Synthesis and Crystal Structure of 3-{[（1E） 1-（2- Hydroxyphenyl） methylidene]amino}-4-cyanopyrazole

The title Schiff base compound （C11H8N4O）, a derivative of pyrazole, has been synthesized by the reaction of salicylaldehyde and 3-amino-4-cyanopyrazole in absolute ethanol and characterized by elemental analyses, IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to the monoclinic system, space group P21/n, with a = 7.5594（7）, b = 18.3342（19）, c = 22.461（2） A^°, β = 98.419（2）°, V = 3079.5（5） A^°3, Mr = 212.21, Z = 12, F（000） = 1320, Dc = 1.373 g/cm^3, T = 298（2） K, 2 = 0.71073 A^°, the final R = 0.0571 and wR = 0.0493. A total of 5412 unique reflections were collected, of which 1612 with I 〉 2σ（I） were observed. The molecular structure adopts a trans configuration about the C=N double bond. The preliminary biological tests show that the compound has high antibacterial activities.     

Synthesis and Crystal Structure of 1,4,7,10-Tetrakis （2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10- tetraazacyclododecane

A novel molecule tetra-N-alkylation of cyclen （1,4,7,10-tetraazacyclododecane）, 1,4,7,10-tetrakis（2-（（4-hydroxy）phenoxy）ethyl）-1,4,7,10-tetraazacyclododecane 2, was synthesized and structurally characterized by single-crystal X-ray diffraction. The molecule turned into chiral helical compound crystals grown from EtOH by slow diffusion at room temperature and three of the four hydroquinone groups of the benzene ring formed a g-electron-rich cavity by C-H…π stacking interaction. The crystal belongs to the monoclinic system, space group P21/C with a = 13.9192（9）, b = 13.2871（6）, c = 22.1894（15）A^°, β = 91.4600（10）°, V = 4102.5（4）A^°3, Z = 4, Dc = 1.219 g/cm^3, C40H52N4O8, Mr = 752.89, F（000） = 1616,μ = 0.088 mm^-1, MoKa radiation （λ = 0.71073）, R = 0.0578 and wR = 0.1389 for 5588 observed reflections with I 〉 2σ（I）. Moreover, compound 2 was characterized with ^1H NMR, ^13C NMR, IR spectra and MS.     

Synthesis,Crystal Structure and Fungicidal Activity of （E）-2-[（4-tert-Butyl-5-（4-methoxybenzyl）thlazol-2 yhmino）methyl]phenol

The title compound （E）-2-[（4-tert-butyl-5-（4-methoxybenzyl）thiazol-2-ylimino）methyl]phenol was synthesized by the reaction of 5-（4-methoxybenzyl）-4-tert- butylthiazol-2-amine with salicylaldehyde, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 5.9362（8）, b = 11.5070（15）, c = 29.460（4）A, β= 97.326（3）°, V = 1995.9（5） A^3, Z = 4, F（000） = 808, C22H24N2O2S, Mr= 380.49, De= 1.266 g/cm^3, S = 1.031,μ = 0.181 mm^-1, the final R = 0.0474 and wR = 0.1441 for 4327 observed reflections （I 〉 2σ（I））. Intramolecular O-H…N hydrogen bond is observed in the crystal. The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.     

Synthesis and Crystal Structure of N,N′,N″- Tris-（2-aminophenyltriphenylphosphium）- benzene- 1,3,5-tricarboxamide

A new tripodal P,N ligand （C63H48N3O3P3） was prepared and characterized by elemental analysis, IR and single-crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P21/c with a = 13.013（3）, b = 28.406（6）, c = 14.911（3） A^°, β= 111.04（3）°, V= 5144.6（18） A^°^3 Z = 4, Dc = 1.276 g/cm^3, Mr = 987.95, λ（MoKa） = 0.71073 A^°,μ = 0.17 mm^-1, F（000） = 2064, R = 0.0786 and wR = 0.1545. A total of 43260 unique reflections were collected, of which 5112 with I 〉 2σ（I） were observed. The title compound has a central benzene ring, which is linked by -NH-CO- bonds to three 2-aminophenyltriphenylphosphium moieties, of which two with P（1） and P（2） centers are pointing to the same face of the central aryl ring, while the third one directs oppositely, forming a pseudo-propeller. In the crystal structure, there exist face-to-face π-π stacking interactions which increase the stability of the crystal structure.     

Synthesis and Crystal Structure of 4-tert-Butyl-6-（4-chlorophenyl）-3,6- dihydro-2H-1,3-thiazin-2-iminium Chloride

The title compound, 4-tert-butyl-6-（4-chlorophenyl）-3,6-dihydro-2H-1,3-thiazin- 2-iminium chloride （C14H18C12N2S）, has been synthesized by the reaction of 1-（4-chlorophenyl）- 4,4-dimethylpent-1-en-3-one with thiourea, and its crystal structure was determined by single- crystal X-ray diffraction. The crystal belongs to the monoclinic system, space group P211c with a = 16.3064（11）, b = 9.4471（6）, c = 11.2626 （8）A, β = 108.400（1）°, Z = 4, V = 1646.28（19） A^3, Mr = 317.26, Dc = 1.280 g/cm^3, S = 1.078,μ = 0.510 mm^-1, F（000） = 664, the final R = 0.0514 and wR = 0.1412 for 3210 observed reflections （I 〉 2σ（I））. The thiazine ring system displays a twisted boat conformation, and three N-H,..Cl hydrogen bonds exist in the crystal. The combination of two N-H...Cl hydrogen bonds generate an R2^1 （6） ring.     

Synthesis and Crystal Structure of N3-（Dimethyl- pyrimidine）-N4-（tri-O-acetyl-xylosyl） Thiourea

The crystal structure of the title compound （C18H24N4O7S, Mr = 440.47） was prepared by the condensation of 2,3,4-tri-O-acetyl-β-D-xylopyranosyl isothiocyanate with 4,6-dimethylpyrimidin-2-amine and structurally determined by single-crystal X-ray diffraction. The crystal belongs to the monochnic system, space group P2 1 with a = 7.5500（17）, b = 10.498（2）, c = 14.208（3） A, β = 99.929（4）°, V = 1109.2（4） A^3, Z = 2, Dc = 1.319 g/cm^3,μ = 0.191, F（000） = 464, Flack = 0.00（15）, R = 0.0684 and wR = 0.1103. In the crystal structure, the xylose ring adopts a ^4C1 chair conformation. Due to the hydrogen bonding interaction between N（4）-H（4A） and N（1）, the pyrimidine ring is well positioned.     

Synthesis,Crystal Structure and Biological Activities of N-（4-Cyanopyrazole-3-yl）- α-（3,5-difluorophenyl）- O,O-diisopropyl- α-aminophosphonate

The title compound has been synthesized by the addition reaction of N-（4-cyanopyrazole-3-yl）-3,5-difluorophenyl-imine and diisopropyl phosphate. Its structure was confirmed by means of IR, ^1H NMR and elemental analysis. The single-crystal structure of the title compound was determined by X-ray crystallography. The compound crystallizes in monoclinic, space group C2/c with a = 18.9959（14）, b = 9.2212（7）, c = 22.1108（16）A^°, β= 90.1540（10）°, V = 3873.0（5） A^°^3, Dc = 1.366 g/cm^3, Z = 8, μ = 0.185, F（000） = 1664, and the final R = 0.0503 and wR = 0.1539 for 2996 observed reflections （I 〉 2σ（I））. The results demonstrate that the dihedral angle between the pyrazole and benzene rings is 105.5°, and there is a full delocalized pyrazole system with sp^2 hydridization of N（3）. The crystal structure is stabilized by two intermolecular hydrogen bonds of N（1）-H（1）…O（3） and N（3）-H（3A）…N（4）. The preliminary biological test shows that the title compound has a moderate antifungal activity.     

Synthesis,Crystal Structure and Antimicrobial Property of 4-Bromo- 2- [（3-methypyridin-2-ylimino）methyl]phenol

The title Schiff base compound 4-bromo-2-[（3-methylpyridin-2-ylimino）methyl]phenol was prepared and structurally characterized by elemental analysis, IR spectrum, and single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P2 1/n, with a = 4.4870（9）, b = 19.953（4）, c = 13.860（3）A, β = 93.13（3）°, V = 1239.0（4）A3 Z = 4, Dc = 1.561 g/cm3, C13H11BrN2O2 , Mr = 291.15, p = 3.302 mm-1 and F（000） = 584. The final refinement gave R = 0.0608 and wR = 0.1377 for 1329 observed reflections with I 〉 2σ（I）. X-ray diffraction reveals that the non-hydrogen atoms in the compound are nearly coplanar, with the mean deviation of 0.0197A from the plane. The molecule adopts an E configuration about the central C=N functional bond. The compound possesses moderate antimicrobial property.     

Synthesis and Crystal Structure of （SiCl3）2Fe（CO）4

The compound （SiCl3）2Fe（CO）4 was synthesized and structurally characterized by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P2 1/n with α = 8.287（2）, b = 9.829（2）, c = 9.042（2） A, β = 96.19（3）°, V= 732.2（3） A^3, C4Cl6FeO4Si2, Mr = 436.77, Z = 2, Dc = 1.981 g/cm^3, F（000） = 424, μ（MoKα） = 2.282 mm^-1, the final R = 0.048 and wR = 0.164 for 1109 observed reflections （I 〉 2σ（I））. The crystal structure of （SiCl3）2Fe（CO）4 reveals that the Si（l）- Fe-Si（l）^a sequence is linear and perpendicular to the Fe（CO）4 cross-shaped plane.     

Synthesis,Crystal Structure and Biological Activity of 1-（β-D-Glucopyranosyl）-3- amino-5-methyl-1H-1,2,4-triazole

The title compound 1-（β-D-glucopyranosyl）-3-amino-5-methyl- 1H- 1,2,4-triazole was synthesized and characterized by IR, 1H-NMR and elemental analysis. Its single crystals of 2H2O adduct suitable for X-ray analysis were obtained by the slow evaporation of a H2O solution and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group P212121 with a = 7.7490（15）, b = 10.424（2）, c = 17.447（4） A^°, V = 1409.3（5） A^°^3, Z= 4, C9H20N4O7, Mr = 296.29, Dc = 1.396 g/cm^3,μ = 0.120 mm^-1, S = 1.007, F（000） = 632, R = 0.0686 and wR = 0.1560 for 1217 observed reflections with I 〉 20（I）. The title molecules are linked through intermolecular hydrogen bonds to form two 1-D chain structures, and such adjacent chains are further linked by intermolecular hydrogen bonds and H2O bridges to form a 3-D supramolecular network structure. The preliminary bioassay results showed that the title compound exhibits fungicidal activities against Gibberella zeae and Colletotrichum orbiculare.     

Synthesis and Crystal Structure of（E）-Ethyl 2-（4-（2,4-dimethoxybenzylideneamino）-5-（3,4,5-trimethoxyphenyl）-4H-1,2,4-triazol-3-ylthio）acetate

The crystal structure of the title compound(E)-ethyl 2-(4-(2,4-dimethoxy benzylide-neamino)-5-(3,4,5-trimethoxyphenyl)-4H-1,2,4-triazol-3-ylthio)acetate(4,C24H28N4O7S,Mr = 516.17) was synthesized and determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 13.162(2),b = 8.4506(13),c = 22.602(4) ,β = 99.888(3)°,μ = 0.183 mm-1,V = 2476.5(7)3,Z = 4,Dc = 1.385 g/cm3,F(000) =1088,T = 110(2) K,R = 0.0426 and wR = 0.1216 for 3859 observed reflections with I > 2σ(Ⅰ).     

Synthesis and Crystal Structure of (Z)-Ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxypheny-tetrahydrofuran-3,3-dicarboxylate

The title compound (Z)-ethyl-4-(4-methoxy)benzylidene-2-(3,5-dimethoxyphenyl)- tetrahydrofuran-3,3-dicarboxylate has been synthesized, and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to triclinic, space group P1-, with a = 8.140(3), b = 11.966(4), c = 13.771(5) α = 67.366(4), β = 85.165(5), γ = 75.806(4)°, V = 1200.1(7) 3, Z = 2, C26H30O8, Mr = 470.50, Dc = 1.302 g/cm3, F(000) = 500, λ(MoKα) = 0.71073 , μ = 0.096 mm–1, R = 0.0659 and wR = 0.1841 for 3080 observed reflections (I > 2σ(I)). As a key intermediate of HIV-1 integrase inhibitor, the synthesis and structure confirmation of the title compound are important for further studies.     

Synthesis, Crystal Structure and Fluorescent Properties of 1-（4-（Dimethylamino）benzylidene）- 4-（naphthalen- 1-yl） Thiosemicarbazide

1 INTRODUCTION Recently, for the fluorescent properties, Schiff base has been more and more important and widely studied in density optical memories, nonlinear op- tics (NLO), organic light-emitting diodes (OLED), polymer LED and electrogenerated chemilumines- cence (ECL)[1~5]. Thiosemicarbazones are a kind of Schiff bases with thiourea and good ligands easily chelating with transition metal ions. Although they have been studied extensively for a long time due to their chemical and b…     

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 and Crystal Structure of 3-（4-Chlorophenyl）-8-cyano-2-（di-isopropylamino）-5-methyl-7-（methylthio）-pyrido[4,3-d]pyrimidine-4（3H）-one

The crystal structure of the new title compound 3-(4-chlorophenyl)-8-cyano-2-(di-iso-propylamino)-5-methyl-7-(methylthio)-pyrido[4,3-d]pyrimidine-4(3H)-one(C22H24ClN5OS,Mr = 441.97)has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic,space group Pna21 with a = 7.6721(5),b = 18.9370(11),c = 15.6260(9),V = 2270.2(2)3,Z = 4,Dc = 1.293 g/cm3,F(000)= 928,μ = 0.283 mm-1,MoKa radiation(λ = 0.71073 ),R = 0.0494 and wR = 0.1062 for 3278 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the py-ridopyrimidinone moiety are almost coplanar. Intramolecular C(20)-H(20)···N(4),C(19)-H(19A)···N(3),C(18)-H(18C)···N(3)and C(16)-H(16B)···O(5)hydrogen bonds together with weak C···π interactions are found in the structure.     

Synthesis and Crystal Structure of 4,4′-(4-(1-Naphthyl)-4-phenyl- 1,3-butadienylidene)-bis[N,N-diethylbenzenamine]

The title compound (C40H42N2) has been synthesized by the reaction of 1-(1-naphthyl)-1-phenyl-3-chloropropylene and bis(4-(diethylamino) phenyl)methanone, and characterized by IR, 1H NMR, MS and X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 17.047(3), b = 10.807(2), c = 1&494(4) (A), β = 105.727(4)°, V=3279.4(11) A3, Mr = 550.76, Z = 4, Dc = 1.115 g/cm3, μ(MoKα) = 0.085 mm-1, F(000) = 1184, the final R = 0.0625 and wR = 0.1384 for 2276 observed reflections (I ＞ 2σ(Ⅰ)). X-ray analysis reveals that the butadiene fragment adopts a planar cisiod conformation and makes a dihedral angel of 69.4(2)° with the naphthalene ring.     

Synthesis,Crystal Structure and Anti-tumor Activity of 2-（2-Chloro-4-nitrophenyl）-4- （4-chlorophenyl）-3a,4-diethoxy-2,3,3a, 4-tetrahydrochromeno[3,4-d] [ 1,2,3]diazaphosphole

The title compound 2-（2-chloro-4-nitrophenyl）-4-（4-chlorophenyl）-3a,4- diethoxy- 2,3,3a, 4-tetrahydrochromeno[3,4-d][1,2,3]diazaphosphole 2 （C29H30Cl2N3O7P, Mr = 633.44） was synthesized and its structure was characterized by IR, MS, ^1H NMR, ^13C NMR, ^31p NMR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1^-, a = 9.1549（3）, b = 10.7168（4）, c = 17.6272（6）A, α = 102.9363（12）, β = 90.2713（9）, γ = 117.4265（10）°, V= 1484.41（9）A^3, Z= 2,μ（MoKa） = 0.323, F（000） = 658, Z= 2, De= 1.417 g/cm^3, the final R = 0.0687 and wR = 0.2066 for 4943 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the diazaphospholine ring is almost planar and the two ethoxy groups bonded on the 3a- and 4-positions are in trans configurations. Its antiproliferative activity was also tested in vitro against four human tumor cell lines.     

Synthesis and Crystal Structure of 2-（ 4-Decarboxydehydroabietyl）- 5-p-tolyl-[ 1,3,4 ]-oxadiazole

2-（4-Decarboxydehydroabietyl）-5-p-toyl-[1,3,4]-oxadiazole, C28H34N2O, has been synthesized and characterized by IR, NMR, elemental analysis and single-crystal X-ray diffraction method. The crystal belongs to the orthorhombic system, space group P212121 with a = 6.1351（5）, b = 14.8495（19）, c = 25.9050（2） A, V = 2360.0（4） A3, Z = 4, Mr = 414.57, Dc = 1.167 Mg/m^3, 2 = 0.71073 A,μ（MoKa） = 0.070 mm^-1, F（000） = 896, the final R = 0.0452 and wR = 0.1076 for 1647 observed reflections with I 〉 2σ（I）. There are five rings in the crystal structure of the title compound, but the oxadiazole ring is non-coplanar with the benzene ring D.     

Synthesis,Crystal Structure and Antifungal Activity of N-（Pyridine-2-methyl）-2-（4- chlorophenyl）-3-methylbutanamide

A novel compound N-（pyridine-2-methyl）-2-（4-chlorophenyl）-3-methylbutanamide, a racemic compound, has been synthesized with 2-（4-chlorophenyl）-3-methylbutyric acid and pyridin- 2-methylanamine as the raw materials, and its crystal structure （C17H19C1N2O, Mr = 302.79） was determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/n with a = 9.624（9）, b = 23.14（2）, c = 15.626（15）A, β = 106.199（14）°, V = 3342（5） A^3, Z = 8, Dc = 1.204 g/cm^3,μ = 0.23 mm^-1, F（000） = 1280, S = 1.032, R = 0.0681 and wR = 0.1508 for 6513 unique reflections （Rint = 0.0421） with 3375 observed ones. In the crystal structure, there are some intermolecular hydrogen bonds which stabilize the crystal structure. The preliminary bioassay shows that the title compound exhibits good antifungal activity against Botrytis cinerea, Gibberella zeae, Dothiorella gregaria and Colletotrichum gossypii.     

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.