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.

Synthesis, Structure and Antimicrobial Activity of 9,9-Dimethyl-9,10-dihydrospiro[benzo[a]-xanthene-12,3'-indoline]-2',11(8H)-dione

One novel spiro-compound（C_（26）H_（21）NO_3） has been synthesized and characterized by means of NMR spectroscopy,elemental analyses and X-ray diffraction. The single crystal belongs to the monoclinic system,space group P21/c with a = 8.8039（7）,b = 24.123（2）,c = 10.0751（9） ？,β = 108.403（3）°,M3r = 395.44,V = 2030.3（3） ？~3,Z = 4,D_c = 1.294 g/cm,F（000） = 832.0,μ = 0.085 mm^（-1）,R = 0.0801 and wR = 0.2228. The title compound shows good activities against Micrococcus tetragenus,Bacillus cereus,Bacillus subtilis,Staphylococcus aureus,S.albus and Escherichia coli.

Solvothermal Synthesis,Crystal Structure and Antimicrobial Activity of a Novel Imide Nickel Complex [Ni(CH_3CONCOCH_3)_2·2(H_2O)]

A novel imide nickel complex [Ni（CH3CONCOCH3）2·2（H2O）] was synthesized by the solvothermal reaction of nickel acetate tetrahydrate and acetonitrile.What amazed us is that acetonitrile had changed into acetyl imide in enol form during the formation process of the title complex.The complex was characterized by elemental analysis,IR spectrum and X-ray single-crystal diffraction analysis.It crystallizes in the orthorhombic system,space group Pbca with a = 7.4503（7）,b = 13.1089（12）,c = 14.1303（14）,V = 1380.0（2）3,Dc = 1.420 g/cm3,Mr = 294.94,Z = 4,F（000） = 616,μ = 1.422 mm-1,the final R = 0.0487 and wR = 0.1482.The four-coordinated nickel（II） center is surrounded by 4O atoms from two imide ligands and has a distorted square planar geometry.The complex is connected to form a supramolecule with an infinite three-dimensional network through intramolecular and intermolecular hydrogen bonds.Antimicrobial activity was investigated by agar diffusion method,and the result showed that the complex was active against coli bacillus,staphylococcus aureus and bacillus subtilis.The thermal stability of the title complex was also studied by TG-DTA method.

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,Bioactivity and Crystal Structure Analysis of Novel Benzo[d]isothiazol-3(2H)-ones

Two compounds,3-oxo-N-o-tolylbenzo[d]isothiazole-2（3H）-carboxamide （1） and N-（2-methoxyphenyl）-3-oxobenzo[d]isothiazole-2（3H）-carboxamide （2）,were synthesized from the initial compound benzo[d]isothiazol-3（2H）-one （BIT） and characterized by 1 H NMR,IR and elemental analysis,respectively.The single crystals of compounds 1 and 2 were obtained and determined by X-ray diffraction analysis.The preliminary results of biological activity experiment show that some of the title compounds exhibited a favorable antimicrobial activity.

Syntheses, Crystal Structures and Antimicrobial Activities of Vanadium(V) Complexes with Similar Tridentate Hydrazone Ligands

Two hydrazone ligands （E）-N＇-（2-hydroxy-5-methoxybenzylidene）-2-hydroxybenzo- hydrazide （HLa） and （E）-N＇-（3,5-dichloro-2- hydroxybenzylidene）-4-methoxybenzohydrazide （HLb） were prepared and characterized by IR, UV-Vis and 1H NMR spectra. Based on the hydrazone ligands, two new structurally similar vanadium（V） complexes, [VOLaL].CH3OH （1） and [vOLbL] （2）, where L is the monoanionic form of benzohydroxamic acid （HL）, were prepared and characterized by IR and UV-Vis spectra, and single-crystal X-ray diffraction. Complex 1 crystallizes as the monoclinic space group P21/n, with a = 7.5208（10）, b = 15.490（2）, c = 20.8929（18） A, β = 96.373（2）°, V = 2418.9（5） A3, Z = 4, R = 0.0831, wR = 0.2607 and GOOF = 1.061. Complex 2 crystallizes as the monoclinic space group P21/c, with a = 11.8577（18）, b = 16.468（2）, c = 12.2288（18） A, β = 106.064（2）°, V= 2294.7（6） A3, Z = 4, R= 0.0741, wR= 0.1745 and GOOF= 1.014. X-ray analysis indicates that the complexes are mononuclear vanadium （V） species, with the V atoms located in the octahedral coordination. The hydrazone ligands and the complexes were evaluated for their antibacterial （Bacillus subtilis, Staphylococcus aureus, Escherichia coli, and Pseudomonas fluorescence） and antifungal （Candida albicans and Aspergillus niger） activities by MTT （3-（4,5-dimethylthiazol-2-yl）-2,5-diphenyl tetrazolium bromide） method.

Synthesis, Structure and Antimicrobial Activity of a Cyclic Compound [Cu(Pmal)(Dadm)(H_2O)]_2·4H_2O

A new copper compound constructed from H2 Pmal （phenylmalonic acid）, Dadm （4,4-diaminodiphenylmethane） and Cu（Ⅱ） has been synthesized from H2O-EtOH-DMF solution, and is characterized by X-ray single-crystal diffraction and other measurements. The compound crystallizes in the monoclinic system, space group C2/c with a=13.7866（6）, b=10.1557（4）, c=30.9036（17）, β=101.422（5）o, V=4241.2（3）3 , Z=4, Dc=1.547g/cm3 , Mr=987.94, F（000）=2056, μ（MoKα）=1.078 mm-1 , S=1.007, R=0.0453 and wR=0.987 for 2806 observed reflections （I〉2σ （I））. The title compound is characteristic of the cyclic dimeric molecules which further aggregate through hydrogen bonds and π-π interactions to form a 3-D supramolecular network. The microbial activities of the title compound and its reagents are investigated with filter paper discs diffusion method. The results show that the activity of the title compound is slightly better than its precursor reagents.

Synthesis, Crystal Structure and Antimicrobial Activity of(E)-2-(2-(4,8,8-Trimethyldecahydro-1,4-methanoazulen-9-ylidene)ethyl)benzo[d]isothiazol-3(2H)-one

The title compound(E)-2-(2-(4,8,8-trimethyldecahydro-1,4-methanoazulen-9-ylidene)ethyl)benzo[d]isothiazol-3(2H)-one(Ic)was synthesized from longifolene and 1,2-benzoisothiazolinone(short as BIT)through Prins,halogenation and nitro-alkylation reaction and structurally identified by means of HRMS,IR,1H-NMR,13C-NMR and single-crystal X-ray diffraction.The crystal of compound Ic is of bi-molecular structure and belongs to orthorhombic system,P212121 space group with a=7.5715(7),b=16.8824(9),c=31.1926(14)?,V=3987.2(5)A^3,Mr=367.53,Dc=1.225 mg/m^3,Z=8,μ=0.174 mm^–1 and F(000)=1584.A total of 17045 reflections were collected,of which 7306 were unique(Rint=0.0566).The structure was refined to R=0.0967 and wR=0.1998 for 7306 observed reflections withⅠ>2σ(Ⅰ).1D chain along the a-axis is formed by two types ofπ-πinteractions between benzene rings from adjacent molecules.Especially,compound Ic shows improved solubility in nonpolar organic solvents and higher antimicrobial activity than longifolene and BIT against bacteria and fungi.The minimum inhibition concentration(MIC)of Ic against two Gram-positive bacteria(S.aureus and B.subtili),two Gram-negative bacteria(E.coli and K.pneumoniae)and three fungi(C.albicans,C.tropicalis and A.niger)are 0.242,0.242,15.6,15.6,1.95,1.95 and 1.95μg/mL,respectively.

Synthesis, Characterization and Antimicrobial Study of a New Schiff Base Paeonol-phenylpropanolamine

A novel Schiff base compound was synthesized by the reaction of paeonol and phenylpropanolamine in absolute methanol. It was characterized by elemental analyses, IR, tH NMR and X-ray single-crystal diffraction. The compound crystallizes in the wiclinic system, space group PI, with a = 6.4075（11）, b = 10.2821（18）, c = 12.573（2） A, α = 92.606（3）,β= 100.980（3）, γ = 90.994（3）°, V= 812.1（2） A3, Mr = 299.36, Z = 2, F（000） = 320, Dc=1.224 g/cm^3, T= 293（2） K,μ = 0.083 mm^-1 and 2 = 0.71073 A, the final R = 0.0555 and wR = 0.1619 for 2442 observed reflections with I 〉 2σ（I）. The colnpound was valued for its antimicrobial activity against bacterial strands using the agar diffusion method. It is found to be active against Candida albicans and Staphylococcus aureus.

One-pot Synthesis,Crystal Structures and Antimicrobial Activities of Two New 1,4-Disubstituted 1,2,3-Triazole-4-Carboxylates

Two new 1,4-disubstituted 1,2,3-triazoles-4-carboxylates were synthesized via click reaction. Compound 1a was synthesized by the interaction of 6-nitro-tetrazolo[1.5-a]-pyridine with ethyl propynoate at room temperature in the presence of Cu（OAc）2 as a catalyst and THF as solvent. Compound 1b was also synthesized by the same manner except that tert-butyl propionate, instead of ethyl propynoate, was used. The compounds were characterized by IR, 1H-NMR, 13C-NMR and single-crystal X-ray diffraction analysis. Compound 1a（C10H9N5O4） crystallizes in the triclinic system, space group P1 with a = 5.0894（9）, b = 8.9834（13）, c = 13.089（2） ？, α= 83.041（7）, β= 80.256（7）, γ=87.296（8）°, V = 585.24（16）？3, Z = 2, Mr = 263.22, crystal size（mm） = 0.37 × 0.20 ×0.18,（I 〉 2σ（I）） = 8557, 2493, 1229, Rint = 0.057. Compound 1b（C12H13N5O4） crystallizes in the monoclinic system, space group P21/c with a = 6.8854（5）, b = 21.783（2）, c = 9.3986（8） ？,β = 93.239（4）°, V = 1407.4（2）？3, Z = 4, Mr = 291.27, crystal size（mm） = 0.38 × 0.22 × 0.20,（I 〉 2σ（I）） = 11842, 3172, 1866, Rint = 0.047. Antimicrobial assay results showed that the title compounds display excellent activities to different bacterial and fungal strains.

Synthesis, Crystal Structures, and Binding Behaviors with CT-DNA/BSA, Antimicrobial and Cytotoxic Activities of Three New Pyrazine Acylhydrazones

Three new acylhydrazones containing pyrazine ring(C12H11N5O2·CH3COOH,1;C13H13N5O·2CH3COOH,2;C13H13N5O3·C13H13N5O3,3)were synthesized and fully characterized.The single-crystal XRD indicated that both 1 and 2 crystallized in monoclinic,P21/c space group but 3 belonged to monoclinic,C2/c space group.The temperature of the maximum thermal decomposition peaks measured by thermogravimetry for 1~3 is 284,289 and 276℃respectively,all showing better thermal stabilities.The interactions of 1~3 with calf thymus DNA(CT-DNA)and bovine serum albumin(BSA)were studied by UV-Vis absorption spectroscopy and fluorescence spectroscopy,respectively,presenting that 1~3 could bind to CT-DNA via groove binding mode and quench the fluorescence of BSA through static process.Moreover,molecular docking studies of the interactions between 1~3 with DNA/BSA were in good agreement with experimental results.From antimicrobial activities of 1~3 and gentamycin sulfate against Staphylococcus aureus,Escherichia coli and Salmonella typhimurium,it was inferred that 3 had generally stronger antibacterial activity than 1 and 2 and is more active against Staphylococcus aureus than gentamycin sulfate.The cytotoxic tests of 1~3 and etoposide on human lung cancer cells(A549)were carried out by using the MTT method.

Molecular Structure and Properties of a Novel Acylhydrazone(C_(14)H_(14)O_6N_4)·HCON(CH_3)_2·2H_2O

[N-（Propionic acid）] terephthalal acyl dihydrazone（H4L） was synthesized and characterized by element analysis, IR, 1H NMR and MS. The theoretical studies on H4L were carried out at HF/6-31＋G（d） and B3LYP/ 6-3 I＋G（oD levels. The main decomposition stage of it was studied with IR track. The kinetic parameters[the apparent activation energy（Ea） and pre-exponential constant（A） of the first and second stages of decomposition reaction] were obtained by Kissinger and Ozawa＇s methods. Furthermore, the antimicrobial activity of HaL against wheat rust was investigated by spore sprout method.

N-亚水杨基苄胺过渡金属配合物的合成、结构与抑菌性能研究(英文)

N-salicylidene-benzylamineato M(Ⅱ) complexes (ZnL2, CuL2 and CdL2) were synthesized, characterized and valued for antimicrobial activities against bacterial strands using the agar diffusion method. The crystal of ZnL2 was determined by X-ray diffraction. It crystallizes in the Monoclinic system, space group C2/c with a=2.269 1(3), b=0.918 2(1), c=1.239 5(2) nm, β=117.89(2), Z=4, R1=0.049 4, wR2=0.138 2. The complexes were found to be active against Staphylococcus aureus and Eschierichia Coli. CCDC: 249474.

硝基苯并咪唑衍生物的合成、表征及抑菌活性的测定

以苯并咪唑为原料,经硝化、二茂铁磺酰化等步骤,合成了8种未见文献报道的硝基苯并咪唑衍生物,其结构经MS,1H NMR和元素分析确证.由于硝基苯并咪唑的互变异构,二茂铁磺酰化后,产生两个异构体,用X射线衍射仪测定了化合物2a的晶体结构.初步的抑菌实验结果表明,该系列化合物具有良好的抑菌作用,其抑菌活性均优于对照药剂50%多菌灵可湿性粉剂.

一种新型不对称三足四胺席夫碱锌(Ⅱ)配合物的合成、结构及杀菌性能研究(英文)

A new tripodal complex (ClO4)2 (C26H31Cl2N7O8Zn) was synthesized by Schiff base condensation of 2-aminoethyl-bi(3-aminopropyl)amine with 2-pyridinecarbaldehyde in the presence of Zn2+ and characterized by X-ray diffraction and ES mass spectral analysis. It crystallized in the Monoclinic system, space group P21/c with a=1.088 5(4) nm, b=1.614 6(6) nm, c=1.783 0(5) nm, a=94.405(2) the four test bacterial organisms. CCDC: 231275.

锌配合物的合成、晶体结构与抗微生物活性

利用水热法合成了一种新的锌三元配合物[Zn(PHT)2(PA)][HPHT:苯妥英(5,5-Diphenylhydantion);PA:1,2-丙二胺(1,2-propanediamine)]。通过元素分析、红外光谱、核磁共振氢谱和X-射线单晶衍射确定了其组成和结构。配合物中Zn离子配位数为4,处于变形四面体配位环境中。配位原子来自于2个苯妥英分子中咪唑环上的氮原子和1个1,2-丙二胺分子的两个氮原子。配合物属于三斜晶系,空间群为P1。利用琼脂扩散法和单片滤纸法测试了配合物、配体和锌盐的抑菌活性,结果表明,它们对4种植物致病真菌和3种细菌均有一定的活性。

新型Co(Ⅱ)配合物的合成,结构和抑菌性能研究

采用水热法成功合成了一种新的钴配合物[Co(Pae)2L](Pae=丹皮酚;L=乙二胺)。用X射线单晶结构分析仪、红外光谱和循环伏安法对该配合物进行了分析和表征。结果表明:该配合物属于单斜晶系,空间群为P2(1)/c,晶胞参数a=1.35141(15)nm,b=0.73190(10)nm,c=2.0897(2)nm,Mr=435.85,V=1.9529(4)nm3,Z=4,F(000)=910,Dc=1.482 g/cm3,μ(Mo-Kα)=0.915 mm-1,最终偏离因子R1=0.0530,wR2=0.1129。利用琼脂扩散法测试了配合物的抑菌活性,结果表明它对大肠杆菌,金黄葡萄球菌和枯草芽孢杆菌均有一定的抑菌活性。

萘甲基苯并咪唑衍生物的合成、表征及其杀菌活性

以1萘乙酸和2萘乙酸为原料,在微波辐射下合成了相应的萘甲基苯并咪唑,经二茂铁磺酰化等步骤,合成了2种未见报道的萘甲基二茂铁磺酰基苯并咪唑衍生物。经元素分析、质谱、核磁共振确证结构。通过X射线衍射,测定了化合物2a的晶体结构。化合物2a为三斜晶系,空间群P1,晶胞参数:a=0.89055(10)nm,b=0.97034(10)nm,c=1.4610(2)nm,α=101.542(2)°,β=95.811(2)°,γ=109.780(10)°,V=1.1443(2)nm3,Z=2,F(000)=526,Mr=507.39,Dc=1.473Mg/m3,μ=1.016mm-1,R1=0.0386,wR2=0.0979。对5种农作物病菌的杀菌活性优于市售50%多菌灵可湿性粉剂。

以N,N′-二(4-甲氧基水杨基)丙烷-1,3-二胺为配体的三核钴(Ⅱ)和镍(Ⅱ)配合物的合成、结构及抗菌活性研究(英文)

本文合成了1个新的三核钴(Ⅱ)配合物[Co{CoL(μ2-CH3COO)}2](1)和1个新的三核镍(Ⅱ)配合物[Ni{NiL(μ2-NO3)(CH3OH)}2](2),其中L代表去质子化的N,N′-二(4-甲氧基水杨基)丙烷-1,3-二胺。通过理化手段和单晶X-射线衍射表征了它们的结构。2个化合物都是中心对称的三核配合物。配合物1中的桥连基团为酚羟基氧原子和醋酸根;配合物2中的桥连基团为酚羟基氧原子和硝酸根。通过MTT比色法研究了配合物对枯草杆菌,金黄色葡萄球菌,大肠杆菌和荧光假单孢菌的抗细菌活性以及对白色念珠菌和黑曲霉的抗真菌活性。

三(2-氨基乙基)胺-镉(Ⅱ)-2-甲基咪唑三元配合物的合成、结构与抗微生物活性(英文)

The complex [Cd(tren)(meim)](ClO4)2 was synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. The compound crystallizes in monoclinic system, space group P21/m with a=0.786 8(2) nm, b=0.834 2(2) nm, c=1.496 2(4) nm, Mr=538.64, Z=2, F(000)=542, Dc=1.822 g·cm-3, T=298(2) K, μ=1.435 mm-1 and λ=0.071 073 nm. The structure was refined to R=0.045 8 and wR=0.123 1 for 1 489 observed reflections with I>2σ(I). The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method. It was found to be active against the four test bacterial organisms. CCDC: 600198.