Syntheses and Crystal Structures of 3-Chloro-N＇-（3,5-dichloro-2-hydroxybenzylidene）-benzohydrazide and Its Oxovanadium（V） Complex with Antimicrobial Activity

A hydrazone compound 3-chloro-N'-(3,5-dichloro-2-hydroxybenzylidene)benzo-hydrazide(H2L) derived from the condensation of 3,5-dichlorosalicylaldehyde with 3-chloro-benzohydrazide and its oxovanadium(V) complex [VOL(CH3OH)(OCH3)] have been successfully prepared and characterized by physico-chemical methods and single-crystal X-ray diffraction.The hydrazone ligand coordinates to the V atom through the phenolate O,imine N,and enolic O atoms.The V atom is hexa-coordinated in a distorted octahedral geometry.The antimicrobial activities(MIC) of the hydrazone ligand and the oxovanadium(V) complex have been evaluated against the bacteria Staphylococcus aureus,Baccilus subtilis,Pseudomonas aeruginosa,and Escherichia coli.     

Syntheses,Crystal Structures,and Antimicrobial Activities of 3-Bromo-N＇-（2- chloro-5-nitrobenzylidene）benzohydrazide and 3-Bromo-N＇-（4-nitrobenzylidene）benzohydrazide

Two new hydrazone compounds, 3-bromo-N'-(2-chloro-5-nitrobenzylidene)-ben- zohydrazide 1 and 3-bromo-N'-(4-nitrobenzylidene)benzohydrazide 2, have been synthesized and characterized by elemental analysis, IR spectra, 1H NMR, and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a=7.7924(10), b=24.490(3), c=7.8989(9) , β=94.987(6)°, V=1501.7(3) 3, Z=4, R=0.0345 and wR=0.0739. Compound 2 crystallizes in monoclinic, space group P21/c with a=7.4099(11), b=24.868(4), c=8.3255(12) , β=112.796(8)°, V=1414.3(4) 3, Z=4, R=0.0744 and wR=0.1912. Both compounds display E configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N-H…N and N-H…O hydrogen bonds, forming chains running along the c axis. In the crystal structure of 2, molecules are linked through N-H…O hydrogen bonds, forming chains running along the c axis. The preliminary antimicrobial activities were studied.     

Synthesis and Crystal Structure of 2-(4-Nitrophenyl)-1,2-benzisoselenazol-3(2H)-one DMF (1:1) Solvate

The title compound (C13H8N2O3Se-C3H7NO) has been synthesized by a simple synthetic route and by recrystallization from DMF. The molecular structure of this compound was obtained by single-crystal X-ray diffraction. The compound crystallized in the triclinic space group P with a = 7.450(6), b = 8.150(7), c = 13.859(12) , α = 75.014(14), β = 83.072(18), γ = 84.409(14)°, V = 805.0(12)3, Z = 2 and R = 0.0271 for 2575 observed reflections with I > 2σ(I). X-ray analysis reveals that not only intermolecular Se…O and C-H…O interactions, but also π…π stacking interactions exist in the adjacent molecules. The above three kinds of intermolecular interactions extend the complex into an infinite three-dimensional layered network.     

Syntheses,Crystal Structures and Antibacterial Activities of 5-Chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic Acid and Its Copper(Ⅱ) Compound

The title compounds 5-chloro-3-methyl-1-phenyl-1H-pyrazole-4-carboxylic acid(C11H9Cl N2O2, HL)(1) and [Cu(L)2(H2O)](2) were prepared and structurally characterized by elemental analysis, IR and single-crystal X-ray diffraction. Compound 1(C11H9Cl N2O2) crystallizes in the monoclinic system, space group P21/n with a = 7.249(3), b = 20.515(10), c = 7.249(3),β= 96.30°, V = 1071.6(9) ?3, Z = 4, Mr = 236.65, Dc = 1.467 g/cm3, F(000) = 488, GOOF = 1.029, μ= 0.341 mm-1, the final R = 0.0736 and w R = 0.1966 for 1500 observed reflections with I 2σ(I). Compound 2(C22H18Cl2Cu N4O5) crystallizes in the monoclinic system, space group P21/c with a = 7.2931(6), b = 24.548(2), c = 13.2726(11), β= 99.4040(10)°, V = 2344.2(3) ?3, Z = 4, Mr = 552.84, Dc = 1.566 g/cm3, F(000) = 1124, GOOF = 1.050, μ= 1.201 mm-1, the final R = 0.0376 and w R = 0.1000 for 3626 observed reflections with I 2σ(I). 1 and 2 are connected through hydrogen bonding interactions to generate 2D and 3D supramolecular structures, respectively. Moreover, the preliminary antibacterial activities of 1 and 2 against the gram positive bacteria(S. aureus, C. albicans and B. subtilis) and gram negative bacteria(E. coli and P. aeruginosa) have been tested by using the microdilution method, and the results indicate that 2 is more active than 1 against the tested bacteria.     

Syntheses and Crystal Structures of Molybdenum-Sulfur Clusters Mo_3S_4 (dtp)_3(o-CH_3OC_6H_4COO)(Py) and Mo_3S_4 (dtp)_3(p-HOC_6H_4COO)(DMF)·EtOH

1 INTRODUCTION Recent years have seen a drastic increase of compounds containing the Mo3S4 core. A major synthetic route to these compounds is by the reaction of the aqua ion [Mo3S4(H2O)9]4+ with different kinds of ligands replacing some or all of the water molecules. In this way, Mo3S4(dtp)4(H2O), which was synthesized by the spontaneous- assembly method in 1986[1] and its structural characterization and chemical reactivity have been well recognized [2], can be rationally synthesize…     

Synthesis and Crystal Structure of （5-Hydroxy-6-methoxybenzofuran- 3-yl）-（4-methoxyphenyl）methanone

Compound 1 (5-hydroxy-6-methoxybenzofuran-3-yl)(4-methoxyphenyl)methanone, C17H14O5 , as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to (5,6-dihydroxybenzofuran-3-yl)(4-methoxyphenyl)methanone (2). The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/n, a=8.908(6), b=10.505(7), c=15.452(11), β=105.043(9)°, V=1396.4(16)3 , Z=4, F(000)=624, Dc=1.419 g/cm3 , μ=0.105 mm1, R=0.0513 and wR=0.1246 for 14459 independent reflections (Rint=0.0647) and 2488 observed ones (I>2σ(I)). Intermolecular O-H···O and π-π stacking interactions contributed to the stability of the structure.     

Synthesis and Crystal Structure Analysis of 5′-O-Tosyl-2,3′-anhydrothymidine

In this paper=5′-O-tosyl-2,3′-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system=space group P1=with a=5.397(2)=b=6.1886(18)=c=3.507(5) =α =87.74(2)=β =89.84(4)=γ =73.79(2)°=C17H18N2O6S=Mr=378.39=Z=1=V=432.8(3)3=Dc=1.452 g/cm3=F(000)=198 and Flack =-0.11(14). No intermolecular hydrogen bonds exist in the crystal=and the angle between benzene ring and pyrimidine planes is 32.23°.     

Syntheses and Crystal Structures of Two New Nickel（Ⅱ） Complexes with Salicylidene-2-ethanolamine

Two new Schiff base complexes of nickle(Ⅱ) [C18H20NiN2O4]·1.5H2O(1) and [C18H20N2NiO4]·H2O(2) were synthesized and characterized by elemental analysis,IR,UV-Vis and X-ray crystal structure analysis.Both 1 and 2 crystallize in the orthorhombic system.Crystal 1:space group Pbcn with a = 12.8591(19),b = 14.779(2),c = 19.749(3) ,V = 3753.3(10) 3,C18H23N2NiO5.5,Mr = 414.07,Z = 8,Dc = 1.445 g/cm3,μ = 1.067 mm-1,F(000) = 1712,S = 1.037,the final R = 0.0741 and wR = 0.2101 for 4353 observed reflections(I > 2σ(I)) and R = 0.1157 and wR = 0.2380 for all data.Crystal 2:space group P21 with a = 9.4673(17),b = 11.559(2),c = 16.347(3) ,V = 1788.9(6) 3,C18H22N2NiO5,Mr = 405.07,Z = 4,Dc = 1.497 g/cm3,μ = 1.116 mm-1,F(000) = 840,S = 1.085,the final R = 0.0330 and wR = 0.0869 for 3151 observed reflections(I > 2σ(I)) and R = 0.0362 and wR = 0.0887 for all data.Each Ni atom of 1 and 2 is six-coordinated with two nitrogen atoms and four oxygen atoms from two salicylidene-2-ethanolamine ligands yielding a distorted octahedral geometry.Dimer structure is observed in the packing diagram of 1.The thermal stability of complex 2 is also studied.     

Synthesis,Characterization and Antitumor Activities of Co,Ni, Cu,Zn Complexes with 1,4,7,10-tetrakis(4-nitrobenzyl)-1,4,7,10 tetraazacyclododecane Macrocyclic Ligand

１　ＩＮＴＲＯＤＵＣＴＩＯＮＣｙｃｌｅｎｄｅｒｉｖａｔｉｖｅｓｃｏｎｔａｉｎｉｎｇｆｏｕｒｎｅｕｔｒａｌｐｅｎｄｅｎｔｇｒｏｕｐｓａｒｅｅｆｆｅｃｔｉｖｅｌｉｇａｎｄｓｆｏｒｌａｎｔｈａｎｉｄｅａｎｄｔｒａｎｓｉｔｉｏｎｍｅｔａｌｉｏｎｓ〔１～４〕．ＴｈｅｙｃａｎｂｅｕｓｅｄａｓｃａｔａｌｙｓｔｓｆｏｒＲＮＡｔｒａｎｓｅｓｔｅｒｉｆｉｃａｔｉｏｎ〔５〕ｏｒｆｏｒｃｌｅａｖａｇｅｏｆｐｈｏｓｐｈａｔｅｅｓｔｅｒｓ〔６〕ｏｒｐｈｏｓｐｈｏｒｉｃａｎｈｙｄｒｉｄｅ〔７〕．Ｓｏｍｅｏｆｔｈｅｍｈａｖｅｂ…     

Synthesis and Crystal Structure of N,N′-Bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]-propane-1,3-diamine

The title compound,N,N′-bis-[3-chloro-5-S-(l-menthyloxy)-2(5H)-4-furanon-yl]-propane-1,3-diamine(C31H48Cl2N2O6,Mr = 615.61),has been synthesized and characterized by IR,1H NMR,MS,elemental analysis and single-crystal X-ray diffraction.The crystal crystallizes in the monoclinic system,space group C2 with a = 16.1091(4),b = 11.1880(3),c = 19.2854(5) ,β = 106.297(2)°,V = 3336.12(15) 3,Z = 4,Dc = 1.226 mg/m3,μ = 0.237 mm-1,F(000) = 1320,the final R = 0.0531 and wR = 0.0700 for 2760 observed reflections(I > 2σ(I)).X-ray analysis reveals that the title compound possesses four rings:two chiral five-membered furanone rings and two six-membered cyclohexane rings with chair conformation,containing eight chiral centers:C2(S),C3(R),C5(R),C10(S),C18(S),C21(R),C22(S) and C25(R).The structure is stabilized by N-H…O hydrogen bonding interaction.     

Synthesis, Crystal structure and Antioxidant of 3,5-Dihydroxy-N＇-（5-bro-2-hydroxybenzylidene） benzohydrazide Hydrate

A new compound, 3,5-dihydroxy-N′-(5-bro-2-hydroxybenzylidene)benzohydrazide hydrate, has been synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in a monoclinic system, space group P21/c with a = 14.267(6), b = 8.079(4), c = 13.157(6) , β = 108.114(4), Z = 4, V = 1441.4(11) 3, Dc = 1.701 g/cm3, F(000) = 744.0, μ = 2.878 and S = 1.021. The final R = 0.0457 and wR = 0.1149 for 3500 observed reflections with I > 2 (I). The ability with which the compound scavenges free radicals of ABTS and DPPH, IC50, is 34.13 and 101.6 μM, respectively.     

Synthesis and Crystal Structure of 2-（1-Naphthalenylamino）-4-thiazolidinone

The compound 2-(1-naphthalenylamino)-4-thiazolidinone was synthesized by the reaction of 1-(naphthalene-1-yl)thiourea with ethyl chloroacetate in an ionic liquid, and its structure was characterized by IR, 1H NMR and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group P21 /c with a=10.0081(3), b=14.5312(4), c=7.8739(2) , β=99.425(3)°, Z=4, V=1129.64(5)3 , Dc=1.425 g/cm3 , μ=0.269 mm-1 , F(000)=504, the final R=0.0519 and wR=0.1507. X-ray analysis indicated that the five-membered ring is essentially planar in this molecule, and intermolecular hydrogen bonds N(1)-H(1)…N(2), C(3)-H(3)…O(1), C(4)-H(4)…O(1) and C(12)-H(12a)…O(1) were observed. π-π Stacking interactions contribute to the stability of the structure. DSC-TG analysis showed that the title compound experienced a phase change at 190 ℃ and began to decompose above 240 ℃.     

Hydrothermal Syntheses and Crystal Structures of Two Complexes with 3,5- Dinitrosalicylate and 2,2′-Bipyridine Ligands

The two title complexes,[Cd{3,5-(NO2)2sal}(2,2′-bipy)]n 1 and [Mn{3,5-(NO2)2sal}(2,2′-bipy)]n 2 (3,5-(NO2)2sal=3,5-dinitrosalicylate,2,2′-bipy=2,2′-bipyridine),were synthesized by the hydrothermal reaction and structurally characterized. Complex 1 crystallizes in triclinic,space group P1,a=5.581(4),b=12.071(8),c=12.88(1),α=92.10(3),β=96.73(3),γ =102.02(2)°,C17H10N4O7Cd,Mr=494.69,V=841(1)3,Z=2,Dc=1.954 g/cm3,F(000)=488,μ =1.353 mm-1,R=0.0248 and wR=0.0761. Complex 2 crystallizes in monoclinic with space group P21/c,a=8.604(3),b=23.88(1),c=8.894(3),β=102.45(1)°,C17H10N4O7Mn,Mr=437.23,V= 1785(1) 3,Z=4,Dc=1.627 g/cm3,F(000)=884,μ=0.791 mm-1,R=0.0471 and wR=0.1250. Complex 1 possesses an infinite 1D polymeric chain structure consisting of the repeated basic four-membered ring units (Cd2O2) and eight-membered ring units (CdOCO)2. Compound 2 displays a linear 1D chain through Mn(Ⅱ) atoms and bridging carboxylate groups of 3,5-dinitrosalicylic acid ligands with the Mn…Mn separation of 4.472(2). The fluorescence properties and cyclic voltammetric behaviors of the complexes are also reported.     

Synthesis and Structure Characterization of a Tetranuclear Manganese(Ⅲ) Complex:[Mn_4O_2(O_2CMe)_6(MeOH)_2(dbm)_2]·2MeCOOH·2CH_2Cl_2

The title compound, [Mn4O2(O2CMe)6(MeOH)2(dbm)2]·2MeCOOH·2CH2Cl2 (Hdbm = dibenzoylmethane), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1, with a = 10.729(3), b = 12.269(3), c = 13.085(4) , α = 106.367(3), β = 107.643(2), γ = 94.771(2)o, V = 1547.9(7) 3, Z = 1, C50H64Cl4Mn4O24, Mr = 1410.57, Dc = 1.513 g/cm3, F(000) = 724, Rint = 0.0147, T = 293(2) K and μ = 1.046 mm–1. The final R = 0.0359 and wR = 0.0938 for 5791 observed reflections with I > 2σ(I). The structure of the complex consists of one [Mn4(μ3-O)2]8+ core with four coplanar Mn atoms disposed in an extended “butterfly-like” arrangement and two O atoms triply bridging each “wing”, and the peripheral ligation is provided by six μ2-MeCO2– , two terminal μ2-dbm– groups at the two ends of the molecule, and two MeOH molecules on the central Mn atoms. Intermolecular O…H–O hydrogen bonding interactions are found within the structure of the compound.     

Synthesis,Crystal Structure and Biological Activity of 2-（Anthracen-9-yl）-5-p-tolyl-1,3,4-oxadiazole

A novel compound,2-(anthracen-9-yl)-5-p-tolyl-1,3,4-oxadiazole(C23H16N2O),has been synthesized by the condensation of 4-methylbenzohydrazide and anthracene-9-carbaldehyde in an ethanol solution with chloramine-T.The compound was characterized by 1H-NMR,13C-NMR,MS and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P with a = 7.7817(4),b = 8.8544(5),c = 12.4726(8) ,β = 92.8520(10)°,Z = 2,V = 826.58(8) 3,Dc = 1.352 g/cm3,Mr = 336.38,λ(MoKα) = 0.71073 ,μ = 0.084 mm-1,F(000) = 352,R = 0.0381 and wR = 0.1099.The dihedral angle between anthracene skeleton and phenyl ring is 64.19°.A total of 6354 unique reflections were collected,of which 3172 with I > 2σ(I) were observed.X-ray analysis indicated an offset face-to-face π-π stacking interaction between anthracene skeletons and an offset face-to-face π-π stacking interaction between phenyl ring planes.The novel compound molecules are connected through the offset face-to-face π-π stacking interactions to generate a three-dimensional network.The preliminary bioassay results showed that the novel compound exhibited significant insect growth inhibitory activity against Spodoptera litura Fabricius larvae.     

Synthesis and Structure of a Novel Macrocyclic Complex [Cd_2(phen)_4(phth)_2]·4H_2O

1 INTRODUCTION In recent years, extensively attention has been fo- cused on the design and synthesis of d10 metal- based complexes[1, 2]. A series of d10 metal-organic frame- works have been described not only because of their intriguing structures but also due to their ptential ap- plications in photoluminescent fields[3～7]. Although phthalate ligand was successfully used to design and synthesize a wide variety of metal complexes, those containing Cd(II) complex are less considered[8～…     

Synthesis, Crystal Structure,and Antioxidant and Antibacterial Activities of 3,5-Dihydroxy-N＇-（4-nitrobenzylidene）benzohydrazide

A new compound, 3,5-dihydroxy-N＇-（4-nitrobenzylidene）benzohydrazide （I）, has been synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 9.632（12）, b = 12.256（15）, c = 11.425（14） A, β = 105.306（11）°, Z = 4, V = 1301（3） A3, Dc = 1.538 g/cm3, F（000） = 704,μ = 0.276 and S = 1.011. The final R = 0.0444 and wR = 0.1186 for 3808 observed reflections with I〉 20（I）. We used methods such as ABTS, DPPH assays and in vitro hydroxyl radical scavenging experiment to assess the in vitro antioxidant activity of the new compound, and found that its IC50 value was 48.59 μg/mL for scavenging ABTS radicals, 48.04 μg/mL for scavenging DPPH radicals, and 1.03 mg/mL for scavenging hydroxyl radicals, indicating that it had a good in vitro antioxidant activity. We also test the antibacterial activities of this compound against three bacteria, and it showed considerable antibacterial activity against S.aureus. The MIC values of S.aureus, K.pneumoniae and P. aeruginosa are respectively 0.156, 0.625 and 1.25 mg/mL.     

Syntheses and Crystal Structures of Two Coordination Polymers Based on a Flexible Ligand N,N＇-Diacetic Acid Imidazolium

Two coordination compounds with a flexible ligand N,N?-diacetic acid imidazolium(HDAM),{[Co(trans-DAM)(bipy)(H2O)2](OH)·4H2O}n 1 and {[Cd(trans-DAM)(bipy)(H2O)](NO3)?2H2O}n 2(bipy = 4,4'-bipyridine),were prepared and characterized by single-crystal X-ray diffraction.Compound 1 crystallizes in monoclinic,space group P2/n with a = 7.589(6),b = 11.444(2),c = 12.894(3),β = 90.99(3)°,V = 1119.8(4)3,Z = 4,C8.5H14N2O5.5Co0.5,Mr = 261.68,Dc = 1.552 g/cm3,F(000) = 546,μ = 0.832 mm-1,the final R = 0.0657 and wR = 0.1958.Compound 2 crystallizes in the monoclinic C2 space group with a = 17.479(4),b = 11.689(2),c = 11.670(2),β = 117.13(3)°,V = 2121.9(7)3,Z = 4,C17H21N5O10Cd,Mr = 567.79,Dc = 1.777 g/cm3,F(000) = 1144,μ = 1.096 mm-1,the final R = 0.0233 and wR = 0.0638.In 1,the Co(II) ions are linked by μ2-trans-DAM-and bipy ligands to build a 2D(4,4) rectangular grid layer,exhibiting a 4-connected sql net.As for 2,μ3-trans-DAM-and bipy bridge Cd(II) ions form a 2D double-layer,consisting of a couple of(4,4) grid layers,which can be viewed as a(3,4)-connected network.In both compounds,the 2D structures are stabilized by hydrogen bonding interactions to give 3D supramolecular frameworks.Additionally,FT-IR spectroscopy,UV-Visible spectroscopy,and the fluorescent properties are discussed.     

Synthesis,Crystal Structure and Spectroscopic Properties of Zn(Ⅱ) with N-carbamylglutamate Ligand

Zn C6H8N2O5.H2O(NCGZn) has been synthesized, and its functional groups present in the title compound were confirmed by elemental analysis, TG and IR spectral studies. Meanwhile, the crystal of NCGZn was obtained by slow evaporation of a saturated aqueous solution at room temperature and confirmed by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P21 with a = 5.03220(1), b = 13.3747(4), c = 12.9944(4) , β = 92.987(2)o, V = 873.39(4) 3, Z = 2, C12H20N4O12Zn2, Mr = 543.10, Dc = 2.065 g/cm3, F(000) = 552, μ(Mo Ka) = 2.826 mm-1, R = 0.0422 and w R = 0.1142. In NCGZn, Zn(1) and the symmetry formed Zn(1) ions are connected by five atoms from four NCG-2H anions and a water molecule. A NCG ligand has two carboxylate groups, one connecting a Zn ion, and the other bridgiong two Zn ions. The NCG ligand bridges four Zn ions through the amino group and two carboxylate groups with a water molecule to yield a 3D coordination polymer structure with hydrogen bonds.