Synthesis and Crystal Structure of N-[4-(4-Methyl-phenylsulfamoyl)-phenyl]- 4-methyl-1,2,3-thiadiazole-5-carboxamide

The crystal structure of the title compound (C17H16N4O3S2, Mr = 388.46) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 13.688(2), b = 16.704(3), c = 8.3308(12) , β = 99.474(6)o, V = 1878.8(5) 3, Mr = 388.46, Z = 4, Dc = 1.373 g/cm3, μ = 0.308 mm–1, F(000) = 808, R = 0.0389 and wR = 0.0917. X-ray analysis reveals that the crystal structure involves intermolecular N–H…O and N–H…N hydrogen bonds, which link the molecules into a layer parallel to the ac plane.     

Synthesis,Crystal Structure and Biological Activities of 1-（（5-（4-（4-Chlorophenoxy）-2-chlorophenyl）-2,2,3- trimethyloxazolidin-5-yl）methyl）-1H-1,2,4-triazole

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.     

Synthesis,Crystal Structure,and Antitumor Activity of 1-（4-Methoxybenzylidene）-2-（1-phenyl-6-trifluoromethyl- 1H-pyrazolo [3,4-d] pyrimidin-4-yl）hydrazine Monohydrate

The novel title compound 1-(4-methoxybenzylidene)-2-(1-phenyl-6-trifluoromethyl-1H-pyrazolo[3,4-d]pyrimidin-4-yl)hydrazine monohydrate(C20H15F3N6O·H2O, Mr = 430.40) has been synthesized by a four-step procedure including the cyclization, chlorination, hydrazinolysis and condensation reaction, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pbca with a = 8.3779(13), b = 17.607(3), c = 26.774(4) , V = 3949.2(11) 3, Z = 8, Dc = 1.448 g/cm3, μ = 0.117 mm–1, F(000) = 1776, the final R = 0.0553 and wR = 0.1516 for 2354 observed reflections with I 2■(I). X-ray diffraction analysis reveals that the title compound is almost coplanar except for the trifluoromethyl and phenyl moieties. In the crystal packing, the molecules are linked by intermolecular O(1W)–H(1WA)···N(2), O(1W)–H(1WA)···N(4) and N(5)–H(5A)···O(1W) hydrogen bonds via water molecules and stacked through π-π stacking interactions. The preliminary bioassay suggested that the title compound exhibits relatively good antitumor activity against HepG2 and BCG-823.     

（E）-1-[4-（2-hydroxy-5-methoxybenzylideneamino）-phenyl]ethanone and （E）-1-[4-（2-hydroxy-4-methoxybenzylideneamino） phenyl]ethanone：X-ray and DFT-calculated structures

The isomeric structures of(E)-1-[4-(2-hydroxy-5-methoxybenzylideneamino)-phenyl] ethanone(I) and(E)-1-[4-(2-hydroxy-4-methoxybenzylideneamino) phenyl]ethanone(Ⅱ) ,both C16H15NO3,have been determined using X-ray diffraction techniques and characterized by IR,and their molecular structures have also been optimized at the B3LYP/6-31G(d,p) level using density functional theory(DFT) . The energetic behaviors of the title compounds in solvent media have been examined using B3LYP method with the 6-31G(d,p) basis set by applying the polarizable continuum model(PCM) . The total energies of the title compounds decrease with the increasing polarity of the solvent. In addition,DFT calculations of the title compounds' molecular electrostatic potentials(MEP) were performed at the B3LYP/6-31G(d,p) level of theory. X-ray study shows that the title compounds both have strong intramolecular O-H…N hydrogen bonds. The molecules of Ⅰ are linked into a one-dimensional framework structure by C-H…π interactions,while in Ⅱ,intermolecular π···π interactions result in the formation of infinite chains running along the [010].     

Analysis of Intra-and Intermolecular Hydrogen Bonds and Quantum Chemical Calculations on 1-(3-Fluorobenzoyl)-3-(4-trifluoromethylphenyl) thiourea

1-(3-Fluorobenzoyl)-3-(4-trifluoromethylphenyl)thiourea, C_(15)H_(10)F_4N_2OS, has been synthesized firstly and determined by single-crystal X-ray diffraction analysis. The title compound crystallizes in monoclinic system, space group C2/c with a = 31.87(3), b = 7.705(9), c = 12.591(14) ?, b = 106.06(2)°, V = 2971(6) ?~3, Z = 8, D_c=1.530 g·cm~(–1), F(000) = 1392, m = 0.266 mm~(–1), S = 1.06, the final R = 0.070 and w R(I 2s(I)) = 0.249. The crystal structure revealed that the carbonyl thiourea unit in the determined compound was mostly planar due in part to the formation of intramolecular N–H···O=C and C–H···S=C hydrogen bonds that form two S(6) rings. The intermolecular contacts of the crystal structure have been preformed based on the Hirshfeld surface and their associated 2D fingerprint plots. In the packing diagram of the synthesized compound, the C=S group formed two types of intermolecular hydrogen bonds by the H–N(C=O) group and the H–C of the phenyl ring, respectively, and they formed R2 2(8) and R_2~2(14) ring motifs, respectively. The crystal packing form was also stabilized by the intermolecular hydrogen bonds C–H···O(1–x, y, 0.5–z) with the R_2~2(10) ring motifs. In addition, supramolecular layers sustained by π-π stacking interactions(between the C(2)~C(7) rings with the C(10)~C(15) rings) are formed in the crystal structure of the title compound. The electronic and reactivity were assessed by the natural bond orbital(NBO) analysis in this study.     

Synthesis and Crystal Structure of an Unusual Dodecacoordinated Lanthanum Complex by Phenanthroline and Nitrate （phenH）_2[La（NO_3）_5（phen）]·CH_3OH

Lanthanum complex (phenH)2[La(NO3)5(phen)]·CH3OH (1, phen=phenanthroline) was synthesized and characterized by single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a=20.3040(3), b=10.7091(1), c=19.0771(2), β=102.090(1)°, V=4056.07(8)3, Z=4, Dc=1.676 g/cm3, μ= 1.142 mm-1, F(000)=2056, the final R=0.0346 and wR=0.0793 for 9981 (Rint=0.0358) independent reflections. The mononuclear complex 1 consists of four parts: two phenH+ cations formed by the protonation of phen, one complex anion [La(NO3)5(phen)]2-, and one solvent methanol molecule. The complex anion contains one phen and five nitrate ligands which both chelate the center La(III) ion, adopting a distorted twelve-coordinated icosahedral geometry. The cations, anion and solvent molecule are linked together by hydrogen bonds. One of the protonated phenanthrolines (phenH+) acting as cation connects to the anion via N–H…O hydrogen bond directly, and the other one links to the anion through an intermediate solvent CH3OH via N–H…O and O–H…O hydrogen bonds. By the plentiful additional weak C–H…O intermolecular hydrogen bonds, the compound molecules construct a two-dimensional layer structure.     

Synthesis, Crystal Structure and Bioactivities of 1-（4-Chlorophenyl）-3- [ 5-（pyrid-4-yl）- 1,3,4-thiadiazol-2-yl] urea

The title compound 1-(4-chlorophenyl)-3-[5-(pyrid-4-yl)-1,3,4-thiadiazol-2-yl]urea (C14H10ClN5OS, Mr = 331.79) has been synthesized by the reaction of 2-amino-5-(pyrid-4-yl)- 1,3,4-thiadiazole with 4-chlorobenzoyl azide, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic system, space group P with a = 5.8550(8), b = 7.5668(10), c = 16.416(2) , α = 78.364(2), β = 81.204(2), γ = 84.749(2)°, V = 702.58(16) 3, Z = 2, Dc = 1.568 g/cm3, μ = 0.429 mm-1, F(000) = 340, the final R = 0.0442 and wR = 0.1092 for 2001 observed reflections (I > 2σ(I)). X-ray diffraction analysis reveals that the title molecule is nearly planar. In the crystal structure, the molecules are linked by strong intermolecular N-H…N hydrogen bonds together with weak nonclassical intermolecular (C-H…Y, Y = N, O and Cl) hydrogen bonds and stacked through π-π interactions. The preliminary bioassay shows that the title compound exhibits good fungicidal activities against Rhizoctonia solani, Botrytis cinerea and Dothiorella gregaria.     

Syntheses,Crystal Structures,and Antimicrobial Activities of 3-Bromo-N＇-（2- chloro-5-nitrobenzylidene）benzohydrazide and 3-Bromo-N＇-（4-nitrobenzylidene）benzohydrazide

Two new hydrazone compounds, 3-bromo-N'-(2-chloro-5-nitrobenzylidene)-ben- zohydrazide 1 and 3-bromo-N'-(4-nitrobenzylidene)benzohydrazide 2, have been synthesized and characterized by elemental analysis, IR spectra, 1H NMR, and single-crystal X-ray diffraction. Compound 1 crystallizes in monoclinic, space group P21/c with a=7.7924(10), b=24.490(3), c=7.8989(9) , β=94.987(6)°, V=1501.7(3) 3, Z=4, R=0.0345 and wR=0.0739. Compound 2 crystallizes in monoclinic, space group P21/c with a=7.4099(11), b=24.868(4), c=8.3255(12) , β=112.796(8)°, V=1414.3(4) 3, Z=4, R=0.0744 and wR=0.1912. Both compounds display E configurations with respect to the C=N double bonds. In the crystal structure of 1, molecules are linked through N-H…N and N-H…O hydrogen bonds, forming chains running along the c axis. In the crystal structure of 2, molecules are linked through N-H…O hydrogen bonds, forming chains running along the c axis. The preliminary antimicrobial activities were studied.     

Syntheses,Crystal Structures,and Antimicrobial Activities of N′-(5-Hydroxy-2-nitrobenzylidene)-4-dimethylaminobenzohydrazide Methanol Solvate and 2-Fluoro-N′-(5-hydroxy-2-nitrobenzylidene)benzohydrazide

Two new hydrazone compounds,N'-(5-hydroxy-2-nitrobenzylidene)-4-dimethyl-aminobenzohydrazide methanol solvate (1) and 2-fluoro-N'-(5-hydroxy-2-nitrobenzylidene)benzo-hydrazide (2),have been synthesized and characterized by elemental analysis,IR spectra,1H NMR,and single-crystal X-ray diffraction.Compound 1 crystallizes in the monoclinic space group P21/c with a=11.571(3),b=12.420(3),c=12.360(2) ?,β=97.495(2)°,V=1761.1(7) 3,Z=4,R=0.0735 and wR=0.1344.Compound 2 crystallizes in the triclinic space group P with a=7.551(3),b=8.254(3),c=11.365(2) ?,α=79.352(2),β=76.154(2),γ=71.624(2)°,V=648.2(4) 3,Z=2,R=0.0393 and wR=0.1008.The hydrazone molecules of the compounds display E configurations with respect to the C=N double bonds.In the crystal structure of 1,the hydrazone molecules are linked by methanol molecules through N-H…O,O-H…N and O-H…O hydrogen bonds,forming chains running along the c axis.In the crystal structure of 2,molecules are linked through N-H…O and O-H…O hydrogen bonds,forming ribbons running along the b axis.The preliminary antimicrobial activities were studied.     

Synthesis and Crystal Structure of 1-[（1＇-Phenyl-5＇-methyl-4＇-pyrazolcarbonyl）-3-methylthio-5-amino-1Hy l-1,2,4-triazole

The title compound (C14H14N6OS, Mr=314.37) has been synthesized and characterized by IR, ^1H NMR and X-ray single-crystal diffraction techniques.The crystal structure shows the presence of a dimmer with intermolecular N(4)H(4)…N(3) hydrogen bonds.     

Synthesis and Structural Studies of 6-（2,5-Dimethyl-1H-pyrrol-1-yl）pyridin-2-amine

6-(2,5-Dimethyl-1H-pyrrol-1-yl)pyridin-2-amine (1) was synthesized and characte-rized by elemental analyses,1H-NMR and 13C-NMR,FTIR,Uv-Vis,mass spectral studies and single-crystal X-ray diffraction.All data obtained from spectral studies support the structural properties of 1.Intermolecular N-H…N hydrogen bonds produce an R22(8) ring.An extensive three-dimensional network formed by C-H…π and N-H…π-facial hydrogen bonds is responsible for the crystal stabilization.The combination of C-H…π interactions produces R33(12),R43(19) and R44(20) rings.     

Synthesis and Crystal Structure of N-(1,3,4-Thiadiazol-2-yl)-1-[1-(6-chloropyridin-3-yl)methy]-5-methyl-1H-[1,2,3]triazol-4-carboxamide

The crystal structure of the title compound (C12H10ClN7OS,Mr=335.78) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic,space group P1 with a=8.4093(11),b=9.4430(12),c=11.1454(14),α=95.508(2),β=111.366(2),γ=115.259(2)°,V=711.42(16) 3,Z=2,Dc=1.568 g/cm3,F(000)=344,μ(MoKα)=0.428 mm-1,the final R=0.0476 and wR=0.1243 for 2353 observed reflections (I > 2σ(I)). The dihedral angles between the pyridine and triazole,thiazole and triazole,and pyridine and thiazole rings are 69.2(1),9.2(1) and 72.7(1)o,respectively. Intramolecular C(8)-H(8B)…O(1) and N(5)-H(5A)…N(4) as well as intermolecular C(5)-H(5)…S(1),C(3)-H(3)…N(6) and N(5)-H(5A)…N(1) hydrogen bonds together with weak C-H…π hydrogen-bonding and π-π stacking interactions contribute to the stability of the structure. There is also evidence for significant electron delocalization in the triazolyl system.     

Synthesis and Crystal Structure of 1-（Trifluoromethyl）-1-（propioloyl）-（E）-3-oxo-（2-thienyl）-（2-naphthylamine）

1INTRODUCTIONTheSchiffbasesderivedfromb-diketonesandaliphaticamineshavebeenshowntoexistastheketo-amines.However,ifsubstituentseitherattheketooraminogrouparearomatic,itmaybeexpectedtheenoliminewillbethefavoredtautomericform[1].Recently,someSchiffbasesderivedfromTTA(4,4,4-trifluoro-1-(2-thienyl)-1,3-butanedione)andPMBPhavebeenstudiedbyWang[2]andYu[3]etal.Inordertostudytherelationshipbetweenthestructuresandperformancesofthesecompounds,thetitlecom-poundwillbereportedherein.2EXPERIMENT…     

Synthesis and Crystal Structure of 5-[（1H-1,2,4-Triazol-1- yl）methyl]-4-（2,3-dimethoxybenzylideneamino）-2- 2H-1,2,4-triazole-3（4H）-thione Monohydrate

1 INTRODUCTION Heterocyclic compounds bearing the 1,2,4-tri- azole moiety have attracted considerable attention over the past few decades since they exhibit some fungicidal activities against Puccinia recondite and applications in the field of root-growth regu- lation[1~3]. Meanwhile, 4-amino-5-mercapto-1,2, 4-triazole moiety has great versatility in fusing tovarious ring systems and possesses a broad spec- trum of biological activities[4, 5]. In our con- tinuous work directed towards the…     

Synthesis and Crystal Structure of 3-（ 2- Hydroxybenzly ）-4-（ 4- Hydro xybenzylideneamino ）-（1H） - 1,2,4- Triazole-5-Thione and Its Antibacterial Activities

1 INTRODUCTION 2. 1 Physical measurements Azole derivatives, such as pyrazole, imidazole, All solvent and chemicals were commercial rea- triazole(including benzotriazole), tetrazole and indole, gents and used without further purification. Ele- have extensive biological activities. They have be- mental analyses were performed on a PE 1700 CHN come the central focus of studies for agricultural che- auto elemental analyzer. IR spectra were recorded on micals, medicines, plant growth regul…     

Synthesis, Crystal Structure and Antibacterial Activities of 3-[（2-Hydroxy-4-diethylamino-phenyl）methylenehydrazinocarbonyl]-4-hydroxy-6-methyl-2（1H）-pyridinones

1 INTRODUCTION Recently, compounds containing pyrazole, imida- zole, triazole (including benzotriazole), pyridine, tetrazole and indole have attracted much interest because of their fungicidal activity, plant-growth regulating activity and antibacterial activity[1～3]. Schiff bases also constitute a good type of biolo- gically active substructures[4～7]. Studies of pyri- dine Schiff base-type fungicides have been repor- ted[8]. However, some structures of pyridine com- pounds containing h…     

Synthesis and Crystal Structure of Bis{2-bromo- 4-chloro-6-[(2-isopropylammonioethylimino)-methyl]phenolato}bisthiocyanatozinc(Ⅱ)

A Schiff base zinc(Ⅱ) complex [Zn(C12H16BrClN2O)2(NCS)2] was prepared and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 8.414(1), b = 9.124(1), c = 22.212(3) (A), α = 79.177(2), β = 86.296(2), γ = 89.899(2)o, V = 1671.3(4) (A)3, Z = 2, Dc = 1.631 g/cm3, Mr = 820.79, λ(MoKα) = 0.71073 (A), μ = 3.444 mm-1, F(000) = 824, R = 0.0646 and wR = 0.1179. A total of 7371 unique reflections were collected, of which 3904 with I＞2σ(I) were observed. The complex crystallizes with two half-molecules per asymmetric unit and each mononuclear molecule is centrosymmetric. The Zn atom lying at the inversion centre is six-coordinated in a slightly distorted octahedral geometry by two phenolate O atoms and two imine N atoms from two Schiff base ligands, as well as two N atoms from two thiocyanate anions. In the crystal structure, the combination of π-π stacking interactions and intermolecular hydrogen bonds (N-H…Br, N-H…O, N-H…N, C-H…O, C-H…S and C-H…Cl) leads to a three-dimensional network.