,V=1367.7(5)3,Z=4,Dc=1.322g/cm3,F(000)=576,μ(MoKa)=0.095 mm-1,the final R=0.0420 and wR=0.1159.Compound 2 is of monoclinic system,space group P21/n with a=12.283(3),b=5.6367(11),c=20.055(4),β=102.00(3)o,C16H15FO4,Mr=290.28,V=1358.2(5)3,Z=4,Dc=1.420 g/cm3,F(000)=608,μ(MoKa)=0.110 mm-1,the final R=0.0353 and wR=0.0860.     

Synthesis and Crystal Structure of a New Supramolecular Compound Constructed from Flexible 1,1'-(1,4-Butanediyl)bis(imidazole)and 1,2,4,5-Benzenetetracarboxylic Acid

A new bis(imidazolium) compound,[H2L(H2btec)2]·H4btec(1,L=1,1'-(butane-1,4-diyl)bis(imidazole),H4btec=1,2,4,5-benzenetetracarboxylatic acid),has been synthesized and structurally characterized by single-crystal X-ray diffraction.The title compound crystallizes in the monoclinic system,space group Pnma,with a=13.3908(11),b=13.9249(12),c=16.2166(14),V=2957.6(4)3,Z=4,Mr=698.55,Dc=1.569 mg/m3,F(000)=1448,μ(MoKα)=0.130 mm-1,the final R=0.0584 and wR=0.1538 for 4295 observed reflections with I>2σ(I).The compoun...     

Syntheses,Crystal Structures and Bioactivities of Two Isatin Derivatives

The title compounds(Z)-3-(2-(3-chloropyridin-2-yl)hydrazono)indolin-2-one(A) and 7-bromo-(Z)-3-((4-pyridinyl)carboxlichydrazono)-2-indolinone(B) have been synthesized and structurally determined by elemental analysis and single-crystal X-ray diffraction studies.Compound A(C13H8ClN4O) belongs to the orthorhombic crystal system,space group Pca21 with a = 20.799(4),b = 4.9312(10),c = 11.764(2),V = 1206.6(4)3,Mr = 271.68,Dc = 1.496 g/cm3,μ = 0.313 mm-1,F(000) = 556,Z = 4,the final R = 0.0346 and wR = 0.0831 for 2683 observed reflections with I > 2σ(I).Compound B(C14H9BrN4O2) belongs to the triclinic crystal system,space group P1 with a = 6.6834(13),b = 7.0727(14),c = 14.285(3),α = 95.56(3),β = 99.00(3),γ = 102.95(3)°,V = 643.8(2)3,Mr = 345.16,Dc = 1.780 g/cm3,μ = 3.203 mm-1,F(000) = 344,Z = 2,the final R = 0.0487 and wR = 0.1167 for 2334 observed reflections with I > 2σ(I).The preliminary herbicidal bioassay reveals that compounds A and B have some inhibition both in vivo and in vitro against AHAS.     

A Novel 3D Cobalt（II） Complex Constructed by 2,2＇-（1,4-Butanediyl）bis（1H-benzimidazole） Ligand

A novel 3D polymer 1 (C26H22CoN4O4, Mr = 513.41) constructed from H2C4BIm (2,2'-(1,4-butanediyl)bis(1H-benzimidazole)], 1,3-bdc (1,3-benzenedicarboxylate) and Co(II) has been successfully synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction analysis. The crystal belongs to the tetragonal system, space group I-42d with a = 24.315(5), b = 24.315(5), c = 8.343(2), V = 4933(2)3, Z = 8, Dc = 1.383 g/cm3, μ(MoKα) = 0.735 mm-1, F(000) = 2120, S = 1.156, the final R = 0.0596 and wR = 0.1346 for 1529 reflections with I > 2σ(I). Complex 1 contains 1D chains which are connected by extensive hydrogen-bonding interactions to form the 2D folded layer and 3D framework, which also stabilize the structure.     

Synthesis and Structure of Ethyl 3-acetamido-4-aryl-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylates

Two ethyl 3-acetamido-4-aryl-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylates(3) were synthesized with high diastereoselectivities and characterized by IR,NMR and MS.The configuration of 3a was confirmed by single-crystal X-ray diffraction,ethyl 3-acetamido-4-(4-nitrophenyl)-6-methyl-2-oxo-3,4-dihydropyran-5-carboxylate(3a),C17H18N2O7.The crystal is of orthorhombic,space group Pbca with a = 11.7781(16),b = 9.5979(10),c = 32.115(3),V = 3630.4(7)3,Z = 8,Mr = 362.33,Dc = 1.326 Mg/m3,λ = 0.71073,μ(MoKα) = 0.104 mm-1,F(000) = 1520,the final R = 0.0646 and wR = 0.1464 for 1788 observed reflections with I > 2σ(I).The N-H and oxygen atom are involved in intermolecular hydrogen bonds which link the molecules into a one-dimensional chain and stabilize the structure.     

A New Copper（Ⅰ） Iodide Coordination Polymer Incorporating Cu2I2 Double-stranded Stair: Synthesis,Crystal Structure and Luminescent Property

A new coordination compound, [(CuI)(Btd)]n(1, Btd=2,1,3-benzothiadiazole), was obtained at room temperature by the reaction of 2,1,3-benzothiadiazole with CuI and KI saturated aqueous solution. It was characterized by elemental analysis, IR spectroscopy, single-crystal X-ray diffraction analysis and photoluminescence. The complex crystallizes in the triclinic Pī space group, with a=4.1620(6), b=10.4590(15), c=10.5052(15), α=69.310(2), β=83.608(2), γ=78.873(2)o, V=419.30(10)3 , Z=2, C6H4N2SCuI, Mr=326.61, Dc=2.587 g/cm3 , F(000)=304 and μ(MoKα)=6.464 mm-1 . The final R=0.0418 and wR=0.0936 for 1451 observed reflections with I>2σ(I) and R=0.0422 and wR=0.0939 for all data. In the complex, the Cu atoms are coordinated by one nitrogen atom and three iodine atoms to form a double-stranded stair, and such stairs are further linked to build a 2D framework via C-H…I interactions.     

Synthesis and Crystal Structure of 1-Ethyl 3-Methyl 6-Benzyl-2-methyl-5-oxo-5,6-dihydropyrrolo[1,2-c]quinazoline-1,3-dicarboxylate

The crystal structure of the title compound(C24H22N2O5, Mr = 418.44) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group P21/c with a = 7.751(2), b = 12.392(4), c = 21.326(6), V = 2048.4(1)3, Z = 4, Dc = 1.357 g/cm3, F(000) = 880, μ(MoKα) = 0.096 mm-1, the final R = 0.0731 and wR = 0.1982 for 3335 observed reflections(I 2σ(I)). Intermolecular C(24)–H(24B)···O(1) hydrogen bond is observed in the structure.     

Crystal Structure and Conformation of an Imino Sugar

The title compound 3 was synthesized and characterized by IR,NMR and H-RMS,and its crystal structure was determined by X-ray diffraction analysis. The crystal is of monoclinic system (C16H23NO7S,Mr=373.41),space group P21,with a=12.000(2),b=5.5970(11),c=13.689(3),β=93.25(3)°,V=917.9(3)3,Z=2,Dc=1.351 g/cm3,F(000)=396,μ=0.213 mm-1,the final R=0.0489 and wR=0.0777 for observed reflections (I > 2σ(I)). Three intramolecular and three intermolecular hydrogen bonds were found. The absolute configuration of this molecule was confirmed by comparing with the original material.     

Synthesis and Crystal Structure of 3-Methyl-10-(4-nitrophenyl)-7,8,10,10a-tetrahydropyrano[4,3-b]chromene-1,9(4aH,6H)-dione

The title compound (C19H15NO6) was synthesized via a three-component reaction and characterized by means of IR and 1H NMR. Its crystal and molecular structures were determined by X-ray diffractometry. It belongs to the monoclinic system, space group P21/c with a = 11.670(3), b = 12.076(3), c = 11.613(3), β = 99.490(4)°, V = 1614.2(7)3, Mr = 353.32, Z = 4, Dc = 1.454 g/cm3, λ = 0.71073, μ = 0.110 mm-1, F(000) = 736, the final R = 0.0503 and wR = 0.1311. A total of 8454 reflections were collected, of which 3497 were independent (Rint = 0.0333) and 2102 were observed with I > 2σ(I).     

Synthesis,Characterization and Crystal Structure of 3-o-Fluorophenyl-6-（4-decarboxydehydroabietyl）-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole

Three novel 1,2,4-triazolo[3,4-b]-1,3,4-thiadiazoles were designed,synthesized and characterized by IR,NMR and APCI-MS.3-o-Fluorophenyl-6-(4-decarboxydehydroabietyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole(6a,C28H31FN4S) was structurally determined by single-crystal X-ray diffraction.The crystal belongs to the orthorhombic system,space group P212121 with a=6.0153(14),b=12.2577(19),c=34.055(3),V=2511.0(7)3,Z=4,Mr=474.63,Dc=1.255Mg/m3,λ=0.71073 ,μ(MoKα)=0.160 mm-1,F(000)=1008,the final R=0.0555 and wR=0.1248 for 3094 observed reflections with I2σ(I).There are six rings in the crystal structure of the title compound.The dihedral angle between 1,2,4-triazole and 1,3,4-thiadiaole rings is 1.4o,and that between 1,2,4-triazole and benzene ring D 25.5o.     

Syntheses and Crystal Structures of 1,5-Disubstituted 1,3,5-Hexahydro-triazine-2-（N-nitro）imines

The title compounds,C9H13ClN6O2S 1 and C15H17ClN6O2S 2,were synthesized and structurally characterized by elemental analysis,IR,1H NMR spectra and single-crystal X-ray diffraction.Compound 1 is in the monoclinic system,space group P21/c with a=13.7711(5),b=10.3883(4),c=9.7623(2),V=1344.47(8)3,Dc=1.506 g/cm3,C9H13ClN6O2S,Mr=304.76,F(000)=632,μ=0.448 mm-1,Z=4,S=1.084,R=0.0497 and wR=0.1328 for 2640 unique reflections(Rint=0.0787) with 2089 observed ones(I2σ(I)).Compound 2 belongs to the monoclinic system,space group P21/n with a=8.3828(5),b=14.5285(7),c=14.2456(4),V=1729.74(14)3,Dc=1.462 g/cm3,C15H17ClN6O2S,Mr=380.86,F(000)=792,μ=0.364 mm-1,Z=4,S=1.057,R=0.0598 and wR=0.1582 for 3384 unique reflections(Rint=0.0469) with 2833 observed ones(I2σ(I)).Compounds 1 and 2 are homologues and stabilized by intermolecular and intramolecular hydrogen bonds.Moreover,compound 2 containing C(2)-H(2)…π(thiazole) interaction is more stable than 1.     

Syntheses and Crystal Structures of Two New Ag(Ⅰ) Complexes with Betaine Derivative: Structure Changes via Metal-to-ligand Ratio

Two new Ag(I) complexes {Ag2(L)(NO3)(H2O)}n(1) and {Ag(L)}n·nH2O(2) have been synthesized via the reaction of silver nitrate and betaine derivative 1-carboxymethylpyridinium-3-carboxylate(L) by only changing the metal-to-ligand ratio. The results of X-ray crystallographic analysis indicate that complexes 1 and 2 both crystallize in the monoclinic space group P21/c with a = 5.0809(14), b = 17.390(5), c = 13.399(4), β = 91.677(5)o, V = 1183.4(6)3, Z = 4, Mr = 475.90, Dc = 2.671 g/cm3, F(000) = 912, μ = 3.352 mm-1, S = 1.259, the final R = 0.0320 and wR = 0.0831 for 2036 observed reflections with I 2σ(I) for 1 and a = 12.180(2), b = 5.0283(10), c = 14.396(3), β = 94.87(3)o, V = 878.5(3)3, Z = 4, Mr = 306.02, Dc = 2.314 g/cm3, F(000) = 600, μ = 2.294 mm-1, S = 1.053, the final R = 0.0283 and wR = 0.0684 for 2011 observed reflections with I 2σ(I) for 2. Complexes 1 and 2 both feature a unique 2D structure. For 1, the 2D undulated network consists of 1D infinite helical chains running parallel to the b axis, while for 2, the 2D network is made up of 1D tubes along the b axis. Moreover, the Ag…Ag interactions in complexes 1 and 2 are also discussed.     

Synthesis and Hydrogen-bonded Interpenetrating Grid Structure of 5,5＇-Bis [4- （2-hydroxyethyl）phenyl] diazo-dipyrromethane

A new 5,5'-bisdiazo-dipyrromethane compound 3 has been synthesized and cha- racterized. The crystal of 3 is of orthorhombic, space group Iba2 with a = 19.1914(17), b = 9.8396(8), c = 13.7643(12) , V = 2599.2(4)3, Z = 4, C29H34N6O2, Mr = 498.62, Dc = 1.274 g/cm3 , F(000) = 1064, μ(MoKα) = 0.083 mm-1, the final R = 0.0302 and wR = 0.0786 for 6361 observed reflections with I > 2σ(I), and R = 0.0320 and wR = 0.08006 for all data. It reveals that the molecules of compound 3 assemble into grid structures through a R22(7) type hydrogen bonding motif between azopyrrole and hydroxyl group. The grids interpenetrate each other with the assistance of C-H···π interaction.     

Synthesis and Crystal Structure of (1R,2S,3S,4S)-(6-O-Acetyl-1,2-O-isoproplidene-3,5-dideoxy-α-D-glucofuranoso)-1,3,5-trihydro-2,3-oxathiaindene-2,2-dioxide

(1R,2S,3S,4S)-(6-O-Acetyl-1,2-O-isoproplidene-3,5-dideoxy-α-D-glucofuranoso)-1,3,5-trihydro-2,3-oxathiaindene-2,2-dioxide(C11H16O8S,Mr=308.30) was synthesized and structurally characterized by NMR,MS and single-crystal X-ray diffraction.It belongs to the triclinic system,space group P1 with a=7.0836(14),b=10.832(2),c=14.895(3),α=96.01(3),β=98.85(3),γ=108.59(3)o,V=1055.8(4)3,Z=3,Dc=1.455g/cm3,F(000)=486,μ=0.264mm-1,the final R=0.0360 and wR=0.0712.It is a tricyclic sultone derivative composed of three five-membered rings.     

Synthesis and Crystal Structure of 2,10-Di-tert-butylindolo[3,2,1-jk]carbazole

The title compound, 2,10-di-tert-butylindolo[3,2,1-jk]carbazole (C26H27N, Mr=353.49), has been synthesized by palladium-catalyzed intramolecular arylation and characterized by 1H NMR, 13C NMR and X-ray crystal structure determination. The crystal crystallizes in the monoclinic system, space group P21/c with a=13.6409(5), b=11.6706(4), c=13.1678(5), β=100.6180(10)°, V=2060.39(13)3 , Z=4, Dc=1.140 mg/m3 , μ=0.065mm-1 , F(000)=760, the final R=0.0456 and wR=0.1209 for 3012 observed reflections (I > 2σ(I)).     

A Mn(Ⅱ) Coordination Polymer with the Flexible Tripodal Ligand 1,3,5-Tris-(imidazol-1-ylmethyl)benzene

A new Mn(Ⅱ) coordination polymer {[Mn(timb)2(H2O)2]·(Cl)2·(H2O)2}n(1,timb = 1,3,5-tris-(imidazol-1-ylmethyl)benzene) has been synthesized and characterized by elemental analysis,IR,TG and single-crystal X-ray diffraction.The title compound crystallizes in the triclinic system,space group P1 with a=9.0774(13),b=9.8720(15),c=11.4898(16),α=93.378(3),β= 95.471(3),γ=101.101(3)°,V=1002.6(3)3,Mr=834.67,Dc=1.382 g/cm3,μ(MoKα)=0.517mm-1,F(000)=435,GOF=0.986,Z=1,the final R=0.0506 and wR=0.1139 for 3517 observed reflections I2σ(I).It consists of one-dimensional double stranded chains formed through bridging bidentate timb ligands,and these chains are further connected to yield a 3D supramolecular framework by hydrogen bonding interactions and π…π stacking interactions.     

Synthesis, Structural Features and Evaluation of Antibacterial Activities of Two Schiff Bases Derived from 3,4-Dihydroxybenzhydrazide

A new Schiff base compound (I), (E)-N'-(2-hydroxy-3-methoxybenzylidene)-3,4-dihydroxybenzohydrazide-ethanol-water (1/1/1), has been synthesized and characterized by elemental analysis, IR spectra, and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 7.459(4), b = 18.316(10), c = 13.638(7), β = 101.585(9)o, V = 1825.2(17)3, Z = 4, μ = 0.104 mm-1, Dc = 1.333 g/cm3, F(000) = 776, the final R = 0.0635 and wR = 0.1302 for 3216 observed reflections with I 2σ(I). Another compound (Ⅱ), (E)-N'-(2,5-dimethoxybenzylidene)-3,4-dihydroxybenzohydrazide-ethanol-water (1/1/1), has been synthesized and reported before. The antibacterial activities of these two compounds against seven bacteria were first evaluated, and one compound showed considerable antibacterial activity against S. aureus.     

X-ray Diffraction Investigation of Ethyl 2-（2-Amino-3-ethoxycarbonyl-4H-benzo[f]chromene-4-yl） Cyanoacetate

The title compound,ethyl 2-(2-amino-3-ethoxycarbonyl-4H-benzo[f]chromene-4-yl) cyanoacetate 4,has been synthesized and its crystal structure was characterized by X-ray single-crystal diffraction.The crystal belongs to monoclinic,space group P21/n with a=12.9408(18),b=11.1870(13),c=13.8975(19),β=109.261(2)°,Z=4,C21H20N2O5,Mr=380.39,V=1899.3(4)3,Dc=1.330 g/cm3,μ=0.096 mm-1,F(000)=800,S=1.027,R=0.0535 and wR=0.1012 for 1365 observed reflections(I 2σ(I)).X-ray analysis reveals N-H…π interactions,π…π interactions and hydrogen bonds in the title molecule.     

Catena-dichloro(4,4′-dimethyl-2,2′-bipyridine)Cadmium(Ⅱ),a New One-dimensional Chain with Blue Fluorescent Emission

A new μ-chloro-bridged one-dimensional coordination polymer Cd(dmbpy)Cl2n(dmbpy=4,4′-dimethyl-2,2′-bipyridine) has been synthesized and structurally characterized by elemental analyses=IR=UV spectra and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic system=space group C2/c with a=17.745(4)=b=10.326(2)=c=7.3382(15)=β=106.85(3)o=V=1286.9(4)3=Z=4=C12H12N2Cl2Cd=Mr=367.54=Dc=1.897 g/cm3=F(000)=720=λ(MoKα)=0.71073=μ=2.089 mm-1=R=0.0368 and wR=0.1048 for 1041 observed reflections(I > 2σ(I)).Cadmium(II) adopts a distorted octahedral coordination geometry and adjacent coordination chains are intercalated in a zipper-like fashion into 2D layers through the π-π stacking interactions between dmbpy.Fluorescent