Synthesis,Crystal Structure and Antifungal Activity of 4-(5-((2,4-Dichlorobenzyl)thio)-4-phenyl-4H-1,2,4-triazol-3-yl)pyridine

The title compound 4-（5-（（2,4-dichlorobenzyl）thio）-4-phenyl-4H-1,2,4-triazol-3- yl）pyridine （C20HI4CI2N4S） was synthesized, and its structure was confirmed by 1H NMR, MS, elemental analyses and X-ray diffraction. It crystallizes in the monoclinic system, space group P21/c with a = 14.885（5）, b = 8.597（2）, c = 16.144（5）A,β= 114.505（4）°, V= 1879.8（10） A3, Z= 8 and R = 0.0320 for 3108 observed reflections with I 〉 2σ（I）. The preliminary biological test shows that the title compound has activities against Stemphylium lyeopersici （Enjoji） Yamamoto, Fusarium oxysporum, sp. cueumebrium, and Botrytis cinerea with inhibitory to be 53.57%, 66.67% and 24.44%, respectively.

Synthesis, Crystal Structure and Antimicrobial Activity of a Novel Ni(II) Complex

A new nickel（Ⅱ） complex, C34H38N8NiO4, has been prepared and characterized by X-ray diffraction analysis. It crystallizes in the monoclinic system, space group P21/c with a = 11.715（5）, b = 12.328（5）, c =11.113（5）A, β= 92.589（5）°, Z = 2, Dc = 1.411 g/cm^3,μ = 0.658 mml, the final R = 0.0427 and wR = 0.1099 for 2229 observed reflections with I 〉 2σ（I）. The complex is a centrosymmetric plane in which nickel（Ⅱ） is coordinated in a regular octahedron to the ligand phenytoin through the nitrogen atoms of ethylenediamine, imine and amine. The complex was valued for its antimicrobial activity against bacterial strands using the agar diffusion method, and found to be active against the four test bacterial organisms. Preliminary screening for antimicrobial activities showed that the title complex is quite active against standard strains of Salmonella species, Staphylococcus aureus, Bacillus pumilus and Eschierichia coli.

Synthesis, Crystal Structure, Docking and Antifungal Activity of a New Pyrazole Acylurea Compound

The title compound N-（（3,5-dimethylphenyl）carbamoyl）-1-methyl-3-（trifluoromethyl）-1 H-pyrazole-4-carboxamide（C（15）H（15）F3N4O2） was synthesized, and its structure was confirmed by 1 H NMR, H RMS and X-ray diffraction. It crystallizes in the triclinic system, space group P1 with a = 11.7147（5）, b = 11.7935（5）, c = 13.6620（5） A, α = 69.755（7）°, β = 66.182（6）°, γ = 72.100（7）°, Dc = 1.423 g/cm^3, Z = 4, V = 1588.88（11） A^3, the final R = 0.0347 and wR = 0.1005 for 7171 observed reflections with I 〉 2σ（I）. The preliminary biological test showed that the title compound has antifungal activities against Fusarium oxysporum, Pseudomonas syringae, Corynespora mazei and Botrytis cinerea at 100 μg/mL as 5.19%, 53.50%, 88.55% and 70.62%, respectively. The docking results indicated the hydrogen bonds formed between the compound and SHD.

Synthesis, Crystal Structure and Biological Activity of a Novel Amino Acid Salt (HGly)_4[HPMo_(12)O_(40) ]_2·22H_2O

A novel compound, (HGly) 4[HPMo 12 O 40 ] 2·22H 2O, was synthesized and characterized by means of elemental analysis, IR and X ray diffraction. The compound crystallized in a monoclinic space group Cc with a =4 0060(0 8) nm, b =1 2527(0 3) nm, c =1 9930(0 4) nm, β =96 36(3)°, V =9 940(3) nm 3, Z =2, R 1=0 0576, wR 2 =0 1746. The anti tumor activity of this compound was tested in two human tumor cell lines in vitro .

Synthesis,Crystal Structure and Biological Activity of N-(2,6-Difluorobenzoyl)-N'-[5-(4-trifluoromethyl-phenyl)-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）-1,3,4-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） ,β = 106.408（2）°,V = 1743.6（4） 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〉 2σ（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.

Synthesis, Crystal Structure and Biological Activity of 1,5-Bis(4-methoxyphenyl)-3-(4-methyl-1,2,3-thiadiazol-5-yl)pentane-1,5-dione

The title compound 1,5-bis（4-methoxyphenyl）-3-（4-methyl-1,2,3-thiadiazol-5-yl）-pentane-1,5-dione （C22H22N2O4S, Mr=410.49） has been synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbaldehyde with 4-methoxyacetophenone, and its structure was characterized by IR, 1H NMR, H RMS, elemental analysis and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group P21/c with a=11.159（3）, b=9.002（3）, c=20.192（6）, β=93.393（5）°, Z=4, V=2024.6（10） 3 , Dc=1.347 g/cm3 , μ=0.191 mm-1 , F（000）=864, R=0.0333 and wR （I〉2σ （I））=0.0840. In this molecule, the 1,2,3-thiadiazol ring is nearly vertical with both phenyl rings, and intermolecular weak hydrogen bonds of C-H…O and C-H…N types together with π-π stacking interactions and interactions between S（1）…N（2） are observed. The above three kinds of interactions extend the molecules into a two-dimensional layer framework. The preliminary biological test showed that the title compound had fungicidal activity.

Synthesis, Crystal Structure and Cytotoxic Activity of a Novel Nickel(II) Complex with Schiff Base Derived from Salicylhydrazide

A novel Schiff base complex with π-conjugated system, [Ni（L1）2（py）2] 1 （L1 =（E）-N′-（2,4-dichlorobenzylidene）-2-oxidobenzohydraizide）, was synthesized and characterized by elemental analysis and single-crystal X-ray determination. Complex 1 crystallizes in the monoclinic system, space group P21/n with a = 12.8286（10）, b = 16.3573（13）, c = 19.0206（14） A, β = 108.2920（10）°, V = 3789.6（5）A^3, Z = 4, Mr = 833.17, Dc = 1.460 g/cm^3,/t = 0.843 mm^-1, F（000） = 1704, the final R = 0.0537 and wR = 0.0640 for 3836 observed reflections with I 〉 2σ（I）. In the molecular structure of 1, the Ni^Ⅱ atoms are six-coordinated by two N and two O atoms from two Schiff base ligands （LI） and two N atoms from two pyridine solvent molecules to form a distorted octahedral geometry. The cytotoxic activities of complex 1 have been experimentally studied against a human HeLa cell in vitro.

Synthesis and Crystal Structure of a Dinuclear Cu(Ⅱ) Complex Based on a Carboxyl-substituted 1H-1,2,3-Triazole and Its DNA Cleavage Activity

The novel dinuclear copper complex [Cu2（H20）2（DMF）2（L）2] （1, H2L = 5-phenyl- 2H-1,2,3-triazole-4-carboxylic acid, DMF = N,N-dimethyl-formamide） has been synthesized and characterized by X-ray single-crystal diffraction. The compound crystallizes in triclinic system, space group P1 with a = 9.591, b = 10.508, c = 15.515A,β = 75.11°, V= 1446.2 A3, Z= 2, Mr = 683.62, Dc = 1.570 g/cm3, μ = 1.531 mm^-1, F（000） = 700, the final R = 0.0404 and wR = 0.1130 for 5327 observed reflections with I 〉 2σ（I）. In each unit of the complex, two Cu2＋ ions coordinated with two triazole ligands to form a dimeric [5,6,5] tricyclic structure. The central Cu atom is five-coordinated, and each copper atom shows a square pyramidal geometry. The crystal structure is stabilized by the inversion-related O-H…O hydrogen bond and C-H…O hydrogen bonding interactions to form a layer structure. Fluorescent spectra show an obvious quenching of fluorescence compared with free 1,2,3-triazole ligand. The results of agarose gel electrophoresis indicate that this complex can cleave the plasmid supercoiled DNA within shorter time in the 50-folds excess of ascorbate under physiological conditions, providing a new example in the research for artificial metal nucleic acid enzyme.

Synthesis, Crystal Structure and Antitumor Activity in Vitro of a New Benzoate Binuclear Cupper(Ⅱ ) Complex

The title compound, [Cu2（C7H5O2）4（C2H6O）2], was synthesized by the reaction of benzoic acid, copper acetate and ethanol in an aqueous solution. Trypan blue dye exclusion method was used in experiment. X-ray single-crystal analysis has revealed that compound 1 （C32H32Cu2O10） crystallizes in the monoclinic system, space group C2/c, Mr = 703.66, a = 47.340（5）, b = 6.6613（4）, c = 22.028（2）A,β = 113.284（4）°, V = 6380.6（10） A^3, Z = 8, Dc= 1.465 g/cm^3, F（000） = 2896,μ = 1.388 mm^-11, the final R = 0.0515 and wR = 0.1172 for 5712 observed reflections with I 〉 2σ（I）. X-ray crystal structure analysis suggests that compound [CH2（C7H5O2）4（C2H6O）2] has a binuclear structure with two Cu（II） atoms coordinated by four benzoate groups and two ethanol molecules. The crystal packing is stabilized by intermolecular O-H...O hydrogen bonds. The compound inhibits the proliferation of K562 cells （chronic myeloid leukemic cells） significantly and dose-dependently in 48 h, and IC50 of K562 is 17.3μg/mL by trypan blue dye exclusion method.

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.

Synthesis,Crystal Structure and Biological Activity of 2-(1-(3-Bromo-1-(3-chloropyridin-2-yl)-1H-pyrazole-5-carbonyl)piperidin-4-yl)-N-isopropyl-1,3-thiazole-4-carboxamide

The title compound 2-（1-（3-bromo-1-（3-chloropyridin-2-yl）-1H-pyrazole-5-carbonyl）piperidin-4-yl）-N-isopropylthiazole-4-carboxamide（C21H22Br Cl N6O2 S,Mr = 536.04） has been synthesized,and its structure was characterized by IR spectra,1H-NMR,13C-NMR,EA,and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic system,space group P/c with a = 15.146（3）,b = 11.573（2）,c = 26.937（5） A,β = 103.64（3）°,V = 1839.0（6） A^3,Z = 4,Dc = 1.557 g/cm^3,μ（Mo Ka） = 0.71073 mm^-1,F（000） = 2192,R = 0.0601 and w R = 0.1392.There exist one intramolecular hydrogen bond at N–H···N and four intermolecular weak interactions at O（2）···H（1）,Cl（1）···H（12）,O（1）···Cl（1） and S（1）···O（2）.Bioassay results indicated that the title compound had good fungicidal and antiviral activities against tobacco mosaic virus.

Synthesis,Crystal Structure,DFT Studies and Biological Activity of a Novel Schiff Base Containing Triazolo[4,3-a]pyridine Moiety

The novel Schiff base（E）-8-chloro-NA-（4-（dimethylamino）benzylidene）-[1,2,4]triazolo[4,3-a]pyridine-3-carbohydrazide was synthesized and characterized by ^1H NMR,MS,elemental analysis and X-ray diffraction.The compound crystallizes in the monoclinic space group P2_1/c with a = 7.091（2）,b = 10.750（3）,c = 21.380（6） A,β = 96.299（6）°,V = 1619.7（8） A^3,Z = 4 and R = 0.0351.Theoretical calculation of the title compound was carried out with the B3LYP/6-31 G basis set.The frontier orbital energy and atomic net charges were discussed.It is found that the experimental data show good agreement with the calculated values.And the compound exhibits good antifungal activity against Stemphylium lycopersici（Enjoji） Yamamoto.

Effects of surface physicochemical properties on NH_3-SCR activity of MnO_2 catalysts with different crystal structures

α‐,β‐,δ‐,andγ‐MnO2nanocrystals are successfully prepared.We then evaluated the NH3selective catalytic reduction(SCR)performance of the MnO2catalysts with different phases.The NOx conversion efficiency decreased in the order:γ‐MnO2>α‐MnO2>δ‐MnO2>β‐MnO2.The NOx conversion with the use ofγ‐MnO2andα‐MnO2catalysts reached90%in the temperature range of140–200°C,while that based onβ‐MnO2reached only40%at200°C.Theγ‐MnO2andα‐MnO2nanowire crystal morphologies enabled good dispersion of the catalysts and resulted in a relatively high specific surface area.We found thatγ‐MnO2andα‐MnO2possessed stronger reducing abilities and more and stronger acidic sites than the other catalysts.In addition,more chemisorbed oxygen existed on the surface of theγ‐MnO2andα‐MnO2catalysts.Theγ‐MnO2andα‐MnO2catalysts showed excellent performance in the low‐temperature SCR of NO to N2with NH3.

Crystal Structure and Antitumor Activity of Tri[2- [N-(4'-methyl-benzylsulfonyl)amino]ethyl]-amine

The crystal structure of the title compound (C27H38N4O7S3, Mr = 626.79) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group Pīwith a = 9.411(1), b = 11.645(2), c = 14.672(2) , a = 91.80(1), b = 95.36(1), g =104.56(1)o, V = 1547.0 3, Z = 2, Dc = 1.346 g/cm3, l = 0.71073 , m(MoKa) = 0.289 mm-1 and F(000) = 664. The structure was refined to R = 0.0406 and wR = 0.1177 for 4103 observed reflections with I > 2s(I). X-ray diffraction analysis reveals that the title compound is a practically distorted tetrahedron and each molecule contains one lattice H2O by hydrogen bond. The antitumor activity of the title compound against HL-60 human leukemia cells has also been studied by MTT method.

Novel Synthesis,Crystal Structure and Herbicidal Activity of(3R,4R)-4,7,7-Trimethyl-6-oxabicyclo[3.2.1]octane-3,4-diol

The title compound, （3R,4R）-4,7,7-trimethyl-6-oxabicyclo[3.2.1]octane-3,4-diol （Cl0HlsO3）, has been synthesized by using one-step catalytic synthetic method from a-pinene and structurally characterized by means of IR, JH-NMR, J3C-NMR, HRMS and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/n with a = 7.277（4）, b = 18.177（11）, c = 7.939（5） A, β = 91.122（8）°, Z = 4, V = 1049.9（11） A, Dc = 1.178 g/cm3, Mr = 186.24, λ（MoKa） = 0.71073 A, μ = 0.09 mm^-1, F（000） = 408, R = 0.051 and wR = 0.144. The title complex molecules contained two hydroxyls and are connected through hydrogen bonds to generate a two-dimensional network. Especially, the preliminary herbicidal activity results show that the title compound exhibits herbicidal activity against rape （Brassica campestris） and barnyard grass （Echinochloa crusgalli）.

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,Crystal Structure and Antitumor Activity of Mixed Ligand Coordination Compound of Copper with Norfloxacin and 1,10-Phen,[Cu(NFLX)(phen)(H2O)]NO3·3H2O

The mixed ligand coordination compound of copper with norfloxacin (NFLX) and 1, 10-phen has been synthesized and characterized by means of X-ray single crystal diffraction. The structure features of the coordination compound are described. Antibacterial activities of the coordination compound have been tested against different microorganisms. The antitumor activities of the coordination compound on leukemia HL-60 cell line and liver cancer BEL-7402 cell line have been measured, respectively. The results indicated that the coordination compound has strong inhibitory effect on HL-60 and BEL-7402 cell lines.

Synthesis,Crystal Structure,DFT Studies and Antifungal Activity of 5-(4-Cyclopropyl-5-((3-fluorobenzyl)sulfonyl)-4H-1,2,4-triazol-3-yl)-4-methyl-1,2,3-thiadiazole

5-（4-Cyclopropyl-5-（（3-fluorobenzyl）sulfonyl）-4H-1,2,4-triazol-3-yl）-4-methyl-1,2,3-thiadiazole was synthesized and recrystallized from Et OH. The compound was characterized by ^1H NMR,MS,elemental analysis and X-ray diffraction. The structure-active relationship and the antifungal activity based on density functional theory calculation（DFT） and antifungal activities were investigated. The compound crystallizes in the monoclinic space group P121/n1 with a = 8.929（3）,b=12.715（4）,c=15.161（5） A°,β = 106.142（3）o,V = 1653.3（9） A°3,Z = 4 and R = 0.0393 for 3930 observed reflections with I 〉 2σ（I）. Theoretical calculation of the title compound was carried out with B3LYP/6-31G（d,p）. The full geometry optimization was carried out using the 6-31G（d,p） basis set.The frontier orbital energy and atomic net charges were discussed. The observed results of the compound have been compared with theoretical results and the experimental data show good agreement with the calculated values. The compound exhibits good antifungal activity.

Synthesis, Crystal Structure and Antitumor Activity of N-[5-(Benzylthio)-1,3,4-thiadiazol-2-yl]-4-chlorobenzamide

The title compound N-[5-（benzylthio）-1,3,4-thiadiazol-2-yl]-4-chlorobenzamide（C（16）H（12）ClN3OS2, Mr = 361.86） was designed and synthesized as anticancer agent, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 5.7417（10）, b = 9.8057（17）, c = 14.330（3） A, a = 91.987（3）, b = 97.154（3）, γ = 93.402（3）°, V = 798.4（2） A3, Z = 2, Dc = 1.505 g/cm^3, μ = 0.507 mm-1） F（000） = 372, the final R = 0.0481 and wR = 0.1290 for 2064 observed reflections with I 〉 2s（I）. In the crystal packing, the molecules form stacks by a three-dimensional framework, which results from intermolecular N（1）-H（1）···N（2） and C（5）-H（5）···N（3） hydrogen bonds together with π-π stacking interactions between the thiadiazole and chlorobenzene rings. The title compound was found to exhibit more potent in vitro antitumor activities against the four tested cancer cell lines than sorafenib.

Synthesis,Crystal Structure and Biological Activity of N-cyanosulfoximine Derivative Containing 1,2,3-Thiadiazole

The title compound N-cyanosulfoximine derivative containing 1,2,3-thiadiazole （C6HsN4OS2, Mr = 216.28） has been synthesized using 4-（chloromethyl）-5-methyl-1,2,3-thiadiazole as the starting material, and its structure was characterized by IR, 1H NMR, HRMS, elemental analysis and single-crystal X-ray diffraction. The crystal of the title compound belongs to orthorhombic, space group Pna21 with a = 14.730（6）, b = 5.478（2）, c = 22.619（9） A, Z = 8, V = 1825.0（13） A3, Dc = 1.574 g/cm3,/a = 0.547 mm-1, F（000） = 896, R = 0.0767 and wR （I〉 2o（/）） = 0.2064. X-ray analysis indicates that in this crystal double enantiomers are found as the basically asymmetrical unit and interactions between S（1）...N（3）, S（3）...N（4） and S（3）...N（7） are observed. This kind of interactions extends the molecules into a one-dimensional double chain. The preliminary biological test showed that the title compound had insecticidal activity against Myzus persicae in a certain degree and also presented moderate potential bioactivity against tobacco mosaic virus （TMV）.