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 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 7-Amino-2,3,4,5-tetrahydro- 1,3-dimethyl- 5-（2-nitrophenyl）-2,4-dioxo-lH-pyrano[2,3- d]pyrimidine-6-carbonitrile DMF Solvate

The title compound 7-amino-2,3,4,5-tetrahydro-1,3-dimethyl-5-（2-nitrophenyl）- 2,4- dioxo-1H-pyrano[2,3-d] pyrirnidine-6-carbonitrile DMF solvate 1 （C19H20N6O6, Mr = 428.41） was synthesized and crystallized. The crystal belongs to the monoclinic system, space group P2 1/c with a = 11.383（2）, b = 13.372（2）, c = 13.673（2）A, β = 97.380（4）°, Z = 4, V = 2063.8（6）A^3, Dc = 1.379 g/cm^3,μ（MoKα） = 0.105 mm^-1, F（000） = 896, the final R = 0.0738 and wR = 0.1647 for 2964 observed reflections （I〉 2σ（I））. X-ray analysis reveals that the new pyran ring is coplanar, which is obviously different from those of other similar compounds. In addition, the unclassical hydrogen bonds of C-H…O and C-H…N are presented in the crystals except for the normal hydrogen bonds of N-H…O.     

Synthesis and Crystal Structure of N-（1′-H-Pyrrol- 2′-ylcarbonyl）-5-amino- 1,10-phenanthroline

The title compound, N-（1′-H-pyrrol-2′-ylcarbonyl）-5-amino-1,10-phenanthroline, was synthesized by the reaction of a-pyrrolyl carbonyl chloride and 5-amino-1,10-phenanthroline in pyridine. Determined by X-ray structure analysis, it crystallizes in triclinic system, space group P1 with the following crystallographic data： C20H21N5O3, Mr = 379.42, a = 7.8559（4）, b = 9.1681（6）, c = 14.6818（9） A, α= 73.254（10）,β= 88.938（15）, γ= 68.080（10）°, V= 934.66（10） A3, Z = 2, F（000） = 400, Dc = 1.348 g/cm^3 and p = 0.094 mm-1. The final R = 0.0680 and wR = 0.1419 for 2142 observed reflections with I 〉 2σ（/）, and R = 0.1084 and wR = 0.1643 for all reflections. Two aromatic ring planes （pyrrole and phenanthroline rings） are connected by the amide plane. Two different types of intermolecular hydrogen bonds, O-H…N and N-H…O, exist in the crystal. The title complex molecules are connected through hydrogen bonds and weak π-π stacking interactions to generate a 3-D supramolecule.     

Synthesis and Crystal Structure of 1-（2,6-Dichloro-4-nitrophenyl）-5-amino-4-cyanopyrazole

The crystal structure of 1-（2,6-dichloro-4-nitrophenyl）-5-amino-4-cyanopyrazole （C10H10Cl2N5O2, Mr = 298.09） has been determined by single-crystal X-ray diffraction. It crystallizes in the triclinic system, space group P1^- with a = 8.1258（10）, b = 8.6460（10）, c = 10.0214（12） A, α = 68.986（2）, β = 71.598（2）, γ = 85.181（2）°, V = 623.26（13） A3, Z = 2, Dc = 1.588 g/cm^3,μ = 0.525 mm^-1, F（000） = 300, R = 0.0613 and wR = 0.1524 for 1890 observed reflections, and the extinction coefficient = 0.010（5）. The crystal structure is stabilized by N-H...N hydrogen bonds.     

Synthesis and Crystal Structure of [2-Hydroxy- 5-（4-hydroxy-3-phenyliminomethylbenzyl）-benzylidene]-phenyl-amine

The title compound [2-hydroxy-5-（4-hydroxy-3-phenyliminomethyl-benzyl）-benzylidene]-phenyl-amine （C27H22N2O2, Mr = 406.47） was synthesized by 5,5′-methylene-bissalicylal- dehyde with aminobenezene, 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 = 4.4026（6）, b = 1.501（13）, c = 0.95818（12） nm, β = 90.868（2）°, V= 4.2813（9） nm^3, Z= 8, Dc= 1.292 g/cm^3,μ = 0.010, F（000） = 1744, R = 0.0576 and wR = 0.1450 for 3766 observed reflections with I 〉 2σ（I）. X-ray analysis reveals that the molecule has a pair of intramolecular OH…N hydrogen bonds.     

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 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

Hydrothermal Synthesis,Crystal Structure and Fluorescence Spectrum Studies of a Supramolecular Compound {[2-（2-Pyridyl）benzimidazoleH2]2＋ ·[SbCls]2-}2

A new supramolecular compound, { [2-（2-pyridyl）benzimidazoleH2]2＋.[SBC15]2-}2, was synthesized by the hydrothermal reaction of o-diaminobenzene, 2-pyridinecarboxylie acid and SbCl3 in 1：1 HC1 solution, and characterized by chemical analysis, elemental analysis, IR spectra, thermogravimetfic 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 P211c, with a = 16.0397（13）, b = 14.3189（12）, c = 15.6370（13） A, β = 105.8980（10）°, V = 3454.0（5） A3, Z = 4, C24H22Cl10N6Sb2, Mr = 992.48, Dc = 1.909 g/cm3,/z = 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.     

Synthesis and Crystal Structure of Ethyl 1-（2-bromoethyl）-3-（4-meth-oxyphenyl）-1H-pyrazole-5-carboxylate

The title compound ethyl 1-(2-bromoethyl)-3-(4-methoxyphenyl)-1H-pyrazole-5-carboxylate 1 has been synthesized and structurally characterized by single-crystal X-ray diffraction.The crystal is of monoclinic(C15H17BrN2O3,Mr = 353.22),space group C21 with a = 24.691(7),b = 6.7678(17),c = 17.884(5) ,β = 97.184(5)o,V = 2965.1(13) 3,Z = 8,Dc = 1.583 g.cm-3,F(000) = 1440,μ = 2.784 mm-1,the final R = 0.0260 and wR = 0.0596 for 2684 observed reflections with I > 2σ(I).All the carbon atoms in the molecule are nearly coplanar except C(15),with a large conjugated system among the carbonyl group,pyrazole ring and the benzene ring.Three non-classical intermolecular hydrogen bonds help to stabilize the crystal lattice.The regioselectivity was rationalized based on the coordination of potassium ion with the N-anion and the carbonyl oxygen atom.     

Synthesis and Crystal Structure of 2-Amino-3-ethoxycarbonyl-4-（4-chlorophenyl）-4H, 5H-pyrano-[3,2-c]-benzopyran-5-one

1 INTRODUCTION The coumarins constitute an important class of bioactive natural products[1]. They have been found to possess diverse biological properties including antimicrobial, insecticidal, estrogenic, anticoagulant and antithrombotic activities. Som…     

Synthesis and Crystal Structure of S-（＋）-N＇-Tertbutylaminocarbonyl-N- [3-methyl-2-（4-chlorophenyl）butyryl] Thiourea

The title compound S-( )-N'-tertbutylaminocarbonyl-N-[3-methyl-2-(4-chlorophenyl)butyryl] thiourea has been synthesized and its crystal structure was determined by singlecrystal X-ray diffraction an alysis. There exist intramolecular N(2)-H(2A)… O(1), C(17)-H(17A)…O(2) and N(3)-H(3A)…S(1) hydrogen bonds as well as intermolecular N-H…O interaction between the carbonyl and amidogen groups. Crystallographic data: C17H24ClN3O2S, Mr = 369.90,monoclinic, space group C2/c with a = 22.9922(19), b = 14.4844(12), c = 12.4618(11) (A),β =92.608(2)°, V= 4145.8(6) (A)3, Z = 8, Dc = 1.185 g/cm3, F(000) = 1568,μ(MoKa) = 0.298 mm-1, R =0.0578 and wR = 0.1308.     

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 2-[（4-Methoxy- 6-methylthio-2-pyrimidinyl）aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

1 INTRODUCTION The sulfonylurea herbicides are characterized by broad-spectrum weed control at very low use rates (c.2~75g ai ha-1), good crop selectivity and very low acute and chronic animal toxicity (acute oral LD50 to rat >4000 mg/kg)[1]. They are e…     

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.     

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, <'1>H NMR, and single-crystal X-ray diffraction.Compound 1 crystallizes in monoclinie, space group P2<,1>/c with a = 7.7924(10), b = 24.490(3), c =7.8989(9)(A),β = 94.987(6)°, V = 1501.7(3)(A)<'3>, Z = 4, R = 0.0345 and wR = 0.0739. Compound 2 crystallizes in monoclinic, space group P2<,1>/c with a = 7.4099(11), b = 24.868(4), c = 8.3255(12)(A),β= 112.796(8)°, V= 1414.3(4)(A)<'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.     

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 （S）-Ethyl-2-（2-methoxy-phenylsulfenamido）-3-（1H-indol-3-yl）propanoate

With an aim to discover novel AHAS inhibitors,the title compound (S)-ethyl-2(2-methoxy-phenylsulfenamido)-3-(1H-indol-3-yl)propanoate (C 21 H 22 N 2 O 4 S,M r=398.47) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis.The crystal belongs to orthorhombic,space group P2 1 2 1 2 1 with a=8.078(2),b=12.824(4),c=18.788(6),V=1946.2(10) 3,Z=4,F(000)=840,D c=1.360 mg/m 3,μ=0.197 mm-1,the final R=0.0433 and wR=0.1035 for 3075 observed reflections with I > 2σ(Ⅰ).The absolute structure Flack parameter X of this compound is 0.00(8).A total of 14375 reflections were collected,of which 3431 were independent (R int=0.0437).X-ray analysis reveals that the crystal structure involves two intermolecular N-H···O and one N-H···S intermolecular hydrogen bonds with the neighboring molecules.The crystal structure was compared with our previously reported (S)-methyl 2-(4-R-phenylsulfonamido)-3-(1H-indol-3-yl)propanoate (R=H(1) and Cl(2)),which provided some useful information of these compounds.