Synthesis, Crystal Structure and Biological Activity of N-(2,6-Difiuorobenzoyl)-N'-[5-(4-trifiuoromethylphenyl)-1,3,4-thiadiazol-2-yl] ure

The title compound N-(2,6-difluorobenzoyl)-N'-[5-(4-trifluoromethylphenyl)-1,3,4-thiadiazol-2-yl]urea(C17H9F5N4O2S, Mr = 428.34) has been synthesized by the reaction of 2-amino-5-(4-trifluoromethylphenyl)-l,3,4-thiadiazole with 2,6-difluorobenzoyl isocyanate, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 10.7316(13), b = 10.5617(13), c = 16.037(2) (A), β =106.408(2)°, V= 1743.6(4) (A)3, Z = 4, Dc = 1.632 g/cm3, μ = 0.260 mm-1, F(000) = 864, the final R = 0.0599 and wR = 0.1420 for 3467 observed reflections with I ＞ 2o(Ⅰ). The urea group, which adopts a planar configuration mediated by the intramolecular N-H…O hydrogen bond, is nearly coplanar with the thiadiazole and 4-trifluoromethylbenzene rings. The title compound was found to exhibit good fungicidal activity against Rhizoctonia solani and Botrytis cinerea.     

Syntheses and Crystal Structures of 3,5-Diiodo-salicylalidehyde and 3,5-Diiodo-salicylalidene-4-nitroaniline

The title compounds, C7H4I2O2 1 and C13H7I2N2O3 2, have been synthesized and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a = 9.802（2）, b = 13.867（3）, c = 7.364（2） A, β = 109.74（3）°, V= 942.1（3） A^3, Dc= 2.636 g/cm^3, C7H4I2O2, Mr= 373.90, F（000） = 672, μ = 6.627 mm^-1, Z = 4, R = 0.0459 and wR = 0.1018 for 1805 observed reflections （I 〉 2 σ（I））. Compound 2 belongs to the monoclinic system, space group P21/n with a = 9.015（2）, b = 12.024（2）, c = 14.072（3） A, β = 103.91（3）°, V = 1480.6（5） A^3, Dc= 2.216 g/cm^3, C13H7I2N2O3, Mr= 494.01, F（000） = 920, p = 4.255 mm^-1, Z = 4, R = 0.0777 and wR = 0.1757 for 2896 observed reflections （I 〉 2σ（I））. Compounds 1 and 2 were assayed for antibacterial activities against three Gram positive bacterial strains （B. subtilis, S. aureus and S. faecalis） and three Gram negative bacterial strains （E. coli, P. aeruginosa and E. cloacae） by MTr method. Fortunately, compound 2 is found to show potent antibacterial activity against these six bacterial strains.     

Synthesis and Crystal Structure of (E)2-(3'-Bromo-5'-chloro-salicylidene amino)-4-methyl Pyridine

A new Schiff base compound,2-bromo-4-chloro-6-[(4-methylpyridin-2-ylimino)me-thyl]phenol(C13H10BrClN2O),has been synthesized by the condensation of equimolar 3-bromo-5-chlorosalicylaldehyde and 4-methylpyridin-2-ylamine in a methanol solution.The compound Was characterized by elemental analysis,IR spectra,and single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21 with a=6.048(3),b=14.063(7),c=7.623(4)(A),β=97.703(7)°,Z=2,V=642.5(6)(A)3,Dc=1.683 g/cm3,Mr=325.59,λ(MoKa)=0.71073(A),μ=3.395 mm-1,F(000)=324,R=0.0370 and wR=0.0662.A total of 3879 reflections were collected,of which 1970 with,I＞2σ(I)were observed.As expected.the molecule adopts a trans configuration about the C=N double bond.The benzene and pyridine rings are nearly coplanar(mean deviation from the combined plane is 0.031(3)(A)),with their dihedral angle of 3.3(3)°.The preliminary biological tests show that the compound has excellent antibacterial activities.     

Synthesis and Crystal Structure of Tert-butyl 4-[(E)-4-(1,3 -Dioxo-1,3-dihydro-2H-isoindol-2-yl)-1-butenyl] Benzoate

1 INTRODUCTION Phthalimide and its derivatives are synthetic mate- rials, which are widely used as important chemical intermediates of biosensors[1] and many drugs such as Citalopran[2], luminal[3], Beta-Lactam[4] and the No. three generation quinolones[5], and they have been identified as active groups of some drugs and chemical luminescence reagents[6, 7]. Tert-butyl 4- [(E)-4-(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)-1- butenyl] benzoate is an intermediate of a new type of insulin sen…     

Synthesis,Crystal Structure and Biological Activity of a Novel Complex： Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-Triazole-yl）-6-chloro-pyridazine）

The title compound, Co（L）2（CH3OH）2Cl2 （L = 3-（1,2,4-triazole-yl）-6-chloro-pyridazine） 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018（3）, b = 9.832（5）, c = 9.921（5）A, a = 78.270（8）, β = 74.550（8）, γ = 83.807（8）°, V = 553.1（5）A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F（000） = 281,μ（MoKα） = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ（I）. The Co（II） ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt（II） complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.     

New 1- and 2-dimensional polymeric structures of cyanopyridine complexes of Ag(I) and Cu(I)

Polymeric transition metal chalcogenides have attracted much attention because of their possible unusual properties directly derived from their extended structures. The molecules n-cyanopyridine (n = 2, 3, and 4) and pyridine-3,4-dicarbonitrile are found to function as bidentate or monodentate (only pyridine nitrogen donor atom) ligands in the coordination of silver(I) and copper(I) ions, respectively. The mode of coordination depends on the anion and the crystallization conditions and has been elucidated in all cases by single-crystal X-ray crystallography. We report here the syntheses, structural characterization, and electrical properties of six new polymers, [Ag(2)(2-cyanopyridine)(2)(NO(3))(2)](n)(1), [Ag(4)(3-cyanopyridine)(8)(SiF(6))(2)(H(2)O)(2)](n) (2), [Ag(3-cyanopyridine)(2)(NO(3))](n)(3), [Ag(pyridine-3,4-dicarbonitrile)(2)(NO(3))](n)(4), [Cu(I)(4-cyanopyridine)(2)(SCN)](n)(5), and [Cu(I)(pyridine-3,4-dicarbonitrile)(2)(SCN)](n)(6). Compounds 1 and 2 exhibit novel two-dimensional networks, while 3-6 have one-dimensional chain structures, in which 3 is a single-stranded helix. Room-temperature conductivities of 1, 2, 4, and 6 have been measured and are 3.1 x 10(-)(7), 2.7 x 10(-)(7), 7.4 x 10(-)(6), and 4.3 x 10(-)(5) S.cm(-)(1), respectively. The effect of temperature on the conductivities has been investigated.     

Configuration Confirmation of Euphorbia Factor L1 by Single-crystal X-ray Diffraction

A 6,（17）-epoxylathyrol diterpenoid （（2S＊3S＊4R＊5R＊6S＊9S＊11S＊15R＊）-5,15-diacetoxy-3- phenylacetoxy-14-oxolathyra-6（17）,（12E）-diene-6（17）-epoxide） was isolated from the seeds of Euhporbia lathyris L. Its configuration was puzzled because of the incomplete X-ray results reported before. In this work, the atom connectivity and configuration were confirmed by single-crystal X-ray diffraction together with ESI-MS, ^1H-, and ^13C-NMR spectroscopy. The compound crystallizes in monoclinic, space group P21 with a = 11.386（1）, b = 8.2839（7）, c = 17.192（2） A, β = 108.305（2）°, Z = 2, V = 1539.5（2）A^3, C32H40O8, Mr = 552.64, Dc = 1.192 g/m^3, /7（000） = 592,μ（MoKα） = 0.085 mm^-l, T = 293（2） K, the final R = 0.0398 and wR = 0.0950 for 2057 observed reflections with Ⅰ 〉 2α（Ⅰ）. The molecule shows a tricyclic terpenoid skeleton, consisting of fused five-, eleven- and three-membered rings. The configuration at C（5） is R^＊ and that at C（6） S^＊.     

Synthesis and Crystal Structure of 1-（4-Bromobenzoyl）-3- [5-（E）-styryl-1,3,4-thiadiazol-2-yl]urea

1 INTRODUCTION 1,3,4-Thiadiazole derivatives represent an interes- ting class of compounds possessing broad spectrum biological activities[1~4]. Aroyl ureas are known to exhibit diverse biological effects, such as insecticidal, fungicidal, herbicidal and plant growth regulating activities[5~8]. Therefore, it is worthwhile to investi- gate the compounds incorporating both 1,3,4-thiadia- zole nucleus and aroyl urea group. In the previous paper[9], a series of aroyl ureas containing 1,3,4-t…     

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.     

Synthesis and Crystal Structure of 2,4-Diiodo-6-[(2-morpholin-4-yl-ethylimino)-methyl]-phenol-copper(Ⅱ)

2,4-Diiodo-6-[(2-morpholin-4-yl-ethylimino)-methyl]-phenol-copper(Ⅱ) has been designed and synthesized.The structure was determined by UV,IR and single-crystal X-ray study.The title complex crystallizes in the triclinic system,space group P1 with a=6.6090(13),b=10.377(2),c=12.550(3),α=113.29(3),β=93.84(3),γ=98.31(3)°,V=774.9(3)3,Dc=2.215g/cm3,C26H30CuO4N4I4,Mr=1033.68,F(000)=487,μ=4.726 mm-1,Z=1,the final R=0.0563 and wR=0.1475 for 2101 observed reflections(I2σ(I)).The central copper(Ⅱ) is four-coordinated by two nitrogen atoms and two oxygen atoms from two 3,5-diiodosalicylaldehyde-2-morpholinoethylamine Schiff bases.The complex is linked into a column by π-π stacking interaction.The complex was assayed for antibacterial activities against three Gram positive bacterial strains(B.subtilis,S.aureus and S.faecalis) and three Gram negative bacterial strains(E.coli,P.aeruginosa and E.cloacae) by MTT method.Fortunately,the title complex shows potent antibacterial activity against these six bacterial strains.     

Synthesis and Crystal Structure of 2-Hydroxybenzoic Acid [1-（3,5-Dibromo-2-hydroxyphenyl）methylidene]hydrazide Methanol

A new Schiff base compound, 2-hydroxybenzoic acid [1-(3,5-dibromo-2-hydroxy- phenyl) methylidene]hydrazide methanol (C14H10Br2N2O3·CH3OH), has been synthesized by the condensation of equimolar 3,5-dibromosalicylaldehyde and 2-hydroxybenzoic acid hydrazide in a methanol solution. The compound was characterized by elemental analysis, IR spectra, and single- crystal X-ray diffraction. The compound consists of a Schiff base moiety 2-hydroxybenzoic acid [1-(3,5-dibromo-2-hydroxyphenyl)methylidene]hydrazide and a lattice methanol molecule. The crystal belongs to the monoclinic system, space group P21/n with a = 7.183(1), b = 15.673(2), c = 15.001(2) , β = 98.345(2)o, Z = 4, V = 1670.9(4) 3, Dc = 1.773 g/cm3, Mr = 446.10, λ(MoKα) = 0.71073 , μ = 4.872 mm-1, F(000) = 880, R = 0.0458 and wR = 0.0963. A total of 3445 unique reflections were collected, of which 2236 with I > 2σ(I) were observed. As expected, the molecule adopts a trans configuration about the C=N double bond. The two benzene rings are nearly coplanar (mean deviation from the combined plane is 0.061(4) ), with the dihedral angle of 7.9(3)o. The preliminary biological tests show that the compound has moderate antibacterial activities.     

Two-dimensional Supramolecular Structure of a Mercury（Ⅱ） Iodide Complex with Organosulfide

A mercury（Ⅱ） iodide complex with organosulfide [Hg（pymt）（pymtH）I] 1 （pymt = the anion of pyrimidine-2-thiolate） has been synthesized by slow evaporation of the solution at room temperature and structurally characterized by single-crystal X-ray diffraction. Basic ideas and data collected are given. X-ray diffraction analysis reveals that complex 1 is mononuclear. Crystallographic data： C8H7HgIN4S2, Mr = 550.79, monoclinic system, space group P21/c, a = 11.218（4）, b = 9.551（3）, c = 15.877（4） A^°, β = 129.697（15）°, V = 1308.9（7） A^°^3, Z = 4, Mr = 550.79, Dc = 2.795 g/cm^3, F（000） = 995, μ（MoKa） = 14.415 mm^-1, 2（MoKa） = 0.71073 A^°, T= 293（2） K, 2θmax = 54.9°, GOOF= 1.053, the final R = 0.0310 and wR = 0.0742 for 2547 observed reflections with I 〉 2σ（I） （refinement on F^2）. Complex 1 is connected through hydrogen bonds to give a one-dimensional supramolecular chain structure. Furthermore, π-π interactions are also found between the pyrimidine rings with the center-to-center distances of 3.439（4） and 3.603（4） A^°, so complex 1 expands the chains into a two-dimensional network.     

Synthesis and Crystal Structure of （E）-N,N＇- dicyclohexyl- 1-（3-（3,4-dihydroxyphenyl）acryloyl）urea

The title compound, (E)-N,N′-dicyclohexyl-1-(3-(3,4-dihydroxyphenyl)acryloyl)- urea (DDA), has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy, ESI- MS, and X-ray single-crystal diffraction. Its crystallizes in monoclinic, space group C2/c with a = 20.483(12), b = 11.153(6), c = 21.134(12) , β = 117.098(7), V = 4298(4) 3, Z = 8, F(000) = 1664, Dc = 1.195 Mg/m3, Mr = 386.48, μ= 0.082 mm-1, the final R = 0.0474 and wR = 0.1370 for 4853 observed reflections with I > 2σ(I).     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Synthesis and Crystal Structure of 5-Methoxy- butyrolacto[3,4-b]-1-N-cyclohexylaziridine

1 INTRODUCTION The study of aziridine derivatives has been an ac-tive area in organic chemistry due to their interestingreactive properties and special structures[1～3]. Aziri-dine compounds contain unique nitrogen skeleton ofthree-membered heterocycle, which is widely presentin many natural products. They have been used toobtain a variety of biologically important moleculessuch as amino acids, amino alcohols, alkaloids, andβ-lactam antibiotics[2～4]. Although the synthetic routesto azir…     

Synthesis and Crystal Structure of a Heterometallic Chain Coordination Polymer:{[Ni_2Mn_2L_2(CH_3CH_2OH)(H_2O)]·CH_3OH·2H_2O}_n

A chain-like coordination polymer with the chemical formula of {[Ni2Mn2L2(CH3CH2OH)-(H2O)]·CH3OH·2H2O}n has been synthesized by the assembly reaction of K2NiL·H2O and Mn(OAC)2·4H2O with a 1:1 mole ratio in methanol,where OAC-=CH3COO-and H4L=2-hydroxy-3-[(E)-({2-[(2-hydroxybenzoyl)imino]ethyl}imino)methyl]benzoic acid.The crystal structure was determined by single-crystal X-ray diffraction analysis.It belongs to the triclinic system,space group P1,with a=9.9464(8),b=13.4718(11),c=14.3877(12),α=87.1930(10),β=85.4280(10),γ=74.6470(10)°,V=1852.4(3)3,Z=2,Dc=1.807g/cm3,Mr=1008.03,λ(MoKα)=0.71073,μ(MoKα)=1.794 mm-1,F(000)=1032,R=0.0527 and wR=0.1284(Ⅰ2σ(Ⅰ)).The compound exhibits a chain-like structure formed by dissymmetrical tetranuclear units.     

Synthesis and antimicrobial activity of N-(substituted)-N'-(2,3-dihydro-2-oxido-5-benzoyl-1H-1,3,2-benzodiazaphosphol-2-yl) ureas

N-(substituted)-N'-(2,3-dihydro-5-benzoyl-2-oxido-1H-1,3,2-benzodiazaphosphol-2-yl) ureas were synthesized by reacting 3,4-diaminobenzophenone (4) with different chlorides of carbamidophosphoric acids (3) in the presence of triethylamine at 40-45 degrees C. Their 1H-, 13C- and 31P-NMR spectral data are discussed. The title compounds were screened for antifungal and antibacterial activity against the fungi Aspergillus niger and Fusarium solani and bacteria Escherichia coli and Staphylococcus aureus. These compounds showed higher antibacterial activity when compared with antifungal activity.     

Synthesis,Crystal Structure and Antimicrobial Property of 4-Bromo-2-[(3-methypyridin-2-ylimino)methyl]phenol

The title Schiff base compound 4-bromo-2-[(3-methylpyridin-2-ylimino)me-thyl]phenol was prepared and structurally characterized by elemental analysis,IR spectrum,and single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/n,with a=4.4870(9),b=19.953(4),c=13.860(3)(A),β=93.13(3)°,V=1239.O(4)(A)3,Z=4,Dc=1.561g/cm3,C13H11BrN2O2,Mr=291.15,μ=3.302mm-1 and F(000)=584.The final refinement gave R =0.0608 and wR=0.1377 for 1329 observed reflections with I＞2σ(I).X-ray diffraction reveals that the non-hydrogen atoms in the compound are nearly coplanar,with the mean deviation of 0.0197 (A) from the plane.The molecule adopts an E configuration about the central C=N functional bond.The compound possesses moderate antimicrobial property.     

Synthesis, Crystal Structure and Biological Activities of 3-[2-（4-Fluoro-phenyl）-ethyl]-5- methyl-4-hydroxyl-4-methyl-7-methylsulfanyl. 3,4-dihydro-pyrido[4,3-d]pyrimidine-8-carbonitrile

The title compound, 3-[2-(4-fluoro-phenyl)-ethyl]-5-methyl-4-hydroxyl-4-methyl- 7-methylsulfanyl-3,4-dihydro-pyrido[4,3-d]pyrimidine-8-carbonitrile, has been prepared and dete- mined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 6.8754(8), b = 10.2617(12), c = 13.3491(16) , α = 93.163(2), β = 96.704(2), γ = 102.421(2)°, V = 910.35(19) 3, Z = 2, Mr = 370.44, Dc = 1.351 g/cm3, μ = 0.203 mm-1, F(000) = 388, the final R = 0.0573 and wR = 0.1497. X-ray analysis reveals that the pyridine and pyrimidine rings are almost coplanar.     

Luminescent homo- and heteropolynuclear platinum(II) chalcogenido aggregates based on [Pt2E2(P empty set N)4] units (E=S,Se)

A series of homodinuclear platinum(II) complexes containing bridging chalcogenido ligands, [Pt(2)(mu-E)(2)(P empty set N)(4)] (P empty set N=dppy, E=S (1), Se (2); P empty set N=tBu-dppy, E=S (3)) (dppy=2-(diphenylphosphino)pyridine, tBu-dppy=4-tert-butyl-2-(diphenylphosphino)pyridine) have been synthesized and characterized. The nucleophilicity of the [Pt(2)E(2)] unit towards a number of d(10) metal ions and complexes has been demonstrated through the successful isolation of a number of novel heteropolynuclear platinum(II)-copper(I), -silver(I), and -gold(I) complexes: [[Pt(2)(mu(3)-E)(2)(dppy)(4)](2)Ag(3)](PF(6))(3) (E=S (4); Se (5)) and [Pt(2)(dppy)(4)(mu(3)-E)(2)M(2)(dppm)]X(2) (E=S, M=Ag, X=BF(4) (6); E=S, M=Cu, X=PF(6) (7); E=S, M=Au, X=PF(6) (8); E=Se, M=Ag, X=PF(6) (9); E=Se, M=Au, X=PF(6) (10)). Some of them display short metal.metal contacts. These complexes have been found to possess interesting luminescence properties. Through systematic comparison studies, the emission origin has been probed.