The title compound, (E)-1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)- 3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol (3a), was synthesized by the Aldol con- densation reaction of 1-(7-methox...The title compound, (E)-1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)- 3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol (3a), was synthesized by the Aldol con- densation reaction of 1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)-2-(1,2,4-triazol- 1-yl)ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction: monoclinic system, space group P21 with a = 6.2002(3), b = 12.8452(7), c = 13.2257(7) ?, Z = 2, V = 1031.23(9) ?3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F(000) = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections (I 〉 2σ(I)). X-ray analysis displays that the title compound adopts an E configuration for the C(7)=C(8) double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O(1)–H???N(3). The antitumor assay exhibits that the title compound 3a (E configuration) has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b (Z configuration).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, C9H9N5OS, was synthesized by the reaction of 3-(1H)-1,2,4 -triazole hydrazine with 3-methyl-2-thiophenecarboxaldehyde in ethanol. The single crystal structure has been determined by X-ray diffrac...The title compound, C9H9N5OS, was synthesized by the reaction of 3-(1H)-1,2,4 -triazole hydrazine with 3-methyl-2-thiophenecarboxaldehyde in ethanol. The single crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group P2 1/n with a = 9.5550(10), b = 11.9847(12), c = 10.1074(11) A,β= 112.995(2)° V= 1065.47(19) A^3, Z = 4,μ = 0.290 mm^-1, Mr= 235.27, Dc = 1.467 g/cm^3 and F(000) = 488. The structure was solved by direct methods and refined to R = 0.0449. The crystal structure involves intermolecular hydrogen bonds of N-H…O and N-H…N as well as intramolecular hydrogen bond of N-H…N. Its biological activity has also been determined showing this type of compounds has certain antibacterial activity.展开更多
The compound of 3,5-diazido-1,2,4-triazole was synthesized by the reaction of 2,5,2',5'-tetrachloro-1,1'-azo-1,3,4-triazole with sodium azide at 50 ℃.Its crystal structure was determined by single-crystal X-ray di...The compound of 3,5-diazido-1,2,4-triazole was synthesized by the reaction of 2,5,2',5'-tetrachloro-1,1'-azo-1,3,4-triazole with sodium azide at 50 ℃.Its crystal structure was determined by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group Cc with a=1.212 4(2) nm,b=2.342 4(5) nm,c=0.804 74(16) nm,β=125.56(3)°,V=1.859 3(6) nm3,Z=4,C2HN9,Mr=151.04,Dc=1.62 g/cm3,F(000)=912 and μ(MoKa)=0.129 mm-1,the final R=0.039 7 and wR=0.087 4.X-ray analysis indicates a stronger intermolecular hydrogen bonding,leading to the formation of a trimmer,containing a nine-membered cyclic ring with graph-set R33(9) in the compound.展开更多
The title compound C15H12N4O2S was synthesized by the reaction of 3-(2-hydroxybenzyl)-4-amino-(1H)-1,2,4-triazole-5-thione with 4-hydroxybenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and element...The title compound C15H12N4O2S was synthesized by the reaction of 3-(2-hydroxybenzyl)-4-amino-(1H)-1,2,4-triazole-5-thione with 4-hydroxybenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and elemental analysis. Its structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic, space group C2/c with a = 27.990(3), b = 13.1326(14), c = 7.9770(8) A, β= 105.787(2)°, V = 2821.6(5)A^3, Z = 8, Mr= 312.35,μ= 0.243 mm^-1, Dc = 1.471 g/cm^3 and F(000) = 1296. The structure was solved by direct methods.and refined to a Rint value of 0.0388. The crystal structure involving in intermolecular N-H…S and O-H…S hydrogen bonds is observed, meanwhile intramolecular O-H…N hydrogen bond is also found. Their biological activities have been measured. The results show that this type of compound has certain antibacterial activity for Staphylococous aureus and Bacillus subtilis.展开更多
The title compound 5-[(1H-1,2,4-triazol-1-yl)methyl]-4-(2,3-dimethoxy-benzylideneamino)- 2H-1,2,4-triazole-3(4H)-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-( 1,2,4-triazol- 1-yl)- ...The title compound 5-[(1H-1,2,4-triazol-1-yl)methyl]-4-(2,3-dimethoxy-benzylideneamino)- 2H-1,2,4-triazole-3(4H)-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-( 1,2,4-triazol- 1-yl)- 1 H- 1,2,4-triazole-5(4H)-thione 3 with 2,3-dimethoxybenzaldehyde. It crystallizes as a monohydrate in the triclinic system, space group P1^- with a = 8.147(2), b = 10.820(2), c = 10.835(2)A, α= 73.770(6), β = 84.916(7),γ = 70.679(6)°, C14H17N7O35, Mr = 363.41, V= 865.4(2)A^3, Z= 2, Dc = 1.395 g/cm^3, F(000) = 380, μ = 0.217 mm^-1, the final R = 0.0400 and wR = 0.0975 for 3454 unique reflections. The dihedral angles made by the thione-substituted triazole ring with the other triazole ring and benzene ring are 74.92(3) and 14.81(2)°, respectively. There are some weak hydrogen bonds and C-H..π supramolecular interactions in the lattice, forming a three-dimensional network, which stabilizes the crystal structure.展开更多
The new title compound 4-dibenzaldehydeamino-4H-1,2,4-triazole diacetate (C16H18N8O4,Mr = 386.38) has been prepared and its crystal structure was determined by single- crystal X-ray diffraction. The crystal is of mo...The new title compound 4-dibenzaldehydeamino-4H-1,2,4-triazole diacetate (C16H18N8O4,Mr = 386.38) has been prepared and its crystal structure was determined by single- crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 8.1371(17),b = 7.1237(12),c = 16.325 (2)A,β = 100.366(2)°,V = 930.9(3) A^3,Z = 2,Dc = 1.378,F(000) = 404,μ = 0.104 mm^-1,MoKa radiation (λ = 0.71073 ),R = 0.0307 and wR = 0.1196 for 4632 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the molecule is not flat and the crystal structure is stabilized mainly by van der Waals interactions.展开更多
N′-(4-fluorobenzylidene)-2-( 1H-1,2,4-triasole-1-yl) acetohydrazide was synthesized by the reaction of 4-flu- orobenzaldehyde with 2-( 1H-1,2,4-triazole-1-yl) acetohydrazide. The structure was confirmed via ele...N′-(4-fluorobenzylidene)-2-( 1H-1,2,4-triasole-1-yl) acetohydrazide was synthesized by the reaction of 4-flu- orobenzaldehyde with 2-( 1H-1,2,4-triazole-1-yl) acetohydrazide. The structure was confirmed via elemental analysis, MS, ^1H NMR, IR, and X-ray diffraction. It crystallized in a monoclinic system with space group P2 ( 1 ), α = 0.4905(1) nm, b =0. 8160(2) nm, c = 1.4105(3) nm, β =93. 33(3)°, Z=2, V=0.5636(2) nm^3, Do =1.457 Mg/m^3,μ =0. 112 mm^-1 , F(000) =256, and final R1 =0. 0685. Several intermolecular hydrogen-bond interactions existed in the crystal structure, facilitating the stabilization of the compound.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 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 title compound2-p-methyloxyphenyl-3a-(2-phenyl-1,2,3-triazole-4-yl)-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine (C31H25N5O2S, Mr = 531.63) has been synthesized and its structure was determined b...The title compound2-p-methyloxyphenyl-3a-(2-phenyl-1,2,3-triazole-4-yl)-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine (C31H25N5O2S, Mr = 531.63) has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.888(2), b = 15.115(3), c = 16.702(3)A, α = 99.90(3), β = 95.21(3), γ = 100.41(3)°, V = 2642.1(9) nm^3, Dc = 1.336 g/cm^3, Z = 4, F(000) = 1112, μ = 0.162 mm^-1 ,λ(MoKα) = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I 〉 2σ(I). X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.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
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 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
The title compound, 4-(tert-butyl)-5-(1 H- 1,2,4-triazol- 1 -yl)-N-(2-hydroxy-3,5-diio- dinebenzyl)thiazol-2-amine, was synthesized via the reduction of 4-(tert-butyl)-5-(1H-l,2,4- triazol-l-yl)-N-benzyliden...The title compound, 4-(tert-butyl)-5-(1 H- 1,2,4-triazol- 1 -yl)-N-(2-hydroxy-3,5-diio- dinebenzyl)thiazol-2-amine, was synthesized via the reduction of 4-(tert-butyl)-5-(1H-l,2,4- triazol-l-yl)-N-benzylidene-thiazol-2-amine with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 7.91944(19), b = 10.5250(3), c = 24.4985(6) A, Z = 4, V = 2041.66(9) A3, Mr = 599.22, Dc = 1,949 Mg/m3, S = 1.120, p = 3.203 mm-1, F(000) = 1152, the final R = 0.0283 and wR = 0.0592 for 3490 observed reflections (I 〉 2σ(I)). X-ray analysis displays that the crystal water takes part in three intermolecular hydrogen bonds of O(2)-H(2A)…O(1), O(2)-H(2B)…N(I) and N(5)-H(5)…O(2), and an octatomic ring R^(8) is formed via intramolecular hydrogen bond of O(I)-H(IA)…N(4). Furthermore, the I…I contacts are involved in stabilizing the overall three-dimensional network structure. The preliminary biological test shows the title compound has good antitumor activity with the IC50 value of 26 μM against the Hela cell line.展开更多
The crystal structure of 5-nitro-4-salicylideneamino-3-methyl-1,2,4-triazole-5-thione ([C 10 H 9N 5O 3S]·HCON(CH 3) 2, M r=352.38)(CCDC No. 216094) was determined by the single crystal X-ray diffraction...The crystal structure of 5-nitro-4-salicylideneamino-3-methyl-1,2,4-triazole-5-thione ([C 10 H 9N 5O 3S]·HCON(CH 3) 2, M r=352.38)(CCDC No. 216094) was determined by the single crystal X-ray diffraction method. The crystal belongs to a triclinic system, the space group is P1 with unit cell constants a= 0.6113(2) nm, b=1.0836(4) nm, c=1.3132(5) nm, α=74.523(7)°, β=117.68(3)°, γ= 79.769(7)°, V=0.8245(5) nm 3, Z=2, D c=1.419 g/cm 3, μ=0.228 mm -1 , F(000)=368, R and wR are 0.0579 and 0.1040, respectively, beasd on 3348 unique reflections of which 1925 reflections were observed[I>2σ(I)]. The results indicate that the title compound can be assigned to the thione tautomeric form rather than the thiol tautomeric form. It contains a five membered triazole ring and a phenyl ring with a dihedral angle of 4.35°. The intermolecular hydrogen bond N3_H3…S1, O1_H1…O4 can be observed.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
The title compound 1-(2-fluorobenzyl)-3-methoxy-4-methyl-lH-1,2,4-triazol- 5(4H)-one (CI1HI2FN302) was synthesized, and its structure was confirmed by 1H NMR, IR, MS, elemental analysis and X-ray diffraction. It...The title compound 1-(2-fluorobenzyl)-3-methoxy-4-methyl-lH-1,2,4-triazol- 5(4H)-one (CI1HI2FN302) was synthesized, and its structure was confirmed by 1H NMR, IR, MS, elemental analysis and X-ray diffraction. It crystallizes in the monoclinic system, space group Pi with a = 6.919(3), b = 8.525(4), c = 9.811(4) A, a = 84.22(2), β = 71.028(19), γ = 86.10(2)°, Dc = 1.448 g/cm3, Z = 2, V= 544.2(4) A3, F(000) = 248, the final R = 0.0379 and WR = 0.0913 for 1709 observed reflections with I〉 2σ(I). The preliminary biological test shows that the title compound shows weak inhibitory activities against Phytophthora infestans, Botrytis cinerea, Corynespora cassiicola, Rhizoctonia solani and Pythium ultimum.展开更多
The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol- 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro- 2-(4-fluorophenoxy)phenyl)-2,3-e...The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol- 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro- 2-(4-fluorophenoxy)phenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229(19), b = 11.516(2), c = 16.047(3)A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7(6)A^3, Z = 4, Dc = 1.3359 g/cm^3, F(000) = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56(3) and 54.78(2)°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.展开更多
The title compound, [t-BuCOCH(C2H2N3)(C6H4N3)], has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in mono-clinic, space group C2/c with a = 11.563(3), b = 10.906...The title compound, [t-BuCOCH(C2H2N3)(C6H4N3)], has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in mono-clinic, space group C2/c with a = 11.563(3), b = 10.906(3), c = 23.602(5) ? b = 98.35(3)? C14H16N6O, Mr = 284.33, V = 2944.8(13) 3, Z = 8, Dc = 1.283 g/cm3, F(000) = 1200, = 0.087 mm-1, R = 0.0535 and wR = 0.1046. The crystal structure consists of discrete 2,2-dimethyl-4-[1H-(1,2,4-triazolyl)]-4-[1H-benzotriazolyl]-3-butanones. The planes of carbonyl group and benzotriazole ring form the dihedral angle of 89.14(1). The molecules of the title compound are connected to each other through extensive hydrogen bonds to form hydrogen networks. Elemen- tal analysis and IR spectra are in good agreement with the structural data.展开更多
基金Project supported by the National Natural Science Foundation of China(No.21442014)
文摘The title compound, (E)-1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)- 3-(2-methoxyphenyl)-2-(1H-1,2,4-triazol-1-yl)propenol (3a), was synthesized by the Aldol con- densation reaction of 1-(7-methoxy-2,2-dimethyl-2,3-dihydrobenzofuran-5-yl)-2-(1,2,4-triazol- 1-yl)ethanone with 2-methoxybenzaldehyde and then reduced with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction: monoclinic system, space group P21 with a = 6.2002(3), b = 12.8452(7), c = 13.2257(7) ?, Z = 2, V = 1031.23(9) ?3, Mr = 407.46, Dc = 1.312 Mg/m3, S = 1.054, μ = 0.091 mm-1, F(000) = 432, the final R = 0.0353 and wR = 0.0769 for 3161 observed reflections (I 〉 2σ(I)). X-ray analysis displays that the title compound adopts an E configuration for the C(7)=C(8) double bond and S configuration for the chirality center with the specific rotation of –63.75°. Furthermore, the stability of the crystal was maintained through the intermolecular hydrogen bond O(1)–H???N(3). The antitumor assay exhibits that the title compound 3a (E configuration) has a good antitumor activity against the Hela cell line with the IC50 value of 36.9 μM, which is better than that of 3b (Z configuration).
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.
基金This work was supported by the Natural Science Foundation of Zhejiang Province (No. M203115) and Scientific Research Fund of Zhejiang Provincial Education Department(NO.20050057)
文摘The title compound, C9H9N5OS, was synthesized by the reaction of 3-(1H)-1,2,4 -triazole hydrazine with 3-methyl-2-thiophenecarboxaldehyde in ethanol. The single crystal structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group P2 1/n with a = 9.5550(10), b = 11.9847(12), c = 10.1074(11) A,β= 112.995(2)° V= 1065.47(19) A^3, Z = 4,μ = 0.290 mm^-1, Mr= 235.27, Dc = 1.467 g/cm^3 and F(000) = 488. The structure was solved by direct methods and refined to R = 0.0449. The crystal structure involves intermolecular hydrogen bonds of N-H…O and N-H…N as well as intramolecular hydrogen bond of N-H…N. Its biological activity has also been determined showing this type of compounds has certain antibacterial activity.
基金Supported by the Program for New Century Excellent Talentsin University (NCET-09-0046)
文摘The compound of 3,5-diazido-1,2,4-triazole was synthesized by the reaction of 2,5,2',5'-tetrachloro-1,1'-azo-1,3,4-triazole with sodium azide at 50 ℃.Its crystal structure was determined by single-crystal X-ray diffraction.It crystallizes in monoclinic,space group Cc with a=1.212 4(2) nm,b=2.342 4(5) nm,c=0.804 74(16) nm,β=125.56(3)°,V=1.859 3(6) nm3,Z=4,C2HN9,Mr=151.04,Dc=1.62 g/cm3,F(000)=912 and μ(MoKa)=0.129 mm-1,the final R=0.039 7 and wR=0.087 4.X-ray analysis indicates a stronger intermolecular hydrogen bonding,leading to the formation of a trimmer,containing a nine-membered cyclic ring with graph-set R33(9) in the compound.
基金This work was supported by the Natural Science Foundation of Zhejiang Province (No. M203115) and Scientific Research Fund of Zhejiang Provincial Education Department (NO. 20050057)
文摘The title compound C15H12N4O2S was synthesized by the reaction of 3-(2-hydroxybenzyl)-4-amino-(1H)-1,2,4-triazole-5-thione with 4-hydroxybenzaldehyde in ethanol and characterized by IR, ^1H NMR spectra and elemental analysis. Its structure has been determined by X-ray diffraction analysis. The crystal belongs to monoclinic, space group C2/c with a = 27.990(3), b = 13.1326(14), c = 7.9770(8) A, β= 105.787(2)°, V = 2821.6(5)A^3, Z = 8, Mr= 312.35,μ= 0.243 mm^-1, Dc = 1.471 g/cm^3 and F(000) = 1296. The structure was solved by direct methods.and refined to a Rint value of 0.0388. The crystal structure involving in intermolecular N-H…S and O-H…S hydrogen bonds is observed, meanwhile intramolecular O-H…N hydrogen bond is also found. Their biological activities have been measured. The results show that this type of compound has certain antibacterial activity for Staphylococous aureus and Bacillus subtilis.
文摘The title compound 5-[(1H-1,2,4-triazol-1-yl)methyl]-4-(2,3-dimethoxy-benzylideneamino)- 2H-1,2,4-triazole-3(4H)-thione monohydrate 4 has been synthesized by the treatment of 4-amino-3-( 1,2,4-triazol- 1-yl)- 1 H- 1,2,4-triazole-5(4H)-thione 3 with 2,3-dimethoxybenzaldehyde. It crystallizes as a monohydrate in the triclinic system, space group P1^- with a = 8.147(2), b = 10.820(2), c = 10.835(2)A, α= 73.770(6), β = 84.916(7),γ = 70.679(6)°, C14H17N7O35, Mr = 363.41, V= 865.4(2)A^3, Z= 2, Dc = 1.395 g/cm^3, F(000) = 380, μ = 0.217 mm^-1, the final R = 0.0400 and wR = 0.0975 for 3454 unique reflections. The dihedral angles made by the thione-substituted triazole ring with the other triazole ring and benzene ring are 74.92(3) and 14.81(2)°, respectively. There are some weak hydrogen bonds and C-H..π supramolecular interactions in the lattice, forming a three-dimensional network, which stabilizes the crystal structure.
基金financially supported by the National Natural Science Foundation of China (No. 2006CB708606)
文摘The new title compound 4-dibenzaldehydeamino-4H-1,2,4-triazole diacetate (C16H18N8O4,Mr = 386.38) has been prepared and its crystal structure was determined by single- crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 8.1371(17),b = 7.1237(12),c = 16.325 (2)A,β = 100.366(2)°,V = 930.9(3) A^3,Z = 2,Dc = 1.378,F(000) = 404,μ = 0.104 mm^-1,MoKa radiation (λ = 0.71073 ),R = 0.0307 and wR = 0.1196 for 4632 observed reflections with I 〉 2σ(I). X-ray diffraction analysis reveals that the molecule is not flat and the crystal structure is stabilized mainly by van der Waals interactions.
文摘N′-(4-fluorobenzylidene)-2-( 1H-1,2,4-triasole-1-yl) acetohydrazide was synthesized by the reaction of 4-flu- orobenzaldehyde with 2-( 1H-1,2,4-triazole-1-yl) acetohydrazide. The structure was confirmed via elemental analysis, MS, ^1H NMR, IR, and X-ray diffraction. It crystallized in a monoclinic system with space group P2 ( 1 ), α = 0.4905(1) nm, b =0. 8160(2) nm, c = 1.4105(3) nm, β =93. 33(3)°, Z=2, V=0.5636(2) nm^3, Do =1.457 Mg/m^3,μ =0. 112 mm^-1 , F(000) =256, and final R1 =0. 0685. Several intermolecular hydrogen-bond interactions existed in the crystal structure, facilitating the stabilization of the compound.
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This work was supported by the National Natural Science Foundation of China (No. 29702007 and 20162004)
文摘The title compound2-p-methyloxyphenyl-3a-(2-phenyl-1,2,3-triazole-4-yl)-3,4- dihydro-1,2,4-oxa-diazolo[4,5-d][1,5] benzothiazepine (C31H25N5O2S, Mr = 531.63) has been synthesized and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1^- with a = 10.888(2), b = 15.115(3), c = 16.702(3)A, α = 99.90(3), β = 95.21(3), γ = 100.41(3)°, V = 2642.1(9) nm^3, Dc = 1.336 g/cm^3, Z = 4, F(000) = 1112, μ = 0.162 mm^-1 ,λ(MoKα) = 0.071073 nm, R = 0.0357 and wR = 0.1126 for 10620 observed reflections with I 〉 2σ(I). X-ray analysis reveals that the molecular backbone consists of a tricyclic system with the central seven- membered ring in a twisted boat-like conformation.
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.
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.
基金supported by the National Undergraduate Training Programs for Innovation and Entrepreneurship of Hunan Universitythe Natural Science Foundation of Hunan Province(No.12jj3012)
文摘The title compound, 4-(tert-butyl)-5-(1 H- 1,2,4-triazol- 1 -yl)-N-(2-hydroxy-3,5-diio- dinebenzyl)thiazol-2-amine, was synthesized via the reduction of 4-(tert-butyl)-5-(1H-l,2,4- triazol-l-yl)-N-benzylidene-thiazol-2-amine with NaBH4, and its crystal structure was determined by single-crystal X-ray diffraction. The compound crystallizes in monoclinic system, space group P21/c with a = 7.91944(19), b = 10.5250(3), c = 24.4985(6) A, Z = 4, V = 2041.66(9) A3, Mr = 599.22, Dc = 1,949 Mg/m3, S = 1.120, p = 3.203 mm-1, F(000) = 1152, the final R = 0.0283 and wR = 0.0592 for 3490 observed reflections (I 〉 2σ(I)). X-ray analysis displays that the crystal water takes part in three intermolecular hydrogen bonds of O(2)-H(2A)…O(1), O(2)-H(2B)…N(I) and N(5)-H(5)…O(2), and an octatomic ring R^(8) is formed via intramolecular hydrogen bond of O(I)-H(IA)…N(4). Furthermore, the I…I contacts are involved in stabilizing the overall three-dimensional network structure. The preliminary biological test shows the title compound has good antitumor activity with the IC50 value of 26 μM against the Hela cell line.
基金the Natural Science Foundation of Shandong Province(Y2 0 0 3B0 1,Z2 0 0 2 B0 2 ),the Outstanding Adult-young Scientific Research Encouraging Foundation of Shandong Province(No. 0 3BS0 81) and the National Natural ScienceFoundation of China(No. 2 0 2 75 0
文摘The crystal structure of 5-nitro-4-salicylideneamino-3-methyl-1,2,4-triazole-5-thione ([C 10 H 9N 5O 3S]·HCON(CH 3) 2, M r=352.38)(CCDC No. 216094) was determined by the single crystal X-ray diffraction method. The crystal belongs to a triclinic system, the space group is P1 with unit cell constants a= 0.6113(2) nm, b=1.0836(4) nm, c=1.3132(5) nm, α=74.523(7)°, β=117.68(3)°, γ= 79.769(7)°, V=0.8245(5) nm 3, Z=2, D c=1.419 g/cm 3, μ=0.228 mm -1 , F(000)=368, R and wR are 0.0579 and 0.1040, respectively, beasd on 3348 unique reflections of which 1925 reflections were observed[I>2σ(I)]. The results indicate that the title compound can be assigned to the thione tautomeric form rather than the thiol tautomeric form. It contains a five membered triazole ring and a phenyl ring with a dihedral angle of 4.35°. The intermolecular hydrogen bond N3_H3…S1, O1_H1…O4 can be observed.
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 Applied Chemistry Foundation of Zhejiang Shuren University(YH2013S09)
文摘The title compound 1-(2-fluorobenzyl)-3-methoxy-4-methyl-lH-1,2,4-triazol- 5(4H)-one (CI1HI2FN302) was synthesized, and its structure was confirmed by 1H NMR, IR, MS, elemental analysis and X-ray diffraction. It crystallizes in the monoclinic system, space group Pi with a = 6.919(3), b = 8.525(4), c = 9.811(4) A, a = 84.22(2), β = 71.028(19), γ = 86.10(2)°, Dc = 1.448 g/cm3, Z = 2, V= 544.2(4) A3, F(000) = 248, the final R = 0.0379 and WR = 0.0913 for 1709 observed reflections with I〉 2σ(I). The preliminary biological test shows that the title compound shows weak inhibitory activities against Phytophthora infestans, Botrytis cinerea, Corynespora cassiicola, Rhizoctonia solani and Pythium ultimum.
文摘The title compound 2-(4-fluoro-2-(4-fluorophenoxy)phenyl)-1-(1H-1,2,4-triazol- 1-ylmethyl)-3-methoxy-isopropy alcohol has been synthesized by the treatment of 1-[2-(4-fluoro- 2-(4-fluorophenoxy)phenyl)-2,3-epoxypropyl]-1H-1,2,4-triazole with sodium methoxide. It belongs to orthorhombic, space group P212121, with a = 9.7229(19), b = 11.516(2), c = 16.047(3)A, C18H17F2 N3O3, Mr = 361.35, V = 1796.7(6)A^3, Z = 4, Dc = 1.3359 g/cm^3, F(000) = 752, p = 0.106 mm^-1, the final R = 0.0329 and wR = 0.0803 for 1821 unique reflections. The dihedral angles made by the triazole ring with two benzene rings are 43.56(3) and 54.78(2)°, respectively. The intermolecular hydrogen bond in the crystal lattice plays an important role in stabilizing the structure.
基金Natural Science Foundation of Shandong Province (No. Y2002B06)
文摘The title compound, [t-BuCOCH(C2H2N3)(C6H4N3)], has been prepared and characterized by elemental analysis, IR spectrum and X-ray studies. It crystallizes in mono-clinic, space group C2/c with a = 11.563(3), b = 10.906(3), c = 23.602(5) ? b = 98.35(3)? C14H16N6O, Mr = 284.33, V = 2944.8(13) 3, Z = 8, Dc = 1.283 g/cm3, F(000) = 1200, = 0.087 mm-1, R = 0.0535 and wR = 0.1046. The crystal structure consists of discrete 2,2-dimethyl-4-[1H-(1,2,4-triazolyl)]-4-[1H-benzotriazolyl]-3-butanones. The planes of carbonyl group and benzotriazole ring form the dihedral angle of 89.14(1). The molecules of the title compound are connected to each other through extensive hydrogen bonds to form hydrogen networks. Elemen- tal analysis and IR spectra are in good agreement with the structural data.