Synthesis and Crystal Structure of 1,2-Dis（1,3-diphenylpropan-2-yl）disulfane

A novel compound of 1,2-dis(1,3-diphenylpropan-2-yl)disulfane(C30H30S2,Mr=454.27)was synthesized in ethanol with 1,3-diphenyl-2-propanone as raw materials,giving high yield of product(90%).Its structure was determined by IR,1H NMR,MS,elemental analysis and X-ray diffraction.The crystal belongs to monoclinic,space group C2 with a=18.727(3),b=6.5179(9),c=13.7576(18),β=131.0610(10)o,V=1266.2(3)3,Z=2,Dc=2.136 g/cm3,μ=1.078 mm-1,F(000)=843,R=0.0490 and wR=0.1247 for 3211 observed reflections with I>2(I).X-ray analysis reveals that the molecule is not symmetrical.There exist no classical hydrogen bonds andπ-πstacking interactions.Moreover,the thermal stability of compound 3 was investigated.     

Synthesis and Crystal Structure of 3-（4-Bromobenzyloxy）-6-morpholinopyridazine

The title compound 3-(4-bromobenzyloxy)-6-morpholinopyridazine(C15H16BrN3O2) was synthesized,and its crystal structure was studied.It crystallizes in the triclinic system,space group P with a = 8.3408(17),b = 8.8620(18),c = 10.832(2) ,α = 108.09(3),β = 91.28(3),γ = 100.90(3)°,Dc = 1.562 g/cm3,Z = 2,λ = 0.71073 ,μ(MoKα) = 2.769 mm-1,Mr = 350.22,V = 744.5(3) 3,F(000) = 356,the final R = 0.0522 and wR = 0.1366 for 2016 observed reflections with I > 2σ(I).In the crystal structure,the morpholine ring adopts a chair conformation with O(2) and N(3) atoms at the flap positions-0.656(7) and 0.622(6)  out of the mean plane formed by the other four C atoms,respectively.These molecules generate centro-symmetric dimers through intermolecular π-π interaction.     

Synthesis, Crystal Structure, and Biological Activity of N-（ （ 1-cy clo h e xyl- 1H-tetrazo l-5-yl）（ 5-methyl- 1,2,3- thiadiazol-4-yl）methyl）-4-nitrobenzenamine

The title compound N-((1-cyclohexyl-1H-tetrazol-5-yl)(5-methyl-1,2,3-thiadiazol-4-yl) methyl)-4-nitrobenzenamine (C17H20N8O2S, Mr = 400.47) was synthesized via Ugi fourcomponents condensation reaction (U-4CR), and its structure was characterized by IR, 1H NMR, high-resolution mass spectrometry and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pna21 with a = 20.390(2), b = 12.9660(14), c = 6.9399(8) , β = 90.00°, Z = 4, V = 1834.7(3)3, Mr = 400.47, Dc = 1.450 g/cm3, μ = 0.210 mm-1, F(000) = 840, R = 0.0348 and wR = 0.0717. X-ray analysis reveals that the dihedral angles formed between the thiadiazole and tetrazole rings, the benzene and tetrazole rings and the thiadiazole and benzene rings are 62.59, 86.73 and 70.07°, respectively. Three intermolecular hydrogen bonds N(1)-H(2)···N(6), C(4)-H(4B)···O(2) and C(17)-H(17)···N(3) are observed. Bioassay shows that the title compound has antifungal and antivirus activities against tobacco mosaic virus.     

Microwave Synthesis and Crystal Structure of Bis {2- [（2,4-dichloro-phenylimino）- methyl]-4,6-diiodo-phenol}-copper（II）

Bis{2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P2 1 /n with a=14.7558(17), b=20.770(2), c=20.3260(19) , β=90.6110(10)°, V=6229.2(11) 3 and Z=8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.     

Synthesis and Crystal Structure of 4,5-Bis（2-chloroethylthio）phthalonitrile

A novel phthalonitrile compound,[C12H10Cl2N2S2],has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 10.6417(8),b = 7.5737(6),c = 18.2758(14),β = 105.2480(10)°,Mr = 317.24,V = 1421.12(19)3,Z = 4,Dc = 1.483 g/cm3,F(000) = 648,μ = 0.733 mm-1,R = 0.0173 and wR = 0.2183.In the structure,the C atoms of the aromatic ring,the two cyanide groups and the two S atoms are almost coplanar(maximum deviation from the mean plane = 0.049(7) ).Two potential weak intermolecular interactions of C-H…N and one type of π…π stacking interaction with a centroid-centroid separation of 3.751(8) stabilize the crystal structure.     

Synthesis and Crystal Structure of 3,9-Bis（pyridin-2-yl）-2,4,8,10-tetraoxaspiro[5.5]undecane

The title compound 3,9-bis(pyridin-2-yl)-2,4,8,10-tetraoxaspiro[5.5]undecane 4(C17H18N2O4) has been synthesized by the reaction of 2,2-bis(hydroxymethyl)propane-1,3-diol with pyridine-2-carbaldehyde in the presence of p-toluenesulfonic acid,and characterized by IR,1H-NMR and X-ray single-crystal diffraction.The crystal belongs to monoclinic system,space group C2/c with a = 25.133(2),b = 5.7219(5),c = 21.942(2) ,β = 99.145(2)°,V = 3115.3(5)3,Z = 8,Dc = 1.340 g/cm3,Mr = 314.33,F(000) = 1328,μ = 0.097 mm-1,MoKa radiation(λ = 0.71073),R = 0.0352 and wR = 0.1022 for 2486 observed reflections with I > 2σ(I).X-ray analysis reveals that the two 1,3-dioxane rings passing through the central spiro-C atom both adopt chair conformation.Intermolecular C-H…π,C-H…O and C-H…N weak interactions link the molecules to form a three-dimensional samdwich,which are effective in the stabilization of the crystal structure.     

Synthesis and Crystal Structure of 2-Nitro-9,9-bis（methylpropionate）fluorine

The title compound of 2-nitro-9,9-bis(methylpropionate)fluorine (C21H21NO6 , Mr=383.39) was synthesized for the first time. Complete assignments were achieved by 1H NMR, IR, EI-MS, elemental analysis and single-crystal X-ray diffraction technique. The crystal belongs to monoclinic, space group P21/c with a=11.4581(15), b=10.3624(14), c=16.573(2) , β=96.629(2) o , V=1954.6(5) 3 , Z=4, Dc=1.303 g/cm 3 , μ=0.096 mm -1 , F(000) = 808, R =0.0493 and wR=0.1499 for 3107 observed reflections with I > 2σ(I). X-ray analysis reveals that three fused rings of the fluorene system are almost coplanar and the two ester groups are nearly perpendicular to the fused-ring system. Weak C-H O hydrogen bonding connects the molecules into centrosymmetric dimmers.     

Synthesis,Bioactivity and Crystal Structure Analysis of N-（2-ethoxyphenyl）-3-oxobenzo[d]isothiazole-2（3H）-carboxamide

The title compound N-(2-ethoxyphenyl)-3-oxobenzo[d]isothiazole-2(3H)-carboxa-mide(C16H14N2O3S,Mr = 314.35) has been synthesized and structurally characterized by IR,1H NMR and single-crystal X-ray diffraction.The crystal belongs to triclinic,space group P with a = 4.6395(15),b = 8.689(3),c = 17.917(7),α = 87.763(9),β = 84.625(9),γ = 82.344(9)°,V = 712.4(4)3,Z = 2,Dc = 1.465 Mg·m-3,λ(MoKa) = 0.71073,F(000) = 328,μ(MoKa) = 0.242 mm-1,the final R = 0.038 and wR = 0.089.A total of 3702 unique reflections were collected,of which 2762 with I > 2σ(I) were observed.X-ray analysis revealed that the benzisothiazolone ring and benzene moieties were essentially planar,and three intramolecular hydrogen bonds N(2)-H(2N)…O(1),N(2)-H(2N)…O(3) and C(10)-H(10)…O(2) were observed.The preliminary biologi-cal test showed that the title compound had antifungal and antibacteria activities against Bacillus subtilis(CMCC63003),Aeromonas hydrophila(ATCC7966),Staphylococcus aureus(ATCC6538),Escherichia coli(JM103),Blastomyces albicans,Gloeosporium papaya P.Henn,Colletotrichum gloeosporioides Penz and Botryodiplodia theobromae.     

Synthesis,Crystal Structure and Biological Activity of 2-（Anthracen-9-yl）-5-p-tolyl-1,3,4-oxadiazole

A novel compound,2-(anthracen-9-yl)-5-p-tolyl-1,3,4-oxadiazole(C23H16N2O),has been synthesized by the condensation of 4-methylbenzohydrazide and anthracene-9-carbaldehyde in an ethanol solution with chloramine-T.The compound was characterized by 1H-NMR,13C-NMR,MS and single-crystal X-ray diffraction.The crystal belongs to the triclinic system,space group P with a = 7.7817(4),b = 8.8544(5),c = 12.4726(8) ,β = 92.8520(10)°,Z = 2,V = 826.58(8) 3,Dc = 1.352 g/cm3,Mr = 336.38,λ(MoKα) = 0.71073 ,μ = 0.084 mm-1,F(000) = 352,R = 0.0381 and wR = 0.1099.The dihedral angle between anthracene skeleton and phenyl ring is 64.19°.A total of 6354 unique reflections were collected,of which 3172 with I > 2σ(I) were observed.X-ray analysis indicated an offset face-to-face π-π stacking interaction between anthracene skeletons and an offset face-to-face π-π stacking interaction between phenyl ring planes.The novel compound molecules are connected through the offset face-to-face π-π stacking interactions to generate a three-dimensional network.The preliminary bioassay results showed that the novel compound exhibited significant insect growth inhibitory activity against Spodoptera litura Fabricius larvae.     

Synthesis and Crystal Structure of 3,3＇-（4-Dimethylaminobenzylidene）- bis-（4-hydroxycoumarin）

The title compound 3,3'-(4-dimethylaminobenzylidene)-bis-(4-hydroxycoumarin) 3 was synthesized by the reaction of 4-hydroxycoumarin with 4-dimethylaminobenzaldehyde, and its chemical structure was determined by X-ray single-crystal diffraction. It crystallizes in monoclinic, space group P21/n with a = 11.698(2), b = 10.882(2), c = 16.594(3) , β = 90.69(3)o, V = 2112.1(7) 3, Z = 4, F(000) = 952, Dc = 1.432 Mg/m3, Mr = 455.45, μ = 0.102 mm-1, λ = 0.71073 , the final R = 0.0779 and wR = 0.2143 for 3031 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of 1,4-Dimethyl-2,5-di{[2’-(3-pyridylmethylamino-formyl)phenoxyl]methyl}benzene Perchlorate

The title compound, 1,4-dimethyl-2,5-di{[2’-(3-pyridylmethylaminoformyl)phenoxyl]- methyl}benzene perchlorate (C36H36Cl2N4O12, Mr = 787.59), has been synthesized and structurally determined by single-crystal X-ray diffraction. The crystal crystallizes in the orthorhombic system, space group Pbca with a = 14.366(4), b = 15.159(4), c = 16.443(5), V = 3580.9(17)3, Z = 4, Dc = 1.461 g/cm3, μ = 0.253 mm-1, F(000) = 1640, R = 0.0618 and wR = 0.1525 for 1615 observed reflections (I > 2σ(I)). In the structure of the title compound, a two-dimensional supramolecular layer is formed via intermolecular hydrogen bonding interactions.     

Synthesis,Crystal Structure and DNA-binding Properties of a New Copper（Ⅱ） Schiff Base Complex

A new asymmetric bidentate copper(Ⅱ) complex,CuL 2(HL=2-((E)-(4-bromophenylimino)methyl)-6-bromo-4-chlorophenol),has been synthesized and characterized by elemental analyses and single-crystal X-ray diffraction.The complex crystallizes in the monoclinic space group P2 1 /c with a=11.218(3),b=9.355(3),c=13.449(4),β=108.722(4)°,V=1336.8(6)3,Z=2,Dc=2.008 g/cm 3,μ(MoKα)=7.024 mm-1,F(000)=806,S=0.999,the final R=0.0342 and wR=0.0641for2611observed reflections (I>2σ(I)).The central copper(Ⅱ) is four-coordinate and bonds to two nitrogen and two oxygen atoms from two Schiff base ligands.The complex is linked into a two-dimensional supramolecular structure by weak intermolecular interactions.In addition,DNA-binding properties of the metal complex were investigated using spectrometric titrations and viscosity measurements.The results show that the complex binds with calf-thymus DNA(CT-DNA),presumably via a partial intercalative mode.The intrinsic binding constant of the Cu(Ⅱ) complex with DNA is 7.335×10 3 M-1.     

Synthesis and Crystal Structure of Cd（tla）（NO_3）_2［TLA＝tris（6－methyl－2－pyridylmethyl） amine］

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Synthesis, Characterization and Crystal Structure of （＋）-N-[（3S）-3-（4- fluoroph enyl）heptan oyl] bornan e-10,2-s ultam

The chiral molecule (+)-N-[(3S)-3-(4-fluorophenyl)heptanoyl]bornane-10,2-sultam (C23H32FNO3S, Mr = 421.56), a fluorine-containing derivative of camphorsultam, was conveniently obtained and crystallized in the orthorhombic space group P212121 with a = 7.9044(11), b = 11.6680(16), c = 24.899(3) , V = 2296.4(5) 3, Z = 4, Dc = 1.219 Mg/m3, λ = 0.71073 , μ(MoKα) = 0.172 mm-1 and F(000) = 904. X-ray diffraction analysis reveals that the six-membered ring of sultam shows a boat conformation (Fig. 1). The planes constructed by ((C6), (C7), (C8), (C9)) and ((C4), (C5), (C6), (C9)) form a dihedral angle of 70.3(3)°. The plane of (C1)-(C2)-(C3) forms dihedral angles to the aforementioned planes of 85.9(4) and 89.5(4)°, respectively. The molecules are linked via C-H···O/F interactions.     

Synthesis and Crystal Structure of （E）-N,N＇- dicyclohexyl- 1-（3-（3,4-dihydroxyphenyl）acryloyl）urea

The title compound, (E)-N,N′-dicyclohexyl-1-(3-(3,4-dihydroxyphenyl)acryloyl)- urea (DDA), has been synthesized and characterized by FT-IR and 1H-NMR spectroscopy, ESI- MS, and X-ray single-crystal diffraction. Its crystallizes in monoclinic, space group C2/c with a = 20.483(12), b = 11.153(6), c = 21.134(12) , β = 117.098(7), V = 4298(4) 3, Z = 8, F(000) = 1664, Dc = 1.195 Mg/m3, Mr = 386.48, μ= 0.082 mm-1, the final R = 0.0474 and wR = 0.1370 for 4853 observed reflections with I > 2σ(I).     

Synthesis and Crystal Structure of （5-Hydroxy-6-methoxybenzofuran- 3-yl）-（4-methoxyphenyl）methanone

Compound 1 (5-hydroxy-6-methoxybenzofuran-3-yl)(4-methoxyphenyl)methanone, C17H14O5 , as a potential anti-breast cancer agent has been synthesized under microwave irradiation, which was further converted to (5,6-dihydroxybenzofuran-3-yl)(4-methoxyphenyl)methanone (2). The compounds were characterized by MS and NMR spectra. Meanwhile, the crystal of 1 was obtained and determined by X-ray single-crystal diffraction. Crystal data: monoclinic system, space group P21/n, a=8.908(6), b=10.505(7), c=15.452(11), β=105.043(9)°, V=1396.4(16)3 , Z=4, F(000)=624, Dc=1.419 g/cm3 , μ=0.105 mm1, R=0.0513 and wR=0.1246 for 14459 independent reflections (Rint=0.0647) and 2488 observed ones (I>2σ(I)). Intermolecular O-H···O and π-π stacking interactions contributed to the stability of the structure.     

Synthesis,Crystal Structure and Antifungal Activity of a New Zn(Ⅱ) Complex Based on 4-(5-(Pyridin-3-yl)-4H-1,2,4-triazol-3-yl) Benzoic Acid

A new complex[Zn(3,4-APT)2(H2 O)4]·8 H2 O(1,3,4-HAPT=4-(5-(pyridin-3-yl)-4 H-1,2,4-triazol-3-yl)benzoic acid)has been prepared and characterized by elemental analysis,X-ray single-crystal diffraction analysis,thermogravimetric analysis and infrared spectrum analysis.Theoretical calculation based on density functional theory(DFT)is also employed to explicate frontier orbitals of 3,4-HAPT.X-ray single-crystal diffraction analysis reveals that 1 belongs to the triclinic system,space group P1 with a=7.5123(3),b=8.6745(3),c=15.2074(6)?,α=78.469(1),β=87.387(1),γ=65.448(1)°,V=882.42(6)?,Z=1,D_c=1.528 g·cm^–3,μ=0.780 mm^–1,M_r=812.09,F(000)=424,the final R=0.0401 and wR=0.1136.Zn(II)ion is coordinated by two N atoms from two 3,4-HAPT as well as four O atoms from four coordinated water molecules,forming a 0D motif with distorted octahedral coordinated geometry.The adjacent 0 D units are linked into a 3 D supramolecular structure through hydrogen bonding interaction.In addition,complex 1 exhibits better antifungal activity against Colletotrichum gloeosporioides Penz than the ligand and metal salt by MIC,MBC tests and Kirby-Bauer disc diffusion method which exhibit potential application in the antifungal fields.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cadmium（Ⅱ） Complex

A metal-organic coordination polymer [Cd2(cbba)4(bix)2] n·nH2O (Hcbba=2-(4′-chlorine-benzoyl)-benzoic acid, bix=1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis, IR, TG, fluorescence spectrum and single-crystal X-ray diffraction. Colorless crystals crystallize in the triclinic system, space group Pī with a=12.9891(15), b=15.3211(19), c=21.154(3), α=108.476(3), β=90.148(2), γ=105.429(3)°, V=3831.5(8)3 , C84H60Cd2Cl4N8O13 , Mr=1756.00, Dc=1.522g/cm3 , F(000)=1776, Z=2, μ(MoKα)=0.765 mm-1 , the final R=0.0724 and wR=0.1208 for 6916 observed reflections (I > 2σ(I)). The structure of 1 exhibits a one-dimensional infinite chain-like structure.     

Hydrothermal Synthesis and Crystal Structure of a One-dimensional Cobalt（Ⅱ） Complex

A metal-organic coordination polymer [Co2(cbba)4(bix)2]n(Hcbba = 2-(4'-chlorine-benzoyl)-benzoic acid,bix = 1,4-bis(imidazol-1-ylmethyl)-benzene) 1 has been hydrothermally synthesized and characterized by elemental analysis,IR,TG,and single-crystal X-ray diffraction.Pink crystals crystallize in the monoclinic system,space group P21/n with a = 21.148(4),b = 15.728(3),c = 23.879(4) ,β = 102.148(3)°,V = 7764(2)3,C316H232Cl15Co8N32O48,Mr = 6248.53,Dc = 1.336 g/cm3,F(000) = 3207,Z = 1,μ(MoKα) = 0.621 mm-1,the final R = 0.0567 and wR = 0.1280 for 8510 observed reflections(I > 2σ(I)).The structure of 1 exhibits a one-dimensional chain-like structure.     

Synthesis, Crystal Structure, Antibacterial Activities and Theoretical Computation of 3-（2-Hydroxybenzly）-4-（4-isopropylbenzylideneamino）-（1H）-1,2,4-triazole-5-thione

1INTRODUCTION Recently,compounds containing pyrazole,imida-zole,triazole(including benzotriazole),pyridine,tetrazole and indole have attracted much interest because they exhibit some fungicidal activity,plant-growth regulating activity and antibacterial acti-vity[1～10].Schiff bases also constitute a good type of biologically active substructure[11～14],and the sulfur-containing Schiff bases are particularly effective.Studies of pyrazole Schiff base-type fungicides andtriazole compounds c…