Synthesis,Crystal Structure and Electrochemical Property of the Ferrocenyl Schiff-base (E)-N’(Ferrocene Ethylidene)Picolino Hydrazide

A novel Schiff-base compound based on ferrocene C18H17OFeN3 (1) has been synthesized and characterized by X-ray diffraction. The title compound crystallizes in monoclinic, space group P21/c with a = 19.2343(17), b = 10.5084(9), c = 7.9373(7) , β = 97.7740°, Z = 4, V = 1589.6(2) 3, Dc = 1.451 g/cm3, μ(MoKα) = 0.956 mm-1, F(000) = 720, the final R = 0.0343 and wR = 0.0973 for 2759 observed reflections (I > 2σ(I)). Electrochemical measurements exhibit that compound 1 undergoes a reversible one-electron redox process.     

Synthesis,Crystal Structure and Biological Activity of N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N’-(4-methyl-1,2,3-thiadiazole)-5-formyl-N’-3,5-dichloropyridin-2-yl-diacylhydrazine

The title compound N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N'-(4-me-thyl-1,2,3-thiadiazole)-5-formyl-N'-3,5-dichloropyrid-2-yl-diacylhydrazines (C18H17Cl2N7O3S2, Mr = 514.41) has been synthesized by the reaction of N-tert-butyl-N'-3,6-dichloropyridine-2-formyl hydrazine with 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride and triethylamine, and its structure was characterized by 1H NMR, HR MS, and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 27.726(8), b = 11.045(3), c = 14.507(4), β = 96.758(4)°, Z = 8, V = 4412(2) 3, Dc = 1.549 g/cm3, μ = 0.521 mm-1, F(000) = 2112, R = 0.0405 and wR = 0.1153. X-ray analysis indicates that all rings are non-planar in this molecule. The bioassay results indicate that both the title compound and the positive control RH-5992 have weak fungicide activities, while the title compound has good insecticidal activity against Plutella xylostella L. and no insecticidal activity against Culex pipiens pallens.     

Synthesis and Characterization of （4R,5R）-1,3-dioxolance-4,5-bis（2-pyridineacrboxylic acid）

The title compound, (4R,5R)-1,3-dioxolance-4,5-bis(2-pyridineacrboxylic acid), has been synthesized and characterized by single-crystal X-ray diffraction, IR, NMR, and MS analyses. Crystal structure of the title compound was grown from ETOH by slow diffusion at room temperature. The title compound crystallizes in monoclinic, space group C2 with a = 17.805(3), b = 11.459(3), c = 11.1656(17) , β = 113.066(4)°, V = 2095.9(6) 3, Z = 4, F(000) = 880, Dc = 1.332 Mg/m-3, C23H20N2O6, Mr = 420.41 and μ = 0.10 mm-1     

Crystal Structure of Isoquinoline Derivatives

The chiral compound 5H-imidazol[2,3-b]isoquinoline-1-ethanol-5-one-1,2, 3, 10b-tetrahydro- β(S)-phenyl-3(S)-phenyl was synthesized from the direct condensation of 2-cyanophenyacetonitrile with optically active (S)-(+)-2-phenylglycinol in chlorobenzene under dry, anaerobic conditions. ZnCl2 was used as a Lewis acid catalyst in this reaction, and the structure of this compound was determined by X-ray diffraction, NMR, MS and IR. Crystal data of the title compound: C25H22N2O2, Mr = 382.45, P 21 21 21, a = 5.341(5), b = 16.735(5), c = 22.129(5) , γ = 90o, V = 1978(2) 3, Z = 4, Dc = 1.284 g/cm3, the final R = 0.0321 for 2269 observed reflections with I > 2σ(I) and Rw = 0.0771 for all data.     

Structure and Luminescence Property of a Hexanuclear Thiosemicarbazone Silver（I） Cluster

A new hexanuclear silver(I) compound containing thiosemicarbazones with groups of 1-naphthalene was synthesized and structurally characterized by single-crystal X-ray diffraction,elemental analysis and fluorescence spectrum.The title compound crystallizes in monoclinic,space group P2 1 /c with a=16.101(4),b=24.855(7),c=14.492(4),β=109.730(5)°,V=5459(3)3,C 90 H 102 Ag 6 N 24 O 6 S 6,M r=2455.54,D c=1.494 g/cm 3,μ(MoKα)=1.228 mm-1,F(000)=2472,Z=2,the final R=0.0761 and wR=0.1507 for 5258 observed reflections (I > 2σ(I)).In the structure,the S atom of ligand L serves as a triply bridged chelator to connect the six silver atoms into a Ag 6 L 6 cluster.Luminescence investigation reveals that the compound exhibits two ligand-independent cluster-centered electron transfer bands and one ligand-dependent charge transfer band.     

Synthesis and Crystal Structure of a New Macrocycle Based on Diethoxycarbonyl Glycoluril: C_(26)H_(30)N_6O_(10)

A new macrocycle based on diethoxycarbonyl glycoluril 3,C26H30N6O10,has been synthesized and characterized by single-crystal X-ray diffraction. It crystallizes in monoclinic,space group P21/c with a = 12.7291（10）,b = 25.157（2）,c = 8.5489（7） A,β = 104.4760（10）°,V = 2650.7（4） A^3,Z = 4,C26H30N6O10,Mr = 586.56,F（000） = 1232,T = 292（2） K,Dc = 1.470 g/cm^3,μ = 0.115 mm^-1,the final R = 0.0590 and wR = 0.1299 for 4918 observed reflections with I 〉 2σ（I）. In the structure of the title compound,a three-dimensional microporous architecture is formed via intermolecular hydrogen bonding interactions.     

Synthesis,Crystal Structure and Antibacterial Activity of （2E,3E）-N1,N2-Bis（2,3,4-trimethoxy-6-methylbenzylidene）ethane-1,2-diamine

The title compound （2E,3E）-N1,N2-bis（2,3,4-trimethoxy-6-methylbenzylidene）- ethane-l,2-diamine （C24H32N2O6, Mr = 444.52） was synthesized and characterized by elemental analysis, IR spectra and single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P2/c, with a = 8.5480（10）, b = 9.3710（12）, c = 15.280（2）A, β = 90.780（2）°, V= 1223.9（3）A3, Z = 2, Dc= 1.206 g/cm3, 2 = 0.71073A,μ（MoKa） = 0.087 mm^-1, F（000） = 476, the final R = 0.0680 and wR = 0.1450 for 2144 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that the molecule adopts an E configuration about the central C=N functional bond. The phenyl rings of two 2,3,4-trimethoxy-6-methylbenzaldehyde groups are symmetrically parallel. The molecules are linked through C-H…O hydrogen bonding interactions. The title compound possesses moderate antibacterial activity.     

Synthesis and Crystal Structure of （Z）-Ethyl-4-（4-methoxy）benzyndene-2-（3,5- dimethoxypheny-tetrahydrofuran-3,3-dicarboxylate

The title compound （Z）-ethyl-4-（4-methoxy）benzylidene-2-（3,5-dimethoxyphenyl）- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1, with a = 8.140（3）, b = 11.966（4）, c = 13.771（5）Aα= 67.366（4）, β= 85.165（5）, γ= 75.806（4）°, V = 1200.1（7） A3, Z = 2, C26H3008, Mr = 470.50, Dc = 1.302 g/cm^3, F（000） = 500,λ（MoKa） = 0.71073 A, μ= 0.096 mm^-1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections （I 〉 2σ（I））. As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.     

Synthesis and Crystal Structure of [2-Hydroxy- 5-（4-hydroxy-3-phenyliminomethylbenzyl）-benzylidene]-phenyl-amine

The title compound [2-hydroxy-5-（4-hydroxy-3-phenyliminomethyl-benzyl）-benzylidene]-phenyl-amine （C27H22N2O2, Mr = 406.47） was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 4.4026（6）, b = 1.501（13）, c = 0.95818（12） nm, β = 90.868（2）°, V= 4.2813（9） nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F（000） = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.     

Synthesis and Crystal Structure of an Interpentateing 3-D Framework Constructed from Mixed Ligands

A novel organic-inorganic hybrid compound constructed from mixed ligands, Co3（SIP）2（bipy）4（H2O）6·6.5H2O （H3SIP = 5-sulfoisophthalic acid, bipy = 4,4′-bipyridyl）, has been hydrothermally synthesized and characterized by IR, TGA and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 11.395（2）, b = 19.395（4）, c = 30.675（6） A^°, Mr = 1513.05, V= 6779（2） A^°^3, Dc= 1.482 g/cm^3, F（000） = 3120, μ = 0.873 mm^-1, Z= 4, the final R = 0.0439 and wR = 0.119 for 13421 observed reflections with I〉 2σ（I）. The structure of the compound presents a 3-D framework containing Co-bipy 1-D chain and 2-D bilayer motifs and carboxylate spacers, and the connection of 1-D chain and 2-D bilayer motifs by carboxylate ligand results in the final open framework with twofold interpenetration net. A probe reaction of the oxidation of benzaldehyde with H2O2 using the title compound as catalyst was carded out in a liquid-solid system, showing that the compound has high oxidative catalytic activity to the reaction.