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,...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.展开更多
Six new transition metal complexes, [Zn(HBTC)(PYTPY)]n·n PYTPY(1), [Cu(HBTC)(PYTPY)]n·n PYTPY(2), [Co(HBTC)(PYTPY)]n·n DMF(3), [Mn(HBTC)(PYTPY)]n·n DMF(4), [Cd(HBTC)(PYTP...Six new transition metal complexes, [Zn(HBTC)(PYTPY)]n·n PYTPY(1), [Cu(HBTC)(PYTPY)]n·n PYTPY(2), [Co(HBTC)(PYTPY)]n·n DMF(3), [Mn(HBTC)(PYTPY)]n·n DMF(4), [Cd(HBTC)(PYTPY)(H2O)]n·2nH2O(5), and [Co(HBTC)(PYTPY)(H2O)2](6),(H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4'-(4-pyridyl)-2,2':6',2''-terpyridine, DMF = N,N?-dimethylformamide), have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional(3D) supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.展开更多
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.T...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.展开更多
The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate (C 14 H 10 N 2 O 2 S,M r=270.31) was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its ...The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate (C 14 H 10 N 2 O 2 S,M r=270.31) was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1 H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a=23.475(5),b=9.6640(19),c=10.814(2),β=90.00°,Z=8,V=2453.2(9) 3,M r=270.30,D c=1.464 g/cm 3,μ=0.262 mm-1,F(000)=1120,R=0.0444 and wR=0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6) H(6)···O(1) and C(14) H(14)···O(1) were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.展开更多
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 singl...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.展开更多
A new Zn(Ⅱ) complex,[Zn(1,2,3-HBTC)(L)]2(1,L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and 1,2,3-H3 BTC = 1,2,3-benzentricarboxylic acid),was synthesized under hydrothermal conditi...A new Zn(Ⅱ) complex,[Zn(1,2,3-HBTC)(L)]2(1,L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and 1,2,3-H3 BTC = 1,2,3-benzentricarboxylic acid),was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction.It crystallizes in triclinic,space group P1 with a = 10.455(2),b = 11.533(2),c = 12.499(3) A,α = 116.97(3),β = 94.08(3),γ = 103.29(3)o,V = 1280.2(4) A^3,Z = 1,C56H28Cl2F2N8O12Zn2,Mr = 1244.50,Dc = 1.614 g/cm^3,F(000) = 628,μ(Mo Ka) = 1.124 mm^-1,R = 0.0502 and w R = 0.1417.In compound 1,two 1,2,3-HBTC anions bridge two Zn(Ⅱ) atoms to give a dimeric structure with Zn···Zn distance of 3.15 A.Adjacent dimers interact through π-π stackings between two L ligands to result in a supramolecular layer.Moreover,N–H···O and O–H···N hydrogen bonds further stabilize the 2D supramolecular architecture of 1.In addition,the luminescent property of 1 has been studied.展开更多
The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determin...The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.展开更多
The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its...The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.展开更多
A novel coordination polymer, [Co3(bta)2(dpe)3(H2O)2]·2H2O (1, H3bta = benzene-1,3,5-triacetic acid, and dpe = 1,2-di(pyridin-4-yl)ethene), has been hydrothermally prepared and characterized by IR spect...A novel coordination polymer, [Co3(bta)2(dpe)3(H2O)2]·2H2O (1, H3bta = benzene-1,3,5-triacetic acid, and dpe = 1,2-di(pyridin-4-yl)ethene), has been hydrothermally prepared and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal is of triclinic system, space group P , with a = 9.5687(15), b = 11.2470(17), c = 13.686(2) , α = 78.262(3), β = 89.271(4), γ = 81.292(3)°, V = 1425.2(4) 3, C60H56N6O16Co3, Mr = 1293.90, Dc = 1.508 g/cm3, F(000) = 667, μ = 0.940 mm-1 and Z = 1. The final R = 0.0707 and wR = 0.1413 for 4950 observed reflections (I 2σ(I)). In the title complex, the bta ligand acts as a four-dentate bridging ligand to link up cobalt atoms into lamellar frameworks which are further interlinked by the dpe ligands to generate a trinodal (3,4,6)-connected (4.62)2(42.68.83.102)(64.82) net.展开更多
The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H1...The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?展开更多
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 ...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.展开更多
The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of ...The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6- methylpyridazine-3-carboxylic acid with chloroformate ethyl ester, then with N′-tert-butyl-N- (2,4-dichlorobenzoyl) hydrazine in the present of triethylamine. The crystal structure has been determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P21/c, with unit cell constants a =11.4948(9), b=12.7495(10), c=35.854(3) ?, β =92.964(2)°, Z=4, V=5247.6(7) ?3, Dc = 1.320 Mg/m3, F(000) = 2156 , μ (MoKa)= 0.385, R = 0.0661, wR = 0.1875, for 9151 observed reflections( I >2σ(I)). The structure is a dimer linked by intermolecular hydrogen bond which can be observed between N(1)- H...O(6), N(5)- H...O(3). The distances are 2.068 and 2.027? respectively.展开更多
A new coordination compound Zn(2,4'-bpt)2(H2O)(1) based on the versatile ligand 2,4'-Hbpt(2,4?-Hbpt = 3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole) was prepared by hydrothermal reactions. The structure...A new coordination compound Zn(2,4'-bpt)2(H2O)(1) based on the versatile ligand 2,4'-Hbpt(2,4?-Hbpt = 3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole) was prepared by hydrothermal reactions. The structure of complex 1 has been characterized by X-ray single-crystal diffraction, elemental analysis, X-ray powder diffraction, IR spectrum analysis and thermogravimetric analysis. Single-crystal X-ray diffraction analysis indicates that the complex belongs to monoclinic system, space group C2/c with a = 23.877(3), b = 0.7483(9), c = 1.2492(2) A, b = 92.681(2)°, V = 2230.6(4) A^3, Z = 4, Dc = 1.572 g/cm^3, m = 1.143 mm^-1, Mr = 527.85 and F(000) = 1080. The final R = 0.0581 and wR = 0.0898 with I 〉 2s(I). 1 is a 0D motif which is connected by hydrogen bonds to form a corrugated 1D pattern. In addition, 1 shows strong photoluminescent emissions in the solid state at room temperature which can be used as potential optical materials. Theoretical calculations based on density functional theory(DFT) were employed in order to explicate the stability and chemical reactivity of 2,4'-Hbpt with different conformations. The results indicated that conformation I is more stable and prior to coordination in the reactions.展开更多
The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-cr...The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5)A,β = 99.364(2) °,V = 4332.58(18) A^3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm^-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.展开更多
The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined...The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215(9), b = 8.5311(4), c = 21.6886(9) A^°, β = 91.607(1)°, V = 3814.0(3)A^°^3, Z = 8, Dc = 1.400 g/cm^3, F(000) = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.展开更多
The title compound 8-chloro-3-((4-chlorobenzyl)thio)-[1,2,4]triazolo[4,3-a]pyridine was prepared from 1-chloro-4-(chloromethyl)benzene and 8-chloro-[1,2,4]triazolo[4,3-a]pyridine-3(2H)-thione in the presence o...The title compound 8-chloro-3-((4-chlorobenzyl)thio)-[1,2,4]triazolo[4,3-a]pyridine was prepared from 1-chloro-4-(chloromethyl)benzene and 8-chloro-[1,2,4]triazolo[4,3-a]pyridine-3(2H)-thione in the presence of Na OH, and its structure was determined by X-ray diffraction analysis. The crystal is of triclinic system, space group P1 with a = 6.8264(6), b = 7.5890(4), c = 13.0960(7) A, α = 93.447(4), β = 98.772(6), γ = 92.615(6)o, V = 668.26(8) A3, Z = 2, the final R = 0.035 and wR = 0.09 for 2259 observed reflections with I 〉 2σ(I). The preliminary biological test showed that the title compound has activities against Stemphylium lycopersici(Enjoji) Yamamoto, Fusarium oxysporum. sp. cucumebrium, and Botrytis cinerea with inhibitory to be 51.19%, 62.02% and 15.56%, respectively.展开更多
The title compound 1-(3-amino-[1,2,4]triazol-1-yl)-3,3-dimethyl-butan-2-one(3) was synthesized by Hofmann-alkylation reaction of 1-chloro-3,3-dimethyl-butan-2-one(1) and ~1H-[1,2,4]triazol-3-ylamine(2) with eq...The title compound 1-(3-amino-[1,2,4]triazol-1-yl)-3,3-dimethyl-butan-2-one(3) was synthesized by Hofmann-alkylation reaction of 1-chloro-3,3-dimethyl-butan-2-one(1) and ~1H-[1,2,4]triazol-3-ylamine(2) with equal amount of K_2CO_3 as acid acceptor. The structure of compound 3 was characterized by ~1H NMR, 13 C NMR, HRMS and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P21/n with a = 5.7227(8), b = 27.924(4), c = 6.2282(7) ?, β = 101.892(11)°, V = 973.9(2) ?~3, Z = 4, T = 180.00(10) K, μ(MoKα) = 0.087 mm^(-1), Dc = 1.243 g/cm^3, 3832 reflections measured(3.648≤θ≤26.022°), 1916 unique reflections(Rint = 0.0359, Rsigma = 0.0572) used in all calculations. The final R = 0.0557(I 〉 2σ(I)) and w R = 0.1276(all data). Bioassay showed that 3 displayed excellent activity as plant growth regulator with inducing lateral root formation and enhancing primary root elongation at 0.27 mmol/L(50 ppm) in soybeen(He Feng-50). Good water solubility was found with 50 mg in 1 m L of water. Therefore, application of 3 in agriculture is more environmentally friendly due to cosolvent-free condition, and results in improved abiotic-stress tolerance by affecting the root growth. And furthermore, it can be used as a precursor to investigate the function of regulating plant root growth.展开更多
A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravim...A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravimetric analysis,fluorescence spectrum,and singlecrystal X-ray diffraction.Yellow crystal crystallizes in the orthorhombic system,space group Pbca with a = 16.220(5),b = 14.980(5),c = 20.521(5) ?,V = 4986(3) ?~3,C(24)H(26)CdN4O7,Mr = 594.89,Dc = 1.585 g/cm^3,μ(Mo Kα) = 0.927 mm^(-1),F(000) = 2416,Z = 8,the final R = 0.0242 and w R = 0.0589 for 4076 observed reflections(I 〉 2s(I)).In 1,the Cd(Ⅱ) ion takes a six-coordination mode,and bib ligand bridges adjacent Cd(Ⅱ) ions to generate 1D zigzag chains; these neighboring chains are connected by O–H···O hydrogen bonding interactions,producing a 2D folded layered structure.Furthermore,by O–H···O hydrogen bonding between layers and layers,a 3D supramolecular architecture is formed.In addition,we analyzed Natural Bond Orbital(NBO) in using the PBE0/LANL2 DZ method built in Gaussian 03 Program.The calculation results indicated obvious covalent interaction between the coordinated atoms and Cd(Ⅱ) ion.展开更多
The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the prese...The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133(2),b = 5.7219(5),c = 21.942(2)(A°) ,β = 99.145(2)°,V = 3115.3(5)(A°)^3,Z = 8,Dc = 1.340 g/cm^3,Mr = 314.33,F(000) = 1328,μ = 0.097 mm-1,MoKa radiation(λ = 0.71073),R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I 〉 2σ(I).X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.展开更多
A new dimeric Mn(Ⅱ) complex,namely,[Mn(L)(PIP)]_2·H_2O(1),was synthesized under hydrothermal condition(H_2L = 3-carboxy-1-carboxymethyl-2-oxidopyridinium and PIP = 2-(pyridin-3-yl)-1H-imidazo[4,5-f][1...A new dimeric Mn(Ⅱ) complex,namely,[Mn(L)(PIP)]_2·H_2O(1),was synthesized under hydrothermal condition(H_2L = 3-carboxy-1-carboxymethyl-2-oxidopyridinium and PIP = 2-(pyridin-3-yl)-1H-imidazo[4,5-f][1,10]phenanthroline).It crystallizes in triclinic,space group P1 with a = 9.2037(13),b = 9.6794(13),c = 14.649(3) A,α = 94.858(3),β = 94.928(3),γ = 114.468(2)o,V = 1172.9(3) A^3,Z = 1,C_(52)H_(34)Mn_2N_(12)O_(11),Mr = 1112.79,Dc = 1.575 g/cm^3,F(000) = 568,μ(Mo Ka) = 0.618 mm^-1,R = 0.0432 and w R = 0.1151.In 1,two L anions bridge two Mn(Ⅱ) atoms to give a dimeric [Mn(L)(PIP)] unit with the Mn···Mn distance of 3.009(2) A.The two PIP ligands are located on both sides of the dimer,which provides suitable π-π stacking interactions between PIP ligands.By these π-π stacking interactions,adjacent dimers are extended into a two-dimensional supramolecular layer.Further,the strong N–H···O hydrogen bond stabilizes the supramolecular layer structure of 1.Moreover,the thermal behavior and luminescent property of 1 have been studied.展开更多
基金supported by the Natural Science Foundation of Hubei Province (No. 2008CDB016)the Research Project for Innovative Research Team of Hubei University for Nationalities
文摘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.
基金Supported by the National Natural Science Foundation of China(No.21576112)Natural Science Foundation of Jilin Province(20150623024TC-19,20170520147JH)the Science and Technology Development Plan of Siping City(2015049)
文摘Six new transition metal complexes, [Zn(HBTC)(PYTPY)]n·n PYTPY(1), [Cu(HBTC)(PYTPY)]n·n PYTPY(2), [Co(HBTC)(PYTPY)]n·n DMF(3), [Mn(HBTC)(PYTPY)]n·n DMF(4), [Cd(HBTC)(PYTPY)(H2O)]n·2nH2O(5), and [Co(HBTC)(PYTPY)(H2O)2](6),(H3BTC = 1,3,5-benzenetricarboxylic acid, PYTPY = 4'-(4-pyridyl)-2,2':6',2''-terpyridine, DMF = N,N?-dimethylformamide), have been synthesized and characterized by elemental analysis, IR and X-ray single-crystal diffraction. Complexes 1~5 all feature one-dimensional chain structures, and complex 6 exhibits a zero-dimensional structure. Complexes 1~5 present three-dimensional(3D) supramolecular frameworks via π-π stacking interactions, whenas 6 has also a 3D supramolecular structure assembled by hydrogen bonding. Meanwhile, complexes 1 ~ 6 exhibit the thermal stabilities and photoluminescent properties.
基金Supported by the National Natural Science Foundation of China (10874047)Natural Science Foundation of Guangdong Province (04300531)
文摘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.
基金Supported by the National Natural Science Foundation of China (Nos. 20872071 and 20911120069)the Natural Science Foundation of Tianjin (10JCZDJC17500)+2 种基金the National Key Project for Basic Research (2010CB126105)the Key Laboratory of Pesticide Chemistry and Application,Ministry of Agriculture (MOA) (No. MOAPCA200903)the Russian Foundation for Basic Research (grant numbers RFBR 08-03-00376 a and RFBR/NNSF 08-03-92208 a)
文摘The title compound naphthalen-2-yl-4-methyl-1,2,3-thiadiazole-5-carboxylate (C 14 H 10 N 2 O 2 S,M r=270.31) was synthesized by the reaction of 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride with 2-naphthol,and its structure was characterized by IR,1 H NMR,high-resolution mass spectrometry and single-crystal X-ray diffraction.The crystal belongs to orthorhombic,space group Pbcn with a=23.475(5),b=9.6640(19),c=10.814(2),β=90.00°,Z=8,V=2453.2(9) 3,M r=270.30,D c=1.464 g/cm 3,μ=0.262 mm-1,F(000)=1120,R=0.0444 and wR=0.1099.X-ray analysis revealed that the thiadiazole and naphthalene rings were non-planar,while the thiadiazole ring and the ester group were essentially planar,and two intermolecular hydrogen bonds C(6) H(6)···O(1) and C(14) H(14)···O(1) were observed.The preliminary biological test showed that the title compound had antifungal and antivirus activities against tobacco mosaic virus.
基金supported by the National Natural Science Foundation of China(No.21262012)the Natural Science Foundation of Hubei Province(No.2016CFB400)the State Undergraduate Innovative Training Program(No.201410517002)
文摘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.
基金Supported by the Institute Foundation of Siping City(No.2013036)
文摘A new Zn(Ⅱ) complex,[Zn(1,2,3-HBTC)(L)]2(1,L = 2-(2-chloro-6-fluorophenyl)-1H-imidazo[4,5-f][1,10]phenanthroline and 1,2,3-H3 BTC = 1,2,3-benzentricarboxylic acid),was synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction.It crystallizes in triclinic,space group P1 with a = 10.455(2),b = 11.533(2),c = 12.499(3) A,α = 116.97(3),β = 94.08(3),γ = 103.29(3)o,V = 1280.2(4) A^3,Z = 1,C56H28Cl2F2N8O12Zn2,Mr = 1244.50,Dc = 1.614 g/cm^3,F(000) = 628,μ(Mo Ka) = 1.124 mm^-1,R = 0.0502 and w R = 0.1417.In compound 1,two 1,2,3-HBTC anions bridge two Zn(Ⅱ) atoms to give a dimeric structure with Zn···Zn distance of 3.15 A.Adjacent dimers interact through π-π stackings between two L ligands to result in a supramolecular layer.Moreover,N–H···O and O–H···N hydrogen bonds further stabilize the 2D supramolecular architecture of 1.In addition,the luminescent property of 1 has been studied.
基金Supported by the Central University Basic Scientific Research Fund of Hunan University (2009)the Key Scientific and Technological Project of Changsha, Hunan Province (No. 0901077-31)
文摘The title compound has been synthesized by the reaction of 3,3-dimethyl-1-(1H-1,2,4-triazol-1-yl)butan-2-one oxime with 2-chlorobenzyl chloride, and then treated with 65~68% HNO3. Its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 14.5481(8), b = 9.3351(5), c = 13.1911(7) , β = 98.9450(10)°, Z = 4, V = 1769.67(17) 3, Mr = 369.81, Dc = 1.388 g/cm3, S = 1.06, μ = 0.247 mm-1, F(000) = 776, the final R = 0.0352 and wR = 0.0960 for 3069 observed reflections (I 2σ(I)). X-ray crystal structure presents the intramolecular N–H…O hydrogen bond. The packing is nearly parallel without π-π stacking interactions between two adjacent phenyl rings and stabilized by Van der Waals force. The preliminary bioassay shows that the title compound possesses fungicidal activity against Gibberella zeae at the dosage of 25 mg/L.
基金the Science Research Foundation of Henan Institute of Science and Technology (No. 06036)
文摘The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl- 1-phenyl-1H-pyrazol-4-yl)methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6)A, α = 112.566(1), β = 92.324(2), γ = 102.91(1)°, V= 1315.65(10) A^3, Z = 2, Dc = 1.344 g/cm^3,μ(MoKa) = 0.282 mm^-1, λ = 0.71073 A, F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C( 12)-H(12)…O(1) and C(28)-H(28)...O(1)# 1 hydrogen bonds were observed in the title compound.
基金supported by the National Natural Science Foundation of China (No. 20971004)the Natural Science Foundation of Anhui Province (No. 11040606M45)
文摘A novel coordination polymer, [Co3(bta)2(dpe)3(H2O)2]·2H2O (1, H3bta = benzene-1,3,5-triacetic acid, and dpe = 1,2-di(pyridin-4-yl)ethene), has been hydrothermally prepared and characterized by IR spectroscopy, elemental analysis and single-crystal X-ray diffraction. The crystal is of triclinic system, space group P , with a = 9.5687(15), b = 11.2470(17), c = 13.686(2) , α = 78.262(3), β = 89.271(4), γ = 81.292(3)°, V = 1425.2(4) 3, C60H56N6O16Co3, Mr = 1293.90, Dc = 1.508 g/cm3, F(000) = 667, μ = 0.940 mm-1 and Z = 1. The final R = 0.0707 and wR = 0.1413 for 4950 observed reflections (I 2σ(I)). In the title complex, the bta ligand acts as a four-dentate bridging ligand to link up cobalt atoms into lamellar frameworks which are further interlinked by the dpe ligands to generate a trinodal (3,4,6)-connected (4.62)2(42.68.83.102)(64.82) net.
基金This work was supported by the foundation of Natural Science Research of Jiangsu Education Department (02KJB150007)
文摘The title complex [Cu3L3(H2O)]DMFH2O (H2L = 4-(3-hydroxy-2-ethyl-4- pyridinone-1-yl)-aniline condensation salicylaldehyde) was obtained. The single-crystal X-ray study shows that it is a trinuclear compound [Cu3(C20H15N2O3)3(H2O)]DMFH2O. The coordi- nation sphere about each copper ion in the complex consists of two oxygen atoms from hydroxylpyridinone moiety of one ligand and one oxygen and one nitrogen atoms from salicyladehyde Schiff-base moiety of another ligand arranged in a slightly distorted square planar geometry. Among the three copper ions, one (Cu(2)) is coordinated by the other oxygen atom of water molecule on the fifth coordinate position to form a distorted square pyramid geometry. The crystal is of monoclinic, space group P21/c with a = 12.9202(5), b = 27.197(1), c = 17.0116(7) ? b = 100.588(1), V = 5875.9(4) 3, Z = 4, C63H57N7O12Cu3, Mr = 1294.78, Dc = 1.464 g/cm3, m = 1.146 mm-1, F(000) = 2668, R = 0.0784 and wR = 0.1546 for 6926 observed reflections with I > 2s(I). The differences of coordinate bond lengths are observed between anhydrous and hydrous units: in the former unit, the average bond lengths are 1.978 ?for CuN (azomethine), 1.883 ?for CuO (phenolic) in Schiff-base moiety, 1.959 ?for CuO (keto), and 1.919 ?for CuO (hydroxy) in hydroxypyridinone moiety; while those in the latter are longer with the following corresponding values: 1.985(5), 1.908(5), 1.993(5) and 1.919(4) ? respectively. The Cu(2)O (water) bond length is 2.375(6) ?
基金funded by National Natural Science Foundation of China(No.21002090)the National Key Technologies R&D Program(2011BAE06B03-01)
文摘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.
文摘The title compound N-tert-butyl-N(-(2,4-dichlorobenzoyl)-N-[1-(4-chlorophenyl)- 1,4-dihydro-6-methylpyridazine-4-oxo-3-carbonyl]hydrazine [(C23H_21N4O3Cl3)2·1.5H_2O, Mr = 1042.60] was prepared by the reaction of 1-(4-chlorophenyl)-1,4-dihydro-4-oxo-6- methylpyridazine-3-carboxylic acid with chloroformate ethyl ester, then with N′-tert-butyl-N- (2,4-dichlorobenzoyl) hydrazine in the present of triethylamine. The crystal structure has been determined by X-ray diffraction. The crystal belongs to Monoclinic, space group P21/c, with unit cell constants a =11.4948(9), b=12.7495(10), c=35.854(3) ?, β =92.964(2)°, Z=4, V=5247.6(7) ?3, Dc = 1.320 Mg/m3, F(000) = 2156 , μ (MoKa)= 0.385, R = 0.0661, wR = 0.1875, for 9151 observed reflections( I >2σ(I)). The structure is a dimer linked by intermolecular hydrogen bond which can be observed between N(1)- H...O(6), N(5)- H...O(3). The distances are 2.068 and 2.027? respectively.
基金Supported by the National Natural Science Foundation of China(Nos.21263019 and 51364038)
文摘A new coordination compound Zn(2,4'-bpt)2(H2O)(1) based on the versatile ligand 2,4'-Hbpt(2,4?-Hbpt = 3-(2-pyridyl)-5-(4-pyridyl)-1H-1,2,4-triazole) was prepared by hydrothermal reactions. The structure of complex 1 has been characterized by X-ray single-crystal diffraction, elemental analysis, X-ray powder diffraction, IR spectrum analysis and thermogravimetric analysis. Single-crystal X-ray diffraction analysis indicates that the complex belongs to monoclinic system, space group C2/c with a = 23.877(3), b = 0.7483(9), c = 1.2492(2) A, b = 92.681(2)°, V = 2230.6(4) A^3, Z = 4, Dc = 1.572 g/cm^3, m = 1.143 mm^-1, Mr = 527.85 and F(000) = 1080. The final R = 0.0581 and wR = 0.0898 with I 〉 2s(I). 1 is a 0D motif which is connected by hydrogen bonds to form a corrugated 1D pattern. In addition, 1 shows strong photoluminescent emissions in the solid state at room temperature which can be used as potential optical materials. Theoretical calculations based on density functional theory(DFT) were employed in order to explicate the stability and chemical reactivity of 2,4'-Hbpt with different conformations. The results indicated that conformation I is more stable and prior to coordination in the reactions.
基金Supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001)the Science Research Project of Yunyang Medical College (No.2008CXG01)
文摘The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5)A,β = 99.364(2) °,V = 4332.58(18) A^3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm^-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I 〉 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.
基金supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001) the Science Research Project of Yunyang Medical College (No. 2006QDJ16)
文摘The crystal structure of the title compound ethyl 3-(4-chlorophenyl)-3,4-dihydro-6- methyl-4-oxo-2-(pyrrolidin-1-yl)furo[2,3-d]pyrimidine-5-carboxylate (C20H20ClN3O4, Mr= 401.84) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215(9), b = 8.5311(4), c = 21.6886(9) A^°, β = 91.607(1)°, V = 3814.0(3)A^°^3, Z = 8, Dc = 1.400 g/cm^3, F(000) = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.
基金funded by the National Natural Science Foundation of China(No.21002090)the Natural Science Foundation of Zhejiang Province(No.LY16C140007)the public program of Science and Technology of Zhejiang Province(2014C31127,2013C32SA700134)
文摘The title compound 8-chloro-3-((4-chlorobenzyl)thio)-[1,2,4]triazolo[4,3-a]pyridine was prepared from 1-chloro-4-(chloromethyl)benzene and 8-chloro-[1,2,4]triazolo[4,3-a]pyridine-3(2H)-thione in the presence of Na OH, and its structure was determined by X-ray diffraction analysis. The crystal is of triclinic system, space group P1 with a = 6.8264(6), b = 7.5890(4), c = 13.0960(7) A, α = 93.447(4), β = 98.772(6), γ = 92.615(6)o, V = 668.26(8) A3, Z = 2, the final R = 0.035 and wR = 0.09 for 2259 observed reflections with I 〉 2σ(I). The preliminary biological test showed that the title compound has activities against Stemphylium lycopersici(Enjoji) Yamamoto, Fusarium oxysporum. sp. cucumebrium, and Botrytis cinerea with inhibitory to be 51.19%, 62.02% and 15.56%, respectively.
基金supported by the National Natural Science Foundation of China(No.2012BAD20B04)
文摘The title compound 1-(3-amino-[1,2,4]triazol-1-yl)-3,3-dimethyl-butan-2-one(3) was synthesized by Hofmann-alkylation reaction of 1-chloro-3,3-dimethyl-butan-2-one(1) and ~1H-[1,2,4]triazol-3-ylamine(2) with equal amount of K_2CO_3 as acid acceptor. The structure of compound 3 was characterized by ~1H NMR, 13 C NMR, HRMS and single-crystal X-ray diffraction. The compound crystallizes in the monoclinic system, space group P21/n with a = 5.7227(8), b = 27.924(4), c = 6.2282(7) ?, β = 101.892(11)°, V = 973.9(2) ?~3, Z = 4, T = 180.00(10) K, μ(MoKα) = 0.087 mm^(-1), Dc = 1.243 g/cm^3, 3832 reflections measured(3.648≤θ≤26.022°), 1916 unique reflections(Rint = 0.0359, Rsigma = 0.0572) used in all calculations. The final R = 0.0557(I 〉 2σ(I)) and w R = 0.1276(all data). Bioassay showed that 3 displayed excellent activity as plant growth regulator with inducing lateral root formation and enhancing primary root elongation at 0.27 mmol/L(50 ppm) in soybeen(He Feng-50). Good water solubility was found with 50 mg in 1 m L of water. Therefore, application of 3 in agriculture is more environmentally friendly due to cosolvent-free condition, and results in improved abiotic-stress tolerance by affecting the root growth. And furthermore, it can be used as a precursor to investigate the function of regulating plant root growth.
基金supported by the Science and Technology Development Project of Jilin Provincial Science&Technology Department(201205080)the Science and Technology Research Projects of the Education Office of Jilin Province(No.2013.384)
文摘A new complex [Cd(hba)2(bib)]n·nH2O(1,Hhba = 3-hydroxybenzoic acid,bib = 1,4-bis(imidazol-1-yl)-butane) has been hydrothermally synthesized and characterized by elemental analysis,IR spectrum,thermogravimetric analysis,fluorescence spectrum,and singlecrystal X-ray diffraction.Yellow crystal crystallizes in the orthorhombic system,space group Pbca with a = 16.220(5),b = 14.980(5),c = 20.521(5) ?,V = 4986(3) ?~3,C(24)H(26)CdN4O7,Mr = 594.89,Dc = 1.585 g/cm^3,μ(Mo Kα) = 0.927 mm^(-1),F(000) = 2416,Z = 8,the final R = 0.0242 and w R = 0.0589 for 4076 observed reflections(I 〉 2s(I)).In 1,the Cd(Ⅱ) ion takes a six-coordination mode,and bib ligand bridges adjacent Cd(Ⅱ) ions to generate 1D zigzag chains; these neighboring chains are connected by O–H···O hydrogen bonding interactions,producing a 2D folded layered structure.Furthermore,by O–H···O hydrogen bonding between layers and layers,a 3D supramolecular architecture is formed.In addition,we analyzed Natural Bond Orbital(NBO) in using the PBE0/LANL2 DZ method built in Gaussian 03 Program.The calculation results indicated obvious covalent interaction between the coordinated atoms and Cd(Ⅱ) ion.
基金supported by the National Natural Science Foundation of China (No. 20872051 and 21002009)the Scientific and Technological Project of Changzhou (CJ20115019)the Priority Academic Program Development of Jiangsu Higher Education Institutions
文摘The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133(2),b = 5.7219(5),c = 21.942(2)(A°) ,β = 99.145(2)°,V = 3115.3(5)(A°)^3,Z = 8,Dc = 1.340 g/cm^3,Mr = 314.33,F(000) = 1328,μ = 0.097 mm-1,MoKa radiation(λ = 0.71073),R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I 〉 2σ(I).X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.
基金Supported by the Institute Foundation of Siping city(No.2013036)
文摘A new dimeric Mn(Ⅱ) complex,namely,[Mn(L)(PIP)]_2·H_2O(1),was synthesized under hydrothermal condition(H_2L = 3-carboxy-1-carboxymethyl-2-oxidopyridinium and PIP = 2-(pyridin-3-yl)-1H-imidazo[4,5-f][1,10]phenanthroline).It crystallizes in triclinic,space group P1 with a = 9.2037(13),b = 9.6794(13),c = 14.649(3) A,α = 94.858(3),β = 94.928(3),γ = 114.468(2)o,V = 1172.9(3) A^3,Z = 1,C_(52)H_(34)Mn_2N_(12)O_(11),Mr = 1112.79,Dc = 1.575 g/cm^3,F(000) = 568,μ(Mo Ka) = 0.618 mm^-1,R = 0.0432 and w R = 0.1151.In 1,two L anions bridge two Mn(Ⅱ) atoms to give a dimeric [Mn(L)(PIP)] unit with the Mn···Mn distance of 3.009(2) A.The two PIP ligands are located on both sides of the dimer,which provides suitable π-π stacking interactions between PIP ligands.By these π-π stacking interactions,adjacent dimers are extended into a two-dimensional supramolecular layer.Further,the strong N–H···O hydrogen bond stabilizes the supramolecular layer structure of 1.Moreover,the thermal behavior and luminescent property of 1 have been studied.