Synthesis and Crystal Structure of a Luminescent Compound 5-（1H-benzoimidazol-2-yl）- 3H-[ 1,2,3 ] triazole-4-carboxylic Acid

The title compound, 5-(1H-benzoimidazol-2-yl)-3H-[1,2,3]triazole-4-carboxylic acid (C10H7N5O2·C3H7NO, Mr=302.30), has been synthesized and characterized by FT-IR and ESI-MS, 1 H-NMR spectroscopy and X-ray single-crystal diffraction. Crystal structure of the title compound was grown from DMF by slow diffusion at room temperature. Crystal data: orthorhombic structure, space group Pna21 with a=6.9635(3), b=19.4398(7), c=30.6165(12), V=4144.5(3)3, Z=12, Dc=1.454 g/cm 3, μ(MoKα)=0.108 mm-1, and F(000)=1896. The structure was refined to R=0.0450 and wR=0.0975 for 3578 observed reflections with I>2σ(I). The intermolecular hydrogen bonds and π-π stacking further stabilize the structure.     

Synthesis and Crystal Structure Analysis of 5′-O-Tosyl-2,3′-anhydrothymidine

In this paper=5′-O-tosyl-2,3′-anhydrothymidine has been synthesized and its crystal structure was analyzed. The crystal belongs to the triclinic system=space group P1=with a=5.397(2)=b=6.1886(18)=c=3.507(5) =α =87.74(2)=β =89.84(4)=γ =73.79(2)°=C17H18N2O6S=Mr=378.39=Z=1=V=432.8(3)3=Dc=1.452 g/cm3=F(000)=198 and Flack =-0.11(14). No intermolecular hydrogen bonds exist in the crystal=and the angle between benzene ring and pyrimidine planes is 32.23°.     

Synthesis and Crystal Structure of Ethyl 4-（2-Chloro-4-fluorophenyl）-6-hydroxy-3-oxo-1,3-dihydro-5-isobenzofurancarboxylate

The crystal structure of the title compound(C17H12ClFO5,Mr=350.72) was determined by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21/c,with a=7.693(1),b=15.767(1),c=12.986(1),β=97.23(1)°,V=1562.6(2)3,Z=4,Dc= 1.491 g/cm3,λ(MoKα)=0.71073,F(000)=720,μ(MoKα)=0.280 mm-1,R=0.0563 and wR=0.1674.A total of 3592 unique reflections were collected,of which 2462 with Ⅰ2σ(Ⅰ) were observed.Five-membered lactone rings and hydroxyl-substituted phenyl rings are approximately coplanar with their dihedral angle of 4.1°.The dihedral angle between two different phenyl rings is 71.3°.To our interest,intramolecular O(1)-H(1)···O(4) hydrogen bonds could be found in each molecule.Intramolecular hydrogen bonds and intermolecular van der Waals force contribute to the stability of the structure.     

Synthesis and Crystal Structur of (4,4′-H_2bipy)[CdBr_4]·H_2O

The title compound (4,4′-H2bipy)[CdBr4]·H2O 1 has been synthesized via hydrothermal reaction and characterized by X-ray diffraction. The crystal belongs to monoclinic,space group P21/c with a=8.260(3),b=23.926(7),c=9.774(2),β=106.777(9)o,C10H12Br4CdN2O,Mr=608.26,V=1849.4(9)3,Z=4,Dc=2.185 g/cm3,S=1.005,μ(MoKα) =9.814 mm–1,F(000)=1128,R=0.0646 and wR=0.0989. The crystal structure analysis of 1 reveals that the title compound features an isolated structure,based on discrete 4,4′-H2bipy moieties and lattice water molecules which are linked by hydrogen bonds together with tetra-hedral cadmium atoms terminally coordinated by four bromine atoms.     

Crystal Structure of Phenol,2-[4（S）-4-Dihydro-4-benzyl-2-ozazolinyl]

The compound phenol,2-[4(S)-4,5-dihydro-4-phenyl-2-ozazolinyl(1,C15H13NO2) was synthesized with a simple,one step method free of water and air.It was obtained in a moderate yield from the reaction of 2-hydroxybenzonitrile with optically active amino alcohol in chloroben-zene under dry,anaerobic conditions.It belongs to the orthorhombic system,space group P212121 with a = 5.786(5),b = 10.730(5),c = 19.722(5),C15H13NO2,Mr = 239.26,V = 1224.4(12)3,Z = 4 and Dc = 1.298 mg/m3.The final R = 0.0324 for 1627 observed reflections with Ⅰ 2σ(Ⅰ) and Rw = 0.0826 for all data.The structure of compound 1 was determined by X-ray diffraction,NMR and HRMS.     

Synthesis and Crystal Structure of 2,3,4,6-Tetra-O-acetyl-1-{2-[(4-nitrophenoxy)methyl]-1,3,4-thiadiazole-5-thione-4-yl}-1-deoxy-β-D-glucopyranose

The title compound has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of orthorhombic system (C23H25N3O12S2,Mr=599.58),space group P212121 with a=6.2102(12),b=17.803(4),c=24.223(5),V=2678.0(9)3,Z=4,Dc=1.487 g/cm3,F(000)=1248,μ=0.268 mm-1,the final R=0.0483 and wR=0.1108 for 4174 observed reflections (I 2σ(I)).The C=S bond,which parallels to the anomeric C-H,adopts α orientation relative to the anomeric position of glucopyranoside.     

Synthesis,Crystal Structure and Antitumor Activity of N-（4-tert-butyl-5-（4-chlorobenzyl）thiazol-2-yl）-2,6-difluorobenzamide

The title compound was synthesized by the reaction of 4-tert-butyl-5-(4-chlorobenzyl)-2-aminothiazole with 2,6-difluorobenzoic acid. The crystal structure of the title compound, C21H19ClF2N2OS, was determined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group Pbca with a = 12.6479(13), b = 13.1204(13), c = 14.1341(15), Z = 4, V = 2011.5(4)3, Mr = 420.89, Dc = 1.390 g/cm3, S = 1.023, μ = 0.326 mm-1, F(000) = 872, the final R = 0.0365 and wR = 0.0880 for 6101 observed reflections(I 2σ(I)), and R = 0.0507, wR = 0.0978 for 7779 independent reflections. X-ray crystal structure displays that the hydrogen bonding interactions observed link the molecules to form a dimeric unit. The preliminary biological test of the title compound shows good antitumor activity, with IC50 of 0.046 μmol/mL against the Hela cell line.     

Synthesis and Crystal Structure of 3,6-Dimethyl- 9-（4-b rom o p h enyl）- 1,8-oxo-2,7,10-trioxanth ene

The crystal structure of the title compound (C19H13BrO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/c,with a=10.508(4),b=11.354(4),c=14.522(5),β=106.255(4)°,V=1663.4(10)3,Mr=401.20,Z=4,Dc=1.602 g/cm3,λ=0.71073,F(000)=808,μ= 2.498 mm-1,R=0.0337 and wR=0.0837 for 2200 observed reflections (I>2σ(I)). X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3,1 and 4,2 and 3,2 and 4,and 3 and 4 are 78.6,82.5,87.4,5.6,9.5 and 4.9°,respectively. There exists a conjugated system in the molecular structure.     

Isolation and Identification of 5,3′,4′-Trihydroxy-7-methoxyflavanone from Artemisia sphaerocephala Kraschen

5,3′,4′-Trihydroxy-7-methoxyflavanone was isolated from Artemisia sphaeroce- phala Kraschen and characterized by 1H-NMR, 13C-NMR, EI-MS, IR, UV spectra, and single- crystal X-ray diffraction. The title compound crystallizes in orhtorhombic space group Pca21, with a = 14.393(3), b = 5.1629(12), c = 36.919(9), V = 2743.4(11)3, Z = 8, Mr = 302.27, Dc = 1.464 g/cm3, F(000) = 1264, μ = 0.113 mm-1, S = 1.015,(Δ/σ)max = 0.000, the final R = 0.0757 and wR = 0.1809. Structural analysis indicates the title compound consists of two 5,3′,4′-trihydroxy- 7-methoxyflavanone enantiomers in a well-defined arrangement within the crystal lattice, which constructs a three-dimensional network by means of multiple O–H···O hydrogen bonds.     

Synthesis,Crystal Structure and Luminescent Property of a New Copper(Ⅰ) Iodide Complex Based on 3,5-Dimethyl-4-amino-triazole

The title compound,[Cu4I4(C4H8N4)4],has been synthesized and characterized by single-crystal X-ray diffraction analysis.It crystallizes in monoclinic,space group Pbca,with a=18.1851(10),b=9.3697(5),c=19.8034(10),V=3374.3(3)3,C16H32Cu4I4N16,Mr=1210.34,Z=4,Dc=2.383 g/cm3,μ=6.183 mm-1,F(000)=2272,S=1.032,the final R=0.0309 and wR=0.1180 for 3854 observer reflections(I2σ(I)).The structure of the title compound consists of tetranuclear copper cluster units bridged by the halogen atoms with the 3,5-dimethyl-4-aminotriazole ligands coordinated to the metal ions through the triazole nitrogen atoms.The luminescent property of 1 was also studied.     

Preparation and Crystal Structure of 15α-Hydroxyl-oleanolic Acid

The compound 15α-hydroxyl-oleanolic acid was biotransformed from oleanolic acid with Colletotrichum lini AS3.4486,and its structure was characterized by 1H NMR,13C NMR,HR-ESI-MS and single-crystal X-ray diffraction.The crystal of the title compound belongs to monoclinic,space group R3 with a=34.255(5),b=34.255(5),c=6.8671(14),β=90°,Z=9,V=6978(2)3,Mr=490.70,Dc=1.051 mg/m3,μ=0.069 mm-1,F(000)=2430,R=0.0375 and wR=0.0808.The title compound is stacked into a three-dimensional network through hydrogen bonds.     

SYNTHESIS OF 1H，1′H BIS（BENZ—Δ^4—IMIDAZ—OLINE）2,2′—SPIRO—TITANIUM DICHLORIDE

New model compound 1H,1′H-Bis（benz-Δ^4-imidazoline)2,2′-spiro-titanium dichloride was prepared and the structure of the compound was determined by 1R,MS and elementary analysis.     

Synthesis and Crystal Structure of 2-（1-Naphthalenylamino）-4-thiazolidinone

The compound 2-(1-naphthalenylamino)-4-thiazolidinone was synthesized by the reaction of 1-(naphthalene-1-yl)thiourea with ethyl chloroacetate in an ionic liquid, and its structure was characterized by IR, 1H NMR and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group P21 /c with a=10.0081(3), b=14.5312(4), c=7.8739(2) , β=99.425(3)°, Z=4, V=1129.64(5)3 , Dc=1.425 g/cm3 , μ=0.269 mm-1 , F(000)=504, the final R=0.0519 and wR=0.1507. X-ray analysis indicated that the five-membered ring is essentially planar in this molecule, and intermolecular hydrogen bonds N(1)-H(1)…N(2), C(3)-H(3)…O(1), C(4)-H(4)…O(1) and C(12)-H(12a)…O(1) were observed. π-π Stacking interactions contribute to the stability of the structure. DSC-TG analysis showed that the title compound experienced a phase change at 190 ℃ and began to decompose above 240 ℃.     

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

The title compound(E)-2-(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)me-thylphenol 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)=β=97.326(3)°=V=1995.9(5)3=Z=4=F(000)=808=C22H24N2O2S=Mr=380.49=Dc=1.266 g/cm3=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.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-(2-Pyridyl)benzimidazoleH_2]~(2 )·[SbCl_5]~(2-)}_2

A new supramolecular compound,{[2-(2-pyridyl)benzimidazoleH2]2 ·[SbCl5]2-}2,was synthesized by the hydrothermal reaction of o-diaminobenzene,2-pyridinecarboxylic acid and SbCl3 in 1:1 HCl solution,and characterized by chemical analysis,elemental analysis,IR spectra,thermogravimetric analysis and fluorescence spectra. The crystal structure was deter-mined by X-ray single-crystal diffraction. The crystal belongs to the monoclinic system,space group P21/c,with a=16.0397(13),b=14.3189(12),c=15.6370(13),β=105.8980(10)°,V=3454.0(5)3,Z=4,C24H22Cl10N6Sb2,Mr=992.48,Dc=1.909 g/cm3,μ=2.366 mm-1,S=1.010,F(000)=1920,R=0.0254 and wR=0.0555. The coordination anion,[SbCl5]2-which is a distorted tetragonal pyramid,is composed by coordinating action with Sb3 ion and five adjacent chloride ions. Every four coordination anions of [SbCl5]2-form a biquaternion ring structure through the secondary bonding of Sb···Cl. Moreover,the compound adopts a three-dimensional network supramolecular structure because of the hydrogen bonds and π-π stacking between the rings and the 2-(2-pyridyl)benzimidazole divalent cations. The title compound also shows good fluorescent behaviors.     

Hydrothermal Synthesis and Crystal Structure of a 2D Zinc（Ⅱ） Coordination Polymer with 5-Hydroxynicotinic Acid

The title compound,[Zn(5-hydroxynicotinate) 2 2H 2 O] n,has been synthesized by reacting zinc sulfate vitriol with 5-hydroxynicotinic acid under hydrothermal conditions,and its structure was determined by X-ray crystallography with the following data:monoclinic,space group C2/c,C 12 H 12 N 2 O 8 Zn,M r=377.61,a=10.223(3),b=10.319(3),c=13.613(4),β=105.922(6)°,Z=4,V=1380.9(8)3,F(000)=768,D c=1.816 g/cm 3,μ(MoKα)=1.826 mm-1,the final R=0.0401 and wR=0.1380 for 1157 observed reflections (I > 2σ(I)).In the structure of the title compound,the Zn II ion located in an inversion center lies in a distorted tetrahedral environment at a N 2 O 2 coordination mode,and the 5-hydroxynicotinic acid ligand links symmetry-related Zn II ions at a μ 2-N,O bridging way forming a two-dimensional covalent structure.In the crystal,solvent water molecules form intermolecular O-H O hydrogen bonds and pyridine rings of adjacent layers form π-π stacking (3.346),which connect adjacent two-dimensional sheets into a three-dimensional supramolecular network.     

Synthesis, Crystal Structure and Antitumor Activity of （E）-4-tert-Butyl-N-（2,4-dichlorobenzylidene）-5-（1,2,4-triazol-1-yl）-thiazol-2-amine

The title compound (E)-4-tert-butyl-N-(2,4-dichlorobenzylidene)-5-(1,2,4-triazol-1-yl)-thiazol-2-amine was synthesized by the reaction of 4-tert-butyl-5-(1,2,4-triazol-1-yl)-thiazol-2-amine with 2,4-dichlorobenzaldehyde, and its crystal structure was determined by singlecrystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 7.9748(4), b = 10.1803(5), c = 11.4603(6), α = 102.882(1), β = 100.253(1), γ = 104.457(1)°, V = 850.95(7)3, Z = 2, F(000) = 392, C16H15Cl2N5S, Mr = 380.29, Dc = 1.484 g/cm3, S = 1.095, μ = 0.512 mm-1, the final R = 0.0301 and wR = 0.0965 for 3334 observed reflections (I 2σ(I)). The preliminary antitumor activity shows that for the title compound the IC50 of Hela is 0.175 μmol/mL and that of Bel7402 is 0.156 μmol/mL.     

S-（＋）-（E）-1-（2-furfuryl）-5-substituted-1,3,5-hexahydrotriazine-2-N-nitroimines：Synthesis,Crystal Structure and DFT Calculations

A novel neonicotinoid analogue(C13H19N5O5,3a)had been synthesized,the structure was characterized by elemental analysis,IR and 1H NMR spectra,and the S-(+)-(E)-configuration was confirmed by single-crystal X-ray diffraction.The crystal belongs to monoclinic,space group P21 with a = 8.7076(17),b = 8.3211(17),c = 10.642(2),β = 92.370(3)o,V = 770.4(3)3,Z = 2,Dc = 1.402 g/cm3,μ = 0.110 mm-1,Mr = 325.33,F(000)= 344,S = 1.027,R = 0.0543 and wR = 0.1229 for 3601 unique reflections with 2919 observed ones(I > 2σ(I)).Compound 3a is stabilized by intramolecular hydrogen bonds and intermolecular force.In addition,the structure of compound 3a was optimized by the B3LYP/6-31G(d,p).DFT/B3LYP optimizations were performed based on X-ray geometries applying 6-31G(d,p)basis set.The optimized structure of compound 3a by the B3LYP/6-31G(d,p)method is more bent than in the crystal.IR spectrum of the solid compound is consistent with the X-ray structure.The HOMO-LUMO gap in 3a(5.3 eV)indicates high kinetic stabilities of compound 3a.The preliminary bioassay test showed that 3a exhibited good activities against Nilaparvata legen,Pseudaletia separate Walker and Aphis medicagini at 500 mg/L.     

Synthesis and Crystal Structure of 4,4′-Diamino-N,N′-diethyl Bisbenzenesulfamide

A new compound of 4,4′-diamino-N,N′-diethyl bisbenzenesulfamide (C18H26N4O4S2, Fw = 426.55) has been synthesized and its structure was determined by X-ray crystallography method. The crystal belongs to the monoclinic system, space group P21/c with a = 10.0623(9), b = 13.6759(13), c =15.5309(14) , β = 100.482(2)o, V = 2101.6(3) 3, Dc = 1.348 g/cm3, F(000) = 904, μ = 0.285 mm–1, Z = 4, the final R = 0.0512 and wR = 0.1363 for 3485 observed reflections with I > 2σ(I). The structure of the title compound is pseudo secondary axisymmetric, and the two sulfamide-groups show distorted tetrahedral configurations.     

A New One-dimensional Chain-like Ag（I） Complex with Schiff Base Ligand Containing 4-Amino-1,2,4-triazole

The title compound,poly[N-[1-(3-pydidyl)ethylidene]-4H-1,2,4-triazol-4-amine sil-ver(I) tetrafluoroborate],[Ag(C9H9N5)(BF4)]n,is the result of complexing Ag cation with N-[1-(3-pydidyl)ethylidene]-4H-1,2,4-triazol-4-amine (L),and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system,space group C2/c with a= 18.899(6),b=9.882(2),c=15.472(4),β=120.158(3)°,V=2498.5(11)3,C9H9AgBF4N5,Mr= 381.89,Dc=2.031 g/cm3,μ(MoKα)=1.659 mm-1,F(000)=1488,Z=8,the final R=0.0441 and wR=0.0619 for 1094 observed reflections (I 2σ(I)).In the structure,ligand L bridges the two metal Ag(I) centers in a bidentate fashion and each metal ion coordinates with two nitrogen atoms,forming a one-dimensional rectangular chain.The neighboring chains are connected by two additional Ag-N weak interactions into a 3D framework structure.The title compound shows blue fluorescence property at room temperature.