Synthesis and Crystal Structure of Diethyl 5-Acetoxy-3-（4-chlorophenyl）- 4,5-dihydroisoxazol-5-yl-5-phosphonate

1INTRODUCTION Isoxazole derivatives are an important class of heterocycles as intermediates for natural product synthesis and building blocks for constructing new molecular systems[1,2].In addition,isoxazole deriva-tives have been long targeted in synthetic inves-tigation for their known biological activities and pharmacological properties such as hypoglycemic,analgesic,anti-inflammatory and anti-bacterial acti-vities[3~6].Therefore,the isoxazolines and isoxazoles with phosphonate group ar…     

Synthesis and Crystal Structure of 3,（5-Amino-4-ethoxycarbonyl-3-methylthio-1-H- pyrazolyl）-5-phenyl-1,2,4-triazine

1 INTRODUCTION Substituted 1,2,4-triazines represent an important class of nitrogen-containing heterocycles. The 1,2, 4-triazine core is a versatile synthetic platform to access a wide range of condensed heterocyclic ring systems via intramolecular Diels-Alder reactions with a vast array of dienophiles[1~5]. In addition, 1,2, 4-triazines have been associated with diverse activi- ties such as antihypertension and inhibition of pla- telets[6] and antiinflammatory[7], and been a key com- po…     

Synthesis and Crystal Structure of 1-（4-Bromobenzoyl）-3- [5-（E）-styryl-1,3,4-thiadiazol-2-yl]urea

1 INTRODUCTION 1,3,4-Thiadiazole derivatives represent an interes- ting class of compounds possessing broad spectrum biological activities[1~4]. Aroyl ureas are known to exhibit diverse biological effects, such as insecticidal, fungicidal, herbicidal and plant growth regulating activities[5~8]. Therefore, it is worthwhile to investi- gate the compounds incorporating both 1,3,4-thiadia- zole nucleus and aroyl urea group. In the previous paper[9], a series of aroyl ureas containing 1,3,4-t…     

Synthesis and Crystal Structure of 3,3-Dimethyl-7,11-di（thiophene- 2-yl）-2,4-dioxyspiro[5. 5]undecane- 1,5,9-trione

The title compound （C19H18O5S2） has been synthesized by the reaction of thio- phene-2-carboxaldehyde, isopropylidene malonate and 4-chloroaniline using [bmim]Br as solvent, and characterized by IR, ^1H NMR and X-ray single-crystal diffraction. The crystal belongs to monoclinic, space group P21/n with a = 9.4872（15）, b = 9.5148（13）, c = 20.634（3）A, β= 92.209（2）°, V= 1861.2（4）A^3, Mr= 390.45, Z = 4, Dc = 1.393 g/cm^3,μ（MoKα） = 0.313 mm^-1, F（000） = 816, the final R = 0.0685 and wR = 0.1685. X-ray analysis reveals that two six-membered rings adopt chair and planar conformations, respectively.     

Synthesis, Crystal Structure, Fluorescent and Thermal Properties of Sodium Tridecafluorodizirconate Na5Zr2F13 Compound

1 INTRODUCTION Considerable research effort on the heavy metal fluoride glasses like barium, zirconium fluoride and a series of rare-earth fluorozirconate compounds du- ring the last two decades was initiated by the broad optical transmission window of these glasses and thereby the potential for ultralow-loss optical fi- bers[1~10]. The fluorozirconate of alkali metals was first reported in 1938[11], and most of the sodium and potassium fluorozirconates were reported amongthe 1940s and 19…     

Synthesis and Crystal Structure of 4-Bromo-5-ethoxy-3-methyl-5- （naphthalen- 1-yl）- 1-tosyl- 1H-pyrrol-2（5H）- one

The title compound 4-bromo-5-ethoxy-3-methyl-5-(naphthalen-1-yl)-1-tosyl-1H- pyrrol-2(5H)-one 1 (C24H22BrNO4S, Mr = 500.40) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in monoclinic, space group P21/n with a = 8.8562(15), b = 18.118(3), c = 14.055(2) , β = 99.855(3)o, V = 2221.9(6) 3, Z = 4, Dc = 1.496 g/cm3, μ = 1.975 mm-1, λ = 0.71073 , F(000) = 1024, R = 0.0607 and wR = 0.1371.     

Synthesis and Crystal Structure of Tetramethyl 4aH-Pyrido [1, 2-a] Quinoline-1,2,3,4-Tetracarboxylate

1 INTRODUCTION Alkaloids and their derivatives are ubiquitous in natural products, and most of those compounds are of biological activities. Therefore, the structure modifi- cation of alkaloids is always the point that organic chemists and medicinal chemists focus on[1~10]. Qui- nolizine ring system is an important kind of alkaloid, which has a nitrogen atom shared by two six-mem- bered rings. Many medicines have quinolizine ring system, such as reserpine[11, 12] and berberine[13]. How- …     

Synthesis,Spectroscopic Properties and Crystal Structural Characterization of a Triphenyltin(IV) Complex with 5-Bromonicotinic Acid

1 INTRODUCTION Organotin esters of carboxylic acids are widely used as biocides, fungicides and homogeneous ca- talysts in industry[1～3]. Recently, pharmaceutical pro- perties of organotin esters of carboxylic acids have been investigated for their antitumour activity[4, 5]. Studies on organotin compounds containing car- boxylate ligands with additional donor atoms (e.g. N, O or S) that are available for coordination to the tin atom have revealed that new structural types may lead to di…     

Synthesis and Crystal Structure of a New(6,3)-Connected Ni(Ⅱ) Coordination Polymer

The coordination polymer [Ni(dpa)(bpp)]n(H2dpa = 2,4'-biphenyl-dicarboxylic acid,bpp = 1,3-di(4-pyridyl)propane) was hydrothermally prepared and characterized by single-crystal X-ray diffraction,FTIR spectra,elemental analysis and thermal analysis.The crystal is of triclinic system,space group P1 with a = 12.516(5),b = 12.943(5),c = 15.130(5) ,α = 94.331(5),β = 91.827(5),γ = 108.382(5)°,C54H44N4Ni2O8,Mr = 497.18,V = 2315.3(15) 3,Dc = 1.426 g/cm3,F(000) = 1032,μ = 0.875 cm-1,Z = 2,the final R = 0.0496 and wR = 0.1100 for 5365 reflections with Ⅰ 2σ(Ⅰ).X-ray diffraction analysis reveals that the carboxylate group of 2,4'-diphenic acids acting as bridging ligands adopts two coordination modes:bis-mondentate and bidentate chelating.The compound exhibits a two-dimensional(6,3)-connected architecture.     

5-芳基-3-二茂铁基二氢吡唑的合成及晶体结构

吡唑环是许多具有生理活性化合物的关键结构,许多吡唑衍生物都显示了较强的生理活性,如镇静止痛、消炎、杀菌、降血糖以及安眠的活性等~([1-3]),特别是芳基吡唑在医药以及农药方面具有重要的应用~([4,5]).     

Synthesis and Crystal Structure of 5,5-Dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexene-1-one

The title compound 5,5-dimethyl-2-(4-chlorophenyl)(3-hydroxy-5,5-dimethyl-2-cyclohexen-1-one-2-yl)methyl-3-(4-methoxyphenylamino)-2-cyclohexen-1-one has been synthesized,and its crystal structure was characterized by X-ray single-crystal diffraction. The crystal belongs to monoclinic,space group P21/c with a=9.4193(13),b=26.915(4),c=21.188(3),β =101.906(3)°,V =5256.2(13)3,Z =4,C60H68Cl2N2O8,Mr=1016.06,Dc=1.284 g/cm3,F(000)=2160,λ(MoKα)=0.71073,μ=0.182 mm–1,R=0.0530 and wR=0.1131 for 4128 observed reflections (I>2σ(I)). X-ray analysis reveals that there are two independent molecules in the unit and the cyclohexenone rings adopt different conformations. In addition,there are four intramolecular hydrogen bonds in the title molecule.     

Synthesis and Crystal Structure of a Novel Aminothiourea Derivative Bearing Sugar Moiety

5-O-Benzoyl-1,2-O-isopropylidene-α-D-erythro-ketofuranose-3-ulose-3-aminothiose 3 was synthesized and characterized by spectral analysis, and its crystal structure was determined by X-ray diffraction analysis. The crystal belongs to orthorhombic, space group P212121 with a = 6.6276(13), b = 10.993(2), c = 25.027(5) , β = 90°, V = 1823.4(6)3, Z = 4, C16H20N3O5S, Mr = 366.41, Dc = 1.335 g/cm3, μ = 0.208 mm-1, F(000) = 772, S = 1.007, the final R = 0.0465 and wR = 0.1061 for 3251 observed reflections (I > 2σ(I)). Four hydrogen bonds are observed. The absolute configuration of this molecule was confirmed by comparing with that of the original material.     

三氯化镓席夫碱配合物的合成与晶体结构

在无水无氧条件下,利用三氯化镓与水杨醛缩间氯苯胺反应合成了一种新的席夫碱配合物C13H10ClNO·GaCl3。利用元素分析、核磁共振、红外光谱和X射线衍射单晶结构分析对其进行了表征。单晶结构表明标题配合物晶体属于正交晶系,Pnma空间群,晶胞参数:a=17.873(3),b=7.0853(13),c=12.677(2),α=90,β=90,γ=90,V=1605.4(5)3,Z=4,F(000)=808,R1=0.0283,wR2=0.0649。该配合物中镓以四配位形式存在,形成畸变的四面体结构,配合物依靠分子间的氢键作用进一步联结成二维网状结构。     

Synthesis,Crystal Structure and Biological Activity of N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N’-(4-methyl-1,2,3-thiadiazole)-5-formyl-N’-3,5-dichloropyridin-2-yl-diacylhydrazine

The title compound N-tert-butyl-N-(4-methyl-1,2,3-thiadiazole)-5-yl-N'-(4-me-thyl-1,2,3-thiadiazole)-5-formyl-N'-3,5-dichloropyrid-2-yl-diacylhydrazines (C18H17Cl2N7O3S2, Mr = 514.41) has been synthesized by the reaction of N-tert-butyl-N'-3,6-dichloropyridine-2-formyl hydrazine with 4-methyl-1,2,3-thiadiazole-5-carbonyl chloride and triethylamine, and its structure was characterized by 1H NMR, HR MS, and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 27.726(8), b = 11.045(3), c = 14.507(4), β = 96.758(4)°, Z = 8, V = 4412(2) 3, Dc = 1.549 g/cm3, μ = 0.521 mm-1, F(000) = 2112, R = 0.0405 and wR = 0.1153. X-ray analysis indicates that all rings are non-planar in this molecule. The bioassay results indicate that both the title compound and the positive control RH-5992 have weak fungicide activities, while the title compound has good insecticidal activity against Plutella xylostella L. and no insecticidal activity against Culex pipiens pallens.     

Synthesis and Crystal Structure of a Genistein-derived Compound

A genistein derivative, 5-hydroxy-3-（4-hydroxyphenyl）-7-（2-（piperidin- 1-yl）ethoxy）- 4H-chromen-4-one 3, was designed, prepared and structurally characterized by single-crystal X-ray diffraction. X-ray structure analysis reveals that 3 crystallizes in the orthorhombic system, space group Pbca, with a = 16.238（3）, b = 10.308（2）, c = 22.987（5）A, V = 3847.6（13）A3, Z = 8,μ= 0.093 mm^-1, Dc = 1.317 g/cm^3, F（000） = 1616, R = 0.0789 and wR = 0.1554 for 1463 observed reflections with I 〉 2σ（I）.     

Synthesis and Crystal Structure of a Co（ Ⅱ ） Complex with Taurine-5-methyl-2-hydroxyisophthalaldehyde Schiff Bases [Co（C13H16N2O7S2）（H2O）3]2·H2O

The title complex [CoL（H20）3]2·H2O （C26H46N4O21S4CO2）, where L = taurine-5- methyl-2-hydroxyisophthalaldehydes, has been synthesized and characterized by IR and X-ray diffraction analysis. The crystal of the complex belongs to the triclinic system, space group P1, with a = 11.197（4）, b = 13.309（5）, c = 14.486（5） ]A, a = 78.827（13）,β = 70.547（11）, γ = 81.058（13）°, Mr = 996.77, S = 1.08, V= 1987.2（13） A3, Z = 2, Dc = 1.666 g/cm3, F（000） = 1032,μ = 1.131 mm^-1, R = 0.0633 and wR = 0.1293. According to the structural analysis, the Co（ Ⅱ ） ion adopts a slightly distorted six-coordinated octahedral geometry. One N atom of the Schiff base of each molecule was hydrogenated to form hydrogen bond with O atom. Two coterminous molecules packed in one crystal water molecule are linked by intermolecular hydrogen bonds, thus generating an infinite chain constructed by hydrogen bonds.     

Synthesis and Crystal Structure of Ethyl 4-(3,4-Methylenedioxylphenyl)-6-methyl-2-oxo-1,2,3,4-tetrahydropyridine-5-carboxylate under Microwave Irradiation

<正>The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 18.520(2), b = 7.8910(1), c = 21.728(3) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-1 and F(000) = 1280. The structure was refined to R = 0.0486 and wR = 0.1287. There exist intermolecular hydrogen bonds in the crystal.     

Hydrothermal synthesis, crystal structure and properties of Ni(II)-4f complexes based on 1H-benzimidazole-5,6-dicarboxylic acid

Nine novel heterometallic coordination polymers [Ln(2)Ni(Hbidc)(2)(SO(4))(2)(H(2)O)(8)](n) (Ln = Pr (1), Sm (2), Eu (3), Gd (4), Tb (5), Dy (6), Ho (7), Er (8), Yb (9), H(3)bidc = 1H-benzimidazole-5,6-dicarboxylic acid) have been synthesized under hydrothermal conditions and characterized by elemental analysis, FT-IR, TG analysis and single crystal X-ray diffraction. X-ray analysis revealed that all complexes present almost identical three-dimensional (3D) structures with PtS-type topology. Complexes 1-7 are all isomorphous, and the structure variation of polymers 8 and 9 is induced by the lanthanide contraction effect. In additional, the luminescence properties of complexes 2, 3 and 5-7, and the magnetic properties of complexes 4 and 6-8 were investigated.     

Synthesis and Crystal Structure of 4-Arylamino-6-chloropyrido[3,2-d]pyrimidine

The title compounds 4a～c were synthesized and characterized by IR,NMR and MS.The crystal structure of C16H13ClN4O2·HBr·H2O(I),the quaternary ammonium salt of 4c,was determined by X-ray diffraction analysis.I crystallizes in triclinic,space group P1 with a = 8.3121(8),b = 9.3885(8),c = 13.2903(12),α = 106.788(2),β = 95.204(3),γ = 110.871(2)o,V = 905.81(14)3,Z = 2,C16H16BrClN4O3,Mr = 427.68,Dc = 1.568 g/cm3,F(000) = 432.00,μ = 2.446 mm-1,R = 0.0496 and wR = 0.127.X-ray analysis reveals that C(15) in the BrCH2COOH molecule binds to the N(1) of pyrimidine ring to form the quaternary ammonium salt.Two adjacent I molecules are connected by hydrogen bonds through carboxylate oxygen,water molecule and hydrobromic acid.     

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.