Two new Cu(Ⅱ) coordination polymers, [Cu2(tbph)2(btb)2]n (1) and {[Cu2(tbph)2- (bth)2]·H2O}n (2), (H2tbph = 4-tert-butyl-phthalic acid, btb = 1,4-bis(1,2,4-triazol-1- yl)butane, bth = 1,6-bis(1...Two new Cu(Ⅱ) coordination polymers, [Cu2(tbph)2(btb)2]n (1) and {[Cu2(tbph)2- (bth)2]·H2O}n (2), (H2tbph = 4-tert-butyl-phthalic acid, btb = 1,4-bis(1,2,4-triazol-1- yl)butane, bth = 1,6-bis(1,2,4-triazol-l-yl)hexane), have been synthesized and characterized by elemental analysis, FT-IR and X-ray single-crystal diffraction. Complex 1 has a 2D sql layer. Complex 2 shows a (3,4)-connected 2D sheet with a (4.6^4.8)(4.8^2) topology. The thermal behavior of the two cor- responding complexes has briefly been investigated.展开更多
Starting with y-butyrolactone, 4-amino-3-(3-hydroxypropyl)-1H-1,2,4-triazole-5-(4H) thione 1 was prepared, and cyclization of it with 4-phenylbromoacetophenone gave 6-(4-biphenylyl)- 3-(3-hydroxypropyl)-7H-1,2...Starting with y-butyrolactone, 4-amino-3-(3-hydroxypropyl)-1H-1,2,4-triazole-5-(4H) thione 1 was prepared, and cyclization of it with 4-phenylbromoacetophenone gave 6-(4-biphenylyl)- 3-(3-hydroxypropyl)-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine Ⅱ. The structures of Ⅰ and Ⅱ were determined by elemental analyses, IR, ^1H NMR, ^13C NMR, and X-ray diffraction. Crystal data for 1: C5H10N4OS, Mr = 174.23, monoclinic system, space group P21/c, a =8.4568(6), b = 22.8905(16), c = 9.2625(6) A, β= 114.172(1)°, V= 1635.82(19) A^3, F(000) = 736, Z= 8, Dc = 1.415 g/cm^3, 2 λ=0.71073 A,μ = 0.346 mm^-1 and the final R = 0.0603 for 2870 unique reflections with 1993 observed ones (I 〉 2σ(I). Crystal data for Ⅱ: C19H18N4OS, Mr = 350.43, monoclinic system, space group P21/c, a = 6.7481(7), b = 8.2647(8), c = 30.075(3) A, β= 94.445(2)°, V= 1672.3(3) A3, F(000) = 736, Z = 4, Dc = 1.392 g/cm^3, λ=0.71073 A,μ= 0.209 mm^-1 and the final R = 0.0667 for 3000 unique reflections with 2534 observed ones (I 〉 2σ(I)). In the crystal of compound Ⅱ, the five-membered triazole ring and two benzene rings are coplanar, while the six-membered thiadiazine ring is slightly distorted, with an r.m.s deviation of 0.227(1) A. Some hydrogen bonding interactions are observed and π-π stacking interactions between adjacent molecules are found in the packing diagrams of the two compounds.展开更多
The crystal structure of the title compound 3-phenyl-6-(4-methylphenyl)-1,2,4- triazolo[4,3-b]-1,2,4-triazine (C17H13N5, Mr = 287.32) was synthesized and determined by singlecrystal X-ray diffraction. It belongs t...The crystal structure of the title compound 3-phenyl-6-(4-methylphenyl)-1,2,4- triazolo[4,3-b]-1,2,4-triazine (C17H13N5, Mr = 287.32) was synthesized and determined by singlecrystal X-ray diffraction. It belongs to monoclinic, space group P21/c, with α = 11.4038(18), b = 11.7675(18), c = 11.0904(18) A, β = 108.439(7)°, V = 1411.9(4) A^3, Z = 2, Dc = 1.352 g/cm^3, p = 0.085 mm^-1, F(000) = 600, R = 0.0445 and wR = 0.1041 for 2888 unique reflections with 1501 observed ones (I 〉20(I)). In the crystal structure, the triazine moiety is almost coplanar with the triazole ring, and the largest deviation for atom C(4) is -0.026 A. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.展开更多
The solvothermal reaction of 3-amino-1H-1,2,4-triazole (ttr) with Zn(ClO4)2·6H2O and NaCl in a 1:1:1 molar ratio gave a new complex [Zn(ttr)Cl]n with a 3-connected (4.82) 2-D structure. The layers stack...The solvothermal reaction of 3-amino-1H-1,2,4-triazole (ttr) with Zn(ClO4)2·6H2O and NaCl in a 1:1:1 molar ratio gave a new complex [Zn(ttr)Cl]n with a 3-connected (4.82) 2-D structure. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interactions to form the crystal structure. The complex [Zn(ttr)Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369(1), b = 10.049(1), c = 11.905(1)A, V = 1120.9(3)A^3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm^3,μ = 4.740 mm^-1, F(000) = 720, S = 1.059 and T = 293(2) K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with Ⅰ〉 2σ(Ⅰ), and R = 0.0689 and wR = 0.2504 for all data.展开更多
The title compound, Co(L)2(CH3OH)2Cl2 (L = 3-(1,2,4-triazole-yl)-6-chloro-pyridazine) 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the tric...The title compound, Co(L)2(CH3OH)2Cl2 (L = 3-(1,2,4-triazole-yl)-6-chloro-pyridazine) 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018(3), b = 9.832(5), c = 9.921(5)A, a = 78.270(8), β = 74.550(8), γ = 83.807(8)°, V = 553.1(5)A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F(000) = 281,μ(MoKα) = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ(I). The Co(II) ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt(II) complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.展开更多
Two new cadmium(II) and zinc(II) coordination polymers, {[Cd(btre)0.5- (mip)(H2O)2]·H2O}n (1) and [Zn(btre)(mip)]n (2), were synthesized at room temperature condition and characterized by IR spe...Two new cadmium(II) and zinc(II) coordination polymers, {[Cd(btre)0.5- (mip)(H2O)2]·H2O}n (1) and [Zn(btre)(mip)]n (2), were synthesized at room temperature condition and characterized by IR spectra, elemental analyses, single-crystal and powder X-ray diffractions (btre = 1,2-bis(1,2,4-triazol-4-yl)ethane, H2mip = 5-methyl-1,3-benzenedicarboxylic acid). Complex 1 belongs to the triclinic system, P space group, with a = 8.9830(6), b = 10.0579(6), c = 10.2479(9) , α = 98.837(6), β = 115.975(8), γ = 106.370(6)°, V = 756.30(11) 3 and Z = 2; complex 2 crystallizes in monoclinic, space group P21/c, with a = 7.0332(3), b = 14.9947(7), c = 15.9689(7) ?, β = 97.1170(10)°, V = 1671.12(13) ?3 and Z = 4. Compounds 1 and 2 based on the same N/O-donor ligands show different structures. The one-dimensional chains of 1 are further linked by hydrogen bonding and π-π interactions to yield a three-dimensional supramolecular structure. The two-dimensional (6,3) networks of 2 are further extended into a 3D framework via π-π interactions. Thermal stabilities and luminescence of 1 and 2 were investigated.展开更多
Studying of charge-transfer (CT) and proton transfer interactions is essential due to their important role in many biological field and industrial applications. The current work will add more information’s about the ...Studying of charge-transfer (CT) and proton transfer interactions is essential due to their important role in many biological field and industrial applications. The current work will add more information’s about the nature of interaction between 3,5-diamino-1,2,4-triazole (DAT) and 6-methyl-1,3,5-triazine-2,4-diamine (MTDA) with 3,6-dichloro-2,5-dihydroxy-p-benzoquinone (chloranilic acid CLA) which was studied spectrophotometrically in Ethanol (EtOH) and Methanol (MeOH) solvents at different temperatures. The molecular composition of the formed complexes was studied by applying continuous variation and spectrophotometric titration methods and found to be 1:1 charge transfer complex for both Complex (DAT:CLA) and (MTDA:CLA) which are produced. Minimum-Maximum absorbance’s method has been applied to calculate the formation constant KCT and molecular extinction coefficient (ε);they recorded high values confirming high stability of the produced complexes. Oscillator strength (f), transition dipole moment (μ), ionization potential (IP) and dissociation energy (W) of the formed CT-complexes were also determined and evaluated;they showed solvent dependency. It is concluded that the formation constant (KCT) of the complexes is found to depend on the nature of both electron acceptor and donors and on the polarity of solvents.展开更多
Solvothermal reactions of 3,5-dimethyl-2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl) pyridine (L), 1,4-benzendicarboxylic acid (H2bdc), and transitional metal cations of M11 (M = Mn, Co, Cd) in the presence of oxa...Solvothermal reactions of 3,5-dimethyl-2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl) pyridine (L), 1,4-benzendicarboxylic acid (H2bdc), and transitional metal cations of M11 (M = Mn, Co, Cd) in the presence of oxalic acid (H2ox) afford three novel supramolecular polymers (CPs), namely, {[M2(ox)(L)2][bdc][M2(Hox)2(OH)(H2O)4]·3H2O}n (M = Mn for 1, Co for 2, Cd for 3). Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2(ox)(L)2]2+ building block. The bdc2- ligand linked with the unprecedented [M2(Hox)2(OH)2(H2O)4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.展开更多
A series of diheterocyclic compounds containing 1,2,4-triazolo [1,5-a]pyrimidine and 1, 3,4-oxadiazole were designed and synthesized starting from 2-mercapto-5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine. The structure...A series of diheterocyclic compounds containing 1,2,4-triazolo [1,5-a]pyrimidine and 1, 3,4-oxadiazole were designed and synthesized starting from 2-mercapto-5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine. The structure of all compounds prepared were confirmed by H-1 NMR spectroscopy and elemental analysis. The preliminary bioassay indicated that the title compounds displayed good fungicidal activity against Rhizoctonia solani.展开更多
In order to find leading compounds with an excellent fungicidal activity, the title compound 2-( 1,3-dithiolan-2- yl-idene)-1-phenyl-2-( 1,2,4-tfiazol-1-yl) ethanone was synthesized according to the biological iso...In order to find leading compounds with an excellent fungicidal activity, the title compound 2-( 1,3-dithiolan-2- yl-idene)-1-phenyl-2-( 1,2,4-tfiazol-1-yl) ethanone was synthesized according to the biological isosterism and its structure was confirmed by means of IR, MS, ^1 H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound exhibits some biological activities.展开更多
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 diffracti...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.展开更多
The thermal decomposition of ammonium 3-nitro-1,2,4-triazol-5-onate monohydrate[NH4(NTO)·H2O] was studied by means of thermal analysis-MS coupling and the combination technique of in situ thermolysis cell with ...The thermal decomposition of ammonium 3-nitro-1,2,4-triazol-5-onate monohydrate[NH4(NTO)·H2O] was studied by means of thermal analysis-MS coupling and the combination technique of in situ thermolysis cell with rapid-scan Fourier transform infrared spectroscopy. The results show that there are two endothermic steps and one exothermic step in the decomposition process of NH4(NTO)·H2O. The detected gas products consist of NH3, H2O, N2, CO2, CO, and NO2.展开更多
The title compound 1-((5-(4-(4-chlorophenoxy)-2-chlorophenyl)-2,2,3-trimethyl-oxazolidin- 5-yl)methyl)-lH-1,2,4-triazole (C21H22Cl2N4O2)has been synthesized and characterized by elemental analysis, IR, 1H NM...The title compound 1-((5-(4-(4-chlorophenoxy)-2-chlorophenyl)-2,2,3-trimethyl-oxazolidin- 5-yl)methyl)-lH-1,2,4-triazole (C21H22Cl2N4O2)has been synthesized and characterized by elemental analysis, IR, 1H NMR, MS and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.891(2), b = 9.074(2), c = 18.258(4)AA, α = 99.292(4), β = 95.105(4), γ = 108.068(3)°, C21H22Cl2N4O2, Mr = 433.33, V= 1059.3(4) Aa, Z = 2, Dc = 1.359 g/cm3, F(000) = 452,μ = 0.331 mm-1, the final R = 0.0448 and wR = 0.0994 for 3727 unique reflections. The dihedral angle between the oxazolidine ring taking an envelope conformation with a local pseudo-mirror and the triazole ring is 27.7(9)°. Weak intermolecular C-H...N hydrogen bonds and π-π interactions exist between the triazole rings of neighboring molecules, forming a three-dimensional network, which stabilizes the crystal structure. The primary biological test shows the target compound has certain fungicidal activity.展开更多
Twelve new (3-benzyl-4-aroyl-1,2,4-triazole-5-yl)[5-(3,4,5-trimethoxyphenyl)-1,3,4- oxadiazole-2-yl]sulfides(2) have been synthesized from the nucleophilic displacements of 3-benzyl-4- trimethoxyphenyl)-1,3,4-oxadiazo...Twelve new (3-benzyl-4-aroyl-1,2,4-triazole-5-yl)[5-(3,4,5-trimethoxyphenyl)-1,3,4- oxadiazole-2-yl]sulfides(2) have been synthesized from the nucleophilic displacements of 3-benzyl-4- trimethoxyphenyl)-1,3,4-oxadiazole(1). Compounds(2) were screened for their antibacterial activity against E.Coli at 0.01%. The results show that some compounds(2) have strong inhibiting effects展开更多
The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline- 1,3-dione (C12H10NaO2S, Mr= 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and s...The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline- 1,3-dione (C12H10NaO2S, Mr= 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and substitution reactions, and its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2/c with a = 12.264(3), b = 14.646(3), c = 14.349(4) A,β = 91.69(3)°,μ = 0.255 mm1, Mr = 274.30, V = 2576.2(10) A3, Z =8, Dc = 1.414 g/cm3, F(000) = 1136, R = 0.0487 and wR = 0.1329 for 4048 observed reflections with I 〉 2σ(I). In addition, the preliminary bioassay suggested that the title compound 6 exhibits relatively good antitumor activity against HT-29 and MCF-7.展开更多
A novel compound 5-(p-tolyl)-4-[2-(2,4-dichlorophenoxy)acetamido]-1,2,4-tria zole- 3-thione 2a has been synthesized by the reaction of 5-(p-tolyl)-4-amino-1,2,4-triazole-3-thione 1 with 2-(2,4-dich/orophenoxy)...A novel compound 5-(p-tolyl)-4-[2-(2,4-dichlorophenoxy)acetamido]-1,2,4-tria zole- 3-thione 2a has been synthesized by the reaction of 5-(p-tolyl)-4-amino-1,2,4-triazole-3-thione 1 with 2-(2,4-dich/orophenoxy)acetyl ch/oride. Interestingly, the title compound 2 was obtained when 2a crystallizes from a mixed solution of petroleum ether and ethyl acetate, and it has been characterized by elemental analysis, IR, ^1H NMR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 9.780(5), b = 10.876(6), c = 11.615(6) /A, a = 104.822(7), β= 94.105(6), ), = 94.305(6)°, V= 1185.7(11)/A3, Z = 2,μ = 0.397 mm^-1, Mr= 497.39, Dx= 1.393 g/cm^3, F(000) = 516, S = 1.097, the final R = 0.0730 and wR = 0.2133 for 4111 unique reflections (Rint = 0.0525) with 3212 observed ones. The dihedral angles made by the triazole ring with the methyl- and chloro-substituted benzene rings are 43.5(7) and 50.2(9)°, respectively. Some intra- and intermolecular hydrogen bonds together with C-H…π interactions existing in the lattice stabilize the crystal structure.展开更多
The title compound, N′-(4-methoxybenzylidene)-2-(1%H%-1,2,4-triazol-1-yl)acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS, 1H NMR and elemental analysis. The single crystal structure...The title compound, N′-(4-methoxybenzylidene)-2-(1%H%-1,2,4-triazol-1-yl)acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS, 1H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.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
基金Supported financially by Henan Province basic and frontier technology research projects of Henan Provincial Department of Science and Technology(No.142300410083)
文摘Two new Cu(Ⅱ) coordination polymers, [Cu2(tbph)2(btb)2]n (1) and {[Cu2(tbph)2- (bth)2]·H2O}n (2), (H2tbph = 4-tert-butyl-phthalic acid, btb = 1,4-bis(1,2,4-triazol-1- yl)butane, bth = 1,6-bis(1,2,4-triazol-l-yl)hexane), have been synthesized and characterized by elemental analysis, FT-IR and X-ray single-crystal diffraction. Complex 1 has a 2D sql layer. Complex 2 shows a (3,4)-connected 2D sheet with a (4.6^4.8)(4.8^2) topology. The thermal behavior of the two cor- responding complexes has briefly been investigated.
基金This work was supported by the Natural Science Foundation of Zhejiang Province (No. M203149)
文摘Starting with y-butyrolactone, 4-amino-3-(3-hydroxypropyl)-1H-1,2,4-triazole-5-(4H) thione 1 was prepared, and cyclization of it with 4-phenylbromoacetophenone gave 6-(4-biphenylyl)- 3-(3-hydroxypropyl)-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine Ⅱ. The structures of Ⅰ and Ⅱ were determined by elemental analyses, IR, ^1H NMR, ^13C NMR, and X-ray diffraction. Crystal data for 1: C5H10N4OS, Mr = 174.23, monoclinic system, space group P21/c, a =8.4568(6), b = 22.8905(16), c = 9.2625(6) A, β= 114.172(1)°, V= 1635.82(19) A^3, F(000) = 736, Z= 8, Dc = 1.415 g/cm^3, 2 λ=0.71073 A,μ = 0.346 mm^-1 and the final R = 0.0603 for 2870 unique reflections with 1993 observed ones (I 〉 2σ(I). Crystal data for Ⅱ: C19H18N4OS, Mr = 350.43, monoclinic system, space group P21/c, a = 6.7481(7), b = 8.2647(8), c = 30.075(3) A, β= 94.445(2)°, V= 1672.3(3) A3, F(000) = 736, Z = 4, Dc = 1.392 g/cm^3, λ=0.71073 A,μ= 0.209 mm^-1 and the final R = 0.0667 for 3000 unique reflections with 2534 observed ones (I 〉 2σ(I)). In the crystal of compound Ⅱ, the five-membered triazole ring and two benzene rings are coplanar, while the six-membered thiadiazine ring is slightly distorted, with an r.m.s deviation of 0.227(1) A. Some hydrogen bonding interactions are observed and π-π stacking interactions between adjacent molecules are found in the packing diagrams of the two compounds.
基金The project was supported by the NNSFC (20572057) and NSF of Shandong Province (Y2006B011)
文摘The crystal structure of the title compound 3-phenyl-6-(4-methylphenyl)-1,2,4- triazolo[4,3-b]-1,2,4-triazine (C17H13N5, Mr = 287.32) was synthesized and determined by singlecrystal X-ray diffraction. It belongs to monoclinic, space group P21/c, with α = 11.4038(18), b = 11.7675(18), c = 11.0904(18) A, β = 108.439(7)°, V = 1411.9(4) A^3, Z = 2, Dc = 1.352 g/cm^3, p = 0.085 mm^-1, F(000) = 600, R = 0.0445 and wR = 0.1041 for 2888 unique reflections with 1501 observed ones (I 〉20(I)). In the crystal structure, the triazine moiety is almost coplanar with the triazole ring, and the largest deviation for atom C(4) is -0.026 A. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.
基金The project was supported by the NNSFC (20571075, 20521101)the NSF for Distinguished Young Scientists of China (20425104) the NSF of Fujian Province (A0420002)
文摘The solvothermal reaction of 3-amino-1H-1,2,4-triazole (ttr) with Zn(ClO4)2·6H2O and NaCl in a 1:1:1 molar ratio gave a new complex [Zn(ttr)Cl]n with a 3-connected (4.82) 2-D structure. The layers stack in the -ABAB- way along the c axis with abundant hydrogen bonding interactions to form the crystal structure. The complex [Zn(ttr)Cl]n crystallizes in the orthorhombic space group Pbca with a = 9.369(1), b = 10.049(1), c = 11.905(1)A, V = 1120.9(3)A^3, Z = 8.00, C2N4H3ZnCl, Mr = 183.90, Dc = 2.180 g/cm^3,μ = 4.740 mm^-1, F(000) = 720, S = 1.059 and T = 293(2) K. The final R = 0.0662 and wR = 0.2457 for 956 observed reflections with Ⅰ〉 2σ(Ⅰ), and R = 0.0689 and wR = 0.2504 for all data.
文摘The title compound, Co(L)2(CH3OH)2Cl2 (L = 3-(1,2,4-triazole-yl)-6-chloro-pyridazine) 1, has been synthesized and its crystal structure has been determined by X-ray analysis. Complex 1 crystallizes in the triclinic system, space group P1 with a = 6.018(3), b = 9.832(5), c = 9.921(5)A, a = 78.270(8), β = 74.550(8), γ = 83.807(8)°, V = 553.1(5)A^3, Z = 1, C14H16Cl4CoN10O2, Mr = 557.10, Dc = 1.673 g/cm^3, F(000) = 281,μ(MoKα) = 1.293 mm^-1, the final R = 0.0453 and wR = 0.1181 for 1539 observed reflections with I 〉 2σ(I). The Co(II) ion is in a distorted centrosymmetric six-coordinate octahedral environment with two Ntriazole, two Omethanol and two Cl atoms. Via hydrogen bonds the configuration of 1 has been extended into 1D chains which are developed to 2D layers via π-π sticking action, and these layers are further extended into a 3D network by hydrogen bonds. The antibacterial activity of the title compound has been detected, and the results show that the ligands and cobalt(II) complex exhibit certain fungicidal activity against several bacteria. Furthermore, the spectral properties of the title compound have been also studied and discussed.
基金Supported by the Natural Science Foundation of Anhui Province(KJ2016A512)Key projects of Anhui Province University Outstanding Youth Talent Support Program(gxyqZD2016372)
文摘Two new cadmium(II) and zinc(II) coordination polymers, {[Cd(btre)0.5- (mip)(H2O)2]·H2O}n (1) and [Zn(btre)(mip)]n (2), were synthesized at room temperature condition and characterized by IR spectra, elemental analyses, single-crystal and powder X-ray diffractions (btre = 1,2-bis(1,2,4-triazol-4-yl)ethane, H2mip = 5-methyl-1,3-benzenedicarboxylic acid). Complex 1 belongs to the triclinic system, P space group, with a = 8.9830(6), b = 10.0579(6), c = 10.2479(9) , α = 98.837(6), β = 115.975(8), γ = 106.370(6)°, V = 756.30(11) 3 and Z = 2; complex 2 crystallizes in monoclinic, space group P21/c, with a = 7.0332(3), b = 14.9947(7), c = 15.9689(7) ?, β = 97.1170(10)°, V = 1671.12(13) ?3 and Z = 4. Compounds 1 and 2 based on the same N/O-donor ligands show different structures. The one-dimensional chains of 1 are further linked by hydrogen bonding and π-π interactions to yield a three-dimensional supramolecular structure. The two-dimensional (6,3) networks of 2 are further extended into a 3D framework via π-π interactions. Thermal stabilities and luminescence of 1 and 2 were investigated.
文摘Studying of charge-transfer (CT) and proton transfer interactions is essential due to their important role in many biological field and industrial applications. The current work will add more information’s about the nature of interaction between 3,5-diamino-1,2,4-triazole (DAT) and 6-methyl-1,3,5-triazine-2,4-diamine (MTDA) with 3,6-dichloro-2,5-dihydroxy-p-benzoquinone (chloranilic acid CLA) which was studied spectrophotometrically in Ethanol (EtOH) and Methanol (MeOH) solvents at different temperatures. The molecular composition of the formed complexes was studied by applying continuous variation and spectrophotometric titration methods and found to be 1:1 charge transfer complex for both Complex (DAT:CLA) and (MTDA:CLA) which are produced. Minimum-Maximum absorbance’s method has been applied to calculate the formation constant KCT and molecular extinction coefficient (ε);they recorded high values confirming high stability of the produced complexes. Oscillator strength (f), transition dipole moment (μ), ionization potential (IP) and dissociation energy (W) of the formed CT-complexes were also determined and evaluated;they showed solvent dependency. It is concluded that the formation constant (KCT) of the complexes is found to depend on the nature of both electron acceptor and donors and on the polarity of solvents.
基金supported by the National Natural Science Foundation of China (No. 21101097)Natural Science Foundation of Shandong Province (ZR2010BQ023)the State Key Laboratory of Solid Lubrication (No. 0701)
文摘Solvothermal reactions of 3,5-dimethyl-2,6-bis(3-(pyrid-2-yl)-1,2,4-triazolyl) pyridine (L), 1,4-benzendicarboxylic acid (H2bdc), and transitional metal cations of M11 (M = Mn, Co, Cd) in the presence of oxalic acid (H2ox) afford three novel supramolecular polymers (CPs), namely, {[M2(ox)(L)2][bdc][M2(Hox)2(OH)(H2O)4]·3H2O}n (M = Mn for 1, Co for 2, Cd for 3). Single-crystal X-ray diffraction analysis reveals that complexes 1-3 are isostructural and the 3D supramolecular structure was connected through non-covalent interactions. With the help of H2ox, the L ligands cheated with center atoms forming a butterfly [M2(ox)(L)2]2+ building block. The bdc2- ligand linked with the unprecedented [M2(Hox)2(OH)2(H2O)4] units through strong O-H...O hydrogen bonds forming a zigzag chain, which are further connected through π-π interactions between L and bdc2- ligands to form a 3D supramolecular structure. Moreover, elemental analyses, IR, thermogravimetric, PXRD and luminescence have been investigated.
基金The project was supported by the NNSF of China (Grant No. 29802002) the NSF of Hubei Province the Dawn Plan of Science and Technology for Young Scientists of Wuhan City and Foundation for University Key Teacher by the Ministry of Education of China.
文摘A series of diheterocyclic compounds containing 1,2,4-triazolo [1,5-a]pyrimidine and 1, 3,4-oxadiazole were designed and synthesized starting from 2-mercapto-5,7-dimethyl-1,2,4-triazolo[1,5-a]pyrimidine. The structure of all compounds prepared were confirmed by H-1 NMR spectroscopy and elemental analysis. The preliminary bioassay indicated that the title compounds displayed good fungicidal activity against Rhizoctonia solani.
文摘In order to find leading compounds with an excellent fungicidal activity, the title compound 2-( 1,3-dithiolan-2- yl-idene)-1-phenyl-2-( 1,2,4-tfiazol-1-yl) ethanone was synthesized according to the biological isosterism and its structure was confirmed by means of IR, MS, ^1 H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound exhibits some biological activities.
基金supported by National Natural Science Foundation of China(No.21002090)the Key Innovation Team of Science and Technology in Zhejiang Province(2010R50018-06)the National Key Technologies R&D Program(2011BAE06B03-01)
文摘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.
文摘The thermal decomposition of ammonium 3-nitro-1,2,4-triazol-5-onate monohydrate[NH4(NTO)·H2O] was studied by means of thermal analysis-MS coupling and the combination technique of in situ thermolysis cell with rapid-scan Fourier transform infrared spectroscopy. The results show that there are two endothermic steps and one exothermic step in the decomposition process of NH4(NTO)·H2O. The detected gas products consist of NH3, H2O, N2, CO2, CO, and NO2.
文摘The title compound 1-((5-(4-(4-chlorophenoxy)-2-chlorophenyl)-2,2,3-trimethyl-oxazolidin- 5-yl)methyl)-lH-1,2,4-triazole (C21H22Cl2N4O2)has been synthesized and characterized by elemental analysis, IR, 1H NMR, MS and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pi with a = 6.891(2), b = 9.074(2), c = 18.258(4)AA, α = 99.292(4), β = 95.105(4), γ = 108.068(3)°, C21H22Cl2N4O2, Mr = 433.33, V= 1059.3(4) Aa, Z = 2, Dc = 1.359 g/cm3, F(000) = 452,μ = 0.331 mm-1, the final R = 0.0448 and wR = 0.0994 for 3727 unique reflections. The dihedral angle between the oxazolidine ring taking an envelope conformation with a local pseudo-mirror and the triazole ring is 27.7(9)°. Weak intermolecular C-H...N hydrogen bonds and π-π interactions exist between the triazole rings of neighboring molecules, forming a three-dimensional network, which stabilizes the crystal structure. The primary biological test shows the target compound has certain fungicidal activity.
文摘Twelve new (3-benzyl-4-aroyl-1,2,4-triazole-5-yl)[5-(3,4,5-trimethoxyphenyl)-1,3,4- oxadiazole-2-yl]sulfides(2) have been synthesized from the nucleophilic displacements of 3-benzyl-4- trimethoxyphenyl)-1,3,4-oxadiazole(1). Compounds(2) were screened for their antibacterial activity against E.Coli at 0.01%. The results show that some compounds(2) have strong inhibiting effects
基金supported by the National Natural Science Foundation of China(21102069 and 21372113)the Project of Science and Technology New Star in Zhujiang Guangzhou city(No.2012J2200051)
文摘The title compound 2-(3-methyl-5-(methylthio)-4H-1,2,4-triazol-4-yl)isoindoline- 1,3-dione (C12H10NaO2S, Mr= 274.30) has been synthesized by a three-step procedure including the cyclization, hydrazinolysis and substitution reactions, and its crystal structure was determined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P2/c with a = 12.264(3), b = 14.646(3), c = 14.349(4) A,β = 91.69(3)°,μ = 0.255 mm1, Mr = 274.30, V = 2576.2(10) A3, Z =8, Dc = 1.414 g/cm3, F(000) = 1136, R = 0.0487 and wR = 0.1329 for 4048 observed reflections with I 〉 2σ(I). In addition, the preliminary bioassay suggested that the title compound 6 exhibits relatively good antitumor activity against HT-29 and MCF-7.
基金supported by the NN S F of China (No. 20672073)Shanghai Leading Academic Discipline (No. T0402)
文摘A novel compound 5-(p-tolyl)-4-[2-(2,4-dichlorophenoxy)acetamido]-1,2,4-tria zole- 3-thione 2a has been synthesized by the reaction of 5-(p-tolyl)-4-amino-1,2,4-triazole-3-thione 1 with 2-(2,4-dich/orophenoxy)acetyl ch/oride. Interestingly, the title compound 2 was obtained when 2a crystallizes from a mixed solution of petroleum ether and ethyl acetate, and it has been characterized by elemental analysis, IR, ^1H NMR spectra and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 9.780(5), b = 10.876(6), c = 11.615(6) /A, a = 104.822(7), β= 94.105(6), ), = 94.305(6)°, V= 1185.7(11)/A3, Z = 2,μ = 0.397 mm^-1, Mr= 497.39, Dx= 1.393 g/cm^3, F(000) = 516, S = 1.097, the final R = 0.0730 and wR = 0.2133 for 4111 unique reflections (Rint = 0.0525) with 3212 observed ones. The dihedral angles made by the triazole ring with the methyl- and chloro-substituted benzene rings are 43.5(7) and 50.2(9)°, respectively. Some intra- and intermolecular hydrogen bonds together with C-H…π interactions existing in the lattice stabilize the crystal structure.
文摘The title compound, N′-(4-methoxybenzylidene)-2-(1%H%-1,2,4-triazol-1-yl)acetohydrazide, was synthesized and its structure was confirmed by means of IR, MS, 1H NMR and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test shows that the synthesized compound has a low antifungal activity.
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.