Synthesis and Crystal Structure of {4-[2-（9- Hexyl-9H-carbazol-3-yl）vinyl]phenyl} Dimethylamine

The title compound {4-[2-(9-hexyl-9H-carbazol-3-yl)vinyl]phenyl} dimethylamine has been synthesized by the well known Wittig reaction, and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/c with a = 47.87(2), b = 10.222(4), c = 9.612(4) , β = 92.401(9)o, V = 4699(3) 3, Z = 8, C28H32N2, Mr = 396.56, Dc = 1.121 g/cm3, F(000) = 1712 and μ(MoKa) = 0.065 mm-1. The final R and wR are 0.0793 and 0.1983, respectively for 3524 observed reflections with I > 2σ(I). In the title compound, the bond lengths are normal, and the crystal is stabilized by Van der Waals’ forces.     

Synthesis and Crystal Structure of N-[（2S）-4-bromo-2-（L-menthyloxy）-5-oxo-2,5-dihydro-3-furyl]-L-leucine

Starting from(5S)-(L-menthyloxy)-3,4-dibromo-5H-furan-2-one and L-leucine,the title compound N-[(2S)-4-bromo-2-(L-menthyloxy)-5-oxo-2,5-dihydro-3-furyl]-L-leucine 5(C20H32BrNO5,Mr = 446.37) was obtained in one-pot process via the tandem Michael addition-elimination reaction in the presence of potassium hydroxide.The chemical structure and absolute configuration of the title compound were confirmed via rotation,UV-Vis,FT-IR,1H NMR,13C NMR,MS and elemental analysis,especially by the X-ray single-crystal diffraction.The crystal crystallizes in an orthorhombic system,space group P212121 with a = 12.5249(16),b = 19.005(3),c = 19.719(3) ,V = 4693.7(10) 3,Z = 8,Dc = 1.263 g/m3,μ = 1.778 mm-1,F(000) = 1872,the final R = 0.0617 and wR = 0.1576 for 3967 observed reflections(I > 2σ(I)).X-ray analysis reveals that the title compound has two independent molecules in the asymmetric part of the unit cell with the two five-membered furanones being almost planar.The essential part of the electron delocalization is concentrated in the N(1),C(3),C(1),C(37) and O(7) region and N(2),C(28),C(27),C(30) and O(4) region in the other molecule respectively,but does not take place at the expense of delocalization within the ester function.     

Synthesis and Crystal Structure of 2-Hydroxybenzoic Acid [1-（3,5-Dibromo-2-hydroxyphenyl）methylidene]hydrazide Methanol

A new Schiff base compound, 2-hydroxybenzoic acid [1-(3,5-dibromo-2-hydroxy- phenyl) methylidene]hydrazide methanol (C14H10Br2N2O3·CH3OH), has been synthesized by the condensation of equimolar 3,5-dibromosalicylaldehyde and 2-hydroxybenzoic acid hydrazide in a methanol solution. The compound was characterized by elemental analysis, IR spectra, and single- crystal X-ray diffraction. The compound consists of a Schiff base moiety 2-hydroxybenzoic acid [1-(3,5-dibromo-2-hydroxyphenyl)methylidene]hydrazide and a lattice methanol molecule. The crystal belongs to the monoclinic system, space group P21/n with a = 7.183(1), b = 15.673(2), c = 15.001(2) , β = 98.345(2)o, Z = 4, V = 1670.9(4) 3, Dc = 1.773 g/cm3, Mr = 446.10, λ(MoKα) = 0.71073 , μ = 4.872 mm-1, F(000) = 880, R = 0.0458 and wR = 0.0963. A total of 3445 unique reflections were collected, of which 2236 with I > 2σ(I) were observed. As expected, the molecule adopts a trans configuration about the C=N double bond. The two benzene rings are nearly coplanar (mean deviation from the combined plane is 0.061(4) ), with the dihedral angle of 7.9(3)o. The preliminary biological tests show that the compound has moderate antibacterial activities.     

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.     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis, Crystal Structure and Biological Activities of 3-[2-（4-Fluoro-phenyl）-ethyl]-5- methyl-4-hydroxyl-4-methyl-7-methylsulfanyl. 3,4-dihydro-pyrido[4,3-d]pyrimidine-8-carbonitrile

The title compound, 3-[2-(4-fluoro-phenyl)-ethyl]-5-methyl-4-hydroxyl-4-methyl- 7-methylsulfanyl-3,4-dihydro-pyrido[4,3-d]pyrimidine-8-carbonitrile, has been prepared and dete- mined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 6.8754(8), b = 10.2617(12), c = 13.3491(16) , α = 93.163(2), β = 96.704(2), γ = 102.421(2)°, V = 910.35(19) 3, Z = 2, Mr = 370.44, Dc = 1.351 g/cm3, μ = 0.203 mm-1, F(000) = 388, the final R = 0.0573 and wR = 0.1497. X-ray analysis reveals that the pyridine and pyrimidine rings are almost coplanar.     

Synthesis and Crystal Structure of 1-（4-Fluorophenyl）-2-hexylthiobenzo[4,5]-furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H）-one

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) ,β = 99.364(2) °,V = 4332.58(18) 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.     

Synthesis and Crystal Structure of 2-[（2-Chloropyridin-4-yl）oxy]-3,3-diphenyl-3-methoxypropionic Acid

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of orthorhombic system(C21H18ClNO4,Mr = 383.81),space group Pca21 with a = 13.913(3),b = 10.273(2),c = 26.488(5),V = 3786.1(13) 3,Z = 8,Dc = 1.347 g/cm3,F(000) = 1600,μ = 0.228 mm-1,the final R = 0.0550 and wR = 0.1278 for 5065 observed reflections(I > 2σ(I)).The title compound in a racemic form was found to exist as a mixture of two enantiomers in an equal ratio in the unit cell.The intermolecular hydrogen bonds link the molecules in a head-to-end manner to generate an infinite chain.     

Synthesis and Crystal Structure of 9-（4-Dimethylaminophenyl）-l,8-dioxo- 9H-dibenzo [c,h ]-2,7,10-trioxanthene

The title compound 9-(4-dimethylaminophenyl)-1,8-dioxo-9H-dibenzo[c,h]- 2,7,10-trioxanthene (3) was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethyla- minobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in triclinic, space group P with a = 7.8753(16), b = 11.029(2), c = 12.913(3) , α = 69.79(3), β = 89.01(3), γ = 81.90(3)°, V = 1041.5(4) 3, Z = 2 , F(000) = 456, Dc = 1.395 Mg/m3, Mr = 437.43, μ = 0.097 mm-1, λ = 0.71073 , the final R = 0.0491 and wR = 0.1314 for 2662 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of 2-（4-Oxo-3-0- tolyl-3,4-dihydroquinazolin-2-ylthio）acetohydrazide

The title compound was synthesized from 3-(2-methylphenyl)-2-thioxo-2,3-dihy- droquinazolin-4(1H)-one (4) which was prepared from 2-methylaniline in two steps. The structure was supported by the spectroscopic data and unambiguously confirmed by single-crystal X-ray diffraction studies. It crystallizes in the orthorhombic space group Pbca with unit cell dimensions a = 6.687(4), b = 24.788(16), c = 30.453(19) , V = 5048(5) 3 and Z = 8.     

Crystal Structure and Herbicidal Activity of N-（5,7-Dimethoxy-2H-[ 1,2,4]thiadiazolo[2,3-a]pyrimidin-2-ylidene）-2-（2,4- dichlorophenoxy）propanamide

The title compound N-（5,7-dimethoxy-2H-[1,2,4]thiadiazolo[2,3-a]pyrimidin-2- ylidene）-2-（2,4-dichlorophenoxy）propanamide 3 has been synthesized through using bromine as cyclic reagent in 66% isolated yield. Suitable single crystals for X-ray diffraction were obtained by recrystallization from the mixture solvents at room temperature. Crystallographic data of 3： C32H28Ci4N8O9S2, Mr = 874.56, monoclinic, space group P21/c, a = 18.612（8）, b = 14.084（6）, c = 14.757（6） A, α = 90.00, β = 95.505（7）, ）, = 90.00°, Z = 4, V= 3850（3） A^3, Dc = 1.509 g/cm^3, F（000） = 1792, R = 0.0704, wR = 0.1454 and ° = 0.479 mm^-1. The title compound 3 was found to be effective in herbicidal activity.     

Synthesis and Crystal Structure of 1-(o-methylphenyl)-2-(p-methoxyphenyl)-1,3,2-diazaphospholidin-4-thione-2-sulfide

11NTRODUCTIoNThederivativesofdiazaphospholidinoneorthecorrespondingthionesareknowntopossessinterestingbiologicalproperties,suchasherbicidalactivity"'2i.Inrecentyears,itwasreportedthatthel,4,2-diazaphospholindine-5-thione-2havegoodselectiveherbicidalactivity"'41.Tolookformoreeffectiveherbicideswithlowtoxicity,aseriesofnovel1-(o-methylphenyl)-2-(p-methoxyphenyl)-phospholidin-4-thione-sulfideshavebeensynthesizedandtheirmolecularstructuresstudied.PreliminarybioassaysshowthatthesecomPoundshaveg…     

Crystal Structure and Biological Activities of (R)-N''-[2-(4-Methoxy-6-chloro)-pyrimidinyl]-N-[3-methyl-2-(4-chlorophenyl)butyryl]-urea

The title compound (R)-N'-[2-(4-methoxy-6-chloro)-pyrimidyl]-N-[3-methyl-2-(4-chlorophenyl)butyryl]-urea has been synthesized, and its crystal structure and biological behaviors were studied. Crystallographic data: C17H18Cl2N4O3, Mr = 397.25, monoclinic, space group P21/c, a = 12.331 (2), b = 14.025(3), c = 23.085(5) (A), β = 99.607(4)°, Z = 8, V = 3936.2(13) (A)3, Dc = 1.341 g/cm3, F(000) = 1648, R = 0.0718, wR = 0.1585 and μ(MoKα) = 0.353 mm-1. The preliminary biological tests showed that the title compound has definite insecticidal and fungicidal activities.     

N-[2-(4,6-二甲氧基嘧啶-2-氧基)苯亚甲基]-2-芳氧乙酰腙的合成与除草活性

通过2-(4,6-二甲氧基嘧啶-2-氧基)苯甲醛(1)与芳氧乙酰肼2的缩合反应,合成了10个含嘧啶结构的芳氧乙酰腙化合物3,其结构经1H NMR、IR、EI-MS或ESI-MS和元素分析测试技术确证。 除草活性测试(活体盆栽)结果表明,大部分目标化合物在1.5 kg/hm2浓度下, 无论苗前或苗后处理对苋菜均显示出很强抑制活性,化合物3e和3h的抑制率分别为100%和97.7%,而化合物3a、3b、3d、3e、3f和3h苗后处理对苋菜的抑制率均超过97%,对马唐的除草活性最差。 苯环4-位取代基性质对除草活性有规律性影响。     

Crystal Structure and Biological Activities of N-(5-(4-Chloro-2-(trifluoromethyl)phenyl)furan-2- carbonyl)-N'-(4,6-dimethylpyrimidin-2-yl)thiourea

The new title compound N-(5-(4-chloro-2-(trifluoromethyl)phenyl)furan-2-carbon-yl)- N?-(4,6-dimethylpyrimidin-2-yl)thiourea (C19H14ClF3N4O2S) has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932(5), b = 33.46(2), c = 7.556(5) , β = 98.058(9)°, V = 1986(2) 3, Mr = 454.85, Z = 4, Dc = 1.521 g/cm3, μ = 0.349 mm–1 and F(000) = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR = 0.1429 for 3494 observed reflections (I > 2σ(I)). Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidal activity for the title compound.     

Crystal Structure and Herbicidal Activity of 5,7-Dimethoxy-(2,4-dichlorophenoxyacetyl- imino)-2H-1,2,4-thiadiazolo[2,3-a]pyrimidine

1 INTRODUCTION 2H-1,2,4-Thiadiazolo[2,3-a]pyrimidine compounds are a new series of ALS inhibiting agents besides sulfonylurea herbicide. Their herbicidal activity is similar to that of sulfonylurea herbicide, but be- cause of weak S–N bond existing in 2H-1,2,4-thiadi- azolo[2,3-a]pyrimidine ring, which is advantageous for the absorption and metabolism of vegetable, 2H- 1,2,4-thiadiazolo[2,3-a]pyrimidine herbicides have better selectivity[1～3]. At present, reports about the synthesis…     

Crystal Structure and Biological Activities of N-（5-（4-Chloro-2-（trifluoromethyl）phenyl）furan-2-carbonyl）-N＇-（4,6,dimethylpyrimidin-2-yl）thiourea

The new title compound N-（5-（4-chloro-2-（trifluoromethyl）phenyl）furan-2-carbon-yl）- N＇-（4,6-dimethylpyrimidin-2-yl）thiourea （C19H14C1F3N4O2S） has been synthesized, and its crystal structure and biological behaviors were studied. The title compound crystallizes in the monoclinic system, space group P21/c with a = 7.932（5）, b = 33.46（2）, c = 7.556（5） A, β = 98.058（9）°, V = 1986（2） A^3 Mr = 454.85, Z = 4, Dc = 1.521 g/cm^3, μ = 0.349 mm^-1 and F（000） = 928. The structure was solved by direct methods and refined to R = 0.0724 and wR= 0.1429 for 3494 observed reflections （I 〉 2σ（I））. Intermolecular hydrogen bonds along the b axis together with the continuous π-π interactions construct the three-dimensional architecture of the title compound. The preliminary biological tests show definite herbicidalactivity for the title compound.     

Synthesis,Crystal Structure and Theoretical Calculation of [2-（2,6-Dioxacyclohexyl）-5-methoxylphenols]2

The title compound [2-（2,6-dioxacyclohexyl）-5-methoxylphenols]2 was synthesized by the reaction of 2-hydroxyl-3-methoxylbenzaldehyde and 1,3-propanediol in the presence of DMF-DMS adduct and characterized by IR spectrum, UV-Vis spectrum and X-ray crystallography. The title compound belongs to monoclinic, space group P21 with a = 9.8967（10）, b = 8.2240（9）, c = 13.3654（14） A^°, β= 90.016（2）°, C11H14O4, Mr = 210.22, V = 1087.8（2）A^°3, Z = 4, Dc = 1.284 Mg/m^3, F（000） = 448,μ = 0.098 mm^-1, the final R = 0.0300 and wR = 0.0761 for 2070 observed reflections with I 〉 2σ（I）. The molecules are connected via intermolecular O-H…O hydrogen bonds into a 2D network structure. Moreover, theoretical investigations of the title compound with HF/6-31G（d） method were performed, and its stability, frontier molecular orbital composition and Mulliken charge distribution were also discussed. The compound is a bis-molecule. The two molecules stay together and could not be separated. Two crystallographically independent molecules exist in an asymmetric unit. The bond lengths and bond angles of the two molecules are slightly different with each other.